US3834952A - Method of manufacturing cold-rolled nonoriented electro-6 magnetic steel sheet and product electromagnetic steel sheet - Google Patents

Method of manufacturing cold-rolled nonoriented electro-6 magnetic steel sheet and product electromagnetic steel sheet Download PDF

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US3834952A
US3834952A US00128673A US12867371A US3834952A US 3834952 A US3834952 A US 3834952A US 00128673 A US00128673 A US 00128673A US 12867371 A US12867371 A US 12867371A US 3834952 A US3834952 A US 3834952A
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steel sheet
cold
oxidized layer
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rolled
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O Honjo
I Matsushita
K Tanada
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Nippon Steel Corp
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Nippon Steel Corp
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    • 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

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  • ATTORNEYS I 3,834,952 Patented Sept. 10, 1974 United States PatehtQfice 3,834,952 METHOD OF MANUFACTURING COLD-ROLLED NONORIENTED ELECTRO-6 MAGNETIC STEEL SHEET AND PRODUCT ELECTROMAGNETIC STEEL SHEET Izumi Matsushita, Kiyoshi Tanada, and Osamu Honjo, Himji, Japan, assignors to Nippon Steel Corporation, Tokyo, Japan Filed Mar. 29, 1971, Ser. No. 128,673 Claims priority, application Japan, Mar. 30, 1970, 45/ 26,295 Int. Cl. H011? N04 US. Cl.
  • Electromagnetic steel sheets have been previously called silicon sheets or electric steel sheets and are widely used to form iron cores for electrical machinery and apparatus.
  • electromagnetic steel sheets classified according to the various rolling methods, rolling orientations, configurations and other factors, such as hot-rolled silicon steel sheets, hot-rolled and welded nonoriented silicon steel sheets or strips, cold-rolled nonoriented silicon steel sheets or strips, and cold-rolled oriented, or anisotropic, silicon steel sheets or strips, which materials are all widely known:
  • these electromagnetic steel sheets are required to have various characteristics, among which the magnetic characteristics in particular should be excellent and which sheets are graded in terms of iron loss.
  • the iron loss In order to improve the magnetic characteristics, the iron loss must be reduced. Since the iron loss consists of the hysteresis loss and eddy current loss, it is necessary should possess a preferred orientation suitable for exhibiting magnetic characteristics.
  • the steel sheet in order to effect a decrease in eddy current loss, it is necessary to coat the steel sheet with an electric insulation film so that, when the steel sheet thus coated is used as material for a laminated iron core, the steel sheet components of the core are electrically insulated.
  • the steel sheet must contain alloying elements which heighten the electrical resistance of steel sheet itself, such as silicon (Si) and aluminum (Al), and further the thickness of the steel sheet should be decreased.
  • a cold-rolled nonoriented electromagnetic steel sheet which is a type of electromagnetic steel sheet
  • manufacturing processes have been devised in view of the above described factors as a matter of course so as to achieve the desired magnetic characteristics.
  • a well known fundamental method for producing cold-rolled nonoriented electromagnetic steel sheets employs the so-called one-step cold-rolling method in which hot-rolled coils formed by the rolling of slabs containing not more than 4.0% Si, 0.1 to 3.0% acid soluble aluminum (Sol. Al) and as small a per centage of other impurities as possible are annealed according to the necessity, cold-rolled to the desired sheet thickness and thereafter subjected to bright continuous annealing or box annealing.
  • iron loss values adopted for this grading are specified with regard to the products by the aforesaid conventional methods, so that W10/50 (the iron loss at a magnetic flux density of 10 kg. and a frequency of 50 Hz.) is the proof value while WIS/50 (the iron loss at magnetic flux density of 15 kg. and a frequency of 50 Hz.), that is, the value at a higher field intensity is the reference value.
  • W10/50 the iron loss at a magnetic flux density of 10 kg. and a frequency of 50 Hz.
  • WIS/50 the iron loss at magnetic flux density of 15 kg. and a frequency of 50 Hz.
  • the prior cold-rolled nonoriented electromagnetic steel sheets have drawbacks in that the iron loss increases markedly as the magnetic flux density heightens when the steel sheets are used as materials for iron cores in electrical machinery, especially for rotating machines. More particularly, the relation between magnetic flux "density and iron loss is such that the iron loss is increased with increasing flux density. This phenomenon is especially remarkable when the flux density is above 15 kg. for this reason, it has so far been extremely diflicult to manufacture desirable cold-rolled nonoriented electromagnetic steel sheet suited to form iron cores for rotary electric machinery.
  • SUMMARY OF THE INVENTION object of this invention is to provide cold-rolled nonoriented electromagnetic steel sheets with markedly reduced iron loss during heightened magnetic field intensity, i of thecarbon in electromagnetic steel sheet products, the by improving the conventional methods ef-manufaeturing content being preferably below 0.005%.
  • Another object of the present invention is to provide a' method for manufacturing a cold-rolled'nonoriented electromagnetic steel sheet excellent in characteristics athigh magnetic field intensity by improving'the prior methods for producing cold-rolled nonoriented electromagnetic steel sheets, the improvement being applicable with effortless ease to any of the aforesaid prior basic methods so that the iron loss under a strong magnetic field is markedly lower.
  • FIG. 1 is a schematic sketch of the oxidized layers formed in the surface portion of the steel sheet at. the hot rolling stage of the present invention.
  • FIG. 3 is a photograph illustrating a cross-sectional aspect immediately beneath the surface of a conventional electromagnetic steel sheet.
  • FIGS. 4 and 5 are respectively photographs showing cross-sectional aspect beneath the surface of electromagnetic steel sheets embodying the present invention.
  • FIG. 6 is a graph for comparison of iron'loss curves of an electromagnetic steel sheet having an inner oxidized erally adopted to lower the carbon content in the product electromagnetic steel sheet is to provide a decarburizing annealing stage adequately following the hot-rolling opera tion
  • a decarburizing anneal ing method is the atmosphere decarburizing method in which annealing is effected in the so-called wet atmosphere which is composed of several tens percent hydrogen and the remaining percentage of nitrogen and steam with a dew point of several tens of degrees C.
  • the scale decarburizing method which makes use of the mill scale of hot-rolled coils, or the vacuum decarburizing and refining method applicable to molten steel is now practically employed.
  • the atmosphere is wet air having a strong oxidizing property, so that an outer oxidized layer (0) consisting, as shown in the sketch of FIG. 1 and the photograph of FIG. 2, of Fe O Fe O- FeO, $0, and 2FeOSiO for example, that is, a layer of scale is formed on the hot-rolled coil surface, while an inner oxidized layer (1) containing SiO A1 0 and iron oxides is formed beneath the outer oxidized layer (0) on the surface portion of the base iron.
  • the outer oxidized layer (O), or the scale can be removed by means of such an ordinary pickling solution as a dilute solution of sulfuric acid or hydrochloric acid, whereas the inner oxidized layer (I) cannot be removed with such a solution.
  • the atmosphere for the decarburizing annealing operation after the hot rolling, has a weak oxidizing quality as well as a decarburizing property.
  • the decarburization is accompanied by the formation of the above described inner oxidized layer, as shown in FIG. 3, in the surface portion of the cold-rolled steel sheet which has no outer oxidized layer, that is, no scale layer.
  • the inner oxidized layer formed in this case is usually as thick as several microns to several tens of microns, and cannot be removed by means of an ordinary pickling solution, just as in the aforesaid case.
  • FIG. 2 1s a photograph showing a cross-sectional aspect present inventors have ascertained that the iron loss at high magnetic field intensity can be markedly decreased by removing the above described inner oxidized layer.
  • FIG. 7 is a graph showing the relationship between the thickness of the inner oxidized layer and the iron loss.
  • FIGS. 8 and 9(A) (B) are respectively work process diagrams based on the method of the invention.
  • Another cold-rolled nonoriented electromagnetic steel sheet (B) was manufactured by pickling the same hot-rolled coil having undergone the scale removal and the intermediate annealing, in a pickling solution composed of 6% nitric acid, 1% hydrofluoric acid and the remaining percentage of distilled water, thereby removing the inner oxidized layer, and thereafter carrying out the skin pass rolling to a final thickness of 0.35 mm., and the subsequent final annealing operation with the use of an annealing atmosphere wherein the PH O/PH (the partial pressure of the steam in the atmosphere divided bythat'of the hydrogen therein) was 0.04.
  • the relationship between the magnetic flux density (MF) and iron 1655 (WL) of each of the steel sheets (A) and (B) thus produced is shown in FIG. 6. It will be apparent from FIG. 6 that, with the final product (B) deprived of the inner oxidized layer, the iron loss (WL) is remarkably lowered at high field intensity values.
  • a further illustration of the invention is as follows: A material C (hot-rolled coil) containing 2.1% Si and 0.23% Sol.Al, and a material D (hot-rolled coil) containing 2.9% Si and 0.25% 801. Al, and a material E (hot-rolled coil) containing-3.0% Si and 0.39% Sol. Al werepiokled', thereby being deprived of the respective scale. Thereafter, the materials were cold-rolled to an intermediate sheet thickness and subjected to decarburizing annealing to a carbon content below 0.005% in a wet atmosphere composed of 20% hydrogen and the remaining percentage of nitrogen and steam (with a dew point of 35 C).
  • the three materials thus annealed were deprived of their inner oxidized layers in different amounts by the use of the same pickling solution as in the preceding'example and by changing the pickling time. Then, the materials were subjected to skin pass rolling, which is cold rolling with a low reduction ratio, to a final thickness of 0.35 mm, and thereafter finally annealed in.a:dry atmosphere (the dew point being 5 C.) composed of 20% hydrogen and the remaining percentage .of nitrogen.
  • the thickness of the inner oxidized layer (T(,u)) of each of the three cold-rolled nonoriented electromagnetic steel (C), (D) and (E) thusmanufactured and the iron loss (WL (W17/50) at a high magnetic fiux density (17 kg.) are related as shown in FIG. 7.
  • the iron loss varies according to the material constituents, and the higher the Si content and the S01. Al content, the lower the iron loss, while the iron loss at the high field strength decreases markedly with the reduction in the thickness of the inner oxidized layer.
  • the mechanism by which the inner oxidized layer alfects the iron loss has not yet been clarified in detail.
  • the iron oxides and alumina, silica and othermetal oxides formed in the inner oxidized layer increase thehysteresis loss by the same action as crystal grain domains, impurity inclusions and other similar inner defects, with the result that the iron loss is increased.
  • This effect of the inner oxidized layer is considered to be particularly remarkable with a strong magnetic field where the magnetic flux tends to concentrate at the surface portion of the steel sheet.
  • the iron loss at a high field intensity is markedly lowered by removing the inner oxidized layer
  • the iron layer is lowered at a high frequency, by which the magnetic flux is concentrated at the surface portion of the steel sheet to a larger extent than by high field intensity.
  • the inner oxidized layer existing in the surface portion of cold-rolled nonoriented electromagnetic steel sheet has a great influence upon the iron loss at a high magnetic field intensity, and accordingly the removal of such an inner oxidized layer is the primary feature of the present invention.
  • the pickling prior to the cold rolling of hot-rolled coils is known in the art.
  • the pickling solution is normally a dilute solution of sulfuric or hydrochloric acid.
  • the object of the coventional pickling is to remove the so-called scale composed of iron oxides (Fe O Fe O FeO, Fe SiO thus not to remove the inner oxidized layer, as in the present invention.
  • the inner oxidized layer cannot be removed at all by means of such acid solutions as have been generally applied.
  • conventional acid solutions includes pickling depressors for preventing the dissolution of steel sheet (base iron).
  • a means for removing the base iron For example, a pickling solution capable of positively dissolving the base iron, an electropolishing method, a mechanical removing method employing sand brushing or the like, or any other suitable means is adequately adopted for the said purpose.
  • the oxide films dealt with in this report are, as specified therein, films separable during the production of machines and apparatus with the use of the steel sheet and films which can be easily rubbed off with a piece of polishing paper and can be removed also by means of a pair of tweezers, that is, they are identical with the iron oxide layer (scale) formed during hot rolling, thus being entirely different from the inner oxidized layer to be removed by the present invention.
  • such inner oxidized layer cannot be removed by the use of the dilute sulfuric acid (at a temperature of 60 to C.) having a concentration of about 10% which is introduced in the report, as will be clear from the foregoing description.
  • the inner oxidized layer is not separated even by a high degree of cold rolling.
  • the above cited report does not suggest anything concerning the removal of the inner oxidized layer.
  • the atmosphere in which the heat treatment is carried out after the removal of the inner oxidized layer is an oxidizingatmosphere, such layer will be again produced.
  • the heat treatment after the removal of the inner oxidized layer is carried out in an atmosphere of less than 0.05 in PH O/PH
  • FIG. 8 shows a process diagram for the method of the present invention practised with the one-step cold rolling method.
  • FIG. 9(A), (B) shows a process diagram for the method of the present invention practised with the twostep cold-rolling method.
  • the process (III) is represented by: Hot-rolling step (1)-pickling step (7) (for removing -seale)primary cold-rolling step (8)--intermediate heat-treatment and decarburizing annealing step (9)the inner oxidized layer jrernoval step '(10)-second'ary cold-rolling step (11) skin pass or temper rolling)final heat-treatment step (12) (dry annealing).
  • the processes (IV), '(V) and (VI) are featured by: Hot-rolling step (1) and the hot-rolled coil decarburizing annealing step (2), respectively; and the processes (VII), (VIII) and (IX) are featured by the vacuum degassing step (6) through the vacuum degassing treatment of molten steel and hot-rolling step (1), respectively.
  • Any v of the above-mentioned processes (IV), (V), (VI), (VII), (VIII) and (IX) may be represented as follows: The processes (1V) and (VII) involve the removal of the inner.
  • theme odof the present invention is so constructed that-an inner oxidized layer removal step is provided leaving'atleas-t one set of a cold-rolling and a heat treatmentsteg'mnd a decarburizing step is provided as a step-previoustoz-said inner oxidized layer removal step; and the heatctreat'ment subsequent to said inner oxidized layer removal rstep'ris carried out in an atmosphere incapable ofproducin'g an inner oxidized layer.
  • Si is limited 'to between 1.0;-4.0% according to the present invention.
  • a steel sheet of less than 1.0% Si content is a low-grade product which does not especially require any iron loss(w+att loss) .”in the high magnetic field intensity, therefore, it is -outs ide'th scope of the present invention; and a steel sh'eet of more than 4.0% Si content is very brittle, making-it difficult to subject it to cold-rolling without encounteringdi flicultiesl
  • Sol. Al is limited to 0.-l'+3 0% The reason is that the S01.
  • Al content of less than 0.1% makes ditficult the recrystallization attlie heat-treatment sub'se quent to the cold-rolling, and 801..
  • Al of more-than 3.0% makes the steel sheet brittle, in combination with the -Si content, making it diflicult to subject it to'cold-roilin'g Without encountering ditliculties
  • ⁇ it is desirable to 're'duce the carbon content to less than 0.005% by decarburizationf'
  • the atmosphere -at the heat treat ment subsequent to the removal ofthe inneroxidized layer is limited to less than 0.05 in; PH O/PH FH thej partial pressure ratio is more than 0.05, an inneroxidi'zed layer forms rapidly, making itimposs'ible to achieve the object of the present invention.
  • the reductionbf'iron loss which is one of the objects of the "present invention; can be achieved, even if such removal is not perfectfbut leaves an inner oxidized layer in a thickness of ash s
  • the iron loss is W /50 3.56 watt/kg. after removal (W /50 3.43 watt/kg. after the perfect removal of inner oxidized layer 0 which has been lowered so sufficiently from the iron loss of W 50" 4.09 watt/kg. (thickness of inner oxide layer 4 before removal to nearly meet the purpose of removal.
  • B (the present invention, the process I shown in FIG. 8): After being pickled with a pickling solution consist- 10
  • A (the conventional method): After being reduced to an intermediate sheet of 0.39 mm.
  • Example 2 the two-step cold rolling met od in the method A above, and annealed at 850 C. for 4 fA being Pickled With Pickling Solution consistminutes in a dry atmosphere consisting of 25% hydrogen ing of 2% hy rochloric acid n he r ing r, and the rest being nitrogen (PH O/PH :0.023) in the to m v S 1 ,a- 0 611 Coil f thick, confinal heat treatment step (12).
  • the cross-section of the 'taining carbon- 0.029% by weight, silicon 3.1 by, so-obtained steel sheet is shown microscope-photographweight, Sol.
  • the r 1 3 so-treated sample was reduced to the intermediate sheet After being pickled w th a pickling solution conslstlng f 039 thi k in the primary cold-rolling step (8), 2% hydrochlonc ac1d h the rest e Water to and subjected to intermediate annealing in the dry atmosremove scale, .
  • the smoothness of the steel sheet obtained by the method of the present invention is excellent, therefore, its commercial value and the space factor are high.
  • a cold-rolled non-oriented electromagnetic steel sheet of low iron loss at high magnetic field intensity consisting essentially of Si in'an amount of 1.0-4.0% by weight and acid-soluble Al in an amount of 0.l3.0% by weight, the rest being substantially iron, having an inner oxidized layer of less than 1, in thickness produced by the process of claim 1.
  • a method of manufacturing a cold-rolled, 'non oriented electromagnetic steel'sheet which'ha's' a greatly reduced iron loss when subjected to a high magnetic'fie'ld said steel sheet containing Si in an amount of 1.0-4.0% by weight, acid-soluble .Al in an amount of 0.1-3.0% by weight and the rest being substantially iron, which comprises:

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3932237A (en) * 1973-10-30 1976-01-13 Kawasaki Steel Corporation Method for forming an insulating glass film on surfaces of an oriented silicon steel sheet
US3932236A (en) * 1973-01-22 1976-01-13 Nippon Steel Corporation Method for producing a super low watt loss grain oriented electrical steel sheet
US4046602A (en) * 1976-04-15 1977-09-06 United States Steel Corporation Process for producing nonoriented silicon sheet steel having excellent magnetic properties in the rolling direction
US4210469A (en) * 1974-07-11 1980-07-01 Nippon Steel Corp. Process of annealing for preventing temper colors on a steel sheet
US4548655A (en) * 1982-07-19 1985-10-22 Allegheny Ludlum Steel Corporation Method for producing cube-on-edge oriented silicon steel
EP0422223A1 (en) * 1988-02-03 1991-04-17 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
EP0423331A1 (en) * 1988-02-03 1991-04-24 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
US5482107A (en) * 1994-02-04 1996-01-09 Inland Steel Company Continuously cast electrical steel strip
US10859370B2 (en) * 2015-09-30 2020-12-08 Arcelormittal Method for the fabrication of a steel product comprising a step of characterization of a layer of oxides on a running steel substrate

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2665181B1 (fr) * 1990-07-30 1994-05-27 Ugine Aciers Procede de fabrication de tole d'acier magnetique a grains non orientes et tole obtenue par ce procede.
JPH04163341A (ja) * 1990-10-22 1992-06-08 Takemitsu Kawaguchi モール状浮模様を形成した織物およびその製造法
JP5768327B2 (ja) * 2010-05-14 2015-08-26 新日鐵住金株式会社 高磁場鉄損の優れた無方向性電磁鋼板の製造方法

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3932236A (en) * 1973-01-22 1976-01-13 Nippon Steel Corporation Method for producing a super low watt loss grain oriented electrical steel sheet
US3932237A (en) * 1973-10-30 1976-01-13 Kawasaki Steel Corporation Method for forming an insulating glass film on surfaces of an oriented silicon steel sheet
US4210469A (en) * 1974-07-11 1980-07-01 Nippon Steel Corp. Process of annealing for preventing temper colors on a steel sheet
US4046602A (en) * 1976-04-15 1977-09-06 United States Steel Corporation Process for producing nonoriented silicon sheet steel having excellent magnetic properties in the rolling direction
US4548655A (en) * 1982-07-19 1985-10-22 Allegheny Ludlum Steel Corporation Method for producing cube-on-edge oriented silicon steel
EP0422223A1 (en) * 1988-02-03 1991-04-17 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
EP0423331A1 (en) * 1988-02-03 1991-04-24 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
EP0423331A4 (en) * 1988-02-03 1993-02-24 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
EP0422223A4 (en) * 1988-02-03 1993-02-24 Nkk Corporation Method of manufacturing non-oriented electromagnetic steel plates with excellent magnetic characteristics
US5482107A (en) * 1994-02-04 1996-01-09 Inland Steel Company Continuously cast electrical steel strip
US10859370B2 (en) * 2015-09-30 2020-12-08 Arcelormittal Method for the fabrication of a steel product comprising a step of characterization of a layer of oxides on a running steel substrate

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CA949858A (en) 1974-06-25
FR2087943A5 (ko) 1971-12-31
DE2114949A1 (de) 1971-11-04
SE367652B (ko) 1974-06-04
JPS4819766B1 (ko) 1973-06-15
DE2114949B2 (de) 1973-05-17

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