US20130233450A1 - Method for manufacturing oriented silicon steel product with high magnetic-flux density - Google Patents
Method for manufacturing oriented silicon steel product with high magnetic-flux density Download PDFInfo
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- 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
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- 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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- 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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- C21D8/1255—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 with diffusion of elements, e.g. decarburising, nitriding
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- 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
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- 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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- 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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- C22C38/001—Ferrous alloys, e.g. steel alloys containing N
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
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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
- H01F1/16—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 in the form of sheets
Definitions
- the present invention relates to a method for manufacturing oriented silicon steel sheet, and particularly, to a method for manufacturing oriented silicon steel sheet with a high magnetic-flux density.
- the conventional process for manufacturing oriented silicon steel with high magnetic-flux density is as follows. After being smelted in a convertor or electric furnace, molten steel is secondarily refined and alloyed, and then continuous-casted into steel slabs. Its basic chemical compositions are: Si 2.5 ⁇ 4.5%, C 0.06 ⁇ 0.10%, Mn 0.03 ⁇ 0.1, S 0.012 ⁇ 0.050, Al 0.02 ⁇ 0.05%, N 0.003 ⁇ 0.012. Some composition systems further contain one or more of the elements Cu, Mo, Sb, B, Bi, etc. The rest is Fe and unavoidable impure inclusions.
- a steel slab is heated to a temperature over 1350 in a special furnace and maintained at the temperature for more than 45 min so as to make the advantageous inclusions MnS or AlN fully solid-dissolved, then rolled into steel plates with a finishing temperature up to over 950° C.; and then a plate is cooled rapidly to below 500° C. by jetting water, thereafter, coiled to be coil-shaped. Subsequently, during normalization, fine and dispersed second phase particles, namely depressant, separate out of silicon steel body. After being normalized, the hot rolled steel plates are pickled and removed of oxidized scale, and then cold-rolled into sheets of the thickness of finished steel sheet product.
- a cold rolled sheet is decarburization annealed and coated with an anneal insulator (main composition is MgO).
- the carbon in the sheet is decarburized to the extent as not to influence the magnetic property of the finished steel sheet product (generally it shall be below 30 ppm); during being high temperature annealed, the steel sheet generates physical and chemical changes such as secondary re-crystallization, formation of bottom layer of magnesium silicate and purification (elements S, N, etc., harmful to magnetic property, are eliminated from the steel sheet), and is made to be a highly-oriented, low-iron-loss and high-magnetic-induction silicon steel sheet; finally, after being coated with insulation layer and tension-annealed, the silicon steel sheet is made to be commercially available oriented silicon steel sheet product.
- the heating temperature must be up to 1400° C. in order to have the depressant fully solid-dissolved. This is the upmost level of a conventional heating furnace.
- burning loss is big and the heating furnace needs to be frequently mended, thus resulting in a low utilization.
- energy consumption is high.
- the hot rolled coil-shaped plate often has larger edge cracks, which may cause difficulty in the subsequent cold rolling procedure, and result in a low yield rate, unsatisfactory magnetic property B 8 of the finished product, and higher manufacture cost.
- the research can be categorized into two types. One is to heat a steel slab to a temperature within the range of 1250 ⁇ 1320° C. and to use AlN and Cu as a depressant. The other is to heat a slab to a temperature within the range of 1100 ⁇ 1250° C. and to acquire depression capability by employing a depressant which is formed by nitriding after decarburization.
- Chinese Patent CN 200510110899 describes a new process, where steel slabs are heated at a temperature not higher than 1200° C., and the cold rolled steel sheets, which have been rolled to the thickness of the finished product, are nitrided prior to decarburized annealing. In this process, however, it is necessary to strictly control the dew point during nitriding, and there will occur a new problem that decarburization becomes more difficult.
- Korean Patent KR 2002074312 disclosed that steel slabs are heated to a temperature not higher than 1200° C., and rolled sheets are decarburized and nitrided simultaneously. Although the difficulties in post-rolling decarburization and post-rolling nitriding can be solved, however, uneven nitriding is still unavoidable and thus will give rise to uneven magnetic property of the finished silicon steel sheet product, and manufacture cost may be higher.
- Nb Adding element Nb is also proposed.
- Nb of 0.02 ⁇ 0.20% is added in the compositions of smelted steel. It is aimed at generating niobium carbide and niobium nitride and thereby to fine the re-crystallized texture, improving grain distribution and collective texture of the decarburization annealed steel sheets, taking the niobium carbide and niobium nitride as an auxiliary depressant to depress the growing up of the normal grains during high temperature annealing, and thus improving the magnetic property of silicon steel sheets.
- nitrates of Al, Fe, Mg and Zn are added into a separant MgO. It aims at making them decomposed during high temperature anneal and thus releasing nitrogen oxide so as to nitride steel sheets.
- the nitrogen oxide and oxygen out of the decomposed nitrates may lead to an explosion risk in practical production.
- sulfanilic acid is added in separant MgO. It is aimed at making sulfanilic acid decompose in high temperature and thus release nitrides for nitriding.
- sulfanilic acid will decompose at a lower temperature (about 205° C.), the nitrogen released at so low temperature is hard to make steel sheet nitrided.
- nitriding of steel sheets during high temperature anneal is realized by adding nitrides of Mn and Si.
- a problem with this method lies in that these nitrides have a high thermostability. Therefore, they can not be decomposed effectively and quickly.
- Japanese patents JP 54040227 and JP200119751 put forward that oriented silicon steels with high magnetic-flux density can be obtained by reducing temperature rise rate in the course of high temperature annealing.
- simply reducing temperature rise rate may result in a greatly reduced production rate.
- the object of the present invention is to provide a method for manufacturing an oriented silicon steel product with high magnetic-flux density, which solves the difficulty in nitriding for manufacturing oriented silicon steel sheet with high magnetic-flux density where steel slabs are heated at a lower temperature.
- the present invention efficiently ensures safe and stable operation and a long life of smelting furnaces by a technique of heating at a lower temperature.
- oriented silicon steel sheets can be fully nitrided during high temperature annealing, which can ensure secondary re-crystallization to take place perfectly, and thereby, the oriented silicon steel sheets with high magnetic-flux density and premium magnetic property can be achieved.
- the invention adopts the following technical solution.
- Nb is added in the compositions of oriented silicon steel so as to make oriented silicon steel sheet be easy to be nitrided because the nitrogen content in steel is crucial in deciding whether the magnetic property of the finished oriented silicon steel sheet product meet specifications.
- Some nitrates are added in MgO separant and the MgO separant added with nitrates is applied on the surfaces of the steel sheets before the sheets are high temperature annealed. During high temperature annealing, the nitrates decompose and release nitrogen which can make the steel sheets fully nitrided.
- the temperature rise rate during high temperature annealing is regulated according to the Nb content, N content prior to secondary heating and the beginning temperature of secondary heating, thus ensuring secondary re-crystallization to take place perfectly, and thereby, the oriented silicon steel sheets with high magnetic-flux density and premium magnetic property can be achieved.
- a method for manufacturing an oriented silicon steel product with high magnetic-flux density includes the following procedures:
- the oriented silicon steel is composed of, by weight, 0.035 ⁇ 0.065% of C, 2.9 ⁇ 4.0% of Si, 0.05 ⁇ 0.20% of Mn, 0.005 ⁇ 0.01% of S, 0.015 ⁇ 0.035% of Al, 0.004 ⁇ 0.009% of N, 0.005 ⁇ 0.090% of Sn, 0.200 ⁇ 0.800% of Nb, the rest is Fe and unavoidable inclusions. After being smelted, molten steel is secondarily refined and then casted into steel slabs.
- Said steel slabs are heated in a heating furnace to 1090 ⁇ 1200° C., and then, are hot rolled into steel plates at a beginning temperature of 1180° C. and are finished with the hot rolling step at a finishing temperature of 860° C., said steel plates are cooled by laminar flow of water to below 650° C. and then coiled into coiled-shape plates.
- a coiled-shape plate is normalized at the normalization temperature of 1050 ⁇ 1180° C. for 1 ⁇ 20 sec and then at the normalization temperature of 850 ⁇ 950° C. for 30 ⁇ 200 sec, and thereafter, is cooled down at a cooling rate of 10 ⁇ 60° C./sec;
- the steel plate After being normalized, the steel plate is cold rolled into steel sheets with the thickness of the finished oriented silicon steel sheet product at a rolling compression ratio not less than 75%;
- a steel sheet is heated to the temperature of 800 ⁇ 860° C. at a temperature rise rate of 15 ⁇ 35° C./sec and maintained at the temperature for 90 ⁇ 160 sec for being decarburized, herein only decarburization must be carried out because nitriding will take place during high temperature annealing;
- said steel sheets After being decarburized, said steel sheets are covered with a coating which is composed of, by weight, 0.1 ⁇ 10% of NH 4 Cl and 0.5 ⁇ 30% of P 3 N 5 , and MgO as rest wherein MgO is a main component.
- the steel sheet After being coated with the isolator, the steel sheet is firstly heated to a temperature of 700 ⁇ 900° C., and then secondarily heated to 1200° C. at temperature rise rate V secondary temperature rise of 9 ⁇ 17° C./hr and maintained at 1200° C. for 20 hr for being purification annealed and nitrided;
- the surfaces of the steel sheet After being high temperature annealed, the surfaces of the steel sheet is coated with an insulation layer, and then is tension and leveling annealed, and finally becomes the oriented silicon steel sheet with high magnetic-flux density and premium magnetic property.
- Nb is added into the silicon steel.
- the first reason is that the oriented silicon steel with Nb in its compositions is much easier to be nitrided, this is because the d sublayer of sub-outer spheres of the atom of Nb is unsaturated with electrons and so Nb is much easier to change into nitrides than Fe and Mn, and nitride of Nb is very stable.
- the second reason is that the N atoms, which penetrate into steel sheets during high temperature annealing, can bond with Al to generate main depressant AlN which is necessary to obtain oriented silicon steel sheet with high magnetic-flux density, and also can be combined into Nb 2 N and NbN.
- These nitrides of Nb can be an auxiliary depressant and can intensify depressing effect on growth of normal crystal grains. In general, this solution is very advantageous to improve the magnetic property of oriented silicon steel sheet.
- a certain amount of NH 4 Cl and P 3 N 5 is added into a liquid MgO coating.
- the intention of doing this is to use decomposition of the two nitrides during high temperature annealing to realize nitriding of silicon steel sheets, and thereby to replace the nitriding which will take place by virtue of decomposition of ammonia during decarburization anneal, the greatest benefit of this solution is to ensure the steel sheets to be nitrided evenly.
- the reason of selecting NH 4 Cl and P 3 N 5 as nitriding material which will decompose at high temperature is that NH 4 Cl will decompose at 330 ⁇ 340° C. and P 3 N 5 will decompose at 760° C.
- the decomposition of the two different nitrides at different temperatures ensures to evenly release active atoms of nitrogen in a relatively long time in the procedure of high temperature annealing, this is advantageous to nitriding of the steel sheets and to maintaining N content therein to be within standard limits of 200 ⁇ 250 ppm.
- the temperature rise rate for the secondary heating during high temperature annealing is controlled to ensure the finished oriented silicon steel sheet product to attain premium magnetic property by setting a proper secondary temperature rise rate. This is because the course of secondary temperature rise for high temperature annealing covers the whole temperature range of secondary re-crystallization. Therefore, a proper temperature rise rate can ensure the Gauss grains which grow during the secondary re-crystallization to have a much better orientation (deviation angle ⁇ 3°) and magnetic property.
- the relatively low temperature rise rate during high temperature annealing can refine the secondary re-crystallization and ensure the finished steel sheet product to have a better magnetic property. This is because gradual coarsening and decomposition of AlN as well as the secondary re-crystallization can take place simultaneously during secondarily heating for high temperature annealing, and so the depressing effect disappears simultaneously. If the temperature rises too quickly within this temperature range, it will result in such a case that the depressant has decomposed and lost its effect before the secondary re-crystallization has not yet finished. As is known, imperfect secondary re-crystallization will bring about poor magnetic property of the finished oriented silicon steel sheet product.
- Material steel of oriented silicon steel sheet with the chemical compositions shown in Table 1 is smelted and casted into slabs.
- the slabs with different chemical compositions are heated to the temperature of 1155° C. in a heating furnace and maintained at the temperature for 1.5 hours, and then hot rolled into plates of 2.3 mm thickness at a beginning temperature of 1062° C. and finishing temperature of 937° C.
- the hot rolled plates are normalized in two phases: at 1120° C. for 15 sec and at 870° C. for 150 sec ((1120° C. ⁇ 15 sec)+(870° C. ⁇ 150 sec)), and then cooled down at the rate of ⁇ 15° C./sec.
- the hot rolled plates are cold rolled to coil-shaped steel sheets with the thickness 0.30 mm of the finished steel sheet product, and then in sequence, the cold rolled coil-shaped sheets are heated at temperature rise rate of 25° C./sec to decarburization temperature of 820° C. and maintained at the temperature for 140 sec for being decarburization annealed; applied and covered with a thick layer of a separant which contains MgO as the main component and NH 4 Cl of 4.5% and P 3 N 5 of 15%; heated to 800° C. for being high temperature annealed and getting nitrogen content b before being secondarily heated; secondarily heated to temperature of 1200° C. and maintained at the temperature for 20 hours for being purification annealed.
- the sheets After being uncoiled to steel sheets of some length, the sheets are applied with an insulation coating layer and then are tension and leveling annealed.
- the nitrogen content b prior to secondary heating and the magnetic property of the finished steel sheet product are both shown in Table 1.
- the selection of various chemical compositions according to the embodiment is in consistence to the standard specification (of smelting and casting) in the production procedures of the present invention.
- the selection of component Nb in the comparison examples is not within the standard limits of 0.200 ⁇ 0.800, therefore, the amount of N measured before secondary heating is not within the standard limits of 200 ⁇ 250 ppm, and finally causes the finished oriented silicon steel sheet product to have a larger iron loss (P 17/50 ) and a poor magnetic property (B 8 ).
- the oriented silicon steel slabs is composed of (by weight percent) the following elements: C 0.05%, Si 3.25%, Mn 0.15%, S 0.009%, Al 0.032%, N 0.005%, Sn 0.02%, Nb 0.5%, the rest is Fe and unavoidable impurities.
- the slabs are heated to the temperature of 1155° C. in a heating furnace and maintained at the temperature for 1.5 hours, and then hot rolled into plates of 2.3 mm thickness at a beginning temperature of 1080° C. and finishing temperature of 910° C.
- the hot rolled plates are normalized in two phases: at 1110° C. for 10 sec and at 910° C.
- the hot rolled plates are cold rolled into coil-shaped sheets with the thickness 0.30 mm of the finished steel sheet product, and then in sequence, the cold rolled coil-shaped sheets are heated to the decarburization temperature of 840° C. at temperature rise rate of 25° C./sec and maintained at the temperature for 130 sec for being decarburization annealed; applied and covered with a thick layer of a separant which contains MgO as the main component and NH 4 Cl and P 3 N 5 of certain small contents; heated to 800° C.
- the selection of NH 4 Cl and P 3 N 5 according to the embodiment is in consistence to the standard ranges of 0.1 ⁇ 10% and 0.5 ⁇ 30% (of MgO coating) in the production procedures of the present invention.
- whatever one is not within the standard limits causes the content of N measured before secondary heating to be not within the standard limits of 200 ⁇ 250 ppm, and finally causes the finished oriented silicon steel sheet product to have a larger iron loss (P 17/50 ) and a poor magnetic property (B 8 ).
- the oriented silicon steel slabs is composed of the following components: C 0.05%, Si 3.25%, Mn 0.15%, S 0.009%, Al 0.032%, N 0.005%, Sn 0.02%, Nb (a)0.2 ⁇ 0.8%, the rest is Fe and unavoidable inclusions.
- the slabs are heated to the temperature of 1155° C. in a heating furnace and maintained at the temperature for 2.5 hours, and then are hot rolled into plates of 2.3 mm thickness at a beginning temperature of 1050° C. and finishing temperature of 865° C.
- the hot rolled plates are normalized in two phases: at 1120° C. for 15 sec and at 900° C.
- the hot rolled plates are cold rolled to coil-shaped sheets with the thickness 0.30 mm of the finished steel sheet product, and then in sequence, the cold rolled coil-shaped sheets are heated to the decarburization temperature of 850° C. at temperature rise rate of 25° C./sec and maintained at the temperature for 115 sec for being decarburization annealed; applied and covered with a thick layer of a separant which contains MgO as the main component and NH 4 Cl of 7.5% and P 3 N 5 of 12.5%; heated to 700 ⁇ 900° C.
- Table 3 The data of the third embodiment are shown in Table 3.
- the present invention provides a new method for manufacturing an oriented silicon steel sheet with high magnetic-flux density based on the procedure of heating steel slabs at a lower temperature. According to the method of the present invention, the above-mentioned problems are all effectively solved.
- the method is characterized in that the steel sheets can be easily nitrided during high temperature annealing by adding a certain amount of Nb in molten steel; the steel sheets can be evenly nitrided during high temperature annealing by adding some nitrides into the separant MgO and letting them decomposing during high temperature annealing; in the course of high temperature annealing, the temperature rise rate can be controlled according to Nb content, N content and the beginning temperature of secondary heating so as to ensure completion of a good secondary re-crystallization course. All these solutions ensure the achievement of oriented silicon steel sheet with high magnetic-flux density and premium magnetic property.
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Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201010298954.7 | 2010-09-30 | ||
CN2010102989547A CN102443736B (zh) | 2010-09-30 | 2010-09-30 | 一种高磁通密度取向硅钢产品的生产方法 |
PCT/CN2011/072768 WO2012041054A1 (zh) | 2010-09-30 | 2011-04-14 | 一种高磁通密度取向硅钢产品的生产方法 |
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CN110055393A (zh) * | 2019-04-28 | 2019-07-26 | 首钢智新迁安电磁材料有限公司 | 一种薄规格低温高磁感取向硅钢带生产方法 |
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RU2552562C2 (ru) | 2015-06-10 |
KR101451824B1 (ko) | 2014-10-16 |
WO2012041054A1 (zh) | 2012-04-05 |
KR20130049823A (ko) | 2013-05-14 |
RU2013114861A (ru) | 2014-11-10 |
CN102443736B (zh) | 2013-09-04 |
MX2013003367A (es) | 2013-05-22 |
MX350000B (es) | 2017-08-23 |
EP2623621A1 (en) | 2013-08-07 |
JP2013545885A (ja) | 2013-12-26 |
CN102443736A (zh) | 2012-05-09 |
EP2623621A4 (en) | 2017-12-06 |
EP2623621B1 (en) | 2019-03-13 |
JP5864587B2 (ja) | 2016-02-17 |
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