CN113969103B - Semi-organic insulating coating for ultrathin oriented silicon steel - Google Patents
Semi-organic insulating coating for ultrathin oriented silicon steel Download PDFInfo
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- CN113969103B CN113969103B CN202111375916.1A CN202111375916A CN113969103B CN 113969103 B CN113969103 B CN 113969103B CN 202111375916 A CN202111375916 A CN 202111375916A CN 113969103 B CN113969103 B CN 113969103B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/325—Calcium, strontium or barium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/326—Magnesium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/327—Aluminium phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a semi-product for ultra-thin oriented silicon steelAn organic insulating paint. The semi-organic insulating paint comprises the following components in percentage by mass: 10 to 25 percent of phosphate, 1 to 10 percent of silane coupling agent containing epoxy group, 0.2 to 2.0 percent of organosilane, 1 to 10 percent of chromic anhydride, 1.5 to 6 percent of silicon dioxide particles, 0.3 to 5 percent of alkali and the balance of water; wherein the particle diameter of the silica particles is 100 to 300nm. When the semi-organic insulating coating is applied to the surface of the ultrathin oriented silicon steel, the adhesiveness of a coating and a base body is improved, the insulativity and the heat resistance of the coating are ensured, the adhesiveness of the coating is A grade, the lamination coefficient is greater than 0.96, the coating can resist the high temperature of 900 ℃, and when the coating is thin (less than 1 mu m), the insulation resistance of a steel plate is greater than 30 omega cm 2 The sheet has excellent insulating property and can meet the application requirement of the ultrathin oriented silicon steel.
Description
Technical Field
The invention belongs to the technical field of insulating coatings, and particularly relates to a semi-organic insulating coating for ultrathin oriented silicon steel.
Background
The ultra-thin oriented silicon steel is used for manufacturing iron cores with the working frequency of more than 400 Hz, is an indispensable soft magnetic alloy in the power and electronic industries, and is also an important metal functional material. The method is mainly applied to high-frequency transformers, high-power electromagnetic amplifiers, pulse transformers, pulse generators, inductors, roughness and memory elements and transformers working under vibration and radiation conditions. The converter valve is used as a core system of an extra-high voltage direct current transmission project, and a thyristor and a saturable reactor are arranged in the converter valve. The ultrathin oriented silicon steel with the thickness not more than 0.1mm is a key material for manufacturing the saturable reactor iron core. For a long time, the high-performance ultrathin oriented silicon steel is monopolized abroad, the technology is restricted by people, and the threat and challenge are formed to the construction of ultrahigh voltage projects in China. One of the key technologies of neck clamping of the high-performance ultrathin oriented silicon steel material is as follows: the lack of a high-performance tension coating component system suitable for direct coating on the surface of the ultrathin silicon steel causes the large difference between the coating performance of domestic ultrathin silicon steel and the performance of imported products, and the application requirement of extra-high voltage direct current engineering cannot be met.
The production method of the domestic ultrathin oriented silicon steel comprises the steps of pickling 0.23-0.30mm of conventional oriented silicon steel products to remove glass films and insulating films, carrying out primary recrystallization annealing after once cold rolling to a target thickness, and coating insulating coatings.
The ultra-thin oriented silicon steel requires that the adhesiveness of a coating is A grade, the thickness of the coating is less than 1 micron, and the insulation resistance is not less than 10 omega cm 2 The laminated steel sheet can resist high temperature of over 800 ℃ for long-time annealing, and the lamination coefficient is more than 0.96. The T2 inorganic coating for the existing oriented silicon steel is only suitable for being coated on a magnesium silicate bottom layer, the adhesiveness is B-D grade after sintering and curing, and if the T2 inorganic coating is directly coated on the surface of the ultrathin silicon steel, the adhesiveness is worse, and the requirement of the ultrathin oriented silicon steel cannot be met. The adhesiveness of various semi-organic coatings for the existing non-oriented silicon steel can reach A level, but the non-oriented silicon steel has low insulation resistance and cannot resist stress relief annealing at the temperature of more than 800 ℃. Therefore, an insulating coating special for the ultrathin oriented silicon steel needs to be prepared. And since the steel sheet is particularly thin, if a coating layer of a conventional thickness is applied to the surface thereof, it results in a lamination factor of the steel sheet of less than 0.96.
In the document 'preparation and performance evaluation of ultrathin oriented silicon steel coating for saturated reactor of extra-high voltage direct current converter valve', an insulating coating for ultrathin oriented silicon steel is provided, aluminum phosphate, nano aluminum silicate and chromic anhydride are used as main raw materials, and an adhesion promoter, a leveling agent and a high-temperature antioxidant are added. But the coating can only resist the high temperature of 700 ℃, and the coating can be burnt excessively when reaching 800 ℃. The requirement of the ultra-thin oriented silicon steel for resisting high temperature of more than 800 ℃ and eliminating stress annealing is not met. Patent CN103406249A proposes a process method for coating insulating paint on the surface of an ultra-thin oriented silicon steel strip, which makes the paint layer of the ultra-thin oriented silicon steel strip product thin, uniform, consistent in thickness, smooth, flat and controllable by an improved coating rod and steel strip coating mode. Patent CN111748248A proposes a chromium-free semi-organic insulating paint suitable for a Bi-containing ultrahigh magnetic induction oriented silicon steel without a bottom layer, which mainly meets the welding performance of the Bi-containing ultrahigh magnetic induction oriented silicon steel coating without the bottom layer, improves the processing performance of the oriented silicon steel coating and is not suitable for an extremely thin oriented silicon steel strip. In patent CN104928567A, a grain-oriented silicon steel with good processability and a manufacturing method thereof are proposed. The surface of the steel plate with the bottom layer of the glass film removed is coated with a semi-organic chromium-free insulating coating, and the effective components of the chromium-free semi-organic coating are phosphate and organic resin. After coating, the steel plate is baked at the plate temperature of 200-450 ℃ to form a film, so that a surface tension coating with high hardness and poor adhesion cannot be formed on the surface of the substrate, and the steel plate has good processing performance. The method only considers the punching performance of the coating, and is not suitable for the extremely thin oriented silicon steel sheet.
Although the coating can better meet the coating performance of the surface of the non-primer oriented silicon steel and the processing performance of the coating after coating, the problem of the insulation of the steel plate when the coating is thinner under the condition of no primer and the lamination coefficient of the steel plate after coating are not considered. Because the thinner the steel plate is, if the coating with the conventional thickness is coated on the surface of the steel plate, the stacking coefficient of the steel plate is less than 0.96, so that the volume of the iron core is influenced, the vibration and the iron loss of the iron core are increased, and the application requirement of the ultrathin oriented silicon steel cannot be met.
The lack of a high-performance tension coating component system suitable for direct coating on the surface of the ultrathin oriented silicon steel causes the large difference between the coating performance of domestic ultrathin oriented silicon steel and the performance of imported products, and the application requirement of extra-high voltage direct current engineering cannot be met. Therefore, a semi-organic insulating coating for ultra-thin oriented silicon steel with excellent performance is urgently needed to be found.
Disclosure of Invention
The invention aims to provide a semi-organic insulating coating for ultrathin oriented silicon steel, when the semi-organic insulating coating is applied to the surface of the ultrathin oriented silicon steel, the adhesiveness of a coating and a base body is improved, the insulativity and heat resistance of the coating are ensured, the lamination coefficient is more than 0.96, and the application requirement of the ultrathin oriented silicon steel can be met.
In order to solve the technical problems, the invention provides the following technical scheme:
the semi-organic insulating coating for the ultrathin oriented silicon steel comprises the following components in percentage by mass: 10 to 25 percent of phosphate, 1 to 10 percent of silane coupling agent containing epoxy group, 0.2 to 2.0 percent of organosilane, 1 to 10 percent of chromic anhydride, 1.5 to 6 percent of silicon dioxide particles, 0.3 to 5 percent of alkali and the balance of water; wherein the particle diameter of the silica particles is 100 to 300nm.
According to the scheme, the phosphate is 1 or 2 selected from Mg, fe, ca, zn and Na.
According to the scheme, the silane coupling agent containing the epoxy group is at least one of glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexane) ethyltrimethoxysilane or gamma-glycidoxypropyltrimethoxysilane.
According to the scheme, the organosilane is at least one of trioxyalkylsilane, tetroxysilane and tridecoxysilane.
According to the scheme, the particle size of the silicon dioxide oxide particles is 100-300nm.
According to the scheme, the alkali is one of ammonia water, amine or sodium hydroxide.
According to the scheme, the pH value of the semi-organic insulating paint is 5-7. If the pH of the coating is less than 4, corrosion of the steel plate substrate is caused with the generation of hydrogen.
The ultra-thin oriented silicon steel with the semi-organic insulating coating is prepared by coating the semi-organic insulating coating on the ultra-thin oriented silicon steel.
According to the scheme, the thickness of the coating is less than 1 mu m.
According to the scheme, the ratio of the thickness of the coating to the thickness of the silicon steel plate matrix is 1: (130-200).
According to the scheme, the semi-organic insulating coating is coated on the ultra-thin oriented silicon steel and annealed at the temperature of 800-900 ℃.
According to the scheme, the ultrathin oriented silicon steel is a conventional oriented silicon steel or high magnetic induction oriented silicon steel product with the thickness of 0.23-0.30mm, the glass film and the insulating film are removed by acid cleaning, and the ultrathin oriented silicon steel is prepared by performing primary recrystallization annealing after being subjected to primary cold rolling to the target thickness of less than 0.1 mm.
The invention provides a semi-organic insulating coating for ultrathin oriented silicon steel, which comprises phosphate, a silane coupling agent containing epoxy groups, organosilane, chromic anhydride, silicon dioxide oxide particles and alkali, and the working principle is as follows:
phosphate is a main film forming material of the coating, is beneficial to the heat resistance of the coating, has not high content, prevents more free phosphoric acid in the coating, and prevents the surface of the coating from being corroded when the coating is sintered to influence the appearance of the coating. The content of the phosphate is not too low, and the low content of the phosphate easily causes low surface insulation resistance and poor heat resistance of the coating.
Chromic anhydride can prevent the hygroscopicity of phosphate after sintering and the surface of the steel plate from rusting or sticking. Cr can be used to trap free P, and Cr forms a chemical bond with Si, O, and P to make the insulating film stronger, defect-free, and excellent in corrosion resistance and magnetic properties.
Silane coupling agent containing epoxy group is combined with organosilane, silanol groups among all molecules of silane are mutually condensed to form a film with a net structure to cover the surface of the bottom layer; the silane coupling agent is beneficial to improving the adhesive force between the metal substrate and the organic polymer, and the silane coupling agent containing the epoxy group can be combined with the organosilane through the epoxy group, so that the tackifier has a greater effect; meanwhile, silane reacts with water molecules in the inorganic substance and is hydrolyzed to generate silanol groups, so that hydrogen bonds are formed with hydroxyl on the surface of the substrate, and the connection with the substrate is enhanced; in conclusion, the silane coupling agent containing epoxy group can greatly improve the adhesion of the coating layer by combining with the organosilane. Furthermore, when at least one of trioxyalkylsilane, tetralkoxysilane, and tridecoxysilane is selected as the organosilane, the replacement group in the organosilane is more easily broken, so that the organosilane is more favorably combined with silicon in the steel plate matrix, and the adhesion of the coating can be further improved.
The reason why the silica oxide particles are cooperatively introduced into the coating system of the invention is presumed to be that the higher interlayer resistance is obtained and the insulating property of the coating is improved: the surface of the steel sheet is not microscopically flat and has many irregularities, and this defect can be compensated by applying a coating liquid containing oxide particles. And the silicon dioxide can be inserted into the silicon base and combined with the poly-silicon ethane in the organic matter to form a compact continuous film, thereby improving the interlayer resistance.
The invention has the following beneficial effects:
1. the invention provides a semi-organic insulating coating for ultrathin oriented silicon steel, which is prepared from phosphorusThe acid salt is used as a main film forming material, an organic high molecular compound formed by matching a silane coupling agent containing an epoxy group and organosilane is used as an auxiliary film forming material, and Cr and silicon dioxide oxide particles are used for enhancing the firmness, corrosion resistance, magnetism, compactness and insulativity of the film; when the coating is used for the ultrathin oriented silicon steel, the adhesiveness of the coating and a matrix is improved, the insulativity and the heat resistance of the coating are ensured, the coating can resist the high temperature of 900 ℃, and when the coating is thin (less than 1 mu m), the insulation resistance of a steel plate is more than 30 omega cm 2 Piece, excellent insulating properties.
2. The invention provides ultrathin oriented silicon steel with a semi-organic insulating coating, the surface quality of a steel plate is excellent, the thickness of the coating is less than 1 mu m, the adhesiveness of the coating is A grade, and the insulation resistance is more than 30 omega cm 2 The lamination coefficient is more than 0.96, and the application requirement of the ultrathin oriented silicon steel can be met.
Detailed Description
The invention is further illustrated by the following specific examples.
Examples 1 to 8 and comparative examples 1 to 3
The semi-organic insulating paint for the ultrathin oriented silicon steel comprises the following components: phosphate, silane coupling agent containing epoxy group, organosilane, chromic anhydride, silicon dioxide oxide particles, alkali and the balance of deionized water. Wherein, the specific material types and the proportions of the components are respectively shown in the table 1 and the table 2.
TABLE 1 EXAMPLES 1-8 AND COMPARATIVE EXAMPLES 1-3 Components specific material types
TABLE 2 ingredient ratios of examples 1 to 8 and comparative examples 1 to 3
Wherein the mass percentage of the rest in the table is pure water.
For a high magnetic induction grain-oriented silicon steel product of 0.23mm, pickling was performed to remove a glass film and an insulating film, primary recrystallization annealing was performed after primary cold rolling to a target thickness of 0.08mm, the insulating coatings obtained in examples 1 to 8 and comparative examples 1 to 3 were coated, and annealing was performed at 900 ℃.
TABLE 3 Properties of the steel sheets after applying the insulating coating in examples 1 to 8 and comparative examples 1 to 3
As can be seen from tables 2 and 3, in examples 1 to 8, the insulating coating solutions prepared according to the present invention were coated on ultra-thin oriented silicon steel and annealed at 800 to 900 ℃ to obtain a steel sheet having excellent surface quality, a coating adhesion of class A, and an interlayer resistance of generally more than 30. Omega. Cm 2 The lamination coefficient of the steel plate is more than 96.0.
Comparative example 1 had a phosphate content of 3.5. Omega. Cm, and the surface coating had poor appearance, poor insulating properties, and an insulation resistance of 2 Coating adhesion is E grade, and the lamination coefficient of the steel plate is less than 96.0.
In comparative example 2, the contents of organosilane and silane coupling agent were small, the coating was liable to fall off after the coating was dried, the adhesion of the coating was poor, and the insulation resistance of the coating was less than 10. Omega. Cm 2 The lamination coefficient of the steel plate is less than 96.0.
In comparative example 3, the particle size of silica oxide particles was 350nm, the coating was liable to come off after the coating was coated and dried, the adhesion of the coating was poor, and the insulation resistance of the coating was less than 10. Omega. Cm 2 The lamination coefficient of the steel plate is less than 96.0.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The semi-organic insulating coating for the ultrathin oriented silicon steel is characterized by comprising the following components in percentage by mass: 10 to 25 percent of phosphate, 1 to 10 percent of silane coupling agent containing epoxy group, 0.2 to 2.0 percent of organosilane, 1 to 10 percent of chromic anhydride, 1.5 to 6 percent of silicon dioxide particles, 0.3 to 5 percent of alkali and the balance of water; wherein:
the particle size of the silicon dioxide particles is 100 to 300 nm;
the organosilane is at least one of trioxyalkylsilane and tetralkoxysilane;
the thickness of the coating formed by the semi-organic insulating paint is less than 1 mu m.
2. Semi-organic insulating coating according to claim 1, characterized in that said phosphate is 1 or 2 phosphates selected from Mg, fe, ca, zn, na.
3. The semi-organic insulating coating of claim 1, wherein the epoxy group-containing silane coupling agent is at least one of glycidoxypropyltrimethoxysilane, 2- (3, 4-epoxycyclohexane) ethyltrimethoxysilane, or gamma-glycidoxypropyltrimethoxysilane.
4. The semi-organic insulating paint according to claim 1, wherein the alkali is one of ammonia, amine or sodium hydroxide.
5. The semi-organic insulating paint according to claim 1, wherein the pH of the semi-organic insulating paint is 5 to 7.
6. An ultra-thin oriented silicon steel having a semi-organic insulating coating layer, wherein the semi-organic insulating coating layer is prepared by applying the semi-organic insulating coating material of any one of claims 1 to 5 on the ultra-thin oriented silicon steel.
7. The ultra-thin oriented silicon steel with semi-organic insulating coating according to claim 6, wherein the ratio of the thickness of the coating to the thickness of the silicon steel plate substrate is 1: (130-200).
8. The ultra-thin oriented silicon steel with a semi-organic insulating coating according to claim 6, wherein the semi-organic insulating coating is coated on the ultra-thin oriented silicon steel and annealed at a temperature of 800-900 ℃.
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| CN105086778B (en) * | 2015-09-10 | 2017-09-29 | 武汉科技大学 | It is a kind of for Chrome-free insulation coating of orientation silicon steel and preparation method thereof |
| CN106995924A (en) * | 2017-05-12 | 2017-08-01 | 盐城工学院 | A kind of aqueous chromium-free high alumina anticorrosive paint and preparation method thereof |
| CN110283488B (en) * | 2019-06-28 | 2021-07-06 | 武汉钢铁有限公司 | Semi-organic insulating coating for ultrahigh magnetic induction oriented silicon steel and use method thereof |
| CN111748248A (en) * | 2020-06-15 | 2020-10-09 | 武汉钢铁有限公司 | Chromium-free semi-organic insulating paint suitable for Bi-containing ultrahigh magnetic induction oriented silicon steel without bottom layer |
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