[0001] The present invention relates to a process for producing aluminum having high purity,
and more particularly to a process for treating aluminum containing eutectic impurities,
such as Fe, Si Cu and Mg, and also peritectic impurities, such as Ti, V and Zr, by
resorting to segregation solidification to obtain aluminum having lower contents of
eutectic impurities and peritectic impurities and a higher purity than the original
aluminum.
[0002] Throughout the specification and the appended claims, the term "eutectic impurities"
refers to the impurities which undergo a eutectic reaction with aluminum, and the
term "peritectic impurities" refers to the impurities which undergo a peritectic reaction
with aluminum.
[0003] When aluminum containing both eutectic impurities and peritectic impurities is melted
and then subjected to equilibrium solidification, the impurity concentration Cs of
the resulting solid aluminum fraction is theoretically represented by the following
equation.

wherein ko is the distribution coefficient, Co is the impurity concentration of the
original aluminum, and fs is the ratio of the solid fraction. The above equation shows
that when the distribution coefficient ko is smaller than 1, the impurity concentration
Cs of the solid fraction is smaller than the impurity concentration Co of the original
aluminum and that when the distribution coefficient ko is larger than 1, the impurity
concentration Cs of the solid fraction is greater than the impurity concentration
Co of the original aluminum. Since eutectic impurities are smaller than 1 in distribution
coefficient, the solid fraction prepared from aluminum containing such impurities
is lower than the original aluminum in impurity concentration. Accordingly when the
original aluminum is melted and thereafter solidified, high-purity aluminum can be
obtained advantageously by selectively separating off the resulting pro-eutectic aluminum.
Segregation solidification processes based on this principle are already known as
disclosed, for example, in U.S. Patents No. 3,671,229, No. 3,211,547, etc. However,
peritectic impurities are larger than 1 in distribution coefficient, so that aluminum
containing such impurities affords a solid fraction which is higher than the original
aluminum in impurity concentration. Accordingly when aluminum containing both eutectic
impurities and peritectic impurities is treated by the conventional segregation solidification
process to obtain pro-eutectic aluminum selectively, the resulting solid fraction
is lower in the concentration of eutectic impurities but higher in the concentration
of peritectic impurities than the original aluminum.
[0004] Aluminum containing both eutectic impurities and peritectic impurities is therefore
usually treated by adding boron to a melt of such aluminum in a container to cause
the boron to react with Ti, V, Zr and like peritectice impurities and form insoluble
metallic borides such as TiE
2, VB
2, ZrB
2, etc., allowing the mixture to stand for a long period of time, for example, for
more than 1 hour to settle the metallic borides, placing the molten aluminum into
another container as separated from the borides, and selectively drawing off pro-eutectic
aluminum only from the container. This process is inefficient since the settlement
of the metallic borides requires much time.
[0005] The object of the present invention is to overcome the above drawback and to provide
a process for treating aluminum containing both eutectic impurities and peritectic
impurities by segregation solidification to remove the impurities of both types from
the aluminum to the greatest possible extent and obtain aluminum having a higher purity
than the original aluminum.
[0006] The process of this. invention for producing high-purity aluminum comprises the steps
of melting aluminum containing both eutectic impurities and peritectic impurities
to obtain molten aluminum, adding boron to the molten aluminum, immersing a cooling
body into the boron-containing molten aluminum, and rotating the cooling body while
introducing a cooling fluid to the interior of the cooling body to crystallize high-purity
aluminum on the surface of the body.
[0007] With this process, the boron reacts with the peritectic impurities to form metallic
borides, which are moved away from the cooling body and dispersed throughout the liquid
phase by the centrifugal force produced by the rotation of the cooling body. Accordingly
an aluminum fraction having lower contents of eutectic impurities and peritectic impurities
than the original aluminum can be crystallized on the surface of the cooling body,
giving high-purity aluminum. Unlike the conventional process, the present process
does not involve the necessity of settling the metallic borides and therefore can
be practiced within a shortened period of time.
[0008] When aluminum containing Fe, Si, Cu, Mg and like eutectic impurities,and Ti, V, Zr
and like peritectic impurities is melted, and boron is added to the resulting melt,
the boron reacts with the Ti, V, Zr and like peritectic impurities to form TiB
2, VB
2' ZrB
2 and like insoluble metallic borides. The amount of boron to be used, which is determined
in accordance with the Ti, V, Zr and like contents of the aluminum to be purified,
is a predetermined amount larger than the amount needed for forming the above metallic
borides. The boron may be added in the form of an Al-B master alloy or NaBF
4 or like salt. Since boron undergoes a eutectic reaction with aluminum, the excess
of boron other than the quantity of boron forming the metallic borides with the peritectic
impurities is removed in the same manner as the eutectic impurities as will be described
below.
[0009] When a cooling body is rotated as immersed in the boron-containing molten aluminum
while introducing a cooling fluid to the interior of the body, high-purity aluminum
crystallizes on the surface of the cooling body. Stated more specifically, when aluminum
containing eutectic impurities is melted and subjected to equilibrium solidification,
pro-eutectic aluminum of high purity separates out first. The ratio between the eutectic
impurity concentration of the solid phase and the eutectic impurity concentration
of the liquid phase at this time is represented by the distribution coefficient ko.
During actual solidification, however, the eutectic impurities are released into the
liquid phase to form a layer of concentrated eutectic impurities in the liquid phase
in the vicinity of the liquid-solid interface or boundary, so that the impurity concentration
of the solid phase is governed by the effective distribution coefficient k
E considering the thickness of the concentrated layer (hereinafter referred to as "diffusion
layer"). Thus the impurity concentration Cs of the solid phase is represented by Equation
(1) wherein k
E is used in place of ko, i.e. by the following equation.
[0010]

[0011] It is already known that the effective distribution coefficient k
E is represented by the following equation.

wherein R is the solidification velocity, δ is the thickness of the diffusion layer
formed in the vicinity of the liquid-solid interface, and D is the diffusion coefficient
of the eutectic impurities in the liquid phase. It therefore follows that the effective
distribution coefficient k
E can be made approximate to the distribution coefficient ko effectively by decreasing
the solidification velociy R and the thickness of the diffusion layer, 8 , and increasing
the diffusion coefficient D. Of these variables, the diffusion coefficient D is considered
to be a constant which is dependent on the kind of the eutectic impurity generally
when the liquid phase has a constant temperature, so that it is difficult to vary
the diffusion coefficient D. It is therefore effective to decrease the solidification
velocity R and the thickness of the diffusion layer, 8 , for making the effective
distribution coefficient k
E approximate to the distribution coefficient ko.
[0012] When the eutectic impurities are released into the liquid phase at the liquid-solid
interface, dendrites are formed at the interface. It is well known that when such
dendrites grow, the impurities released into the liquid phase in the vicinity of the
liquid-solid interface are trapped, as they are or in the form of eutectic crystals
of several microns, in the interstices of the dendrites. This phenomenon is undesirable
for the purification of aluminum. The growth of dendrites occurs when the actual temperature
of the liquid phase is lower than the temperature of the equilibrium liquidus in the
vicinity of the liquid-solid interface. This phenomenon is referred to as constitutional
undercooling. The growth of dendrites is promoted when the difference (degree of undercooling)
AT between the temperature of the equilibrium liquidus and the actual liquid phase
temperature increases. Accordingly the growth of dendrites can be inhibited effectively
by decreasing the difference ΔT. To decrease ΔT, there is the need to increase the
temperature gradient of the melt in the vicinity of the liquid-solid interface. Ideally,
the temperature gradient should be smaller than the temperature gradient of the equilibrium
liquidus to make ΔT smaller than 0.
[0013] The foregoing leads to the following three requirements for purifying aluminum with
improved efficiency.
(a) To decrease the solidification velocity to the greatest possible extent.
(b) To decrease to the greatest possible extent the thickness of the diffusion layer
in the vicinity of the liquid-solid interface.
(c) To increase to the greatest possible extent the temperature gradient involved
in the liquid phase in the vicinity of the interface.
[0014] When a cooling body is immersed in molten aluminum containing boron, aluminum having
a high purity starts to crystallize on the surface of the cooling body. The solidification
proceeds while the eutectic impurities are being released into the liquid phase.in
the vicinity of the liquid-solid interface to form a diffusion layer. The solidification
velocity at this time is governed by the difference between the amount of heat removed
from the molten aluminum by the cooling body and the amount of heat supplied to the
molten aluminum by heating from outside. Thus the velocity is controlled by these
amounts of heat. Further when an increased amount of heat is supplied to the molten
aluminum by external heating, with an increased amount of heat removed from the melt
by cooling with the cooling body, greater transfer of heat occurs between the cooling
body and the melt, consequently giving a greater temperature gradient to the liquid
phase in the vicinity of the liquid-solid interface. The greater the temperature gradient,
the more effectively is the formation of dendrites inhibited at the interface to .prevent
the eutectic impurities from being arrested by the dendrites. Ideally, the temperature
gradient involved in the liquid phase in the vicinity of the liquid-solid interface
should be greater than that of the equilibrium liquidus. The formation of dendrites
can then be inhibited completely. From the viewpoint of industrial productivity, however,
it is desirable to effect suitable transfer of heat from the molten aluminum to the
cooling body by advantageously controlling the external heating and cooling with the
cooling body. Further when the cooling body is rotated, the solid phase and the liquid
phase move relative to each other, whereby the diffusion layer formed near the liquid-solid
interface is effectively agitated and mixed with the other major portion of the liquid
phase to disperse the impuri- ites in the diffusion layer throughout the entire liquid
phase, consequently greatly reducing the thickness of the diffusion layer. At'=the
same time, the boundary layer in the temperature distribution of the liquid phase
is made thinner, consequently permitting the liquid phase to have an increased temperature
gradient in the vicinity of The liquid-solid interface. The thicknesses of the diffusion
layer and the boundary layer in the temperature distribution can be decreased by increasing
the speed of rotation of the cooling body, in other words, the speed of the relative
movement between the cooling body and the molten aluminum. However, if the speed is
exceedingly high, the aluminum crystallized on the surface of the cooling body is
likely to separate off easily due to the increase of the centrifugal force, resulting
in reduced productivity. Preferably the speed of the relative movement is within the
range of 400 to 8000 mm/sec because if the speed is lower than 400 mm/sec, the diffusion
layer will not be made thinner effectively, whereas if it is higher than 8000 mm/sec,
the increased centrifugal force will lead to reduced productivity. When the cooling
body is in the form of a cylinder having a diameter of 160 mm, for example, the body
can be rotated at 50 to 1000 r.p.m., but especially good results are obtained at 2,00
to 700 r.p.m. Further improved results can be achieved if the direction of rotation
of the body is reversed with suitable frequency. Since boron undergoes a eutectic
reaction with aluminum, the excess of boron other than the amount of boron forming
metallic borides with the peritectic impurities is removed in the same manner as Fe,
Si, Cu, Mg and like eutectic impurities.
[0015] The high-purity aluminum deposited on the surface of the cooling body on crystallization
is recovered, for example, by melting the high-purity fraction or by scraping off
the fraction.
[0016] The present invention further provides a process comprising the steps of melting
aluminum containing both eutectic impurities and peritectic impurities to obtain molten
aluminum, placing the molten aluminum into a holding container, adding boron to the
molten aluminum within the container, and rotating a cooling body as immersed in the
boron-containing molten aluminum within the container while introducing a cooling
fluid to the interior of the cooling body to crystallize high-purity aluminum on the
surface of the body.
[0017] In the above process, the cooling body is immersed into the molten aluminum preferably
after causing the boron to react with the peritectic impurities by allowing the molten
aluminum to stand for at least about 5 minutes following the addition of the boron.
To promote the reaction, it is desirable to agitate the boron-containing molten aluminum.
[0018] The present invention further provides a process comprising melting aluminum-containing
both eutectic impurities and peritectic impurities to obtain molten aluminum, placing
the molten aluminum into a boron adding vessel, causing the molten aluminum placed
into the vessel to be forwarded to a plurality of purifying tanks from tank to tank
and to be discharged from the last tank, adding boron to the molten aluminum within
the vessel, and rotating a cooling body as immersed in the boron-containing molten
aluminum within each of the tanks while introducing a cooling fluid to the interior
of the cooling body to crystallize high-purity aluminum on the surface of the body.
This process affords a large quantity of high-purity aluminum efficiently by a continuous
operation.
[0019] The boron adding vessel and the purifying tanks are prepared, for example, by dividing
a single large container into a plurality of sections by partitions each having a
communication opening, one of the sections serving as the vessel and the other sections
as the tanks. Alternatively a plurality of crucibles may be arranged in a row, with
each crucible communicating with another through a trough, such that one of the crucibles
serves as the boron adding vessel and the others as the purifying tanks.
[0020] Boron is placed into the vessel continuously so that the molten aluminum therein
has a constant boron concentration during operation. Preferably the molten aluminum
in the vessel is agitated to accelerate the reaction between the boron and the peritectic
impurities. The cooling body is immersed in the molten aluminum in each of the purifying
tanks. The supply of the melt to the purifying tanks is so adjusted that the amount
of the melt in each tank remains unchanged during operation. To allow equal amounts
of aluminum to crystalize on the surfaces of the cooling bodies in the purifying tanks,
the temperature of the molten aluminum, the speed of rotation and cooling capacity
of the cooling bodies are suitably controlled. The eutectic impurity concentration
of the molten aluminum in the purifying tanks progressively increases from tank to
tank away from the melting furnace. The average impurity concentration of all the
aluminum fractions obtained is variable by varying the ratio of the total amount'of
aluminum fractions recovered by the cooling bodies to the total amount of the melt
supplied. (The ratio will be referred to as "recovery ratio".) The smaller the recovery
ratio, the lower is the average impurity concentration. Accordingly aluminum having
a constant purity which is higher than the purity of the original aluminum supplied
from the melting furnace for purification can be obtained by rendering the recovery
ratio constant. Further at the same recovery ratio, the purity of the aluminum obtained
increases with the increase in the number of purifying tanks.
[0021] The invention will be described below in greater detail with reference to the accompanying
drawings.
[0022]
Fig. 1 is a view in vertical section showing a first embodiment of apparatus for producing
high-purity aluminum by the process of the invention;
Fig. 2 is a view in vertical section showing a second embodiment of apparatus for
producing high-purity aluminum by the process of the invention;
Fig. 3 is an enlarged fragmentary view of Fig. 2 partly broken away;
Fig. 4 is a graph showing the result achieved when the process of the invention was
practiced with use of the second apparatus, the graph showing the relation of the
amount of aluminum (yield) crystallized on the peripheral surface of a cooling body
in each purifying tank to'the-ratio of the eutectic impurity concentration of the
molten aluminum in the tank to the eutectic impurity concentration of the aluminum
to be purified; and
Fig. 5 is a graph showing the relation between the number of purifying tanks and the
ratio of the eutectic impurity concentration of the aluminum obtained to that of the
aluminum to be purified, the relation being determined by practicing the process of
the invention with use of the second apparatus.
[0023] With reference to a first apparatus for practicing the process of the invention,
the aluminum to be purifyied and containing both eutectic impurities and peritectic
impurities is melted and placed in a holding container comprising a crucible 2. The
molten aluminum 1 is heated and maintained at a temperature exceeding the solidifying
temperature thereof. Boron is added to the molten aluminum 1, and the mixture is agitated
for at least 5 minutes. A cooling body 3 is thereafter immersed in the melt 1. The
cooling body 3 is in the form of a hollow cylinder having closed opposite ends and
is movable upward and downward. A hollow rotary shaft 4 extends upward from the upper
end of the body 3. The interior of the hollow rotary shaft 4 is in communication with
the interior of the cooling body 3. A cooling fluid supply pipe 5 extends through
the shaft 4 into the cooling body 3. The rotary shaft 4 is provided at its upper end
with a drive device (not shown), by which the shaft 4 and the body 3 are rotated.
The top and bottom of the body 3 and the portion of the shaft 4 to be exposed to the
melt 1 are preferably covered with a heat insulating material 6 so as not to permit
aluminum to crystallize on these portions. This is due to the reason that since the
effect produced by the rotation of the body 3 is lower at these portions than at the
periphery of the body 3, aluminum, if crystallizing on these portion,will have a lower
purity than the aluminum crystallizing on the periphery. The cooling body 3 is rotated
while introducing a cooling fluid, such as air, nitrogen or argon, from the pipe 5
into the body 3 at an adjusted rate so that the portion of the melt 1 around the body
3 will be cooled slowly. Pro-eutectic aluminum having a high purity then starts to
crystallize on the periphery of the body 3. After a specified quantity of aluminum
has been deposited on the body 3, the body is raised and withdrawn from the melt 1,
and the high-purity aluminum obtained is collected.
[0024] The above procedure is repeated in aluminum melts of progressively higher purities
to obtain aluminum of greatly improved purity.
[0025] With reference to Figs. 2 and 3 showing a second apparatus, there is provided a melting
furnace 11 for melting the aluminum to be purified and containing both eutectic impurities
and peritectic impurities. A large container 12 in the form of a horizontally elongated
rectangular parallelepiped is disposed on the right side of the furnace 11. The container
12 is divided into five sections by partitions 13. Of these sections, the one at the
left end serves as a boron adding vessel 14, and the other four sections serve as
purifying tanks 15 to 18. The partitions 13 are formed at their upper ends with openings
19 through which the vessel 14 and the tanks 15 to 18 communicate with one another.
The vessel 14 has an agitator 20 in its interior. The agitator 20 comprises a vertical
rotary shaft 21, a propeller-shaped stirring blade 22 attached to the lower end of
the shaft 21 and unillustrated drive means. Each of the tanks 15 to 18 is provided
with a cooling body 23 which is movable upward and downward. The body 23 is in the
form of a downwardly tapered hollow cylinder having closed opposite ends and a hollow
rotary shaft 24 extending upward from its top. The interior of the shaft 24 is in
communication with the interior of the body 23. A cooling fluid supply pipe 26 extending
through the shaft 24 into the body 23 has a large number of cooling fluid outlets
25 in its peripheral wall. The upper end peripheral portion and the bottom of the
cooling body 23 are covered with heat insulating members 27 and 28 respectively.
[0026] Before molten aluminum 30 is placed into the tanks 14 to 18, the cooling bodies 23
are held raised as indicated in broken lines in Fig. 2.
[0027] The aluminum to be purified and containing both eutectic-impurities and peritectic
impurities is melted in the furnace 11, and the molten aluminum 30 is first placed
into the vessel 14, in which boron is added to the melt 30. The mixture is agitated
by the agitator 20. In this vessel 14, the boron reacts with Ti, V, Zr and like peritectic
impurities, forming TiB
2, VB
2, ZrB
2 and like insoluble metallic borides. The molten aluminum containing the eutectic
impurities, insoluble metallic borides and an excess of boron flows into the tanks
15 to 18 through the communication openings 19. After a predetermined amount of molten
aluminum 30 has been placed into each of the tanks 15 to 18, the cooling body 23 is
lowered and immersed in the melt, with the upper heat insulating member 27 in contact
with the melt 30 and with the lower edge of the member 27 located within the mass
of the melt 30 at such a position that it will not be influenced by the temperature
of the atmosphere. The upper end peripheral portion of the body 23 is covered with
the insulating member 27, and the body is so immersed in the melt 30 that the member
27 is in contact with the surface of the melt 30 with its lower edge at a position
where it is free of the influence of the atmospheric temperature, for the following
reason. The portion of the melt 30 near the surface thereof exposed to the atmosphere
has a lower temperature than the other portion by being affected by the atmospheric
temperature and is therefore liable to solidify on the periphery of the body 23 in
the vicinity of.the above surface. Consequently aluminum solidifies at a higher velocity
at this portion than at the other portion of the periphery of the body 23, with the
result that the aluminum fraction deposited on this portion has a lower purity than
the fraction on the other portion and becomes mixed with the latter fraction when
the purified aluminum is removed from the outer periphery of the body 23 for collection
after the completion of the purifying operation. This results in a reduced overall
purifying efficiency. Further the bottom of the cooling body 23 is covered with the
heat insulating member 28 becausa the rotation of the body 23 will not produce a satisfactory
effect at the bottom, such that the aluminum fraction deposited on the bottom of the
body 23 has a lower purity than the other fraction on the periphery of the body.
[0028] The cooling body 23 in this state is rotated while injecting a cooling fluid into
the body through the inlets 25 of the supply pipe 26. This causes aluminum to crystallize
on the portion of the peripheral surface of the body 23 which is immersed in the melt
30 and which is not covered with the insulating members 27 and 28. Since the metallic
borides contained in the melt 30 are centrifugally forced away from the body 23 by
the rotation thereof, the aluminum deposited on the periphery of'the body 23 is free
from such borides. The excess of boron, which forms a eutectic with aluminum, is removed
like the eutectic impurities. The temperature of the molten aluminum, and the speed
of rotation and cooling capacity of the bodies 23 are so controlled that equal amounts
of aluminum will be deposited on the peripheral surfaces of the bodies in the purifying
tanks 15 to 18, while the supply and discharge of molten aluminum are controlled so
that the tanks 15 to 18 contain equal amounts of melt, with the recovery ratio maintained
at a constant value. Assuming that the molten aluminum supplied from the furnace 11
has a eutectic impurity concentration of CO and that the melt portions contained in
the tanks 15 to 18 have eutectic impurity concentrations of Cl, C2, C3 and C4 respectively,
GO < Cl < C2 < C3 < C4. Further the ratio of the eutectic impurity concentration of
the melt in each of the tanks 15 to 18 to C0, namely the ratio CN/CO where N is 1
to 4, increases with the start of the operation but levels off when the amount of
aluminum deposit on the periphery of the cooling body 23 reaches a value as shown
in Fig. 4. At this time, the total amount of eutectic impurities, Ms, in the aluminum
recovered by the cooling bodies 23 plus the amount of eutectic impurities, Mn, in
the molten aluminum discharged from the tank 18 at the right end is always equal to
the amount of eutectic impurities, Mo, in the aluminum to be purified. Accordingly,
if the eutectic impurity concentration and the effective distribution coefficient
of the eutectic impurities of the molten aluminum in each of the tanks 15 to 18 are
known, high-purity aluminum can be obtained with the desired eutectic impurity concentration
when the recovery ratio is set to a definite value. The smaller the recovery ratio,
the lower is the eutectic impurity concentration of the molten aluminum in each purifying
tank, so that the cast block obtained has a higher purity. The purity of the aluminum
to be obtained can be determined by varying the recovery ratio. At a definite recovery
ratio, the eutectic impurity concentration of the molten aluminum discharged increases
with the increase of the number of purifying tanks as seen in Fig. 5, enabling the
cooling bodies 23 to afford aluminum of higher purity.
[0029] When the same operation as above is repeated again with use of the aluminum collected
by the cooling bodies 23, aluminum having a higher purity can be obtained. Since the
molten aluminum resulting from the second operation usually has a higher purity than
the original aluminum used as the material for the first operation, the molten aluminum,
if returned to the furnace 11, gives an improved yield.
Example 1
[0030] The apparatus shown in Fig. 1 was used. Aluminum containing 0.08 wt.% of Fe, 0.05
wt. % of Si, 0.0015 wt. % of Ti, 0.004 wt. % of V and 0.0005 wt. % of Zr was melted,
and the molten aluminum 1 was maintained at 670° C in the crucible 2. Al-3 wt. % B
master alloy was added to the aluminum 1 so that the resulting melt had a boron concentration
of 0.004 wt. %. The mixture was agitated for 5 minutes after the addition of the alloy.
The cooling body 3, 100 mm in outside diameter, was immersed in the melt 1 and rotated
at a speed of 400 r.p.m. while supplying air into the body 3 through the supply pipe
5. The body 3 was rotated for 10 minutes and thereafter withdrawn from the melt 1
by raising. The body 3 was found to have aluminum deposited on its periphery in an
amount of 20 wt.% based on the amount of the original aluminum. When checked for impurity
concentration, the cast aluminum block was found to contain 0.008 wt.% of Fe, 0.012
wt.% of Si, less than 0.0001 wt.% of Ti, 0.0002 wt . % of V, less than 0.0002 wt.%
of Zr and 0.0003 wt.% of B.
Example 2
[0031] The apparatus shown in Fig. 1 was also used. Aluminum containing 0.08 wt.% of Fe,
0.05 wt.% of Si, 0.002 wt. % of Ti, 0.008 wt. % of V and 0.001 wt. % of Zr was melted,
and the molten aluminum 1 was maintained at 670° C in the crucible 2. Al-3 wt. % B
master alloy was added to the aluminum 1 so that the resulting melt had a boron concentration
of 0.008 wt.%. The mixture was agitated for 5 minutes after the addition of the alloy.
The cooling body 3, 200 mm in outside diameter, was then immersed in the melt 1 and
rotated at a speed of 650 r.p.m. while supplying air into the body through the pipe
5. After rotating the body 3 for 10 minutes, the body 3 was withdrawn from the melt.
The body 3 was found to have aluminum deposited on its periphery in an amount of 20%
based on the amount of the original aluminum. When checked for impurity concentration,
the cast aluminum block was found to contain 0.005 wt.% of Fe, 0.009 wt. % of Si,
less than 0.0001 wt.% of Ti and V, less than 0.0002 wt. % of Zr and 0.0005 wt. % of
B.
Example 3
[0032] The apparatus shown in Figs. 2 and 3 was used. The cooling bodies 23 were held raised.
Aluminum containing 0.08 wt. % of Fe, 0.05 wt. % of Si, 0.002 wt. % of Ti and 0.008
wt.% of V was melted in the furnace 11, and the.molten aluminum was supplied to the
boron adding vessel 14. Boron was added to the aluminum so that the resulting melt
had a boron concentration of 0.008 wt.% at all times. The mixture was agitated by
the agitator 20. When the purifying tanks 15 to 18 were filled with the molten aluminum
flowing through the communication openings 19, each cooling body 23 having a diameter
of 200 mm at the portion thereof covered with the heat insulating member 27was lowered
into the molten aluminum 30. The body 23 was rotated at 400 r.p.m. while supplying
a cooling fluid into its interior from the pipe 26. During operation, the molten aluminum
was continuously supplied from the furnace 11 to the vessel 14 and tanks 15 to 18
so as to fill up these containers to a constant level. Boron was also continuously
placed into the vessel 14 to maintain the boron concentration at 0.008 wt. % at all
times. The eutectic impurity concentrations C1, C2, C3 and C4 of the melt portions
in the tanks 15 to 18 remained in the relation of Cl C2 C3 C4 from the start of the
operation, and a steady state was established after the amount of aluminum deposit
on the body 23 reached a specified amount. When the effective distribution coefficient
of iron was 0.1 at a recovery ratio of 0.7, the ratios of the iron concentrations
Cl, C2, C3 and C4 to the iron concentration CO of the molten aluminum supplied from
the furnace 11, namely Cl/CO, C2/C0, C3/CO and C4/CO, levelled off at 1.3, 1.6, 2
and 2.7, respectively. The operation was continued in this state. When checked for
impurity concentration, the resulting cast aluminum blocks were found to contain 0.008
wt. % of Fe, 0.008 wt. % of Si, 0.0001 wt.% of Ti, 0.0002 wt. % of V and 0.0006 wt.
% of B on the average.
Example 4
[0033] The operation of Example 3 was repeated under the same conditions except that the
recovery ratio was 0.4. The operation was continued in a steady state. All the aluminum
blocks obtained were found to have average impurity concentrations of: 0.005 wt. %
Fe, 0.006 wt.% Si, 0.0001 wt. % Ti, 0.0002 wt. % V and 0.0005 wt.% B.
Example 5
[0034] The operation of Example 3 was repeated under the same conditions as in Example 3
except that eight purifying tanks were used in place of the four tanks. The operation
was continued in a steady state. The aluminum blocks obtained were found to have the
following average impurity concentrations: 0.0065 wt.% Fe, 0.007 wt. % Si, 0.0001
wt. % Ti, 0.0002 wt. % V, 0.0005 wt. % B. The aluminum had a higher purity than that
obtained in Example 3 with use of the four purifying tanks and was produced at twice
the speed therein.
[0035] The present invention may be embodied differently without departing from the spirit
and basic features of the invention. Accordingly the embodiments herein disclosed
are given for illustrative purposes only and are not in any way limitative. It is
to be understood that the scope of the invention is defined by the appended claims
rather than by the specification and that various alterations and modifications within
the definition and scope of the claims are included in the claims.
1. A process for producing high-purity aluminum comprising the steps of belting the
aluminum to be purified end containing both eutectic impurities and peritectic impurities
to obtair melten aluminum, and adding boron to the molten aluminum, characterised
by rotating a cooling body (3, ?3) as immersed in the boron-containing Molten oluminum
(1) while introducing a cooling fluid to the interior of the cooling body (3, 23)
to crystallize high-purity aluminum on the surface of the body (3, 23)
2. A process according to claim 1, characterised by placing the molten aluminum into
a holding container (2), adding the boron to the molten aluminum within the container
(2), and rotating the cooling body (3) as immersed in the boron-containing molten
aluminum within the container (2).
3. A process according to claim 1 or 2, characterised in that the molten aluminum
is agitated after the boron is added thereto,
A process according to claim 1, characterised by placing the molten etuminum into
a boron adding vessel (14), causing the molten aluminum placed into the vessel (14)
to be forwarded to a plurality of purifying tanks (15-18) from tank to tank and to
be discharged from the lost tank (18), adding the boron to the molten aluminum within
the vessel (14), and rotating one of the cooling bodies (23) as immersed in the boron-containing
molten aluminum within each of the tanks (15-18).
5. process according to claim 4, chorocterised in that the molten aluminum having
the boron added thereto in the vessel is agitated.
6. A process according to claim 4 or 5, characterised in that the supply and the discharge
of the molten aluminum are controlled so that the amounts of the molten aluminum in
the purifying tanks (15-18) remain unchanged during operation, and the cooling bodies
(23) are controlled so that equal amounts of high-purity aluminum are crystallized
on the surfaces of the cooling bodies (23).
7. A process according to any of the preceding claims, characterised in that the speed
of the relative movement between the cooling body (3, 23) and the molten aluminum
is about 400 to about 8000 mm/sec when the cooling body is rotated.