A composite ceramic coating spraying processing device

Abstract

The application provides a composite ceramic coating spraying processing device, which can form an alumina coating and a silicon oxide coating through first spraying, can form an aluminum fluoride coating through second spraying, and can form a yttrium fluoride coating through third spraying; the three layers of coatings are sequentially distributed from inside to outside, forming a plasma-resistant ceramic coating with a multilayer composite structure, which enriches the structure of the composite ceramic coating and improves the overall protection capability against plasma etching, so that safety accidents can be avoided. The application solves the problems of single structure and poor protection capability of the traditional composite ceramic coating.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of composite ceramic coating, in particular to a composite ceramic coating spraying processing device. BACKGROUND

[0002] In the process of semiconductor manufacturing, plasma is often used to etch or clean semiconductor substrates and wafers. The reaction gas for generating plasma contains a large amount of fluorine, chlorine and other highly corrosive halogens. These plasmas not only etch wafers, but also etch the inner surface of the reaction chamber of the plasma etching machine made of aluminum or aluminum alloy and the parts working in the chamber, thereby causing the etching products to adhere to the surface of the wafer, affecting the quality of the product. Moreover, the damage to the inner surface of the cavity and the parts will shorten the service life of the equipment, and even cause serious defects and safety problems.

[0003] Some enterprises will prepare a protective coating on the surface of the parts serving in the plasma environment to effectively slow down the etching damage. For example, patent document: Use of nano-alumina-based composite ceramic coating (CN102443753B) describes a method for preparing a corrosion-resistant and voltage-resistant coating. In this method, alumina is used as the base powder, which is mixed and ground with zirconia and rare earth oxide powder in a specific ratio to obtain a 20-100 μm particle size powder. Then, the powder is sprayed onto the substrate by plasma spraying or supersonic flame spraying process to obtain a 50-2000 μm coating. The material shows that the coating has a porosity, which can significantly improve the plasma corrosion resistance of the coating and has high insulation properties.

[0004] However, the composite ceramic coating still has the following shortcomings:

[0005] 1. The mixed and ground multi-component powder has a controllable overall particle size distribution, but the particle size of each component varies within and between batches, which may cause changes in the microstructure of the coating and affect the stable performance of the coating.

[0006] 2. The coating structure is single, and the chemical components and microstructure of the inner and outer surfaces of the coating are consistent. If a factor causes a defect in the coating, the defect will be throughout the coating, thereby causing the coating to lose its original protective ability.

[0007] 3. The existing semiconductor etching gas is mainly fluorine-containing gas, and the coating of the existing technology uses metal oxide as the main coating component. Fluorine has stronger electronegativity than oxygen, which can easily replace the oxygen in the coating composition, thereby causing the coating to be damaged. This phenomenon becomes more and more obvious with the increase of the plasma etching power. SUMMARY

[0008] In view of the above problems, the application provides a composite ceramic coating spraying processing device, which solves the problems of single structure and poor protection of the traditional composite ceramic coating.

[0009] To solve the above problems, the application adopts the technical scheme of:

[0010] A composite ceramic coating preparation method, comprising the following steps:

[0011] S1, surface treatment: removing surface pollutants of the substrate by physical means to form a certain surface roughness for facilitating coating adhesion;

[0012] S2, first spraying: after the surface treatment in step S1 is completed, selecting alumina and silicon oxide powders with particle sizes of D50≥5 μm and D90≤20 μm, mixing them uniformly at a ratio of 2:1, adjusting the plasma spraying parameters: argon 35-45 L / Min, hydrogen 6-11 L / Min, voltage 35-40 V, and current 550-600 A to form a corrosion-resistant coating one.

[0013] S3, second spraying: after the first spraying in step S2 is completed, selecting aluminum fluoride powder with a particle size of D50≥5 μm and D90≤20 μm, adjusting the plasma spraying parameters: argon 25-35 L / Min, hydrogen 3-6 L / Min, voltage 15-20 V, and current 350-450 A to form a corrosion-resistant coating two.

[0014] S4, third spraying: after the second spraying in step S3 is completed, selecting yttrium fluoride powder with a particle size of D50≥5 μm and D90≤20 μm, adjusting the plasma spraying parameters: argon 35-45 L / Min, hydrogen 4-8 L / Min, voltage 30-35 V, and current 500-600 A to form a corrosion-resistant coating three.

[0015] Preferably, before each spraying, the substrate surface is sequentially subjected to cleaning processing and preheating processing; the cleaning processing uses high-pressure pure water to thoroughly flush the substrate surface particles; and the preheating processing heats the substrate to 80-100℃.

[0016] Preferably, the substrate is subjected to drying processing between the cleaning processing and the preheating processing, and an oven is used to heat the substrate to stabilize at 100-105℃ to remove the water adsorbed by the substrate.

[0017] Preferably, after the third spraying is completed, the substrate is subjected to annealing processing, specifically: placing the substrate in a vacuum oven and slowly heating it to 200-300℃, maintaining for 1-2 h, and then naturally cooling to eliminate the internal stress of the substrate and the coating; and then sequentially cleaning and drying the substrate.

[0018] Preferably, the first spraying process controls the first corrosion-resistant coating layer to have a thickness of 80-120 mu m; the second spraying process controls the second corrosion-resistant coating layer to have a thickness of 20-50 mu m; and the third spraying process controls the third corrosion-resistant coating layer to have a thickness of 50-80 mu m.

[0019] Preferably, the physical means in step S1 is performed by sand blasting, and the surface roughness Ra of the substrate is controlled to be 5-10 mu m.

[0020] A composite ceramic coating spraying processing device, comprising a hollow processing main body, a protective cover body is arranged at the upper end of the processing main body, a spraying gun head is arranged in the protective cover body, a processing platform is fixedly connected to the inner wall of the processing main body, the processing platform divides the processing main body into a first processing chamber and a second processing chamber, a flip opening penetrating up and down is formed in the surface of the processing platform, a bearing platform is arranged in the flip opening, a clamping device for clamping the substrate and controlling the rotation thereof is arranged at the upper end of the bearing platform, the bearing platform is rotatably connected to the inner wall of the flip opening, and a flip driving device is arranged in the processing main body for controlling the rotation of the bearing platform.

[0021] Preferably, the bearing platform is rotatably connected to the processing platform through a hollow rotating shaft, an electric control device for controlling the rotation of the hollow rotating shaft is arranged in the processing main body, a negative pressure air suction device is arranged on the surface of the bearing platform, the negative pressure air suction device is in communication with the hollow rotating shaft, the end of the hollow rotating shaft is in communication with the first processing chamber through a connecting pipeline, and a pump body for controlling the flow of gas is arranged in the connecting pipeline.

[0022] Preferably, the negative pressure air suction device comprises air suction ends arranged at both sides of the bearing platform, the air suction ends extend along the length direction of the substrate, a control pipeline is embedded in the bearing platform, the two ends of the control pipeline are in communication with the two air suction ends respectively, and a sealing ball is arranged in the control pipeline.

[0023] Preferably, a sealing cover body for mounting the spraying gun head is arranged on the inner wall of the protective cover body, and a position control device is arranged on the inner wall of the sealing cover body for driving the spraying gun head to be in different positions.

[0024] The present application has the following beneficial effects:

[0025] 1. The aluminum oxide coating and the silicon oxide coating can play an insulating role and have certain plasma resistance, the aluminum fluoride layer has excellent insulation and plasma resistance, can fill the interlayer pores, and the yttrium fluoride coating has excellent plasma resistance, so that the coating structure is enriched and the overall plasma etching protection capability is improved, and safety accidents are avoided.

[0026] 2. By re-selecting the type of coating powder and spraying it according to a specific process, a plasma-resistant ceramic coating with a multi-layer composite structure is finally formed. According to the test, when the coating thickness is 200μm, the coating adhesion reaches 16MPa, the voltage resistance reaches 6KV, and the plasma corrosion resistance time (simulated with 5% hydrochloric acid) can reach more than 6 hours.

[0027] 3. By controlling the rotation of the carrying platform through a flipping drive device, the position of the clamping device and the substrate can be changed. This allows for simultaneous processing of substrates on both sides in the first and second processing chambers, enabling continuous three-stage spraying operations without the need for frequent substrate removal by operators. This shortens the spraying production time and improves spraying efficiency. Furthermore, by incorporating a negative pressure suction device, a hollow rotating shaft, and connecting pipes, the waste heat generated during plasma spraying can be directionally transported, fully recovering and utilizing the heat to ensure a high-temperature atmosphere in the first processing chamber. Additionally, the waste heat in the second processing chamber can be promptly discharged, facilitating timely removal by operators while preventing gas leaks and ensuring a stable and normal processing environment. Attached Figure Description

[0028] Figure 1 This is a flowchart of the method of the present invention;

[0029] Figure 2 This is a three-dimensional structural diagram of the processing device of the present invention;

[0030] Figure 3 For the present invention Figure 2 Front view structural diagram;

[0031] Figure 4 For the present invention Figure 2 A top-view structural diagram;

[0032] Figure 5 For the present invention Figure 4 A schematic diagram of the AA-line cross-sectional structure;

[0033] Figure 6 For the present invention Figure 5 A magnified structural diagram at point B.

[0034] In the diagram: 100, main processing unit; 110, first processing chamber; 120, second processing chamber; 130, processing platform; 140, protective cover; 200, substrate; 300, clamping device; 400, bearing platform; 500, tilting drive device; 510, hollow rotating shaft; 520, electrical control device; 600, spray gun head; 700, sealing cover; 710, position control device; 800, connecting pipe; 900, negative pressure suction device; 910, suction end; 920, control pipe; 930, sealing sphere. Detailed Implementation

[0035] The application will be further described below in conjunction with the accompanying drawings and examples.

[0036] With reference to Figure 1 A composite ceramic coating preparation method, comprising the following steps:

[0037] S1, surface treatment: removing the surface contaminants of the substrate by physical means to form a certain surface roughness for facilitating the adhesion of the coating; the physical means is performed by sand blasting, and the surface roughness Ra of the substrate is controlled to be 5-10 μm for facilitating the adhesion of the coating; and the thickness of the corrosion-resistant coating one is controlled to be 80-120 μm in the first spraying process.

[0038] S2, first spraying: after the surface treatment in step S1 is completed, the alumina and silica powders with particle size D50≥5 μm and D90≤20 μm are mixed uniformly at a ratio of 2:1, the plasma spraying parameters are adjusted as follows: argon 35-45 L / Min, hydrogen 6-11 L / Min, voltage 35-40 V, and current 550-600 A, to form the corrosion-resistant coating one, i.e. the alumina and silica coating, which is located in the innermost layer and mainly plays an insulating role while having certain plasma resistance.

[0039] S3, second spraying: after the first spraying in step S2 is completed, the aluminum fluoride powder with particle size D50≥5 μm and D90≤20 μm is selected, and the plasma spraying parameters are adjusted as follows: argon 25-35 L / Min, hydrogen 3-6 L / Min, voltage 15-20 V, and current 350-450 A, to form the corrosion-resistant coating two, i.e. the aluminum fluoride coating, which is the intermediate layer and has excellent plasma resistance; in addition, it has a lower melting point and a better flowability in the molten state than the inner and outer layers, and can fill the interlayer pores; and it can act as a catalyst to catalyze the surface reaction of the inner layer to generate dense mullite crystals at high temperature during spraying, thereby further increasing the insulation and plasma resistance of the inner layer; and the thickness of the corrosion-resistant coating two is controlled to be 20-50 μm in the second spraying process.

[0040] S4, third spraying: after the second spraying in step S3 is completed, the yttrium fluoride powder with particle size D50≥5 μm and D90≤20 μm is selected, and the plasma spraying parameters are adjusted as follows: argon 35-45 L / Min, hydrogen 4-8 L / Min, voltage 30-35 V, and current 500-600 A, to form the corrosion-resistant coating three, i.e. the yttrium fluoride coating, which is the outermost layer and has excellent plasma resistance; and the thickness of the corrosion-resistant coating three is controlled to be 50-80 μm in the third spraying process.

[0041] Before each spraying, the substrate surface is sequentially subjected to cleaning processing and preheating processing; the cleaning processing uses high-pressure pure water to completely flush the substrate surface particles and remove physical and chemical residues; the preheating processing heats the substrate to 80-100 DEG C to prevent the sprayed powder from contacting the substrate to form a too large temperature difference, thereby causing thermal stress deformation of the substrate.

[0042] The substrate is subjected to drying processing between the cleaning processing and the preheating processing, the substrate is heated by an oven to stabilize at 100-105 DEG C, remove the water adsorbed by the substrate, prevent the coating from falling off due to the expansion of heated water vaporization during spraying, shorten the overall spraying time, and improve the overall spraying efficiency.

[0043] After the third spraying is completed, the substrate is subjected to annealing processing, specifically: the substrate is placed in a vacuum oven and slowly heated to 200-300 DEG C, maintained for 1-2 h, and then naturally cooled to eliminate the internal stress of the substrate and the coating to ensure the quality of the finished product; then the substrate is sequentially subjected to cleaning and drying, and finally the substrate surface particles are completely flushed to remove physical and chemical residues.

[0044] Finally, it should be noted that: the coating is a three-layer composite structure, and the materials from inside to outside are alumina + silicon oxide, aluminum fluoride and yttrium fluoride; the inner layer is made of alumina and silicon oxide mixed according to a specific particle size and proportion, and has a thickness of about 80-120 μm, mainly serving as an insulating layer, and also having certain plasma resistance; the middle layer is an aluminum fluoride layer, having a thickness of about 20-50 μm, and itself having excellent plasma resistance; in addition, it has a lower melting point and better flowability in a molten state than the inner and outer layers, and can fill the interlayer pores; and can act as a catalyst to catalyze the reaction on the surface of the inner layer to generate dense mullite crystals at high temperatures during spraying, further increasing the insulation and plasma resistance of the inner layer; the outer layer is a yttrium fluoride coating, having a thickness of about 50-80 μm, and having excellent plasma resistance.

[0045] The above three-layer structure macroscopically utilizes the composite structure to reduce the risk probability of simultaneous defects of the coating; microscopically, by selecting suitable particle size powder and spraying according to a certain spraying process, the porosity of the coating can be reduced to below 2%, and the interlayer barrier can be formed by utilizing the physical and chemical properties of the powder to further prevent the penetration of plasma.

[0046] The present application reselects the types of coating powder and sprays according to a specific process to finally form a multi-layer composite plasma-resistant ceramic coating; detection shows that when the thickness of the coating is 200 μm, the bonding strength of the coating reaches 16 MPa, the voltage resistance reaches 6 KV, and the plasma corrosion resistance time (using 5% hydrochloric acid simulation) can reach more than 6 h.

[0047] Reference Figures 2-6The utility model provides a kind of composite ceramic coating spraying processing device, including hollow processing main body 100, the upper end of processing main body 100 is provided with protective cover body 140, protective cover body 140 inside is provided with spraying gun head 600, wherein protective cover body 140 can be rotatably connected or linearly slidingly connected between processing main body 100, during the process of spraying processing, protective cover body 140 is covered with processing main body 100, when spraying gun head 600 is located the surface of substrate 200 to be sprayed, it can realize the plasma spraying of substrate surface, realizes spraying processing.

[0048] Processing platform 130 is fixedly connected on the inner wall of processing main body 100, and processing platform 130 divides processing main body 100 into first processing chamber 110 and second processing chamber 120, wherein the substrate completes the processing process of cleaning, drying and preheating in first processing chamber 110, and first processing chamber 110 is located at the lower end of processing platform 130; second processing chamber 120 is located at the upper end of processing platform 130, i.e. the side where spraying gun head 600 is located, and spraying operation is realized in the processing chamber;

[0049] A turnover opening is opened on the surface of processing platform 130, and a bearing platform 400 is arranged in the turnover opening, the upper end of bearing platform 400 is provided with a clamping device 300 for clamping the substrate 200 and controlling the rotation thereof, the substrate 200 can rotate around a predetermined axis by controlling the clamping device 300, and the different surfaces of the substrate 200 can correspond to the spraying gun head 600 by controlling the rotation of the substrate 200 by the clamping device 300, so as to realize continuous spraying processing of the surface of the substrate 200.

[0050] The bearing platform 400 is rotatably connected with the inner wall of the turnover opening, and a turnover driving device 500 is arranged in the processing main body 100 for controlling the rotation of the bearing platform 400, the bearing platform 400 can rotate by controlling the turnover driving device 500, i.e. different clamping devices 300 and substrates 200 are turned over to different processing chambers to realize automatic switching of processing state; the substrate 200 at the upper end is subjected to plasma spraying processing, and the substrate 200 at the lower end is subjected to cleaning, drying, preheating and other processing in first processing chamber 110, the two processing processes are carried out synchronously, three spraying operations can be realized continuously, the substrate 200 does not need to be disassembled and assembled by workers during processing, the preparation time consumed by traditional single-sided spraying is reduced, the efficiency of spraying processing is greatly improved, and the spraying time is shortened.

[0051] The bearing platform 400 is rotationally connected with the processing platform 130 through the hollow rotating shaft 510, the processing main body 100 is internally provided with an electric control device 520 for controlling rotation of the hollow rotating shaft 510, the electric control device 520 is selected as a motor and a gear structure, and the clamping device 300, the bearing platform 400 and other devices can be provided in multiple groups along the length direction of the hollow rotating shaft 510, a plurality of bearing platforms 400 can be driven through the same hollow rotating shaft 510, the number of substrates sprayed in one spraying process is increased, and the spraying efficiency is improved.

[0052] The bearing platform 400 is rotationally connected with the processing platform 130 through the hollow rotating shaft 510, the processing main body 100 is internally provided with an electric control device 520 for controlling rotation of the hollow rotating shaft 510, the electric control device 520 is selected as a motor and a gear structure, and the clamping device 300, the bearing platform 400 and other devices can be provided in multiple groups along the length direction of the hollow rotating shaft 510, a plurality of bearing platforms 400 can be driven through the same hollow rotating shaft 510, the number of substrates sprayed in one spraying process is increased, and the spraying efficiency is improved.

[0053] Here, it should be noted that a filter element can be arranged at the front section of the connecting pipeline 800 to purify the gas entering the first processing chamber 110, so as to avoid cross contamination in the first processing chamber 110 and the second processing chamber 120 and affect the processing quality; or a serpentine pipeline can be arranged in the first processing chamber 110 to make the high-temperature gas flow directionally in the metal serpentine pipeline and exchange heat with the gas in the first processing chamber 110, so as to realize heat exchange in a sealed state and also avoid cross contamination of the gas.

[0054] Specific reference is made to the accompanying drawings Figure 6The negative pressure suction device 900 comprises suction ends 910 located on both sides of the bearing platform 400, the suction ends 910 extend along the length direction of the base material 200, a control pipeline 920 is embedded in the bearing platform 400, two ends of the control pipeline 920 are communicated with the two suction ends 910 respectively, and a sealed ball 930 is arranged in the control pipeline 920; wherein the control pipeline 920 penetrates through the bearing platform 400 and is communicated with the two suction ends 910, under the action of the pump body, the directional flow of the gas can be controlled, that is, the gas flows through the suction ends 910, the control pipeline 920 and the hollow rotating shaft 510 in turn and finally flows into the first processing chamber 110 from the connecting pipeline 800, so that the directional flow of the gas is realized; wherein the sealed ball 930 realizes the automatic switching of the position in the rotation of the bearing platform 400, can automatically seal the bottom end of the control pipeline 920, realizes the automatic conduction control of the control pipeline 920, in the process of spraying work, the bottom end of the control pipeline 920 is automatically sealed and the gas cannot enter, and the top end is automatically opened and the residual heat gas is transported; through the above structure, the control valve is not arranged inside to control the conduction of the control pipeline 920, the control structure space volume is reduced, the whole device can work stably for a long time, and the failure rate is low.

[0055] The sealing cover 700 for mounting the spraying gun head 600 is arranged on the inner wall of the protective cover 140, the position control device 710 is arranged on the inner wall of the sealing cover 700 and used for driving the spraying gun head 600 to be in different positions, the position control device 710 can be an electric control track, a mechanical arm or the like control structure, and the spraying gun head 600 is controlled to be in different positions to spray the base material 200 in different positions; the hydraulic telescopic device is arranged between the protective cover 140 and the sealing cover 700, can control the linear movement of the sealing cover 700 away from or close to the bearing platform 400, so that the bearing platform 400, the clamping device 300 and the like can be normally turned over, and the sealing cover 700 can seal the connecting gap of the bearing platform 400, so that the two processing chambers can normally work.

[0056] The above only describes the preferred embodiments of the present application and is not used to limit the present application, any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A composite ceramic coating spraying processing device, comprising a hollow processing body (100), wherein a protective cover (140) is provided at the upper end of the processing body (100), and a spray gun head (600) is provided inside the protective cover (140), characterized in that: The processing body (100) is fixedly connected to the inner wall of the processing platform (130), which divides the processing body (100) into a first processing chamber (110) and a second processing chamber (120). The substrate is cleaned, dried and preheated in the first processing chamber, and the substrate is sprayed in the second processing chamber. The surface of the processing platform (130) has a vertically penetrating flip opening, and a bearing platform (400) is provided in the flip opening. The upper end of the bearing platform (400) is provided with a clamping device (300) for clamping the substrate (200) and controlling its rotation. The bearing platform (400) is rotatably connected to the inner wall of the flip opening. The processing body (100) is provided with a flip driving device (500) for controlling the rotation of the bearing platform (400).

2. The composite ceramic coating spraying device according to claim 1, characterized in that, The support platform (400) is rotatably connected to the processing platform (130) via a hollow rotating shaft (510). The processing body (100) is equipped with an electrical control device (520) for controlling the rotation of the hollow rotating shaft (510). The surface of the support platform (400) is equipped with a negative pressure suction device (900). The negative pressure suction device (900) is connected to the hollow rotating shaft (510). The end of the hollow rotating shaft (510) is connected to the first processing chamber (110) via a connecting pipe (800). The connecting pipe (800) is equipped with a pump body for controlling gas flow.

3. The composite ceramic coating spraying device according to claim 2, characterized in that, The negative pressure suction device (900) includes suction terminals (910) located on both sides of the support platform (400). The suction terminals (910) extend along the length of the substrate (200). A control pipe (920) is embedded inside the support platform (400). The two ends of the control pipe (920) are respectively connected to the two suction terminals (910). A sealing ball (930) is provided inside the control pipe (920).

4. The composite ceramic coating spraying device according to claim 1, characterized in that, The inner wall of the protective cover (140) is provided with a sealing cover (700) for installing the spray gun head (600), and the inner wall of the sealing cover (700) is provided with a position control device (710) for driving the spray gun head (600) to different positions.

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