CN105154646A - Annealing separant for high-magnetic-induction oriented silicon steel and preparation method thereof - Google Patents
Annealing separant for high-magnetic-induction oriented silicon steel and preparation method thereof Download PDFInfo
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- CN105154646A CN105154646A CN201510691804.5A CN201510691804A CN105154646A CN 105154646 A CN105154646 A CN 105154646A CN 201510691804 A CN201510691804 A CN 201510691804A CN 105154646 A CN105154646 A CN 105154646A
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- silicon steel
- oriented silicon
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Abstract
The invention relates to an annealing separant for high-magnetic-induction oriented silicon steel, which is composed of the following raw materials in percentage by weight: 1-6% of TiO2, 0.1-2% of Sb2(SO4)3 and the balance of MgO. Water is additionally added, wherein the MgO:water ratio is 1:(8-15). The preparation method comprises the following steps: mixing the MgO and water; adding TiO2, and stirring sufficiently and uniformly; adding the Sb2(SO4)3, and stirring; and continuing stirring for not less than 2 hours for later use. The annealing separant enables the high-magnetic-induction oriented silicon steel to have favorable magnetic induction property and bottom quality, has favorable insulating property, is suitable for the operating requirements of high-capacity transformers, and can lower the concession rate of the product.
Description
Technical field
The present invention relates to a kind of silicon steel separant and preparation method, belong to a kind of high magnetic induction grain-oriented silicon steel annealing separating agent and preparation method particularly.
Background technology
Oriented silicon steel is in a large number for the magnetive cord material of transformer.Magnetive cord material requirements magneticflux-density (B
8) high, iron loss (P
17/50) low.Transformer is constantly to super-huge future development in recent years, also requires volume of transformer miniaturization simultaneously, and will meet the requirement such as national energy-saving, saving resource, therefore, in the urgent need to using the oriented silicon steel with high magnetic strength, being conducive to reducing the wastage, reducing volume of transformer.
For meeting this requirement, as the method improving oriented silicon steel magnetic induction density, in steel plate, add Sn or Sb element.But, because the fusing point of Sn or Sb element is lower, in secondary recrystallization process, [%Sn] or [%Sb] gasification in steel, from surface of steel plate diffusion, easily pile up at the interface of bottom/surface of steel plate, cause the bottom tack of oriented silicon steel poor.
Current major part research is all devoted to develop the minute surface high magnetic induction grain-oriented silicon steel without bottom.If Chinese Patent Application No. is the document of CN201010518037.5, disclose a kind of annealing separating agent preparing the mirror surface-oriented silicon steel with fine magnetic property, its composition by weight percent is: Al
2o
3powder 77 ~ 98%, alkaline earth metallic oxide powder end 1 ~ 8%, alkali metal chloride is or/and alkaline earth metal chloride 1 ~ 15%.The annealing separating agent of this invention makes high-temperature annealing process light plate surface not form glassy membrane bottom, utilizes muriatic corrosion reaction to remove the embedded oxide on the nearly surface of substrate simultaneously, thus obtains any surface finish and magnetic property stable product.Chinese Patent Application No. is the document of CN201110299949.2, discloses the mirror surface-oriented silicon steel manufacture method with fine magnetic property, and its annealing separating agent composition quality percentage ratio is: Al
2o
3powder, 65-96 part, silicate powder, 2-15 part, its particle diameter between 0.1-100 μm, alkaline earth metal oxide, 1-10 part, metal chloride, 1-10 part; Wherein, silicate powder comprises Al
4(SiO
4)
3, CaSiO
3, Mg
2siO
4, Fe
2siO
4in more than one; Metal chloride comprises alkali metal chloride LiCl, NaCl, KCl, RbCl, alkaline earth metal chloride BeCl
2, MgCl
2, CaCl
2, SrCl
2, BaCl
2in more than one; Alkaline earth metal oxide comprise in BeO, MgO, CaO, SrO, BaO more than one; Be nitrogen and hydrogen mixture in atmosphere after oven dry, 25% ~ 100%H
2, D.P.<0 DEG C, temperature is carry out the insulation high temperature annealing of more than 15 hours under the condition of 1150 ~ 1250 DEG C, then through being coated with insulating coating and stretching and leveling annealing obtains the minute surface grain-oriented silicon-iron product of excellent magnetic.But this mirror surface-oriented silicon steel insulating property without bottom and surface quality poor, and traditional production technique and insulating coating solution be difficult to meet produce this oriented silicon steel without bottom, R&D costs and production cost higher.
The formation of bottom is main containing SiO by what formed when the MgO in annealing separating agent and decarburizing annealing
2oxide film reaction form forsterite film, be usually referred to as glassy membrane reaction (2MgO+SiO
2→ Mg
2siO
4).MgO may become very active under certain condition, hydration reaction MgO → Mg (OH)
2just may occur under some mixing and stirring state.Namely thus be brought in coiled material therefore steam, and produce dew point between plate and plate and improve, the atmosphere problem of non-uniform of length and width.In addition, the type of additive and high number ground affect quality and the quantity of glassy membrane, and this depends on the existence of excessive oxygen and the effect of reaction acceleration.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, under a kind of prerequisite ensureing orientation steel plate magnetic property is provided, make bottom layer quality and insulating property more excellent, and reduce high magnetic induction grain-oriented silicon steel annealing separating agent and the preparation method of product concession rate.
Realize the measure of above-mentioned purpose:
A kind of high magnetic induction grain-oriented silicon steel annealing separating agent, its raw material composition and weight percent content are: TiO
2: 1 ~ 6%, Sb
2(SO
4)
3: 0.1 ~ 2%, all the other are MgO; External adding water, amount of water is according to MgO: water=1:8 ~ 15; Annealing separating agent also will meet: Mg (OH)
2amount <1.5%, dried amount of moisture controls below 2%, and at 1000 DEG C, igloss is less than 0.5%, CAA value >200sec, granularity D50<5 μm.
It is: it is applicable to component and weight percent content is: C:0.04%-0.08%, Si:2.0%-4.5%, Mn:0.06%-0.12%, S:0.02%-0.03%, Als:0.02%-0.03%, N:0.006%-0.01%, Sn or Sb:0.001%-0.2%, separant when surplus carries out decarburizing annealing by the oriented silicon steel hot-rolled sheet of Fe and inevitable impurity after cold rolling.
A preparation method for high magnetic induction grain-oriented silicon steel annealing separating agent, its step:
1) mixed with water by MgO, the additional proportion of MgO and water carries out according to 1:8 ~ 15, and stirs full and uniform; Control Mg (OH)
2amount <1.5%;
2) TiO is added according to 1 ~ 6%
2, and stir full and uniform;
3) Sb is added according to 0.1 ~ 2%
2(SO
4)
3,and stir;
4) Sb
2(SO
4)
3continue after adding end to stir, the time is no less than 2 hours again;
5) stand-by.
It is: stir the strong mixing mode adopting and be not less than 4000rpm/min.
High magnetic induction grain-oriented silicon steel used in the present invention, the i.e. C:0.04%-0.08% of % by weight, Si:2.0%-4.5%, Mn:0.06%-0.12%, S:0.02%-0.03%, Als:0.02%-0.03%, N:0.006%-0.01%, Sn or Sb:0.001%-0.2% is as basal component, because the fusing point of its Sn or Sb element contained is lower, in secondary recrystallization process, Sn or Sb in steel can produce vaporization, the gas produced spreads from surface of steel plate, thus easily piles up at the interface of the bottom/surface of steel plate of steel plate.Thus, the present invention, through by lot of experiments, obtains and add TiO in separant
2and Sb
2(SO
4)
3, be conducive to MgO and earlier form bottom in high temperature annealing temperature-rise period, make inhibitor in steel more stable, promote the restraining effect of AlN, and be conducive to improving B
8.
Why the present invention takes the strong mixing mode being not less than 4000rpm/min, to make MgO abundant aquation under strong agitation, contributes to the bonding of bottom after high temperature annealing, namely improves bottom tack.
In addition, control MgO generates Mg (OH)
2amount <1.5%, the amount of moisture brought into after annealing separating agent drying is controlled below 2%, at 1000 DEG C, igloss is less than 0.5%, effectively can prevent from decompositing constitution water when high temperature annealing and making steel band peroxidation, destroy magnetic property to make annealing separating agent.
Why by MgO Task-size Controlling at D50<5 μm, during to make to mix with water, MgO slurries are uniformly dispersed, and not easily condense, thus the bottom layer quality formed is good.
The present invention compared with prior art, high magnetic induction grain-oriented silicon steel not only magnetic induction performance and bottom layer quality excellent, and good insulation preformance, is applicable to the service requirements of heavy body transformer, can also reduce the concession rate of product simultaneously.
Embodiment
Below the present invention is described in detail:
Table 1 is raw material composition and the content list of various embodiments of the present invention and comparative example;
Table 2 is the main technologic parameters value list of various embodiments of the present invention and comparative example;
Table 3 is for inventing the performance test results list of each embodiment and comparative example.
Various embodiments of the present invention are all produced according to following steps:
1) mixed with water by MgO, the additional proportion of MgO and water carries out according to 1:8 ~ 15, and stirs full and uniform; Control Mg (OH)
2amount <1.5%;
2) TiO is added according to 1 ~ 6%
2, and stir full and uniform;
3) Sb is added according to 0.1 ~ 2%
2(SO
4)
3,and stir;
4) Sb
2(SO
4)
3continue after adding end to stir, the time is no less than 2 hours again;
5) stand-by.
In table 1 and table 2, the data of each embodiment are not one_to_one corresponding.
The raw material composition of table 1 various embodiments of the present invention and comparative example and content list (wt%)
The main technique list of table 2 various embodiments of the present invention and comparative example
The performance test results of table 3 various embodiments of the present invention and comparative example
Illustrate: the differentiation of annealing separating agent tack of the present invention is the result drawn according to GB/T2522-1988.
For component and weight percent content be as can be seen from Table 3: C:0.04%-0.08%, Si:2.0%-4.5%, Mn:0.06%-0.12%, S:0.02%-0.03%, Als:0.02%-0.03%, N:0.006%-0.01%, Sn or Sb:0.001%-0.2%, surplus by Fe and inevitable impurity oriented silicon steel hot-rolled sheet through cold rolling, carry out decarburizing annealing after, after coating the present invention limits the annealing separating agent of index and processing parameter, there is excellent bottom and high magnetic strength.
This embodiment is only the best and exemplifies, the restricted enforcement not to technical solution of the present invention.
Claims (4)
1. a high magnetic induction grain-oriented silicon steel annealing separating agent, its raw material composition and weight percent content are: TiO
2: 1 ~ 6%, Sb
2(SO
4)
3: 0.1 ~ 2%, all the other are MgO; External adding water, amount of water is according to MgO: water=1:8 ~ 15; Annealing separating agent also will meet: Mg (OH)
2amount <1.5%, dried amount of moisture controls below 2%, and at 1000 DEG C, igloss is less than 0.5%, CAA value >200sec, granularity D50<5 μm.
2. a kind of high magnetic induction grain-oriented silicon steel annealing separating agent as claimed in claim 1, it is characterized in that: it is applicable to component and weight percent content is: C:0.04%-0.08%, Si:2.0%-4.5%, Mn:0.06%-0.12%, S:0.02%-0.03%, Als:0.02%-0.03%, N:0.006%-0.01%, Sn or Sb:0.001%-0.2%, separant when surplus carries out decarburizing annealing by the oriented silicon steel hot-rolled sheet of Fe and inevitable impurity after cold rolling.
3. a preparation method for high magnetic induction grain-oriented silicon steel annealing separating agent, its step:
1) mixed with water by MgO, the additional proportion of MgO and water carries out according to 1:8 ~ 15, and stirs full and uniform; Control Mg (OH)
2amount <1.5%;
2) TiO is added according to 1 ~ 6%
2, and stir full and uniform;
3) Sb is added according to 0.1 ~ 2%
2(SO
4)
3,and stir;
4) Sb
2(SO
4)
3continue after adding end to stir, the time is no less than 2 hours again;
5) stand-by.
4. the preparation method of a kind of high magnetic induction grain-oriented silicon steel annealing separating agent as claimed in claim 3, is characterized in that: stir the strong mixing mode adopting and be not less than 4000rpm/min.
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|---|---|---|---|
| CN201510691804.5A CN105154646B (en) | 2015-10-23 | 2015-10-23 | A kind of high magnetic induction grain-oriented silicon steel annealing separating agent and preparation method |
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| CN105154646B CN105154646B (en) | 2018-06-08 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319174A (en) * | 2016-09-23 | 2017-01-11 | 武汉钢铁股份有限公司 | Annealing isolation agent capable of improving quality of low-temperature casting blank heating high induction grain oriented silicon steel bottom layer |
| CN107746929A (en) * | 2017-11-23 | 2018-03-02 | 武汉钢铁有限公司 | High magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced |
| CN108893587A (en) * | 2018-08-24 | 2018-11-27 | 首钢智新迁安电磁材料有限公司 | A kind of preparation method and its application of MgO interleaving agent slurries |
| CN109248996A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of continuous casting steel billet burr interleaving agent and burr minimizing technology |
| CN113981196A (en) * | 2021-11-02 | 2022-01-28 | 无锡普天铁心股份有限公司 | Annealing separant for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof |
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| CN102952931A (en) * | 2011-08-30 | 2013-03-06 | 宝山钢铁股份有限公司 | Glass-film-free oriented silicon steel manufacture method and annealing isolation agent |
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| CN102952931A (en) * | 2011-08-30 | 2013-03-06 | 宝山钢铁股份有限公司 | Glass-film-free oriented silicon steel manufacture method and annealing isolation agent |
| CN104884646A (en) * | 2012-12-28 | 2015-09-02 | Posco公司 | Grain-oriented electrical steel sheet, and method for manufacturing same |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106319174A (en) * | 2016-09-23 | 2017-01-11 | 武汉钢铁股份有限公司 | Annealing isolation agent capable of improving quality of low-temperature casting blank heating high induction grain oriented silicon steel bottom layer |
| CN106319174B (en) * | 2016-09-23 | 2018-10-16 | 武汉钢铁有限公司 | Improve the annealing separating agent of low temperature casting blank heating high magnetic induction grain-oriented silicon steel bottom layer quality |
| CN109248996A (en) * | 2017-07-13 | 2019-01-22 | 鞍钢股份有限公司 | A kind of continuous casting steel billet burr interleaving agent and burr minimizing technology |
| CN109248996B (en) * | 2017-07-13 | 2020-05-29 | 鞍钢股份有限公司 | Continuous casting billet burr separant and burr removing method |
| CN107746929A (en) * | 2017-11-23 | 2018-03-02 | 武汉钢铁有限公司 | High magnetic induction grain-oriented silicon steel annealing agent and preparation method and its application on aquation rate is reduced |
| CN108893587A (en) * | 2018-08-24 | 2018-11-27 | 首钢智新迁安电磁材料有限公司 | A kind of preparation method and its application of MgO interleaving agent slurries |
| CN113981196A (en) * | 2021-11-02 | 2022-01-28 | 无锡普天铁心股份有限公司 | Annealing separant for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof |
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