Preparation method of yttrium oxide thermal spraying powder for plasma etching resistant coating

Abstract

The invention relates to the technical field of thermal spraying, and discloses a preparation method of yttrium oxide thermal spraying powder for a plasma etching resistant coating, which comprises the following steps: step 1, raw material preparation: preparing required raw materials including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, a stabilizing agent, a tackifier, an anti-agglomeration agent and a thermal stabilizer; step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion; thirdly, powder treatment is conducted, specifically, the mixed powder is treated according to needs so as to ensure the uniformity and proper particle size of the powder; and 4, solvent treatment: carrying out suspension treatment on the mixed powder in a solvent, and adding a required surfactant to improve the dispersity. By adding anti-etching materials such as carbon nanotubes and aluminum oxide, the coating can show higher plasma etching resistance, so that the coating is more durable in a high-temperature plasma environment.

Description

Technical Field

[0001] The invention relates to the technical field of thermal spraying, in particular to a method for preparing yttria thermal spraying powder for plasma etching resistant coating. Background Art

[0002] Plasma etching is a commonly used surface treatment technology that requires a protective coating that can withstand extreme environments such as high temperature, acidity and alkalinity. Yttria thermal spray coatings have the advantages of high temperature resistance, chemical stability, insulation and mechanical strength, making them an ideal choice for plasma etching resistant coatings. The application of yttria in the fields of aviation, aerospace, and ceramics also shows its superior performance. It is mainly used to manufacture microwave magnetic materials and important materials for military use. It is also used as an additive for optical glass and ceramic materials, high-brightness phosphors for large-screen TVs, and other cathode ray tube coatings. It is also used to manufacture high-temperature and strong heat-resistant alloys, aircraft nozzles, etc. In recent years, yttria powder has also been used more in the electronics industry and the semiconductor industry, especially as a spray material for semiconductor etcher to prevent plasma corrosion and radiation corrosion.

[0003] The existing yttrium oxide thermal spray powder for plasma etching resistant coating has uneven mixing during the powder preparation process, improper reaction condition control or unstable raw material quality, which will cause the particle structure and component distribution of the yttrium oxide thermal spray powder to affect the uniformity and performance of the coating. At the same time, the existing yttrium oxide thermal spray powder used is often made of a single or a small amount of material. Although it has a certain effect, the plasma etching resistance of the yttrium oxide thermal spray powder will be reduced in a high-temperature plasma environment, affecting the normal use of the yttrium oxide thermal spray powder, and it is very inconvenient to use. Therefore, a preparation method of yttrium oxide thermal spray powder for plasma etching resistant coating is proposed to solve the above problems. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a method for preparing yttria thermal spray powder for plasma etching resistant coating, which solves the problem that the existing yttria thermal spray powder has poor uniformity during use and reduced plasma etching resistance in a high-temperature plasma environment.

[0005] To achieve the above objectives, the present invention is implemented through the following technical scheme: an yttrium oxide thermal spray powder for a plasma etching resistant coating, comprising 65 to 90 parts of yttrium oxide powder, 5 to 10 parts of carbon nanotubes, 3 to 8 parts of aluminum oxide nanoparticles, 1 to 6 parts of an organic resin, 1 to 3 parts of a stabilizer, 1 to 2 parts of a tackifier, 2 to 8 parts of an anti-agglomeration agent, and 1 to 3 parts of a thermal stabilizer.

[0006] Preferably, the stabilizer may be any one of lanthanum oxide and gadolinium oxide; the viscosity enhancer may be any one of polyacrylamide and polyvinyl alcohol; the anti-agglomeration agent may be any one of silica particles and alumina particles; and the thermal stabilizer may be any one of alumina, calcium silicate, magnesium silicate and rare earth element compounds.

[0007] Preferably, the yttrium oxide thermal spray powder formula also includes silicone oil or dimethyl sulfoxide for adjusting the fluidity of the yttrium oxide thermal spray powder, and contains 3 parts.

[0008] A method for preparing yttria thermal spray powder for plasma etching resistant coating comprises the following steps:

[0009] Step 1, raw material preparation: prepare the required raw materials, including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, stabilizer, viscosity enhancer, anti-agglomeration agent and thermal stabilizer;

[0010] Step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion;

[0011] Step 3, powder processing: as needed, the mixed powder is processed to ensure the uniformity of the powder and the appropriate particle size;

[0012] Step 4, solvent treatment: suspending the mixed powder in a solvent and adding a desired surfactant to improve dispersibility;

[0013] Step 5, drying: the suspended powder solvent is subjected to appropriate drying treatment;

[0014] Step 6: Screening and pulverizing: The dried powder is screened and pulverized to obtain the desired particle size and uniformity.

[0015] Preferably, after step 2, the crystal structure of the material is regulated by controlling the heat treatment temperature and atmosphere to adjust the crystal structure of yttrium oxide and affect its thermal stability and mechanical properties.

[0016] Preferably, the temperature range selected for the crystal structure regulation is 500° C. to 850° C. for 2 hours.

[0017] Preferably, after step 2, a stabilizer, a tackifier, an anti-agglomeration agent and a heat stabilizer are added to the mixed material and mixed again.

[0018] Preferably, after step three, the powder particle size of the mixed material is controlled by using an efficient ball mill and a screen to control the particle size distribution of the yttrium oxide powder.

[0019] Preferably, after step three, the diameter of the obtained material particles is 15 to 40 μm.

[0020] Preferably, after step six, the particle diameter of the obtained yttria thermal spraying powder is 70-80 μm.

[0021] The present invention provides a method for preparing yttria thermal spray powder for plasma etching resistant coating, which has the following beneficial effects:

[0022] 1. The present invention adds anti-etching materials such as carbon nanotubes and aluminum oxide, so that the coating can exhibit higher plasma etching resistance and is therefore more durable in a high-temperature plasma environment.

[0023] 2. The present invention can improve the thermal stability of the powder by adding a thermal stabilizer and a stabilizer, so that the coating can maintain structural stability under high temperature conditions and reduce changes in the crystal structure.

[0024] 3. The present invention can improve the adhesion of powder by using tackifiers and surfactants, which helps to improve the adhesion between the coating and the substrate.

[0025] 4. The present invention can prevent powder from agglomerating during storage and transportation by using an anti-agglomeration agent, thereby maintaining the uniformity of the powder. DETAILED DESCRIPTION

[0026] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0027] Embodiment 1:

[0028] The embodiment of the present invention provides a method for preparing yttrium oxide thermal spray powder for plasma etching resistant coating, comprising 80 parts of yttrium oxide powder, 8 parts of carbon nanotubes, 5 parts of aluminum oxide nanoparticles, 4 parts of organic resin, 2 parts of stabilizer, 2 parts of viscosity enhancer, 5 parts of anti-agglomeration agent, and 2 parts of thermal stabilizer. The stabilizer can be any one of lanthanum oxide and gadolinium oxide; the viscosity enhancer can be any one of polyacrylamide and polyvinyl alcohol; the anti-agglomeration agent can be any one of silicon dioxide particles and aluminum oxide particles; the thermal stabilizer can be any one of aluminum oxide, calcium silicate, magnesium silicate and rare earth element compounds. The formula of the yttrium oxide thermal spray powder also includes silicone oil or dimethyl sulfoxide for adjusting the fluidity of the yttrium oxide thermal spray powder, and contains 3 parts.

[0029] As part of the above embodiment, the present invention also provides a method for preparing yttria thermal spray powder for plasma etching resistant coating, comprising the following steps:

[0030] Step 1, raw material preparation: prepare the required raw materials, including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, stabilizer, viscosity enhancer, anti-agglomeration agent and thermal stabilizer;

[0031] Step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion;

[0032] After step 2, the crystal structure of the material is regulated by controlling the heat treatment temperature and atmosphere to adjust the crystal structure of yttrium oxide, affecting its thermal stability and mechanical properties. The selected temperature range for crystal structure regulation is: 500°C to 850°C, and it lasts for 2 hours.

[0033] After step 2, a stabilizer, a tackifier, an anti-agglomeration agent and a heat stabilizer are added to the mixed material and mixed again;

[0034] Step 3, powder processing: as needed, the mixed powder is processed to ensure the uniformity of the powder and the appropriate particle size;

[0035] After step three, the mixed material is subjected to powder particle size control, and a high-efficiency ball mill and screen are used to control the particle size distribution of the yttrium oxide powder.

[0036] After step 3, the obtained material particles have a diameter of 15 to 40 μm.

[0037] Step 4, solvent treatment: suspending the mixed powder in a solvent and adding a desired surfactant to improve dispersibility;

[0038] Step 5, drying: the suspended powder solvent is subjected to appropriate drying treatment;

[0039] Step 6, screening and crushing: the dried powder is screened and crushed to obtain the required particle size and uniformity. After step 6, the particle diameter of the obtained yttrium oxide thermal spraying powder is 70-80 μm.

[0040] Embodiment 2:

[0041] Different from the above embodiments, the embodiments of the present invention also provide a method for preparing yttrium oxide thermal spray powder for plasma etching resistant coating, including 75 parts of yttrium oxide powder, 5 parts of carbon nanotubes, 3 parts of aluminum oxide nanoparticles, 2 parts of organic resin, 1 part of stabilizer, 1 part of thickener, 2 parts of anti-agglomeration agent, and 1 part of thermal stabilizer. The stabilizer can be any one of lanthanum oxide and gadolinium oxide; the thickener can be any one of polyacrylamide and polyvinyl alcohol; the anti-agglomeration agent can be any one of silicon dioxide particles and aluminum oxide particles; the thermal stabilizer can be any one of aluminum oxide, calcium silicate, magnesium silicate and rare earth element compounds. The formula of the yttrium oxide thermal spray powder also includes silicone oil or dimethyl sulfoxide, which is used to adjust the fluidity of the yttrium oxide thermal spray powder, and contains 3 parts.

[0042] As part of the above embodiment, the present invention also provides a method for preparing yttria thermal spray powder for plasma etching resistant coating, comprising the following steps:

[0043] Step 1, raw material preparation: prepare the required raw materials, including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, stabilizer, viscosity enhancer, anti-agglomeration agent and thermal stabilizer;

[0044] Step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion;

[0045] After step 2, the crystal structure of the material is regulated by controlling the heat treatment temperature and atmosphere to adjust the crystal structure of yttrium oxide, affecting its thermal stability and mechanical properties. The selected temperature range for crystal structure regulation is: 500°C to 850°C, and it lasts for 2 hours.

[0046] After step 2, a stabilizer, a tackifier, an anti-agglomeration agent and a heat stabilizer are added to the mixed material and mixed again;

[0047] Step 3, powder processing: as needed, the mixed powder is processed to ensure the uniformity of the powder and the appropriate particle size;

[0048] After step three, the mixed material is subjected to powder particle size control, and a high-efficiency ball mill and screen are used to control the particle size distribution of the yttrium oxide powder.

[0049] After step 3, the obtained material particles have a diameter of 15 to 40 μm.

[0050] Step 4, solvent treatment: suspending the mixed powder in a solvent and adding a desired surfactant to improve dispersibility;

[0051] Step 5, drying: the suspended powder solvent is subjected to appropriate drying treatment;

[0052] Step 6, screening and crushing: the dried powder is screened and crushed to obtain the required particle size and uniformity. After step 6, the particle diameter of the obtained yttrium oxide thermal spraying powder is 70-80 μm.

[0053] Embodiment three:

[0054] Different from the above embodiments, the embodiments of the present invention also provide a method for preparing yttrium oxide thermal spray powder for plasma etching resistant coating, including 90 parts of yttrium oxide powder, 10 parts of carbon nanotubes, 8 parts of aluminum oxide nanoparticles, 4 parts of organic resin, 3 parts of stabilizer, 2 parts of thickener, 4 parts of anti-agglomeration agent, and 2 parts of thermal stabilizer. The stabilizer can be any one of lanthanum oxide and gadolinium oxide; the thickener can be any one of polyacrylamide and polyvinyl alcohol; the anti-agglomeration agent can be any one of silicon dioxide particles and aluminum oxide particles; the thermal stabilizer can be any one of aluminum oxide, calcium silicate, magnesium silicate and rare earth element compounds. The formula of the yttrium oxide thermal spray powder also includes silicone oil or dimethyl sulfoxide, which is used to adjust the fluidity of the yttrium oxide thermal spray powder, and contains 3 parts.

[0055] As part of the above embodiment, the present invention also provides a method for preparing yttria thermal spray powder for plasma etching resistant coating, comprising the following steps:

[0056] Step 1, raw material preparation: prepare the required raw materials, including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, stabilizer, viscosity enhancer, anti-agglomeration agent and thermal stabilizer;

[0057] Step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion;

[0058] After step 2, the crystal structure of the material is regulated by controlling the heat treatment temperature and atmosphere to adjust the crystal structure of yttrium oxide, affecting its thermal stability and mechanical properties. The selected temperature range for crystal structure regulation is: 500°C to 850°C, and it lasts for 2 hours.

[0059] After step 2, a stabilizer, a tackifier, an anti-agglomeration agent and a heat stabilizer are added to the mixed material and mixed again;

[0060] Step 3, powder processing: as needed, the mixed powder is processed to ensure the uniformity of the powder and the appropriate particle size;

[0061] After step three, the mixed material is subjected to powder particle size control, and a high-efficiency ball mill and screen are used to control the particle size distribution of the yttrium oxide powder.

[0062] After step 3, the obtained material particles have a diameter of 15 to 40 μm.

[0063] Step 4, solvent treatment: suspending the mixed powder in a solvent and adding a desired surfactant to improve dispersibility;

[0064] Step 5, drying: the suspended powder solvent is subjected to appropriate drying treatment;

[0065] Step 6, screening and crushing: the dried powder is screened and crushed to obtain the required particle size and uniformity. After step 6, the particle diameter of the obtained yttrium oxide thermal spraying powder is 70-80 μm.

[0066] Comparative Example 1:

[0067] The only difference from the first embodiment is that no organic resin is added to the raw material of the yttria thermal spraying powder.

[0068] Comparative Example 2:

[0069] The only difference from the first embodiment is that no anti-agglomeration agent is added to the raw material of the yttrium oxide thermal spraying powder.

[0070] Comparative Example 3:

[0071] The only difference from the first embodiment is that no heat stabilizer is added to the raw material of the yttria thermal spraying powder.

[0072] Comparative Example 4:

[0073] The only difference from the first embodiment is that, in the preparation process of the yttrium oxide thermal spraying powder, no crystal structure control treatment is performed.

[0074] The results are shown in Table 1 below.

[0075] Table 1:

[0076] Thermal stability / ℃ Adhesion strength / MPa Agglomeration index / % Etching rate nm / hour Embodiment 1 ＞1530 35 11 101 Embodiment 2 ＞1450 32 16 114 Embodiment 3 ＞1610 38 13 85 Comparative Example 1 ＞1530 32 11 119 Comparative Example 2 ＞1530 35 18 134 Comparative Example 3 ＞1360 34 11 140 Comparative Example 4 ＞1530 34 11 136

[0077] Conclusion: As shown in Table 1, by adding anti-etching materials such as carbon nanotubes and aluminum oxide to yttria thermal spray powder, the coating can exhibit higher plasma etching resistance and is therefore more durable in a high-temperature plasma environment; the addition of thermal stabilizers and stabilizers can improve the thermal stability of the powder, so that the coating can maintain structural stability under high temperature conditions and reduce changes in the crystal structure; the use of tackifiers and surfactants can improve the adhesion of the powder and help improve the adhesion between the coating and the substrate; the use of anti-agglomeration agents can prevent the powder from agglomerating during storage and transportation, thereby maintaining the uniformity of the powder.

[0078] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A yttria thermal spray powder for plasma etching resistant coating, characterized in that: The invention comprises 65-90 parts of yttrium oxide powder, 5-10 parts of carbon nanotubes, 3-8 parts of aluminum oxide nanoparticles, 1-6 parts of organic resin, 1-3 parts of stabilizer, 1-2 parts of tackifier, 2-8 parts of anti-agglomeration agent and 1-3 parts of thermal stabilizer.

2. The yttria thermal spraying powder for plasma etching resistant coating according to claim 1, characterized in that: The stabilizer may be any one of lanthanum oxide and gadolinium oxide; the viscosity enhancer may be any one of polyacrylamide and polyvinyl alcohol; the anti-agglomeration agent may be any one of silica particles and alumina particles; the thermal stabilizer may be any one of alumina, calcium silicate, magnesium silicate and rare earth element compounds.

3. The yttria thermal spraying powder for plasma etching resistant coating according to claim 1, characterized in that: The yttrium oxide thermal spray powder formula also includes silicone oil or dimethyl sulfoxide, which is used to adjust the fluidity of the yttrium oxide thermal spray powder and contains 3 parts.

4. A method for preparing yttria thermal spray powder for plasma etching resistant coating, characterized in that: Using the yttria thermal spraying powder for plasma etching resistant coating according to any one of claims 1 to 3 comprises the following steps: Step 1, raw material preparation: prepare the required raw materials, including yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles, stabilizer, viscosity enhancer, anti-agglomeration agent and thermal stabilizer; Step 2, material mixing: uniformly mixing yttrium oxide powder, carbon nanotubes, aluminum oxide nanoparticles and organic resin according to a required proportion; Step 3, powder processing: as needed, the mixed powder is processed to ensure the uniformity of the powder and the appropriate particle size; Step 4, solvent treatment: suspending the mixed powder in a solvent and adding a desired surfactant to improve dispersibility; Step 5, drying: the suspended powder solvent is subjected to appropriate drying treatment; Step 6: Screening and pulverizing: The dried powder is screened and pulverized to obtain the desired particle size and uniformity.

5. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 4, characterized in that: After step 2, the crystal structure of the material is regulated by controlling the heat treatment temperature and atmosphere to adjust the crystal structure of yttrium oxide and affect its thermal stability and mechanical properties.

6. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 5, characterized in that: The temperature range selected for the crystal structure regulation is 500° C. to 850° C., and lasts for 2 hours.

7. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 4, characterized in that: After step 2, stabilizer, tackifier, anti-agglomeration agent and heat stabilizer are added to the mixed material and mixed again.

8. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 4, characterized in that: After step three, the powder particle size of the mixed material is controlled by using an efficient ball mill and a screen to control the particle size distribution of the yttrium oxide powder.

9. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 4, characterized in that: After step three, the diameter of the obtained material particles is 15 to 40 μm.

10. The method for preparing yttria thermal spray powder for plasma etching resistant coating according to claim 4, characterized in that: After step six, the particle diameter of the obtained yttrium oxide thermal spraying powder is 70-80 μm.