EP2644715B1 - Herstellungsverfahren für einen kornorientierten siliziumstahl mit hoher magnetkraft - Google Patents
Herstellungsverfahren für einen kornorientierten siliziumstahl mit hoher magnetkraft Download PDFInfo
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- EP2644715B1 EP2644715B1 EP11842864.8A EP11842864A EP2644715B1 EP 2644715 B1 EP2644715 B1 EP 2644715B1 EP 11842864 A EP11842864 A EP 11842864A EP 2644715 B1 EP2644715 B1 EP 2644715B1
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- Prior art keywords
- steel
- martensite
- annealing
- strip
- magnetic performance
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/48—Tension control; Compression control
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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
- 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
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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
- 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
- C21D8/1272—Final recrystallisation annealing
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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
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
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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
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1283—Application of a separating or insulating coating
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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
- C21D2201/00—Treatment for obtaining particular effects
- C21D2201/05—Grain orientation
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/008—Martensite
Definitions
- the present invention relates to a method for manufacturing a grain-oriented silicon steel, especially to a method for manufacturing a grain-oriented silicon steel with excellent magnetic performance.
- Oriented silicon steel is an indispensable and important soft magnetic alloy in electric, electronic and military industries, which is mainly utilized for the iron core for transformer, as well as the electric generator and large electric machine and like. It is desired that the grain-oriented silicon steel has excellent magnetic performance, especially degradation of iron loss.
- Oriented silicon steel may have excellent magnetic performance in a rolling direction by utilizing a secondary re-crystallizing technology, making Goss texture (Goss texture: ⁇ 110 ⁇ means that crystal face is parallel to rolling plane, ⁇ 001> means that crystal direction is parallel to rolling direction) to undergo an abnormal grain growth so as to merge grains in other orientations.
- Goss texture ⁇ 110 ⁇ means that crystal face is parallel to rolling plane, ⁇ 001> means that crystal direction is parallel to rolling direction
- a traditional method for manufacturing a grain-oriented silicon steel having high magnetic induction is as follows.
- a steel blank is heated to a temperature of 1350°C to 1400°C in a special high temperature heating furnace, then the temperature is maintained for more than 1h, so as to facilitate the sufficient solid solution of impurities of AlN, MnS or MnSe, and then the steel blank is rolled, the roll-finishing temperature is over 950 °C, the hot-rolled steel strip is coiled after being rapidly splashed and cooled with water.
- fine and diffusive second phase particles namely, a grain growth inhibitor
- pickling is carried out to the hot-rolled steel after normalization to remove a ferric oxide skin from its surface.
- the steel sheet After being further cold rolled to a thickness of a final product, the steel sheet is subjected to decarburizing and annealing process to reduce [C] content in steel sheet to the extent that will not affect the magnetic property of the final product ( ⁇ 30ppm), and then an annealing separator, whose main composition is MgO, is coated on the steel sheet to carry out high temperature annealing, and the steel sheet is subjected to a secondary recrystallization to form an under coating of Mg 2 SiO 4 as well as purify the steel, and finally, the steel sheet is coated with an insulation coating, stretched and annealed, and thus the product of the grain-oriented silicon steel with high performance that has high magnetic induction, low iron loss and good insulation is obtained.
- an annealing separator whose main composition is MgO
- Some steel mills such as Russian Novolipetsk Iron & Steel Corporation (NLMK), and VIZ etc., utilize an intermediate temperature oriented silicon steel manufacturing technology, the steel-blank-heating temperature is 1200 - 1300°C, chemical composition contains a relatively high content of Cu (0.4% - 0.7%), while AlN and CuS are used as inhibitors.
- This method can avoid several problems due to heat steel blank in high temperature, the disadvantage is that only general oriented silicon steels can be manufactured.
- the steel-blank-heating temperature can be reduced to be lower than 1250 °C, and the method can be utilize to produce not only general oriented silicon steel but also oriented silicon steel with high magnetic.
- the grain-oriented silicon steel can be manufactured by utilizing difference between travel speeds of high energy grain boundary and other grain boundaries.
- M. Barisoni et al. propose that steel sheet is cooled to 800 ⁇ 850 °C at a speed of 20°C/s after being normalized, then the steel sheet is quenched at a cooling speed of 100°C/s, so as to form dispersed martensite phase whose volumetric percentage is about 8%, and hardness H v ⁇ 600 (the hardness of steel plate matrix H v ⁇ 230), as well as to segregate out a great amount of AlN of about 10nm.Martensite is formed to make stored energy increased, and accordingly the stored energy after cold rolling is increased, while the stored energy will make ⁇ 110 ⁇ grain to recrystallize and grow more easily in decarburizing and annealing process, and ⁇ 110 ⁇ composition after subjected to decarburizing and annealing is strengthened, and thus the magnetic performance of the final product is improved.
- Martensite phase transition can be induced by rapidly cooling (quenching), which is named as thermally induced martensite phase transition. Also, Martensite phase transition can be induced due to stress or strain, which is named as stress or strain induced martensite phase transition.
- the driving force of martensite phase transition is composed of two parts, i.e., a chemical driving force and a mechanical driving force.
- the temperature of martensite phase transition decreases.
- Curie temperature 770°C
- the grain-oriented silicon steel presents spontaneous ferromagnetic elongation, which can partly counteract automatic contraction in volume when cooling, so as to increase the decrease of the temperature of martensite phase transition.
- Martensite phase transition goes through two phases of nucleation and growth.
- nucleation rate of martensite is greatly increased, whose extent may reach tens of order of magnitude to hundreds of order of magnitude.stored energy does not greatly influence the growing speed of crystal nucleus of martensite.
- water is utilized to control a cooling speed from 700 ⁇ 900°C to the room temperature
- the control is likely to be limited by site conditions, for example air temperature, damage or obstruction of nozzle , which may render cooling speed unstable; and secondly, the temperature of steel sheets cannot be accurately measured due to artificial factors, it is difficult to achieve an accurate control, and accordingly it is difficult to achieve a fine tuning of cooling speed.
- An alternative manufacturing method for oriented silicon steel sheets is disclosed in CN1743127A .
- the object of the present invention is to provide a method for manufacturing a grain-oriented silicon steel with excellent magnetic performance, in which the content of martensite in steel plate and distribution thereof after normalizing can be optimized by adjusting the stress in the steel sheet in normalizing phase transition, so as to enable the content of martensite is in the range that a better magnetic performance of the final product can be obtained, and an optimization in the magnetic performance of the final product is realized.
- a method for manufacturing oriented silicon steels with good magnetic performance comprising steps as follows:
- the tension force can be applied to the strip of steel by disposing a tension roller within a normalizing furnace or varying front and rear tension rollers.
- the stress or strain induces the martensite phase to be transited, so as to achieve reasonable and effective control on the amount of the martensite in the steel sheet after normalizing, and finally, the magnetic performance of the final product is improved.
- a relatively homogeneous martensite structure can be derived in the direction of the thickness of the steel sheet. Due to utilize a tension control, limit due to the site conditions is fewer, for a sample sheet with same thickness, the desired amount of martensite can be obtained stably, while the tension control is quantified with a little human factor, so that it is more easy to control accurately, and fine tuning can be achieved.
- the amount of martensite after normalizing is optimized so as to make the content of the martensite in normalized steel sheet in a range that a better magnetic performance of the final product can be obtained, and finally, a better magnetic performance of the final product is obtained.
- the composition of steel sheets is identical, conditions of manufacturing processes are identical and methods for measuring martensite amount are identical, the amounts of martensite in the sheets are identical. So, the relation between the martensite amount and the magnetic performance of the final product can be calculated in advance in accordance with the amount of martensite in the steel sheet after normalizing and before cold rolling measured by the same measuring method in the sample sheet that is produced in advance, a target range of the amount of martensite in the steel sheet after normalizing and before cold rolling can be calculated.
- the steps (1), (2), (3) and (4) in the method in accordance with the present invention are all general technical means for manufacturing the grain-oriented silicon steel, and the description thereof will be omitted.
- the present invention can obtain relatively homogeneous martensite texture in the direction of plate thickness, and can perform the fine tuning with respect to the content of martensite as desired.
- the present invention utilizes the tension control with few limits due to the site condition, and with respect to the sample plates having the same thickness, the desired amount of martensite can be obtained stably; the tension control is more quantified, influence of artificial factors is few, it is easy to conduct an accurate control, and the fine tuning can be realized.
- Table 1 (% by weight) NO. Si C Als N Mn S 1 3.03 0.0456 0.0264 0.0078 0.12 ⁇ 0.0060 2 3.22 0.0507 0.0261 0.0081 0.12 ⁇ 0.0060 3 3.41 0.0542 0.0269 0.0083 0.12 ⁇ 0.0060
- the steel sheet which comprises the above-described compositions, is heated to 1200°C, which temperature is held preserved for 180 minutes. Then, the steel sheet is directly rolled to 2.0mm. Two-stage normalizing process is carried out to the sheet which is hot rolled. Firstly, the steel sheet is heated to 1200°C, then cooled to 900°C within 200s, and next, the steel sheet is rapidly cooled in water having the temperature of 100°C.
- Stress (1 ⁇ 200N/mm 2 ) in the steel sheet at the normalizing phase transition can be varied by at least one of adjusting a tension roller disposed within the furnace or varying front and rear tension rollers, so as to optimize of the content and distribution of martensite in the normalized sheet within a range that a better magnetic performance range can be achieved.
- a single-stage cold rolling is carried out to the steel sheet for 5 rolling passes, wherein the third and fourth passes are at 220 °C, and the steel sheet is pressed to have a thickness of 0.30mm.
- Decarburization and nitride annealing is carried out to the cold rolled sheet at 850 °C.
- an annealing separator whose main composition is MgO, is coated on the surface of the sheet, being heated to 1220°C in an atmosphere of 25% N 2 and 75% H 2 , then the atmosphere is changed to pure H 2 , and the sheet is preserved in this temperature for 30 hours.
- the main chemical compositions of the steel sheet are Si 3.05% by weight, C 0.060% by weight, Als 0.0290% by weight, N 0.0077% by weight, Mn 0.13% by weight and S ⁇ 0.006% by weight.
- the steel sheet which contains the above-described compositions, is heated to 1200°C, which temperature is held for 180 minutes.Then, the steel sheet is directly rolled to 2.0mm. Two-stage normalizing process is carried out to the hot rolled sheet, firstly, the steel sheet is heated to 1100°C, and then cooled to 1000°C in 50s, and next, the steel sheet is rapidly cooled in water having the temperature of 50°C.Stress (1 ⁇ 200N/mm 2 ) in steel sheet in the normalizing phase transition (in 900°C to 500°C) can be varied by at least one of adjusting a tension roller disposed within furnace or varying a winding tension, so as to optimize the content and distribution of martensite in the normalized sheet within a range that a better magnetic performance range can be achieved.
- a single-stage cold rolling is carried out to the steel sheet for 5 rolling passes, wherein the third and fourth passes are at 220 °C, and the steel sheet is pressed to have a thickness of 0.30mm.
- Decarburization and nitride annealing is carried out to the cold rolled strip at 850°C.
- an annealing separator whose main composition is MgO, is coated on the surface of the sheet, being heated to 1220°C in an atmosphere of 25% N 2 and 75% H 2 , then the atmosphere is changed to pure H 2 , and the sheet is preserved in this temperature for 30 hours.
- the main chemical compositions of the steel sheet are Si 2.9wt%, C 0.048wt%, Als 0.0255wt%, N 0.0073wt%, Mn 0.10wt% and S ⁇ 0.006wt%.
- the steel sheet which contains the above-described compositions, is heated to 1200°C, which temperature is held for 180 minutes. Then, the steel sheet is directly rolled to 2.0mm. Two-stage normalizing process is carried out to the hot rolled sheet, firstly, the steel sheet is heated to 1100°C, and then cooled to 900 °C in 100s. Next, the steel sheet is quick cooled in water having the temperature of 80 °C.
- Stress (1 ⁇ 200N/mm 2 ) in the steel sheet in the normalizing phase transition can be varied by at least one of adjusting a tension roller disposed within furnace or varying a winding tension, so as optimize the content and distribution of martensite in the normalized sheet within a range that a better magnetic performance can be achieved.
- a single-stage cold rolling is carried out to the sheet for 5 rolling passes, wherein the third and fourth passes are at 220 °C, and the steel sheet is pressed to have a thickness of 0.30mm.
- Decarburization and nitride annealing is carried out to the cold rolled sheet at 850°C.
- an annealing separator whose main composition is MgO, is coated on the surface of the sheet, being heated to 1220°C in an atmosphere of 25% N 2 and 75% H 2 , then the atmosphere is changed to pure H 2 , and the sheet is preserved in this temperature for 30 hours.
- the main chemical compositions of the steel sheet are Si 3.41% by weight, C 0.0542% by weight, Als 0.0269% by weight, N 0.0083% by weight, Mn 0.12% by weight and S ⁇ 0.006% by weight.
- the steel sheet which contains the above-described compositions, is heated to 1200°C, which temperature is held for 180 minutes. Then, the steel sheet is directly rolled to 2.0mm. Normalizing annealing is carried out by means of the method described below, respectively.
- the steel sheet is heated to 1180°C, and then cooled to 920°C in 200s, and next, the steel sheet is rapidly cooled in water having a temperature of 100°C.
- the single-stage cold rolling is carried out to the sheet for 5 rolling passes, wherein the third and fourth passes are at 220 °C, the steel sheet is pressed to have a thickness of 0.30mm.
- Decarburization and nitride annealing are carried out to the cold rolled strip at 850°C.
- an annealing separator whose main composition is MgO, is coated on the surface of the sheet, being heated to 1220°C in an atmosphere of 25% N 2 and 75% H 2 , then the atmosphere is changed into pure H 2 , and the sheet is preserved in the temperature for 30 hours.
- a relatively homogeneous martensite texture in the sheet-thickness direction can be obtained by means of the tension control.
- the desired amount of martensite can be obtained stably; a better magnetic performance of the final product can be obtained.
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Claims (2)
- Verfahren zur Herstellung von kornorientiertem Siliciumstahl mit hervorragender magnetischer Leistung, umfassend die folgenden Schritte:1) konventionelles Schmelzen und Gießen, um einen Stahlrohling zu bilden;2) Erhitzen des Stahlrohlings und Warmwalzen des Stahlrohlings zu einem Stahlstreifen;3) Normalisierungsprozess
Durchführen des Normalisierungsprozesses mit zwei Stufen, wobei der Streifen zuerst auf 1100-1200 °C erhitzt wird, und dann in 50-200 s auf 900-1000 °C abgekühlt wird; und der Streifen als nächstes in Wasser mit einer Temperatur von 10-100 °C rasch abgekühlt wird; wobei in diesem Zeitraum eine Zugkraft auf den Stahlstreifen ausgeübt wird, wobei der Stahlstreifen in einem Temperaturbereich von 900°C-500 °C eine Spannung von 1-200 N/mm2 aufweist;4) Kaltwalzen;
Durchführen eines primären Kaltwalzens oder eines doppelten Kaltwalzens mit zwischendurch erfolgendem Glühen;5) Durchführen eines primären Umkristallisierungsglühens, dann Beschichten mit einem Glühseparator, dessen Hauptzusammensetzung MgO ist, um Glühen zu einem Endprodukt durchzuführen, wobei Glühen sekundäres Umkristallisationsglühen und Reinigungsglühen umfasst. - Verfahren zur Herstellung eines kornorientierten Siliciumstahls mit hervorragender magnetischer Leistung nach Anspruch 1, dadurch gekennzeichnet, dass die Zugkraft auf den Stahlstreifen ausgeübt wird, indem eine Zugwalze in einem Normalisierungsofen vorgesehen wird oder vordere und hintere Zugwalzen variiert werden.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2010105610513A CN102477483B (zh) | 2010-11-26 | 2010-11-26 | 一种磁性能优良的取向硅钢生产方法 |
PCT/CN2011/073419 WO2012068830A1 (zh) | 2010-11-26 | 2011-04-28 | 一种磁性能优良的取向硅钢生产方法 |
Publications (3)
Publication Number | Publication Date |
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EP2644715A1 EP2644715A1 (de) | 2013-10-02 |
EP2644715A4 EP2644715A4 (de) | 2016-12-14 |
EP2644715B1 true EP2644715B1 (de) | 2018-04-25 |
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EP11842864.8A Active EP2644715B1 (de) | 2010-11-26 | 2011-04-28 | Herstellungsverfahren für einen kornorientierten siliziumstahl mit hoher magnetkraft |
Country Status (7)
Country | Link |
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EP (1) | EP2644715B1 (de) |
JP (1) | JP5845275B2 (de) |
KR (1) | KR101512090B1 (de) |
CN (1) | CN102477483B (de) |
MX (1) | MX351880B (de) |
RU (1) | RU2552792C2 (de) |
WO (1) | WO2012068830A1 (de) |
Cited By (1)
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CN110724808A (zh) * | 2019-10-09 | 2020-01-24 | 马鞍山钢铁股份有限公司 | 一种由3.01~4.5mm的热轧卷冷轧生产电工钢的方法 |
Families Citing this family (9)
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CN103526000A (zh) * | 2013-09-13 | 2014-01-22 | 任振州 | 一种低碳高锰取向硅钢片的制备方法 |
CN104726651B (zh) * | 2013-12-23 | 2016-11-16 | 鞍钢股份有限公司 | 一种提高普通取向硅钢成材率的常化方法 |
CN104475460B (zh) * | 2014-11-14 | 2017-03-15 | 武汉钢铁(集团)公司 | 一种控制高磁感取向硅钢常化后冷轧边裂的方法 |
JP6455468B2 (ja) * | 2016-03-09 | 2019-01-23 | Jfeスチール株式会社 | 方向性電磁鋼板の製造方法 |
CN114107787A (zh) * | 2020-08-27 | 2022-03-01 | 宝山钢铁股份有限公司 | 一种高磁感取向硅钢及其制造方法 |
CN113211325B (zh) * | 2021-05-07 | 2022-07-12 | 包头市威丰稀土电磁材料股份有限公司 | 一种物理喷砂方式制备取向硅钢薄带无底层原料的方法 |
CN113930589A (zh) * | 2021-09-22 | 2022-01-14 | 包头钢铁(集团)有限责任公司 | 一种取向硅钢实验室常化工艺方法 |
CN114622076A (zh) * | 2022-03-11 | 2022-06-14 | 安阳钢铁股份有限公司 | 一种低温高磁感取向硅钢的制备方法 |
CN115747650B (zh) * | 2022-11-14 | 2023-08-18 | 鞍钢股份有限公司 | 一种低温高磁感取向硅钢及提高其磁性能稳定性的方法 |
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2010
- 2010-11-26 CN CN2010105610513A patent/CN102477483B/zh active Active
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2011
- 2011-04-28 JP JP2013538037A patent/JP5845275B2/ja active Active
- 2011-04-28 WO PCT/CN2011/073419 patent/WO2012068830A1/zh active Application Filing
- 2011-04-28 MX MX2013005869A patent/MX351880B/es active IP Right Grant
- 2011-04-28 KR KR20137013154A patent/KR101512090B1/ko active IP Right Grant
- 2011-04-28 RU RU2013127584/02A patent/RU2552792C2/ru active
- 2011-04-28 EP EP11842864.8A patent/EP2644715B1/de active Active
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110724808A (zh) * | 2019-10-09 | 2020-01-24 | 马鞍山钢铁股份有限公司 | 一种由3.01~4.5mm的热轧卷冷轧生产电工钢的方法 |
CN110724808B (zh) * | 2019-10-09 | 2021-01-26 | 马鞍山钢铁股份有限公司 | 一种由3.01~4.5mm的热轧卷冷轧生产电工钢的方法 |
Also Published As
Publication number | Publication date |
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KR20130101099A (ko) | 2013-09-12 |
CN102477483A (zh) | 2012-05-30 |
WO2012068830A1 (zh) | 2012-05-31 |
JP5845275B2 (ja) | 2016-01-20 |
MX351880B (es) | 2017-11-01 |
CN102477483B (zh) | 2013-10-30 |
EP2644715A4 (de) | 2016-12-14 |
JP2013544970A (ja) | 2013-12-19 |
KR101512090B1 (ko) | 2015-04-14 |
EP2644715A1 (de) | 2013-10-02 |
RU2013127584A (ru) | 2015-01-10 |
MX2013005869A (es) | 2013-07-15 |
RU2552792C2 (ru) | 2015-06-10 |
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