US3853641A - Method for producing single-oriented silicon steel sheets having high magnetic induction - Google Patents

Method for producing single-oriented silicon steel sheets having high magnetic induction Download PDF

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US3853641A
US3853641A US00183686A US18368671A US3853641A US 3853641 A US3853641 A US 3853641A US 00183686 A US00183686 A US 00183686A US 18368671 A US18368671 A US 18368671A US 3853641 A US3853641 A US 3853641A
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steel sheet
cold
present
annealing
steel
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A Sakakura
K Ueno
T Yamamoto
S Taguchi
T Wada
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Nippon Steel Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H01F1/14775—Fe-Si based alloys in the form of sheets
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
    • C21D8/1261—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest following hot rolling
    • 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
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
    • C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
    • C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
    • C21D8/1233—Cold rolling

Definitions

  • ABSTRACT Ingot steel for use in producing a single-Oriented silicon steel sheet having a high magnetic induction
  • the ingot steel is hot-rolled to form a steel sheet, the hot-rolled steel sheet is subjected to an annealing for precipitating AlN in a temperature range of 850 to 1,200 C when Si is present in an amount of from 1 to 2.5%, and at a temperature range of 960 to 1,200C when Si is present in an amount of 2.5 to 4%, the annealing being for a time of seconds to 30 minutes.
  • the annealed sheet is coldrolled to obtain a steel sheet Offinal thickness, the cold-rolling being at a reduction rate of to when there is a single cold-rolling step, and when there is a plurality of cold-rolling steps the final coldrolling step is at a reduction rate of 60 to 95%.
  • the final steel sheet has a B value of over 19,100 gauss.
  • This invention relates to ingot steel and a method for producingfrom said ingot steel, single-oriented electromagnetic steel sheets having an. easy magnetization axis l in the rolling direction of the steel sheet.
  • Single-oriented steel sheets are used mostly as iron cores for transformers and other electric devices. Therefore their magnetic characteristics, excitation characteristics and core loss values must be favorable.
  • a steel sheethaving high B characteristics has a muchlower core loss inthe region ofhigh magnetic induction, and-.moreover-the increase in the core loss is at a lower rate, as the magnetic induc? tion rises.
  • the present invention has for its object the supply of products which can meet the requirements as abovementioned. That is, according to the-present'invention it is possible to produce electromagnetic steel sheets which are markedly superior to any conventional single-oriented silicon steel sheets with respect to the magnetic induction B in.the rolling direction, that is, steel sheets which have a magnetic induction above 19,100 gausses, andup to 20,100 gausses.
  • An object of the present invention is to provide a composition of ingot steel suited to the production of single-oriented silicon steel sheets having high magnetic induction.
  • Another object of the present invention is to provide a method for producing from said ingot steel singleoriented silicon steel sheets having high magnetic induction.
  • FIG. l' shows excitation characteristics of a typical product of the present invention and FIG. 2 shows core loss values of the product of the present invention respectively.
  • the present invention relates to a method for producing single-oriented silicon steel sheets having high magnetic induction, in which a normal steel material or silicon steel-material which contains C and Al as indis pensable elements.
  • a small amount of either Se or Te or both and/or S are added to the above-mentioned steel materials according to known steel-making methods, melting methods and casting methods used in normal industrial techniques.
  • the present invention is particularly characterizedin that the final cold-rolling is carried out ata reduction rate of 60 to depending upon the Si content and one of the intermediate annealings after the hot-rolling or between a cold-rolling and a sequential cold-rolling step is carried out in such a temperature range that the y-transformation may occur at least in a part of the steel material. This temperature range is 850 to 1,200C.
  • the said intermediate annealing is called a special intermediate annealing.
  • These steps cause AlN of desirable size to precipitate, so that the magnetic induction in the rolling direction will reach above 19,100 gausses andmaximum of 20,100 gausses.
  • ingot obtained by a continuous casting method which recently came into wide use, can also be used as a material in the present invention.
  • the atmosphere in the case-of casting is usually air but may be'a vacuum or an inert gas as well.
  • the material in the present invention may be made by any steel-making, melting and casting'methods. But the composition of the material must satisfy the following conditions, irrespective of the methods for producing the same, that is, irrespec tive of what steel-making, melting and casting methods are used.
  • the abovementioned composition can contain 0.003 to 0.060% S. It is necessary that C in the above-mentioned material should be present in an amount sufficient to produce a 'y-transformation at least in a part of the steel in response to the Si content. According to our experiences, C in a steel ingot must be at least 0.025% where Si is 3% but may be about 0.005% where Si is In regard to the added elements, the inventors have the following view. Generally, in the production of a single-oriented electromagnetic steel sheet, a selected direction will be obtained since a secondary recrystallization in the ⁇ 1 100 direction occurs in the final annealing. However, in such case, the precipitate produced by the slight amount of added element, plays an important role.
  • Such precipitate may be examplified by nitrides, sulfides and oxides.
  • Such role has been considered to merely finely disperse and precipitate the precipitate so that the normalgrain growth will be inhibited and the secondary recrystallization will be accelerated.
  • the present inventors have discovered that, besides the above-mentioned role of the precipitate, a part'of the precipitate which has been precipitated in strictly regulated direction in coexistence with AlN,
  • Table 1 shows the relationship between the magnetic induction B and the elements S and Se of products obtained by hot-rolling each of 18 silicon steel ingots (made in an electric furnace) containing about 38% Si and about 0.029% Al so as to obtain a hot-rolled sheet of a thickness of 3 mm.
  • Table 2 shows the relationship be Table 2 Al Secondary recrystal grain generation (generating (wt.%) rate in and B Characteristic (at a generating rate of 100%) S no addition It is found from this that, when Se is added, even for an Al content lower than in the case when only S is added, a product having a high B characteristic will be obtained.
  • the object of the present invention cannot be achieved.
  • Table 3 shows the relationship between the magnetic induction B and S and Se of a productobtained by hotrolling each of 17 silicon steel ingots (made with an electric furnace).
  • B values achieved according to the invention are outlined with a heavy line.'The steel contains about 1% Si and, about 0.035% Also as to be 2.0 mm. thick, and after hot-rolling, is continuously annealed in N at l,050C. for 2 minutes, then cold-rolled once at a reduction rate of 82.5% so as to reach a final gauge of a thickness of 0.35 mm., then decarburized (continuously annealing) at 800C. and finally annealed in H at 950C. for 10 hours.
  • Te in a range of 0.007 to 0.200% has the same effect as Se.
  • a product having a B characteristic exceeding 19,100 gausses by having AlN coexist with Te (0.007 to 0.200%), AlN coexist with Se 1 (0.007 to 0.300%) and Te (0.007 to 0.200%), AlN coexist with S (0.003 to 0.060%), Se (0.007 to 0.300%) and Te (0.007 to 0.200%) or AlN coexist with Te (0.007 to 0.200%) and S (0.003 to 0.60%).
  • the precipitate produced by the addition of these elements coexists with AlN and plays a role in inhibiting the normal grain growth and accelerating the secondary recrystallization in the final annealing. Therefore, even in the present invention, in a step before the final annealing such as, for example, in the intermediate annealing or hot-rolling step, or at the time of heating it, or at the time of elevating the temperature in the final annealing, these elements may be made to diffuse into the steel sheet so as to be contained in fixed amounts.
  • C is adjusted so as to be present in an amount below 0.080% so that a -y-transformation will occur in at least a part of the steel sheet due to the Si content while carrying out a special intermediate annealing.
  • less than 1% Si less than 0.080%C is used (a steel ingot of less than 0.085% C).
  • the C in the steel ingot is 0.005% higher than before the steel sheet is important in carrying out the special intermediate annealing.
  • Si ispresent in an amount less than 3.5%.
  • the present invention has an object to improve the B characteristic and B, characteristic. Therefore, the lower limit is not defined. But, as regards the upper limit, if Si is present in an amount greater than 3.5%,. the industrial coldrolling to produce the very high B value becomes impossible. i
  • the basis for generating secondary recrystal grains having a particularly excellent orientation of, the present invention is the formation of AlN. Therefore, in the present invention, the presence of any nitride other than that of Al and the nitride-forming elements must be noted in relation to the formation of AlN. As described above, the presence of the nitride contributes to the secondary recrystallization in the sense of inhibadd nitrogen in theannealing.
  • the method of adding nitrogen is not critical but, in the present invention, it
  • a material which has a composition conforming to the above-mentioned composition is made into product sheet thickness by at least one cold-rolling step.
  • the annealing after the hot-rolling or at least one intermediate annealing between the cold-rollings is carried out in a high temperature range in which a y-transformation will occur in a part of the steel sheet so that a desirable size of AlN may be precipitated.
  • This annealing temperature is in the range of 750 to 1,200C. in which a 'y-transformation will occur in response to the Si content.
  • the annealing be carried out in a neutral or reductive gas containing at least 10% N byvolume.
  • the above-mentioned special intermediate annealing may be carried out at any time during the period after the hot-rolling until the final cold-rolling,' and the time is not critical so long as it is in this period.
  • the cold-rolling is carried out one or more times and the final cold-rolling step may be carried out at a reduction rate of 60 to 95%, depending on the Si content so that the higher the Si content, the higher the reduction rate may be. It is not necessary to have any specific reduction rate in any other cold-rolling step. This can be said to be due to the effect of the coexistence of AlN, Se, Te and S in the material.
  • any other intermediate annealing than the abovementioned special intermediate annealing at a specified high temperature may be carried out at a temperature and for a time which are sufficient to make the coldrolled structure a primary recrystal structure and are not critical.
  • the number of times the cold-rolling step is repeated may be determined by the thickness of the hot-rolled sheet and the specified final cold-rolling reduction rate.
  • the annealing time in this temperature range is 30 seconds to 30 minutes.
  • this annealing exceeds 30 minutes, the growth of crystal grainswill occur during the annealing and the development of the secondary recrystal grains in the final annealing will become imperfect. Further, this annealing may be a box-annealing but generally it is industrially advantageous to carry it out by a continuous annealing. With an annealing for less than 30 seconds, the sought for effect can not be obtained.
  • the annealing atmosphere is related to the precipitation of AlN required for the secondary recrystallization as already described. Usually the steel ingot obtained from an open-hearth furnace contains, without any additions, more than 0.0040% N which is sufficient to precipitate the required AlN.
  • the annealing atmosphere may be a reductive or neutral atmosphere such as, for example, of H Ar, a gaseous mixture thereof or air.
  • a reductive or neutral atmosphere such as, for example, of H Ar, a gaseous mixture thereof or air.
  • the ingot is obtained by vacuum melting or the like, there ,will be so little N that it will .be necessary to to the hot-rolled sheet.
  • the thickness is 3.5
  • the sheet is treated in two cold-rolling steps. F-urther, if the hot-rolled sheet is thicker, it can be coldrolled more than three times. However, from the industrial technical viewpoint, the hot-rolled sheet is usually 1.5 to 7 mm. thick.
  • the steel sheet of a product sheet thickness after the final cold-rolling is then subjected to a decarburi-zing annealing.
  • This annealing is to make the cold-rolled structure a primary recrystal structure and at the same time to remove C which is detrimental when developing secondary recrystal grains in the ⁇ l10 ⁇ l00 direction in the final annealing. Any known process may be used for this step.
  • the final annealing should be carried out at such a temperature and for such a time that secondary recrystal grains in the ⁇ 110 ⁇ direction can develop well. It is preferable to develop the secondary recrystal grains in a temperature range wherein no y-transformation is produced in response to the Si content and at a temperature as high as industrially possible, because the generation of 'y-transformation will change .the once obtained secondary recrystal grains in. the ⁇ l10 ⁇ 100 direction so that they are in another direction.
  • Si is present in an amount less than 1%, it should be carried out at 950C. or usually at a temperature lower than that. However, the higher the Si content, the higher the temperature can be elevated.
  • a product which has an excellent iron loss value can not for the generation of secondary recrystal grains if it is more than 1 hour but more than 5 hours is necessary in order to obtain a product having a low iron loss value with a high Si content.
  • a product having a B characteristic of more than 19,100 gausses according to the present invention can be obtained.
  • it is preferable to carry out the annealing in H it is preferable to carry out the annealing in H
  • the description of such time and atmosphere has nothing to do with the substance of the present invention.
  • the product may be annealed for a long time in H
  • Se, Te or S can be removed by annealing at a temperature of above 1,000C.
  • it may be reduced to an amount less than 0.05%.
  • it is reduced to an amount less than 0.01%, a favorable result can be obtained.
  • EXAMPLE 1 An Al-killed steel ingot containing 0.020% C, 0.041% A1, 0.024% S and 0.010% Se was bloomed and hot-rolled to a hot-rolled sheet 2.2 mm. thick. The content of C in the hot-rolled steel sheet was 0.017%.
  • EXAMPLE 2 A silicon steel ingot (prepared in an electric furnace) containing 0.030% C, 1.05% Si. 0.065% Se and 0.025% Al was bloomed and hotrolled to a'hot-rolled steel sheet 2.0 mm. thick. Afterthis hot-ro1led steel sheet was annealed in N at 950C. for 2 minutes, it was pickled and cold-rolled to make the thickness of the sheet 0.50 mm. (at a reduction rate of 75%).
  • the coldrolled steel sheet was decarburized by an open-coilsystem in a wet H at 750C. for -5 hours and thereupon fi- EXAMPLE 3
  • a silicon steel ingot containing 0.043%C, 2.15% Si, 0.010% S, 0.07% Se and 0.030% Al was bloomed and hot-rolled to a hot-rolled steel sheet 3.0 mm. thick.
  • the C content of the hot-rolled steel sheet was 0.041% and was only slightly decarburized.
  • This hot-rolled steel sheet was first cold-rolled by 30% to make the thickness of the sheet 2.] mm. and then annealed in N at 1,100C. for 2 minutes and thereafter pickled and coldrolled to make the thickness of the sheet 0.35 mm.
  • the thus cold-rolled steel sheet was decarburized in a wet H at 800C. for 3 minutes and then subjected to a final annealing, simultaneously attended with the desulfurization and deseleniumization.
  • the magnetic characteristics in the rolling direction of the product were as shown in FIG. 1(C), that is,
  • EXAMPLE 4 A silicon steel ingot containing 0.055% C, 2.95% Si, 0.025% S, 0.053% Se and 0.025% Al was bloomed and hot-rolled to a hot-rolled steel sheet 2.8 mm. thick. The
  • C content of the hot-rolled steel sheet was 0.051%.
  • The" steel sheet was cold-rolled by 30% and then subjected to a continuous annealing in N at 1-,l50C. for 2 minutes. Then, the cold-rolled steel sheet was pickled and then again cold-rolled to make the thickness of the sheet 0.35 mm. (at a reduction rate of.82.1%). After the cold-rolled steel sheet was then decarburized in a wet H at 800C. for 3 minutes, it was subjected to a final annealing at 1,200C. for 20 hours, simultaneously attended with a desulfurization-and deseleniumization.
  • EXAMPLE 5 A silicon steel ingot containing 0.075% C, 3.09% Si, 0.025% 5,0030% Te and 0.060% Al was bloomed and hot-rolled to a hot-rolled steel sheet 3.2 mm thick. The C content of the hot-rolled steel sheet was 0.071%. The thus obtained hot-rolled steel sheet'was first cold-rolled by 20% to a thickness of 2.56 mm. After the cold-rolled steel sheet was continuo'uslyannealed in N at 1,150C.
  • the prod-' uct had magnetic characteristics in the rolling direction A as shown in FIG. 1(B), that is,
  • composition of the product C was 0.003%, S 0.003% and the sume of Se and Te 0.008%.
  • a process for producing a single-oriented silicon steel sheet having a magnetic induction value above 19,100 gauss consisting essentially of:
  • the silicon steel sheet contains 0.007 to 0.30% Se and 0.007 to 0.20% Te.

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Cited By (13)

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Publication number Priority date Publication date Assignee Title
US3930906A (en) * 1974-02-28 1976-01-06 Kawasaki Steel Corporation Method for forming an insulating glass film on a grain-oriented silicon steel sheet having a high magnetic induction
US3932234A (en) * 1972-10-13 1976-01-13 Kawasaki Steel Corporation Method for manufacturing single-oriented electrical steel sheets comprising antimony and having a high magnetic induction
US3933537A (en) * 1972-11-28 1976-01-20 Kawasaki Steel Corporation Method for producing electrical steel sheets having a very high magnetic induction
US3940299A (en) * 1973-10-31 1976-02-24 Kawasaki Steel Corporation Method for producing single-oriented electrical steel sheets having a high magnetic induction
US4280856A (en) * 1980-01-04 1981-07-28 Kawasaki Steel Corporation Method for producing grain-oriented silicon steel sheets having a very high magnetic induction and a low iron loss
EP0125653A1 (en) * 1983-05-12 1984-11-21 Nippon Steel Corporation Process for producing a grain-oriented electrical steel sheet
US4596614A (en) * 1984-11-02 1986-06-24 Bethlehem Steel Corporation Grain oriented electrical steel and method
US4623407A (en) * 1982-09-24 1986-11-18 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a high magnetic flux density
US4623406A (en) * 1982-09-24 1986-11-18 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a high magnetic flux density
US5393321A (en) * 1991-07-27 1995-02-28 British Steel Plc Method and apparatus for producing strip products by a spray forming technique
US20030062147A1 (en) * 2001-09-13 2003-04-03 Ak Properties, Inc. Method of continuously casting electrical steel strip with controlled spray cooling
EP1006207A4 (en) * 1998-03-11 2005-01-05 Nippon Steel Corp UNIDIRECTIONAL MAGNETIC STEEL PLATE
CN110218853A (zh) * 2019-06-26 2019-09-10 武汉钢铁有限公司 制备低温高磁感取向硅钢的工艺方法

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3932234A (en) * 1972-10-13 1976-01-13 Kawasaki Steel Corporation Method for manufacturing single-oriented electrical steel sheets comprising antimony and having a high magnetic induction
US3933537A (en) * 1972-11-28 1976-01-20 Kawasaki Steel Corporation Method for producing electrical steel sheets having a very high magnetic induction
US3940299A (en) * 1973-10-31 1976-02-24 Kawasaki Steel Corporation Method for producing single-oriented electrical steel sheets having a high magnetic induction
US3930906A (en) * 1974-02-28 1976-01-06 Kawasaki Steel Corporation Method for forming an insulating glass film on a grain-oriented silicon steel sheet having a high magnetic induction
US4280856A (en) * 1980-01-04 1981-07-28 Kawasaki Steel Corporation Method for producing grain-oriented silicon steel sheets having a very high magnetic induction and a low iron loss
US4623406A (en) * 1982-09-24 1986-11-18 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a high magnetic flux density
US4623407A (en) * 1982-09-24 1986-11-18 Nippon Steel Corporation Method for producing a grain-oriented electrical steel sheet having a high magnetic flux density
EP0125653A1 (en) * 1983-05-12 1984-11-21 Nippon Steel Corporation Process for producing a grain-oriented electrical steel sheet
US4596614A (en) * 1984-11-02 1986-06-24 Bethlehem Steel Corporation Grain oriented electrical steel and method
US5393321A (en) * 1991-07-27 1995-02-28 British Steel Plc Method and apparatus for producing strip products by a spray forming technique
EP1006207A4 (en) * 1998-03-11 2005-01-05 Nippon Steel Corp UNIDIRECTIONAL MAGNETIC STEEL PLATE
EP1728885A1 (en) * 1998-03-11 2006-12-06 Nippon Steel Corporation A grain-oriented electrical steel sheet and method for producing the same
US20030062147A1 (en) * 2001-09-13 2003-04-03 Ak Properties, Inc. Method of continuously casting electrical steel strip with controlled spray cooling
US6739384B2 (en) 2001-09-13 2004-05-25 Ak Properties, Inc. Method of continuously casting electrical steel strip with controlled spray cooling
CN110218853A (zh) * 2019-06-26 2019-09-10 武汉钢铁有限公司 制备低温高磁感取向硅钢的工艺方法

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SE355199B (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1973-04-09
GB1266941A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1972-03-15
FR2005396A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1969-12-12
CA920036A (en) 1973-01-30
BE730896A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1969-09-15

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