CN113981196A - Annealing separant for improving quality of ultrahigh magnetic induction oriented silicon steel bottom layer and preparation method and application thereof - Google Patents

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

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CN113981196A
CN113981196A CN202111291459.8A CN202111291459A CN113981196A CN 113981196 A CN113981196 A CN 113981196A CN 202111291459 A CN202111291459 A CN 202111291459A CN 113981196 A CN113981196 A CN 113981196A
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CN113981196B (en
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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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    • C21—METALLURGY OF IRON
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    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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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 separant for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel and a preparation method and application thereof. The annealing release agent comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 221.9-40%, boric acid 0.05-0.1%, Na2O 1～5％，Sb2(SO4)31 to 5 percent. The annealing separant prepared by the method improves the yield of the ultrahigh magnetic induction oriented silicon steel; the bottom layer adhesiveness of the oriented silicon steel is improved, and the yield of the product is reduced; the prepared ultrahigh magnetic induction oriented silicon steel can meet the use requirement of a high-capacity transformer.

Description

Annealing separant 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 separant, in particular to an annealing separant for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer and a preparation method and application thereof.
Background
Oriented silicon steel is widely used as a magnetic iron core material, the social requirements on energy conservation and resource conservation are increasingly urgent in recent years, the requirements on reducing the iron loss and improving the magnetization characteristic of the oriented silicon steel are strong, and in the design of a motor, the further improvement of the magnetic induction intensity is urgently desired, so that the cost of an electric appliance is saved.
Sb, Sn or Bi is optionally added to the steel sheet in order to obtain oriented silicon steel with high magnetic flux density. However, Bi inhibits the formation of the bottom layer of the glass film, and thus the glass film cannot be stably formed in the width direction, and thus the adhesion of the bottom layer of the ultra-high magnetic induction oriented silicon steel is poor.
ZL201410611409.7 proposes a method for producing Bi-containing high magnetic induction oriented silicon steel with an excellent bottom layer. The method mainly controls the time for forming the bottom layer by adjusting the high-temperature annealing process, but the change of the temperature and the atmosphere can influence the production process and bring certain difficulty to the field implementation.
The annealing separating agent for high-magnetic induction oriented silicon steel is an annealing separating agent for oriented silicon steel containing Sn or Sb, but is not suitable for ultrahigh-magnetic induction oriented silicon steel added with Bi, because Bi is the same as AlN in a steel plate and is an effective inhibitor, the Bi is beneficial to improving the magnetic induction, but has adverse effect on the generation of a glass film.
At present, the ultrahigh 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 ultrahigh magnetic induction oriented silicon steel is not beneficial to being used in transformers and motors. Therefore, a special annealing separant needs to be found to help improve the quality of the bottom layer of the ultrahigh magnetic induction oriented silicon steel and solve the problem of the quality of the bottom layer of the ultrahigh magnetic induction oriented silicon steel.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an annealing separant for improving the quality of an ultrahigh magnetic induction oriented silicon steel bottom layer and a preparation method and application thereof. The annealing release agent provided by the invention adopts non-hydrated magnesium oxide as a main component, and the bottom layer adhesiveness of the ultrahigh magnetic induction oriented silicon steel is effectively improved by controlling the indexes and additives of magnesium oxide in the annealing release agent.
The technical scheme of the invention is as follows:
an annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 221.9-40%, boric acid 0.05-0.1%, Na2O 1～5％， Sb2(SO4)3 1～5％。
Further, the MgO is non-hydrated MgO; the CAA activity value of the MgO is 180-300 s, and the ignition loss at 1000 ℃ is less than 1.3%.
Furthermore, the CAA activity value of the MgO is 180-220 s, and the ignition loss at 1000 ℃ is less than 1.0%.
Further, the particle size of the MgO is 0.01-3 μm;
further, the particle size of the MgO is 2.3 to 3 μm.
The preparation method of the annealing release agent comprises the following steps:
(1) the MgO mass is taken as a standard, and 1.9-40% of TiO is added according to the mass percentage20.05 to 0.1 percent of boric acid and 1 to 5 percent of Na2O, 1-5% of Sb2(SO4)3Adding into water, stirring to obtain a mixture;
(2) and (2) adding 100% of MgO into the mixture obtained in the step (1), and stirring to obtain the annealing separant.
Further, in the preparation process of the annealing release 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 the MgO is 8-12: 1.
further, the stirring speed in the step (2) is 1500-3000 rpm, and the time is 2-3 h.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
Further, the annealing release agent is coated on the surface of the ultrahigh magnetic induction oriented silicon steel; the coating amount is 3-5 g/m3. During coating, the generation of Mg (OH) in the coating residual liquid is controlled2Measurement of<5 percent. The residual liquid is prepared by pumping the prepared liquid from a using tank to a coating machine for coating, flowing the redundant liquid, namely the coating residual liquid, back to the using tank, cooling the using tank by a cooling coil pipe, recycling the coating liquid, and adding the newly prepared coating liquid when the coating liquid is nearly used up.
Further, the coating amount of the annealing release agent and TiO in the annealing release agent2The magnesium oxide accounts for the mass fraction of the magnesium oxide and satisfies the following formula:
2*A1/2+5≤B*C≤200
wherein, the Bi content in the raw material of the oriented silicon steel A is ppm; B. TiO 22Accounts for the mass fraction of magnesium oxide,%; C. coating amount of annealing separator, g/m2。
Further, the percentage content of Bi in the ultrahigh magnetic induction oriented silicon steel in the raw material is 0.0005 to 0.01 percent; the percentage content of Sn in the raw material is 0.05-0.25%.
Further, the annealing release 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: 0.04-0.08% of C, 3.14-3.4% of Si, 0.06-0.12% of Mn, 0.02-0.03% of S, Als: 0.02-0.03%, N: 0.006-0.01%, Bi: 0.0005 to 0.01%, Sn: 0.01-0.06% of the grain-oriented silicon steel is used as a basic component, and the balance is Fe and inevitable impurities, and the grain-oriented silicon steel is cold-rolled and then subjected to decarburization annealing to obtain the ultrahigh magnetic induction grain-oriented silicon steel.
The beneficial technical effects of the invention are as follows:
(1) aiming at the quality optimization of the ultrahigh magnetic induction oriented silicon steel bottom layer containing 0.0005 to 0.01 percent of Bi and 0.05 to 0.25 percent of Sn, the annealing separating agent capable of improving the quality of the ultrahigh magnetic induction oriented silicon steel bottom layer is prepared by controlling the content of magnesium oxide in the annealing separating agent and the amount of additives.
(2) In the annealing release agent prepared by the invention, through the addition of boric acid and the limitation of the relative dosage, B decomposed by the boric acid permeates into steel to form BN, the secondary crystal grains are inhibited from being overlarge, meanwhile, the steel is prevented from absorbing excessive N, and the quality and magnetism of a bottom layer are improved; na (Na)2The addition of O is favorable for reducing the melting point of the glass film, quickening the initial generation time of the bottom layer, is favorable for the formation of the bottom layer and improves B8(ii) a Adding Sb2(SO4)3Can help the absorption of Bi in the bottom layer of the steel plate, and the Bi in the steel plate is used as an inhibitor like AlN, so Sb is added2(SO4)3B, when Bi in the surface layer is increased and the restraining force is enhanced8Heightening; by controlling the adding amount, the phenomenon that the Bi content is too high due to too high adding amount is prevented, and the Bi is gasified to influence the formation of a bottom layer during secondary recrystallization.
(3) According to the invention, the reasonable titanium dioxide addition amount and the coating amount of the steel plate surface separant are determined by establishing the inequality of the titanium dioxide addition amount, the annealing proportion and the coating amount, the titanium dioxide addition amount is beneficial to earlier formation of a bottom layer of magnesium oxide in the high-temperature annealing and heating process, so that the inhibitor in the steel is more stable, and thus the B content is improved8(ii) a By controlling the content of titanium dioxide, the generation amount of water in the high-temperature annealing process can be adjusted, so that the magnetic induction B of the steel plate is improved8。
(4) The annealing separant prepared by the method improves the yield of the ultrahigh magnetic induction oriented silicon steel; meanwhile, the bottom layer adhesiveness of the oriented silicon steel is improved, and the yield of the product is reduced; the prepared ultrahigh magnetic induction oriented silicon steel can meet the use requirement of a high-capacity transformer.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 222.0 percent, boric acid 0.05 percent and Na2O 5％，Sb2(SO4)31 percent. The MgO is non-hydrated MgO and has the particle size of 2.5 mu m; the CAA activity value of the MgO is 182s, and the ignition loss is 1.0 percent at 1000 ℃. .
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 25 ℃, and mixing 2.0 percent of TiO according to weight percentage20.05 percent of boric acid and 5 percent of Na2O, 1% of Sb2(SO4)3Adding water with the mass being 8 times of that of MgO, and stirring for 1.5h at 2500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 3 hours at the speed of 2500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.04% of C, 3.14% of Si, 0.06% of Mn, 0.02% of S, Als: 0.02%, N: 0.006%, Bi: 0.0005%, Sn: 0.01% as a basic component, and the balance consisting of Fe and unavoidable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 3g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 4.9%.
TiO in annealing release agent2The addition amount of the annealing release agent and the coating amount of the annealing release agent meet the requirement of a formula (1):
2*A1/2+5≤B*C≤200(1)
wherein A is the content of Bi in ppm; b is TiO2MgO in percentage by weight; c represents the coating weight of the release agent on each surface of the steel plate, and g/m2。
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 2
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 225%, boric acid 0.1%, Na2O 1％，Sb2(SO4)35 percent. The MgO is non-hydrated MgO and has a particle size of 3.0 μm; the CAA activity value of the MgO is 180s, and the ignition loss is 0.85% at 1000 ℃. .
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature in the preparation process to be 25 ℃, and mixing 5.0 percent of TiO according to weight percentage20.1% of boric acid and 1% of Na2O, 5% of Sb2(SO4)3Adding water with the mass equivalent to 9 times of MgO, and stirring for 1h at 2500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 3h at 1500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.08% of C, 3.14% of Si, 0.08% of Mn, 0.025% of S, Als: 0.02%, N: 0.006%, Bi: 0.0010%, Sn: 0.06% as a basic component, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 5g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 2.8%.
TiO in annealing release agent2The addition amount of (2) and the coating amount of the annealing separator satisfy those of example 1The requirement of the formula (1) is described.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 3
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2226%, boric acid 0.06%, Na2O 3％，Sb2(SO4)32 percent. The MgO is non-hydrated MgO and has the particle size of 2.9 mu m; the CAA activity of the MgO is 290s, and the ignition loss is 0.88% at 1000 ℃. .
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 23 ℃, and mixing 26 percent of TiO according to weight percentage20.06% of boric acid and 3% of Na2O, 2% of Sb2(SO4)3Adding water with the mass 10 times of that of MgO, and stirring for 1h at 3500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2h at 3000r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.06% of C, 3.4% of Si, 0.12% of Mn, 0.03% of S, Als: 0.03%, N: 0.01%, Bi: 0.0030%, Sn: 0.01% as a basic component, and the balance consisting of Fe and unavoidable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 4g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 4.5%.
AnnealingTiO in the release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 4
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2235%, boric acid 0.07%, Na2O 4％，Sb2(SO4)33 percent. The MgO is non-hydrated MgO and has the particle size of 2.6 mu m; the MgO has a CAA activity of 200s and a scorch reduction of 0.95% at 1000 ℃. .
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature in the preparation process to be 25 ℃, and mixing 35 percent of TiO according to weight percentage20.07% of boric acid and 4% of Na2O, 3% of Sb2(SO4)3Adding water with the mass being 11 times of that of MgO, and stirring for 2 hours at 3500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2h at 3000r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.05% of C, 3.2% of Si, 0.08% of Mn, 0.025% of S, Als: 0.024%, N: 0.008%, Bi: 0.0050%, Sn: 0.02% as a basic component, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 3g/m3When the coating is carried out,control of Mg (OH) formation in coating raffinate2The amount was 4.0%.
TiO in annealing release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 5
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2240%, boric acid 0.08%, Na2O 5％，Sb2(SO4)34 percent. The MgO is non-hydrated MgO and has the particle size of 2.8 mu m; the CAA activity value of the MgO is 195s, and the ignition loss is 0.9% at 1000 ℃. .
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 24 ℃, and mixing 40 percent of TiO according to weight percentage20.08 percent of boric acid and 5 percent of Na2O, 4% of Sb2(SO4)3Adding water with the mass being 12 times of that of MgO, and stirring for 1h at 3000r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2h at 2000r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of 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, and the balance consisting of Fe and inevitable impurities.
Cold rolling the hot rolled plate, decarbonizing, annealing and coatingThe annealing separator prepared in this example was coated on one side in an amount of 4g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 3.5%.
TiO in annealing release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 6
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2210%, boric acid 0.09%, Na2O 2％，Sb2(SO4)32.5 percent. The MgO is non-hydrated MgO and has the particle size of 2.5 mu m; the CAA activity value of the MgO is 260s, and the ignition loss is 0.78% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 25 ℃, and mixing 10 percent of TiO according to weight percentage20.09% of boric acid and 2% of Na2O, 2.5% of Sb2(SO4)3Adding water with the mass 10 times of that of MgO, and stirring for 1.5h at 2800r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2 hours at the speed of 2500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.07% of C, 3.24% of Si, 0.10% of Mn, 0.025% of S, Als: 0.025%, N: 0.009%, Bi: 0.0070%, Sn: 0.04% as a basic component, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 5g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 3.2%.
TiO in annealing release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 7
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2220%, boric acid 0.1%, Na2O 1％，Sb2(SO4)31.5 percent. The MgO is non-hydrated MgO and has the particle size of 2.3 mu m; the CAA activity value of the MgO is 300s, and the ignition loss is 0.7% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 24 ℃, and mixing 20 percent of TiO according to weight percentage20.1% of boric acid and 1% of Na2O, 1.5% of Sb2(SO4)3Adding water with the mass 8 times of that of MgO, and stirring for 1h at 3000r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2 hours at the speed of 2500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.08 percent of C, 3.4 percent of Si, 0.12 percent of Mn, 0.026 percent of S, Als: 0.022%, N: 0.0062%, Bi: 0.0080%, Sn: 0.06% as a basic component, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 3g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 1.8%.
TiO in annealing release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Example 8
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2214%, boric acid 0.05%, Na2O 1.5％，Sb2(SO4)33.5 percent. The MgO is non-hydrated MgO and has the particle size of 2.9 mu m; the CAA activity of the MgO is 196s, and the ignition is reduced by 0.8% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 25 ℃, and mixing 14 percent of TiO according to weight percentage20.05% of boric acid and 1.5% of Na2O, 3.5% of Sb2(SO4)3Adding water with the mass equivalent to 9 times of MgO, and stirring for 2 hours at 2900r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 3h at 2800r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of 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, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared in the embodiment, wherein the single-side coating amount is 5g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 2.4%.
TiO in annealing release agent2The amount of the annealing separator and the coating amount of the annealing separator satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Comparative example 1
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2245%, boric acid 0%, Na2O 0％，Sb2(SO4)30.9 percent. The MgO is non-hydrated MgO and has a particle size of 3.1 μm; the CAA activity value of the MgO is 310s, and the ignition loss is 1.4% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 25 ℃, and mixing 45 percent of TiO according to weight percentage20% of boric acid and 0% of Na2O, 0.9% of Sb2(SO4)3Adding water with the mass being 8 times of that of MgO, and stirring for 2 hours at 3500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 3h at 1500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.04% of C, 3.14% of Si, 0.06% of Mn, 0.02% of S, Als: 0.02%, N: 0.006%, Bi: 0.0070%, Sn: 0.01% as a basic component, and the balance consisting of Fe and unavoidable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared by the comparative example, wherein the single-side coating amount is 5g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount is 5%.
TiO in annealing release agent2The amount of (2) and the amount of the annealing separator applied do not satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Comparative example 2
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 221.0%, boric acid 0.12%, Na2O 5％，Sb2(SO4)35 percent. The MgO is non-hydrated MgO and has a particle size of 3.5 μm; the CAA activity value of the MgO is 175s, and the ignition loss is 1.5% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 25 ℃, and mixing 2.0 percent of TiO according to weight percentage20.05 percent of boric acid and 5 percent of Na2O, 1% of Sb2(SO4)3Adding water with the mass being 12 times of that of MgO into the mixture, and stirring the mixture for 1 hour at the speed of 2500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 3h at 1500r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of 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, and the balance consisting of Fe and unavoidable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared by the comparative example, wherein the single-side coating amount is 3g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount is 5%.
TiO in annealing release agent2The amount of (2) and the amount of the annealing separator applied do not satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Comparative example 3
An annealing release agent for improving the quality of a bottom layer of ultrahigh magnetic induction oriented silicon steel comprises the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking the mass of MgO as a standard, the mass percentages of the other components relative to MgO are as follows: TiO 2220%, boric acid 0.12%, Na2O 5％，Sb2(SO4)35 percent. The MgO is hardly water-soluble MgO and has a particle size of 3.5 μm; the CAA activity value of the MgO is 175s, and the ignition loss is 1.5% at 1000 ℃.
The preparation method of the annealing release agent comprises the following steps:
(1) controlling the temperature of the preparation process to be 24 ℃, and mixing 20 percent of TiO according to weight percentage20.12 percent of boric acid and 5 percent of Na2O, 5% of Sb2(SO4)3Adding water with the mass being 9 times of that of MgO, and stirring for 2 hours at 3500r/min to obtain a mixture;
(2) and (2) adding MgO into the mixture obtained in the step (1), and stirring for 2h at 1000r/min to obtain the annealing separant.
The application of the annealing release agent is used for the ultrahigh magnetic induction oriented silicon steel.
The ultrahigh magnetic induction oriented silicon steel consists of the following raw materials in percentage by mass: 0.08% of C, 3.4% of Si, 0.12% of Mn, 0.03% of S, Als: 0.03%, N: 0.01%, Bi: 0.0080%, Sn: 0.06% as a basic component, and the balance consisting of Fe and inevitable impurities.
The oriented silicon steel hot rolled plate is subjected to decarburization annealing after cold rolling, and is coated with the annealing release agent prepared by the comparative example, wherein the single-side coating amount is 3g/m3During coating, the generation of Mg (OH) in the coating residual liquid is controlled2The amount was 6.5%.
TiO in annealing release agent2The amount of (2) and the amount of the annealing separator applied do not satisfy the requirement of the formula (1) described in example 1.
And drying the steel plate coated with the annealing release agent, performing high-temperature annealing to form a glass film bottom layer, coating an insulating coating, and performing stretching, leveling and annealing to obtain a final product.
Test example
The final products prepared in examples 1-8, comparative examples 1-3 were subjected to a performance test in which adhesion was determined according to GB/T2522-1988; the magnetic induction intensity, namely the iron loss, is obtained by measuring GB/T3655-:
TABLE 1
Figure BDA0003333527600000121
Figure BDA0003333527600000131
As is clear from Table 1, examples 1 to 8 were conducted by controlling TiO content in MgO isolation agent2The content, Bi content and MgO coating amount in the steel sheet satisfy the following relational expression (1). When TiO in MgO isolating agent2When the content, the Bi content and the MgO coating weight in the steel plate satisfy the following relational expression (1), the bottom layer can be formed earlier by the MgO in the high-temperature annealing and heating process, the initial generation time of the bottom layer is shortened, the bottom layer forming thickness is increased, the bottom layer adhesiveness is improved, the inhibitor in the steel is more stable, the inhibition effect of AlN is promoted, and the improvement of the magnetic induction B is facilitated8. With the use of non-hydrated MgO, control of Mg (OH) in MgO paints2Measurement of<5 percent, and the ignition loss at 1000 ℃ is less than 1 percent, thereby controlling H2The amount of O accelerates the time for the formation of the bottom layer, which is beneficial to the adhesion of the bottom layer. Magnetic induction B of annealing separator coated steel plate prepared in the examples of the present application800Above 1.94T, the iron loss is significantly reduced compared to the comparative example.
As is clear from Table 1, in comparative example 1, Na was not added2O and boric acid are not favorable for reducing the formation temperature of the bottom layer, and the formation of the bottom layer is not favorable for the Bi-containing oriented silicon steel, so that the bottom layer is not formed or is easy to fall off after the release agent is coated. Comparative example 2, TiO in MgO isolation agent2The content is too small, which is not favorable for lowering the formation temperature of the underlayer, and the formation of the underlayer is not favorable for the Bi-containing oriented silicon steel, so that the underlayer is not formed or easily falls off after the release agent is coated. In comparative example 3, hardly water-wettable MgO, Mg (OH) formed in MgO was used2The content is more than 5 percent, which is not beneficial to secondary recrystallization of the Bi-containing oriented silicon steel and reduces the magnetism of the steel plate, and the steel plate B8The value is below 1.94T.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that it is obvious to those skilled in the art that various modifications and improvements can be made without departing from the principle of the present invention, and these modifications and improvements should also be considered as the protection scope of the present invention.

Claims (10)

1. The annealing release agent for improving the quality of the ultrahigh magnetic induction oriented silicon steel bottom layer is characterized by comprising the following components: MgO, TiO2Boric acid and Na2O、Sb2(SO4)3(ii) a Taking MgO quality as a standard, and the rest componentsThe relative MgO mass percentage is: TiO 221.9-40%, boric acid 0.05-0.1%, Na2O 1～5％，Sb2(SO4)3 1～5％。
2. The annealing separator of claim 1, wherein the MgO is non-hydrated MgO; the CAA activity value of the MgO is 180-300 s, and the ignition loss at 1000 ℃ is less than 1.3%.
3. The annealing separator according to claim 1, wherein the MgO has a CAA activity of 180 to 220s and a scorch at 1000 ℃ of < 1.0%.
4. The annealing separator according to claim 1, wherein the particle size of MgO is 0.01 to 3 μm.
5. A method for preparing the annealing separator according to claim 1, wherein the method comprises the following steps:
(1) the MgO mass is taken as a standard, and 1.9-40% of TiO is added according to the mass percentage20.05 to 0.1 percent of boric acid and 1 to 5 percent of Na2O, 1-5% of Sb2(SO4)3Adding into water, stirring to obtain a mixture;
(2) and (2) adding 100% of MgO into the mixture obtained in the step (1), and stirring to obtain the annealing separant.
6. The preparation method according to claim 5, wherein 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 the MgO is 8-12: 1.
7. the method according to claim 5, wherein the stirring speed in the step (2) is 1500 to 3000rpm for 2 to 3 hours.
8. The application of the annealing separator as claimed in any one of claims 1 to 4, wherein the annealing separator is used for ultrahigh magnetic induction oriented silicon steel.
9. The use of claim 8, wherein the annealing separator is coated on the surface of the ultrahigh-magnetic-induction oriented silicon steel; the coating amount is 3-5 g/m2。
10. Use according to claim 9, characterised in that the annealing separator is applied in an amount corresponding to the amount of TiO in the annealing separator2The magnesium oxide accounts for the mass fraction of the magnesium oxide and satisfies the following formula:
2*A1/2+5≤B*C≤200
wherein, the Bi content in the raw material of the oriented silicon steel A is ppm; B. TiO 22Accounts for the mass fraction of magnesium oxide,%; C. coating amount of annealing separator, g/m2。
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