(19)
(11) EP 0 745 694 B1

(12) EUROPEAN PATENT SPECIFICATION

(45) Mention of the grant of the patent:
08.12.2004 Bulletin 2004/50

(21) Application number: 96108499.3

(22) Date of filing: 29.05.1996
(51) International Patent Classification (IPC)7C22C 1/00, B22D 17/00

(54)

Method and apparatus for shaping semisolid metals

Verfahren und Vorrichtung zum Formen halbfester Metalle

Procédé et dispositif pour mettre des métaux semi-solides en forme


(84) Designated Contracting States:
DE FR GB IT

(30) Priority: 29.05.1995 JP 13013495
27.06.1995 JP 16089095
14.09.1995 JP 23650195
22.09.1995 JP 24410995
22.09.1995 JP 24411195
26.09.1995 JP 24789795
27.09.1995 JP 24948295
29.09.1995 JP 25276295
29.09.1995 JP 25276895
29.09.1995 JP 25276995
09.11.1995 JP 29076095
08.12.1995 JP 32065095
21.12.1995 JP 33295595
10.04.1996 JP 8784896

(43) Date of publication of application:
04.12.1996 Bulletin 1996/49

(60) Divisional application:
02028272.9 / 1331279

(73) Proprietor: Ube Industries, Ltd.
Ube-shi, Yamaguchi-ken 755-0052 (JP)

(72) Inventors:
  • Adachi, Mitsuru, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)
  • Sasaki, Hiroto, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)
  • Harada, Yasunori, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)
  • Sakamoto, Tatsuo, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)
  • Sato, Satoru, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)
  • Yoshida, Atsushi, c/o Ube Industries, Ltd.
    Oaza Kogushi, Ube-shi, Yamaguchi (JP)

(74) Representative: Strehl Schübel-Hopf & Partner 
Maximilianstrasse 54
80538 München
80538 München (DE)


(56) References cited: : 
EP-A- 0 392 998
EP-A- 0 719 606
EP-A- 0 701 002
WO-A-92/13662
   
  • PATENT ABSTRACTS OF JAPAN vol. 011, no. 078 (M-570), 10 March 1987 & JP-A-61 235047 (NIPPON KOKAN KK), 20 October 1986,
  • PATENT ABSTRACTS OF JAPAN vol. 017, no. 574 (M-1498), 19 October 1993 & JP-A-05 169227 (UBE IND LTD), 9 July 1993,
   
Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention).


Description

Background of the Invention



[0001] This invention relates to a method of shaping semisolid metals , in which a liquid alloy crystal nuclei at a temperature not lower than a is fed into an insulated vessel having heat insulateing effect, holding the alloy for a period from 5 seconds to 60 minutes as it is cooled to the molding temperature where a specified fraction liquid is established, thereby generating fine primary crystals in the alloy solution and the alloy is shaped under pressure. The invention also relates to an apparatus for implementing this method.

[0002] Various methods for shaping semisolid metals are known in the art. A thixo-casting process is attracting researcher's attention these days since it involves a fewer molding defects and segregations,produces uniform metallographic structures and features longer mold lives but shorter molding cycles than the existing casting techniques. The billets used in this molding method (A) are characterized by spheroidized structures obtained by either performing mechanical or electromagnetic agitation in temperature ranges that produce semisolid metals or by taking advantage of recrystallization of worked metals. On the other hand, raw materials cast by the existing methods may be molded in a semisolid state. There are three examples of this approach; the first two concern magnesium alloys that will easily produce an equiaxed microstructure and Zr is added to induce the formation of finer crystals [method (B)] or a carbonaceous refiner is added for the same purpose [method (C)]; the third approach concerns aluminum alloy and a master alloy comprising an Al-5% Ti-1% B system is added as a refiner in amounts ranging from 2 - 10 times the conventional amount [method (D)]. The raw materials prepared by these methods are heated to temperature ranges that produce semisolid metals and the resulting primary crystals are spheroidized before molding. It is also known that alloys within a solubility limit are heated fairly rapidly up to a temperature near the solidus line and, thereafter, in order to ensure a uniform temperature profile through the raw material while avoiding local melting, the alloy is slowly heated to an appropriate temperature beyond the solidus line so that the material becomes sufficiently soft to be molded [method (E)].

[0003] EP-A-0 719 606 discloses a method of shaping a semi-solid metal, in which a partially solid, partially liquid alloy is brought into contact with a cooling unit in the form of an inclined passage and the molten metal flows down on the inclined cooling unit to be fed into an insulated vessel where it is held for a given time whereafter the metallic slurry is shaped under pressure. An essential feature of this known process is the cooling step carried out by means of an inclined cooling unit. ,

[0004] EP-A-0 392 998 discloses a method for making semi-liquid cast aluminium alloys which comprises heating the aluminium alloy to a temperature of about 700°C in a melting oven, generating a laminar flow of aluminium alloy and conveying the said fused alloy onto a tiltable surface so as to adjust the alloy flow falling rate, cooling this surface by a refrigerating medium circulating therein, collecting the semi-liquid aluminium alloy in a vessel and cooling the alloy. This method also requires the use of a cooling jig consisting of a tiltable surface and it is therefore difficult to achieve a uniform temperature of the melt when it is poured into a holding vessel.

[0005] These methods in which billets are molded after they are heated to temperatures that produce semisolid metals are in sharp contrast with a rheo-casting process (F), in which molten metals containing spherical primary crystals are produced continuously and molded as such without being solidified to billets.

[0006] However, the above-described conventional methods have their own problems. method (A) is cumbersome and the production cost is high irrespective of whether the agitation or recrystallization technique is utilized. When applied to magnesium alloys, method (B) is economically disadvantageous since Zr is an expensive element and speaking of method (C), in order to ensure that carbonaceous refiners will exhibit their function to the fullest extent, the addition of Be as an oxidation control element has to be reduced to a level as low as about 7 ppm but then the alloy is prone to burn by oxidation during the heat treatment just prior to molding and this is inconvenient in operations.

[0007] In the case of aluminum alloys, about 500 µm is the size that can be achieved by the mere addition of refiners and it is not easy to obtain crystal grains . finer than 100 µm. To solve this problem, increased amounts of refiners are added in method (D) but this is industrially difficult to implement because the added refiners are prone to settle on the bottom of the furnace; furthermore, the method is costly. Method (E) is a thixo-casting process which is characterized by heating the raw material slowly after the temperature has exceeded the solidus line such that the raw material is uniformly heated and spheroidized. In fact, however, an ordinary dendritic microstructure will not transform to a thixotropic structure (in which the primary dendrites have been spheroidized). What is more, thixo-casting methods (A) - (E) have a common problem in that they are more costly than the existing casting methods because in order to perform molding in the semisolid state, the liquid phase must first be solidified to prepare a billet, which is heated again to a temperature range that produces a semisolid metal. In contrast, method (F) which continuously generates and supplies a molten metal containing spherical primary crystals is more advantageous than the thixocasting approach from the viewpoint of cost and energy but, on the other hand, the machine to be installed for producing a metal material consisting of a spherical structure and a liquid phase requires cumbersome procedures to assure effective operative association with the casting machine to yield the final product.

[0008] The present invention has been accomplished under these circumstances and has as an object providing a method that does not use billets or any cumbersome procedures but which ensures convenience and ease in the production of semisolid metals having fine primary crystals and shaping them under pressure.

[0009] Another object of the invention is to provide an apparatus that can implement this method.

Summary of the Invention



[0010] The object of the invention can be attained by the method of shaping a semisolid metal recited in claim 1, in which a molten aluminum alloy or magnesium alloy containing an element for promoting the generation of crystal nuclei held superheated to less than 100°C above the liquidus temperature is directly poured without using a cooling jig into an insulated vessel made of a material having a thermal conductivity of at least 1.0 kcal/hr·m·°C (at room temperature), held in said insulated vessel for a period from 5 seconds to 60 minutes as it is cooled to the molding temperature where a specified liquid fraction is established wherein said specified liquid fraction ranges from 20% to 90% in the case of high pressure casting operations and from 0.1% to 70% in the case of extruding and forging operations, thereby crystallising fine primary crystals in the alloy solution, and the alloy solution is fed into a forming mold, where it is shaped under pressure.

[0011] According to claim 2, said alloy is an aluminum alloy of a composition within the maximum solubility limit or a hypoeutectic aluminum alloy of a composition at or above the maximum solubility limit.

[0012] According to claim 3, said alloy is a magnesium alloy of a composition within the maximum solubility limit.

[0013] According to claim 4, said aluminum alloy has 0.001% - 0.01% B and 0.005% - 0.3% Ti added thereto.

[0014] According to claim 5, said magnesium alloy has 0.005% - 0.1% Sr added thereto or 0.01% - 1.5% Si and 0.005% - 0.1% Sr added thereto or 0.05% - 0.30% Ca added thereto.

[0015] According to claim 6, in the method of claim 1 the liquid alloy that has been superheated by a degree (X°C) of less than 10°C above the liquidus line is held in the insulated vessel for a period from 5 seconds to 60 minutes as it is cooled to a molding temperature where a specified liquid fraction, which ranges from 20% to 90% in the case of high pressure casting operations and from 0.1% to 70% in the case of extruding and forging operations, is established, such that the cooling from the initial temperature at which said alloy is held in said insulated vessel to its liquidus temperature is completed within a time shorter than the time Y (in minutes) calculated by the relation Y=10-X and that the period of cooling from said initial temperature to a temperature 5°C lower than said liquidus temperature is not longer than 15 minutes, whereby fine primary crystals are crystallised in the alloy solution, which is then fed into a forming mold, where it is shaped under pressure.

[0016] Claim 7 relates to the method according to claim 1, wherein the molten alloy is cooled to a temperature at which a solid fraction appropriate for shaping, which is 10%-80% in the case of high pressure casting operations or 30%-99,9% in the case of extruding and forging operations, is established and wherein the step of cooling said alloy is performed with the top and bottom portions of the vessel being heated by a greater degree than the middle portion or heat-retained with a heat-retaining material having a thermal conductivity of less than 1.0 kcal/hr · m · °C or with either the top or bottom portion of the vessel being heated while the remainder is heat-retained, and said alloy, after being cooled, is fed into a forming mold, where it is shaped under pressure.

[0017] Claim 8 relates for an embodiment of the method according to claim 7, wherein the step of cooling said alloy is performed with the vessel holding said alloy being accommodated in an outer vessel that is capable of accommodating said alloy holding vessel and that has a smaller thermal conductivity than said holding vessel, or that has a thermal conductivity equal to or greater than that of said holding vessel and which has a higher initial temperature than said holding vessel, or that is spaced from said holding vessel by a gas-filled gap, at a rapid cooling rate to obtain a uniform temperature through the alloy in said holding vessel no later than the start of the shaping steep.

[0018] Claim 9 relates to the method according to claim 1, wherein the pressure forming is accomplished with the alloy being inserted into a container on an extruding machine.

[0019] Claim 10 relates to the method according to claim 9, wherein the extruding machine is of either a horizontal or a vertical type or of such a horizontal type in which the container changes position from being vertical to horizontal before shaping and wherein the method of extrusion is either direct or indirect.

[0020] Claim 11 relates to the method according to claim 1, wherein the crystal nuclei are generated by a method in which two or more liquid alloys having different melting points that are held superheated to less than 50°C above the liquidus temperature are mixed directly within the insulated vessel made of a material having a thermal conductivity of at least 1.0 kcal/hr ·m· °C (at room temperature) such that the temperature of the metal as mixed is either just above or below the liquidus temperature.

[0021] Claim 12 relates to the method according to claim 8, wherein the outer vessel is heated either from inside or outside or by induction heating, with such heating being performed only before or after the insertion of the holding vessel into the outer vessel or continued throughout the period not only before but also after said insertion. The process of this invention may be performed using an apparatus for managing the temperature of a semisolid metal slurry to be used in molding equipment in which a molten metal containing a large number of crystal nuclei is poured from a melt holding furnace into a vessel, where it is cooled to produce a semisolid metal slurry containing both a solid and a liquid phase in specified amounts and in which said slurry is directly fed into a molding machine for shaping under pressure, which apparatus is further characterized by compriseing the vessel for holding said molten metal, a vessel temperature control section for managing the temperature of said vessel, a semisolid metal cooling section for managing the temperature of the as-poured molten metal such that it is cooled at an intended rate, and a vessel transport mechanism comprising basically a robot for gripping, moving and transporting said vessel and a conveyor for carrying, moving and transporting said vessel.

[0022] The vessel temperature control section mentioned above 20 comprises a vessel cooling furnace for cooling the vessel in an ambient temperature not higher than a target temperature for the vessel and a vessel heat-retaining furnace for holding the vessel at an ambient temperature equal to said target temperature.

[0023] The semisolid metal cooling section mentioned above comprises a semisolid metal cooling furnace and a semisolid metal annealing furnace for managing the temperature in itself to be higher than the temperature in said semisolid metal cooling furnace.

[0024] The above mentioned semisolid metal cooling furnace in the semisolid metal cooling section mentioned is such that the area around the vessel carried on the conveyor device moving to pass trough said furnace is partitioned into three regions, the upper, middle and lower parts, by means of two pairs of heat insulating plate, one pair consisting of an upper right and an upper left plate and the other pair consisting of a lower right and a lower left plate, with a heater being installed in both said upper and lower parts for heating said two parts at a higher temperature than hot air to be supplied to said central part.

[0025] A preheating furnace is installed at a stage prior to the above mentioned semisolid metal cooling furnace to ensure that both a plinth having a lower thermal conductivity than the vessel and which carries said vessel before it is directed to said semisolid metal cooling furnace and a lid having a lower thermal conductivity than said vessel and which is to be placed to cover it after it accommodate, said molten metal are preheated by being moved to pass through said preheating furnace in advance.

[0026] According to one embodiment the semisolid metal cooling furnace is equipped with a control unit with which the temperature or the velocity of hot air to be supplied into said semisolid metal cooling furnace is controlled to vary with the lapse of time.

[0027] According to one embodiment, the semisolid metal cooling furnace comprises an array of housings each accommodating the vessel as it contains the molten metal and being equipped with an openable cover and hot air feed/exhaust pipes, as well as a mechanism by which a receptacle for carrying said vessel is rotated about a vertical shaft.

[0028] According to one embodiment, a vibrator for vibrating the receptacle mentioned above is provided for each housing.

[0029] According to one embodiment, the semisolid metal cooling furnace for treating the molten metal as poured into a vessel having a thermal conductivity of at least 1.0 kcal/hr·m·°C is supplied with hot air having a temperature in the range from 150°C to 350°C for aluminum alloys and from 200°C to 450°C for magnesium alloys.

[0030] According to one embodiment, the semisolid metal cooling furnace for treating the molten metal as poured into a vessel having a thermal conductivity of less than 1.0 kcal/hr·m·°C is supplied with hot air having a temperature in range from 50°C to 200°C for aluminum alloys and from 100°C to 250°C for magnesium alloys.

[0031] According to one embodiment, the molten metal as poured into the insulated vessel is isolated from the ambient atmosphere by closing the top surface of said vessel with an insulating lid having a heat insulating effect as long as said molten metal is held within said vessel until the molding temperature is reached.

[0032] According to one embodiment the alloy is specified to a hypereutectic Al-Si alloy having 0.005% - 0.03% P added thereto or a hypereutectic Al-Si alloy containing 0.005% - 0.03% P having either 0.005% - 0.03% Sr or 0.001% - 0.01% Na or both added thereto.

[0033] According to one embodiment the alloy in claim 1 or 2 is specified to a hypoeutectic Al-Mg alloy containing Mg in an amount not exceeding a maximum solubility limit and which has 0.3% - 2.5% Si added thereto.

[0034] The pressure forming may be accomplished with the alloy being inserted into a container on an extruding machine.

[0035] According to one embodiment the extruding machine is of either a horizontal or a vertical type or of such a horizontal type in which the container changes position from being vertical to horizontal and the method of extrusion is either direct or indirect.

[0036] According one embodiment, the outer vessel of claim 8 is heated either from inside or outside or by induction heating, with such heating being performed only or before or after the insertion of the holding vessel into the outer vessel or continued throughout the period not only before but also after the insertion.

[0037] With these methods of the invention, liquid alloys (as exemplified by molten Al and Mg alloys) are charged into an insulated vessel having a heat insulating effect and held there for a period from 5 seconds to 60 minutes as they are cooled to a molding temperature, whereby fine and spherical primary crystals are generated in the solution and the resulting semisolid alloy is fed into a mold, where it is pressure formed to produce a shaped part having a homogeneous microstructure.

Brief Description of the Drawings



[0038] In these drawings a part of the figures shows embodiments of a method of shaping a semisolid metal in which - different from the present invention - a cooling jig is used.
The process using a cooling jig is not included in the present invention.

Fig. 1 is a diagram showing a process sequence for the semisolid forming of a hypoeutectic aluminum alloy having a composition at or above a maximum solubility limit;

Fig. 2 is a diagram showing a process sequence for the semisolid forming of a magnesium or aluminum alloy having a composition within a maximum solubility limit;

Fig. 3 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step (not according to this invention);

Fig. 4 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 3;

Fig. 5 is an equilibrium phase diagram for an Al-Si alloy as a typical aluminum alloy system;

Fig. 6 is an equilibrium phase diagram for a Mg-Al alloy as a typical magnesium alloy system;

Fig. 7 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention;

Fig. 8 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art;

Fig. 9 is a diagram showing a process sequence for the semisolid forming of hypoeutectic aluminum alloys having a composition at or above a maximum solubility limit according to examples of the invention.

Fig. 10 is a diagram showing a process sequence for the semisolid forming of magnesium or aluminum alloys having a composition within a maximum solubility limit according to examples of the invention ;

Fig. 11 is an equilibrium phase diagram for Al-Si alloys as a typical aluminum alloy system according to the invention (as recited in claims 11 - 13 and 18);

Fig. 12 is an equilibrium phase diagram for Mg-Al alloys as a typical magnesium alloy system according to the invention;

Fig. 13 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention

Fig. 14 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art (for comparison with the invention);

Fig. 15 is a graph showing how the holding time affects the crystal grain size of a prior art alloy (AZ91);

Fig. 16 is a graph showing how the holding time affects the crystal grain size of a prior art alloy (AC4CH);

Fig. 17 is a graph showing how the degree of superheating of the prior art alloy AZ91 (above the liquidus line) and the holding time (from the initial temperature within an insulated vessel to the liquidus temperature) affect the crystal grain size of the alloy;

Fig. 18 is a graph showing how the degree of superheating of the prior art alloy AC4H (above the liquidus line) and the holding time (from the initial temperature within the insulated vessel to the liquidus temperature) affect the crystal grain size of the alloy;

Fig. 19 is a graph showing how the holding time (from the initial temperature within the insulated vessel to the liquidus temperature minus 5°C) affects the crystal grain size of the prior art alloy AZ91;

Fig. 20 is a graph showing how the holding time (from the initial temperature within the insulated vessel to the liquidus temperature minus 5°C) affects the crystal grain size of the prior art alloy AC4CH;

Fig. 21 is a side view of an apparatus for producing a semisolid forming metal;

Fig. 22 is a perspective view of a cooling jig as part of the nucleus generating section of the apparatus shown in Fig. 21;

Fig. 23 shows in cross section two types of a cooling jig as part of the nucleus generating section of an apparatus for producing a semisolid forming metal;

Fig. 24 is a sectional side view of a cooling jig as part of the nucleus generating section of an apparatus for producing a semisolid forming metal;

Fig. 25 is a plan view showing the general layout of an apparatus for producing a semisolid forming metal;

Fig. 26 is a longitudinal section A-A of Fig. 25;

Fig. 27 is a longitudinal section B-B of Fig. 25;

Fig. 28 is a longitudinal section of an insulated vessel;

Fig. 29 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step ;

Fig. 30 compares two graphs plotting the temperature changes in the metal being cooled within a vessel

Fig. 31 illustrates four methods of managing the temperature within a vessel according to the invention ;

Fig. 32 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step;

Fig. 33 compares the temperature profiles through two semisolid metals one being held within a vessel according to an example of the method of the invention and the other treated by the prior art;

Fig. 34 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art;

Fig. 35 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part obtained according to an example of the method of the invention (as recited in claim 8);

Fig. 36 is a plan view showing the general layout of molding equipment (its first embodiment) according to an example of the method of the invention

Fig. 37 is a plan view of a temperature management unit (its first embodiment) according to an example of the method of the invention

Fig. 38 is a graph showing the specific positions of temperature measurement within a vessel according to an example of the method of the invention

Fig. 39 is a graph showing the temperature history of cooling within the vessel according to an example of the method of the invention ;

Fig. 40 is a graph showing the temperature history of cooling within the vessel according to another example of the method of the invention

Fig. 41 is a graph showing the temperature history of cooling within the vessel according to another example of the method of the invention;

Fig. 42 is a longitudinal section of a semisolid metal cooling furnace according to another example of the method of the invention;

Fig. 43 is a plan view of a temperature management unit (its second embodiment) according to other examples of the method of the invention;

Fig. 44 is a longitudinal section A-A of Fig. 43;

Fig. 45 shows the temperature profiles in the vessel fitted with heat insulators according to an example of the method of the invention as compared with the temperature profile in the absence of such heat insulators;

Fig. 46 is a plan view of a temperature management unit (its third embodiment) according to another example of the method of the invention;

Fig. 47 shows schematically the composition of a temperature controller (its first embodiment) for a semisolid metal cooling furnace according to an example of the method of the invention;

Fig. 48 shows schematically the composition of a temperature controller (its second embodiment) for a semisolid metal cooling furnace according to another example of the method of the invention;

Fig. 49 is a longitudinal section of a vessel rotating unit according to an example of the method of the invention;

Fig. 50 is a plan view showing the general layout of molding equipment according to an example of the method of the invention;

Fig. 51 is a longitudinal sectional view showing in detail the position of temperature measurement within the holding vessel in the example shown in Fig. 50;

Fig. 52 is a graph showing the temperature history of cooling within the holding vessel in the example shown in Fig. 50;

Fig. 53 is a longitudinal section of a semisolid metal cooling furnace (equipped with a vessel vibrator) according to the third embodiment of the method of the invention

Fig. 54 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step;

Fig. 55 is a diagram showing a process sequence for the semisolid forming of a zinc alloy of a hypoeutectic composition ;

Fig. 56 is an equilibrium phase diagram for a binary Zn-Al alloy as a typical zinc alloy system according to the invention

Fig. 57 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the method of the invention

Fig. 58 is a diagrammatic representation of micrograph showing the metallographic structure of a shaped part according to the prior art (for comparison with the method of the invention);

Fig. 59 is a diagram showing a process sequence for the semisolid forming of a hypereutectic Al-Si alloy according to an example of the method of the invention;

Fig. 60 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step according to the example shown in Fig. 59;

Fig. 61 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 60;

Fig. 62 is an equilibrium phase diagram for a binary Al-Si alloy according to another example of the method of the invention ;

Fig. 63 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the method of the invention;

Fig. 64 is a diagrammatic representation of a' micrograph showing the metallographic structure of a shaped part according to the prior art (for comparison with the method of the invention);

Fig. 65 is an equilibrium phase diagram for a binary Al-Mg alloy according to the method of the invention

Fig. 66 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to an example of the method of the invention;

Fig. 67 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art (for comparison with the method of the invention;

Fig. 68 shows process flow starting with the generation of spherical primary crystals and ending with the molding step

Fig. 69 shows two process sequences for the semisolid forming of a hypoeutectic aluminum alloy;

Fig. 70 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step according to the example shown in Fig. 69;

Fig. 71 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 70;

Fig. 72 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the example shown in Fig. 69;

Fig. 73 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art (for comparison with the method of the invention); and

Fig. 74 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step.


Detailed Description of the Invention



[0039] A molten aluminum alloy or magnesium alloy containing an element for promoting the generation of crystal nuclei held superheated to less than 100°C above the liquidus temperature is directly poured without using a cooling jig ... into an insulated vessel having a heat insulating effected, and the alloys are held in that vessel for a period from 5 seconds to 60 minutes as they are cooled to the molding temperature, thereby generating fine and spheroidized primary crystals in the alloy solution and the resulting semisolid alloy is fed into a mold, where it is pressure formed into a shaped part having a homogeneous microstructure.

Example 1



[0040] An example of the invention will now be described in detail with reference to accompanying Figs. 1-8, in which: Fig. 1 is a diagram showing a process sequence for the semisolid forming of a hypoeutectic aluminum alloy having a composition at or above a maximum solubility limit; Fig. 2 is a diagram showing a process sequence for the semisolid forming of a magnesium or aluminum alloy having a composition within a maximum solubility limit; Fig. 3 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step; Fig. 4 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 3; Fig. 5 is an equilibrium phase diagram for an Al-Si alloy as a typical aluminum alloy system; Fig. 6 is an equilibrium phase diagram for a Mg-Al alloy as a typical magnesium alloy system; Fig. 7 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention; and Fig. 8 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art.

[0041] As shown in Figs. 1, 2, 5 and 6 the first step of the process according to the invention comprises:
   superheating the melt of am aluminum or magnesium alloy containing an element for promoting the generation of crystal nuclei, holding the melt superheated to less than 100°C above the liquidus temperature.

[0042] The melt is directly poured into the insulated vessel without being cooled with a jig. The melt is held within the insulated vessel for a period from 5 seconds to 60 minutes at a temperature not higher than the liquidus temperature but higher than the eutectic or solidus temperature, whereby a large number of fine spherical primary crystals are generated in the alloy, which is then shaped at a specified fraction liquid.

[0043] The term "jig" (cooling jig) as used herein means any device that provides a cooling action on the melt as it flows down.

[0044] The term "a specified fraction liquid" means a relative proportion of the liquid phase which is suitable for pressure forming. In high-pressure casting operations such as die casting and squeeze casting, the fraction liquid ranges from 20% to 90%, preferably from 30% to 70%. If the fraction liquid is less than 30%, the formability of the raw material is poor; above 70%, the raw material is so soft that it is not only difficult to handle but also less likely to produce a homogeneous microstructure. In extruding and forging operations, the fraction liquid ranges from 0.1% to 70%, preferably from 0.1% to 50%, beyond which an inhomogeneous structure can potentially occur.

[0045] The "insulated vessel" as used in the invention is a metallic or nonmetallic vessel, or a metallic vessel having a surface coated with nonmetallic materials or semiconductors, or a metallic vessel compounded of nonmetallic materials or semiconductor, which vessels are adapted to be either heatable or coolable from either inside or outside.

[0046] According to the invention, semisolid metal forming will proceed by the following specific procedure. In step (1) of the process shown in Figs. 3 and 4, a complete liquid form of metal M is contained in a ladle 10. In step (2), the metal is treated by the following method to produce an alloy having a large number of crystal nuclei which is of a composition just below the liquidus line: the low-temperature melt of a composition just above the melting point which contains an element to promote the generation of a fine structure is directly poured into the insulated vessel (or a ceramics-coated metallic vessel 30A) having a heat insulating effect. In subsequent step (3) the alloy is held partially molten within the insulated vessel 30 (or 30A). In the meantime, very fine, isotropic dendritic primary crystals result from the introduced crystal nuclei [step (3)-a] and grow into spherical primary crystals as the fraction solid increases with the decreasing temperature of the melt [steps (3)-b and (3)-c]. Metal M thus obtained at a specified fraction liquid is inserted into a die casting injection sleeve 40 [step (3)-d] and thereafter pressure formed within a mold cavity 50a on a die casting machine to produce a shaped part [step (4)].

[0047] The semisolid metal forming process of the invention shown in Figs. 1 - 4 has obvious differences from the conventional thixocasting and rheocasting methods. In the inventive method, the dendritic primary crystals that have been crystallized within a temperature range for the semisolid state are not ground into spherical grains by mechanical or electromagnetic agitation as in the prior art but the large number of primary crystals that have been crystallized and grown from the introduced crystal nuclei with the decreasing temperature in the range for the semisolid state are spheroidized continuously by the heat of the alloy itself (which may optionally be supplied with external heat and held at a desired temperature). In addition, the semisolid metal forming method of the invention is very convenient since it does not involve the step of partially melting billets by reheating in the thixocasting process.

[0048] The casting, spheroidizing and molding conditions that are respectively set for the step of generating and spheroidizing primary crystals and the forming step, are set forth below more specifically. Also discussed below is the criticality of the numerical limitations.

[0049] Insulated vessel 30 for holding the melt the temperature of which has dropped to just below the liquidus line shall have a heat insulating effect in order to ensure that the primary crystals generated will spheroidize and have the desired fraction liquid after the passage of a specified time. The constituent material of the insulated vessel is in no way limited and those which have a heat-retaining property and which wet with the melt only poorly are preferred. If a gas-permeable ceramic container is to be used as the insulated vessel 30 for holding magnesium alloys which are prone to oxidize and burn, the exterior to the vessel is preferably filled with a specified atmosphere (e.g. an inert or vacuum atmosphere). For preventing oxidation, it is desired that Be or Ca is preliminarily added to the molten metal. The shape of the insulated vessel 30 is by no means limited to a tubular form and any other shapes that are suitable for the subsequent forming process may be adopted. The molten metal need not be poured into the insulated vessel but it may optionally be charged directly into a ceramic injection sleeve. If the holding time within the insulated vessel 30 is less than 5 seconds, it is not easy to attain the temperature for the desired fraction liquid and it is also difficult to generate spherical primary crystals. If the holding time exceeds 60 minutes, the spherical primary crystals and eutectic structure generated are so coarse that deterioration in mechanical properties will occur. Hence, the holding time within the insulated vessel is controlled to lie between 5 seconds and 60 minutes. If the fraction liquid in the alloy which is about to be shaped by high-pressure casting processes is less than 20%, the resistance to deformation during the shaping is so high that it is not easy to produce shaped parts of good quality. If the fraction liquid exceeds 90%, shaped parts having a homogeneous structure cannot be obtained. Therefore, as already mentioned, the fraction liquid in the alloy to be shaped is preferably controlled to lie between 20% and 90%. By adjusting the effective fraction liquid to range from 30% to 70%, shaped parts having a more homogeneous structure and higher quality can be easily obtained by pressure forming. If, in the case of shaping Al-Si alloy systems having a near eutectic composition, it is necessary to generate eutectic Si within the insulated vessel while reducing the fraction liquid to 80% or below, Na or Sr may be added as an Si modifying element and this is advantageous for refining the eutectic Si grains, thereby providing improved ductility. The means of pressure forming are in no way limited to high-pressure casting processes typified by squeeze casting and die casting and various other methods of pressure forming may be adopted, such as extruding and casting operations.

[0050] In order to generate more crystal nuclei so as to produce a homogeneous structure comprising fine spherical grains or to ensure that a semisolid alloy containing a large number of crystal nuclei and which has a temperature not higher than the liquidus line is produced from a melt that has been superheated to less than 100°C above the liquidus line and which is not contacted with any jig, various elements may be added to the melt, as exemplified by Ti and B for the case where the melt is an aluminum alloy, and Sr, Si and Ca for the case where the melt is a magnesium alloy. If the Ti addition is less than 0.005%, the intended refining effect is not attained; beyond 0.30%, a coarse Ti compound will form to cause deterioration in ductility. Hence, the Ti addition is controlled to lie between 0.005% and 0.30%. Boron (B) cooperates with Ti to promote the refining of crystal grains but its refining effect is small if the addition is less than 0.001%; on the other hand, the effect of B is saturated at 0.02% and no further improvement is expected beyond 0.02%. Hence, the B addition is controlled to lie between 0.001% and 0.02%. If the Sr addition is less than 0.005%, the intended refining effect is not attained; on the other hand, the effect of Sr is saturated at 0.1% and no further improvement is expected beyond 0.1%. Hence, the Sr addition is controlled to lie between 0.005% and 0.1%. If 0.01% - 1.5% of Si is added in combination with 0.005% - 0.1% of Sr, even finer crystal grains will be formed than when Sr is added alone. If the Ca addition is less than 0.05%, the intended refining effect is not attained; on the other hand, the effect of Ca is saturated at 0.30% and no further improvement is expected beyond 0.30%. Hence, the Ca addition is controlled to lie between 0.05% and 0.30%.

[0051] To obtain fine spherical primary crystals without employing jig 20, the degree of superheating above the liquidus line is set to be less than 100°C and this is to ensure that the molten alloy poured into the insulated vessel 30 having a heat insulating effect is brought to either a liquid state having crystal nuclei or a partially solid, partially liquid state having crystal nuclei at a temperature not lower than the molding temperature. If the melt poured into the insulated vessel 30 is unduly hot, so much time will be taken for the temperature of the melt to decrease to establish a specified fraction liquid that the operating efficiency becomes low. Another inconvenience is that the poured melt M is oxidized or burnt at the surface.

[0052] Table 1 shows the conditions of various samples of semisolid metal to be shaped, as well as the qualities of shaped parts. As shown in Fig. 3, the shaping operation consisted of inserting the semisolid metal into an injection sleeve and subsequent forming on a squeeze casting machine. The forming conditions were as follows: pressure, 950 kgf/cm2; injection speed, 1.5 m/s; mold cavity dimensions, 100 x 150 x 10; mold temperature, 230°C.





[0053] With Comparative Sample 7, the jig 20 was not used; the starting alloy did not contain any grain refiners, so the number of crystal nuclei generated was insufficient.

[0054] In each of Invention Samples 12, 17 and 18 a homogeneous microstructure comprising fine (<150µm) spherical primary crystals was obtained to enable the production of a shaped part having good appearance.

Example 2



[0055] An example of the invention will now be described in detail with reference to accompanying drawings. As shown in Figs. 9 - 12, the invention is such that:
the melt of an aluminum or magnesium alloy that is held superheated to less than 100°C above the liquidus temperature is directly poured into an insulated vessel without using any jig, thereby generating crystal nuclei in the liquid alloy.

[0056] Subsequently, the liquid alloy having crystal nuclei that has been superheated by a degree (X°C) of less than 10°C above the liquidus temperature is held in the insulated vessel for a period from 5 seconds to 60 minutes as said alloy is cooled to a molding temperature that is higher than the eutectic or solidus temperature and where a specified fraction liquid is established, such that the cooling to the liquidus temperature of said alloy is completed within a time shorter than the time Y (in minutes) calculated by the relation Y=10-X and that the period of cooling from the initial temperature at which said alloy is held in the insulated vessel to a temperature 5°C lower than the liquidus temperature is not longer than 15 minutes, whereby fine spherical primary crystals are crystallized in the alloy solution, which is then fed into a forming mold, where it is shaped under pressure.

[0057] The specific procedure of semisolid metal forming to be performed in Example 2 is essentially the same as described in Example 1.

[0058] The casting, spheroidizing and molding conditions that are respectively set for the steps shown in Fig. 3, namely, the step of pouring the molten metal on to the ceramic jig 20, a process step not according to this invention the step of generating and spheroidizing primary crystals and the forming step, are set forth below more specifically. Also discussed below is the criticality of the numerical limitations set forth in subclaims.

[0059] If the alloy to be held within the insulated vessel 30 is superheated such that its initial temperature is at least 10°C above the liquidus line, only unspherical primary crystals of a size of 300µm and larger will form and fine, spherical primary crystals cannot be obtained no matter what conditions are used to cool the alloy to the molding temperature where a specified fraction liquid is established with a view to introducing crystal nuclei into the melt. To avoid this problem, the initial temperature of the alloy held within the insulated vessel 30 is controlled to be less than 10°C above the liquidus line.

[0060] If the alloy to be held within the insulated vessel 30 is superheated such that its initial temperature is less than 10°C above the liquidus line, the alloy must be cooled to the liquidus temperature within a shorter time than the period calculated by the relation Y=10-X , where Y is the time (in minutes) taken for the alloy temperature to drop to the liquidus temperature and X is the degree of superheating (in °C). Otherwise, unspherical primary crystals of a size of 300µm and larger will form as is the case where the degree of superheating is 10°C or more above the liquidus line. To avoid this problem, the alloy is cooled to the liquidus temperature within a shorter time than the period calculated by the relation Y=10-X .

[0061] Even if the alloy is cooled from the initial temperature to the liquidus temperature within a shorter time than the period determined by the relation Y=10-X , unspherical primary crystals of a size of 300µm and larger will form or the size of spherical crystals to be obtained tends to be larger than 200µm if the cooling from the initial temperature to the temperature 5°C lower than the liquidus temperature is completed within 15 minutes. Therefore, the period of cooling from the initial temperature to the temperature 5°C lower than the liquidus temperature should not be longer than 15 minutes.

[0062] Figs. 15 and 16 show how the holding time affects the crystal grain sizes of AZ91 and AC4CH which respectively are typical magnesium and aluminum alloys. The "holding time" is the time for which the metal as poured into the insulated vessel is held until the molding temperature is reached. The "molding temperature" is a typical value at which about 50% fraction liquid is established and it is 570°C for AZ91 and 585t for AC4CH. Obviously, the dependency of the crystal grain size on the holding time differs with the alloy type but in both cases the grain size tends to be greater than 200µm if the holding time exceeds 60 minutes. On the other hand, primary crystals finer than 200µm are prone to occur in the present invention. Figs. 17 and 18 show how the degree by which the AZ91 and AC4CH within the holding vessel are superheated above the liquidus temperature and the holding time from the initial temperature within the insulated vessel to the liquidus temperature will affect the crystal grain sizes of the respective alloys.

[0063] In the area of each graph where the degree of superheating (°C) and the holding time (min) are below the line connecting two points (10, 0) and (0, 10), fine (<200µm) primary crystals are generated in accordance with the invention as shown diagrammatically in Fig. 13. In the area above the line, coarse (>300µm) unspherical primary crystals occur as shown diagrammatically in Fig. 14. Even finer and more homogeneous primary crystals are obtained under the conditions for the holding time and the degree of superheating that are represented by area (C) in Fig. 17 and 18 [the region bound by points (0,6), (5,5) and (6,0) in Fig. 17 and the region bound by points (0,7), (5,5) and (5,0) in Fig. 18]. Figs. 19 and 20 show how the holding time (from the initial temperature within the insulated vessel to the liquidus temperature minus 5°C) affects the crystal grain sizes of AZ91 and AC4CH, respectively. Obviously, the crystal grain size increases with the holding time and if the latter exceeds 15 minutes, there is a marked tendency for the crystal grain size to exceed 200µm and coarse unspherical primary crystals occur. In the present invention where the holding time is less than 15 minutes, there is a marked tendency for the primary crystals to be generated in small sizes less than 200µ m.

Example 3



[0064] An example of the invention will now be described with reference to accompanying Figs. 1, 2, 4 - 8 and 29 - 31, in which: Fig. 1 is a diagram showing a process sequence for the semisolid forming of a hypoeutectic aluminum alloy having a composition at or above a maximum solubility limit; Fig. 2 is a diagram showing a process sequence for the semisolid forming of a magnesium or aluminum alloy having a composition within a maximum solubility limite; Fig. 29 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step; Fig. 4 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 29; Fig. 30 compares two graphs plotting the temperature changes in the metal being cooled within a vessel during step 3 shown in Fig. 29; Fig. 31 illustrates four methods of managing the temperature within a vessel according to the invention; Fig. 5 is an equilibrium phase diagram for an Al-Si alloy as a typical aluminum alloy system; Fig. 6 is an equilibrium phase diagram for a Mg-Al alloy as a typical magnesium alloy system; Fig. 7 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention; and Fig. 8 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art.

[0065] As shown in Figs 1, 2, 5 and 6, the invention is such that:
the melt of an aluminum or magnesium alloy that is held superheated to less than 100°C above the liquidus temperature as it contains an element to promote the generation of crystal nuclei is directly poured into the vessel 30 without using the jig 20. The vessel 30 of a specified wall thickness is adapted to be heatable or coolable from either inside or outside, is made of a material having a thermal conductivity of at least 1.0 kcal/hr·m·°C (at room temperature) and is held at a temperature not higher than the liquidus temperature of said alloy prior to its pouring, and the melt is subsequently cooled to a temperature at which a fraction solid appropriate for shaping is established, such that while the alloy is poured into the vessel 30, its top and bottom portions are heated by a greater degree than the middle portion or that the top or bottom portion is heat-retained with a heat-retaining material having a thermal conductivity of less than 1.0 kcal/hr·m·°C or that the top portion of the vessel is heated by a greater degree than the middle portion while the bottom portion is heat-retained or that the top portion is heat-retained while the bottom portion is heated by a greater degree than the middle portion, whereby nondendritic fine primary crystals are crystallized in the alloy solution while, at the same time, the alloy is cooled at a sufficiently rapid rate to provide a uniform temperature profile through the alloy in the vessel 30, with the cooled alloy being subsequently supplied into a forming mold 50, where it is pressure formed to a shape.

[0066] Four methods of managing the temperature of the vessel 30 and that of the alloy within the vessel 30 are collectively shown in Fig. 31, wherein (a) -(d) correspond to the methods of temperature management.

[0067] The wall thickness of the vessel 30 is desirably such that after pouring of the molten metal, no dendritic primary crystals will result from the metal in contact with the inner surface of the' vessel and yet no solidified layer will remain in the vessel at the stage where the semisolid metal has been discharged from within the vessel just before shaping. The exact value of the wall thickness of the vessel is appropriately determined in consideration of the alloy type and the weight of the alloy in the vessel 30.

[0068] The term "fraction solid appropriate for shaping" means a relative proportion of the solid phase which is suitable for pressure forming. In high-pressure casting operations such as die casting and squeeze casting, the fraction solid ranges from 10% to 80%, preferably from 30% to 70%. If the fraction solid is more than 70%, the formability of the raw material is poor; below 30%, the raw material is so soft that it is not only difficult to handle but also less likely to produce a homogeneous structure. In extruding and forging operations, the fraction solid ranges from 30% to 99.9%, preferably from 50% to 99.9%; if the fraction solid is less than 50%, an inhomogeneous structure can potentially occur.

[0069] The "temperature not higher than the liquidus temperature" means such a temperature that even if the temperature of the metal within the vessel is rapidly lowered to the level equal to the molding temperature, no dendritic primary crystals will result from the melt in contact with the inner surface of the vessel and yet no solidified layer will remain in the vessel at the stage where the semisolid metal is discharged from within the vessel just before shaping. The exact value of the "temperature not higher than the liquidus temperature" varies with the alloy type and the weight of the alloy within the vessel.

[0070] The "vessel" as used in the invention is a metallic or nonmetallic vessel, or a metallic vessel having a surface coated with nonmetallic materials or semiconductors, or a metallic vessel compounded of nonmetallic materials or semiconductors. Coating the surface of the metallic vessel with a nonmetallic material is effective in preventing the sticking of the metal. To heat the vessel, its interior or exterior may be heated with an electric heater; alternatively, induction heating with high-frequency waves may be employed if the vessel is electrically conductive.

[0071] The specific procedure of semisolid metal forming to be performed in Example 3 is essentially the same as described in Example 1.

[0072] Vessel 30 is used to hold the molten metal until it is cooled to a specified fraction solid after its temperature has dropped just below the liquidus line. If the thermal conductivity of the vessel 30 is less than 1.0 kcal/hr·m·°C at room temperature, it has such a good heat insulating effect that an unduly prolonged time will be required for the molten metal M in the vessel 30 to be cooled to the temperature where a specified fraction solid is established, thereby reducing the operational efficiency. In addition, the generated spherical primary crystals become coarse to deteriorate the formability of the alloy. It should, however, be mentioned that if the vessel contains a comparatively small quantity of the melt, the holding time necessary to achieve the intended cooling becomes short even if the thermal conductivity of the vessel is less than 1.0 kcal/hr·m·°C at room temperature. If the temperature of the vessel 30 is higher than the liquidus temperature, the molten metal M as poured into the vessel is higher than the liquidus temperature, so that only a few crystal nuclei will remain in the liquid phase to produce large primary crystals. If the top and bottom portions of the vessel are neither heated nor heat-retained as the molten metal M is cooled until the fraction solid in the metal reaches the value appropriate for shaping, dendritic primary crystals may occur at the site in the top or bottom portion of the vessel that is contacted by the metal M or a solidified layer will grow at that site, thereby creating a nonuniform temperature profile through the metal in the vessel which makes the subsequent shaping operation difficult to accomplish on account of the remaining solidified layer within the vessel. To avoid these difficulties, it is preferred to heat the top or bottom portion of the vessel by a greater degree than the middle portion while the bottom or top portion is heat-retained during the cooling process after the pouring of the metal; if necessary, the top or bottom portion of the vessel may be heated not only during the cooling process following the pouring of the metal but also prior to its pouring and this is another preferred practice in the invention.

[0073] The constituent material of the vessel 30 is in no way limited except on the thermal conductivity and those which are poorly wettable with the molten metal are preferred.

[0074] Table 2 shows the conditions of various samples of semisolid metal to be shaped, as well as the qualities of shaped parts. As shown in Fig. 29, the shaping operation consisted of inserting the semisolid metal into an injection sleeve and subsequent forming on a squeeze casting machine. The forming conditions were as follows: pressure, 950 kgf/cm2; injection speed, 1.0 m/s; casting weight (including biscuits), 30 kg; mold temperature, 230°C.





[0075] In Comparative Sample 1, the thermal conductivity of the holding vessel was small and, in addition, the vessel was heated or heat-retained inappropriately after the pouring of the metal so that the holding time to the shaping temperature was unduly long; what is more, the formation of a solidified layer within the vessel prevented the discharge of the semisolid metal, thus making it impossible to perform shaping. In Comparative Sample 2, the thermal conductivity of the holding vessel was so small that the holding time to the shaping temperature was unduly prolonged. In Comparative Sample 3, the holding vessel was heated or heat-retained inappropriately after the pouring of the metal so that a solidified layer formed within the vessel to prevent the discharge of the semisolid metal; thus making it impossible to start the shaping step. In Comparative Sample 4, the wall thickness of the holding vessel was unduly great and, in addition, the vessel was heated or heat-retained inappropriately after the pouring of the metal so that unspherical primary crystals were generated; what is more, the formation of a solidified layer within the vessel prevented the discharge of the semisolid metal, thus making it impossible to perform shaping. In Comparative Sample 5, the casting temperature was so high that very few crystal nuclei remained within the vessel to yield only coarse unspherical primary crystals as shown in Fig. 8. In Comparative Sample 6, the cooling jig had such a high temperature that the number of crystal nuclei formed was insufficient to produce fine spherical primary crystals and, instead, only coarse unspherical primary grains formed as in Comparative Sample 5. In Comparative Sample 7, the fraction solid in the metal was so small that many segregations occurred within the shaped part.

[0076] In Invention Sample 13 , the metal in the vessel 30 was rapidly cooled with its temperature profile being maintained sufficiently uniform that semisolid metal having nondendritic fine primary crystals was produced in a convenient and easy way. Such alloy was then fed into a forming mold and pressure formed to produce shaped parts of a homogeneous structure having fine (<200µm) spherical primary crystals.

Example 4



[0077] An example of the invention (as recited in claim 8 ) will now be described with reference to the accompanying Figs. 4, 9, 10 and 32 - 35, in which: Fig. 9 is a diagram showing a process sequence for the semisolid forming of hypoeutectic aluminum alloys having a composition at or above a maximum solubility limit; Fig. 10 is a diagram showing a process sequence for the semisolid forming of magnesium or aluminum alloys having a composition within a maximum solubility limit; Fig. 32 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step; Fig. 4 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig. 32; Fig. 33 compares the temperature profiles through two semisolid metals, one being held within a vessel in step (3) shown in Fig. 32 and the other being treated by the prior art without using any outer vessel; Fig. 34 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art; and Fig. 35 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention.

[0078] According to the invention, semisolid metal forming will proceed by the following specific procedure. In step (1) of the process shown n Figs. 32 and 4, a complete liquid form of metal M is contained in a ladle 10. In step (2), the low-temperature melt which contains an element that is added to promote the generation of crystal nucleit is directly poured into the holding vessel 29 which is preliminarily maintained at a temperature not higher than the liquidus temperature.

[0079] In subsequent step (3), the holding vessel 29 is accommodated within the outer vessel 31 lined with a heat insulator 33 on the bottom and then fitted with a lid. Thereafter, the alloy in the holding vessel is held in a semisolid condition with its temperature being lowered, whereby fine particulate (nondendritic) primary crystals are generated from the introduced crystal nuclei. In order to ensure that the temperature in the holding vessel 29 is lowered under the temperature conditions specified in Figs. 9 and 10, the outer vessel 31 is temperature managed such as by internal or external heating or by induction heating, with the heating being performed only before or after the insertion of the holding vessel 29 or for a continued period starting prior to the insertion of the holding vessel and ending after its insertion.

[0080] The "holding vessel" as used in the invention is a metallic or nonmetallic vessel, or a metallic vessel having a surface coated with nonmetallic materials or semiconductors, or a metallic vessel compounded of nonmetallic materials or semiconductors. Coating the surface of the metallic vessel with a nonmetallic material is.effective in preventing the sticking of the metal.

[0081] The "outer vessel" as used in the invention serves to ensure that the alloy in the holding vessel will be cooled within a specified time. To this end, the outer vessel, must have the ability to cool the holding vessel 29 rapidly in addition to a capability for heat-retaining or heating said vessel. To meet this requirement, the temperature of the outer vessel 31 should be lowered to the level equal to the molding temperature within a specified time.

[0082] In order to provide a more uniform temperature profile through the alloy within the holding vessel 29, the outer vessel 31 may be provided with a temperature profile by,for example, heating the top and bottom portions of the outer vessel 31 in a high-frequency heating furnace by a greater degree than the middle portion. In the case where the outer vessel 31 starts to be heated before the holding vessel 29 is inserted and continues to be heated until after its insertion, the heating of the outer vessel 31 may be interrupted temporarily if it is necessary for adjusting the temperature of the alloy within the holding vessel 29.

[0083] The inside diameter of the outer vessel 31 is made sufficiently larger than the outside diameter of the holding vessel 29 to provide a clearance between the outer vessel 31 and the holding vessel 29 accommodated in it. To insure the clearance, a plurality of projections are provided along the outer circumference of the holding vessel 29 and/or the inner circumference of the outer vessel 31. Alternatively, the clearance may be insured by replacing the projections with recesses formed in either the outer circumference of the holding vessel or the inner circumference of the outer vessel.

[0084] The gap between the holding vessel 29 and the outer vessel 31 is typically filled with air but various other gases may be substituted such as inert gases, carbon dioxide and SF6.

[0085] Metal M thus obtained at a specified fraction solid is inserted into a die casting injection sleeve 70 and thereafter pressure formed within a mold cavity 50a on a die casting machine to produce a shaped part.

[0086] The casting, spheroidizing and molding conditions that are respectively set for the steps shown in (see Fig. 9), namely, the step of pouring the molten metal on to the cooling jig, the step of generating and spheroidizing primary crystals and the forming step, are set forth below more specifically. Also discussed below is the criticality of the numerical limitations set forth in claim 8.

[0087] The holding vessel 29 is used to hold the molten metal until it is cooled to a specified fraction solid after its temperature has dropped just below the liquidus line. If the thermal conductivity of the vessel 29 is less than 1.0 kcal/hr·m·°C (at room temperature), it has such a good heat insulating effect that an unduly prolonged time is required for the molten metal M in the holding vessel 29 to be cooled to the temperature where a specified fraction solid is established, thereby reducing the operational efficiency. In addition, the generated spherical primary crystals become coarse to deteriorate the formability of the alloy.

[0088] It should, however, be mentioned that if the holding vessel contains a comparatively small quantity of the melt, the holding time necessary to achieve the intended cooling becomes short even if the thermal conductivity of the vessel is less than 1.0 kcal/hr·m·°C at room temperature. If the temperature of the holding vessel 29 is higher than the liquidus temperature, the molten metal M as poured into the vessel is higher than the liquidus line, so that only a few crystal nuclei will remain in the liquid phase to produce large primary crystals. In order to endure a more uniform temperature profile through the alloy within the holding vessel 29 by means of the outer vessel 31 while the molten metal M is cooled to a temperature where the fraction solid appropriate for shaping is established, either one of the following conditions should be satisfies: the top of the holding vessel 29 should be fitted with a lid; an adequate clearance should be provided between the holding vessel 29 and the outer vessel 31; a heat insulator should be provided in the area where the bottom of the holding vessel 29 contacts the outer vessel 31; or projections or recesses should be provided on either the holding vessel 29 or the outer vessel 31.

[0089] In the example under discussion, the crystal nuclei were generated by the method of the invention recited in claims 2, 9 and 10.

[0090] Table 3 shows the conditions of the holding vessel, the alloy within the holding vessel, and the outer vessel, as well as the qualities of shaped parts. As shown in Fig. 32, the shaping operation consisted of inserting the semisolid metal into an injection sleeve and subsequent forming on a squeeze casting machine. The forming conditions were as follows: pressure, 950 kgf/cm2; injection speed; 1.0m/s; casting weight (including biscuits), 2 kg; mold temperatures, 250°C.





[0091] With Comparative Samples 10 and 11 which did not use the outer vessel, the temperature of the alloy within the holding vessel dropped so rapidly that fine primary crystals formed but, on the other hand, the temperature profile through the semisolid alloy in the holding vessel was poor as shown in the graph on left side of Fig. 33. With Comparative Sample 12, the semisolid metal holding time within the holding vessel was sufficiently long to provide a good temperature profile through the metal in the holding vessel but, on the other hand, unduly large primary crystals formed. With Comparative Sample 13, the casting temperature was so high that the alloy as poured into the holding vessel acquired a sufficiently high temperature to either substantially preclude the generation of crystal nuclei or cause rapid disappearance of crystal nuclei, thereby yielding unduly large primary crystals. With Comparative Sample 14, the fraction liquid in the semisolid metal was high whereas the holding time was short, thereby providing only a poor temperature profile through the semisolid alloy within the holding vessel.

[0092] In Invention Samples 1 - 9, the metal in the vessel was rapidly cooled with its temperature profile being maintained sufficiently uniform that semisolid metals having nondendritic fine primary crystals were produced in a convenient and easy way. Such alloys were then fed into a mold and pressure formed to produce shaped parts of a homogeneous structure having fine (<200µm) spherical primary crystals.

Example 5



[0093] Examples of the invention will now be described in detail with reference to accompanying drawings 36 - 49 and 53, in which: Fig.36 is a plan view showing the general layout of molding equipment (its first embodiment) according to an example of the invention; Fig.37 is a plan view of a temperature management unit (its first embodiment) according to the example of the invention; Fig. 38 is a graph showing the specific positions of temperature measurement within a vessel according to an example of the invention; Figs. 39, 40 and 41 are graphs showing the temperature history of cooling within the vessel under different conditions; Fig. 42 is a longitudinal section of a semisolid metal cooling furnace according to another example of the invention; Fig. 43 is a plan view of a temperature management unit (its second embodiment) according to yet another example of the invention;Fig.44 is a longitudinal section A - A of Fig.43; Fig.45 shows the temperature profiles in the vessel fitted with heat insulators according to an example of the invention; Fig. 46 is a plan view of a temperature management unit (its third embodiment) according to another example of the invention; Fig. 47 shows schematically the composition of a temperature controller for a semisolid metal cooling furnace (its first embodiment) according to an example of the invention; Fig. 48 shows schematically the composition of a temperature controller (its second embodiment) for a semisolid metal cooling furnace according to another example of the invention;Fig.49 is a longitudinal section of a vessel rotating unit according to an example of the invention; and Fig. 53 is a longitudinal section of a semisolid metal cooling furnace as it is equipped with a vessel vibrator according to another example of the invention.

[0094] As Fig.36 shows, the molding equipment generally indicated by 300 consists of a melt holding furnace 14 for feeding the molten metal as a molding material (containing a large number of crystal nuclei), a molding machine 200, and a temperature management unit 104 for managing the temperature of the melt until it is fed to the molding machine 200. The molten metal held within the furnace 14 contains a large number of crystal nuclei.

[0095] As also shown in Fig.36, the temperature management unit 104 consists of a semisolid metal cooling section 110 and a vessel temperature control section 140; the semisolid metal cooling section 110 is composed of a semisolid metal cooling furnace 120 and a semisolid metal slowly cooling furnace 130 which are connected in a generally rectangular arrangement by means of a transport mechanism such as a conveyor 170 whereas the vessel temperature control section 140 is composed of a vessel cooling furnace 150 and a vessel heat-retaining furnace 160. The temperature management unit 104 is also equipped with a robot 180 which grips the vessel 102 and transports it to one of the specified positions A - F (to be described below).

[0096] The temperature management unit 104 is operated as follows. An empty vessel 102 is first located in the heating vessel pickup position A. The robot 180 then transfers the vessel 102 to the position B, where the vessel is charged with a prescribed amount of the molten metal from the melt holding furnace 14. Thereafter, the robot 180 transports the vessel 102 to the filled vessel rest position C; subsequently, the vessel is cooled as it is carried by the conveyor 170 to pass through the semisolid metal cooling furnace 120 in a specified period of time. The vessel 102 leaving the furnace 120 reaches the slurry vessel rest position D, from which it is immediately transferred to the sleeve position E by the robot 180 if the injection sleeve 202 in the molding machine 200 is ready to accept the molten metal; at position E, the slurry ofsemisolid metal in the vessel is poured into the injection sleeve 202. If the injection sleeve 202 is not ready to acceptthe molten metal when the vessel 102 has reached the slurry vessel rest position D (i. e., if the molding machine is operating to perform pressure forming), the slurry of semisolid metal within the vessel will progressively solidify upon cooling while it is waiting for acceptance in the position D, thereby making it impossible for all the slurry to be discharged from the vessel or the crystal nuclei in the slurry will disappear to cause deterioration in the quality of the shaped part. In order to avoid these problems, the vessel 102 is forwarded to the semisolid metal slowly cooling furnace 130,where it waits for the molding machine 200 to become completely ready for the acceptance of the molten metal while ensuring against its rapid cooling.

[0097] The vessel 102 from which the slurry of semisolid metal having satisfactory properties has been emptied into the injection sleeve 202 is then transferred to the empty vessel rest position F by means of the robot 180, carried by the conveyor 170 into the vessel cooling furnace 150, where it is cooled for a specified time, passed through the vessel heat-retaining furnace 160 as it is held at a suitable temperature, and is thereafter returned to the heating vessel pick up position A.

[0098] A specific embodiment of the temperature management unit 104 is shown in Fig.37. In this first embodiment, aluminum alloys are to be treated at a comparatively small scale with the molten metal being poured in an amount of no more than 10 kg; the system configuration is such that the molding cycle on the molding machine 200 is about 75 seconds and the time of passage through the semisolid metal cooling furnace 120 and the vessel temperature controller 140 (i. e., consisting of the vessel cooling furnace 150 and the vessel heat-retaining furnace 160) is 600 seconds in total. If the total passage time is longer than 600 seconds, the overall equipment becomes impractically bulky and the volume of the slurry in process which results from machine troubles and which has to be discarded is increased and these are by no means preferred or the purpose of constructing commercial production facilities. Considering these points and in order to achieve consistent temperature management for a small quantity of slurry having good properties, the vessel 102 is made of an Al2O3 · SiO2 composite having a small thermal conductivity (0.3 kcal/hr·m·°C). As a result, a slurry of semisolid metal having satisfactory properties can be obtained if only the temperature of the vessel 102 is retained by circulation of hot air the temperature of which is set at a constant value of 120°C.

[0099] The system shown in Fig.37 has the following differences from the system of Fig.36. Since the vessel 102 is made of the Al2O3 · SiO2 composite, it has a sufficiently small thermal conductivity that one only need supply the interior of the semisolid metal cooling furnace 120 (which is set at a temperature of 200°C) with a circulating hot air flow of a constant temperature from a hot air generating furnace 122. In addition, one only need equip the semisolid metal slowly cooling furnace 130 (which is set at a temperature of 550 °C) and the vessel heat-retaining furnace 160 (which is set at a temperature of 100°C) with heaters 132 and 162, respectively.With these provisions, the temperature in the vessel 102 can be managed correctly to ensure that slurries of semisolid metal having satisfactory properties can be produced in a short time while assuring farily consistent temperature management. The temperature in the vessel is optimally at 70°C; to ensure that the temperature in the vessel is consistently managed at the optimal 70°C, adequate heat removal must be effected in the vessel cooling furnace 150; otherwise, the temperature in the vessel 102 becomes undesirably high. To deal with this problem, the vessel cooling furnace 150 is fitted with a blower 152 and a blow nozzle 152a such that a fast air flow is blown at room temperature to achieve forced cooling.

[0100] For system assessment on the management of the temperature in the vessel 102, a sheathed thermocouple was set up in the vessel and temperature data were taken under various conditions. Fig. 38 shows five different positions (A) - (E) of temperature measurement in the vessel 102, into which the 1.0- mm thick sheathed thermocouple was inserted.

[0101] Fig.39 shows the temperature history of cooling under condition I, i. e., the vessel temperature control section 140 was not divided into the vessel cooling furnace 150 and the vessel heat-retaining furnace 160 and a hot air flow having the target temperature of 70°C was circulated within the monolithic vessel temperature control section 140 at a velocity of about 5 m/sec. With this approach, the temperature in the vessel dropped to only about 200 °C which was far from the target value.

[0102] Fig.40 shows the temperature history of cooling under condition II, i. e., a hot air flow having a temperature of 70°C was circulated at a higher velocity of about 30 m/sec. This approach was effective in further reducing the temperature in the vessel but not to the desired level of 70°C.

[0103] Fig.41 shows the temperature history of cooling under condition III, i. e., the vessel temperature control section 140 was divided into the vessel cooling furnace 150 and the vessel heat-retaining furnace 160, with an air flow at ordinary temperature being circulated within the cooling furnace 150 at a velocity of 30 m/sec whereas the atmosphere in the vessel heat-retaining furnace 160 had its temperature raised to 70°C by means of an electric heater. It was only with this system that the temperature in the vessel could be managed to be stable at the intended 70°C.

[0104] If, in the case of treating aluminum alloys at a large scale, the vessel 102 is made of ceramics having thermal conductivities of no more than 1 kcal/m·hr·°C, the time to cool the slurry of semisolid metal becomes impractically long. Therefore, in the second embodiment of the temperature management unit 104 which is adapted for handling comparatively large volumes of aluminum alloys such that the molten alloy is poured in an amount of 20 kg or more, the vessel 102 is made of SUS304 (see Fig.43) rather than the ceramics which are used with the first embodiment shown in Fig.37 and which require a prolonged cooling time. The resulting differences between the first embodiment of the temperature management unit 104 (Fig.37) and the second embodiment are as follows.

[0105] In order to ensure smooth recovery of the slurry from the vessel 102, its inner surfaces have to be coated with a water-soluble (which is desirable for ensuring against gas evolution) spray of a lubricant and, to this end, a spray position (spray equipment) is provided between the vessel cooling furnace 150 and the vessel heat-retaining furnace 160. Accordingly, the vessel 102 emerging from the vessel cooling furnace 150 must be kept at a sufficient temperature (200 °C) to allow for the deposition of the spray solution; to meet this requirement, hot air at 200°C is applied against the vessel through a blow nozzle. As the result of the application of the water-soluble spray, the vessel 102 experiences a local temperature drop. In order to ensure that the vessel 102 has a uniform temperature of 200 °C throughout, a hot air flow at 200 °C is circulated within the vessel heat-retaining furnace 160 while it is agitated by a rotating fan to ensure uniformity in the temperature of the vessel 102.

[0106] The vessel 102 which is made of SUS304 allows thermal diffusion through it, so even if the semisolid metal cooling furnace 120 is of the design shown in Fig.42, no sharp border line can be drawn between the high-temperature range of the vessel (consisting of its top and bottom portions) and the low-temperature range (the middle portion of the vessel). To deal with this problem, a preheating furnace 190 is provided as accessory equipment on a lateral side of the semisolid metal cooling furnace 120 and, as shown in Fig.44, a lid 102a made of a ceramic material (Al2O3 · SiO2 composite) and a plinth 102b are used to heat-retain the top and bottom of the vessel 102 while it is heated in the preheating furnace 190 before it is charged into the semisolid metal cooling furnace 120.

[0107] The interior of the semisolid metal cooling furnace 120 is supplied with hot air from the hot air generating furnace via two sets of blow nozzles 124, one being in the upper position and the other in the lower position. The supplied hot air is circulated within the cooling furnace 120 with its temperatureand velocity being 220°C and 5 m/sec at the entrance and 180 C and 20 m/sec at the exit, whereby the semisolid metal is cooled comparatively slowly in the initial cooling period but cooled rapidly in the latter period.

[0108] Thus, the present invention provides a method of temperature management in which the step of managing the temperature in the vessel 102 at an appropriate level before it is supplied with the molten metal is distinctly separated from the step of managing the temperature in the vessel 102 in such a way that the as poured molten metal can be cooled at a desired appropriate rate; the invention also provides the apparatus for temperature management 104 which is capable of automatic performance of these steps in an efficient and continuous manner. Also proposed by the invention is a system configuration that implements the respective steps by means of the vessel temperature control section 140 and the semisolid metal cooling section 110.

[0109] In a specific embodiment, the vessel temperature control section 140 is composed of the vessel cooling furnace 150 capable of forced cooling with a circulating hot air flow that provides an appropriate cooling capacity by controlling the temperature and velocity of the air passing through the furnace and the vessel heat-retaining furnace 160 which controls the temperature of the atmosphere to lie at the target value in the vessel 102 and which maintains the vessel 102 at said temperature of the atmosphere. It should be noted here that the temperature to which the vessel cooling furnace 150 and the vessel heat-retaining furnace 160 should be controlled differs between aluminum and magnesium alloys. In the case of aluminum alloys, the interior of the vessel cooling furnace 150 is controlled to lie between room temperature and 300 °C whereas the interior of the vessel heat-retaining furnace 160 is controlled to lie between 50 °C and 350 °C; in the case of magnesium alloys, the interior of the vessel cooling furnace 150 is controlled to lie between room temperature and 350°C whereas the interior of the vessel heat-retaining furnace 160 is controlled to lie between 200 °C and 450 °C.

[0110] The semisolid metal cooling section 110 is composed of the semisolid metal cooling furnace 120 which is adapted to circulate hot air at an appropriate temperature such as to accomplish cooling within the shortest possible time that produces the slurry of semisolid metal with satisfactory properties and the semisolid metal slowly cooling furnace 130 which is designed to maintain the slurry of semisolid metal for 2 - 5 minutes in a temperature range appropriate for shaping such as to be adaptive for the specific molding cycle on the molding machine 200. Again, the temperature to which the semisolid metal cooling furnace 120 should be controlled differs between aluminum and magnesium alloys. In the case of aluminum alloys, the temperature should be controlled to lie between 150 °C and 350 °C and in the case of magnesium alloys, the temperature should be controlled to lie between 200 °C and 450 °C. On the other hand, the interior of the semisolid metal slowly cooling furnace 130 should be controlled to be at 500 °C and above in both cases.

[0111] If the injection sleeve 202 on the molding machine 200 is ready to accept the molten metal just at time when the vessel 102 holding the metal has left the semisolid metal cooling furnace 120, the metal is immediately fed (poured) into the molding machine 200 without being directed into the semisolid metal slowly cooling furnace 130. Conversely, if the injection sleeve 202 is not ready to accept the molten metal since the molding machine 200 is operating, the vessel 102 leaving the semisolid metal cooling furnace 120 is transferred to the semisolid metal slowly cooling furnace 130.

[0112] As shown in Figs.37 and 42, the semisolid metal cooling furnace 120 has the vessel 102 carried on the conveyor 170 via a heat insulating plate 120c and the inner surfaces on the sidewall of the furnace 120 is partitioned by an upper and a lower heat insulating plate 120b in the middle portion of its height, with hot air (set at an appropriate temperature of 120°C) being circulated through the partitioned area to establish a low-temperature region; at the same time, the inner surfaces of both top and bottom portions of the furnace 120 are heated with electric heaters 120a (set at a temperature of 500°C) to establish a high-temperature (ca. 500 °C) region, thereby ensuring that a uniform temperature is provided throughout the molten metal in the vessel 102.

[0113] A first version of the heating system in the semisolid metal cooling furnace 120 according to the invention is such that either the temperature or the velocity of the circulating hot air is controlled to vary appropriately with the lapse of time or, alternatively, both the temperature and the velocity of the hot air are controlled to vary simultaneously with the lapse of time.

[0114] The first specific embodiment of the heating system is as shown in Fig.47 and comprises a hot air line for supplying a hot air flow into the semisolid metal cooling furnace 120, an air line from which an air flow at ordinary temperature emerges to combine with the hot air to lower its temperature, a damper for controlling the quantity of the air flowing through the air line, and a damper opening controller.

[0115] The second specific embodiment of the heating system is as shown in Fig.48 and comprises a temperature sensor installed within the semisolid metal cooling furnace 120, a hot air line for supplying a hot air flow into the furnace, an air line that combines with the hot air line, an automatic damper installed on the air line, and a damper opening controller that performs feed back control on the damper opening on the basis of the data obtained by measurement with the temperature sensor. The opening of the automatic damper is controlled on the basis of the data for the temperature in the furnace and the hot air is mixed with an appropriate amount of air and fed into the furnace, whereby the temperature and the velocity of the circulating hot air are controlled such that the molten metal will be cooled at a desired rate.

Example 6



[0116] An example of the invention will now be described specifically with reference to accompanying Figs. 43 - 53, in which: Fig.50 is a plan view showing the general layout of molding equipment; Fig. 43 is a plan view of the temperature management unit (its first embodiment); Fig.51 is a longitudinal sectional view showing in detail the position of temperature measurement within the holding vessel; Fig. 52 is a graph showing the temperature history of cooling within the holding vessel; Fig.44 is a longitudinal section A - A of Fig.43; Fig.46 is a plan view of the temperature management unit (its second embodiment) according to another example of the invention; Fig. 45 shows the temperature profiles in the vessel fitted with heat insulators as compared with the temperature profile in the absence of such heat insulators; Fig.47 shows schematically the composition of the temperature control unit (its first embodiment) for a semisolid metal cooling furnace; Fig.48 shows schematically the composition of the temperature control unit (its second embodiment) for a semisolid metal cooling furnace according to another example of the invention; Fig.49 is a longitudinal section of the semisolid metal cooling furnace according to the second embodiment in which it is equipped with a vessel rotating mechanism; and Fig.53 is a longitudinal section of the semisolid metal cooling furnace according to the third embodiment in which it is equipped with a vessel vibrating mechanism.

[0117] As shown in Fig.50, the molding equipment generally indicated by 104 consists of a melt holding furnace 10 for feeding the molten metal as a molding material, a molding machine 200 and a temperature management unit 100 for managing the temperature of the melt until it is fed to the molding machine 200.

[0118] As also shown in Fig.50, the temperature management unit generally indicated by 104 consists of a semisolid metal cooling section 110 and a vessel temperature control section 140; the semisolid metal cooling section 110 is composed of a semisolid metal cooling furnace 120 and a semisolid metal slowly cooling furnace 130 which are connected in a generally rectangular arrangement by means of a transport mechanism such as a conveyor 170 whereas the vessel temperature control section 140 is composed of a vessel cooling furnace 150 and a vessel heat-retaining vessel 160. The temperature management unit 100 is also equipped with a robot 180 which grips the vessel 102 and transports it to one of the specified positions A F (to be described below). The vessel 102 moves in the direction of arrows.

[0119] In the first embodiment of the temperature management unit 104, the preheating furnace 190 is provided near and parallel to the semisolid metal cooling furnace as shown in Figs.43 and 44. The purpose of the preheating furnace 190 is to ensure that both the plinth 102b placed under the melt containing vessel 102 and the lid 102a placed on top of the vessel 102 are preliminarily heated to a higher temperature than the hot air to be passed through the semisolid metal cooling furnace 120 such that uniformity will be assured for the temperature of the melt within the vessel as it is cooled in the semisolid metal cooling furnace 120. To this end, both the lid 102a and the plinth 102b which are carried on the conveyor 170 will be heated by the hot air being injected through the blow nozzle 192 as they move together with the conveyor 170 (see Fig.44).

[0120] The temperature management unit 104 is operated as follows. An empty vessel 102 is first located in the heating vessel pickup position A. The robot 180 then transfers the vessel 102 to the position B, where the vessel is charged with a prescribed amount of the molten metal from the melt holding furnace 10 (which holds the molten metal containing a large number of crystal nuclei). Thereafter, the robot 180 transports the vessel 102 to the filled vessel rest position C, where it is placed on the plinth 102b and has its top covered with the lid 102a (both the lid 102a and the plinth 102b are preliminarily heated with the preheater 190); subsequently, the vessel is cooled as it is carried by the conveyor 170 to pass through the semisolid metal cooling furnace 120 in a specified period of time. The vessel 102 leaving the furnace 120 reaches the slurry vessel rest position D, from which it is immediately transferred to the sleeve position E by the robot 180 if the injection sleeve 202 in the molding machine 200 is ready to accept the molten metal; at position E, the slurry of semisolid metal in the vessel is poured into the injection sleeve 202. If the injection sleeve 202 is not ready to accept the molten metal when the vessel 202 has reached the slurry vessel rest position D (i. e., if the molding machine is operating to perform pressure forming), the slurry of semisolid metal within the vessel will progressively solidify upon cooling while it is waiting for acceptance in position D, thereby making it impossible for all the slurry to be discharged from the vesselor the crystal nuclei in the slurry will disappear to cause deterioration in the quality of the shaped part. In order to avoid these problems, the vessel 102 is forwarded to the semisolid metal slowly cooling furnace 130, where it waits for the molding machine 200 to become completely ready for the acceptance of the molten metal while ensuring against its rapid cooling.

[0121] The vessel 102 from which the slurry of semisolid metal having satisfactory properties has been emptied into the injection sleeve 202 is then transferred to the empty vessel rest position F by means of the robot 180, carried by the conveyor 170 into the vessel cooling furnace 150, where it is cooled for a specified time, passed through the vessel heat-retaining furnace 160 as it is held at a suitable temperature, and is thereafter returned to the heating vessel pickup position A.

[0122] A specific embodiment of the temperature management unit 104 is shown in Fig.43. In this first embodiment, aluminum alloys are to be treated on a comparatively large scale with the molten metal being poured in an amount of at least 20 kg; the system configuration is such that the molding cycle on the molding machine 200 is about 150 seconds and the time of passage through the semisolid metal cooling furnace 120 and the vessel temperature control section 140 (i. e. consisting of the vessel cooling furnace 150 and the vessel heat-retaining furnace 160) is 600 seconds in total. If the total passage time is longer than 600 seconds, the overall equipment becomes impractically bulky and the volume of the slurry in process which results from machine troubles and which has to be discarded is increased and these are by no means preferred for the purpose of constructing commercial production facilities.

[0123] To satisfy these cycle conditions and yet to produce slurries of good properties, details of the system have been determined as follows. SUS304 was adopted as the constituent material of the vessel (in the case of a comparatively small-scale operation with the molten metal being poured in an amount of no more than 10 kg, materials of small thermal conductivity provide comparative ease in temperature management; however, in a large-scale operation like the case under discussion, the use of ceramics and other materials of small thermal conductivity as the constituent material of the vessel requires an unduly prolonged time to cool the slurry, resulting in the failure to satisfy the cycle time requirementset forth above).

[0124] In order to ensure smooth recovery of the slurry from the vessel 102, its inner surfaces had to be coated with a water-soluble (which is desirable for ensuring against gas evolution) spray of a lubricant and, to this end, a spray position was provided between the vessel cooling furnace 150 and the vessel heat-retaining furnace 160. The vessel 102 emerging from the vessel cooling furnace 150 had to be cooled within 5 minutes down to a temperature (200 °C - 250 °C) that would allow for effective deposition of the spray; to meet this requirement, hot air at 100 °C was applied against the vessel through a blow nozzle.

[0125] As the result of the application of the water-soluble spray, the vessel 102 experienced a local temperature drop. In order to ensure that the vessel 102 would have a uniform temperature of 180°C - 190 °C throughout to provide a uniform temperature profile through the slurry, the vessel 102 was heated in the vessel heat-retaining furnace 160 in which a hot air flow at 190 °C was circulated by means of a fan.

[0126] In order to provide a uniform temperature profile through the slurry in the vessel, preheating furnace 190 was installed as an accessory and the plinth 102b and lid 102a which were each made of a heat insulator (Al2O3 • SiO2 composite) were heated at 350 °C before they were set up on the vessel 102; this arrangement allowed the vessel 102 to be inserted into the semisolid metal cooling furnace 120 together with the lid 102a and plinth 102b.

[0127] The interior of the semisolid metal cooling furnace 120 was equipped with two sets each of hot air generating furnaces and blow nozzles, through which hot air was supplied to circulate within the furnace 120, with its temperature and velocity being 220°C and 5 m/sec at the entrance and 180 °C and 20 m/sec at the exit, whereby the semisolid metal was cooled comparatively slowly in the initial cooling period but cooled rapidly in the latter period.

[0128] For management of the temperature in the vessel 102, a sheathed thermocouple was set in the vessel to take data on the temperature. Detailed discussion will follow based on the thus taken temperature data.

[0129] Fig.51 shows the position of temperature measurement in the vessel 102. As shown enlarged on the right-hand illustration, a hole was made in the outer surface of the sidewall of the vessel to a depth at one half the wall thickness and thermocouple was inserted into the hole and spotwelded.

[0130] Fig.52 shows the temperature history of cooling of the vessel 102. The vessel temperature control section 140 was divided into the vessel cooling furnace 150 and the vessel heat-retaining furnace 160 and, as already mentioned above, the vessel cooling furnace 150 was so adapted that "hot air at 100 °C was applied against the vessel through the blow nozzles" whereas the vessel heat-retaining vessel 160 was designed to "permit circulation of hot air at 190 °C."

[0131] The system under discussion requires that the " spray should be deposited" within a limited time period while "a uniform temperature (180°C - 190 °C) should be established throughout the vessel 102". To meet these requirements, the vessel temperature control section 140 was divided into the vessel cooling furnace 150 and the vessel heat-retaining furnace 160 and optimal temperature management was performed in each furnace.

[0132] The second embodiment of the temperature management unit 100 shown in Fig. 46 was chiefly intended for the treatment of magnesium alloys. As typically shown in Fig.49, the temperature management unit 100 comprises a plurality of linearly arranged housings 120A in a generally cubic shape, each being fitted with a top cover 120B that could be opened or closed by means of an air cylinder 120C. Hot air could be forced into the housings 120A. With the cover 120B open, the melt containing vessel 102 was placed on the plinth 102b at the bottom of each housing 120A and a lid 102a fixed to the inside surface of the cover 120B was fitted over the top of the vessel 102 so that it would ensure a heat insulating effect during the cooling of the vessel 102. The vessel was adapted for transfer into or out of the housing 120A by manipulation of the robot 180.

[0133] Thus, the semisolid metal cooling furnace 120 according to the first embodiment shown in Fig.44 is of a continuous type in which the vessel 102 is carried by the conveyor 170 while the furnace is operating and, in contrast, the semisolid metal cooling furnace 120 according to the second embodiment shown in Fig.46 is of a batch system.

[0134] As also shown in Fig.49, the plinth 102b seated on the bottom of the housing 120A is coupled to a rotational drive mechanism consisting of a motor 121a, a chain 121b, a sprocket121c, a bearing 121d, etc. and this drive mechanism allows the vessel 102 to rotate freely during its cooling operation.

[0135] Another embodiment of the semisolid metal cooling furnace 120 is shown in Fig.53; it is fitted with not only a vibrator 121f that is actuated with an ultrasonic oscillator 121e but also a water-cooled booster 121g and this arrangementwill provide effective vibrations to the vessel 102.

[0136] Fig.45 shows the temperature profiles obtained by fitting the top and bottom of the vessel with the lid 102a and the plinth 102b which were each made of a heat insulator (Al2O3 • SiO2 composite). Obviously, the use of the heat insulator produced uniform temperature profiles as compared with the case of using no such heat insulators. The uniformity in temperature profile was further improved by preheating the insulator.

[0137] We next discuss the "high-viscosity region". The alloy to be treated in the case at issue is AC4C which has a eutectic temperature of 577 °C. Within a narrow temperature range centered at this eutectic point, the fraction solid increases sharply from 56 % to 100 % and the viscosity will inturn rises noticeably. Hence, the region of 56 % to 100 % fraction solid may well be considered as the "high-density region". When no heat insulator was used, both the top and bottom portions of the vessel were entirely covered with the "high-density region" and in a case like this, the desired slurry would not form smoothly. In contrast, the mere use of the heat insulator resulted in a significant decrease in the "high-density region", which barely remained at the corners. Obviously, the "high-density region" totally disappeared when the heat insulator was heated. In the case under discussion, the heat insulator had to be heated but with smaller vessel sizes, there was no particular need to heat the heat insulator.

[0138] Magnesium alloys involve difficulty in temperature management since they have small latent heat and will cool rapidly. To deal with this problem, the semisolid metal cooling furnace 120 according to the second embodiment shown in Fig.46 have the following differences from the first embodiment shown in Fig.43.

[0139] First, silicon nitride was used as the constituent material of the vessel but it was difficult to obtain a uniform temperature profile through the slurry in the vessel. Under the circumstances, the semisolid metal cooling furnace 120 for handling vessels having a diameter of more than 100 mm had to be equipped with a vessel rotating mechanism as indicated by 120X in Fig.49 or a vessel vibrator as indicated by 120Y in Fig.53. (With vessels having diameters ranging from 50 mm to less than 100 mm, neither the vessel rotating mechanism nor the vessel vibrator had to be installed. With vessel diameters of 100 mm - 200 mm, a vessel vibrator as indicated by 120Y in Fig. 53 was necessary and with vessel diameters of more than 200 mm, a vessel rotating mechanism capable of more vigorous agitation as indicated by 120X in Fig. 49 had to be employed.)

[0140] It was also necessary to perform the temperature management in such a manner as to be flexible with time; to meet this need, a furnace temperature controller as indicated by 120Z in Fig.47 or 48 was installed. (With vessel diametersof less than 100 mm, the rate of cooling the slurry was so sensitive to the variations in the temperature within the furnace that it was necessary to control the temperature in the furnace by the mechanism shown in Fig.47. With vessel diameters of less than 70 mm, not only the furnace temperature controller but also a feedback control system as shown in Fig.48 was necessary.)

[0141] In order to permit the addition of these capabilities, the semisolid metal cooling furnace 120 was designed as a batch system of the type shown in Fig.46 and the timing for the transfer of the vessel into and out of the furnace 120 was controlled by the robot 180.

[0142] Thus, the present invention provides a method of temperature management in which the step of managing the temperature in the vessel 102 at an appropriate level before it is supplied with the molten metal is distinctly separated from the step of managing the temperature in the vessel 102 in such a way that the as poured molten metal can be cooled at a desired appropriate rate; the invention also provides the apparatus for temperature management 104 which is capable of automatic performance of these steps in an efficient and continuous manner. Also proposed by the invention is a system configuration that implements the respective steps by means of the vessel temperature control section 140 and the semisolid metal cooling section 110.

[0143] In a specific embodiment, the vessel temperature control section 140 is composed of the vessel cooling furnace 150 capable of forced cooling with a circulating hot air flow that provides an appropriate cooling capacity by controlling the temperature and velocity of the air passing through the furnace and the vessel heat-retaining furnace 160 which controls the temperature of the atmosphere to lie at the target value in the vessel 102 and which maintains the vessel 102 at said temperature of the atmosphere. It should be noted here that the temperature to which the vessel cooling furnace 150 and the vessel heat-retaining furnace 160 should be controlled differs between aluminum and magnesium alloys. In the case of aluminum alloys, the interior of the vessel cooling furnace 150 is controlled to lie between room temperature and 300 °C whereas the interior of the vessel heat-retaining furnace 160 is controlled to lie between 50 °C and 350 °C; in the case of magnesium alloys, the interior of the vessel cooling furnace 150 is controlled to lie between room temperature and 350°C whereas the interior of the vessel heat-retaining vessel 160 is controlled to lie between 200 °C and 450 °C.

[0144] The semisolid metal cooling section 110 is composed of the semisolid metal cooling furnace 120 which is adapted to circulate hot air at an appropriate temperature such as to accomplish cooling within the shortest possible time that produces the slurry of semisolid metal with satisfactory properties and the semisolid metal slowly cooling furnace 130 which is designed to maintain the slurry of semisolid metal for 2 - 5 minutes in a temperature range appropriate for shaping such as to be adaptive for the specific molding cycle on the molding machine 200. Again, the temperature to which the semisolid metal cooling furnace 120 should be controlled differs between aluminum and magnesium alloys. In the case ofaluminum alloys, the temperature should be controlled to lie between 150 °C and 350 °C and in the case of magnesium alloys, the temperature should be controlled to lie between 200 °C and 450 °C. On the other hand, the interior of the semisolid metal slowly cooling furnace 130 should be controlled to be at 500 °C and above in both cases.

[0145] If the injection sleeve 202 on the molding machine 200 is ready to accept the molten metal just at the time when the vessel 102 holding the metal has left the semisolid metal cooling furnace 120, the metal is immediately fed (poured) into the molding machine 200 without being directed into the semisolid metal slowly cooling furnace 130. Conversely, if the injection sleeve 202 is not ready to accept the molten metal since the molding machine 200 is operating, the vessel 102 leaving the semisolid metal cooling 120 is transferred to the semisolid metal annealing furnace 130.

[0146] A first version of the heating system in the semisolid metal cooling furnace 120 according to the invention is such that either the temperature or the velocity of the circulating hot air is controlled to vary appropriately with the lapse of time or, alternatively, both the temperature and the velocity of the hot air are controlled to vary simultaneously with the lapse of time.

[0147] The first specific embodiment of the heating system (furnace temperature control unit 120Z) is as shown in Fig. 47 and comprises a hot air line for supplying a hot air flow into the semisolid metal cooling furnace 120, an air line from which an air flow at ordinary temperature emerges to combine with the hot air to lower its temperature, a damper for controlling the quantity of the air flowing through the air line, and a damper opening controller.

[0148] The second specific embodiment of the heating system (furnace temperature control unit 120Z) is as shown in Fig.48 and comprises a temperature sensor installed within the semisolid metal cooling furnace 120, a hot air line for supplying a hot air flow into the furnace, an air line that combines with the hot air line, an automatic damper installed on the air line, and a damper opening controller that performs feedback control on the damper opening on the basis of the data obtained by measurement with the temperature sensor. The opening of the automatic damper is controlled on the basis of the data for the temperature in the furnace and the hot air is mixed with an appropriate amount of air and fed into the furnace, whereby the temperature and the velocity of the circulating hot air are controlled such that the molten metal will be cooled at a desired rate.

Example 7



[0149] An example of the invention will now be described specifically with reference to accompanying drawings. The example was implemented by the same method as in Example 1, except that Fig.3 was replaced by Fig.54 and the top surface of the insulated vessel 30 (or 30A) was fitted with a heat insulating lid 42 (or a ceramics coated metallic lid 42A). Thus, Figs.1, 2, 54 and 4 - 7 concern Example 8, in which: Fig.1 is a diagram showing a process sequence for the semisolid forming of a hypoeutectic aluminum alloy having a composition at or above a maximum solubility limit; Fig.2 is adiagram showing a process sequence for the semisolid forming of a magnesium or aluminum alloy having a composition within amaximum solubility limit; Fig. 54 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step; Fig.4 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig.54; Fig.5 is an equilibrium phase diagram for an Al-Si alloy as a typical aluminum alloy system; Fig.6 is an equilibrium phase diagram for a Mg-Al alloy as a typical magnesium alloy system; Fig.7 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention; and Fig.8 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped according to the prior art.

[0150] The insulated vessel 30 for holding the molten metal the temperature of which has dropped to just below the liquidus line shall have a heat insulating effect in order to ensure that the primary crystals generated will spheroidize and have the desired fraction liquid after the passage of a specified time. Problems, however, will occur in certain cases, such as where near-eutectic Al-Si alloys and others that are prone to form skins are to be held, or where the molten metal is so heavy that it has to be held in a semisolid condition for more than 10 minutes, or where the height to diameter ratio of the insulated vessel 30 exceeds 1:2. Although, there is no problem with the internal microstructure of the molten metal, a solidified layer is prone to grow on the surface of the melt and can potentially cover the top of the semisolid metal, thus, making it difficult to insert the metal into the injection sleeve 40. To deal with this situation, the top of the insulated vessel 30 is fitted with the heat insulating lid 42 in order to ensure against solidification from the surface of the molten metal which is being held within the insulated vessel 30, thereby enabling the metal to be cooled while providing uniformity in temperature throughout the metal.

[0151] The constituent material of the insulated vessel 30 and the heat-insulating lid 42 is in no way limited to metals and those which have a heat-retaining property and which yet wet with the melt only poorly are preferred. If a gas-permeable ceramic vessel is to be used as the insulated vessel 30 and the heat-insulating lid 42 for holding magnesium alloys which are easy to oxidize and burn, the exterior to the vessel is preferably filled with a specified atmosphere (e. g. an inert or vacuum atmosphere). For preventing oxidation, it is desired that Be or Ca is preliminarily added to the molten metal. The shape of the insulated vessel 30 and the heat-insulating lid 42 is by no means limited to a tubular or cylindrical form and any other shapes that are suitable for the subsequent forming process maybe adopted. The molten metal need not be poured into the insulated vessel 30 but it may optionally be charged directly into the ceramic injection sleeve 40.

[0152] Table 4 shows how the presence or absence of the heat insulating lid 42 affected the procedure of making shaped parts. Comparative Samples 19 - 22 refer to the case of holding the molten metal without the insulating lid. In Comparative Sample 19, the insulated vessel 30 held the melt of an alloy that was prone to form a skin and, hence, a solidified layer formed over the semisolid metal, making it impossible to recover the metal from the vessel 30. In Comparative Sample 20, it was attempted to have the semisolid metal inserted into the injection sleeve with the molding temperature lowered; in Comparative Sample 22, the metal was unduly heavy.

[0153] Hence, in both cases, the holding time was prolonged and the result was substantially the same as with Comparative Sample 1 shown in Table 1. In Comparative Sample 21, the height-to-diameter ratio of the insulated vessel 30 was greater than 1:2 and, hence, the temperature profile through the semisolid metal was so poor that the result was substantially the same as with Comparative Sample 1 shown in Table 1.

[0154] Invention Samples 23 - 26 refer to the case of using the insulated vessel 30 fitted with the heat-insulating lid 42; they showed better results than Comparative Samples 19 - 22 in the recovery of the semisolid metal.


Example 8



[0155] An example of the invention will now be described in detail with reference to Figs.1, 3, 4 and 65 - 67, in which: Fig.1 is a diagram showing a process sequence for the semisolid forming of an Al-Mg alloy; Fig.3 shows a process flow starting with the generation of granular primary crystals and ending with the molding step; Fig.4 shows diagrammatically the metallogrphic structures obtained in the respective steps shown in Fig.3; Fig.65 is an equilibrium phase diagram for a binary Al-Mg alloy; Fig. 66 is a. diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention; and Fig.67 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art.

[0156] As shown in Figs.1 and 65, the invention recited in claim 33 is such that:

the melt of an Al-Mg alloy that contains an element to promote the generation of crystal nuclei and that is held superheated to less than 100°C above the liquidus temperature is directly poured into the insulated vessel without cooling the melt with a jig.



[0157] The poured metal is held within the insulated vessel at a temperature not higher than the liquidus temperature but higher than the eutectic or solidus temperature for a period from 5 seconds to 60 minutes until a specified liquid fractionis established, whereby a large number of fine granular primary crystals are generated to produce a semisolid Al-Mg alloy at the specified fraction liquid.

[0158] The specific procedure of semisolid metal forming to be performed in Example 11 is essentially the same as described in Example 1.

[0159] Silicon (Si) is added in order to promote the spheroidization of the generated granular primary crystals. If the Si addition is less than 0.3 %, the intended effect in promoting the spheroidization is not expected; adding more than 2.5 % of Si will merely result in deteriorated properties of the alloy and no further improvement in spheroidization is expected. Hence, the Si addition is controlled to lie between0.3 % and 2.5 %.

[0160] It should be noted that the Al-Mg alloy of the invention may incarporate up to 1 % of Mn or up to 0.5 % of Cu with a view to improving its strength.

[0161] Table 7 sets forth the conditions for the preparation of semisolid metal samples and the results of evaluation of their metallorgraphic structures by microscopic examination.





[0162] In Comparative Sample 9, the temperature of jig 20 with which the melt M was contacted was so high that the number of crystal nuclei generated was insufficient to produce fine primary crystals; instead, coarse primary crystals formed. In Comparative Sample 10, the casting temperature was so high that very few crystal nuclei remained within the ceramic vessel 30, yielding the same result as with Comparative Sample 9. In Comparative Sample 11, the holding time was so long that the fraction liquid in the metal to be shaped was low, making the alloy unsuitable for shaping. In addition, the size of primary crystals was undesirably large. In Comparative Sample 12, the holding time within the ceramic vessel 30 was short whereas the fraction liquid in the metal to be shaped was high; hence, only coarse primary crystals formed. In addition, the high fraction liquid caused many segregations of components within the shaped part. In Comparative Sample 13, the hot molten metal was directly poured into the insulated vessel, where it was solidified as such, yielding coarse, dendritic primary crystals (see Fig.67).

[0163] In each of Invention Sample 5 and 6, there was obtained a homogeneous microstructure having fine (< ca. 100 µm) granular primary crystals that were adapted for pressure forming.

Example 9



[0164] An example of the invention (as recited in claim 11 will now be described in detail with reference to accompanying Figs.69 - 73, in which Fig.69 shows two process sequences for the semisolid forming of a hypoeutectic aluminum alloy; Fig.70 shows a process flow starting with the generation of spherical primary crystals and ending with the molding step; Fig.71 shows diagrammatically the metallographic structures obtained in the respective steps shown in Fig.70; Fig.72 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the invention; and Fig.73 is a diagrammatic representation of a micrograph showing the metallographic structure of a shaped part according to the prior art.

[0165] The invention concerns a process which starts with either one of the following steps:

(1) two or more liquid alloys having different melting points that are held superheated to less than 50°C above the liquidus temperature are mixed either directly within an insulated vessel having a heat insulating effect or along a trough in a channel into the insulated vessel, thereby generating crystal nuclei in the alloy solution (see Fig.69); or

(2) two or more metals to be mixed are preliminarily contacted with respective cooling plates so as to generate crystal nuclei and the metals that have attained temperatures just above or below the liquidus temperature are mixed either directly within an insulated vessel having a heat insulating effect or along a trough in a channel into the insulated vessel, thereby generating more crystal nuclei (see Fig.70).



[0166] Either of the metals thus obtained is held within the insulated vessel for a period from 5 seconds to 60 minutes as it is cooled to a molding temperature where a specified fraction liquid is established, whereby the fine grains that have formed within the alloy solution are crystallized out as no dendrites, and the metal is then fed into a mold, where it is subjected to pressure forming.

[0167] The "specified fraction liquid" and the "insulated vessel " have the same meanings as defined in Example 1.

[0168] According to the invention, semisolid metal forming will proceed by the following specific procedure. In step (1) of the process shown in Figs.70 and 71, two complete liquid forms of metals MA and MB are contained in ladles 10 and poured into a ceramic container 30 (or ceramic-coated metal container30A) which is an insulated vessel having a heat insulating effect. As a result, an alloy having a large number of crystal nuclei is obtained at a temperature either just below or above the liquidus line. Molten metals MA and MB may be poured either simultaneously or successively with one coming after the other. Alternatively, molten metals MA and MB may be poured into partitioned compartments in the insulated vessel 30 and the partition is removed all of a sudden so as to achieve mutual contact between the two metals.

[0169] In subsequent step (2), the alloy mixture MC is held partially molten within the insulated vessel 30. In the meantime, extremely fine primary crystals result from the introduced crystal nuclei [step (2)-a] and grow into spherical primary crystals as the fraction solid increases with the decreasing temperature of the alloy mixture MC [steps (2)-b and (2)-c]. Alloy mixture MC thus obtained at a specified fraction liquid is inserted into an injection sleeve 40 [step (2)-d] and, thereafter, pressure formed within a mold cavity 50a on a die casting machine to produce a shaped part [step (3)].

[0170] The semisolid metal forming process of the invention shown in Figs.69, 70 and 71 has obvious differences from the conventional thixocasting and rheocasting methods.

[0171] The casting, spheroidizing and molding conditions that are respectively set for the steps shown in Fig.69, namely, the step of generating and spheroidizing primary crystals and the forming step, are set forth below. Also discussed below is the criticality of the numerical limitations set forth in claims 36 and 37.

[0172] If the molten (liquid) metals MA and MB to be mixed have been superheated to more than 50°C above the liquidus temperature, the temperature of either metal just after the mixing will neither be just above or below the liquidus temperature of the alloy mixture MC to be eventually formed. If the mixed metals are held within the insulated vessel 30, a microstructure consisting of coarse dendrites will form rather than a structure of uniform, near-spherical nondendritic crystals. To avoid these problems, the temperatures of molten (liquid) metals MA and MB to be mixed need be superheated to no more than 50 °C above the liquidus temperature. The "temperature either just above or below the liquidus temperature of the metal mixture to be eventually formed" means a temperature within the liquidus temperature ±15°C. The liquid metals to be mixed shall include alloys. The insulated vessel 30 for holding the metals the temperature of which have dropped to be within the defined range after the mixing shall have a heat insulating effect in order to ensure that the crystal nuclei generated will grow into nondendritic (near-spherical) primary crystals and have the desired fraction liquid after a specified time. The constituent material of the insulated vessel is in no way limited to metals and those which have a heat-retaining property and which yet wet with the melt only poorly are preferred. If a gas-permeable ceramic container is to be used as the insulated vessel 30 for holding magnesium alloys which are prone to oxidize and burn, the exterior to the vessel is preferably filled with a specified atmosphere (e. g. an inert or vacuum atmosphere).

[0173] If the holding time within the insulated vessel is less than 5 seconds, it is not easy to attain the temperature for the desired fraction liquid and it is also difficult to generate spherical primary crystals. What is more, semisolid metals of a uniform temperature profile cannot be attained. If the holding time exceeds 60 minutes, coarse spherical primary crystals will be generated.

[0174] It should also be mentioned that if the fraction liquid in the alloy which is about to be shaped by high-pressure casting is less than 20 %, the resistance to deformation during the shaping is so high that it is not easy to produce shaped parts of good quality. If the fraction liquid exceeds 90 %, shaped parts having a homogeneous structure cannot be obtained. Therefore, as already mentioned, the fraction liquid in the alloy to be shaped is preferably controlled to lie between 20 % and 90 %. More preferably, the fraction liquid should be adjusted to range between 30 % and 70 % in order to ensure that shaped parts of high quality can easily be produced by pressure forming. The means of pressure forming are in no way limited to high-pressure casting processes typified by squeeze casting and die casting and various other method of pressure forming may be adopted, such as extruding and casting operations.

[0175] By mixing two or more aluminum alloys having different liquidus temperature and holding the mixture within the insulated vessel 30, one can produce a semisolid metal of a fine spherical structure. If it is desired to generate more crystal nuclei so as to yield uniform and more fine-grained spherical structure in aluminum alloys, Ti and B may be added to the alloys. If the Ti content of the alloy mixture is less than 0.003 %, the intended refining effect of Ti is not attained; beyond 0.30 %, a coarse Ti compound will form to cause deterioration in ductility. Hence, the Ti addition is controlled to lie between 0.003 % and 0.30 %. Boron (B) in the mixed metal MC cooperates with Ti to promote the refining of crystal grains but its refining effect is small if the addition is less than 0.0005 %; on the other hand, the effect of B is saturated at 0.01 % and no further improvement is expected beyond 0.01 %. Hence, the B addition is controlled to lie between 0.0005 % and 0.01 %.

[0176] Table 9 sets forth the conditions for the preparation of semisolid samples and the qualities of shaped parts. As shown in Fig.70, the shaping operation consisted of inserting the semisolid metal into an injection sleeve and subsequent forming on a squeeze casting machine. The forming conditions were as follows: pressure, 950 kgf/cm2 ; injection speed, 1.5m/s; mold cavity dimensions, 100 x 150 x 10; mold temperature,230 °C.

[0177] In Comparative Sample 9, the holding time was so long that undesirably large primary crystals formed. In Comparative Sample 10, the temperatures of the alloys to be mixed were high and so was the temperature of the resulting mixture; hence, the number of the crystal nuclei generated was small enough to produce only dendritic primary crystals. In Comparative Sample 11, the holding time was short whereas the liquid fraction in the alloy mixture was high and this caused extensive segregations in the interior of the sharped part.





[0178] In each of Invention Samples 1 - 8, a homogeneous microstructure comprising fine (< 150 µm) spherical primary crystals was obtained to enable the production of a shaped part having no internal segregations.

Example 10



[0179] This example was implemented by the same method as in Example 1, except that at the end of the step of holding the alloy partially molten within the insulated vessel 30 (or 30A), an oxide W forming on the semisolid metal was removed by means of a metallic or nonmetallic jig [step (3)-c in Fig.74].

[0180] As also shown in Fig.74, the shaping operation consisted of inserting the semisolid metal into an injection sleeve and subsequent forming on a squeeze casting machine. The forming conditions were as follows: pressure, 950 kgf/cm2 ; injection speed, 1.5 m/s; mold cavity dimensions, 100 x 150 x 10; mold temperature, 230°C.

[0181] Table 10 shows how the quality of shaped parts was affected by the presence or absence of the oxide. Obviously, Invention Samples 23 - 26 had better results than Comparative Samples 21 and 22.






Claims

1. A method of shaping a semisolid metal, in which a molten aluminum alloy or magnesium alloy containing an element for promoting the generation of crystal nuclei held superheated to less than 100°C above the liquidus temperature is directly poured without using a cooling jig into an insulated vessel made of a material having a thermal conductivity of at least 1.0 kcal/hr·m·°C (at room temperature), held in said insulated vessel for a period from 5 seconds to 60 minutes as it is cooled to the molding temperature where a specified liquid fraction is established wherein said specified liquid fraction ranges from 20% to 90% in the case of high pressure casting operations and from 0.1% to 70% in the case of extruding and forging operations, thereby crystallising fine primary crystals in the alloy solution, and the alloy solution is fed into a forming mold, where it is shaped under pressure.
 
2. The method according to claim 1, wherein the alloy is an aluminum alloy of a composition within the maximum solubility limit or a hypoeutectic aluminum alloy of a composition at or above the maximum solubility limit.
 
3. The method according to claim 1, wherein the alloy is a magnesium alloy of a composition within the maximum solubility limit.
 
4. The method according to claim 2, wherein the aluminum alloy has 0.001% - 0.01% B and 0.005% - 0.3% Ti added thereto.
 
5. The method according to claim 3, wherein the magnesium alloy has 0.005% - 0.1% Sr added thereto or 0.01% - 1.5% Si and 0.005% - 0.1% Sr added thereto or 0.05% - 0.30% Ca added thereto.
 
6. The method according to claim 1, wherein the liquid alloy that has been superheated by a degree (X°C) of less than 10°C above the liquidus line is held in the insulated vessel for a period from 5 seconds to 60 minutes as it is cooled to a molding temperature where a specified liquid fraction, which ranges from 20% to 90% in the case of high pressure casting operations and from 0.1% to 70% in the case of extruding and forging operations, is established, such that the cooling from the initial temperature at which said alloy is held in said insulated vessel to its liquidus temperature is completed within a time shorter than the time Y (in minutes) calculated by the relation Y=10-X and that the period of cooling from said initial temperature to a temperature 5°C lower than said liquidus temperature is not longer than 15 minutes, whereby fine primary crystals are crystallised in the alloy solution, which is then fed into a forming mold, where it is shaped under pressure.
 
7. The method according to claim 1, wherein the molten alloy is cooled to a temperature at which a solid fraction appropriate for shaping, which is 10%-80% in the case of high pressure casting operations or 30%-99,9% in the case of extruding and forging operations, is established and wherein the step of cooling said alloy is performed with the top and bottom portions of the vessel being heated by a greater degree than the middle portion or heat-retained with a heat-retaining material having a thermal conductivity of less than 1.0 kcal/hr · m ·°C or with either the top or bottom portion of the vessel being heated while the remainder is heat-retained, and said alloy, after being cooled, is fed into a forming mold, where it is shaped under pressure.
 
8. The method according to claim 7, wherein the step of cooling said alloy is performed with the vessel holding said alloy being accommodated in an outer vessel that is capable of accommodating said alloy holding vessel and that has a smaller thermal conductivity than said holding vessel, or that has a thermal conductivity equal to or greater than that of said holding vessel and which has a higher initial temperature than said holding vessel, or that is spaced from said holding vessel by a gas-filled gap, at a rapid cooling rate to obtain a uniform temperature through the alloy in said holding vessel no later than the start of the shaping step.
 
9. The method according to claim 1, wherein the pressure forming is accomplished with the alloy being inserted into a container on an extruding machine.
 
10. The method according to claim 9, wherein the extruding machine is of either a horizontal or a vertical type or of such a horizontal type in which the container changes position from being vertical to horizontal before shaping and wherein the method of extrusion is either direct or indirect.
 
11. The method according to claim 1, wherein the crystal nuclei are generated by a method in which two or more liquid alloys having different melting points that are held superheated to less than 50°C above the liquidus temperature are mixed directly within the insulated vessel made of a material having a thermal conductivity of at least 1.0 kcal/hr ·m· °C (at room temperature) such that the temperature of the metal as mixed is either just above or below the liquidus temperature.
 
12. The method according to claim 8, wherein the outer vessel is heated either from inside or outside or by induction heating, with such heating being performed only before or after the insertion of the holding vessel into the outer vessel or continued throughout the period not only before but also after said insertion.
 


Ansprüche

1. Verfahren zum Formen eines halbfesten Metalls, bei dem eine geschmolzene Aluminiumlegierung oder Magnesiumlegierung, die ein Element zur Förderung der Erzeugung von Kristallkeimen enthält und auf weniger als 100 °C über dem Liquiduspunkt überhitzt gehalten wird, ohne die Verwendung einer Kühlvorrichtung direkt in ein isoliertes Gefäß aus einem Material mit einer thermischen Leitfähigkeit von mindestens 1,0 kcal/h · m · °C (bei Raumtemperatur) gegossen wird, während eines Zeitraums von 5 s bis 60 min., während sie auf die Verformungstemperatur gekühlt wird, gehalten wird, wobei eine spezifische flüssige Fraktion gebildet wird, wobei die spezifische flüssige Fraktion 20% bis 90% im Fall von Hochdruckgießverfahren und von 0,1 bis 70% im Fall von Extrudier- oder Schmiedeverfahren ist, wodurch feine Primärkristalle in der Legierungslösung kristallisieren, und die Legierungslösung in eine Gießform gespeist wird, wo sie unter Druck geformt wird.
 
2. Verfahren nach Anspruch 1, wobei die Legierung eine Aluminiumlegierung einer Zusammensetzung mit einer maximalen Löslichkeitsgrenze oder eine hypoeutektische Aluminiumlegierung einer Zusammensetzung bei oder über der maximalen Löslichkeitsgrenze ist.
 
3. Verfahren nach Anspruch 1, wobei die Legierung eine Magnesiumlegierung einer Zusammensetzung innerhalb der maximalen Löslichkeitsgrenze ist.
 
4. Verfahren nach Anspruch 2, wobei die Aluminiumlegierung 0,001 bis 0,01 % B und 0,005 bis 0,3 % Ti zugegeben enthält.
 
5. Verfahren nach Anspruch 3, wobei die Magnesiumlegierung 0,005 bis 0,1 % zugegebenes Sr oder 0,01 bis 1,5 % Si und 0,005 bis 0,30 % zugegebenes Sr oder 0,05 bis 0,30 % zugegebenes Ca enthält.
 
6. Verfahren nach Anspruch 1, wobei die flüssige Legierung, die um ein Ausmaß (X °C) von weniger als 10 °C über der Liquiduslinie überhitzt worden ist, in dem isolierten Gefäß während eines Zeitraums von 5 s bis 60 min. gehalten wird, während es auf die Verformungstemperatur abkühlt, bei der eine spezifische flüssige Fraktion, die 20 bis 90 % im Fall von Hochdruckformverfahren und 0,1 bis 70 % im Fall von Extrudier- oder Schmiedeverfahren ausmacht, gebildet wird, so dass das Kühlen von der Anfangstemperatur, bei der die Legierung in dem isolierten Gefäß gehalten wird, zu ihrem Liquiduspunkt innerhalb einer Zeitraums vollständig abläuft, der kürzer ist als die Zeit Y (in Minuten), berechnet aus der Beziehung Y=10-X, und dass die Kühldauer von der Anfangstemperatur zu einer Temperatur 5 °C unter dem Liquiduspunkt nicht länger als 15 Minuten ist, wodurch feine Primärkristalle in der Legierungslösung kristallisiert werden, die dann in die Gießform gespeist wird, wo sie unter Druck geformt wird.
 
7. Verfahren nach Anspruch 1, wobei die geschmolzene Legierung auf eine Temperatur abgekühlt wird, bei der eine feste Fraktion erhalten wird, die für das Formen geeignet ist und 10-80% im Fall von Hochdruckformverfahren oder 30-99,9% im Fall von Extrudier- oder Schmiedeverfahren ausmacht, und wobei das Kühlen der Legierung mit den oberen und unteren Teilen des Gefäßes durchgeführt wird, welche stärker erwärmt werden als der mittlere Teil, oder die Wärme mit einem Wärmespeichermaterial mit einer thermischen Leitfähigkeit von weniger als 1,0 kcal/h . m . °C gespeichert wird, oder wobei entweder der obere oder untere Teil des Gefäßes erwärmt wird, während der Rest mit einem Wärmespeicher versehen ist, und die Legierung nach dem Abkühlen in eine Gießform gespeist wird, wo sie unter Druck geformt wird.
 
8. Verfahren nach Anspruch 7, wobei das Kühlen der Legierung mit dem Gefäß durchgeführt wird, wobei die Legierung in einem äußeren Gefäß vorliegt, das das Legierungshaltegefäß aufnehmen kann und eine geringere thermische Leitfähigkeit als das Haltegefäß hat, oder das eine thermische Leitfähigkeit hat, die gleich ist wie oder größer als diejenige des Haltegefäßes und das eine höhere Anfangstemperatur als das Haltegefäß hat, oder das von dem Haltegefäß durch einen gasgefüllten Spalt getrennt ist, bei einer raschen Kühlgeschwindigkeit durchgeführt wird, um eine gleichförmige Temperatur durch die Legierung in dem Haltegefäß nicht später als zum Start der Formungsstufe zu erhalten.
 
9. Verfahren nach Anspruch 1, wobei das Druckformen mit der Legierung, die in ein Gefäß gegeben worden ist, auf einer Extrudiermaschine durchgeführt wird.
 
10. Verfahren nach Anspruch 9, wobei die Extrudiermaschine entweder vom horizontalen oder vertikalen Typ ist oder von einem solchen horizontalen Typ, bei dem das Gefäß seine Position von der Vertikalen zur Horizontalen vor dem Formen ändert und wobei das Extrudierverfahren entweder direkt oder indirekt ist.
 
11. Verfahren nach Anspruch 1, wobei die Kristallkeime durch ein Verfahren erzeugt werden, bei dem zwei oder mehr flüssige Legierungen mit unterschiedlichen Schmelzpunkten, die auf weniger als 50 °C über dem Liquiduspunkt überhitzt gehalten werden, direkt mit dem isolierten Gefäß aus einem Material mit einer thermischen Leitfähigkeit von mindestens 1,0 kcal/h . m . °C (bei Raumtemperatur) gemischt werden, so dass die Temperatur des Metalls beim Mischen entweder knapp über oder unter dem Liquiduspunkt ist.
 
12. Verfahren nach Anspruch 8, wobei das äußere Gefäß entweder von innen oder außen durch Induktionserhitzen erhitzt wird, wobei dieses Erhitzen nur vor oder nach dem Einsetzen des Haltegefäßes in das äußere Gefäß oder fortgesetzt über den Zeitraum nicht nur vor sondern auch nach dem Einsetzen durchgeführt wird.
 


Revendications

1. Procédé pour mettre un métal semi-solide en forme, dans lequel un alliage d'aluminium ou un alliage de magnésium fondu, contenant un élément pour favoriser la génération de noyaux cristallins maintenus surchauffés à moins de 100°C au-dessus de la température du liquidus est directement versé, sans utiliser un gabarit conformateur, dans un réservoir isolé réalisé en un matériau ayant une conductivité thermique d'au moins 1,0 kcal/hr.m.°C (à la température ambiante), maintenu dans ce réservoir isolé pendant une durée allant de 5 secondes à 60 minutes pendant qu'il est refroidi à la température de moulage à laquelle une fraction liquide spécifiée est établie, ladite fraction liquide spécifiée allant de 20 % à 90 % dans le cas d'opérations de coulée à pression élevée et de 0,1 % à 70 % dans le cas d'opérations d'extrusion et de forgeage, cristallisant ainsi de fins cristaux primaires dans la solution d'alliage, et la solution d'alliage est amenée dans un moule de formage où elle est mise en forme sous pression.
 
2. Procédé selon la revendication 1, dans lequel l'alliage est un alliage d'aluminium d'une composition dans la limite maximale de solubilité ou un alliage d'aluminium hypoeutectique d'une composition à la limite maximale de solubilité ou au-dessus de celle-ci.
 
3. Procédé selon la revendication 1, dans lequel l'alliage est un alliage de magnésium d'une composition dans la limite maximale de solubilité.
 
4. Procédé selon la revendication 2, dans lequel l'alliage d'aluminium comporte 0,001 % - 0,01 % de B et 0,005 % - 0,3 % de Ti qui lui sont ajoutés.
 
5. Procédé selon la revendication 3, dans lequel l'alliage de magnésium comporte 0,005 % - 0,1 % de Sr qui lui est ajouté ou 0,01 % - 1,5 % de Si et 0,005 % - 0,1 % de Sr qui lui sont ajoutés ou 0,05 % - 0,30 % de Ca qui lui est ajouté.
 
6. Procédé selon la revendication 1, dans lequel l'alliage liquide qui a été surchauffé d'un degré (X°C) inférieur à 10°C au-dessus de la ligne du liquidus est maintenu dans le réservoir isolé pendant une durée allant de 5 secondes à 60 minutes pendant qu'il est refroidi à une température de moulage à laquelle une fraction liquide spécifiée, qui va de 20 % à 90 % dans le cas d'opérations de coulée à pression élevée et de 0,1 % à 70 % dans le cas d'opérations d'extrusion et de forgeage, est établie, de sorte que le refroidissement à partir de la température initiale à laquelle ledit alliage est maintenu dans ledit réservoir isolé à sa température de liquidus est achevé en un temps plus court que le temps Y (en minutes) calculé par la relation Y=10-X et que la durée de refroidissement à partir de ladite température initiale à une température de 5°C inférieure à ladite température du liquidus ne dépasse pas 15 minutes, moyennant quoi de fins cristaux primaires sont cristallisés dans la solution d'alliage qui est alors amenée dans un moule de formage où il est mis en forme sous pression.
 
7. Procédé selon la revendication 1, dans lequel l'alliage fondu est refroidi à une température à laquelle une fraction solide appropriée pour la mise en forme, qui est de 10 % - 80 % dans le cas d'opérations de coulée à pression élevée ou de 30 % - 99,9 % dans le cas d'opérations d'extrusion et de forgeage, est établie et dans lequel l'étape de refroidissement dudit alliage est réalisée avec les parties supérieure et inférieure du réservoir chauffées d'un degré plus élevé que la partie médiane ou rendues adiathermiques par un matériau adiathermique ayant une conductivité thermique inférieure à 1,0 kcal/hr.m.°C ou avec la partie supérieure ou inférieure du réservoir chauffée tandis que le reste est rendu adiathermique et ledit alliage, après être refroidi, est amené dans un moule de formage où il est mis en forme sous pression.
 
8. Procédé selon la revendication 7, dans lequel l'étape de refroidissement dudit alliage est réalisée avec le réservoir maintenant ledit alliage logé dans un réservoir extérieur qui est capable de loger ledit réservoir maintenant l'alliage et qui a une conductivité thermique plus faible que ledit réservoir de maintien ou qui a une conductivité thermique égale ou supérieure à celle dudit réservoir de maintien et qui a une température initiale plus élevée que ledit réservoir de maintien, ou qui est espacé dudit réservoir de maintien par un intervalle rempli de gaz, à un taux rapide de refroidissement afin d'obtenir une température uniforme à travers l'alliage dans ledit réservoir de maintien pas plus tard qu'au commencement de l'étape de mise en forme.
 
9. Procédé selon la revendication 1, dans lequel la mise en forme sous pression est réalisée avec l'alliage introduit dans un récipient sur une presse à extrusion.
 
10. Procédé selon la revendication 9, dans lequel la presse à extrusion est d'un type horizontal ou vertical ou d'un type horizontal dans lequel le récipient change de position, de la verticale à l'horizontale, avant la mise en forme, et dans lequel le procédé d'extrusion est direct ou indirect.
 
11. Procédé selon la revendication 1, dans lequel les noyaux cristallins sont générés par un procédé dans lequel deux alliages liquides ou plus ayant des points de fusion différents, qui sont maintenus surchauffés à moins de 50°C au-dessus de la température du liquidus, sont mélangés directement à l'intérieur du réservoir isolé réalisé en un matériau ayant une conductivité thermique d'au moins 1,0 kcal/hr.m.°C (à la température ambiante), de sorte que la température du métal tel qu'il est mélangé est juste au-dessus ou en dessous de la température du liquidus.
 
12. Procédé selon la revendication 8, dans lequel le réservoir extérieur est chauffé de l'intérieur ou de l'extérieur ou par chauffage à induction, ce chauffage étant réalisé seulement avant ou après l'introduction du réservoir de maintien dans le réservoir extérieur ou en continu pendant toute la durée non seulement avant, mais aussi après ladite introduction.
 




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