CN105154646B - A kind of high magnetic induction grain-oriented silicon steel annealing separating agent and preparation method - Google Patents
A kind of high magnetic induction grain-oriented silicon steel annealing separating agent and preparation method Download PDFInfo
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- CN105154646B CN105154646B CN201510691804.5A CN201510691804A CN105154646B CN 105154646 B CN105154646 B CN 105154646B CN 201510691804 A CN201510691804 A CN 201510691804A CN 105154646 B CN105154646 B CN 105154646B
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Abstract
A kind of high magnetic induction grain-oriented silicon steel annealing separating agent, raw material composition and weight percent content are:TiO2:1 ~ 6%, Sb2(SO4)3:0.1 ~ 2%, remaining is MgO;External adding water, amount of water is according to MgO:Water=1:8~15;Preparation method:MgO is mixed with water;Add in TiO2And it stirs full and uniform;Add in Sb2(SO4)3,And it stirs;It is further continued for stirring and is no less than 2 hours;For use.The present invention not only makes high magnetic induction grain-oriented silicon steel magnetic induction performance and bottom layer quality excellent, but also good insulation preformance, suitable for the requirement of high power capacity transformer, while can also reduce the concession rate of product.
Description
Technical field
The present invention relates to a kind of silicon steel interleaving agent and preparation method, a kind of high magnetic induction grain-oriented silicon steel is specifically belonged to moving back
Fiery interleaving agent and preparation method.
Background technology
Orientation silicon steel is largely used to the magnetive cord material of transformer.Magnetive cord material requirements magnetic flux density(B8)High,
Iron loss(P17/50)It is low.Transformer constantly develops to super-huge direction in recent years, while also volume of transformer is required to minimize, and will
Meet national energy-saving, save the requirements such as resource, therefore, there is an urgent need to use the orientation silicon steel with high magnetic strength, advantageously reduce
Loss reduces volume of transformer.
To meet the requirement, as the method for improving orientation silicon steel magnetic induction intensity, Sn or Sb members are added in steel plate
Element.But since the fusing point of Sn or Sb elements is relatively low, during secondary recrystallization, [%Sn] or [%Sb] gasification in steel, from
Surface of steel plate is spread, and is easily come in the interface heap of bottom/surface of steel plate, the bottom adhesion for leading to orientation silicon steel is poor.
Most of research is devoted to develop the minute surface high magnetic induction grain-oriented silicon steel of no bottom at present.Such as Chinese Patent Application No.
For the document of CN201010518037.5, a kind of annealing isolation for preparing the mirror surface-oriented silicon steel with fine magnetic property is disclosed
Agent, composition by weight percent are:Al2O3Powder 77~98%, alkaline earth metallic oxide powder end 1~8%, alkali metal chloride
Or/and alkaline earth metal chloride 1~15%.The annealing separating agent of the invention makes high-temperature annealing process light plate surface not form glass
Glass film bottom, while the embedded oxide of the corrosion reaction removal substrate near surface using chloride, so as to obtain surface light
The product that clean and magnetic property is stablized.Chinese Patent Application No. is the document of CN201110299949.2, is disclosed with excellent magnetic
The mirror surface-oriented silicon steel manufacturing method of performance, annealing separating agent composition quality percentage are:Al2O3Powder, 65-96 parts, silicic acid
Salt powder, 2-15 parts, grain size is between 0.1-100 μm, alkaline earth oxide, 1-10 parts, metal chloride, 1-10 parts;
Wherein, silicate powder includes Al4(SiO4)3、CaSiO3、Mg2SiO4、Fe2SiO4In more than one;Metal chloride includes alkali
Metal chloride LiCl, NaCl, KCl, RbCl, alkaline earth metal chloride BeCl2、MgCl2、CaCl2、SrCl2、BaCl2Middle one kind
More than;Alkaline earth oxide includes one or more of BeO, MgO, CaO, SrO, BaO;It is mixed after drying in atmosphere for nitrogen hydrogen
Close gas, 25%~100%H2、D.P. <0 DEG C, temperature carries out heat preservation 15 hours or more under conditions of being 1150~1250 DEG C
High annealing anneals to obtain the minute surface grain-oriented silicon-iron product of excellent magnetic using painting insulating coating and stretching and leveling.But
The poor and traditional production technology of the mirror surface-oriented silicon steel insulation performance and surface quality of this no bottom and insulating coating solution are difficult
Meet the orientation silicon steel for producing this no bottom, R&D costs and production cost are higher.
The formation of bottom is by being formed when the MgO in annealing separating agent and decarburizing annealing mainly containing SiO2Oxidation
Object film reaction forms forsterite film, normally referred to as glass film reaction(2MgO+ SiO2 → Mg2SiO4).MgO is in certain item
It may become extremely active under part, hydration reaction MgO → Mg (OH)2It may occur under certain mixing and stirring state.
Therefore steam generates dew point between plate and plate and improves i.e. so as to be brought into coiled material, the atmosphere in length and width direction is uneven
Even problem.In addition, the type and quantity of additive greatly influence the quality and quantity of glass-film, this depends on excessive oxygen
In the presence of and reaction accelerate effect.
Invention content
The present invention is in view of the deficienciess of the prior art, offer one kind makes under the premise of ensureing to be orientated steel plate magnetic property
Bottom layer quality and insulation performance are more excellent, and reduce high magnetic induction grain-oriented silicon steel annealing separating agent and the preparation of product concession rate
Method.
Realize the measure of above-mentioned purpose:
A kind of high magnetic induction grain-oriented silicon steel annealing separating agent, raw material composition and weight percent content are:TiO2:1~
6%, Sb2(SO4)3:0.1 ~ 2 %, remaining is MgO;External adding water, amount of water is according to MgO:Water=1:8~15;Annealing separating agent simultaneously will
Meet:Mg(OH)2Amount<1.5 %, dried amount of moisture control is 2% hereinafter, igloss is less than 0.5%, CAA values at 1000 DEG C>
200 sec, granularity D50< 5μm.
It is:It is suitable for components and weight percent content to be: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 is carried out by the orientation silicon steel hot rolled plate of Fe and inevitable impurity after cold rolling using during decarburizing annealing
Interleaving agent.
A kind of preparation method of high magnetic induction grain-oriented silicon steel annealing separating agent, step:
1)MgO is mixed with water, the additional proportion of MgO and water is according to 1:8 ~ 15 carry out, and stir full and uniform;Control
Mg (OH) processed2Amount< 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(SO4)3,And it stirs;
4)Sb2(SO4)3It is further continued for stirring after addition, the time is no less than 2 hours;
5)For use.
It is:Stirring is using the strong mixing mode not less than 4000 rpm/min.
High magnetic induction grain-oriented silicon steel used in the present invention, i.e., the C of % by weight: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% is used as basis, since the fusing point of Sn or Sb elements that it contains is relatively low, in secondary recrystallization mistake
Cheng Zhong, Sn or Sb in steel can generate vaporization, and generated gas is spread from surface of steel plate, so as to easily in bottom/steel of steel plate
The interface heap of plate surface comes.Thus, the present invention is by by lot of experiments, obtaining and TiO being added in interleaving agent2
And Sb2(SO4)3, be conducive to MgO and form bottom earlier in high annealing temperature-rise period, make inhibitor in steel more stable, promote
Into the inhibiting effect of AlN, and be conducive to improve B8。
Why the present invention takes the strong mixing mode not less than 4000 rpm/min, so that MgO is abundant under strong agitation
Aquation contributes to the bonding of bottom after high annealing, that is, improves bottom adhesion.
In addition, control MgO generation Mg (OH)2Amount<1.5 %, the amount of moisture control brought into after annealing separating agent is dried exist
2% hereinafter, igloss is less than 0.5% at 1000 DEG C, so that annealing separating agent can effectively prevent decomposites water of constitution in high annealing
And make steel band peroxidating, destroy magnetic property.
Why MgO granularities are controlled in D50<It 5 μm, so that MgO slurries are uniformly dispersed when mixing with water, is not easy to coagulate
It is poly-, so as to which the bottom layer quality formed is good.
Compared with prior art, the present invention not only magnetic induction performance and bottom layer quality are excellent for high magnetic induction grain-oriented silicon steel, but also absolutely
Edge performance is good, suitable for the requirement of high power capacity transformer, while can also reduce the concession rate of product.
Specific embodiment
The present invention is described in detail below:
Table 1 is the raw material of various embodiments of the present invention and comparative example composition and content list;
Table 2 is various embodiments of the present invention and the main technologic parameters comparative example of comparative example;
Table 3 is the performance test results list of each embodiment of invention and comparative example.
Various embodiments of the present invention are produced according to following steps:
1)MgO is mixed with water, the additional proportion of MgO and water is according to 1:8 ~ 15 carry out, and stir full and uniform;Control
Mg (OH) processed2Amount< 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(SO4)3,And it stirs;
4)Sb2(SO4)3It is further continued for stirring after addition, the time is no less than 2 hours;
5)For use.
The data of each embodiment not correspond in table 1 and table 2.
The raw material of 1 various embodiments of the present invention of table and comparative example forms and content list (wt%)
The main technique list of 2 various embodiments of the present invention of table and comparative example
The performance test results of 3 various embodiments of the present invention of table and comparative example
Explanation:The differentiation of the annealing separating agent adhesion of the present invention is the result obtained according to GB/T2522-1988.
It is for component and weight percent content 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 the orientation silicon steel hot rolled plate of Fe and inevitable impurity through cold rolling, carry out decarburizing annealing after,
After the coating present invention limits the annealing separating agent of index and technological parameter, there is excellent bottom and high magnetic strength.
Present embodiment is only the best example, not to the restricted implementation of technical solution of the present invention.
Claims (2)
1. a kind of high magnetic induction grain-oriented silicon steel annealing separating agent, raw material composition and weight percent content are:TiO2:1 ~ 6%,
Sb2(SO4)3:0.1 ~ 0.35 %, remaining is MgO;External adding water, amount of water is according to MgO:Water=1:8~15;Annealing separating agent simultaneously will
Meet:Mg(OH)2Amount<1.5 %, dried amount of moisture control is 2% hereinafter, igloss is less than 0.5%, CAA values at 1000 DEG C>
200 sec, granularity D50< 5μm;
Preparation method:
1)MgO is mixed with water, the additional proportion of MgO and water is according to 1:8 ~ 15 carry out, and stir 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 ~ 0.35%2(SO4)3, and stir;
4)Sb2(SO4)3It is further continued for stirring after addition, the time is no less than 2 hours;
5) it is for use;
The stirring is using the strong mixing mode not less than 4000 rpm/min.
2. a kind of high magnetic induction grain-oriented silicon steel annealing separating agent as described in claim 1, it is characterised in that:It is suitable for components
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%, surplus is by Fe and can not
Interleaving agent when the orientation silicon steel hot rolled plate of impurity being avoided to carry out decarburizing annealing after cold rolling.
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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 |
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 |
CN113981196B (en) * | 2021-11-02 | 2023-07-28 | 无锡普天铁心股份有限公司 | Annealing isolating agent 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 |
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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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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