WO2020168679A1 - Method for preparing protective coating for plasma etching chamber of ic equipment - Google Patents

Method for preparing protective coating for plasma etching chamber of ic equipment Download PDF

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WO2020168679A1
WO2020168679A1 PCT/CN2019/097064 CN2019097064W WO2020168679A1 WO 2020168679 A1 WO2020168679 A1 WO 2020168679A1 CN 2019097064 W CN2019097064 W CN 2019097064W WO 2020168679 A1 WO2020168679 A1 WO 2020168679A1
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powder
etching chamber
protective coating
plasma etching
coating
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PCT/CN2019/097064
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French (fr)
Chinese (zh)
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郑广文
侯涛
熊天英
崔新宇
沈艳芳
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沈阳富创精密设备有限公司
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Publication of WO2020168679A1 publication Critical patent/WO2020168679A1/en
Priority to ZA2021/05559A priority Critical patent/ZA202105559B/en

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C24/00—Coating starting from inorganic powder
    • C23C24/02—Coating starting from inorganic powder by application of pressure only
    • C23C24/04—Impact or kinetic deposition of particles

Definitions

  • the invention relates to the technical field of preparation of cermet coatings, in particular to a preparation method of protective coatings for plasma etching chambers of IC equipment.
  • the Al+(Y 2 O 3 -ZrO 2 ) composite coating prepared in this implementation has a porosity of 1.9%, and the interface bonding strength between the coating and the base material is 40 MPa.
  • the IC equipment plasma etching chamber protective coating prepared by the present invention is first used to prepare micron-sized agglomerated YSZ powder with nanocrystalline structure through the use of surfactants and hydrothermally.
  • YSZ coating prepared by cold spray technology The coating is well combined with the substrate, the porosity of the coating is less than 2%, the interface bonding strength is 20-50 MPa, and the coating thickness is 10-400 ⁇ m.

Abstract

Disclosed is a method for preparing a protective coating for a plasma etching chamber of a piece of IC equipment, the method comprising depositing a mixed powder of Al and Y2O3-ZrO2 at a high speed by using a cold spraying and deposition technique. For the cold spraying, compressed air is used as a working gas, the spraying distance is 10-60 mm, the spraying temperature is 200-600 ºC, the gas pressure is 1.5-3 MPa, and a powder particle size is 1-50 µm. A metal ceramic protective coating, which is uniformly distributed, is formed on a surface of the plasma etching chamber. The coating can reduce or prevent the corrosion of the etching chamber by corrosive gases and the contamination of a chip by plasma, and can improve the service life of the plasma etching chamber during the production of a chip. The method comprises: firstly mixing Al and Y2O3-ZrO2 powders in proportion until uniform, and drying same; and secondly, spraying the powder on a surface of a substrate by using the cold spraying and deposition technique, so as to obtain a metal ceramic composite coating by controlling process parameters. The method has a high deposition efficiency, and the thickness of the coating can be adjusted at will according to the actual use, so that same can be used to prepare a thick protective coating for a plasma etching chamber of a piece of IC equipment.

Description

一种IC装备等离子体刻蚀腔防护涂层的制备方法Method for preparing protective coating of plasma etching cavity for IC equipment 技术领域Technical field
本发明涉及金属陶瓷涂层的制备技术领域，具体为一种IC装备等离子体刻蚀腔防护涂层的制备方法。The invention relates to the technical field of preparation of cermet coatings, in particular to a preparation method of protective coatings for plasma etching chambers of IC equipment.
背景技术Background technique
以往研究中，多采用热喷涂设备制备YSZ涂层，需要加热到2000℃以上，条件苛刻，而且费用昂贵。涂层最外层有横向裂纹，致密性差，质量有待提高。In previous studies, thermal spraying equipment was mostly used to prepare YSZ coatings, which needed to be heated to above 2000°C, under harsh conditions and expensive. The outermost layer of the coating has transverse cracks, and its compactness is poor, and the quality needs to be improved.
使用冷喷涂技术制备陶瓷涂层时，使用的陶瓷粉末的性质是至关重要的。普通的纳米粉末不适合用于冷喷涂制备涂层，这是由于冷喷涂的高压高速气流会在基体表面形成弓激波阻碍纳米粉体的沉积。而喷涂颗粒度偏大时，会对基体形成冲蚀，很难形成涂层。因此，欲使用冷喷涂制备YSZ陶瓷涂层，制备适宜冷喷涂的YSZ粉末至关重要。When using cold spray technology to prepare ceramic coatings, the nature of the ceramic powder used is critical. Ordinary nano-powders are not suitable for cold spraying to prepare coatings, because the high-pressure and high-speed airflow of cold spraying will form bow shock waves on the surface of the substrate to hinder the deposition of nano-powders. When the spray particle size is too large, the substrate will be eroded and it is difficult to form a coating. Therefore, to prepare YSZ ceramic coating by cold spraying, it is very important to prepare YSZ powder suitable for cold spraying.
目前的国际趋势是研究氧化钇稳定氧化锆陶瓷涂层以提高涂层的综合性能。Seok等(Seok H W，Kim Y C，Chol E Y，et a1.Multi-component thermal spray coatingmaterial and production method and coating method thereof：US，13/915976[P].2013-06-12.)采用大气等离子喷涂的方法制备了几种耐刻蚀涂层，例如Al 2O 3涂层、Y 2O 3涂层、不同氧化钇含量的Y 2O 3-ZrO 2涂层、Y 2O 3-ZrO 2-A1 2O 3涂层等，并测试了它们的刻蚀速率，得出结论：Y 2O 3-ZrO：涂层的刻蚀速率基本小于氧化钇涂层，且当Y 2O 3：ZrO 2为70：30时，涂层的刻蚀速率最小，约为5nm/min，即耐等离子刻蚀性能最好。 The current international trend is to study yttria stabilized zirconia ceramic coatings to improve the overall performance of the coatings. Seok et al. (Seok HW, Kim YC, Chol EY, et a1. Multi-component thermal spray coating material and production method and coating method thereof: US, 13/915976[P]. 2013-06-12.) using atmospheric plasma spraying Several corrosion-resistant coatings were prepared by the method, such as Al 2 O 3 coating, Y 2 O 3 coating, Y 2 O 3 -ZrO 2 coating with different yttrium oxide content, Y 2 O 3 -ZrO 2 -A1 2 O 3 coatings, etc., and tested their etching rate, and concluded that: Y 2 O 3 -ZrO: The etching rate of the coating is basically smaller than that of the yttrium oxide coating, and when Y 2 O 3 :ZrO 2 is At 70:30, the etching rate of the coating is the smallest, about 5nm/min, that is, the plasma etching resistance is the best.
发明内容Summary of the invention
针对现有技术中存在的上述不足之处，本发明的目的是提供一种IC装备等离子体刻蚀腔防护涂层的制备方法，解决当前IC装备等离子体刻蚀腔防护涂层在高功率刻蚀过程中容易失效的问题，开辟一种新的制备IC装备等离子体刻蚀腔防护涂层的有效途径，以期早日获得实际应用。In view of the above-mentioned shortcomings in the prior art, the purpose of the present invention is to provide a method for preparing IC equipment plasma etching chamber protective coating, which solves the problem of current IC equipment plasma etching chamber protective coating in high power etching The problem of easy failure during the etching process opens up a new effective way to prepare the protective coating of the plasma etching chamber for IC equipment, in order to obtain practical application as soon as possible.
为实现上述目的，本发明所采用的技术方案如下：In order to achieve the above objectives, the technical solutions adopted by the present invention are as follows:
一种IC装备等离子体刻蚀腔防护涂层的制备方法，采用Al和Y 2O 3-ZrO 2的混合粉末制备等离子刻蚀腔体表面防护涂层，利用高速气流将Al和Y 2O 3-ZrO 2的混合粉末直接喷涂于等离子刻蚀腔体表面，喷涂参数为：使用压缩空气为工作气体，气体温度为200-600℃，气体压力为1.5-3.0MPa，喷涂距离为10-60mm，使混合粉末沉积在等离子刻蚀腔的内表面上，形成均匀分布的防护涂层；其中，Al粉末和Y 2O 3-ZrO 2粉末的重量比例为0.1-1:1；其中Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为3-5：1。 A method for preparing protective coatings for plasma etching chambers for IC equipment. A mixed powder of Al and Y 2 O 3 -ZrO 2 is used to prepare protective coatings on the surface of plasma etching chambers, and the Al and Y 2 O 3 -The mixed powder of ZrO 2 is sprayed directly on the surface of the plasma etching chamber. The spraying parameters are: compressed air is used as the working gas, the gas temperature is 200-600℃, the gas pressure is 1.5-3.0MPa, and the spraying distance is 10-60mm. The mixed powder is deposited on the inner surface of the plasma etching chamber to form a uniformly distributed protective coating; where the weight ratio of Al powder and Y 2 O 3 -ZrO 2 powder is 0.1-1:1; where Y 2 O 3 -ZrO 2 powder, Y 2 O 3 powder and ZrO 2 weight ratio of 3-5: 1.
(1)微米级混合粉末的制备：(1) Preparation of micron-level mixed powder:
将Al粉末和Y 2O 3-ZrO 2粉末按照重量比例为0.1-1:1比例混合，在Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为3～5：1，经干燥得到微米级混合粉末，粉末粒度1～50μm； The Al powder and Y 2 O 3 -ZrO 2 powder are mixed in a weight ratio of 0.1-1:1. In the Y 2 O 3 -ZrO 2 powder, the weight ratio of Y 2 O 3 to ZrO 2 powder is 3 to 5 :1. After drying, a micron-sized mixed powder is obtained, the powder size is 1-50μm;
(2)冷喷涂沉积等离子体刻蚀腔防护涂层：(2) Cold spray deposition plasma etching chamber protective coating:
将步骤(1)得到的微米级混合粉末经压缩空气预热后沉积在刻蚀腔材料内表面，获得离子 体刻蚀腔防护涂层；所述冷喷涂沉积过程中：使用压缩空气作为工作气体，工作气体温度为200-600℃，工作气体压力为1.5-3.0MPa，喷涂距离为10-60mm。The micron-level mixed powder obtained in step (1) is preheated by compressed air and deposited on the inner surface of the etching chamber material to obtain a protective coating for the ion etching chamber; during the cold spray deposition process: compressed air is used as the working gas , The working gas temperature is 200-600℃, the working gas pressure is 1.5-3.0MPa, and the spraying distance is 10-60mm.
等离子体刻蚀腔防护涂层的喷涂装置，具有进气管1、加热器2、送粉器5、电磁阀6、超音速喷嘴4、控制柜1；进气管的一端与空气压缩机相连，另一端与送粉器、加热器、超音速喷嘴相连，进气管置于加热器中的部分为螺旋形结构。The spraying device for the protective coating of the plasma etching chamber has an air inlet pipe 1, a heater 2, a powder feeder 5, a solenoid valve 6, a supersonic nozzle 4, and a control cabinet 1. One end of the air inlet pipe is connected with an air compressor, and the other One end is connected with a powder feeder, a heater, and a supersonic nozzle, and the part of the air inlet pipe placed in the heater has a spiral structure.
制备等离子体刻蚀腔防护涂层的过程中，由空气压缩机输出的工作气体分为两路，一路进入加热器，经预热后气体进入超音速喷嘴的混合腔；另一路进入送粉器，作为载气将粉末引入超音速喷嘴与第一路经过预热的气体相混合，将粉末瞬时预热后，经过超音速喷嘴的缩放区，膨胀加速，形成超音速气固双相流，高速撞击刻蚀腔材料内表面使粉末发生剧烈变形实现沉积，并在刻蚀腔材料内表面形成复合型防护涂层。In the process of preparing the protective coating of the plasma etching chamber, the working gas output by the air compressor is divided into two paths. One path enters the heater. After preheating, the gas enters the mixing chamber of the supersonic nozzle; the other path enters the powder feeder , As the carrier gas, the powder is introduced into the supersonic nozzle and mixed with the first preheated gas. After instantaneous preheating, the powder passes through the zoom zone of the supersonic nozzle, expands and accelerates to form a supersonic gas-solid two-phase flow, high-speed The impact on the inner surface of the etching cavity material causes the powder to be violently deformed to achieve deposition, and a composite protective coating is formed on the inner surface of the etching cavity material.
防护涂层的孔隙率低于2％，陶瓷涂层与基体材料的界面结合强度为20-50MPa，涂层厚度为10-400μm。The porosity of the protective coating is less than 2%, the interface bonding strength between the ceramic coating and the base material is 20-50 MPa, and the coating thickness is 10-400 μm.
本发明的优点及有益效果如下：The advantages and beneficial effects of the present invention are as follows:
本发明则借助冷喷涂沉积技术，仅使用较低成本的压缩空气作为载气就能制备厚度为10-400μm的IC装备等离子体刻蚀腔防护涂层。该方法沉积效率高，可根据实际使用情况随意调节涂层的厚度，可以用来制备厚的IC装备等离子体刻蚀腔防护涂层。The present invention utilizes cold spray deposition technology and only uses low-cost compressed air as a carrier gas to prepare a protective coating for IC equipment plasma etching chambers with a thickness of 10-400 μm. The method has high deposition efficiency, and the thickness of the coating can be adjusted at will according to actual use conditions, and can be used to prepare thick protective coatings for plasma etching chambers of IC equipment.
附图说明Description of the drawings
图1是本发明采用的喷涂装置示意图。Figure 1 is a schematic diagram of a spraying device used in the present invention.
具体实施方式detailed description
以下结合附图1和实施例详述本发明。The present invention will be described in detail below with reference to FIG. 1 and embodiments.
一种IC装备等离子体刻蚀腔防护涂层的制备方法，该方法包括如下步骤：A method for preparing a protective coating for a plasma etching chamber for IC equipment, the method includes the following steps:
(1)微米级混合粉末的制备：(1) Preparation of micron-level mixed powder:
将Al粉末和Y 2O 3-ZrO 2粉末按照重量比例为(0.1～1):1比例混合，在Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为(3～5)：1，经干燥得到微米级混合粉末，粉末粒度1～50μm； The Al powder and Y 2 O 3 -ZrO 2 powder are mixed in a weight ratio of (0.1～1):1. In the Y 2 O 3 -ZrO 2 powder, the weight ratio of Y 2 O 3 to ZrO 2 powder is ( 3～5): 1. Micron-sized mixed powder is obtained after drying, the powder size is 1～50μm;
(2)冷喷涂沉积等离子体刻蚀腔防护涂层：(2) Cold spray deposition plasma etching chamber protective coating:
将步骤(1)得到的微米级混合粉末经加热的压缩空气预热后高通量沉积在刻蚀腔材料内表面，获得离子体刻蚀腔防护涂层；所述冷喷涂沉积过程中：使用压缩空气作为工作气体，工作气体温度为200-600℃，工作气体压力为1.5-3.0MPa，喷涂距离为10-60mm。The micron-level mixed powder obtained in step (1) is preheated by heated compressed air and then deposited with high flux on the inner surface of the etching chamber material to obtain a plasma etching chamber protective coating; during the cold spray deposition process: Compressed air is used as the working gas, the working gas temperature is 200-600℃, the working gas pressure is 1.5-3.0MPa, and the spraying distance is 10-60mm.
上述步骤(1)中，纯Al粉末和Y 2O 3-ZrO 2粉末的重量比例为(0.1～1):1。 In the above step (1), the weight ratio of pure Al powder and Y 2 O 3 -ZrO 2 powder is (0.1-1):1.
上述步骤(1)中，Y 2O 3与ZrO 2粉末的重量比为(3～5)：1。 In the above step (1), the weight ratio of Y 2 O 3 to ZrO 2 powder is (3 to 5):1.
上述步骤(1)中，所述微米级Al粉末和Y 2O 3-ZrO 2粉末经干燥得到微米级混合粉末，混合粉末粒度1～50μm。 In the above step (1), the micron-sized Al powder and Y 2 O 3 -ZrO 2 powder are dried to obtain a micron-sized mixed powder, and the particle size of the mixed powder is 1-50 μm.
上述步骤(2)中，所述的工作气体为压缩空气。In the above step (2), the working gas is compressed air.
上述步骤(2)中，所述的沉积工艺参数为：工作气体温度为200-600℃，工作气体压力为1.5-3.0MPa，喷涂距离为10-60mm。In the above step (2), the deposition process parameters are: working gas temperature is 200-600°C, working gas pressure is 1.5-3.0 MPa, and spraying distance is 10-60 mm.
采用上述方法制备了一种IC装备等离子体刻蚀腔防护涂层，该防护涂层的孔隙率低于2％，陶瓷涂层与基体材料的界面结合强度为20-50MPa，涂层厚度为10-400μm。A protective coating for the plasma etching chamber of IC equipment is prepared by the above method. The porosity of the protective coating is less than 2%, the interface bonding strength between the ceramic coating and the base material is 20-50MPa, and the coating thickness is 10%. -400μm.
本发明将Al粉末和Y 2O 3-ZrO 2粉末按照重量比例为(0.1～1):1比例混合，在Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为(3～5)：1，经干燥得到微米级混合粉末，粉末粒度1～50μm。将上述混合粉末经加热的压缩空气预热后沉积在刻蚀腔材料内表面，获得离子体刻蚀腔防护涂层；所述冷喷涂沉积过程中：使用压缩空气作为工作气体，工作气体温度为200-600℃，工作气体压力为1.5-3.0MPa，喷涂距离为10-60mm。 In the present invention, Al powder and Y 2 O 3 -ZrO 2 powder are mixed according to a weight ratio of (0.1～1):1. In Y 2 O 3 -ZrO 2 powder, the weight ratio of Y 2 O 3 to ZrO 2 powder is The ratio is (3～5):1, and the micron-level mixed powder is obtained after drying, and the powder particle size is 1-50μm. The above-mentioned mixed powder is preheated by heated compressed air and deposited on the inner surface of the etching chamber material to obtain the plasma etching chamber protective coating; during the cold spray deposition process: compressed air is used as the working gas, and the working gas temperature is 200-600℃, working gas pressure is 1.5-3.0MPa, spraying distance is 10-60mm.
实施例1Example 1
本实施例是在6061合金基体上制备IC装备等离子体刻蚀腔防护涂层，制备方法具体步骤如下：In this embodiment, the protective coating of the plasma etching chamber for IC equipment is prepared on the 6061 alloy substrate. The specific steps of the preparation method are as follows:
(1)称量20g纯Al粉，160gY 2O 3粉末和40gZrO 2粉末，混合后干燥备用； (1) Weigh 20g pure Al powder, 160g Y 2 O 3 powder and 40g ZrO 2 powder, mix and dry for later use;
(2)以步骤(1)中制备的微米级Al+(Y 2O 3-ZrO 2)混合粉末为喷涂粉末，采用冷喷涂沉积技术在6061合金基体上制备Al+(Y 2O 3-ZrO 2)复合涂层，厚度约为180μm。 (2) Using the micron-sized Al+(Y 2 O 3 -ZrO 2 ) mixed powder prepared in step (1) as spraying powder, cold spray deposition technology is used to prepare Al+(Y 2 O 3 -ZrO 2 ) on the 6061 alloy substrate Composite coating, the thickness is about 180μm.
制备涂层时，冷喷涂工艺条件为：使用压缩空气为工作气体，气体温度为400℃，气体压力为2.0MPa，喷涂距离为20mm。When preparing the coating, the cold spraying process conditions are: compressed air is used as the working gas, the gas temperature is 400 ℃, the gas pressure is 2.0 MPa, and the spraying distance is 20 mm.
本实施制备的Al+(Y 2O 3-ZrO 2)复合涂层，孔隙率为2.0％，涂层与基体材料的界面结合强度为45MPa。 The Al+(Y 2 O 3 -ZrO 2 ) composite coating prepared in this implementation has a porosity of 2.0%, and the interface bonding strength between the coating and the base material is 45 MPa.
实施例2Example 2
本实施例是在Al基体上制备IC装备等离子体刻蚀腔防护涂层，制备方法具体步骤如下：In this embodiment, the protective coating of the plasma etching chamber for IC equipment is prepared on the Al substrate. The specific steps of the preparation method are as follows:
(1)称量30g纯Al粉，240g Y 2O 3粉末和60g ZrO 2粉末，混合后干燥备用； (1) Weigh 30g pure Al powder, 240g Y 2 O 3 powder and 60g ZrO 2 powder, mix and dry for later use;
(2)以步骤(1)中制备的微米级Al+(Y 2O 3-ZrO 2)混合粉末为喷涂粉末，采用冷喷涂沉积技术在Al基体上制备Al+(Y 2O 3-ZrO 2)复合涂层，厚度约为150μm。 (2) Using the micron-sized Al+(Y 2 O 3 -ZrO 2 ) mixed powder prepared in step (1) as spraying powder, cold spray deposition technology is used to prepare Al+(Y 2 O 3 -ZrO 2 ) composite on the Al matrix The thickness of the coating is about 150μm.
制备涂层时，冷喷涂工艺条件为：使用压缩空气为工作气体，气体温度为500℃，气体压力为2.2MPa，喷涂距离为25mm。When preparing the coating, the cold spraying process conditions are: compressed air is used as the working gas, the gas temperature is 500 ℃, the gas pressure is 2.2 MPa, and the spraying distance is 25 mm.
本实施制备的Al+(Y 2O 3-ZrO 2)复合涂层，孔隙率为1.8％，涂层与基体材料的界面结合强度为43MPa。 The Al+(Y 2 O 3 -ZrO 2 ) composite coating prepared in this implementation has a porosity of 1.8%, and the interface bonding strength between the coating and the base material is 43 MPa.
实施例3Example 3
本实施例是在6061合金基体上制备IC装备等离子体刻蚀腔防护涂层，制备方法具体步骤如下：In this embodiment, the protective coating of the plasma etching chamber for IC equipment is prepared on the 6061 alloy substrate. The specific steps of the preparation method are as follows:
(1)称量15g纯Al粉，90gY 2O 3粉末和30gZrO 2粉末，混合后干燥备用； (1) Weigh 15g pure Al powder, 90g Y 2 O 3 powder and 30g ZrO 2 powder, mix and dry for later use;
(2)以步骤(1)中制备的微米级Al+(Y 2O 3-ZrO 2)混合粉末为喷涂粉末，采用冷喷涂沉积技术在6061合金基体上制备Al+(Y 2O 3-ZrO 2)复合涂层，厚度约为220μm。 (2) Using the micron-sized Al+(Y 2 O 3 -ZrO 2 ) mixed powder prepared in step (1) as spraying powder, cold spray deposition technology is used to prepare Al+(Y 2 O 3 -ZrO 2 ) on the 6061 alloy substrate Composite coating, the thickness is about 220μm.
制备涂层时，冷喷涂工艺条件为：使用压缩空气为工作气体，气体温度为600℃，气体压力为2.3MPa，喷涂距离为20mm。When preparing the coating, the cold spraying process conditions are: compressed air is used as the working gas, the gas temperature is 600°C, the gas pressure is 2.3MPa, and the spraying distance is 20mm.
本实施制备的Al+(Y 2O 3-ZrO 2)复合涂层，孔隙率为1.9％，涂层与基体材料的界面结合 强度为40MPa。 The Al+(Y 2 O 3 -ZrO 2 ) composite coating prepared in this implementation has a porosity of 1.9%, and the interface bonding strength between the coating and the base material is 40 MPa.
以上实施例结果表明，本发明制备的IC装备等离子体刻蚀腔防护涂层，先通过表面活性剂的使用，采用水热法制备具有纳米晶结构的微米级团聚型YSZ粉体，然后才用冷喷涂技术制备YSZ涂层。该涂层与基体结合良好，涂层孔隙率低于2％，界面结合强度为20～50MPa，涂层厚度为10～400μm。The results of the above examples show that the IC equipment plasma etching chamber protective coating prepared by the present invention is first used to prepare micron-sized agglomerated YSZ powder with nanocrystalline structure through the use of surfactants and hydrothermally. YSZ coating prepared by cold spray technology. The coating is well combined with the substrate, the porosity of the coating is less than 2%, the interface bonding strength is 20-50 MPa, and the coating thickness is 10-400 μm.
以上是以发明技术方案为前提下给出详细的实施方式和具体操作过程，但本发明的保护范围不限于上面的实施例。The above is based on the technical solution of the invention as a prerequisite to give detailed implementation and specific operation process, but the protection scope of the present invention is not limited to the above embodiments.

Claims (5)

  1. 一种IC装备等离子体刻蚀腔防护涂层的制备方法，其特征在于，采用Al和Y 2O 3-ZrO 2的混合粉末制备等离子刻蚀腔体表面防护涂层，利用高速气流将Al和Y2O3-ZrO2的混合粉末直接喷涂于等离子刻蚀腔体表面，喷涂参数为：使用压缩空气为工作气体，气体温度为200-600℃，气体压力为1.5-3.0MPa，喷涂距离为10-60mm，使混合粉末沉积在等离子刻蚀腔的内表面上，形成均匀分布的防护涂层；其中，Al粉末和Y 2O 3-ZrO 2粉末的重量比例为0.1-1:1；其中Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为3-5：1。 A method for preparing a protective coating for a plasma etching chamber for IC equipment, which is characterized in that a mixed powder of Al and Y 2 O 3 -ZrO 2 is used to prepare a protective coating on the surface of the plasma etching chamber, and the Al and The mixed powder of Y2O3-ZrO2 is directly sprayed on the surface of the plasma etching chamber. The spraying parameters are: compressed air is used as the working gas, the gas temperature is 200-600℃, the gas pressure is 1.5-3.0MPa, and the spraying distance is 10-60mm. The mixed powder is deposited on the inner surface of the plasma etching chamber to form a uniformly distributed protective coating; where the weight ratio of Al powder and Y 2 O 3 -ZrO 2 powder is 0.1-1:1; where Y 2 O 3 -ZrO 2 powder, Y 2 O 3 powder and ZrO 2 weight ratio of 3-5: 1.
  2. 根据权利要求1所述的一种IC装备等离子体刻蚀腔防护涂层的制备方法，其特征在于：The method for preparing a protective coating for a plasma etching chamber for IC equipment according to claim 1, wherein:
    (1)微米级混合粉末的制备：(1) Preparation of micron-level mixed powder:
    将Al粉末和Y 2O 3-ZrO 2粉末按照重量比例为0.1-1:1比例混合，在Y 2O 3-ZrO 2粉末中，Y 2O 3与ZrO 2粉末的重量比为3～5：1，经干燥得到微米级混合粉末，粉末粒度1～50μm； The Al powder and Y 2 O 3 -ZrO 2 powder are mixed in a weight ratio of 0.1-1:1. In the Y 2 O 3 -ZrO 2 powder, the weight ratio of Y 2 O 3 to ZrO 2 powder is 3 to 5 :1. After drying, a micron-sized mixed powder is obtained, the powder size is 1-50μm;
    (2)冷喷涂沉积等离子体刻蚀腔防护涂层：(2) Cold spray deposition plasma etching chamber protective coating:
    将步骤(1)得到的微米级混合粉末经压缩空气预热后沉积在刻蚀腔材料内表面，获得离子体刻蚀腔防护涂层；所述冷喷涂沉积过程中：使用压缩空气作为工作气体，工作气体温度为200-600℃，工作气体压力为1.5-3.0MPa，喷涂距离为10-60mm。The micron-level mixed powder obtained in step (1) is preheated by compressed air and deposited on the inner surface of the etching chamber material to obtain a protective coating for the ion etching chamber; during the cold spray deposition process: compressed air is used as the working gas , The working gas temperature is 200-600℃, the working gas pressure is 1.5-3.0MPa, and the spraying distance is 10-60mm.
  3. 根据权利要求1所述的一种IC装备等离子体刻蚀腔防护涂层的制备方法，其特征在于：等离子体刻蚀腔防护涂层的喷涂装置，具有进气管1、加热器2、送粉器5、电磁阀6、超音速喷嘴4、控制柜1；进气管的一端与空气压缩机相连，另一端与送粉器、加热器、超音速喷嘴相连，进气管置于加热器中的部分为螺旋形结构。The method for preparing the protective coating of a plasma etching chamber for IC equipment according to claim 1, wherein the spraying device for the protective coating of the plasma etching chamber has an air inlet pipe 1, a heater 2, and a powder feeding device. Device 5, solenoid valve 6, supersonic nozzle 4, control cabinet 1. One end of the air inlet pipe is connected to the air compressor, and the other end is connected to the powder feeder, heater, and supersonic nozzle. The part where the air inlet pipe is placed in the heater It is a spiral structure.
  4. 根据权利要求1所述的一种IC装备等离子体刻蚀腔防护涂层的制备方法，其特征在于：制备等离子体刻蚀腔防护涂层的过程中，由空气压缩机输出的工作气体分为两路，一路进入加热器，经预热后气体进入超音速喷嘴的混合腔；另一路进入送粉器，作为载气将粉末引入超音速喷嘴与第一路经过预热的气体相混合，将粉末瞬时预热后，经过超音速喷嘴的缩放区，膨胀加速，形成超音速气固双相流，高速撞击刻蚀腔材料内表面使粉末发生剧烈变形实现沉积，并在刻蚀腔材料内表面形成复合型防护涂层。The method for preparing a protective coating for a plasma etching chamber for IC equipment according to claim 1, characterized in that: in the process of preparing the protective coating for the plasma etching chamber, the working gas output by the air compressor is divided into Two routes, one enters the heater, and the gas enters the mixing chamber of the supersonic nozzle after preheating; the other enters the powder feeder, which is used as carrier gas to introduce the powder into the supersonic nozzle and mix with the first preheated gas. After instantaneous preheating, the powder passes through the zoom zone of the supersonic nozzle, expands and accelerates to form a supersonic gas-solid two-phase flow, and hits the inner surface of the etching chamber material at high speed to cause the powder to undergo violent deformation to achieve deposition, and to deposit on the inner surface of the etching chamber material Form a composite protective coating.
  5. 根据权利要求4所述的一种IC装备等离子体刻蚀腔防护涂层的制备方法，其特征在于：防护涂层的孔隙率低于2％，陶瓷涂层与基体材料的界面结合强度为20-50MPa，涂层厚度为10-400μm。The method for preparing a protective coating for a plasma etching chamber for IC equipment according to claim 4, wherein the porosity of the protective coating is less than 2%, and the interface bonding strength between the ceramic coating and the base material is 20%. -50MPa, the coating thickness is 10-400μm.
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