US3438820A - Silicon steel process - Google Patents

Silicon steel process Download PDF

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Publication number
US3438820A
US3438820A US445023A US3438820DA US3438820A US 3438820 A US3438820 A US 3438820A US 445023 A US445023 A US 445023A US 3438820D A US3438820D A US 3438820DA US 3438820 A US3438820 A US 3438820A
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steel
temperature
strip
silicon
ladle
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US445023A
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Norman P Goss
James Black
William J Stewart
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ArcelorMittal Dofasco Inc
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Dominion Foundries and Steel Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon

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  • SILICON STEEL PROCESS Filed April 2. 1965 INVENTORS NORMAN P. GOSS-JAMES B LACK WlLLI M J. STEWART BY PATENT AGENTS United States Patent Office 3,438,820 Patented Apr. 15, 1969 3,438,820 SILICON STEEL PROCESS Norman P. Goss, Mentor, Ohio, and James Black and William J. Stewart, Burlington, Ontario, Canada, as-
  • the vessel in the vessel and is discharged at at least about 2900" F, to the ladle; the steel is stirred in the ladle and discharged to an ingot mould; the resulting ingot is hot rolled and then cold rolled to obtain the oriented crystal structure; the cold rolled material is unexpectedly magnetically clean, giving improved magnetic properties, and can be decarburized unexpectedly rapidly in a period of not less than about 5 seconds and not more than about one minute to carbon contents of not more than about .005
  • This invention relates to processes for the production of silicon steel of the type suitable for the production of highly grain-orientated silicon steel for magnetic purposes, and to processes for the production of such highly grain-orientated silicon steel. More particularly, the invention relates to processes for the production of silicon steel suitable for the production of strip and sheet having the desired Goss texture, and in which there is a high degree of [110] (001) orientation (or cube-on-edge crystal orientation) in the direction of rolling, and to processes for the production of such strip and sheet.
  • the silicon steels used commercially for this purpose have a silicon content of about 2.5% to 4%, the higher silicon contents being preferred because of the better magnetic properties that are obtainable.
  • a silicon content greater than about 3.3% has not been commercially economical hitherto, because of the extensive edge cracking and breaking encountered during the subsequent cold rolling operations.
  • the carbon content of the steel must be kept as low as possible and to this end it has either been produced by an open hearth process using oxygen, for example a process as described by US. Patent No. 2,580,164 issued Jan. 1, 1952 to Slottman, or by processes known in the industry as Basic Oxygen steelmaking processes, particularly that known as the LD Process, as described in U.S. Patent No. 2,800,621, issued July 23, 1957 to Suess et a1. Problems encountered hitherto in obtaining low carbon contents with an LD process are described in U. S. Patent No. 3,030,203, issued Apr.
  • Silicon and sulphur are added to the steel at the end of the steelmaking process, and may be added in the furnace, or in the ladle into which the steel is poured from the furnace; more usally the latter.
  • the purpose of the sulphur is to form manganese sulphide with the maganese always present; this particular sulphide has the property of entering the grain boundaries as the steel cools and crystallizes and ensuring the formation of the desired primary grain structure during the hot rolling operation.
  • the silicon is usually added to the steel in the form of ferrosilicon which dissolves readily to form layers of silicon content higher than is desired, and these higher-silicon-content layers tend to remain separate from the lower-silicon-content layers unless positive action is taken to prevent this so-called Stratification.
  • ferrosilicon dissolves readily to form layers of silicon content higher than is desired, and these higher-silicon-content layers tend to remain separate from the lower-silicon-content layers unless positive action is taken to prevent this so-called Stratification.
  • Hilliard patent it is proposed in the above-mentioned Hilliard patent to rock the furnace.
  • the ingots thus produced are usually heat soaked for a predetermined period and then rolled to slab form, each sla'b thereafter being hot rolled to strip form, either by the so-called direct hot working process or by the slab-reheating process.
  • the slab is rolled without any intermediate reheating, while in the second process it is reheated to a high temperature in the neighbourhood of 2300 F. to 2550 F. before being rolled into strip.
  • the hot rolling to strip form is a critical step in the formation of commercially useful material because of the formation of the abovedescribed primary grain structure and relatively precise control of the rolling temperatures has been regarded as essential.
  • the hot rolled strip is descaled and is cooled quickly to prevent further grain growth and keep the primary grains small and highly dispersed.
  • the rapid cooling also prevents conversion of the finely dispersed carbon inclusions into carbides that can only be removed with considerable dilficulty.
  • the cooled strip is then given a first cold roll to a thickness usually of about 50% of the desired final thickness, the degree of reduction employed being carefully selected because of its effect on the desired orientation of the grain structures in the direction of rolling. It has also been essential, once a particular intermediate thickness has been selected, to maintain that thickness to within very close limits.
  • the cold rolled strip is cleaned and open annealed, usually at about 1650-1750 F. to provide stress relief and cause recrystallisation.
  • the partially reduced strip is then cold rolled to its final thickness, which usually is about .006 inch to .014 inch, the degree of reduction again being carefully selected and the rolling limits carefully controlled for the same reason.
  • the rolled strip is subjected to a decarburization treatment intended to reduce the carbon content to the lowest commercially practical value.
  • U.S. Patent No. 2,287,467 issued June 23, 1942 to Carpenter et al., describes a process in which the decarburizing conditions are intended to achieve a carbon content of about 0.005% and comprise a temperature within the range 1350 to 1650" F., and an atmosphere predominantly of hydrogen, but containing 4% to 35% water vapour; preferably the duration of the Carpenter et al. process is not to exceed 30 minutes, and more particularly it is take between 2 and '14 minutes.
  • the strip is coated with a refractory oxide and subjected to a desulphurizing box anneal at about 2000-2200 F. in an atmosphere of pure hydrogen, this process causing the desired exaggerated secondary grain growth of the orientated cube-on-edge primary grains. Thereafter, the oxide coating is removed, the strip is thermally flattened if necessary, and the strip is cut to its final strip or sheet form.
  • a premium quality magnetic steel preferably has an A.C. permeability at a magnetizing force of oersteds of not less than about 1800,
  • a process for the production of silicon steel containing substantially 2.5% to 4% silicon and suitable for the production of highly grain-oriented silicon steel for magnetic purposes comprising the steps of making the steel by a process in which gaseous oxygen is directed into the vessel interior to react with the contents of the vessel, the steel making process being continued until the contents of the vessel are at a temperature of at least about 3000" F., and discharging the resultant steel from the vessel at a temperature of at least about 2900 F.
  • the steel making process is continued until the contents of the vessel are at a temperature of at least about 3100" F. to 3250 F.
  • the steel may be stirred in the said ladle to ensure the absence of Stratification of the contents thereof, and preferably it is stirred with an ingot of substantially the same composition as the said steel.
  • the steel preferably is discharged from the ladle at a temperature of at least about 2850 F. directly into ingot moulds.
  • the ingots thus produced are rolled into slabs which may be hot rolled with an exit temperature of anywhere between 1400 F. and 1700 F.
  • the hot rolled strip is thereafter cold rolled and annealed to produce a strip having the desired grainorientation in the direction of rolling, and subsequently decarburized, preferably by subjecting it for not less than about 5 seconds and not more than about 1 minute to decarburizing conditions such as to reduce the carbon content of the cold rolled strip to not more than about 005%, preferably 004%.
  • the said decarburizing conditions comprise a temperature of between about 1350 F. and about 1800" F., and an atmosphere comprising between about 5% and about 40% hydrogen, preferably 20%, remainder nitrogen, with a dew point of about F. and above. More preferably, the said decarburizing conditions comprise a temperature of between about 1650 F.
  • the cold rolled strip being subjected to such conditions for a period of not less than about 5 seconds and not more than about 20 seconds.
  • the decarburized cold rolled strip may be subjected to a desulphurizin'g box anneal in pure hydrogen at between about 2000 F. and 2200 F. to provide the necessary secondary grain growth and provide a highly grainorientated magnetically clean silicon steel having an A.C. magnetic permeability in a field of 10 oersteds of at least 1900.
  • the said magnetically clean silicon steel comprises from 3.3% to 3.7% silicon.
  • the steel is produced by a process that comes within the terms of the A.S.T.M. definition of a Basic Oxygen steelmaking process, namely one in which molten iron is refined to steel under a basic slag in a cylindrical furnace lined with basic refractories, by directing a jet of high purity gaseous oxygen onto the surface of the hot metal bath.
  • the process may be defined as an LD process, in which a vertically extending vessel has a lance extending vertically into the vessel, through which lance the jet of oxygen is directed into the vessel interior to react with the contents thereof.
  • the charge to the furnace is convenional for the production of silicon steel and the oxygen blowing is begun with the lance in an elevated position.
  • the height of the lance above the furnace contents and the rate of blowing of the oxygen are adjusted by the operator, based upon a predetermined schedule for the particular steel to be produced, and the observation by the operator of the progress of the process, usually comprising visual observation of the furnace and measurement of the temperature of the steel bath from time to time.
  • the steel making process is controlled by the operator so as to achieve a bath temperature near to the end of the process of at least about 3000 F.
  • the operator controls the process so that a temperature greater than 3050" F. is obtained, and more particularly it is preferred to obtain a temperature of between about 3l0O F. and 3250 F.
  • the upper temperature limit to be achieved by the process appears to be at least partly determined by the ability of the conventional LD furnace to operate safely at these unusually elevated temperatures.
  • the upper limit is also affected by commercial economic considerations in that at the elevated temperatures there is a higher conversion of the iron in the furnace charge to iron oxide that is retained in the slag, with a consequent loss of iron.
  • This discharge temperature should be at least 2900 F. and preferably is as high as possible, as close as possible to the maximum temperature achieved during the conversion process.
  • the silicon and sulphur can be added to the furnace, or to the ladle, and if to the latter will be added before the ladle is full, so that the remainder of the entering steel will stir the additions into the ladle contents.
  • the contents of the ladle are stirred before the ingots are poured, using an already-formed ingot of substantially the same composition as the steel.
  • a vertical-extending LD process furnace vessel 1 having a lance 2 through which a jet of oxygen is directed into the vessel onto the surface of the hot metal bath.
  • steel has been discharged from the vessel 1 through a tap hole 3 into a ladle 4.
  • the contents 5 of the ladle are in the process of being stirred by means of an ingot 6 which is suspended by a chain 7 from an overhead crane 8 with its lower portion in the molten metal.
  • the crane controls the operator thereof can move the ingot in the ladle with a circular backand-forth stirring motion that will in about 2 to 5 minutes of operation ensure adequate homogeneity of the whole of the ladles contents.
  • the stirred homogeneous steel is thereafter discharged from the ladle into preheated ingot moulds, the steel being discharged from the ladle at a temperature of at least about 2850 F. and preferably in the range 2870 F. to 2900 F., so that the ingots will be poured at a temperature of not less than about 2840 F., and preferably higher. It is known in prior art processes to maintain the ladle contents at as high a temperature as possible by the addition of slag thereto, but such a method is avoided in the practice of this invention because of the possibility of returning deleterious slag inclusions to the relatively magnetically clean steel.
  • the Table 2 below gives a desirable range and a typical value for the analysis of the steel discharged from the ladle.
  • the removal of these inclusions is also assisted by assuring that the deoxidization products produced in the ladle are such that the slag or scum developed therefrom has a high fluidity and high surface tension at the elevated temperature of opreation, causing the desired rapid coalescence of slag particles in the melt to more readily separated particles and the high retention of r these particles in the slag or scum.
  • the cast ingots are reheated prior to the hot rolling operation to about 2250 F. to 2350 F., and are held at this temperature for a period sufficient to ensure homogenisation of the microsegregation of the various elements of the steel.
  • Each ingot is first reduced in a hot rolling mill to an intermediate thickness of about As-P/z inches, usually A; inch.
  • the temperature at which this rolling is effected should be as high as possible, and the rolling should be completed as quickly as possible, but we have found that with a silicon steel in accordance with this invention a much lower temperature is permissible. In particular with our improved practice the temperature just before entering the finishing stands of the mill can be as low as 1800 F.
  • the hot rolled intermediate thickness material is then subjected to a final hot rolling in which its thickness is reduced to .060 to .120 inch, usually about 070-080 inch.
  • temperature control during hot rolling is essential in that it causes the development of the primary grain structure which will be developed into the described secondary grain structure during the desulphurizing treatment.
  • exit temperatures anywhere between about 1400 F. and 1700 F., and in particular the temperature gap found in the prior art processes no longer appears to exist, or if it does exist its effect on the production of commercial materials need not be considered.
  • exit temperature range available for hot rolling can be determined by consideration of other factors, such as the proper loading of the rolling mill and the surface finish required on the rolled Strip.
  • the Table 3 below shows the effect of the annealing temperature and the soak time of the decarburizing atmosphere on the carbon content of steels in accordance with this invention.
  • the decarburizing atmosphere employed was 20% hydrogen, nitrogen with water vapour to give dew point of 6070 F.
  • the preferred decarburizing conditions comprise a temperature of between about 1350 F. and about 1800 F., using an atmosphere comprising between about 5% and about 40% of hydrogen, the balance nitrogen and water vapour, with a dew point of about 60 F. and above.
  • the cold rolled strip is subjected to such conditions for a period of not less than about 5 seconds and not more than a period of one minute, preferably not more than 30 seconds and generally not more than 15 seconds.
  • the faster decarburization times will of course be accomplished at the higher temperatures, and we have found that the carbon removal process has commenced at temperatures at low as 1300 F.
  • the dwell time of the strip in the annealing furnace will usually be greater than the actual decarburizing time, since the strip enters the furnace at ambient atmospheric temperature and will take time to reach the minimum reaction temperature.
  • the decarburized strip may then be subjected to conventional processes of coating with an inorganic refactory material such as magnesium oxide, and desulphurization by a box anneal in pure hydrogen at about 2000 F.2200 F., preferably about 2050 F. Thereafter, the refactory material may be removed, the strip thermally flattened if necessary, and a suitable protective coating applied.
  • an inorganic refactory material such as magnesium oxide
  • desulphurization by a box anneal in pure hydrogen at about 2000 F.2200 F., preferably about 2050 F.
  • Table 4 sets out the general chemical ananlysis of highly grain-orientated silicon steel strip material produced in accordance with the present invention, together with a typical analysis of a particular material.
  • decarburizing conditions comprise a temperature of between about 1350 F. and about 1800 F., and an atmosphere comprising about between 5% and 40% hydrogen, balance nitrogen and water vapour with a dew point of about 60 F. and above.
  • decarburizing conditions comprise a temperature of between about 1650 F. and 1800 F. and an atomsphere comprising between about 5% and about 40% hydrogen, the balance nitrogen and water vapour with a dew point of about 60 F. and above, and the cold rolled strip is subjected to such conditions for a period of not less than about 5 seconds and not more than about 30 seconds.

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3662810A (en) * 1969-09-02 1972-05-16 Howmet Corp Method of internal nucleation of a casting
DE2348249A1 (de) * 1972-09-28 1974-04-04 Allegheny Ludlum Ind Inc Kornorientierter siliciumstahl und verfahren zu seiner herstellung
US3915694A (en) * 1972-09-05 1975-10-28 Nippon Kokan Kk Process for desulphurization of molten pig iron
US3955967A (en) * 1973-05-02 1976-05-11 The Algoma Steel Corporation, Limited Treatment of steel
DE2620593A1 (de) * 1975-05-15 1976-11-25 Allegheny Ludlum Ind Inc Verfahren zur herstellung von kornorientiertem siliciumstahl
JPS5431967B1 (cs) * 1971-04-08 1979-10-11
US4198035A (en) * 1977-10-11 1980-04-15 Voest-Alpine Aktiengesellschaft Blowing lance media-supply arrangement
FR2511045A1 (fr) * 1981-08-05 1983-02-11 Nippon Steel Corp Tole en acier electromagnetique a grain oriente et son procede d'obtention
AU601422B2 (en) * 1986-10-14 1990-09-13 Allegheny Ludlum Corporation Method of making steel
DE102011054004A1 (de) 2011-09-28 2013-03-28 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten, für elektrotechnische Anwendungen bestimmten Elektrobands oder -blechs
CN113897558A (zh) * 2021-10-08 2022-01-07 北京北冶功能材料有限公司 一种高饱和磁感高磁导率铁基软磁材料及其制备方法

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2287467A (en) * 1940-01-03 1942-06-23 American Rolling Mill Co Process of producing silicon steel
US2529373A (en) * 1947-03-25 1950-11-07 American Steel & Wire Co Treating silicon steel
US2599340A (en) * 1948-10-21 1952-06-03 Armco Steel Corp Process of increasing the permeability of oriented silicon steels
US2867557A (en) * 1956-08-02 1959-01-06 Allegheny Ludlum Steel Method of producing silicon steel strip
GB845167A (en) * 1956-12-31 1960-08-17 Gen Electric Improvements in magnetic material
US3021237A (en) * 1958-08-05 1962-02-13 Allegheny Ludlum Steel Processing of metal
US3030203A (en) * 1960-10-10 1962-04-17 Allegheny Ludlum Steel Process of producing steel
US3039902A (en) * 1958-04-15 1962-06-19 Allegheny Ludlum Steel Method of treating steel
US3196054A (en) * 1963-08-14 1965-07-20 Armco Steel Corp Process of decarburizing and annealing of open coil silicon-iron sheet stock without intervening surface treatment

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2287467A (en) * 1940-01-03 1942-06-23 American Rolling Mill Co Process of producing silicon steel
US2529373A (en) * 1947-03-25 1950-11-07 American Steel & Wire Co Treating silicon steel
US2599340A (en) * 1948-10-21 1952-06-03 Armco Steel Corp Process of increasing the permeability of oriented silicon steels
US2867557A (en) * 1956-08-02 1959-01-06 Allegheny Ludlum Steel Method of producing silicon steel strip
GB845167A (en) * 1956-12-31 1960-08-17 Gen Electric Improvements in magnetic material
US3039902A (en) * 1958-04-15 1962-06-19 Allegheny Ludlum Steel Method of treating steel
US3021237A (en) * 1958-08-05 1962-02-13 Allegheny Ludlum Steel Processing of metal
US3030203A (en) * 1960-10-10 1962-04-17 Allegheny Ludlum Steel Process of producing steel
US3196054A (en) * 1963-08-14 1965-07-20 Armco Steel Corp Process of decarburizing and annealing of open coil silicon-iron sheet stock without intervening surface treatment

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3662810A (en) * 1969-09-02 1972-05-16 Howmet Corp Method of internal nucleation of a casting
JPS5431967B1 (cs) * 1971-04-08 1979-10-11
US3915694A (en) * 1972-09-05 1975-10-28 Nippon Kokan Kk Process for desulphurization of molten pig iron
DE2348249A1 (de) * 1972-09-28 1974-04-04 Allegheny Ludlum Ind Inc Kornorientierter siliciumstahl und verfahren zu seiner herstellung
US3955967A (en) * 1973-05-02 1976-05-11 The Algoma Steel Corporation, Limited Treatment of steel
DE2620593A1 (de) * 1975-05-15 1976-11-25 Allegheny Ludlum Ind Inc Verfahren zur herstellung von kornorientiertem siliciumstahl
US4198035A (en) * 1977-10-11 1980-04-15 Voest-Alpine Aktiengesellschaft Blowing lance media-supply arrangement
FR2511045A1 (fr) * 1981-08-05 1983-02-11 Nippon Steel Corp Tole en acier electromagnetique a grain oriente et son procede d'obtention
AU601422B2 (en) * 1986-10-14 1990-09-13 Allegheny Ludlum Corporation Method of making steel
DE102011054004A1 (de) 2011-09-28 2013-03-28 Thyssenkrupp Electrical Steel Gmbh Verfahren zum Herstellen eines kornorientierten, für elektrotechnische Anwendungen bestimmten Elektrobands oder -blechs
WO2013045339A1 (de) 2011-09-28 2013-04-04 Thyssenkrupp Steel Europe Ag Verfahren zum herstellen eines kornorientierten, für elektrotechnische anwendungen bestimmten elektrobands oder -blechs
CN113897558A (zh) * 2021-10-08 2022-01-07 北京北冶功能材料有限公司 一种高饱和磁感高磁导率铁基软磁材料及其制备方法

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DE1458845B2 (de) 1975-09-11
DE1458845A1 (de) 1969-01-09
SE313067B (cs) 1969-08-04

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