CN108752984B - Surface wear-resistant oxidation-resistant coating, preparation method and application thereof - Google Patents
Surface wear-resistant oxidation-resistant coating, preparation method and application thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a surface wear-resistant and oxidation-resistant coating, a preparation method and application thereof. The preparation method of the surface wear-resistant oxidation-resistant coating comprises the following steps: (1) stirring and mixing 15-20 parts by weight of mullite powder, 20-30 parts by weight of andalusite powder, 12-16 parts by weight of elemental silicon powder, 12-16 parts by weight of silicon carbide powder, 7-8 parts by weight of alumina powder, 20-25 parts by weight of dextrin, 40-70 parts by weight of water, 0.1-0.3 part by weight of dispersing agent, 0.1-0.3 part by weight of thickening agent and 0.09-0.2 part by weight of adhesion promoter uniformly to form coating slurry; (2) coating the composite material on the surface to form a coating; (3) sintering at 1300-1400 ℃ for 2-4 hours. The surface wear-resistant and oxidation-resistant coating which is firmly combined with the substrate is coated on the surface, so that the safety, oxidation resistance and impact resistance of the material are improved, the use temperature of the material is effectively improved, and the service life is prolonged.
Description
Technical Field
The invention relates to a coating, a preparation method and application thereof, in particular to a surface wear-resistant and oxidation-resistant coating, a preparation method and application thereof.
Background
The core component of industrial and domestic electric heating appliances on the market is an electric heating element. The quality of the electric heating element is good, and the service life of the electric heating element depends on the service performance and the service life of the electric heating appliance.
In order to use the electric heating element for a long time under a higher temperature field, the surface layer of the electric heating element is coated by adopting a coating technology, and the coating slowly generates a glass state phase so as to isolate the contact of oxygen and a matrix, so that little oxygen is diffused into the matrix from the outside, and the high-temperature oxidation resistance effect is achieved.
A reliable, effective, long-term high-temperature oxidation-resistant coating must have the following characteristics: 1. the high-temperature oxidation resistance of the coating is required to be excellent, the coating is compact, and an effective shielding layer can be formed between a corrosion medium and a silicon carbide substrate; 2. the coating has good bonding property with the substrate. If the combination of the coating and the substrate is weak, the coating is easy to peel off under the action of external force or internal thermal stress; 3. the thermal shock resistance of the coating is excellent. If the thermal shock resistance of the coating is not good, the coating can crack due to sudden temperature change in the using process, and the oxidation protection effect of the coating disappears; 4. the chemical stability of the coating is good. The coating has certain chemical corrosion resistance, otherwise, the composition of the environment is changed slightly, and the coating is corroded and fails; 5. the coating has good high-temperature thermal stability. The structure and the performance do not change in the high-temperature long-time work, the coating is not easy to volatilize and does not have phase transition, and if the coating has structural change in the service period, the volume change of the coating caused by the structural change is often failed; 6. the difference in thermal expansion coefficient between the coating and the base material is as small as possible. Otherwise thermal stresses may be induced by temperature changes, initiating crack initiation and propagation, and the final coating may peel off from the substrate.
Among the currently used coatings, there are the following categories: glass coatings, superalloy metal coatings, high temperature ceramic coatings and composite coatings.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the following technical scheme:
a preparation method of a surface wear-resistant oxidation-resistant coating comprises the following steps:
(1) stirring and mixing 15-20 parts by weight of mullite powder, 20-30 parts by weight of andalusite powder, 12-16 parts by weight of elemental silicon powder, 12-16 parts by weight of silicon carbide powder, 7-8 parts by weight of alumina powder, 20-25 parts by weight of dextrin, 40-70 parts by weight of water, 0.1-0.3 part by weight of dispersing agent, 0.1-0.3 part by weight of thickening agent and 0.09-0.2 part by weight of adhesion promoter uniformly to form coating slurry;
(2) coating the coating slurry prepared in the step (1) on the surface of the composite material to form a coating;
(3) sintering at 1300-1400 ℃ for 2-4 hours.
The composite material of step (2) may be a carbon/carbon composite material or a carbon/silicon carbide composite material, such as an electric heating element. The electric heating element can be a commercially available electric heating element, or can be prepared by referring to the existing literature and patents, for example, the invention patent of patent application No. 201510043900.9.
The thickness of the coating in the step (2) is 400-600 mu m.
The mullite powder in the step (1) is preferably modified mullite powder or mullite powder.
The modified mullite powder is prepared by the following method:
weighing the following raw materials in percentage by weight: 10-20 wt% of acrylic acid, 0.2-1.5 wt% of silane coupling agent, 0.7-1.5 wt% of polyethylene glycol 400 monooleate, 0.1-0.15 wt% of acetic acid, 0.1-0.2 wt% of sodium dodecyl sulfate and the balance of deionized water;
uniformly mixing acetic acid and water, and stirring for 10-20 minutes at 200-400 revolutions per minute to form an acid solution; adding a silane coupling agent, and stirring for 20-30 minutes at 200-400 r/min; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 30-50 minutes at 200-400 revolutions per minute; adding mullite powder, reducing the rotating speed to 100-150 revolutions per minute, heating to 70-75 ℃, and stirring for 90-120 minutes to obtain a modified solution; centrifuging the modified solution, and collecting bottom solids; and drying the bottom solid at 100-105 ℃ for 3-6 hours, and sintering at 600-700 ℃ for 1-3 hours to obtain the modified mullite powder.
The mullite powder used in the invention can be natural mineral mullite powder sold in the market, and can also be obtained by a chemical preparation method.
The mullite powder is prepared by the following method:
weighing 20-25 g of anhydrous aluminum chloride, and stirring 12-14 mL of tetraethoxysilane for 30-40 minutes at 300-500 revolutions per minute; adding 14-17 mL of diethyl ether, and continuously stirring for 20-30 minutes at 300-500 rpm; then adding 20-30 mL of dichloromethane, and stirring for 20-30 minutes at 300-500 rpm to obtain a reaction solution; then pouring the reaction liquid into a hydrothermal reaction kettle, and reacting for 16-24 hours at 110-130 ℃; after the reaction is finished, taking out the reactant, drying at 50-60 ℃ for 7-12 hours, ball-milling for 20-30 minutes by a dry method, wherein the ball-milling rotation speed is 400-600 r/min, and the mass ratio of the material to the ball-milling medium is 1: (2-3); and (3) taking the reactant subjected to dry ball milling, carrying out heat treatment at 900-950 ℃ for 0.5-1 hour, and naturally cooling to 30-40 ℃ to obtain the mullite powder.
The adhesion promoter in the step (1) is one or a combination of a plurality of polysiloxane adhesion promoters, polyurethane adhesion promoters, cyano acetoxy adhesion promoters, acetic acid acetyl adhesion promoters and urea ring adhesion promoters. Preferably, the adhesion promoter is a mixture of a polysiloxane adhesion promoter and a polyurethane adhesion promoter in a mass ratio of (1-3) to (1-3).
In the step (1), the thickener is one or a mixture of more of methylcellulose, ammonium polyacrylate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and sodium polyacrylate.
The invention also provides a surface wear-resistant and oxidation-resistant coating which is prepared by adopting the method.
The invention also provides application of the surface wear-resistant and oxidation-resistant coating in improving safety, oxidation resistance and impact resistance of the electric heating element.
Compared with the prior art, the invention has the advantages that:
the coating raw material adopts andalusite and mullite which are mixed for use, the andalusite powder is decomposed in the sintering process, and a mullite network structure arranged in a staggered structure is formed, so that the fiber reinforcement effect of mullite crystals can be fully exerted; and the silica glass phase sodium decomposed in the andalusite sintering process can well wet mullite powder and other inorganic materials, and the glass phase can be filled in pores of the mullite skeleton after cooling.
The modified mullite powder is adopted, active functional groups are grafted on the surface of the mullite powder, the surface property of the mullite powder is improved, the surface caking property of the mullite powder is enhanced, and the mullite powder is protected.
Compared with the mullite powder sold in the market, the preparation period of the self-made mullite powder is short, the raw material can be mixed in a molecular level, and the problem that the mullite powder sold in the market is easy to agglomerate is solved.
According to the invention, the raw materials and the composition proportion of the coating slurry are adjusted by a slurry coating method, so that the composite coating mainly comprising mullite and andalusite is prepared, the combination between the coating and the substrate is facilitated, the bonding strength is improved, and the residual stress in the coating is relaxed and eliminated.
The surface wear-resistant and oxidation-resistant coating which is firmly combined with the substrate is coated on the surface, so that the safety, oxidation resistance and impact resistance of the material are improved, the use temperature of the material is effectively improved, and the service life is prolonged.
Detailed Description
In the examples, the sources of the raw materials are as follows:
the electric heating element in the embodiment is a silicon carbide electric heating element provided by Songbo high-temperature materials of Zhenzhou city, model 12 x 200.
The commercially available mullite powder in the examples was provided by the firm, Youxing mineral products, Inc., with a particle size of 320 mesh.
The andalusite powder in the examples is provided by Deteng mineral processing factory in Lingshu county, first grade, and has a particle size of 600 meshes.
In the examples, elemental silicon powder was supplied by xu Lingyun silicon industries, Inc. and had a particle size of 1000 mesh.
In the examples, silicon carbide powder having a particle size of 300 mesh was supplied from Henan super China silicon industries, Ltd.
Examples alumina powder, CAS No.: 21645-51-2, 1000 mesh, supplied by soaring chemical Co., Ltd.
Examples dextrin, CAS No.: 9004-53-9, available from Hefeijian chemical Co.
In the examples, a polycarboxylate dispersant provided by cunninghamia lanceolata chemical Co., Ltd, of Dongguan was specifically used, and the model of the dispersant was S-407.
In the examples, the thickener is ammonium polyacrylate thickener provided by Sihai Biotech Co., Ltd, Henan gold, and has a molecular weight of 1000 ten thousand.
Examples polysiloxane adhesion promoters were prepared according to the first example of patent application No. 201310566143.4 "a high performance adhesion promoter and method of preparation".
Examples tetraethyl orthosilicate, CAS number: 562-90-3, available from jilede new materials science and technology, inc.
Examples acrylic acid, CAS No.: 79-10-7, available from Yonghua chemical technology (Jiangsu) Ltd.
In the examples, a silane coupling agent, specifically KH550 silane coupling agent provided by new materials ltd, bainhong, shandong, was used.
Polyethylene glycol 400 monooleate in the examples was supplied by ten thousand new materials, Inc. in Guangzhou.
Examples acetic acid, CAS number: 72196-32-8, supplied by Nanjing Conman chemical industry Co.
Examples sodium lauryl sulfate, CAS number: 151-21-3, available from steganochemical (shanghai) ltd.
Examples anhydrous aluminum chloride, CAS No.: 7446-70-0, provided by Gallery Peng color Fine chemical Co., Ltd, with a fineness of 80 mesh.
In the examples, zirconia beads, 0.2mm in size, were used as the ball milling media.
The polyurethane adhesion promoter in the examples was prepared by reference to example 8 of patent application No. 201610064118. X.
The carbon/carbon composite materials in the examples were provided by the Haoxin composite Co., Ltd.
Example 1
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of commercially available mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent and 0.1g of polysiloxane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) and sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere.
Example 2
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of commercially available mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent and 0.1g of polysiloxane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere; and (3) coating tetraethyl orthosilicate on the surface of the sintered electric heating element coating, and drying at 150 ℃ for 2 hours to form a sealing and filling layer with the thickness of 30 mu m.
Example 3
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of modified mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent and 0.1g of polysiloxane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere; and (3) coating tetraethyl orthosilicate on the surface of the sintered electric heating element coating, and drying at 150 ℃ for 2 hours to form a sealing and filling layer with the thickness of 30 mu m.
The modified mullite powder is obtained by the following method: weighing the following raw materials in percentage by weight: 20 wt% of acrylic acid, 1.5 wt% of silane coupling agent, 1.2 wt% of polyethylene glycol 400 monooleate, 0.15 wt% of acetic acid, 0.1 wt% of sodium dodecyl sulfate and the balance of deionized water; uniformly mixing acetic acid and deionized water, and stirring at 300 revolutions per minute for 10 minutes to form an acidic solution; adding a silane coupling agent into the acidic solution, and stirring at 300 revolutions per minute for 20 minutes; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 50 minutes at 300 revolutions per minute; adding commercially available mullite powder, reducing the rotating speed to 100 revolutions per minute, heating to 70 ℃ at the speed of 5 ℃/minute, and stirring for 90 minutes to obtain a modified solution; centrifuging the modified solution at 4000 rpm for 15 minutes, and collecting a bottom solid; and drying the bottom solid at 105 ℃ for 3 hours, and sintering at 600 ℃ for 2 hours to obtain the modified mullite powder.
Example 4
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of modified mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent and 0.1g of polysiloxane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere; and (3) coating tetraethyl orthosilicate on the surface of the sintered electric heating element coating, and drying at 150 ℃ for 2 hours to form a sealing and filling layer with the thickness of 30 mu m.
The modified mullite powder is obtained by the following method: weighing the following raw materials in percentage by weight: 20 wt% of acrylic acid, 1.5 wt% of silane coupling agent, 1.2 wt% of polyethylene glycol 400 monooleate, 0.15 wt% of acetic acid, 0.1 wt% of sodium dodecyl sulfate and the balance of deionized water; uniformly mixing acetic acid and deionized water, and stirring at 300 revolutions per minute for 10 minutes to form an acidic solution; adding a silane coupling agent into the acidic solution, and stirring at 300 revolutions per minute for 20 minutes; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 50 minutes at 300 revolutions per minute; adding self-made mullite powder, reducing the rotating speed to 100 revolutions per minute, heating to 70 ℃ at the speed of 5 ℃/minute, and stirring for 90 minutes to obtain a modified solution; centrifuging the modified solution at 4000 rpm for 15 minutes, and collecting a bottom solid; and drying the bottom solid at 105 ℃ for 3 hours, and sintering at 600 ℃ for 2 hours to obtain the modified mullite powder.
The preparation process of the mullite powder comprises the following steps: weighing 21g of anhydrous aluminum chloride, and stirring 14mL of tetraethoxysilane at 300 revolutions per minute for 40 minutes; adding 15mL of diethyl ether, and continuing stirring at 300 rpm for 20 minutes; then adding 20mL of dichloromethane, and stirring at 300 revolutions per minute for 20 minutes to obtain a reaction solution; then pouring the reaction liquid into a hydrothermal reaction kettle, and reacting at 110 ℃ for 24 hours, wherein the volume filling ratio of the hydrothermal kettle is kept at 40% in the reaction process; after the reaction is finished, taking out the reactant, drying the reactant at 60 ℃ for 8 hours, performing dry ball milling for 30 minutes at a ball milling rotation speed of 400 r/min, wherein the mass ratio of the material to the ball milling medium is 1: 2; and (3) taking the reactant subjected to dry ball milling, carrying out heat treatment at 900 ℃ for 1 hour, and naturally cooling to 30 ℃ to obtain the mullite powder.
Example 5
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of modified mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent and 0.1g of polyurethane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere; and (3) coating tetraethyl orthosilicate on the surface of the sintered electric heating element coating, and drying at 150 ℃ for 2 hours to form a sealing and filling layer with the thickness of 30 mu m.
The modified mullite powder is obtained by the following method: weighing the following raw materials in percentage by weight: 20 wt% of acrylic acid, 1.5 wt% of silane coupling agent, 1.2 wt% of polyethylene glycol 400 monooleate, 0.15 wt% of acetic acid, 0.1 wt% of sodium dodecyl sulfate and the balance of deionized water; uniformly mixing acetic acid and deionized water, and stirring at 300 revolutions per minute for 10 minutes to form an acidic solution; adding a silane coupling agent into the acidic solution, and stirring at 300 revolutions per minute for 20 minutes; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 50 minutes at 300 revolutions per minute; adding self-made mullite powder, reducing the rotating speed to 100 revolutions per minute, heating to 70 ℃ at the speed of 5 ℃/minute, and stirring for 90 minutes to obtain a modified solution; centrifuging the modified solution at 4000 rpm for 15 minutes, and collecting a bottom solid; and drying the bottom solid at 105 ℃ for 3 hours, and sintering at 600 ℃ for 2 hours to obtain the modified mullite powder.
The preparation process of the mullite powder comprises the following steps: weighing 21g of anhydrous aluminum chloride, and stirring 14mL of tetraethoxysilane at 300 revolutions per minute for 40 minutes; adding 15mL of diethyl ether, and continuing stirring at 300 rpm for 20 minutes; then adding 20mL of dichloromethane, and stirring at 300 revolutions per minute for 20 minutes to obtain a reaction solution; then pouring the reaction liquid into a hydrothermal reaction kettle, and reacting at 110 ℃ for 24 hours, wherein the volume filling ratio of the hydrothermal kettle is kept at 40% in the reaction process; after the reaction is finished, taking out the reactant, drying the reactant at 60 ℃ for 8 hours, performing dry ball milling for 30 minutes at a ball milling rotation speed of 400 r/min, wherein the mass ratio of the material to the ball milling medium is 1: 2; and (3) taking the reactant subjected to dry ball milling, carrying out heat treatment at 900 ℃ for 1 hour, and naturally cooling to 30 ℃ to obtain the mullite powder.
Example 6
The thermal shock resistant electric heating element is prepared by adopting the process comprising the following steps:
(1) using absolute ethyl alcohol as a solvent, removing oil stains on the surface of the electric heating element by using an ultrasonic cleaning machine, wherein the ultrasonic frequency is 30kHz, the ultrasonic temperature is 50 ℃, and drying the cleaned electric heating element for 3 hours at 50 ℃;
(2) uniformly mixing the coating raw materials, and stirring at 300 revolutions per minute for 1 hour to form coating slurry; the coating comprises the following raw materials in percentage by weight: 20g of modified mullite powder, 30g of andalusite powder, 16g of elemental silicon powder, 15g of silicon carbide powder, 7g of alumina powder, 23g of dextrin, 70g of water, 0.23g of dispersing agent, 0.2g of thickening agent, 0.06g of polysiloxane adhesion promoter and 0.04g of polyurethane adhesion promoter;
(3) uniformly and densely brushing the slurry on the surface of the electric heating element treated in the step (1) to form a coating with the thickness of 500 mu m;
(4) sintering the electric heating element coated with the slurry for 3 hours at 1400 ℃ in an air atmosphere; and (3) coating tetraethyl orthosilicate on the surface of the sintered electric heating element coating, and drying at 150 ℃ for 2 hours to form a sealing and filling layer with the thickness of 30 mu m.
The modified mullite powder is obtained by the following method: weighing the following raw materials in percentage by weight: 20 wt% of acrylic acid, 1.5 wt% of silane coupling agent, 1.2 wt% of polyethylene glycol 400 monooleate, 0.15 wt% of acetic acid, 0.1 wt% of sodium dodecyl sulfate and the balance of deionized water; uniformly mixing acetic acid and deionized water, and stirring at 300 revolutions per minute for 10 minutes to form an acidic solution; adding a silane coupling agent into the acidic solution, and stirring at 300 revolutions per minute for 20 minutes; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 50 minutes at 300 revolutions per minute; adding self-made mullite powder, reducing the rotating speed to 100 revolutions per minute, heating to 70 ℃ at the speed of 5 ℃/minute, and stirring for 90 minutes to obtain a modified solution; centrifuging the modified solution at 4000 rpm for 15 minutes, and collecting a bottom solid; and drying the bottom solid at 105 ℃ for 3 hours, and sintering at 600 ℃ for 2 hours to obtain the modified mullite powder.
The preparation process of the mullite powder comprises the following steps: weighing 21g of anhydrous aluminum chloride, and stirring 14mL of tetraethoxysilane at 300 revolutions per minute for 40 minutes; adding 15mL of diethyl ether, and continuing stirring at 300 rpm for 20 minutes; then adding 20mL of dichloromethane, and stirring at 300 revolutions per minute for 20 minutes to obtain a reaction solution; then pouring the reaction liquid into a hydrothermal reaction kettle, and reacting at 110 ℃ for 24 hours, wherein the volume filling ratio of the hydrothermal kettle is kept at 40% in the reaction process; after the reaction is finished, taking out the reactant, drying the reactant at 60 ℃ for 8 hours, performing dry ball milling for 30 minutes at a ball milling rotation speed of 400 r/min, wherein the mass ratio of the material to the ball milling medium is 1: 2; and (3) taking the reactant subjected to dry ball milling, carrying out heat treatment at 900 ℃ for 1 hour, and naturally cooling to 30 ℃ to obtain the mullite powder.
Example 7
A preparation method of a surface wear-resistant oxidation-resistant coating comprises the following steps:
(1) stirring and uniformly mixing 18 parts by weight of commercially available mullite powder, 25 parts by weight of andalusite powder, 14 parts by weight of elemental silicon powder, 13 parts by weight of silicon carbide powder, 8 parts by weight of alumina powder, 21 parts by weight of dextrin, 60 parts by weight of water, 0.2 part by weight of dispersing agent, 0.2 part by weight of thickening agent and 0.16 part by weight of polysiloxane adhesion promoter to form coating slurry;
(2) coating the coating slurry prepared in the step (1) on the surface of a carbon/carbon composite material to form a coating with the thickness of 400 mu m;
(3) sintering in a vacuum furnace at 1300 ℃ for 3 hours.
The surface wear-resistant oxidation-resistant coating of the embodiment is oxidized for 5 hours at 1300 ℃, and the weight loss rate is 13.8%.
Example 8
A preparation method of a surface wear-resistant oxidation-resistant coating comprises the following steps:
(1) stirring and uniformly mixing 18 parts by weight of commercially available mullite powder, 25 parts by weight of andalusite powder, 14 parts by weight of elemental silicon powder, 13 parts by weight of silicon carbide powder, 8 parts by weight of alumina powder, 21 parts by weight of dextrin, 60 parts by weight of water, 0.2 part by weight of dispersing agent, 0.2 part by weight of thickening agent and 0.16 part by weight of polyurethane adhesion promoter to form coating slurry;
(2) coating the coating slurry prepared in the step (1) on the surface of a carbon/carbon composite material to form a coating with the thickness of 400 mu m;
(3) sintering in a vacuum furnace at 1300 ℃ for 3 hours.
The surface wear-resistant oxidation-resistant coating of the embodiment is oxidized for 5 hours at 1300 ℃, and the weight loss rate is 13.4%.
Example 9
A preparation method of a surface wear-resistant oxidation-resistant coating comprises the following steps:
(1) stirring and mixing 18 parts by weight of commercially available mullite powder, 25 parts by weight of andalusite powder, 14 parts by weight of elemental silicon powder, 13 parts by weight of silicon carbide powder, 8 parts by weight of alumina powder, 21 parts by weight of dextrin, 60 parts by weight of water, 0.2 part by weight of dispersing agent, 0.2 part by weight of thickening agent, 0.08 part by weight of polysiloxane adhesion promoter and 0.08 part by weight of polyurethane adhesion promoter uniformly to form coating slurry;
(2) coating the coating slurry prepared in the step (1) on the surface of a carbon/carbon composite material to form a coating with the thickness of 400 mu m;
(3) sintering in a vacuum furnace at 1300 ℃ for 3 hours.
The surface wear-resistant oxidation-resistant coating of the embodiment is oxidized for 5 hours at 1300 ℃, and the weight loss rate is 12.2%.
Test example 1
The oxidation resistance of the electric heating element is tested by using the oxidation weight gain in a constant temperature oxidation state by adopting an oxidation weight gain method.
The electric heating element is placed in a resistance furnace, the temperature is raised to 1400 ℃ at the heating rate of 5 ℃/minute, the temperature is preserved for 60 hours, then the electric heating element is taken out and cooled to 25 ℃ in the air, and the weight of the electric heating element is recorded by a precision electronic balance (the precision is 0.01 mg).
The oxidation weight gain was calculated according to the following formula: g ═ G2-G1)/G1 × 100%.
Wherein G is the oxidation weight gain; g1 is the weight (g) of the electric heating element before oxidation; g2 is the weight (g) of the element after oxidation.
For each example, 5 samples were taken and the average was taken as the final test result.
The specific test results are shown in table 1.
TABLE 1 Oxidation resistance test results table
| Oxidation weight gain (%) | |
| Example 1 | 0.078 |
| Example 2 | 0.065 |
| Example 3 | 0.047 |
| Example 4 | 0.039 |
| Example 5 | 0.036 |
| Example 6 | 0.032 |
Test example 2
The thermal shock resistance of the electric heating element is detected by the following method:
the electric heating element is placed in a resistance furnace at 1300 ℃ for heat preservation for 15 minutes, taken out and cooled to 25 ℃ in air, and then placed in an electric furnace at 1300 ℃ for heat preservation for 15 minutes, thus forming a cycle.
After 50 cycles of thermal shock resistance, the weight of the element was recorded.
The oxidation weight gain was calculated according to the following formula: g ═ G2-G1)/G1 × 100%.
Wherein G is the oxidation weight gain; g1 is the weight (g) of the electric heating element before oxidation; g2 is the weight (g) of the element after oxidation.
For each example, 5 samples were taken and the average was taken as the final test result.
The specific test results are shown in table 2.
TABLE 2 thermal shock resistance test results table
| Oxidation weight gain (%) | |
| Example 1 | 0.139 |
| Example 2 | 0.115 |
| Example 3 | 0.097 |
| Example 4 | 0.085 |
| Example 5 | 0.082 |
| Example 6 | 0.076 |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a surface wear-resistant oxidation-resistant coating comprises the following steps:
(1) stirring and mixing 15-20 parts by weight of modified mullite powder, 20-30 parts by weight of andalusite powder, 12-16 parts by weight of elemental silicon powder, 12-16 parts by weight of silicon carbide powder, 7-8 parts by weight of alumina powder, 20-25 parts by weight of dextrin, 40-70 parts by weight of water, 0.1-0.3 part by weight of dispersing agent, 0.1-0.3 part by weight of thickening agent and 0.09-0.2 part by weight of adhesion promoter uniformly to form coating slurry;
(2) coating the coating slurry prepared in the step (1) on the surface of the composite material to form a coating;
(3) sintering at 1300-1400 ℃ for 2-4 hours;
the modified mullite powder is prepared by the following method:
uniformly mixing acetic acid and deionized water, and stirring for 10-20 minutes at 200-400 revolutions per minute to form an acidic solution; adding a silane coupling agent, and stirring for 20-30 minutes at 200-400 r/min; adding acrylic acid, polyethylene glycol 400 monooleate and sodium dodecyl sulfate, and stirring for 30-50 minutes at 200-400 revolutions per minute; adding mullite powder, reducing the rotating speed to 100-150 revolutions per minute, heating to 70-75 ℃, and stirring for 90-120 minutes to obtain a modified solution; centrifuging the modified solution, and collecting bottom solids; and drying the bottom solid at 100-105 ℃ for 3-6 hours, and sintering at 600-700 ℃ for 1-3 hours to obtain the modified mullite powder.
2. The preparation method of the surface wear-resistant and oxidation-resistant coating according to claim 1, wherein the coating thickness in the step (2) is 400-600 μm.
3. The method for preparing the surface wear-resistant and oxidation-resistant coating according to claim 1, wherein the adhesion promoter in the step (1) is one or a combination of polysiloxane adhesion promoter, polyurethane adhesion promoter, cyanoacetoxy adhesion promoter, aceto-acetate adhesion promoter and urea-ring adhesion promoter.
4. The method for preparing the surface wear-resistant and oxidation-resistant coating according to claim 3, wherein the adhesion promoter in the step (1) is a mixture of a polysiloxane adhesion promoter and a polyurethane adhesion promoter in a mass ratio of (1-3) to (1-3).
5. The method for preparing the surface wear-resistant and oxidation-resistant coating according to claim 1, wherein the thickener in the step (1) is one or a mixture of more of methylcellulose, ammonium polyacrylate, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene oxide and sodium polyacrylate.
6. A wear-resistant and oxidation-resistant surface coating prepared by the method of any one of claims 1 to 5.
7. Use of a surface abrasion and oxidation resistant coating according to claim 6 to improve the safety, oxidation resistance and impact resistance of an electrical heating element.
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