A method for preparing an anti-etching ceramic coating material

Abstract

The present invention discloses a method for preparing an etch-resistant ceramic coating material, by introducing elements such as Al, Sc, Yb, La, and forming an entropy-stabilized material with yttrium oxide, optimizing its chemical composition and crystal structure, thereby preparing a coating with high density, high bonding strength and excellent etch-resistant performance. By adopting an improved spray granulation process, a powder with controllable particle size and a narrow distribution range is prepared, and combined with suspension plasma spraying technology, the uniformity, density and low surface roughness of the coating are achieved. The coating material of the present invention has high-temperature stability, chemical inertness and excellent etch-resistant performance in extreme working environments, and can meet the long-term stable operation requirements of high-end precision equipment such as semiconductor manufacturing and photolithography equipment, and provide a reliable protection solution for these devices. Therefore, the present invention not only promotes the application progress of yttrium oxide materials in the field of etch-resistant coatings, but also effectively improves the performance and reliability of coatings in related fields.

Description

Technical Field

[0001] The invention relates to the technical field of material surface engineering, in particular to a method for preparing an etching-resistant ceramic coating material. Background Art

[0002] In semiconductor manufacturing and lithography equipment, components are often exposed to extremely harsh operating environments, such as high temperatures, vacuum, high-energy particle bombardment, and highly corrosive gas environments. These complex operating conditions place stringent demands on material performance, with the most prominent challenge being the combined effects of chemical corrosion, thermal stress, and plasma erosion. This not only leads to rapid failure of precision equipment components but also directly impacts the manufacturing quality of semiconductor chips and the operating life of lithography equipment. Currently, key materials for etch resistance include oxides such as aluminum oxide, zirconium oxide, and yttrium oxide (Y2O3). Yttrium oxide has become a research hotspot due to its unique physical and chemical properties. This material has a high melting point (approximately 2430°C), low vapor pressure, extremely strong chemical stability, and excellent resistance to plasma impact. During semiconductor manufacturing, particularly during etching, cleaning, and deposition, component surfaces are often exposed to high-energy plasma. In these situations, yttrium oxide coatings can effectively block the corrosive effects of plasma, significantly improving equipment reliability and durability.

[0003] However, traditional yttrium oxide coating preparation technologies (such as thermal spraying) still face many challenges in practical applications. First, thermal spraying technology uses powder as raw material, and the prepared coatings often have a high porosity, which makes them exhibit limited corrosion resistance in corrosive media. In addition, the bonding method between the coating and the substrate in thermal spraying is mostly mechanical bonding, which has low bonding strength and is prone to failure due to peeling during long-term use. As semiconductor processes continue to develop towards higher precision and more stringent working conditions, traditional thermal spray coatings can no longer meet the requirements for density, bonding strength and long-term high stability.

[0004] To overcome the limitations of traditional coating technologies, suspension plasma spraying (SPS) has gained increasing attention in recent years. This technology, combined with spray granulation and using a suspension as the coating raw material, effectively addresses the large particle size and poor flowability of powders commonly found in traditional thermal spraying. The uniform dispersion of micron-sized spherical powders within the suspension enables more precise coating deposition and significantly improves the density and uniformity of the coating. Furthermore, SPS technology can achieve coating structures with lower porosity, enhancing corrosion resistance. By manipulating granulation and plasma spraying parameters, the suspension properties and the adhesion between the coating and the substrate can be further optimized. While suspension plasma spraying holds great promise for the preparation of yttrium oxide coatings, several technical bottlenecks remain. For example, the stability of the suspension significantly impacts the ultimate coating performance. Optimizing the powder granulation process to improve the dispersion and flowability of the powder remains an urgent challenge. Furthermore, during the plasma spraying process, if the particle size distribution is wide and the fluidity is poor, agglomeration and nozzle clogging are likely to occur, affecting the coating's uniformity and corrosion resistance. Furthermore, existing pure yttrium oxide coatings have poor oxygen barrier properties, which negatively impacts the substrate during re-service. Therefore, there is an urgent need to develop a coating material that can achieve a dense coating with minimal surface roughness and resistance to etching and oxidation to meet the demands of high-performance equipment. Summary of the Invention

[0005] The purpose of this section is to summarize some aspects of the embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the abstract and title of this application to avoid blurring the purpose of this section, the abstract and the title of the invention, and such simplifications or omissions should not be used to limit the scope of the present invention.

[0006] Therefore, the present invention aims to provide a method for preparing an etch-resistant ceramic coating material by overdoping it with rare earth elements, optimizing the coating's microstructure and enhancing its corrosion resistance. In particular, the incorporation of rare earth elements (such as Yb and Sc) significantly improves the coating's oxidation resistance and effectively slows oxygen ion diffusion.

[0007] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:

[0008] A method for preparing an anti-etching ceramic coating material, comprising the following steps:

[0009] S1. High-purity yttrium oxide Y2O3 and scandium oxide Sc2O3 or ytterbium oxide Yb2O3 or aluminum oxide Al2O3 or lanthanum oxide La2O3 are mixed in a molar ratio according to a stoichiometric ratio to form a multi-element stable body composition;

[0010] S2. Add ZrO2 ball milling beads to the multi-stabilizer composition, and fully ball mill for 1-8 hours using ethanol or deionized water as a dispersion medium to form a slurry;

[0011] S3, drying the ball-milled slurry to constant weight and sieving it using a 200-mesh sieve;

[0012] S4. Prepare a slurry with a solid content of 20-40 wt%, and adjust the slurry viscosity to 10-50 mPa·s;

[0013] S5, granulating the slurry treated in step S4 using a spray drying device to obtain granular powder with a particle size distribution of 0.5 μm to 50 μm;

[0014] S6. Disperse the spray-granulated powder in an ethanol-water mixed solution, add a dispersant, and use an ultrasonic dispersing device for 15-60 minutes, accompanied by magnetic stirring to ensure that the suspension is evenly dispersed;

[0015] S7. Select the base material and improve the surface roughness by sandblasting or chemical cleaning;

[0016] S8. Use suspension plasma spraying equipment to spray the suspension obtained in step S6 onto the base material. During the spraying process, the coating thickness is controlled to be 30-200 μm and the spraying rate is 5-30 μm / min. After spraying, high-temperature sintering treatment is performed, and the heat is kept for 1-8 hours, and then cooled to room temperature at a rate of 5-10°C / min to form a ceramic coating material.

[0017] As a preferred embodiment of the method for preparing an anti-etching ceramic coating material according to the present invention, in step S1, the multi-stabilizing body composition is Y 1-x Sc x O 1.5 , 0.1≤x≤0.5 or Y 1-x Yb x O 1.5 , 0.1≤x≤0.5 or Y 1-x La x O 1.5 , 0.1≤x≤0.5 or Y 1-x (Sc 1-y Yb y ) x O 1.5 , 0.1≤x≤0.5, 0.1≤y≤0.5) or Y 1-x (Al 1- y Yb y ) x O 1.5, 0.1≤x≤0.5, 0.1≤y≤0.5.

[0018] As a preferred embodiment of the method for preparing an anti-etching ceramic coating material described in the present invention, in step S5, the inlet temperature of the spray drying equipment is set to 150-200°C, the outlet temperature is 80-120°C, the atomizer speed is 12500r / min-21000r / min, and the atomization pressure is 0.2-0.5MPa.

[0019] As a preferred embodiment of the method for preparing an anti-etching ceramic coating material according to the present invention, the volume fraction of ethanol in the ethanol-water mixed solution in step S6 is 70-90%.

[0020] As a preferred solution of the method for preparing an anti-etching ceramic coating material according to the present invention, in step S6, the dispersant is polyvinyl pyrrolidone (PVP) or polyvinyl alcohol (PVA), and the concentration is 0.1-0.5 wt %.

[0021] As a preferred embodiment of the method for preparing an anti-etching ceramic coating material described in the present invention, in step S8, the spraying parameters of the suspension plasma spraying equipment are: plasma gas flow rate: argon main gas 40-80 slpm, hydrogen auxiliary gas 5-20 slpm; current and voltage: current 300-600 A, voltage 40-90 V; spraying distance: 50-100 mm; feed rate: 2-50 mL / min.

[0022] As a preferred embodiment of the method for preparing an anti-etching ceramic coating material according to the present invention, in step S8, the high-temperature sintering heating rate is 5-10°C / min, from room temperature to 1100-1500°C.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] 1. The present invention introduces elements such as Al, Sc, Yb, La, and forms an entropy-stabilized material with yttrium oxide to optimize its chemical composition and crystal structure, thereby preparing a coating with high density, high bonding strength and excellent etching resistance. By adopting an improved spray granulation process, a powder with controllable particle size and narrow distribution range is prepared, and combined with suspension plasma spraying (SPS) technology, the uniformity, density and low surface roughness of the coating are achieved. The coating material of the present invention has high temperature stability, chemical inertness and excellent etching resistance in extreme working environments, and can meet the long-term stable operation requirements of high-end precision equipment such as semiconductor manufacturing and photolithography equipment, and provide reliable protection solutions for these devices. Therefore, the present invention not only promotes the application progress of yttrium oxide materials in the field of anti-etching coatings, but also effectively improves the performance and reliability of coatings in related fields.

[0025] 2. By optimizing the doping ratio and combination of rare earth elements (e.g., the ratio of Yb, Sc, and La), the present invention can improve the coating's resistance to plasma erosion and chemical corrosion while ensuring the coating's density and adhesion to the substrate. Therefore, the coating material of the present invention not only has excellent etch resistance but also provides long-term, stable protection for high-precision industrial equipment such as semiconductor manufacturing and photolithography equipment. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be derived from these drawings without inventive effort. Among them:

[0027] Figure 1 The XRD pattern of the ceramic coating prepared in Example 1 of the present invention;

[0028] Figure 2 This is a cross-sectional SEM image of the ceramic coating prepared in Example 1 of the present invention;

[0029] Figure 3 Schematic diagram of characterization of the surface roughness of the ceramic coating prepared in Example 1 of the present invention;

[0030] Figure 4 Schematic diagram of characterization of the surface roughness of the ceramic coating prepared in Example 2 of the present invention;

[0031] Figure 5 Schematic diagram of characterization of the surface roughness of the ceramic coating prepared in Example 5 of the present invention;

[0032] Figure 6 This is a schematic diagram of the surface morphology of the ceramic coating prepared in Example 7 of the present invention;

[0033] Figure 7 Schematic diagram showing the characterization of the surface roughness of the ceramic coating prepared in Example 7 of the present invention;

[0034] Figure 8 Schematic diagram of characterization of the surface roughness of the ceramic coating prepared in Example 8 of the present invention. DETAILED DESCRIPTION

[0035] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below with reference to the accompanying drawings.

[0036] The present invention provides a method for preparing an anti-etching ceramic coating material by overdoping with rare earth elements, optimizing the coating's microstructure and enhancing its corrosion resistance. In particular, the incorporation of rare earth elements (such as Yb and Sc) significantly improves the coating's oxidation resistance and effectively slows oxygen ion diffusion. Specific examples are as follows:

[0037] Example 1

[0038] S1, using Y2O3 and Yb2O3 as raw materials, according to the molar ratio of Y 0.8 Yb 0.2 O 1.5 Mix.

[0039] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0040] S3. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 18,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 12 μm and D90 = 20 μm.

[0041] S4. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0042] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0043] S6. After spraying, sintering treatment was carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept warm for 3 hours, and then cooled to room temperature at 3°C / min. The final coating was dense and uniform with a surface roughness of Sq = 2.2172 μm.

[0044] Example 2

[0045] S1, using Y2O3 and La2O3 as raw materials, according to the molar ratio of Y 0.7 La 0.3 O 1.5 Mix.

[0046] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0047] S3. The ball-milled slurry was sieved (200 mesh) and dried at 120° C. to constant weight.

[0048] S4. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 18,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 10 μm and D90 = 18 μm.

[0049] S5. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0050] S6. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60slpm, hydrogen auxiliary gas flow rate 10slpm, current 500A, voltage 60V, spraying distance 80mm, feed rate 3mL / min, and control the coating thickness to 50μm.

[0051] S7. After spraying, sintering treatment is carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept at this temperature for 3 hours, and then cooled to room temperature at 3°C / min. The final coating is dense and uniform with a surface roughness of Sq = 1.7575 μm.

[0052] Example 3

[0053] S1, using Y2O3 and Sc2O3 as raw materials, according to the molar ratio of Y 0.8 Sc 0.2 O 1.5 Mix.

[0054] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0055] S3. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 18,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 12 μm and D90 = 20 μm.

[0056] S4. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0057] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0058] S6. After spraying, sintering treatment was carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept warm for 3 hours, and then cooled to room temperature at 3°C / min. The final coating was dense and uniform with a surface roughness of Sq = 2.2172 μm.

[0059] Example 4

[0060] S1, using Y2O3 and Yb2O3 as raw materials, according to the molar ratio of Y 0.8 Yb 0.2 O 1.5 Mix.

[0061] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0062] S3. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 18,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 12 μm and D90 = 20 μm.

[0063] S4. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0064] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 50 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0065] S6. After spraying, sintering treatment was carried out, with a heating rate of 5°C / min from room temperature to 1300°C, kept at this temperature for 3 hours, and then cooled to room temperature at 3°C / min. The final coating was dense and uniform, with a surface roughness of Sq = 2.2172 μm

[0066] Example 5

[0067] S1, using Y2O3 and Yb2O3 as raw materials, according to the molar ratio of Y 0.8 Yb 0.2 O 1.5 Mix.

[0068] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0069] S3. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 15,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 12 μm and D90 = 20 μm.

[0070] S4. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0071] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0072] S6. After spraying, sintering treatment was carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept warm for 3 hours, and then cooled to room temperature at 3°C / min. The final coating was dense and uniform with a surface roughness of Sq = 2.2172 μm.

[0073] Example 6

[0074] S1, using Y2O3 and Yb2O3 as raw materials, according to the molar ratio of Y 0.8 Yb 0.2 O 1.5 Mix.

[0075] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0076] S3. Prepare a slurry with a solid content of 30 wt%, adjust the viscosity to 45 mPa·s, and then pass it through a spray drying equipment with the inlet temperature set at 180°C, the outlet temperature set at 100°C, the atomizer speed set at 18,000 r / min, and the atomizing air pressure set at 0.3 MPa to obtain a powder with a particle size distribution in the range of D10 = 12 μm and D90 = 20 μm.

[0077] S4. The spray-dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% sodium polyacrylate was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0078] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0079] S6. After spraying, sintering treatment was carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept warm for 3 hours, and then cooled to room temperature at 3°C / min. The final coating was dense and uniform with a surface roughness of Sq = 2.2172 μm.

[0080] Example 7

[0081] S1, using Y2O3 and La2O3 as raw materials, according to the molar ratio of Y 0.7 La 0.3 O 1.5 Mix.

[0082] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling. The ball milling time was 0.5 hours to ensure that the slurry was evenly mixed.

[0083] S3. The ball-milled slurry was sieved (200 mesh) and dried at 120° C. to constant weight.

[0084] S4. The dried powder was dispersed in an ethanol-water mixed solution (ethanol volume fraction was 80%), 0.3 wt% polyvinylpyrrolidone (PVP) was added as a dispersant, and ultrasonic treatment was performed for 30 minutes to ensure a uniform suspension.

[0085] S5. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 50 μm.

[0086] S6. After spraying, sintering treatment is carried out with a heating rate of 5°C / min from room temperature to 1300°C, keeping the temperature for 3 hours, and then cooling to room temperature at 3°C / min.

[0087] S7. The final coating has poor density and surface roughness Sq = 11.1672 μm.

[0088] Example 8

[0089] S1, using Y2O3 and Yb2O3 as raw materials, according to the molar ratio of Y 0.8 Yb 0.2 O 1.5 Mix.

[0090] S2. The above raw materials were passed through a planetary high-energy ball mill with ethanol as the dispersion medium, and ZrO2 ball milling beads were added for ball milling for 4 hours to ensure that the slurry was evenly mixed.

[0091] S3. Disperse the dried powder in an ethanol-water mixed solution (ethanol volume fraction is 80%), add 0.3 wt % polyvinylpyrrolidone (PVP) as a dispersant, and perform ultrasonic treatment for 30 minutes to ensure a uniform suspension.

[0092] S4. Use suspension plasma spraying (SPS) equipment to spray on the single crystal silicon substrate. The spraying parameters are as follows: argon flow rate 60 slpm, hydrogen auxiliary gas flow rate 10 slpm, current 500 A, voltage 60 V, spraying distance 80 mm, feed rate 3 mL / min, and control the coating thickness to 100 μm.

[0093] S5. After spraying, sintering treatment was carried out with a heating rate of 5°C / min from room temperature to 1300°C, kept warm for 3 hours, and then cooled to room temperature at 3°C / min. The final coating had poor density and a surface roughness of Ra = 10.9 μm.

[0094] The coatings prepared in Examples 1 to 8 were subjected to performance tests, as follows:

[0095] 1. The coating prepared in Example 1 was subjected to X-ray diffraction test, and the results were as follows: Figure 1 As shown by Figure 1 It can be concluded that the ceramic coating prepared by the present invention has good crystallinity.

[0096] 2. Scanning electron microscope analysis was performed on the ceramic coating interface prepared in Example 1. Figure 2 As shown in the figure, the surface coating is dense inside with a density of 97% and no obvious pores.

[0097] 3. The surface roughness of the ceramic coating prepared in Example 1 was characterized as follows: Figure 3 As shown, the surface roughness was found to be relatively low, only Sq = 2.2172 μm.

[0098] 4. Scanning electron microscope analysis was performed on the cross section of the ceramic coating prepared in Example 2. Figure 4 As shown, the coating is also dense, with no obvious pores, and the density reaches 99%. The surface roughness is low, only Sq = 1.7575 μm.

[0099] 5. Scanning electron microscope analysis of the cross section of the ceramic coating prepared in Example 3 revealed that the interior of the coating was also dense, with no obvious pores, and the density could also reach 99%.

[0100] 6. Scanning electron microscopy analysis of the cross section of the ceramic coating prepared in Example 4 revealed that the surface roughness of the coating was slightly increased.

[0101] 7. Scanning electron microscope analysis was performed on the cross section of the ceramic coating prepared in Example 5. Figure 5 As shown, it was found that the internal density of the coating was reduced to 90%, and the surface roughness Sq = 5.1213 μm.

[0102] 8. Scanning electron microscopy analysis of the cross section of the ceramic coating prepared in Example 6 revealed that the coating was dense internally, with a density of approximately 97%.

[0103] 9. Scanning electron microscope analysis was performed on the cross section of the ceramic coating prepared in Example 7. Figure 7 and Figure 8 As shown in the figure, the coating surface has large fluctuations due to insufficient slurry fluidity, and the surface roughness Ra = 16.8 μm.

[0104] 10. Scanning electron microscope analysis was performed on the cross section of the ceramic coating prepared in Example 8. Figure 8 As shown in the figure, the coating surface has large fluctuations due to the insufficient fluidity of the slurry, and the surface roughness Ra = 10.9 μm.

[0105] Although the present invention has been described above with reference to embodiments, various modifications may be made thereto and equivalent components may be substituted without departing from the scope of the present invention. In particular, as long as there are no structural conflicts, the various features of the embodiments disclosed herein may be combined with each other in any manner, and the omission of an exhaustive description of such combinations in this specification is solely for the sake of space and resource conservation. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for preparing an etching-resistant ceramic coating material, characterized in that: Here are the steps: S1. High-purity yttrium oxide Y2O3 and scandium oxide Sc2O3 or ytterbium oxide Yb2O3 or aluminum oxide Al2O3 or lanthanum oxide La2O3 are mixed in a molar ratio according to a stoichiometric ratio to form a multi-element stable body composition; S2. Add ZrO2 ball milling beads to the multi-stabilizer composition, and fully ball mill for 1-8 hours using ethanol or deionized water as a dispersion medium to form a slurry; S3, drying the ball-milled slurry to constant weight and sieving it using a 200-mesh sieve; S4. Prepare a slurry with a solid content of 20-40 wt%, and adjust the slurry viscosity to 10-50 mPa·s; S5, granulating the slurry treated in step S4 using a spray drying device to obtain granular powder with a particle size distribution of 0.5 μm to 50 μm; S6. Disperse the spray-granulated powder in an ethanol-water mixed solution, add a dispersant, and use an ultrasonic dispersing device for 15-60 minutes, accompanied by magnetic stirring to ensure that the suspension is evenly dispersed; S7. Select the base material and improve the surface roughness by sandblasting or chemical cleaning; S8. Use suspension plasma spraying equipment to spray the suspension obtained in step S6 onto the base material. During the spraying process, the coating thickness is controlled to be 30-200 μm and the spraying rate is 5-30 μm / min. After spraying, high-temperature sintering treatment is performed, and the heat is kept for 1-8 hours, and then cooled to room temperature at a rate of 5-10°C / min to form a ceramic coating material.

2. The method for preparing an etching-resistant ceramic coating material according to claim 1, characterized in that: In step S1, the multi-stable body composition is Y 1-x Sc x O 1.5 , 0.1≤x≤0.5 or Y 1-x Yb x O 1.5 , 0.1≤x≤0.5 or Y 1- x La x O 1.5 , 0.1≤x≤0.

5.

3. The method for preparing an etching-resistant ceramic coating material according to claim 1, characterized in that: In step S5, the inlet temperature of the spray drying equipment is set to 150-200°C, the outlet temperature is 80-120°C, the atomizer speed is 12500r / min-21000r / min, and the atomization pressure is 0.2-0.5MPa.

4. The method for preparing an etching-resistant ceramic coating material according to claim 1, characterized in that: In the ethanol-water mixed solution of step S6, the volume fraction of ethanol is 70-90%.

5. The method for preparing an etching-resistant ceramic coating material according to claim 1, characterized in that: In step S6, the dispersant is polyvinyl pyrrolidone (PVP) or polyvinyl alcohol (PVA) with a concentration of 0.1-0.5 wt%.

6. The method for preparing an etching-resistant ceramic coating material according to claim 1, characterized in that: In step S7, the substrate material is single crystal silicon, ceramic or metal alloy.

7. The method for preparing an etching-resistant ceramic coating material according to claim 2, characterized in that: In step S8, the spraying parameters of the suspension plasma spraying equipment are: plasma gas flow: argon main gas 40-80 slpm, hydrogen auxiliary gas 5-20 slpm; current and voltage: current 300-600 A, voltage 40-90 V; spraying distance: 50-100 mm; feed rate: 2-50 mL / min.

8. The method for preparing an etching-resistant ceramic coating material according to claim 2, characterized in that: In step S8, the high temperature sintering temperature is increased from room temperature to 1100-1500°C at a rate of 5-10°C / min.

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