CN113981196B - Annealing isolating agent for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof - Google Patents

Annealing isolating agent for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof Download PDF

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CN113981196B
CN113981196B CN202111291459.8A CN202111291459A CN113981196B CN 113981196 B CN113981196 B CN 113981196B CN 202111291459 A CN202111291459 A CN 202111291459A CN 113981196 B CN113981196 B CN 113981196B
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蔡子祥
闫成亮
许庆松
叶芹
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Wuxi Putian Iron Core Co Ltd
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    • 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
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    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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Abstract

The invention discloses an annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer, and a preparation method and application thereof. The annealing isolating agent comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 1.9 to 40 percent of boric acid, 0.05 to 0.1 percent of Na 2 O 1～5％，Sb 2 (SO 4 ) 3 1 to 5 percent. The annealing isolating agent prepared by the invention improves the yield of the ultrahigh magnetic induction oriented silicon steel; the adhesion of the bottom layer of the oriented silicon steel is improved, and the yield rate of the product is reduced; the prepared ultra-high magnetic induction oriented silicon steel can meet the use requirement of a high-capacity transformer.

Description

Annealing isolating agent for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof
Technical Field
The invention relates to the technical field of preparation of oriented silicon steel annealing isolating agents, in particular to an annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer, and a preparation method and application thereof.
Background
The oriented silicon steel is used as a magnetic iron core material in a large quantity, the social requirements for energy conservation and resource conservation are increasingly eager in recent years, the requirements for reducing the iron loss and improving the magnetization characteristic of the oriented silicon steel are also strong, and the oriented silicon steel is highly expected to further improve the magnetic induction intensity in the motor design, so that the oriented silicon steel is beneficial to saving the cost of electric appliances.
To obtain oriented silicon steel having a high magnetic flux density, sb, sn or Bi is optionally added to the steel sheet. However, bi prevents formation of a glass film underlayer, and the glass film cannot be formed stably in the width direction, so that the adhesion of the ultra-high magnetic induction oriented silicon steel underlayer is poor.
ZL201410611409.7 proposes a production process of Bi-containing high magnetic induction oriented silicon steel with excellent bottom layer. The method mainly controls the formation time of the bottom layer by adjusting the high-temperature annealing process, but the change of temperature and atmosphere can influence the production process, and certain difficulty is brought to field implementation.
The annealing isolating agent for high magnetic induction oriented silicon steel is aimed at the annealing isolating agent for oriented silicon steel containing Sn or Sb, but is not suitable for the ultra-high magnetic induction oriented silicon steel added with Bi, because Bi is an effective inhibitor like AlN in a steel plate, bi contributes to the improvement of magnetic induction, but has adverse effect on the generation of a glass film.
The existing preparation of the ultra-high magnetic induction oriented silicon steel is difficult to generate an excellent bottom layer, so that the yield is low, the insulating property is poor, and the ultra-high magnetic induction oriented silicon steel is not beneficial to use in transformers and motors. Therefore, a special annealing isolating agent needs to be found to help improve the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel and solve the problem of the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an annealing isolating agent for improving the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel, and a preparation method and application thereof. According to the annealing isolating agent disclosed by the invention, non-hydrated magnesium oxide is adopted as a main component, and the indexes of magnesium oxide and additives in the annealing isolating agent are controlled, so that the prepared annealing isolating agent effectively improves the adhesion of the bottom layer of the ultrahigh magnetic induction oriented silicon steel.
The technical scheme of the invention is as follows:
an annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 1.9 to 40 percent of boric acid, 0.05 to 0.1 percent of Na 2 O 1～5％， Sb 2 (SO 4 ) 3 1～5％。
Further, the MgO is non-hydrated MgO; the CAA activity value of MgO is 180-300 s, and the burning loss is less than 1.3% at 1000 ℃.
Further, the CAA activity value of MgO is 180-220 s, and the burning loss is less than 1.0% at 1000 ℃.
Further, the particle size of MgO is 0.01-3 mu m;
further, the MgO has a particle size of 2.3 to 3. Mu.m.
The preparation method of the annealing isolating agent comprises the following steps:
(1) MgO mass is standard, and according to mass percent, tiO 1.9-40 percent 2 Boric acid 0.05-0.1% and Na 1-5% 2 O, 1-5% of Sb 2 (SO 4 ) 3 Adding the mixture into water, and stirring to obtain a mixture;
(2) And (3) adding 100% of MgO into the mixture in the step (1), and stirring to obtain the annealing separator.
Further, in the preparation process of the annealing isolating agent, the temperature is controlled to be 23-25 ℃.
Further, the stirring speed in the step (1) is 2500-3500 rpm, and the time is 1-2 h; the mass ratio of the water to MgO is 8-12: 1.
further, the stirring speed in the step (2) is 1500-3000 rpm, and the stirring time is 2-3 h.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
Further, the annealing isolating agent is coated on the surface of the ultrahigh magnetic induction oriented silicon steel; the coating amount is 3-5 g/m 3 . Controlling Mg (OH) generation in the coating residual liquid during coating 2 Measuring amount<5%. The residual liquid is prepared liquid which is pumped from a using tank to a coating machine for coating, the redundant liquid is coated residual liquid which flows back to the using tank, the using tank is provided with a cooling coil for cooling, the coating liquid is recycled, and the newly prepared coating liquid is added when the coating liquid is used up.
Further, the coating amount of the annealing separator and TiO in the annealing separator 2 The mass fraction of the magnesium oxide satisfies the following formula:
2*A 1/2 +5≤B*C≤200
wherein, the content of Bi in the oriented silicon steel raw material is ppm; B. TiO (titanium dioxide) 2 The mass of the magnesium oxideThe mass fraction,%; C. coating amount of annealing separator, g/m 2 。
Further, the percentage content of Bi in the raw materials in the ultrahigh magnetic induction oriented silicon steel is 0.0005% -0.01%; the percentage content of Sn in the raw material is 0.05-0.25%.
Further, the annealing isolating agent is coated on the ultrahigh magnetic induction oriented silicon steel, and the preparation steps of the ultrahigh magnetic induction oriented silicon steel are as follows: 0.04 to 0.08 percent of C, 3.14 to 3.4 percent of Si, 0.06 to 0.12 percent of Mn, 0.02 to 0.03 percent of S and Als: 0.02-0.03%, N:0.006 to 0.01 percent, bi:0.0005 to 0.01 percent, sn:0.01 to 0.06 percent of oriented silicon steel hot rolled plate which is used as basic components and the balance of Fe and unavoidable impurities is subjected to decarburization annealing after cold rolling to obtain the ultrahigh magnetic induction oriented silicon steel.
The beneficial technical effects of the invention are as follows:
(1) The invention aims at optimizing the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel containing 0.0005-0.01% of Bi and 0.05-0.25% of Sn, and the annealing isolating agent capable of improving the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel is prepared by controlling the content of magnesium oxide and the amount of additives in the annealing isolating agent.
(2) According to the annealing isolating agent prepared by the invention, through the addition of boric acid and the limitation of the relative dosage, B which is decomposed by boric acid can infiltrate into steel to form BN, so that overlarge secondary grains are inhibited, and meanwhile, the steel is prevented from absorbing excessive N, and the quality and magnetism of a bottom layer are improved; na (Na) 2 The addition of O is beneficial to reducing the melting point of the glass film, accelerating the initial generation time of the bottom layer, facilitating the formation of the bottom layer and improving B 8 The method comprises the steps of carrying out a first treatment on the surface of the Adding Sb 2 (SO 4 ) 3 Can help the absorption of Bi in the bottom layer of the steel plate, and Bi plays the role of an inhibitor in the steel plate like AlN, so Sb is added 2 (SO 4 ) 3 Increase Bi in the surface layer and enhance the inhibition force, B 8 Heightening; by controlling the addition amount, the excessive addition amount can prevent the Bi content from being excessively high, and the Bi generates gasification to influence the formation of the bottom layer during secondary recrystallization.
(3) The invention establishes the adding amount of titanium dioxide and the annealing proportion and coatsThe amount inequality determines the reasonable titanium dioxide addition amount and the coating amount of the steel plate surface isolating agent, and the addition of the titanium dioxide is beneficial to the magnesium oxide to form a bottom layer earlier in the high-temperature annealing and heating process, so that the inhibitor in the steel is more stable, and the B is improved 8 The method comprises the steps of carrying out a first treatment on the surface of the The generation amount of water in the high-temperature annealing process can be regulated by controlling the content of titanium dioxide, so that the magnetic induction B of the steel plate is improved 8 。
(4) The annealing isolating agent prepared by the invention improves the yield of the ultrahigh magnetic induction oriented silicon steel; meanwhile, the adhesiveness of the bottom layer of the oriented silicon steel is improved, and the yield rate of products is reduced; the prepared ultra-high magnetic induction oriented silicon steel can meet the use requirement of a high-capacity transformer.
Detailed Description
The present invention will be specifically described with reference to examples.
Example 1
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 2.0%, boric acid 0.05%, na 2 O 5％，Sb 2 (SO 4 ) 3 1%. The MgO is non-hydrated MgO, and the grain size is 2.5 mu m; the CAA activity value of MgO is 182s, and the burning loss is 1.0% at 1000 ℃. .
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 2.0 percent of TiO according to the weight percentage 2 Boric acid 0.05%, na 5% 2 O, 1% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass equal to 8 times of MgO, and stirring at 2500r/min for 1.5 hours to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 3 hours at 2500r/min to obtain the annealing isolating agent.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.04% of C, 3.14% of Si, 0.06% of Mn, 0.02% of S and Als:0.02%, N:0.006%, bi:0.0005%, sn:0.01% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet was subjected to decarburization annealing after cold rolling, and the annealing separator prepared in this example was coated in an amount of 3g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 4.9%.
TiO in annealing separator 2 The addition amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1):
2*A 1/2 +5≤B*C≤200(1)
wherein A is Bi content, ppm; b is TiO 2 The weight percentage of MgO is percent; c represents the coating amount of the release agent on each surface of the steel plate, g/m 2 。
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 2
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 5%, boric acid 0.1%, na 2 O 1％，Sb 2 (SO 4 ) 3 5%. The MgO is non-hydrated MgO, and the grain diameter is 3.0 mu m; the CAA activity value of MgO is 180s, and the burning loss is 0.85% at 1000 ℃. .
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 5.0 percent of TiO according to the weight percentage 2 Boric acid 0.1%, na 1% 2 O, 5% Sb 2 (SO 4 ) 3 Adding inStirring in water with the mass of 9 times of MgO at 2500r/min for 1h to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 3 hours at 1500r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.08% of C, 3.14% of Si, 0.08% of Mn, 0.025% of S and Als:0.02%, N:0.006%, bi:0.0010%, sn:0.06% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet is subjected to decarburization annealing after cold rolling, and the annealing separator prepared in the embodiment is coated, wherein the single-sided coating amount is 5g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 2.8%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 3
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 26%, boric acid 0.06%, na 2 O 3％，Sb 2 (SO 4 ) 3 2%. The MgO is non-hydrated MgO, and the grain size is 2.9 mu m; the CAA activity value of MgO is 290s, and the burning loss is 0.88% at 1000 ℃. .
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to be 23 ℃, and mixing 26% of TiO according to weight percentage 2 Boric acid 0.06%, na 3% 2 O, 2% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is equivalent to 10 times of MgO, and stirring at 3500r/min for 1h to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 3000r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.06 percent of C, 3.4 percent of Si, 0.12 percent of Mn, 0.03 percent of S and Als:0.03%, N:0.01%, bi:0.0030%, sn:0.01% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet was subjected to decarburization annealing after cold rolling, and the annealing separator prepared in this example was coated in an amount of 4g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 4.5%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 4
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 35%, boric acid 0.07%, na 2 O 4％，Sb 2 (SO 4 ) 3 3%. The MgO is non-hydrated MgO, and the grain diameter is 2.6 mu m; the CAA activity value of MgO is 200s, and the burning loss is 0.95% at 1000 ℃. .
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 35 percent of TiO according to weight percentage 2 Boric acid 0.07% and Na 4% 2 O, 3% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is 11 times of that of MgO, and stirring at 3500r/min for 2 hours to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 3000r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.05% of C, 3.2% of Si, 0.08% of Mn, 0.025% of S and Als:0.024%, N:0.008%, bi:0.0050%, sn: 0.02% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet was subjected to decarburization annealing after cold rolling, and the annealing separator prepared in this example was coated in an amount of 3g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 4.0%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 5
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 40%, boric acid 0.08%, na 2 O 5％，Sb 2 (SO 4 ) 3 4%. The MgO is non-hydrated MgO, and the grain diameter is 2.8 mu m; the CAA activity value of MgO is 195s, and the burning loss is 0.9% at 1000 ℃. .
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to be 24 ℃, and adding 40% of TiO according to weight percentage 2 Boric acid 0.08%, na 5% 2 O, 4% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is 12 times of that of MgO, and stirring for 1h at 3000r/min to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 2000r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.05% of C, 3.3% of Si, 0.09% of Mn, 0.026% of S, als:0.028%, N:0.009%, bi:0.0060%, sn: 0.05% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet was subjected to decarburization annealing after cold rolling, and the annealing separator prepared in this example was coated in an amount of 4g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 3.5%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 6
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 10%, boric acid 0.09%, na 2 O 2％，Sb 2 (SO 4 ) 3 2.5%. The MgO is non-hydrated MgO with a grain size of 2.5μm; the CAA activity value of MgO is 260s, and the burning loss is 0.78% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and mixing 10% of TiO according to weight percentage 2 Boric acid 0.09%, na 2% 2 O, 2.5% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass equivalent to 10 times of MgO, and stirring at 2800r/min for 1.5h to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 2500r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.07% of C, 3.24% of Si, 0.10% of Mn, 0.025% of S and Als:0.025%, N:0.009%, bi:0.0070%, sn:0.04% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet is subjected to decarburization annealing after cold rolling, and the annealing separator prepared in the embodiment is coated, wherein the single-sided coating amount is 5g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 3.2%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 7
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 20%, boric acid 0.1%, na 2 O 1％，Sb 2 (SO 4 ) 3 1.5%. The MgO is non-hydrated MgO, and the grain diameter is 2.3 mu m; the CAA activity value of MgO is 300s, and the burning loss is 0.7% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to be 24 ℃, and mixing 20% of TiO according to weight percentage 2 Boric acid 0.1%, na 1% 2 O, 1.5% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass equal to 8 times of MgO, and stirring for 1h at 3000r/min to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 2500r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.08% of C, 3.4% of Si, 0.12% of Mn, 0.026% of S, als:0.022%, N:0.0062%, bi:0.0080%, sn:0.06% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet was subjected to decarburization annealing after cold rolling, and the annealing separator prepared in this example was coated in an amount of 3g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 1.8%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Example 8
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass of MgO is taken as a standard,the mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 14%, boric acid 0.05%, na 2 O 1.5％，Sb 2 (SO 4 ) 3 3.5%. The MgO is non-hydrated MgO, and the grain size is 2.9 mu m; the CAA activity value of MgO is 196s, and the burning loss is 0.8% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 14% of TiO according to weight percentage 2 Boric acid 0.05%, na 1.5% 2 O, 3.5% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass of 9 times of MgO, and stirring at 2900r/min for 2 hours to obtain a mixture;
(2) MgO is added into the mixture in the step (1), and the mixture is stirred for 3 hours at 2800r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.07% of C, 3.24% of Si, 0.11% of Mn, 0.027% of S, als:0.021%, N:0.01%, bi:0.0100%, sn:0.06% as a basic component, the balance being Fe and unavoidable impurities.
The oriented silicon steel hot rolled sheet is subjected to decarburization annealing after cold rolling, and the annealing separator prepared in the embodiment is coated, wherein the single-sided coating amount is 5g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 2.4%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Comparative example 1
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 45%, boric acid 0%, na 2 O 0％，Sb 2 (SO 4 ) 3 0.9%. The MgO is non-hydrated MgO, and the grain diameter is 3.1 mu m; the CAA activity value of MgO is 310s, and the burning loss is 1.4% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 45% of TiO according to weight percentage 2 Boric acid 0%, na 0% 2 O, 0.9% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is 8 times of that of MgO, and stirring at 3500r/min for 2 hours to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 3 hours at 1500r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.04% of C, 3.14% of Si, 0.06% of Mn, 0.02% of S and Als:0.02%, N:0.006%, bi:0.0070%, sn:0.01% as a basic component, the balance being Fe and unavoidable impurities.
The annealing separator prepared in this comparative example was applied to a hot rolled oriented silicon steel sheet, which was decarburized after cold rolling, in an amount of 5g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 5%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, do not satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Comparative example 2
Oriented silicon steel capable of improving ultrahigh magnetic inductionAn annealing isolating agent for the bottom layer quality, wherein the annealing isolating agent comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 1.0%, boric acid 0.12%, na 2 O 5％，Sb 2 (SO 4 ) 3 5%. The MgO is non-hydrated MgO, and the grain size is 3.5 mu m; the CAA activity value of MgO is 175s, and the burning loss is 1.5% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to 25 ℃, and adding 2.0 percent of TiO according to the weight percentage 2 Boric acid 0.05%, na 5% 2 O, 1% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is 12 times of that of MgO, and stirring for 1h at 2500r/min to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 3 hours at 1500r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.08% of C, 3.4% of Si, 0.12% of Mn, 0.02% of S, als:0.02%, N:0.006%, bi:0.0080%, sn:0.01% as a basic component, the balance being Fe and unavoidable impurities.
The annealing separator prepared in this comparative example was applied to a hot rolled oriented silicon steel sheet, which was decarburized after cold rolling, in an amount of 3g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 5%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, do not satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Comparative example 3
An annealing isolating agent for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer comprises the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 20%, boric acid 0.12%, na 2 O 5％，Sb 2 (SO 4 ) 3 5%. The MgO is MgO which is difficult to be water and has the particle size of 3.5 mu m; the CAA activity value of MgO is 175s, and the burning loss is 1.5% at 1000 ℃.
The preparation method of the annealing isolating agent comprises the following steps:
(1) Controlling the temperature of the preparation process to be 24 ℃, and mixing 20% of TiO according to weight percentage 2 Boric acid 0.12%, na 5% 2 O, 5% Sb 2 (SO 4 ) 3 Adding the mixture into water with the mass which is 9 times of that of MgO, and stirring at 3500r/min for 2 hours to obtain a mixture;
(2) MgO is added into the mixture in the step (1) and stirred for 2 hours at 1000r/min to obtain the annealing separator.
The application of the annealing isolating agent is that the annealing isolating agent is used for ultrahigh magnetic induction oriented silicon steel.
The ultra-high magnetic induction oriented silicon steel disclosed by the invention comprises the following raw materials in percentage by mass: 0.08% of C, 3.4% of Si, 0.12% of Mn, 0.03% of S and Als:0.03%, N:0.01%, bi:0.0080%, sn:0.06% as a basic component, the balance being Fe and unavoidable impurities.
The annealing separator prepared in this comparative example was applied to a hot rolled oriented silicon steel sheet, which was decarburized after cold rolling, in an amount of 3g/m 3 Controlling the generation of Mg (OH) in the coating residual liquid during coating 2 The amount was 6.5%.
TiO in annealing separator 2 The amount of the additive, and the coating amount of the annealing separator, do not satisfy the requirement of the formula (1) described in example 1.
And (3) drying the steel plate coated with the annealing isolating agent, performing high-temperature annealing to form a glass film bottom layer, and then coating an insulating coating to perform stretching leveling annealing to obtain a final product.
Test case
The final products prepared in examples 1 to 8, comparative examples 1 to 3 were subjected to performance tests, in which adhesion was determined according to GB/T2522-1988; the magnetic induction, i.e. the iron loss, was measured by GB/T3655-2008 and the performance test of the final product is shown in Table 1:
TABLE 1
As is clear from Table 1, examples 1 to 8 were prepared by controlling TiO in MgO release agent 2 The content satisfies the following relational expression (1) with the Bi content and the MgO coating weight in the steel sheet. TiO as in MgO release agent 2 When the content of Bi and the MgO coating weight in the steel plate meet the following relational expression (1), mgO is facilitated to form a bottom layer earlier in the high-temperature annealing and heating process, the starting time of the bottom layer is shortened, the forming thickness of the bottom layer is increased, the adhesiveness of the bottom layer is improved, meanwhile, an inhibitor in the steel is more stable, the inhibition effect of AlN is promoted, and the magnetic induction B is facilitated to be improved 8 . Control of Mg (OH) in MgO coating fluid using non-hydrated MgO at the same time 2 Measuring amount<5%, ignition at 1000 ℃ is reduced by less than 1%, thereby controlling H 2 The amount of O accelerates the generation starting time of the bottom layer, and is favorable for the adhesion of the bottom layer. Magnetic induction B of annealed spacer-coated steel sheet prepared in the examples of the present application 800 More than 1.94T, the iron loss is obviously reduced compared with the comparative example.
As is clear from Table 1, in comparative example 1, na was not added 2 O and boric acid are not favorable for reducing the formation temperature of the bottom layer, and for Bi-containing oriented silicon steel, the bottom layer is not formed, so that the bottom layer is not formed or is easy to fall off after the release agent is coated. In comparative example 2, tiO in MgO spacer 2 Excessive content ofThe formation of the bottom layer is not utilized in the case of the Bi-containing oriented silicon steel, and therefore, after the release agent is coated, the bottom layer is not formed or is easy to fall off. In comparative example 3, mgO, which is difficult to be water-compatible, was used, and Mg (OH) generated in MgO 2 The content is more than 5 percent, which is unfavorable for secondary recrystallization of Bi-containing oriented silicon steel, reduces the magnetism of the steel plate, and the steel plate B 8 The value is below 1.94T.
The foregoing is merely a preferred embodiment of the invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the principles of the invention, and these modifications and variations should also be considered as being within the scope of the invention.

Claims (10)

1. The annealing isolating agent for improving the quality of the bottom layer of the ultra-high magnetic induction oriented silicon steel is characterized by comprising the following components: mgO, tiO 2 Boric acid, na 2 O、Sb 2 (SO 4 ) 3 The method comprises the steps of carrying out a first treatment on the surface of the The mass percentage of the rest components relative to MgO is as follows: tiO (titanium dioxide) 2 1.9 to 40 percent of boric acid, 0.05 to 0.1 percent of Na 2 O 1～5％，Sb 2 (SO 4 ) 3 1～5％；
The ultra-high magnetic induction oriented silicon steel comprises the following raw materials in percentage by mass: 0.04 to 0.08 percent of C, 3.14 to 3.4 percent of Si, 0.06 to 0.12 percent of Mn, 0.02 to 0.03 percent of S, als: 0.02-0.03%, N:0.006 to 0.01 percent, bi:0.0005 to 0.01 percent, sn:0.01 to 0.06 percent of the alloy is taken as a basic component, and the balance is Fe and unavoidable impurities.
2. The annealing separator of claim 1, wherein the MgO is non-hydrated MgO; the CAA activity value of MgO is 180-300 s, and the burning loss is less than 1.3% at 1000 ℃.
3. The annealing separator of claim 1, wherein MgO has CAA activity value of 180 to 220s and a burn off at 1000 ℃ of < 1.0%.
4. The annealing separator according to claim 1, wherein the MgO has a particle size of 0.01 to 3 μm.
5. A method of preparing the annealing separator of claim 1, comprising the steps of:
(1) MgO mass is standard, and according to mass percent, tiO 1.9-40 percent 2 Boric acid 0.05-0.1% and Na 1-5% 2 O, 1-5% of Sb 2 (SO 4 ) 3 Adding the mixture into water, and stirring to obtain a mixture;
(2) And (3) adding 100% of MgO into the mixture in the step (1), and stirring to obtain the annealing separator.
6. The method according to claim 5, wherein the stirring speed in the step (1) is 2500 to 3500rpm for a period of 1 to 2 hours; the mass ratio of the water to MgO is 8-12: 1.
7. the process according to claim 5, wherein the stirring speed in the step (2) is 1500 to 3000rpm for 2 to 3 hours.
8. Use of an annealing separator according to any one of claims 1 to 4, characterized in that the annealing separator is used for ultra-high magnetic induction oriented silicon steel.
9. The use according to claim 8, wherein the annealing separator is coated on the surface of the ultra-high magnetic induction oriented silicon steel; the coating amount is 3-5 g/m 2 。
10. The use according to claim 9, wherein the annealing separator is coated in an amount corresponding to the amount of TiO in the annealing separator 2 The mass fraction of the magnesium oxide satisfies the following formula:
2*A 1/2 +5≤B*C≤200
wherein A is oriented siliconBi content in the steel raw material, ppm; B. TiO (titanium dioxide) 2 The mass percent of the magnesium oxide is calculated; C. coating amount of annealing separator, g/m 2 。
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