EP1052043A2 - Silizium-Stahlblech und Verfahren zur Herstellung dieses Bleches - Google Patents

Silizium-Stahlblech und Verfahren zur Herstellung dieses Bleches Download PDF

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Publication number
EP1052043A2
EP1052043A2 EP00109188A EP00109188A EP1052043A2 EP 1052043 A2 EP1052043 A2 EP 1052043A2 EP 00109188 A EP00109188 A EP 00109188A EP 00109188 A EP00109188 A EP 00109188A EP 1052043 A2 EP1052043 A2 EP 1052043A2
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EP
European Patent Office
Prior art keywords
powder
steel plate
rolling
silicon steel
sheet metal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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EP00109188A
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English (en)
French (fr)
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EP1052043A3 (de
Inventor
Tatsuya Pastoral-heim Meitoku Tomioka
Hiroshi Ohmori
Kenji Watanabe
Takao Yabumi
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Daido Steel Co Ltd
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Daido Steel Co Ltd
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Priority claimed from JP11372351A external-priority patent/JP2001026822A/ja
Priority claimed from JP2000035402A external-priority patent/JP2001226751A/ja
Priority claimed from JP2000035435A external-priority patent/JP2001226752A/ja
Application filed by Daido Steel Co Ltd filed Critical Daido Steel Co Ltd
Publication of EP1052043A2 publication Critical patent/EP1052043A2/de
Publication of EP1052043A3 publication Critical patent/EP1052043A3/de
Withdrawn legal-status Critical Current

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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
    • H01F1/14783—Fe-Si based alloys in the form of sheets with insulating coating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • 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
    • C21D8/1227—Warm rolling
    • 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
    • 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
    • C21D8/1238—Flattening; Dressing; Flexing

Definitions

  • This invention relates to a silicon steel plate, which is used for magnetic materials in a shape of plate, strip, hoop, sheet, foil or the like, and excellent in insulation property, corrosion resistance, heat resistance, adhesion, punching quality, magnetostriction property, space factor, alternative magnetic property or so, and further relates to a method of production for such the silicon steel plate.
  • the magnetic steel plate is punched out into core disks with predetermined shapes after strain relieving annealing.
  • the laminated iron core is used, which is made by stacking up predetermined number of the core disks and fixed them together in the stacked state through welding, caulking, adhesion or so.
  • an electrical insulating film is formed in the surface of the magnetic steel plate (strip), and the film of this kind is required to be excellent in the corrosion resistance, adhesion, solvent resistance, heat resistance, seizure resistance, oil resistance, slidability after annealing, punching quality, weldability, space factor, auto-caulkability and so on in addition to the insulation property.
  • the insulating film of the magnetic steel plate (strip) of this kind films of inorganic type, organic type, inorganic-organic mixed type and so have been used, generally the inorganic films have a tendency to be excellent in the slidability after annealing, but not excellent in the punching quality as compared with the organic and the mixed types, and the organic films are excellent in the punching quality and the adhesion.
  • high silicon steel plates containing Si of 2.0 to 4.0 wt% are used as soft magnetic materials for iron cores of transformers or electric motors.
  • the core loss in the high-silicon steel plate can be considered by dividing into direct current core loss and eddy-current loss, and the eddy-current loss is energy loss according to Joule heat caused by induction.
  • the eddy current becomes larger in proportion to changing speed of magnetic flux density with passage of time, therefore, becomes larger with increase of frequency of the alternative current.
  • the reduction of eddy current has been tried by decreasing thickness of the steel plate, by forming a film with different thermal expansion coefficient on a surface of the steel plate in order to give tension on the surface of the steel plate, by refining crystal grains in order to decrease width of magnetic domain and so on in addition to increase of Si content so as to increase the electric resistance.
  • Grain oriented magnetic steels are steels of which ⁇ 1 0 0 ⁇ orientation of the crystal grain, that is the axis of easy magnetization is directed to a magnetizing direction.
  • the steel of which grains directed to (110) ⁇ 001 ⁇ orientation (the so-called "Goss orientation") are arranged uniformly in the rolling direction of the steel plate is called as an unidirectional grain oriented magnetic steel plate, and manufactured by using secondary recrystallization.
  • the unidirectional grain oriented magnetic steel plate of which Goss orientation is developed is magnetized mainly by movement of 180°-magnetic wall, thereby improving the soft magnetic properties of the steel plate.
  • sticking layers consisting of oxides, chlorides and sulphides of Sn and/or B on linear regions arranged plurally in the direction substantially perpendicular to the rolling direction of the steel plate after cold rolling in Japanese Patent Application First Publication No.6-65644/94.
  • Japanese Patent Application First Publication No.6-100997/94 which consists of forming grooves with maximum depth of 2 ⁇ 50 ⁇ m in average with spaces in the surface of the steel plate after the primary recrystallization annealing and subjecting the steel to final annealing after coating annealing separation agent.
  • the high-silicon steel plates containing Si of 6.5 % are well known as magnetic materials further suitable for the iron core of the transformer.
  • a silicon steel plate which contains Si of 11.5 % as the upper limit value.
  • Si 11.5 %
  • workability of alloys becomes lower according to increase of Si content and cold rolling becomes very difficult if the Si content exceeds 4.5 %.
  • This invention is made in order to solve the aforementioned problems of the non-oriented magnetic steel plate in the prior art, for the purpose of providing a silicon steel plate excellent in punching quality and adhesion of the insulating films, a high-silicon steel plate excellent in the magnetic properties, and providing a method possible to easily produce such the silicon steel plate with high Si content.
  • the silicon steel plate according to this invention is characterized by being made from metal powder through powder rolling and coated with an insulating film on a surface thereof, preferably after sintering.
  • the silicon steel plate according to another embodiment of this invention is characterized by being made from metal powder through powder rolling and diffusion annealing, and roughness caused by metal powder in a surface of the steel plate is controlled through cold rolling and so.
  • the production method of the silicon steel plate according to this invention is characterized by coating the insulating film on a surface of a sheet metal obtained by powder-rolling the metal powder containing Si, preferably after subjecting the sheet metal to diffusion sintering prior to the coating of the insulating film.
  • the production method of the silicon steel plate according to the other embodiment of this invention is characterized by comprising the steps of powder-rolling the metal powder containing Si into a sheet metal; subjecting the obtained sheet metal to diffusion annealing, and controlling roughness caused by the metal powder in a surface of the sheet metal through cold rolling and so.
  • the silicon steel plate according to this invention is coated with an insulating film on the surface of a sheet metal obtained by powder-rolling metal powder containing Si, or the surface of a sheet metal further subjected to diffusion sintering after the powder rolling of the metal powder.
  • magnetic steel powder such as Fe-3wt% Si, Fe-4.5wt% Si, Fe-6.5wt% Si, Fe-Si series alloying composition and the like
  • metal powder such as Fe-3wt% Si, Fe-4.5wt% Si, Fe-6.5wt% Si, Fe-Si series alloying composition and the like
  • pre-mixed powder obtained by mixing powders in advance so as to accord with the chemical compositions of the magnetic steel pre-alloy powder partially alloyed in advance and having the chemical compositions of the magnetic steel and the like may be used. It is possible to sufficiently utilize characteristics of iron powder excellent in moldability by using a powder mixture of the iron powder and Fe-Si alloy powder containing Si of 8 to 65 wt%.
  • inorganic matter is used, such as slurry-like material containing MgO, SiO 2 , Al 2 O 3 , ZrO 2 , SnO 2 , TiO 2 , CrO 3 , B 2 O 3 , Mg 2 SiO 4 or the like, phosphoric acid and phosphates, chromic acid and chromates, boracic acid and borates or so.
  • Organic matter is also used, such as acrilic resins, alkyd resins, phenol resins, epoxy resins, melamine resins, silicone resins, amino resins, styrene resins, ethylene resins, polyvinyl chloride resins, polyvinyle acetate resins, isocyanate resins, polyester, polyamido, polystyrene, polypropylene, polycarbonate, polyurethane, or so.
  • acrilic resins alkyd resins, phenol resins, epoxy resins, melamine resins, silicone resins, amino resins, styrene resins, ethylene resins, polyvinyl chloride resins, polyvinyle acetate resins, isocyanate resins, polyester, polyamido, polystyrene, polypropylene, polycarbonate, polyurethane, or so.
  • a pitch of the roughness may be controlled by selecting particle size of the metal powder.
  • the depth of the roughness may be controlled by selecting the reduction ratio at the time of powder rolling or selecting the sintering temperature at the time of diffusion sintering (diffusion annealing) of the sheet metal.
  • the sheet metal obtained through the powder rolling may be subjected to cold rolling, warm rolling at a temperature lower than recrystallization temperature, or hot rolling after the sintering, and the depth of the roughness caused on the surface of the sheet metal owing to use of the metal powder may be controlled by selecting the reduction ratio at the time of the rolling.
  • the insulating film is formed on the surface of the sheet metal after forming by the powder rolling, after subjecting the sheet metal to the diffusion sintering or after further subjecting the sintered sheet metal to rolling such as the cold rolling.
  • the insulating film can be formed in a single layer or double layers by selecting among the aforementioned various substances.
  • the insulating film is not limited only in the single layer and it is possible to form, for example, Mg-Si complex oxide, such as forsterite (Mg 2 SiO 4 ) on the powder-rolled Fe-3% Si magnetic steel sheet as a lower layer, and further form Cr-oxide and epoxy resin on the phorstelite layer as an upper layer.
  • Mg-Si complex oxide such as forsterite (Mg 2 SiO 4 )
  • the forming method of the insulating film is not limited in the specific method in this invention.
  • a brushing method, a spraying method, a dipping method and the like are available.
  • the thickness of the insulating film is suitable to be 0.5 to 5 ⁇ m or so, and the applicating amount of the insulating film is suitable to be 0.5 to 3.0 g/m 2 or so, however it is disirable to select the thickness and the applicating amount in accordance with the coating method, the type of the film, the number of the coating layer and so on.
  • the roughness is formed on the surface of the powder-rolled sheet metal, powder-rolled and sintered sheet metal or further cold-rolled sheet metal because the metal powder is used, accordingly the adhesion of the insulating film on the surface of the silicon steel plate (sheet metal) becomes excellent remarkably.
  • the insulating property becomes satisfactory by forming the insulating film, the slidability after annealing and the punching quality are also improved.
  • the corrosion resistance, oil resistance, solvent resistance, rusting resistance and so are further improved, and the magnetostriction is reduced by the tension caused by the insulating film.
  • the magnetic steel powder of Fe-6.5wt% Si steel is used as the metal powder, it is not necessary to cope with the magnetostriction by cancelling the tension with the insulating film since the magnetostriction of the magnetic steel containing Si of 6.5 wt% is zero, so that the high-tension film becomes unnecessary to be formed.
  • the silicon steel plate according to another embodiment of this invention which is made from the metal powder through powder rolling and diffusion annealing, and of which roughness caused by the metal powder in the surface thereof is controlled through cold rolling and so, roops of magnetic flux is formed between pitches of the roughness parts caused by the metal powder as the material, so that magnetic domain is fractionated sufficiently and suitably, the eddy-current loss becomes lower and the silicon steel plate improved in the alternative magnetic properties is provided.
  • the Si content is preferable to be 5 to 12 wt%. Namely, in the case where the Si content of the silicon steel is less than 5 wt%, the steel is possible to be produced through the conventional rolling process using the ordinary ingot steel and there is not so many merits obtained by introducing the powder rolling process for the production of the steel, so that it is not desirable to apply the powder rolling in the production of the steel containing Si less than 5 wt%. Meanwhile, the Si content in the steel is not desirable to exceed 12 wt% because electric resistance of the steel becomes lower in addition of decrease of the suturated magnetism and the high-frequency property is remarkably degraded.
  • powder of Fe-5 to 12 wt% Si alloy may be use, besides mixed powder may be also used, which is a mixture of iron powder excellent in the moldability and Fe-Si alloy powder containing Si of 8 to 65 wt% and mixed in a ratio so as to obtain the powder-rolled silicon steel plate with Si content of 5 to 12 wt% after the diffusion annealing.
  • Such the iron powder with the desirable Si content and the high-silicon steel powder are manufactured by the reduction method, the pulverization method, the water atomizing method, the mist atomizing method or the like, and used after adjusting the particular size appropriately.
  • the pre-mixed powder obtained by mixing in advance, the pre-alloy powder alloyed in advance or the like may be used, and it is suitable to use the fine and irregular shaped metal powder with particle size of under 100 mesh.
  • the iron powder and the high-silicon steel powder are subjected to the powder rolling and further subjected to the diffusion annealing in a non-oxidative atmosphere, thereby obtaining annealed plate (solid) from the high-silicon steel powder.
  • the pitch of the roughness on the surface may be controlled by regulating the particle size of the metal powder.
  • the depth of the roughness on the surface of the sheet metal also may be controlled by regulating annealing temperature at the time of the diffusion annealing.
  • the depth of the roughness can be controlled by regulation of reduction ratio at the time of the cold rolling.
  • the rolling has also the advantage in that it is possible to improve the space factor of the silicon steel plates piled up so as to be used for the iron core or so as compared with the case in which the rolling is not performed.
  • the method for producing the silicon steel plate according to the other embodiment of this invention although the powder rolling of the metal powder, the diffusion annealing of the powder-rolled sheet metal, the rolling and so are carried out, the method may be divided into a basic form and a simplified form.
  • the basic method for producing the silicon steel plate according to this invention comprises, as shown in FIG.1, the processes of [A] powder mixing process, [B] powder rolling process, [C] sintering process, [D] cold rolling process, [E] diffusion annealing process and [F] finish rolling process.
  • the simplified method for producing the silicon steel plate according to this invention comprises, as shown in FIG.2, the processes of [A] powder mixing process, [B] powder rolling process, [E'] diffusion annealing process and [F] finish rolling process.
  • the following process [G] may be performed successively after the finish rolling process [F];
  • FIG.3 The flow diagram in the case of adding the flattening treatment process [G] to the basic method shown in FIG.1 is shown in FIG.3, and the flow diagram in the case of adding the flattening treatment process [G] to the simplified method shown in FIG.2 is shown in FIG.4.
  • any one of the following processes [H] and [I] may be carried out at least one time in advance of the diffusion annealing process [E] or [E'], especially in a case where the thin plate is intended to be obtained with high dimensional accuracy;
  • FIG.6 The flow diagram of the modified method in which annealing and cold rolling [H] is performed in addition to the simplified method shown in FIG.2 is shown in FIG.6.
  • iron powder used for powder material it is suitable to use the so-called reduced iron powder and atomized iron powder.
  • the iron powder manufactured from iron carbonyl compounds is not suitable because it has excessively fine grain size and nearly spherical shape, and poor in the moldability in addition to its high price.
  • Fe-Si alloy powder it is suitable to use powder manufactured by spraying water against the molten alloy.
  • the particle size of these iron and Fe-Si alloy powders it is suitable to use the powder comprising fine and irregular shaped particles possible to pass 100 mesh or so.
  • Two kinds of material powders to be mixed are desirable in the average and distribution of the particle size. If they are different remarkably from each other, there is the possibility that the two kinds of powders separates from each other during the handling of the mixed powder.
  • the diffusion annealing of the powder-rolled metal is carried out in the non-oxidative atmosphere, such as an atmosphere of argon, nitrogen, hydrogen or so, or in vacuum.
  • the non-oxidative atmosphere such as an atmosphere of argon, nitrogen, hydrogen or so, or in vacuum.
  • the sintering of the sheet metal formed by the powder rolling enables the product to be obtained as a result of the succeeding cold rolling to exhibits strength at the same time of maintaining the workability as the mixture.
  • the cold rolling is carried out in order to realize desired thickness and increase the bulk density of the sintered body by smashing holes in the sintered body and giving internal strain energy, whereby it is possible to mitigate the condition in the diffusion annealing of the next process.
  • "cold rolling” means the rolling in the temperature range at which recrystallization is never caused.
  • the cold-rolled sheet having an increased density in this manner is uniformed in the composition and promoted to be compacted by the diffusion annealing, thereby exhibiting intended magnetic properties.
  • the obtained sheet metal is rolled into the predetermined thickness by the finish rolling.
  • the skin pass rolling for finish has merits of not only improvement of accuracy in the thickness of the silicon steel plate to be obtained, but also improvement of flexibility of the product.
  • the improvement of the flexibility is an unexpected profit, the advancement of the workability improves the punching quality and enables to manufacture the product with complicated or minute shape.
  • the simplified method is a production method for proceeding microstructual uniformization of the alloying compositions by diffusion, revelation of strength of the sheet metal material and improvement of the magnetic properties at the same time according to the diffusion annealing by heating at a large sinter parameter than that of the sintering process.
  • Si content of the Fe-Si alloy powder to be mixed with the iron powder can be selected from the wide range of 8 to 65 wt%, excessive or too little content of Si is not suitable.
  • alloy powder containing Si of less than 8 % is not suitable for manufacturing 6.5 % Si steel, especially in a case of manufacturing thin plate of the steel because the oxygen content which is harmful to the magnetic properties is apt to become higher and the amount of iron powder required for adjusting the compositions of the steel is decreased extremely, thereby degrading the moldability of the powder mixture.
  • alloy powder containing too much Si is also not suitable since the blending ratio of the Fe-Si alloy powder against the iron powder becomes lower and it is difficult to obtain uniformity of the powder mixture.
  • This invention has a meaning in producing the silicon steel plate containing high Si content, that is Si content higher than 5 % which is difficult to realize through the conventional technique, and Fe-Si alloy is required to contain Si more than certain limitation value, however too much content of Si is also disadvantageous in consideration of the present situation that the upper limit of Si to be contained Fe-Si alloy steel as the magnetic materials is 11 to 12 % in practical application.
  • Concerning the blending ratio of the iron powder and the Fe-Si alloy powder unbalanced combination such as the ratio 95:5 or above by weight is not desirable from a view point of ensuring the uniformity of the mixture, and it is preferable to select the ratio 90:10 and further preferable to select the ratio close to the ratio 50:50.
  • Fe-Si alloy powder of which Si content is more than 10 % and does not exceed 30 % so remarkably can be used easily in general.
  • a eutectic point (Fe 3 Si, melting point : 1200 °C) at a point of 18 % Si in the Fe-Si alloy series, accordingly, it is advisable to use powder of the above-mentioned eutectic alloy.
  • the former is rather advantageous. Especially in a case of obtaining the thin plate, it is recommended to use the iron powder in the large quantity in order to ensure the moldability. It is facilitated to realize the uniform alloying compositions by using the powder mixture of which deviation of the microscopic compositions is smaller, that is the later combination of the powders. In addition to the above, it is necessary to regard the value of Si content of the silicon steel plate to be manufactured as important, and the concrete combination of the chemical compositions should be decided by considering these various factors synthetically.
  • the sintering process is a process for the purpose of obtaining sintered body of which holes is easy to be smashed in the succeeding cold rolling process without promoting diffusion so much.
  • the sintering does not proceed in the practical speed at a temperature lower than 950 °C of the lower limit of the sintering temperature range, and the upper limit of 1400 °C is set because the alloy powder is molten at a temperature higher than 1400 °C.
  • This sintering process should be executed under conditions that areal percentage of the part of which Si content is 5.5 % or below is in a range of 30 to 80 % in order to ensure the workability at the proceeding process as mentioned above.
  • "The part of which Si content is 5.5 % or below” is, of course, a part holding the workability, therefore if the sintering is advanced until the areal percentage of this part becomes lower than 30 %, the workability is remarkably degraded in the successive process.
  • EPMA Electro Probe Micro-Analyzer
  • value of the sinter parameter P 1 for setting the areal percentage A 1 of "the part of which Si content is 5.5 % or below" in the aforementioned optimum range of 30 to 80 % is in a range of (230 ⁇ 310) ⁇ 10 2 , and sintering conditions corresponding to such the sinter parameter value are 950 °C ⁇ 30 min and 1350 °C ⁇ 10 min, respectively. Therefore, it is possible to select the actual operating condition as combination of the temperature and time within the aforementioned range.
  • Especially desirable value of sinter parameter P 1 is within a range of (270 ⁇ 280) ⁇ 10 2 approximately as is apparent from FIG.7.
  • the diffusion annealing is a process for contriving to uniformize the compositions by diffusion of Si and directing the increase of the density, therefore it is necessary to heat at a high temperature of 1150 °C or more.
  • the diffusion proceeds in some degree even in a temperature lower than above, it is not possible to expect the increase of the density and the magnetic properties of the steel plate product is not improved, the effect on the improvement of the magnetic properties becomes higher according as the heating temperature is raised, but is saturated in the region of 1350 °C.
  • the alloy is molten at a temperature higher than 1400 °C.
  • the diffusion annealing can be performed either in the batch furnace or the continuous furnace, however it is necessary to apply the anti-seizure agents such as almina for fear that seizure may be caused in the works overlapping one another in a case of using the batch furnace.
  • value of the sinter parameter P 2 for setting the areal percentage A 2 of "the part of which Si content is 6 to 7 %" in the optimum range of 50 % or more is in a range of (170 ⁇ 200) ⁇ 10 2
  • sintering conditions corresponding to such the parameter value are 1200 °C ⁇ 30 min (or 1150 °C ⁇ 60 min) and 1350 °C ⁇ 120 min, respectively.
  • the actual operating condition may be selected from the combination of the temperature and time within the aforementioned range.
  • Desirable value of sinter parameter P 2 is especially in a range of (180 ⁇ 200) ⁇ 10 2 approximately as is apparent from FIG.8.
  • the annealing process is an operation for facilitating the following cold rolling by relieving the strain caused by rolling, and it is not possible to improve the strength of the product in this process.
  • the relieving of work-strain does not proceed at a temperature lower than 600 °C, however even if the annealing temperature is raised at 950 °C or above, further improvement of the workability can not be expected any longer and the energy is merely dissipated wastefully.
  • the silicon steel plates were made by using two kinds of metal powder as raw materials, and the two kinds of powder mixtures of Fe-3.5wt% Si powder and Fe-6.5wt% Si powder were prepared.
  • the metal powder was charged into the hopper from the upper part, and powder-rolled sheet metal was formed by subjecting the metal powder supplied successively from the bottom part of the hopper to the powder rolling, and then the powder-rolled sheet metal was subjected to primary sintering at a temperature of 700 °C, subsequently subjected to secondary sintering at a temperature of 1300 °C. Consequently, four kinds of powder-rolled sheet metal having thickness of 0.1 mm and respective surface roughness as shown in Table 1 were obtained by further performing cold rolling, warm rolling and hot rolling in combination.
  • the adhesion was indicated with the minimum diameter of bent portion at the time when the outer insulating film does not separate from the steel plate by peeling test using the adhesive tape even by bending the silicon steel plate with the insulating film at an angle of 180°.
  • the corrosion resistance was evaluated with percentage of rusting area after leaving the silicon steel plate with the insulating film in an atmosphere of 40 °C - 80 °C RHD for 100 hrs.
  • the punching quality was indicated with the number of punchings at the time when the height of burr comes up to 50 ⁇ m at clearance of 5 % using the steel die of SKD-1 (alloy tool steel containing Cr). The test was discontinued at 2 million times which are the practical life time.
  • the high-silicon steel having chemical compositions shown in Table 4 were molten, and then the high-silicon steel powder having particle size distribution as shown in Table 5 were obtained by water aotmizing method.
  • C Si Mn P S Sol.Al N Fe 0.008 11.76 0.08 0.020 0.025 0.025 0.009 Bal . -350 +350/-200 +200/-150 +150/-100 +100/-50 51.7 37.0 11.2 0.1 0
  • a powder preparation with composition of Fe-6.5wt% Si was obtained by mixing the above-mentioned high-silicon steel powder and iron powder, and the powder preparation was powder-rolled into sheet metal of 0.11 mm in thickness, successively the powder-rolled sheet metal was subjected to diffusion annealing at at temperature of 1300 °C as shown in Table 6.
  • iron powder and Fe-18% Si alloy powder were manufactured by water atomizing method, and powders passed through a 100 mesh seive were collected. The respective powders were confirmed that average particle size was 40 ⁇ m, approximately. These powders were mixed in the ratio 60:34 by the tumbler so that Si content in the mixture may be 6.5 wt%.
  • Nine kinds of silicon steel plates were manufactured by treating the powder mixture in the following various processes.
  • the horizontal rolling mill provided with two rolls of 200 mm diameter and 240 mm in length was used, the powder mixture was supplied to the rolling mill through the vibrator plate and the powder rolling was performed at constant pressure of 70 ton in kiss roll method.
  • the diffusion annealing is executed by using the batch furnace or the continuous furnace, and the tension annealing was carried out in the condition of 750 °C ⁇ 2 min and the tension of 3 kg/mm 2 except for special mention of the condition.
  • the finish rolling (skin pass rolling) was carried out in the reduction ratio of 0.5 to 5 %.
  • the thickness of the silicon steel plate can be accurately controlled by subjecting to the skin pass rolling in the finish rolling process.
  • the skin pass rolling improves flexibility and workability of the silicon steel and facilitates the punching of the steel plate, and it is favourable to manufacture the iron core of the transformer as main usage of the silicon steel plate. FUrthermore, it is confirmed that the silicon steel plate subjected to the tension annealing exhibits the high flatness.

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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)
EP00109188A 1999-05-10 2000-05-09 Silizium-Stahlblech und Verfahren zur Herstellung dieses Bleches Withdrawn EP1052043A3 (de)

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JP12925099 1999-05-10
JP12925099 1999-05-10
JP11372351A JP2001026822A (ja) 1999-05-10 1999-12-28 珪素鋼板とその製造方法
JP37235199 1999-12-28
JP2000035402A JP2001226751A (ja) 2000-02-14 2000-02-14 交流磁気特性が改善された高珪素鋼板およびその製造方法
JP2000035435 2000-02-14
JP2000035435A JP2001226752A (ja) 2000-02-14 2000-02-14 絶縁性等に優れた粉末圧延帯およびその製造方法
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US7435304B2 (en) 2002-11-11 2008-10-14 Posco Coating composition, and method for manufacturing high silicon electrical steel sheet using thereof
KR100946070B1 (ko) * 2002-11-27 2010-03-10 주식회사 포스코 고규소 전기강판 제조방법
KR101103449B1 (ko) * 2009-11-19 2012-01-09 현대하이스코 주식회사 고효율 무방향성 전기 강판 제조 방법
CN103014613A (zh) * 2012-12-31 2013-04-03 上海大学 热扩散连续制备高硅钢片的方法及其高硅钢片连轧装置
US20130298730A1 (en) * 2011-02-22 2013-11-14 Diamet Corporation Composite soft magnetic material having low magnetic strain and high magnetic flux density, method for producing same, and electromagnetic circuit component
CN103817331A (zh) * 2014-02-27 2014-05-28 华南理工大学 通过滚压实现粉末冶金烧结材料表面致密化的装置及方法

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CN107626927A (zh) * 2016-07-18 2018-01-26 鞍钢股份有限公司 一种高硅复合电工钢窄带产品的制造方法

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7435304B2 (en) 2002-11-11 2008-10-14 Posco Coating composition, and method for manufacturing high silicon electrical steel sheet using thereof
KR100946070B1 (ko) * 2002-11-27 2010-03-10 주식회사 포스코 고규소 전기강판 제조방법
KR101103449B1 (ko) * 2009-11-19 2012-01-09 현대하이스코 주식회사 고효율 무방향성 전기 강판 제조 방법
US20130298730A1 (en) * 2011-02-22 2013-11-14 Diamet Corporation Composite soft magnetic material having low magnetic strain and high magnetic flux density, method for producing same, and electromagnetic circuit component
US9773597B2 (en) * 2011-02-22 2017-09-26 Mitsubishi Materials Corporation Composite soft magnetic material having low magnetic strain and high magnetic flux density, method for producing same, and electromagnetic circuit component
CN103014613A (zh) * 2012-12-31 2013-04-03 上海大学 热扩散连续制备高硅钢片的方法及其高硅钢片连轧装置
CN103817331A (zh) * 2014-02-27 2014-05-28 华南理工大学 通过滚压实现粉末冶金烧结材料表面致密化的装置及方法
CN103817331B (zh) * 2014-02-27 2016-09-21 华南理工大学 通过滚压实现粉末冶金烧结材料表面致密化的装置及方法

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