CN113584417B - Rare earth metal salt ceramic composite coating and preparation method and application thereof - Google Patents

Rare earth metal salt ceramic composite coating and preparation method and application thereof Download PDF

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CN113584417B
CN113584417B CN202110881661.XA CN202110881661A CN113584417B CN 113584417 B CN113584417 B CN 113584417B CN 202110881661 A CN202110881661 A CN 202110881661A CN 113584417 B CN113584417 B CN 113584417B
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sio
composite coating
plasma
rare earth
earth metal
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CN113584417A (en
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梁福坤
陈立航
余宜璠
贺邦杰
杨佐东
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Chongqing Zhenbao Technology Co ltd
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Chongqing Zhenbao Industrial Co ltd
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    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
    • 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
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/32—Gas-filled discharge tubes
    • H01J37/32431—Constructional details of the reactor
    • H01J37/32458—Vessel
    • H01J37/32477—Vessel characterised by the means for protecting vessels or internal parts, e.g. coatings

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Abstract

The invention relates to a rare earth metal salt ceramic composite coating and a preparation method and application thereof, belonging to the technical field of plasma spraying. Will Y 2 O 3 、Al 2 O 3 And SiO 2 Powder, mixing, preparing Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder is plasma sprayed on the surface of the pretreated base material to prepare Y 2 SiO 5 ‑Y 3 Al 5 O 12 And (4) composite coating. Y in the composite coating 2 SiO 5 Is amorphous Y 2 SiO 5 Structure and mass fraction of 60-75%, Y 3 Al 5 O 12 Has a cubic crystal structure. Amorphous Y 2 SiO 5 Y as an amorphous material with a more uniform structure and composition, cubic crystal structure 3 Al 5 O 12 The corrosion resistance is excellent. Y is 2 SiO 5 ‑Y 3 Al 5 O 12 The composite coating layer combines amorphous Y 2 SiO 5 And Y 3 Al 5 O 12 The method has the advantages of better plasma etching resistance and longer service life.

Description

Rare earth metal salt ceramic composite coating and preparation method and application thereof
Technical Field
The invention belongs to the technical field of plasma spraying, and relates to a rare earth metal salt ceramic composite coating, and a preparation method and application thereof.
Background
With the reduction in the size of semiconductor devices, the increase in the size of Liquid Crystal Displays (LCDs) and silicon wafers (from 200mm to 300mm), plasma etching is becoming a widely used etching technique in the fabrication processes of semiconductor devices and microelectronics, which are on the order of micrometers. Plasma etching refers to an etching technique for completing pattern transfer by generating plasma containing charged particles such as plasma, electrons and the like, neutral atoms with high chemical activity, molecules and free radicals in a glow discharge mode, diffusing the active particles to a part to be etched to react with an etched material to form volatile products to be removed, and realizing the irreplaceable process of transferring a fine pattern from a photoetching template to a wafer with high fidelity in the production of a super-large scale integrated circuit.
The reaction gas for plasma etching comprises CF 4 /O 2 、NF 3 、Cl 2 、CH 4 and/Ar and the like can generate a large amount of active free radicals such as Cl radicals and F radicals in the plasma etching process, and when the active free radicals etch semiconductor devices, the active free radicals can also corrode the inner surface of a plasma etching process cavity prepared from aluminum and aluminum alloy, and the strong corrosion generates a large amount of particles, so that not only is the production equipment required to be frequently maintained, but also the failure of the etching process cavity and the damage of the devices can be even caused in severe cases.
Early plasma etching protection technology was to deposit a dense hard anodic protection layer on an aluminum substrate, but since the corrosion resistance of hard anodic alumina is very limited and the hard anodic alumina inevitably has voids and partial damages during deposition, corrosive media will penetrate to the substrate surface through these voids and damaged surfaces, causing the substrate corrosion. There is therefore a need to develop corrosion-resistant coatings that are economical and practical. With the development of plasma spraying technology, Atmospheric Plasma Spraying (APS) Al 2 O 3 The coating has been widely applied as a protective coating for a plasma etching chamber due to its high insulation and high durability against plasma. With the development of semiconductor technology, high purity Al 2 O 3 Coating (>99.9%) is gradually used to eliminate the influence of purity on the performance of the equipment, but as the size of the wafer increases, the inner diameter of the plasma etching process chamber increases from 400mm to 500-600mm, the corresponding plasma power increases, the damage to the inner wall of the etching process chamber increases, and the A1 is increased 2 O 3 The coating is easy to generate particles in the etching process, and the coating and the substrate are easy to fall off. Under higher power operating conditions, Y 2 O 3 Coating, especially high purity Y 2 O 3 The tendency of coatings to be applied to plasma chambers due to their stability in Cl and F radicals, and their higher durability to plasma, has greatly facilitated the application of plasma sprayed high purity ceramic coatings to resist plasma erosion inside plasma etch chambers, especially the preferred coating materials for etchers above 8 inches. Nevertheless, under high power plasma attack, Y prepared by the prior art 2 O 3 The coating has limited plasma etching resistance and short service life.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a rare earth metal salt ceramic composite coating.
The second purpose of the invention is to provide a preparation method of the rare earth metal salt ceramic composite coating.
The invention also aims to provide the application of the rare earth metal salt ceramic composite coating as a plasma etching process cavity coating.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a rare earth metal salt ceramic composite coating is Y 2 SiO 5 -Y 3 Al 5 O 12 Composite coating of Y 2 SiO 5 Is amorphous Y 2 SiO 5 Amorphous Y in the composite coating 2 SiO 5 The mass fraction of (A) is 60-75%.
Preferably, the thickness of the composite coating is 100-400 μm.
2. A preparation method of a rare earth metal salt ceramic composite coating specifically comprises the following steps:
(1) get Y 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 2-4 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1);
(2) will Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder is sprayed on the surface of the pretreated base material by plasma spraying.
Preferably, in step (1), Y is 2 O 3 、Al 2 O 3 And SiO 2 The mass ratio of the powder is 60-75: 10-15: 15-25.
Preferably, in step (1), Y is 2 O 3 、Al 2 O 3 And SiO 2 The particle size of the powder is 300-600 nm.
Preferably, in the step (1), Y in the mixed powder 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm.
Preferably, in the step (2), the plasma spraying is specifically: spraying at voltage of 30-60V and current of 800-900A at powder feeding speed of 10-40g/min and distance of 90-150 mm.
Preferably, in the step (2), argon and helium gas or argon and hydrogen gas are used as plasma gas in the plasma spraying, the flow rate of the argon gas is 60-90L/min, and the flow rate of the helium gas or the hydrogen gas is 10-20L/min.
Preferably, the pretreatment of the substrate in step (2) is: cleaning and drying the base material, and then carrying out roughening treatment and purification treatment on the surface of the base material in sequence.
Preferably, the surface roughness Ra of the substrate after the roughening treatment is 4 to 10 μm.
Preferably, the roughening treatment is specifically: the surface of the base material is sandblasted, the sandblasting pressure is 0.2-0.3Mpa, and the sandblasting height is 300-400 mm.
Preferably, the purification treatment is: the roughened substrate was blown with compressed air.
3. Application of rare earth metal salt ceramic composite coating as plasma etching protective coating
The invention has the beneficial effects that:
with Y 2 O 3 、Al 2 O 3 And SiO 2 Preparation of Y from powder 2 SiO 5 And Y 3 Al 5 O 12 Then amorphous Y obtained by plasma spraying 2 SiO 5 -Y 3 Al 5 O 12 And (4) composite coating. Y in the composite coating 2 SiO 5 Is of an amorphous structure, Y 3 Al 5 O 12 Is of cubic crystal structure, wherein amorphous Y 2 SiO 5 Compared with crystalline materials, the amorphous material is more uniform in organization structure and composition, does not have channels which are easy to cause local rapid corrosion such as crystal boundary, dislocation and the like, and has extremely high strength and toughness and more excellent wear resistance and corrosion resistance. Y is 3 Al 5 O 12 The material has a cubic crystal structure, no birefringence effect, small high-temperature creep and excellent corrosion resistance. Amorphous Y 2 SiO 5 -Y 3 Al 5 O 12 The composite coating layer combines amorphous Y 2 SiO 5 Excellent mechanical properties and corrosion resistance, and Y 3 Al 5 O 12 Small creep at high temperature and excellent corrosion resistance, and has a specific Y ratio under high-power plasma attack 2 O 3 The coating has better plasma etching resistance and longer service life.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a graph showing the results of corrosion resistance tests of the coatings of examples 1, 2, 3 and 4.
FIG. 2 shows Y in example 4 2 SiO 5 And Y 3 Al 5 O 12 XRD patterns of powder and composite coatings.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
Cleaning and drying an aluminum substrate, performing sand blasting treatment on the surface of the substrate under the conditions that the sand blasting pressure is 0.2Mpa and the sand blasting height is 400mm to obtain the substrate with the surface roughness Ra of 4 mu m, and then blowing the sand blasted substrate by using compressed air. And (3) adding the following components in an amount of 60: 15: 25 mass ratio of Y with the particle size of 300-600nm 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 2 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1), Y in the mixed powder prepared 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm. Argon and helium are used as plasma gas, argon is used as main gas, helium is used as secondary gas, wherein the flow rate of argon is 60L/min, the flow rate of helium is 20L/min, under the conditions that the voltage is 30V and the current is 800A, plasma spraying is carried out at the powder feeding speed of 40g/min and the distance from the surface of the base material to 120mm, a composite coating with the thickness of 389 micrometers is obtained, and Y in the prepared coating 2 SiO 5 Is 60 percent.
Example 2
Cleaning and drying an aluminum substrate, performing sand blasting treatment on the surface of the substrate under the conditions that the sand blasting pressure is 0.3Mpa and the sand blasting height is 400mm to obtain the substrate with the surface roughness Ra of 6 mu m, and then blowing the sand blasted substrate by using compressed air. Mixing the following raw materials in a ratio of 65: 15: 20 mass ratio of Y with the particle size of 300-600nm 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 2 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1), Y in the mixed powder prepared 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm. Argon and hydrogen are used as plasma gas, argon is used as main gas, hydrogen is used as secondary gas, the flow rate of the hydrogen is 90L/min, the flow rate of the hydrogen is 10L/min, plasma spraying is carried out at the powder feeding speed of 20g/min and the distance of 150mm from the surface of a base material under the conditions that the voltage is 40V and the current is 860A, a composite coating with the thickness of 194 mu m is obtained, and Y in the prepared coating 2 SiO 5 Is 67% by mass.
Example 3
Cleaning and drying an aluminum substrate, performing sand blasting treatment on the surface of the substrate under the conditions that the sand blasting pressure is 0.3Mpa and the sand blasting height is 350mm to obtain the substrate with the surface roughness Ra of 10 mu m, and blowing the sand-blasted substrate by using compressed air. And (3) adding 70: 10: 20 mass ratio of Y with the particle size of 300-600nm 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 3 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1), Y in the mixed powder prepared 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm. Argon and hydrogen are used as plasma gas, argon is used as main gas, hydrogen is used as secondary gas, the flow rate of the hydrogen is 60L/min, the flow rate of the hydrogen is 20L/min, plasma spraying is carried out at the powder feeding speed of 30g/min and the distance of 140mm from the surface of a base material under the conditions that the voltage is 50V and the current is 840A, a composite coating with the thickness of 306 mu m is obtained, and Y in the prepared coating 2 SiO 5 The mass fraction of (b) is 71%.
Example 4
Cleaning and drying an aluminum substrate, performing sand blasting treatment on the surface of the substrate under the conditions that the sand blasting pressure is 0.3Mpa and the sand blasting height is 350mm to obtain the substrate with the surface roughness Ra of 10 mu m, and blowing the sand-blasted substrate by using compressed air. And (3) at a speed of 75: 10: 15 mass ratio of Y with the particle size of 300-600nm 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 4 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1), Y in the mixed powder prepared 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm. Argon and helium are used as plasma gas, argon is used as main gas, helium is used as secondary gas, wherein the flow rate of argon is 90L/min, the flow rate of helium is 10L/min, under the conditions that the voltage is 60V and the current is 900A, plasma spraying is carried out at the powder feeding speed of 10g/min and the distance from the surface of the base material to 90mm, a composite coating with the thickness of 110 microns is obtained, and Y in the prepared coating 2 SiO 5 Is 75 percent.
The composite coatings of examples 1-4 were etched in 7% HCl solution, and the time for each composite coating to peel was recorded, and the test results are shown in FIG. 1. As can be seen from FIG. 1, the time for the composite coatings of examples 1-4 to peel was: 184min, 195min, 217min and 238 min. Taking Y prepared by conventional process 2 O 3 The plasma sprayed coating is corroded in 7 percent HCl solution, and the stripping time is 45min, so that the coating prepared by the method is more favorable than Y prepared by the conventional process 2 O 3 The plasma spraying coating has better corrosion resistance.
Taking Y prepared under the conditions of example 4 2 SiO 5 And Y 3 Al 5 O 12 XRD component analysis is carried out on the powder and the composite coating respectively, and the analysis result is shown in figure 2. As can be seen from FIG. 2, the XRD pattern of the composite coating has the amorphous scattering characteristic of obvious dispersion and broadening, which corresponds to Y in the mixed powder 2 SiO 5 Position of (2), description of Y 2 SiO 5 After the melting and shooting, the amorphous Y is in the composite coating 2 SiO 5 And Y is 3 Al 5 O 12 The corresponding positions are all characterized by diffraction of the crystalline sample, which indicates Y in the composite coating 3 Al 5 O 12 Is a crystalline structure, therefore, the amorphous Y prepared by the invention 2 SiO 5 -Y 3 Al 5 O 12 And (4) composite coating.
Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (9)

1. The rare earth metal salt ceramic composite coating is characterized in that Y is adopted as the composite coating 2 SiO 5 -Y 3 Al 5 O 12 A composite coating consisting of Y 2 SiO 5 And Y 3 Al 5 O 12 Is plasma sprayed on the surface of the pretreated substrate, wherein Y is 2 SiO 5 Is amorphous Y 2 SiO 5 Amorphous Y in the composite coating 2 SiO 5 The mass fraction of (A) is 60-75%.
2. The rare earth metal salt ceramic composite coating of claim 1, wherein the thickness of the composite coating is 100-400 μm.
3. The method for preparing the rare earth metal salt ceramic composite coating according to claim 1, wherein the method comprises the following steps:
(1) get Y 2 O 3 、Al 2 O 3 And SiO 2 Mixing the powders, calcining at 1500 deg.C for 2-4 hr to obtain Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder of (1);
(2) will Y 2 SiO 5 And Y 3 Al 5 O 12 The mixed powder is sprayed on the surface of the pretreated base material by plasma spraying.
4. The method of claim 3, wherein in step (1), Y is 2 O 3 、Al 2 O 3 And SiO 2 The mass ratio of the powder is 60-75: 10-15: 15-25.
5. The method of claim 3, wherein in step (1), Y is 2 O 3 、Al 2 O 3 And SiO 2 The particle size of the powder is 300-600 nm.
6. The method of claim 3, wherein in step (1), Y is in the mixed powder 2 SiO 5 And Y 3 Al 5 O 12 The particle diameters of the particles are all 15-65 μm.
7. The method according to claim 3, wherein in the step (2), the plasma spraying is specifically: spraying at voltage of 30-60V and current of 800-900A at powder feeding speed of 10-40g/min and distance of 90-150 mm.
8. The method of claim 7, wherein in the step (2), argon and helium or argon and hydrogen are used as plasma gas for the plasma spraying, the flow rate of the argon is 60-90L/min, and the flow rate of the helium or hydrogen is 10-20L/min.
9. Use of a rare earth metal salt ceramic composite coating according to any one of claims 1-2 as a protective coating for plasma etching.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030134134A1 (en) * 2002-01-11 2003-07-17 Saint-Gobain Ceramics & Plastics, Inc. Method for forming ceramic layer having garnet crystal structure phase and article made thereby
CN103194715A (en) * 2012-01-05 2013-07-10 中国科学院微电子研究所 Preparation of amorphous Y by atmospheric plasma spraying technology3Al5O12Method for coating
CN105648386A (en) * 2016-02-18 2016-06-08 中国科学院上海硅酸盐研究所 Thermal spraying aluminum oxide-yttrium oxide composite ceramic coating and preparing method thereof
KR102259919B1 (en) * 2020-03-06 2021-06-07 주식회사 그린리소스 Coating member of a chamber and method for manufacturing the same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030134134A1 (en) * 2002-01-11 2003-07-17 Saint-Gobain Ceramics & Plastics, Inc. Method for forming ceramic layer having garnet crystal structure phase and article made thereby
CN103194715A (en) * 2012-01-05 2013-07-10 中国科学院微电子研究所 Preparation of amorphous Y by atmospheric plasma spraying technology3Al5O12Method for coating
CN105648386A (en) * 2016-02-18 2016-06-08 中国科学院上海硅酸盐研究所 Thermal spraying aluminum oxide-yttrium oxide composite ceramic coating and preparing method thereof
KR102259919B1 (en) * 2020-03-06 2021-06-07 주식회사 그린리소스 Coating member of a chamber and method for manufacturing the same

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Title
"等离子喷涂法制备炭/炭复合材料硅酸钇涂层研究";黄敏等;《新型炭材料》;20100630;第25卷(第3期);第187-191页 *

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