CN110903074A - High-temperature oxidation-resistant coating on surface of silicon carbide substrate and preparation method thereof - Google Patents
High-temperature oxidation-resistant coating on surface of silicon carbide substrate and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of inorganic materials, and particularly relates to a high-temperature oxidation-resistant coating on the surface of a silicon carbide substrate and a preparation method thereof. The high-temperature oxidation resistant coating on the surface of the silicon carbide substrate is characterized by comprising 20-100 percent of Al by weight percent2O30 to 80% of mullite and 0 to 3% of TiO2，0～30％SiO2And 0-10 nm of alumina powder. The invention improves the durability of the high-temperature oxidation resistant coating on the surface of the silicon carbide substrate, and the coating not only has good bonding strength with the substrate material in the use process for a longer period, but also does not have the problems of adhesion, coloring and the like with the fired product, thereby meeting the use requirements of various ceramic customersAnd (4) requiring.
Description
Technical Field
The invention belongs to the technical field of inorganic materials, and particularly relates to a high-temperature oxidation-resistant coating on the surface of a silicon carbide substrate and a preparation method thereof.
Background
The silicon carbide material has excellent high-temperature mechanical properties such as high-temperature strength, creep resistance, high thermal conductivity, thermal shock resistance and the like, so that the silicon carbide material becomes an ideal choice for materials such as high-temperature structural materials, electric heating elements and the like.
At higher temperature, the compact silicon dioxide film formed at low temperature has different expansion coefficient from silicon carbide, so that cracks are easily formed by repeated heating and cooling, the silicon carbide resistivity is increased, and the service life is shortened. In order to improve the durability of the silicon carbide material used under high temperature conditions, it is effective to coat the surface thereof with a coating. The coating on the surface of the silicon carbide substrate material can prevent oxygen from diffusing and permeating or reacting with oxygen to generate a protective glass phase so as to isolate the silicon carbide substrate material from external oxygen and achieve the purpose of oxidation resistance.
In order to improve the service life of silicon carbide materials, the following properties of the coating are required:
1. the permeability of oxygen is low so that the diffusion of oxygen is effectively prevented. And the function of a medium and matrix shielding layer is realized.
2. Has a self-healing function, i.e. a function of reacting with oxygen to generate a dense and uniform oxide in situ, thus sealing the cracks, which will allow the oxygen to be consumed before reaching the substrate.
3. High-temperature thermal stability, difficult volatilization and stable thermal shock resistance of the coating.
4. The thermal expansion coefficient of the coating and the base body is similar, otherwise, the thermal stress is caused by the temperature change, the crack is initiated to be initiated and expanded, and finally the coating is peeled off from the base body.
5. The high-temperature binding force is strong, the adhesive force with the matrix is good, and the problem of the combination of oxide and non-oxide ceramic is solved.
6. The coating is high temperature resistant, corrosion resistant and adhesion resistant, and the service life of the coating is greatly prolonged compared with that of the traditional coating.
Disclosure of Invention
In order to meet the requirements of the prior art, the invention provides a high-temperature oxidation-resistant coating on the surface of a silicon carbide substrate and a preparation method thereof, aiming at improving the service durability of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate, wherein the coating not only can have good bonding strength with a substrate material in a longer-period use process, but also can not cause the problems of adhesion, coloring and the like with a fired product, thereby meeting the use requirements of various ceramic customers.
The high-temperature oxidation resistant coating on the surface of the silicon carbide substrate consists of 20 to 100 percent of Al in percentage by weight2O30 to 80% of mullite and 0 to 3% of TiO2、0～30％SiO2And 0-10% of nano alumina powder.
Wherein, said Al2O3And mullite powder with the granularity of 300-500 meshes, wherein the SiO is2And ZrO2The granularity of the powder is 800-1500 meshes.
The TiO is2And (4) stabilizing.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate comprises the following steps:
(1) putting the raw materials into a ball milling tank for ball milling;
(2) adding methyl cellulose (CMC) accounting for 2-3 percent of the weight of the raw materials, polyvinyl alcohol (PVA) accounting for 5-10 percent of the weight of the raw materials and deionized water accounting for 50-80 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls with the weight 1.5-3 times that of the raw materials into a ball milling tank, and carrying out ball milling for 8-20 h to obtain a coating material;
(4) and spraying the coating layer on the silicon carbide substrate to obtain the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate.
Wherein the raw material comprises 20-100% of Al by weight percent2O30 to 80% of mullite and 0 to 3% of TiO2、0～30％SiO2And 0-10% of nano alumina powder.
And (4) after the coating layer is sprayed on the silicon carbide substrate, oxidizing and sintering the silicon carbide substrate for 2 to 3 times at the temperature of 1300-1500 ℃.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
the invention provides a high-temperature oxidation resistant coating on the surface of a silicon carbide substrate and a preparation method thereof2Is added for improving the compactness and the toughness of the coatingAdding SiO2In order to increase the content of this component in the raw material to form a more dense oxide film. Wherein the alumina can react with SiO generated on the surface of the substrate in the sintering process2The reaction further forms mullite phase, and the chemical reaction between the coating and the substrate can greatly increase the bonding strength between the coating and the substrate. The thermal expansion coefficients of the mullite and the SiC matrix in the coating are highly consistent, so that the generation of thermal stress in the heating process can be reduced, the coating is prevented from generating cracks or falling off, and the service life of the coating is prolonged. ZrO with higher melting point is also added in the scheme2ZrO used2Must be stabilized, otherwise, the crystal transformation at 1200 ℃ causes cracks and falling off.
The granularity of the raw materials is combined with the fineness, so that the spraying performance of slurry is ensured, and the compactness of the coating is improved.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment comprises 60 percent of Al in percentage by weight2O337% mullite and 3% TiO2And (4) forming.
Wherein, said Al2O3And mullite powder with the granularity of 300-500 meshes, wherein the TiO is2And (4) stabilizing.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) mixing 60% of Al according to weight percentage2O337% mullite and 3% TiO2Putting the raw materials into a ball milling tank for ball milling;
(2) adding CMC accounting for 3 percent of the weight of the raw materials, PVA accounting for 6 percent of the weight of the raw materials and deionized water accounting for 75 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls 2 times of the weight of the raw materials into a ball milling tank, carrying out ball milling for 10 hours to obtain a coating material, and detecting the performance of the coating material: fluidity of 15-30s, ratioWeight of 1.5-1.8g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
In this example, TiO was added2The coating is a coating with high temperature resistance less than 1200 ℃ in order to improve the compactness and the toughness of the coating.
Example 2
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment comprises 60 percent of Al in percentage by weight2O325% mullite and 15% SiO2And (4) forming.
Wherein, said Al2O3And mullite powder with the granularity of 300-500 meshes, wherein the SiO is2The granularity of the powder is 800-1500 meshes.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) mixing 60% of Al according to weight percentage2O325% mullite and 15% SiO2Putting the raw materials into a ball milling tank for ball milling;
(2) adding CMC accounting for 2 percent of the weight of the raw materials, PVA accounting for 8 percent of the weight of the raw materials and deionized water accounting for 70 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls 2 times of the weight of the raw materials into the ball milling tank, carrying out ball milling for 20 hours to obtain a coating material, and detecting the performance of the coating material: fluidity of 20-30s, specific gravity of 1.5-1.7g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
In this example, SiO was added2In order to increase the content of this component in the feedstock to form a more dense oxidationA film which is a coating resistant to high temperatures of 1200 ℃ to 1350 ℃.
Example 3
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment comprises 20 percent of Al in percentage by weight2O3And 80% mullite.
Wherein, said Al2O3And the granularity of the mullite powder is 300-500 meshes.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) according to the weight percentage, 20 percent of Al2O3And 80% mullite in a ball milling tank;
(2) adding CMC accounting for 2.5 percent of the weight of the raw materials, PVA accounting for 6 percent of the weight of the raw materials and deionized water accounting for 70 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls 2 times of the weight of the raw materials into the ball milling tank, carrying out ball milling for 20 hours to obtain a coating material, and detecting the performance of the coating material: fluidity of 22-30s, specific gravity of 1.6-1.8g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
In this embodiment, the low content of alumina is formed with SiO generated on the surface of the substrate during the firing process2The reaction takes place further to form the mullite phase. The chemical reaction between the coating and the substrate can greatly increase the bonding strength between the two. The overall content of the mullite in the coating is high and is highly consistent with the thermal expansion coefficient of the substrate, the service life of the coating is further prolonged, and the coating is high-temperature-resistant and capable of resisting 1200-1400 ℃.
Example 4
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment is composed of, by weight, 70% of Al2O315% mullite and 15% ZrO2And (4) forming.
Wherein, said Al2O3And the granularity of mullite powder is 300-500 meshes, wherein ZrO is2The granularity of the powder is 800-1500 meshes.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) according to the weight percentage, 70 percent of Al2O315% mullite and 15% ZrO2Putting the raw materials into a ball milling tank for ball milling;
(2) adding CMC accounting for 3 percent of the weight of the raw materials, PVA accounting for 10 percent of the weight of the raw materials and deionized water accounting for 80 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls with the weight 1.5 times of that of the raw materials into a ball milling tank, carrying out ball milling for 15 hours to obtain a coating material, and detecting the performance of the coating material: fluidity of 20-30s, specific gravity of 1.6-1.8g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
High melting point Al in this example2O3High content and addition of higher melting point ZrO2ZrO used2Must be subjected to a stabilizing treatment, otherwise, the 1200 ℃ crystal transformation causes cracks and falling off, and the coating is high-temperature resistant at 1350 ℃ and 1550 ℃.
Example 5
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment comprises 80 percent of Al by weight percentage2O310 percent of mullite and 10 percent of nano alumina powder.
Wherein, said Al2O3And the granularity of the mullite powder is 300-500 meshes.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) according to the weight percentage, the following components are added80％Al2O3Putting raw materials of 10% of mullite and 10% of nano alumina powder into a ball milling tank for ball milling;
(2) adding CMC accounting for 2 percent of the weight of the raw materials, PVA accounting for 6 percent of the weight of the raw materials and deionized water accounting for 75 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls with 3 times of the weight of the raw materials into the ball milling tank, carrying out ball milling for 15 hours to obtain a coating material, and detecting the performance of the coating material: the fluidity is 17-30s, and the specific gravity is 1.5-1.8g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
The nano alumina powder is added in the embodiment to increase the compactness of the coating, which is a coating resistant to high temperature of 1350-.
Example 6
The high temperature oxidation resistant coating on the surface of the silicon carbide substrate of the embodiment comprises 95% of Al by weight percent2O3And 5% mullite.
Wherein, said Al2O3And the granularity of the mullite powder is 300-500 meshes.
The preparation method of the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate of the embodiment comprises the following steps:
(1) according to the weight percentage, 95 percent of Al2O3And 5% mullite in a ball milling tank;
(2) adding CMC accounting for 2.5 percent of the weight of the raw materials, PVA accounting for 6 percent of the weight of the raw materials and deionized water accounting for 75 percent of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls with 3 times of the weight of the raw materials into the ball milling tank, carrying out ball milling for 15 hours to obtain a coating material, and detecting the performance of the coating material: fluidity of 20-30s, specific gravity of 1.5-1.7g/cm3；
(4) The coating layer is sprayed on the silicon carbide substrate, the substrate is thoroughly cleaned and dried before spraying, and impurities are prevented from being introduced in the process. During the spraying process, the coating thickness is uniform, and the excessive thickness of the coating is avoided, generally less than 0.5mm, so that the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate is obtained.
Extremely high Al in this example2O3The content is a coating which resists high temperature of 1400 ℃ and 1550 ℃ by virtue of good high-temperature performance.
The spraying mode enables the coating material to be attached to the substrate conveniently and quickly, but the binding force between the coating and the substrate is relatively poor. In order to improve the defect, before the loaded product is used, the loaded product can be oxidized and sintered for 2-3 times at the temperature of 1300-1500 ℃, so that the binding force between the coating and the substrate can be obviously improved.
The coated plate of the embodiment is subjected to idle firing for 10 circulating heats in the air atmosphere at corresponding temperature sections, and the coating does not crack or fall off, which shows that the coating of the embodiment has good service performance.
Claims (6)
1. The high temperature antioxidant coating on the surface of silicon carbide substrate is characterized by comprising 20-100 percent of Al by weight percent2O30 to 80% of mullite and 0 to 3% of TiO2、0～30％SiO2And 0-10% of nano alumina powder.
2. The high temperature oxidation resistant coating for the surface of a silicon carbide substrate as claimed in claim 1, wherein said Al is selected from the group consisting of Al, Cu, Al, Cu2O3And mullite powder with the granularity of 300-500 meshes, wherein the SiO is2And ZrO2The granularity of the powder is 800-1500 meshes.
3. The high temperature oxidation resistant coating as claimed in claim 1, wherein the TiO is selected from the group consisting of2And (4) stabilizing.
4. A preparation method of a high-temperature oxidation-resistant coating on the surface of a silicon carbide substrate is characterized by comprising the following steps:
(1) putting the raw materials into a ball milling tank for ball milling;
(2) adding methyl cellulose accounting for 2-3% of the weight of the raw materials, polyvinyl alcohol accounting for 5-10% of the weight of the raw materials and deionized water accounting for 50-80% of the weight of the raw materials into a ball milling tank;
(3) adding grinding balls with the weight 1.5-3 times that of the raw materials into a ball milling tank, and carrying out ball milling for 8-20 h to obtain a coating material;
(4) and spraying the coating layer on the silicon carbide substrate to obtain the high-temperature oxidation-resistant coating on the surface of the silicon carbide substrate.
5. The method for preparing a high-temperature oxidation-resistant coating on the surface of a silicon carbide substrate as claimed in claim 4, wherein the raw material comprises, by weight, 20-100% of Al2O30 to 80% of mullite and 0 to 3% of TiO2、0～30％SiO2And 0-10% of nano alumina powder.
6. The method as claimed in claim 4, wherein the coating layer is applied by spraying on the silicon carbide substrate in the step (4), and then the silicon carbide substrate is oxidized and fired at 1300-1500 ℃ for 2-3 times.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811084199.5A CN110903074A (en) | 2018-09-17 | 2018-09-17 | High-temperature oxidation-resistant coating on surface of silicon carbide substrate and preparation method thereof |
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| CN201811084199.5A CN110903074A (en) | 2018-09-17 | 2018-09-17 | High-temperature oxidation-resistant coating on surface of silicon carbide substrate and preparation method thereof |
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| CN110903074A true CN110903074A (en) | 2020-03-24 |
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