| (19) |
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(11) |
EP 0 538 519 B2 |
| (12) |
NEW EUROPEAN PATENT SPECIFICATION |
| (45) |
Date of publication and mentionof the opposition decision: |
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13.06.2001 Bulletin 2001/24 |
| (45) |
Mention of the grant of the patent: |
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07.01.1998 Bulletin 1998/02 |
| (22) |
Date of filing: 21.10.1991 |
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| (54) |
Method of making high silicon, low carbon regular grain oriented silicon steel
Verfahren zum Herstellen von normal kornorientiertem Stahl mit hohem Silizium- und
niedrigem Kohlenstoffgehalt
Procédé de fabrication d'acier ordinaire à haute teneur en silicium, à basse teneur
en carbone et à grains orientés
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Designated Contracting States: |
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DE FR GB IT SE |
| (43) |
Date of publication of application: |
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28.04.1993 Bulletin 1993/17 |
| (73) |
Proprietor: ARMCO Inc. |
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Middletown,
Ohio 45043 (US) |
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| (72) |
Inventor: |
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- Schoen, Jerry W.
Middletown,
Ohio 45044 (US)
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| (74) |
Representative: Fisher, Adrian John et al |
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CARPMAELS & RANSFORD
43 Bloomsbury Square London WC1A 2RA London WC1A 2RA (GB) |
| (56) |
References cited: :
EP-A- 0 047 129 EP-A- 0 334 223 FR-A- 2 228 855
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EP-A- 0 253 904 DE-C- 2 550 426 FR-A- 2 439 238
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TECHNICAL FIELD
[0001] The invention relates to a process for producing high silicon regular grain oriented
electrical steel with low melt carbon and in thicknesses ranging from 14 mils (0.35
mm) to 6 mils (0.15 mm) or less, and more particularly to such a process including
an intermediate anneal following the first cold rolling stage having a very short
soak time and a two-part temperature-controlled cooling cycle, and preferably an ultra-rapid
anneal prior to decarburization.
BACKGROUND ART
[0002] The teachings of the present invention are applied to silicon steel having a cube-on-edge
orientation, designated (110) [001] by Miller's Indices. Such silicon steels are generally
referred to as grain oriented electrical steels. Grain oriented electrical steels
are divided into two basic categories: regular grain oriented and high permeability
grain oriented. Regular grain oriented electrical steel utilizes manganese and sulfur
(and/or selenium) as the principle grain growth inhibitor and generally has a permeability
at 796 A/m of less than 1870. High permeability electrical steel relies on aluminum
nitrides, boron nitrides or other species known in the art made in addition to or
in place of manganese sulphides and/or selenides as grain growth inhibitors and has
a permeability greater than 1870. The teachings of the present invention are applicable
to regular grain oriented silicon steel.
[0003] Conventional processing of regular grain oriented electrical steel comprises the
steps of preparing a melt of electrical steel in conventional facilities, refining
and casting the electrical steel in the form of ingots or strand cast slabs. The cast
electrical steel preferably contains in weight percent less than about 0.1% carbon,
0.025% to 0.25% manganese, 0.01% to 0.035% sulfur and/or selenium, 2.5% to 4.0% silicon
with an aim silicon content of about 3.15%, less than 50 ppm nitrogen and less than
100 ppm total aluminum, the balance being essentially iron. Additions of boron and/or
copper can be made, if desired.
[0004] If cast into ingots, the steel is hot rolled into slabs or directly rolled from ingots
to strip. If continuous cast, the slabs may be pre-rolled in accordance with U.S.
Patent 4,718,951. If developed commercially, strip casting would also benefit from
the process of the present invention. The slabs are hot rolled at about 2550° F (1400°
C) to hot band thickness and are subjected to a hot band anneal of about 1850° F (1010°
C) with a soak of about 30 seconds. The hot band is air cooled to ambient temperature.
Thereafter, the material is cold rolled to intermediate gauge and subjected to an
intermediate anneal at a temperature of about 1740° F (950° C) with a 30 second soak
and is cooled as by air cooling to ambient temperature. Following the intermediate
anneal, electrical steel is cold rolled to final gauge. The electrical steel at final
gauge is subjected to a conventional decarburizing anneal which serves to recrystallize
the steel, to reduce the carbon content to a non-aging level and to form a fayalite
surface oxide. The decarburizing anneal is generally conducted at a temperature of
from 1525° F to 1550° F (830° C to 845° C) in a wet hydrogen bearing atmosphere for
a time sufficient to bring the carbon content down to about 0.003% or lower. Thereafter,
the electrical steel is coated with an annealing separator such as magnesia and is
final annealed at a temperature of about 2200° F (1200° C) for twenty-four hours.
This final anneal brings about secondary recrystallization. A forsterite or "mill"
glass coating is formed by reaction of the fayalite layer with the separator coating.
[0005] Representative processes for producing regular grain oriented (cube-on-edge) silicon
steel are taught in U.S. Patent Nos. 4,202,711; 3,764,406; and 3,843,422.
[0006] In recent years, to lower the core loss of regular grain oriented products, attention
has been turned to increasing the volume resistivity by raising the silicon content
to suppress macro-eddy current losses. However, the expected improvement from higher
silicon content has generally not been realized. A typical prior art approach has
been to increase both silicon and carbon in particular ratios in an attempt to achieve
improved magnetic quality. It has been found that raising carbon and silicon together
will make the steel more prone to incipient grain boundary melting during the high
temperature ingot/slab heating process and more brittle in subsequent processing after
hot rolling. Particularly the handling and cold rolling characteristics of the higher
silicon and carbon material are degraded. In the process of making regular grain oriented
silicon steel, decarburization to 0.003% carbon or less is required to provide nonaging
magnetic properties in the finished grain oriented electrical steel. However, higher
silicon retards decarburization, making high silicon, high melt carbon materials more
difficult to produce.
[0007] The present invention is based upon the discovery that in the production of regular
grain oriented electrical steel the nature of the intermediate anneal following first
stage of cold rolling, and its cooling cycle, have a marked effect on the magnetic
quality of the final product. The volume fraction of austenite formed during the anneal,
the austenite decomposition product and the carbide precipitate formed during cooling
are all of significant importance. A cooling rate after the intermediate anneal which
does not allow for austenite decomposition subsequent to the precipitation of fine
iron carbide produces lower permeability, less stable secondary grain growth, and/or
an enlarged secondary grain size. Added to this, higher silicon will raise the activity
of carbon, increasing the carbide precipitation temperature and producing a coarser
carbide As a result, the problems created by improper cooling alter the intermediate
anneal are aggravated at higher silicon. The teachings of the present invention overcome
these problems
[0008] The present invention is directed to the production of regular grain oriented silicon
steel starting with a melt chemistry having a silicon content of from 3% to 45% and
a low carbon content of less than 0 07% The routing of The present invention follows
the conventional routing given above with two exceptions
[0009] First, the present invention contemplates a modified intermediate anneal procedure
following the first stage of cold rolling The modified intermediate anneal procedure
preferably has a short soak at a lower temperature than the typical prior art intermediate
anneal and includes a temperature controlled two-stage cooling cycle, as will be fully
described hereinafter.
[0010] The intermediate anneal cooling practice of the present invention provides for austenite
decomposition in the first slow stage of cooling prior to precipitation of fine iron
carbide in the second rapid stage of cooling. The short soak feature and austenite
decomposition are facilitated by the low melt carbon
[0011] Second the routing of the present invention preferably includes an ultra-rapid annealing
treatment prior to decarburization. The ultra-rapid annealing treatment improves the
overall magnetic quality by improving the recrystallization texture The ultra-rapid
annealing treatment is of the type set forth in U S Patent 4,898,626.
[0012] Brietly. U.S Patent 4,898,626 teaches that the ultra-rapid annealing treatment is
performed by heating the electrical steel at a rate in excess ot 180° F (100° C) per
second to a temperature above the recrystallization temperature. nominally 1250° F
(675° C) The ultra-rapid annealing treatment can be performed at any point in the
routing after at least a first stage of cold rolling and before the decarburization
anneal preceding the final anneal. A preferred point in the routing is after the completion
of cold rolling and before the decarburization anneal. The ultra-rapid annealing treatment
may be accomplished either prior to the decarburization anneal. or may be incorporated
into the decarburization anneal as a heat-up portion thereof
[0013] US-A-3 929 522 discloses first, slow and second, fast, coding stages, the second
stage being made by water quenching, wherein the second stage produces a high permeability
silicon steel.
DISCLOSURE OF THE INVENTION
[0014] According to the invention there is provided a method for processing regular grain
onented silicon steel naving a thickness in the range of from 14 mils (0.35 mm) to
6 mils (0.15 mm) or less comprising the steps or providing electrical steel consisting
of, in weight percent, less than 0 07% carbon, 0 025% to 0 25% manganese, 0.01% to
0.035% sulfur and/or selenium. 3.0% to 4 5% silicon, less than 100 ppm total aluminum,
less than 50 ppm nitrogen the balance being iron and impurities. Additions of boron
and/or copper can be made, if desired.
[0015] To this end, the starting material referred to as "hot band" can be produced by a
number of methods known in the an such as ingot casting/continuous casting and hot
rolling, or by strip casting.
[0016] The hot band is subjected to an anneal at about 1850° F (1010° C) for a soak time
of about 30 seconds, followed by air cooling to ambient temperature it has been found
that this not band anneal can be omitted, particularly when making a regular grain
oriented electrical steel having a silicon content at the lower portion or the range.
[0017] Thereafter. the electrical steel is cold rolled to intermediate gauge. The cold rolled
intermediate thickness electrical steel is subjected to an intermediate anneal at
1650° F to 2100° F (900° C to 1150° C) and preferably from 1650° F to 1700° F (from
900° C to 930° C) for a soak time of from 1 to 30 seconds, and preferably from 3 to
8 seconds Following this soak, the electrical steel is cooled in two stages. The first
is a slow cooling stage from soak temperature to a temperature of from 1000° F to
1200° F (540° C to 650° C), and preferably to a temperature of 1100° F ± 50° F (595°
C ± 30° C) at a rate less than 1500° F (835° C) per minute, and preferably at a rate
of from 500° F (280° C) to 1050° F (585°C) per minute. The second stage is a last
cooling stage at a rate of greater than 1500° F (835° C) per minute and preferably
at a rate of 2500° F to 3500° F (1390° C to 1945° C) per minute, followed by a water
quench at 600° F to 1000° F (315° C to 540° C). Following the intermediate anneal,
the electrical steel is cold rolled to final gauge. decarburized, coated with an annealing
separator, and subjected to a final anneal to effect secondary recrystallization
[0018] In a preferred practice of the invention, the electrical steel is subjected to an
ultra-rapid annealing treatment of the type described above This can be performed
at any point in the routing after at least a first stage of cold rolling, and before
decarburization. It is generally preferred to perform the ultra-rapid annealing treatment
upon completion of cold rolling and before the decarburization anneal. As indicated
above, the ultra-rapid anneal may be incorporated into the decarburization annealing
step as a heat-up portion thereof
BRIEF DESCRIPTION OF THE DRAWING
[0019] The Figure is a graph illustrating the intermediate anneal time/temperature cycle
of the present invention and of a typical prior an intermediate anneal
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0020] In the practice of the present invention, the routing for the high silicon, low melt
carbon regular grain oriented electrical steel is conventional and is essentially
the same as that given above with three exceptions. The first exception is that the
hot band anneal can be omitted, if desired. Where equipment and conditions permit,
the practice of a hot band anneal is recommended since it makes the high silicon regular
grain oriented electrical steel less brittle and more amenable to cold rolling. Furthermore,
it tends to contribute to more stable secondary recrystallization. When practiced,
a hot band anneal is provided at a temperature of about 1850°F (1010° C) at a soak
time of about 30 seconds. The hot band anneal is followed by air cooling to ambient
temperature. The second exception is the development of the intermediate anneal and
cooling practice of the present invention following the first stage of cold rolling.
Finally, the third exception is the optional, but preferred, use of an ultra-rapid
annealing treatment prior to decarburization.
[0021] Following the first stage of cold rolling, the silicon steel is subjected to an intermediate
anneal in accordance with the teachings of the present invention. Reference is made
to the Figure, which is a schematic of the time/temperature cycle for the intermediate
anneal of the present invention. The Figure also shows, with a broken line, the time/temperature
cycle for a typical, prior art intermediate anneal.
[0022] A primary thrust of the present invention is the discovery that the intermediate
anneal and its cooling cycle can be adjusted to provide a fine carbide dispersion.
The anneal and its cooling cycle overcome the adverse effects of a higher silicon
content, described above.
[0023] During the heat-up portion of the intermediate anneal, recrystallization occurs at
about 1250° F (675° C), roughly 20 seconds after entering the furnace, after which
normal grain growth occurs. The start of recrystallization is indicated at "O" in
the Figure. Above about 1280° F (690° C) carbides will begin dissolving, as indicated
at "A" in the Figure. This event continues and accelerates as the temperature increases.
Above about 1650° F (900° C), a small amount of ferrite transforms to austenite. The
austenite provides for more rapid solution of carbon and restricts normal grain growth,
thereby establishing the intermediate annealed grain size. Prior art intermediate
anneal practice provided a soak at about 1740° F (950° C) for a period of at least
25 to 30 seconds. The intermediate anneal procedure of the present invention provides
a soak time of from 1 to 30 seconds, and preferably from 3 to 8 seconds. The soak
temperature has been determined not to be critical. The soak can be conducted at a
temperature of from 1650° F (900° C) to 2100° F (1150° C). Preferably, the soak is
conducted at a temperature of from 1650° F (900° C) to 1700° F (930° C), and more
preferably at about 1680° F (915° C). The shorter soak time and the lower soak temperature
are preferred because less austenite is formed. Further, the austenite present in
the form of dispersed islands at the prior ferrite grain boundaries is finer. Thus,
the austenite is easier to decompose into ferrite with carbon in solid solution for
subsequent precipitation of fine iron carbide. To extend either the soak temperature
or time results in the enlargement of the austenite islands which rapidly become carbon-rich
compared to the prior ferrite matrix. Both growth and carbon enrichment of the austenite
hinder its decomposition during cooling. The desired structure exiting the furnace
consists of a recrystallized matrix of ferrite having less than about 5% austenite
uniformly dispersed throughout the material as fine islands. At the end of the anneal,
the carbon will be in solid solution and ready for reprecipitation on cooling. The
primary reason behind the redesign of the intermediate anneal time and temperature
at soak is the control of the growth of the austenite islands. The lower temperature
reduces the equilibrium volume fraction of austenite which forms. The shorter time
reduces carbon diffusion, thereby inhibiting growth and undue enrichment of the austenite.
The lower strip temperature, the reduced volume fraction and the finer morphology
of the austenite make it easier to decompose during the cooling cycle.
[0024] Immediately after the soak, the cooling cycle is initiated. The cooling cycle of
the present invention contemplates two stages. The first stage extending from soak
to the point "E" on the Figure is a slow cool from soak temperature to a temperature
of from 1000° F (540° C) to 1200° F (650° C) and preferably to 1100° ± 50° F (595°
C ± 30° C). This first slow cooling stage provides for the decomposition of austenite
to carbon-saturated ferrite. Under equilibrium conditions, austenite decomposes to
carbon-saturated ferrite between from about 1650° F (900° C) and 1420° F (770° C).
However, the kinetics of the cooling process are such that austenite decomposition
does not begin in earnest until the mid 1500° F (815° C) range and continues somewhat
below 1100° F (595° C).
[0025] Failure to decompose the austenite in the first cooling stage will result in the
formation of martensite and/or pearlite. Martensite, if present, will cause an enlargement
of the secondary grain size, and the deterioration of the quality of the (110)[001]
orientation. Its presence adversely affects energy storage in the second stage of
cold rolling, and results in poorer and more variable magnetic quality of the final
electrical steel product. Lastly, martensite degrades the mechanical properties, particularly
the cold rolling characteristics. Pearlite is more benign, but still ties up carbon
in an undesired form.
[0026] As indicated above, austenite decomposition begins at about point "C" in the Figure
and continues to about point "E". At point "D" fine iron carbide begins to precipitate
from the carbon-saturated ferrite. Under equilibrium conditions, carbides begin to
precipitate from carbon-saturated ferrite at temperatures below 1280° F (690° C).
However, the actual process requires some undercooling to start precipitation, which
begins in earnest at about 1200° F (650° C). It will be noted that the austenite decomposition
to carbon-rich ferrite and carbide precipitation from the ferrite overlap somewhat.
The carbide is in two forms. It is present as an intergranular film and as a fine
intragranular precipitate. The former precipitates at temperatures above about 1060°
F (570° C). The latter precipitates below about 1060° F (570° C). The slow cooling
first stage, extending from point "C" to point "E" of the Figure has a cooling rate
of less than 1500° F (835° C) per minute, and preferably from 500° F to 1050° F (280°
C to 585° C) per minute.
[0027] The second stage of the cooling cycle, a fast cooling stage, begins at point "E"
in the Figure and extends to point "G" between 600° F and 1000° F (315° C and 540°
C) at which point the strip can be water quenched to complete the rapid cooling stage.
The strip temperature after water quenching is 150° F (65° C) or less, which is shown
in the Figure as room temperature (75° F or 25° C). During the second cooling stage,
the cooling rate is preferably from 2500° F to 3500° F (1390° C to 1945° C) per minute
and preferably greater than 3000° F (1665° C) per minute. This assures the precipitation
of fine iron carbide.
[0028] It will be evident from the above that the entire intermediate anneal and cooling
cycle of the present invention is required in the process of obtaining the desired
microstructure, and precise controls are critical. The typical prior art cycle time
shown in the Figure required at least 3 minutes, terminating in a water bath, not
shown, at a strip speed of about 220 feet per minute (57 meters per minute). The intermediate
anneal cycle time of the present invention requires about 2 minutes, 10 seconds which
enabled a strip speed of about 260 feet per minute (80 meters per minute) to be used.
It will therefore be noted that the annealing cycle of the present invention enables
greater productivity of the line. No aging treatment after the anneal is either needed
or desired, since it has been found to cause the formation of an enlarged secondary
grain size which degrades the magnetic quality of the final electrical steel product.
[0029] The intermediate anneal is followed by the second stage of cold rolling reducing
the electrical steel to the desired final gauge. At this stage, the electrical steel
can be decarburized, coated with an annealing separator and subjected to a final anneal
to effect secondary recrystallization.
[0030] In the preferred practice of the present invention, the electrical steel is given
an ultra-rapid annealing treatment after cold reduction and prior to decarburization.
To this end, the electrical steel at final gauge is heated at a rate above 180° F
(100° C) per second to a temperature above 1250° F (675° C). Preferably, the electrical
steel is heated at a rate of 1000° F (540° C) per second. It is additionally preferred
that the ultra-rapid annealing treatment be performed as a heat-up portion of the
decarburizing anneal.
[0031] The preferred chemistry of the present invention in weight % is as follows: less
than 0.05% carbon, 0.04% to 0.08% manganese, 0.015% to 0.025% sulfur and/or selenium,
3.25% to 3.75% silicon, less than 100 ppm aluminum, less than 50 ppm nitrogen, additions
of boron and/or copper, can be made if desired, the balance being essentially iron.
[0032] The ultra-rapid annealing treatment improves the recrystallization texture after
decarburization by creating more (110)[001] primary grains. It also contributes to
smaller secondary grain size. When an ultra-rapid annealing treatment is incorporated
into the process, the process is less sensitive to intermediate and final gauge variations
and the magnetic characteristics of the regular grain oriented silicon steel are improved
and more consistent.
EXAMPLE I
[0033] Four heats were melted having the compositions in weight % shown in Table I. The
heats were prepared by continuous casting into 8" (200 mm) thick slabs, prerolling
the 8" thick slabs to 6" (150 mm), reheating to 2550° F (1400° C) and hot rolling
to 0.084" (2.1 mm) hot bands for subsequent processing. The plant processing followed
a routing using a 1850° F (1010° C) hot band annealing treatment and cold rolling
to various intermediate thicknesses; however, Heats A and B were processed using a
typical prior art intermediate anneal with a 1740° F (950° C) soak for 25-30 seconds
followed by normal ambient cooling while Heats C and D were intermediate annealed
according to the practice of the present invention. After intermediate annealing,
the materials were cold rolled to final thicknesses of 7-mils (0.18 mm) and 9-mils
(0.28 mm). After completing cold rolling, the materials were decarburized at 1525°
F (830° C) in a wet hydrogen-bearing atmosphere, MgO coated and given a final anneal
at 2200° F (1200° C). The resulting magnetic quality obtained in these trials are
summarized in Table III.
TABLE I
| Code |
C |
Mn |
S |
Si |
Al |
Cu |
P |
N |
| A |
0.0288 |
0.059 |
0.0198 |
3.41 |
0.0013 |
0.092 |
0.006 |
0.0042 |
| B |
0.0296 |
0.059 |
0.0209 |
3.42 |
0.0014 |
0.118 |
0.006 |
0.0038 |
| C |
0.0265 |
0.058 |
0.0218 |
3.44 |
0.0012 |
0.097 |
0.005 |
0.0040 |
| D |
0.0274 |
0.058 |
0.0212 |
3.36 |
0.0012 |
0.085 |
0.006 |
0.0035 |

[0034] The results clearly show that the practice of the intermediate anneal cycle of the
present invention provided improved core loss and enhanced stability of secondary
grain growth for these regular grain oriented materials.
EXAMPLE II
[0035] Additional samples from Heats A and B were secured during plant processing trials
for laboratory processing. Plant processing followed the conventional routing of example
I; however, after cold rolling to intermediate thickness was completed, the samples
were secured in the plant and processed in the laboratory in accordance with the teachings
of the present invention wherein the intermediate annealing soak temperatures and
times and controlled cooling practice were employed and the more preferred practice
utilizing an ultra-rapid annealing treatment after completion of cold rolling and
prior to decarburization was employed. In the practice of the latter, a 1000° F (556°
C) per second heating rate from room temperature to 1375° F was incorporated into
the heat-up portion of the decarburization anneal. After the intermediate anneal,
the materials were cold rolled to 7-mils (0.18 mm) final thickness and decarburized
at 1525° F (830° C) in a wet hydrogen-bearing atmosphere using either conventional
techniques and ultra-rapid annealing treatment during heating. After decarburization,
the samples were MgO coated and given a final anneal at 2200° F (1200° C). The results
of these runs are summarized in Table III.

[0036] The results clearly show that the practice of the intermediate anneal cycle of the
present invention provided improved core loss and enhanced the stability of secondary
grain growth for these regular grain oriented materials. The more preferred practice
whereby an ultra-rapid annealing treatment in addition to the intermediate anneal
cycle of the present invention further provided for still more improvement in the
magnetic quality.
1. A process for producing high silicon, low melt carbon, regular grain oriented electrical
steel having a thickness of from 14 mils (0.35 mm) to 6 mils (0.15 mm) or less, comprising
the steps of providing a hot band of silicon steel wherein said silicon steel consists
of, in weight percent, less than 0.07% carbon, 0.025% to 0.25% manganese, 0.01% to
0.035% sulfur and/or selenium, 3.0% to 4.5% silicon, less than 100 ppm aluminum, less
than 50 ppm nitrogen, additions of boron and/or copper, if desired, the balance being
iron and impurities, annealing said hot band, removing the hot band scale if required,
cold rolling to intermediate gauge, subjecting said intermediate gauge material to
an intermediate anneal at a soak temperature of from 1650°F (900°C) to 2100°F (1150°C)
for a soak time of from 1 second to 30 seconds, conducting a slow cooling stage from
said soak temperature to a temperature of from 1000°F (540°C) to 1200°F (650°C) at
a cooling rate less than 1500°F (835°C) per minute, thereafter conducting a fast cooling
stage to a temperature of from 600°F (315°C) to 1000°F (540°C) at a rate greater than
1500°F (835°C) per minute, followed by a water quench, cold rolling said silicon steel
to final gauge, subjecting said final gauge silicon steel to a decarburizing anneal,
coating said decarburized silicon steel with an annealing separator, and subjecting
said silicon steel to a final anneal to effect secondary recrystallization.
2. The process claimed in claim 1 wherein said silicon content in weight percent is 3.25%-3.75%.
3. The process claimed in claim 1 wherein said hot band anneal is conducted at a temperature
of about 1850°F (1010°C) with a soak time of about 30 seconds and air cooling to ambient
temperature.
4. The process claimed in claim 1 including the step of subjecting said silicon steel
at a final gauge and before decarburization to an ultra-rapid annealing treatment
to a temperature greater than 1250°F (675°C) at a heating rate greater than 180°F
(100°C) per second.
5. The process claimed in claim 1 including the step of conducting said intermediate
anneal with a soak time of from 3 to 8 seconds.
6. The process claimed in claim 1 including the step of conducting said intermediate
anneal at a soak temperature of from 1650°F (900°C) to 1700°F (930°C).
7. The process claimed in claim 1 including the step of conducting said intermediate
anneal at a soak temperature of about 1680°F (915°C).
8. The process claimed in claim I including the step of terminating said slow cooling
stage at a temperature of 1100° ± 50°F (595°C ± 30°C).
9. The process claimed in claim 1 including the step of conducting said slow cooling
stage at a cooling rate of from 500°F (280°C) to 1050°F (585°C) per minute.
10. The process claimed in claim I including the step of conducting said fast cooling
stage at a cooling rate of 2500°F (1390°C) to 3500°F (1945°C) per minute.
11. The process claimed in claim 1 including the steps of conducting said intermediate
anneal with a soak temperature of about 1680°F (915°C) for a soak time of 3 to 8 seconds,
conducting said slow cooling stage at a cooling rate of 500°F (280°C) to 1050°F (585°C)
per minute, terminating said slow cooling stage at a temperature of 1100°f ± 50°F
(595°C ± 30°C), and conducting said fast cooling stage at a rate of from 2500°F (1390°C)
to 3500°F (1945°C) per minute.
12. The process claimed in claim 1 including the step of subjecting said silicon steel
at final gauge and before decarburization to an ultra-rapid annealing treatment to
a temperature greater than 1250°F (675°C) at a heating rate greater than 180°F (100°C)
per second.
13. The process claimed in claim 11 wherein said hot band anneal is conducted at a temperature
of about 1850°F (1010°C) with a soak of about 30 seconds and air cooling to ambient
temperature.
14. The process claimed in claim 12 including the step of performing said ultra-rapid
annealing treatment as a heat-up portion of said decarburizing anneal.
15. The process claimed in claim 13 including the step of subjecting said silicon steel
at final gauge and before decarburization to an ultra-rapid annealing treatment to
a temperature greater than 1250°F (675°C) at a heating rate greater than 180°F (100°C)
per second.
16. The process claimed in claim 15 including the step of performing said ultra-rapid
annealing treatment as a heat-up portion of said decarburizing anneal.
17. The process claimed in claim 1 wherein said silicon steel contains, in weight percent,
less than 0.05% carbon, 0.04% to 0.08% manganese, 0.015% to 0.025% sulfur and/or selenium,
and 3.25% to 3.75% silicon.
1. Verfahren zur Herstellung von regulär-kornorientiertem Elektrostahl mit einem hohen
Anteil an Silizium und einem niedrigen Anteil an Kohlenstoff in der Schmelze sowie
einer Stärke von 14 mil (0,35 mm) bis 6 mil (0,15 mm) oder weniger, das folgende Schritte
umfaßt: Bereitstellung eines Warmwalzbandes aus Siliziumstahl, wobei der Siliziumstahl
aus weniger als 0,07 Gew.-% Kohlenstoff, 0,025 bis 0,25 Gew.-% Mangan, 0,01 bis 0,035
Gew.-% Schwefel und/oder Selen, 3,0 bis 4,5 Gew.-% Silizium, weniger als 100 ppm Aluminium,
weniger als 50 ppm Stickstoff, gegebenenfalls Bor- und/oder Kupferzusätzen, und zum
Rest aus Eisen und Verunreinigungen besteht, Glühen des Warmwalzbandes, gegebenenfalls
Entfernung des Walzzunders vom Warmwalzband, Kaltwalzen auf eine mittlere Stärke,
Zwischenglühen dieses Materials mittlerer Stärke bei einer Durchwärmtemperatur von
1650° F (900°C) bis 2100° F (1150° C) und einer Durchwärmzeit von 1 Sekunde bis 30
Sekunden, langsames Abkühlen des Materials von der Durchwärmtemperatur auf eine Temperatur
von 1000° F (540° C) bis 1200° F (650° C) mit einer Abkühlgeschwindigkeit von weniger
als 1500° F (835° C) pro Minute, danach schnelles Abkühlen auf eine Temperatur von
600° F (315° C) bis 1000° F (540° C) mit einer Abkühlgeschwindigkeit von mehr als
1500° F (835° C) pro Minute, anschließendes Abschrecken mit Wasser, Kaltwalzen des
Siliziumstahls auf die endgültige Stärke, Entkohlen des Siliziumstahls endgültiger
Stärke, Beschichten des entkohlten Siliziumstahls mit einem Glühtrennmittel und Endglühen
des Siliziumstahls zum Zwecke der Nachkristallisation.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Siliziumgehalt 3,25-3,75
Gew.-% beträgt.
3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Warmwalzband bei einer
Temperatur von etwa 1850° F (1010° C) während einer Durchwärmzeit von etwa 30 Sekunden
geglüht und mit Luft auf Raumtemperatur abgekühlt wird.
4. Verfahren nach Anspruch 1, ferner gekennzeichnet durch Ultraschnellglühen des Siliziumstahls
endgültiger Stärke vor dem Entkohlen mit einer Erwärmungsgeschwindigkeit von mehr
als 180° F (100° C) pro Sekunde auf eine Temperatur von mehr als 1250° F (675° C).
5. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Zwischenglühen während
einer Durchwärmzeit von 3 bis 8 Sekunden erfolgt.
6. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Zwischenglühen bei einer
Durchwärmtemperatur von 1650° F (900° C) bis 1700° F (930° C) erfolgt.
7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Zwischenglühen bei einer
Durchwärmtemperatur von etwa 1680° F (915° C) erfolgt.
8. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die langsame Abkühlung bei
einer Temperatur von 1100° F ± 50° F (595° C ± 30° C) beendet wird.
9. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die langsame Abkühlung mit
einer Abkühlgeschwindigkeit von 500° F (280° C) bis 1050° F (585° C) pro Minute erfolgt.
10. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die schnelle Abkühlung mit
einer Abkühlgeschwindigkeit von 2500° F (1390° C) bis 3500° F (1945° C) pro Minute
erfolgt.
11. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Zwischenglühen bei einer
Durchwärmtemperatur von etwa 1680° F (915° C) während einer Durchwärmzeit von 3 bis
8 Sekunden erfolgt, das langsame Abkühlen mit einer Abkühlgeschwindigkeit von 500°
F (280° C) bis 1050° F (585° C) pro Minute erfolgt und bei einer Temperatur von 1100°
F ± 50° F (595° C ± 30° C) beendet wird, und daß die schnelle Abkühlung mit einer
Abkühlgeschwindigkeit von 2500° F (1390° C) bis 3500° F (1945° C) pro Minute erfolgt.
12. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Siliziumstahl endgültiger
Stärke vor dem Entkohlen in einem Ultraschnellglühverfahren mit einer Erwärmungsgeschwindigkeit
von mehr als 180° F (100° C) pro Sekunde auf eine Temperatur von mehr als 1250° F
(675° C) gebracht wird.
13. Verfahren nach Anspruch 11, dadurch gekennzeichnet, daß das Warmwalzband bei einer
Temperatur von etwa 1850° F (1010° C) während einer Durchwärmzeit von etwa 30 Sekunden
geglüht und mit Luft auf Raumtemperatur abgekühlt wird.
14. Verfahren nach Anspruch 12, dadurch gekennzeichnet, daß das Ultraschnellglühen als
eine Erwärmungsphase der Entkohlung durchgeführt wird.
15. Verfahren nach Anspruch 13, dadurch gekennzeichnet, daß der Siliziumstahl endgültiger
Stärke vor dem Entkohlen in einem Ultraschnellglühverfahren mit einer Erwärmungsgeschwindigkeit
von mehr als 180° F (100° C) pro Sekunde auf eine Temperatur von mehr als 1250° F
(675° C) gebracht wird.
16. Verfahren nach Anspruch 15, dadurch gekennzeichnet, daß das Ultraschnellglühen als
eine Erwärmungsphase der Entkohlung durchgeführt wird.
17. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Siliziumstahl weniger als
0,05 Gew.-% Kohlenstoff, 0,04 bis 0,08 Gew.-% Mangan, 0,015 bis 0,025 Gew.-% Schwefel
und/oder Selen und 3,25 bis 3,75 Gew.-% Silizium enthält.
1. Procédé de production d'acier électrique ordinaire à haute teneur en silicium, à faible
teneur en carbone fondu et à grains orientés ayant une épaisseur de 0,35 mm (14 mils)
à 0,15 mm (6 mils) ou moins, comprenant les étapes consistant à mettre en oeuvre une
bande chaude d'acier au silicium, dans lequel ledit acier au silicium comprend, en
pourcentage en poids, moins de 0,07 % de carbone, 0,025 à 0,25 % de manganèse, 0,01
à 0,035 % de soufre et/ou de sélénium, 3,0 à 4,5 % de silicium, moins de 100 ppm d'aluminium,
moins de 50 ppm d'azote, des additions de bore et/ou de cuivre, si on le souhaite,
le reste étant essentiellement du fer, à recuire ladite bande chaude, à éliminer la
calamine de la bande chaude si c'est nécessaire, à laminer à froid à un calibre intermédiaire,
à soumettre ledit matériau à calibre intermédiaire à un recuit intermédiaire à une
température de trempe de 900 °C (1 650 °F) à 1 150 °C (2 100 °F) pendant une période
de trempe de 1 à 30 secondes, à réaliser une étape de refroidissement lente à partir
de ladite température de trempe jusqu'à une température de 540 °C (1 000 °F) à 650
°C (1 200 °F) à une cadence de refroidissement inférieure à 835 °C (1 500 °F) par
minute, à réaliser ensuite une étape de refroidissement rapide jusqu'à une température
de 315 °C (600 °F) à 540 °C (1 000 °F) à une cadence supérieure à 835 °C (1 500 °F)
par minute, le tout étant suivi d'une trempe à l'eau, à laminer à froid ledit acier
au silicium jusqu'au calibre final, à soumettre ledit acier de silicium au calibre
final à un recuit de décarburation, à revêtir ledit acier au silicium décarburé par
un séparateur de recuit et à soumettre ledit acier de silicium à un recuit final pour
effectuer une recristallisation secondaire.
2. Procédé selon la revendication 1, dans lequel ladite teneur en silicium est de 3,25
à 3,75 % en poids.
3. Procédé selon la revendication 1, dans lequel ledit recuit de la bande chaude est
réalisé à une température d'environ 1 010 °C (1 850 °F) avec une durée de trempe d'environ
30 secondes et un refroidissement à l'air jusqu'à la température ambiante.
4. Procédé selon la revendication 1, comprenant l'étape consistant à soumettre ledit
acier au silicium, au calibre final et avant décarburation, à un traitement de recuit
ultra-rapide jusqu'à une température supérieure à 675 °C (1 250 °F) à une cadence
de chauffage supérieure à 100 °C (180 °F) par seconde.
5. Procédé selon la revendication 1, comprenant l'étape consistant à réaliser ledit recuit
intermédiaire avec une durée de trempe de 3 à 8 secondes.
6. Procédé selon la revendication 1, comprenant l'étape consistant à réaliser ledit recuit
intermédiaire à une température de trempe de 900 °C (1 650 F) à 930 °C (1 700 °F).
7. Procédé selon la revendication 1, comprenant l'étape consistant à réaliser ledit recuit
intermédiaire à une température de trempe d'environ 915 °C (1 680 °F).
8. Procédé selon la revendication 1, comprenant l'étape consistant à terminer ladite
étape de refroidissement lente à une température de 595 °C plus ou moins 30 °C (1
100 °F plus ou moins 50 °F).
9. Procédé selon la revendication 1, comprenant l'étape consistant à effectuer ladite
étape de refroidissement lente à une cadence de refroidissement de 280 °C (500 °F)
à 585 °C (1 050 °F) par minute.
10. Procédé selon la revendication 1, comprenant l'étape consistant à réaliser ladite
étape de refroidissement rapide à une cadence de refroidissement de 1 390 °C (2 500
°F) à 1 945 °C (3 500 °F) par minute.
11. Procédé selon la revendication 1, comprenant les étapes consistant à effectuer ledit
recuit intermédiaire à une température de trempe d'environ 915 °C (1 680 °F) pendant
une période de trempe de 3 à 8 secondes, à réaliser ladite étape de refroidissement
lente à une cadence de refroidissement de 280 °C (500 °F) à 585 °C (1 050 °F) à la
minute, à terminer ladite étape de refroidissement lente à une température de 595
°C plus ou moins 30 °C (1 100 °F plus ou moins 50 °F) et à réaliser ladite étape de
refroidissement rapide à une cadence de 1 390 °C (2 500 °F) à 1 945 °C (3 500 °F)
par minute.
12. Procédé selon la revendication 1, comprenant l'étape consistant à soumettre ledit
acier au silicium, au calibre final et avant décarburation, à un traitement de recuit
ultra-rapide jusqu'à une température supérieure à 675 °C (1 250 °F) à une cadence
de chauffage supérieure à 100 °C (180 °F) par seconde.
13. Procédé selon la revendication 11, dans lequel ledit recuit de la bande chaude est
réalisé à une température d'environ 1 010 °C (1 850 °F) avec une période de trempe
d'environ 30 secondes et un refroidissement à l'air jusqu'à la température ambiante.
14. Procédé selon la revendication 12, comprenant l'étape consistant à effectuer ledit
traitement de recuit ultra-rapide en tant que partie de réchauffement dudit recuit
de décarburation.
15. Procédé selon la revendication 13, comprenant l'étape consistant à soumettre ledit
acier au silicium, au calibre final et avant décarburation, à un traitement de recuit
ultra-rapide jusqu'à une température supérieure à 675 °C (1 250 °F) à une cadence
de chauffage supérieure à 100 °C (180 °F) par seconde.
16. Procédé selon la revendication 15, comprenant l'étape consistant à effectuer ledit
traitement de recuit ultra-rapide en tant que partie de réchauffement dudit recuit
de décarburation.
17. Procédé selon la revendication 1, dans lequel ledit acier au silicium comprend, en
pourcentage en poids, moins de 0,05 % de carbone, 0,04 à 0,08 % de manganèse, 0,015
à 0,025 % de soufre et/ou de sélénium et 3,25 à 3,75 % de silicium.
