CN110578143B - Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3Method for producing composite coating material - Google Patents
Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3Method for producing composite coating material Download PDFInfo
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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
- 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
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
- C23C28/324—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer with at least one metal matrix material layer comprising a mixture of at least two metals or metal phases or a metal-matrix material with hard embedded particles, e.g. WC-Me
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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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
- C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
- C23C28/3455—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer with a refractory ceramic layer, e.g. refractory metal oxide, ZrO2, rare earth oxides or a thermal barrier system comprising at least one refractory oxide layer
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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
- C23C4/11—Oxides
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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
- C23C4/12—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
Abstract
The invention discloses a method for preparing Al-ZrO by using atmospheric plasma spraying technology2/Y2O3A method for compounding coating materials belongs to the technical field of coating preparation. The method comprises the following steps: (1) mixing Al powder and ZrO2Proportioning and uniformly mixing the powder; spraying on the surface of the matrix by adopting a cold spraying solid deposition technology to prepare Al-ZrO2Priming a coating; (2) by atmospheric plasma spraying on Al-ZrO2Preparation of high purity Y on top of coating2O3Coating to form Al-ZrO2/Y2O3The composite coating has compact structure and low porosity, and the coating and the aluminum alloy matrix are well combined, and the bonding strength reaches 20-80 MPa.
Description
Technical Field
The invention relates to the technical field of coating preparation, in particular to Al-ZrO prepared by atmospheric plasma spraying2/Y2O3A method for preparing composite coating material.
Background
Y2O3And ZrO2The ceramic material has wide application in the fields of protection of IC equipment key parts and high-temperature oxidation resistance of metal materials. Taking the reaction chamber of the etching machine as an example, the etching uses the bombardment of high-energy plasma of strong corrosive gas to generate a high-strength corrosion environment, metal parts in the high-strength corrosion environment can be seriously corroded, and gold is releasedThe ions or particles pollute the cavity, and the circuit of the chip is short-circuited. In this case, a high purity dense oxide ceramic material is an ideal protective material.
The traditional IC equipment parts are protected by an anodic aluminum oxide coating. Because the parts are in a strong corrosive environment and an ion bombardment interaction state, once metal ions generated by corrosion dissolve out to cause system pollution, the loss cannot be estimated. Research shows that the yttrium oxide coating has better plasma erosion resistance and longer service life than aluminum oxide, so that the yttrium oxide coating becomes a novel coating for protecting IC equipment parts. Besides etchers, yttria coatings have great application value in other IC equipment components. However, yttrium is a precious metal and the yield of yttrium oxide, an oxide, is limited. The zirconium oxide can be used as a substitute of yttrium oxide, has similar antioxidant and protective effects, and can be used at a lower cost. Therefore, zirconia coatings and yttria-stabilized zirconia coatings are also the focus of research in this field.
The cold spraying solid deposition technology is a novel spraying technology which takes compressed gas (nitrogen, helium, air or mixed gas and the like) as an accelerating medium to drive metal particles to collide a substrate at a very high speed in a solid state, so that the particles are subjected to strong plastic deformation to deposit and form a coating. The atmospheric plasma spraying technology is to burn hydrocarbon gas such as propane, propylene and the like or liquid fuel such as aviation kerosene, alcohol and the like and high-pressure oxygen in a combustion chamber or a special nozzle to generate high-temperature and high-pressure flame flow, the temperature of the flame flow can reach 3200 ℃, the speed of the flame flow can reach more than 1500m/s, powder is axially or radially fed into plasma to generate molten or semi-molten particles, and the molten or semi-molten particles impact the surface of a substrate at high speed to form a coating. The bond strength, density and hardness of the sprayed coating are very high due to the spray particles impinging on the substrate surface at supersonic flight. ZrO (ZrO)2And Y2O3And the ceramic material is a more common ceramic material and has wider application in corrosive environments such as high-temperature oxidation and plasma erosion resistance. At the same time, ZrO2Is less costly than Y2O3Low, resources are comparativelyIs rich in Y and can replace Y in some use environments2O3The ceramic material achieves similar protection effect. At present, no atmosphere plasma spraying method for preparing Al-ZrO exists in China2/Y2O3Research on composite coating materials reports that work on high purity, high density Al-ZrO2/Y2O3The research on the composite coating material has important significance.
Disclosure of Invention
The invention aims to provide a method for preparing Al-ZrO by using atmospheric plasma spraying2/Y2O3Method for preparing Al-ZrO on inner surface of IC equipment key parts by using composite coating material2/Y2O3And (4) protective coating.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
Al-ZrO prepared by using atmospheric plasma spraying technology2/Y2O3A method of compounding a coating material comprising the steps of:
(1) preparing Al powder and ZrO powder with purity of more than 99.9%2Powder and Y2O3The powder is taken as a raw material;
(2) the surface of the base material is pretreated, wherein the pretreatment comprises degreasing, derusting and sand blasting;
(3) weighing Al powder and ZrO powder in required proportion2Mixing the powder until the powder is uniformly mixed; then spraying on the surface of the matrix by adopting a cold spraying solid deposition technology to obtain Al-ZrO deposited on the matrix2Coating;
(4) by atmospheric plasma spraying on Al-ZrO2Spraying Y on the surface of the coating2O3Coating to obtain Al-ZrO2/Y2O3And (4) composite coating.
In the step (1), the Al powder and ZrO2Powder and Y2O3The particle size of the powder is in the range of 3-60 μm.
In the above step (3), the Al powder and ZrO2The mass ratio of the powder is 1:9-9: 1.
In the step (2), the degreasing is performed by cleaning with acetone and alcohol; the rust removal and sand blasting treatment are carried out by using white corundum, and the granularity range of the white corundum is 20-100 mu m.
In the step (3), in the cold spraying solid deposition technique, compressed air (which may be nitrogen, argon, or a mixture thereof) is used as the working gas, the spraying distance is 15-40mm, the spraying pressure is 1.5-3.0MPa, and the spraying temperature is 200-650 ℃. Prepared Al-ZrO2The thickness of the coating is 10-50 μm.
In the step (4), in the atmospheric plasma spraying technology, the spraying distance is 5-50mm, the used fuel gas is propane, the combustion-supporting gas is oxygen, the powder feeding gas is nitrogen, and the gas flow rates of the fuel gas, the combustion-supporting gas and the powder feeding gas are respectively 20-80mL/min, 200-400mL/min and 20-80 mL/min; in the presence of Al-ZrO2Y prepared on the coating2O3The thickness of the coating is 80-200 μm.
The spraying distance of the used atmosphere plasma spraying equipment is 40-120mm, and the length of a spray pipe is 60-200 mm.
Compared with the prior art, the invention has the following beneficial effects:
Al-ZrO produced by the invention2/Y2O3The coating has compact structure and low porosity which reaches 0.5 to 4 percent; the binding force between the coating and the substrate reaches 20-80MPa, and is higher than that of the common plasma spraying and cold spraying coatings. Therefore, the Al-ZrO prepared by the atmospheric plasma spraying of the invention2/Y2O3The coating has more excellent mechanical properties.
Drawings
FIG. 1 shows the preparation of Al-ZrO by the present invention2/Y2O3A process flow chart of the composite coating.
Detailed Description
For a further understanding of the present invention, the following description is given in conjunction with the examples which are set forth to illustrate, but are not to be construed to limit the present invention, features and advantages.
Example 1:
the embodiment provides a method for preparing an Al-ZrO2/Y2O3 coating by atmospheric plasma spraying (the flow is shown in figure 1), which specifically comprises the following steps:
(1) preparing Al powder and Y with purity of more than 99.9%2O3Powder and ZrO2The powder has the granularity range of 5-60 mu m and a single cubic structure;
(2) pretreating key aluminum alloy parts of the IC equipment, cleaning the key aluminum alloy parts by using acetone and alcohol, and then performing rust removal and sand blasting treatment by using white corundum with the granularity of 50-100 mu m;
(3) weighing the following components in a weight ratio of 1: 1.5 of Al powder and ZrO2Mixing the powder until the powder is uniformly mixed; spraying Al-ZrO on the surface of the matrix by adopting a cold spraying solid deposition technology to deposit2And (4) coating. In the deposition process: compressed air is used as working gas, the spraying distance is 30mm, the spraying pressure is 2.0MPa, and the spraying temperature is 600 ℃.
Al-ZrO produced on the surface of substrates2The coating thickness reached 30 μm.
(4) Applying atmosphere plasma spraying technology to Al-ZrO2Spraying Y on the surface of the coating2O3Coating to obtain Al-ZrO2/Y2O3A composite coating; in the spraying process, the used fuel gas is propane, the flow rate of the propane is 40mL/min, the combustion-supporting gas is oxygen, the flow rate of the oxygen is 180mL/min, the powder feeding gas is nitrogen, the flow rate of the nitrogen is 80mL/min, the spraying distance is 90mm, and the length of the spraying pipe is 60 mm. Preparation of Y2O3The coating thickness was 150. mu.m.
As detected, Al-ZrO produced in this example2/Y2O3The porosity of the composite coating is 2.5%, the bonding force between the coating and the substrate is 35MPa, and the overall thickness of the coating is 180 mu m. .
Example 2:
this example provides an atmospheric plasma spray process for preparing Al-ZrO2/Y2O3The coating method specifically comprises the following steps:
(1) selecting Al powder and Y2O3Powder and ZrO2Powder, granules thereofThe degree ranges from 20 to 40 mu m;
(2) pretreating key aluminum alloy parts of the IC equipment, cleaning the key aluminum alloy parts by using acetone and alcohol, and then performing rust removal and sand blasting treatment by using white corundum with the granularity of 50-100 mu m;
(3) weighing the following components in a weight ratio of 1: 1.5 of Al powder and ZrO2Mixing the powder until the powder is uniformly mixed; and spraying the Al-ZrO2 coating on the surface of the matrix by adopting a cold spraying solid deposition technology. In the deposition process: compressed air is used as working gas, the spraying distance is 35mm, the spraying pressure is 1.8MPa, and the spraying temperature is 600 ℃.
Al-ZrO produced on the surface of substrates2The coating thickness reached 30 μm.
(4) Applying atmosphere plasma spraying technology to Al-ZrO2Spraying Y on the surface of the coating2O3Coating to obtain Al-ZrO2/Y2O3A composite coating; in the spraying process, the used fuel gas is propane, the flow rate of the propane is 60mL/min, the combustion-supporting gas is oxygen, the flow rate of the oxygen is 180mL/min, the powder feeding gas is nitrogen, the flow rate of the nitrogen is 70mL/min, the spraying distance is 100mm, and the length of the spraying pipe is 60 mm.
Preparation of Y2O3The coating thickness was 120. mu.m.
As detected, Al-ZrO produced in this example2/Y2O3The porosity of the composite coating is 1.2%, the bonding force between the coating and the substrate is 45MPa, and the overall thickness of the coating reaches 150-160 mu m. .
Example 3:
this example provides an atmospheric plasma spray process for preparing Al-ZrO2/Y2O3The coating method specifically comprises the following steps:
(1) al powder, Y2O3Powder and ZrO2Powder with the granularity ranging from 40 to 60 mu m;
(2) pretreating key aluminum alloy parts of the IC equipment, cleaning the key aluminum alloy parts by using acetone and alcohol, and then performing rust removal and sand blasting treatment by using white corundum with the granularity of 50-100 mu m;
(3) weighing the following components in a weight ratio of 1: 1.5 of Al powder and ZrO2Mixing the powder until the powder is uniformly mixed; spraying Al-ZrO on the surface of the matrix by adopting a cold spraying solid deposition technology to deposit2And (4) coating. In the deposition process: compressed air (nitrogen, argon or their mixture) is used as working gas, the spraying distance is 30mm, the spraying pressure is 2.0MPa, and the spraying temperature is 550 ℃.
Al-ZrO produced on the surface of substrates2The coating thickness reached 30 μm.
(4) Al-ZrO cold spraying by adopting atmospheric plasma spraying technology2Priming coating surface spraying Y2O3Coating to obtain Al-ZrO2/Y2O3A composite coating; in the spraying process, the used fuel gas is propane, the fuel gas flow is 35mL/min, the combustion-supporting gas is oxygen, the oxygen flow is 150mL/min, the powder feeding gas is nitrogen, the nitrogen flow is 40mL/min, the spraying distance is 80mm, and the length of the spraying pipe is 60 mm. Preparation of Y2O3The coating thickness was 170. mu.m.
As detected, Al-ZrO produced in this example2/Y2O3The porosity of the composite coating is 0.5%, the bonding force between the coating and the substrate is 40MPa, and the overall thickness of the coating is 200 microns.
Claims (6)
1. Al-ZrO prepared by using atmospheric plasma spraying technology2/Y2O3A method of compounding a coating material, characterized by: the method comprises the following steps:
(1) preparing Al powder and ZrO powder with purity of more than 99.9%2Powder and Y2O3The powder is taken as a raw material;
(2) the surface of the base material is pretreated, wherein the pretreatment comprises degreasing, derusting and sand blasting;
(3) weighing Al powder and ZrO powder in required proportion2Mixing the powders until uniformly mixing the Al powder and the ZrO powder2The mass ratio of the powder is 1:9-9: 1; then spraying on the surface of the matrix by adopting a cold spraying solid deposition technology to obtain Al-ZrO deposited on the matrix2Coating; in the cold spray solid state deposition technique, theCompressed air is used as working gas, the spraying distance is 15-40mm, the spraying pressure is 1.5-3.0MPa, and the spraying temperature is 200-; the Al-ZrO2The thickness of the coating is 10-50 μm;
(4) by atmospheric plasma spraying on Al-ZrO2Spraying Y on the surface of the coating2O3Coating to obtain Al-ZrO2/Y2O3And (4) composite coating.
2. The method of claim 1, wherein the Al-ZrO is prepared by using an atmospheric plasma spraying technique2/Y2O3A method of compounding a coating material, characterized by: in the step (1), the Al powder and ZrO2Powder and Y2O3The particle size of the powder is in the range of 3-60 μm.
3. The method of claim 1, wherein the Al-ZrO is prepared by using an atmospheric plasma spraying technique2/Y2O3A method of compounding a coating material, characterized by: in the step (2), the degreasing is carried out by cleaning with acetone and alcohol; the derusting and the sand blasting are carried out by using white corundum, and the granularity range of the white corundum is 20-100 mu m.
4. The method of claim 1, wherein the Al-ZrO is prepared by using an atmospheric plasma spraying technique2/Y2O3A method of compounding a coating material, characterized by: in the step (4), in the atmospheric plasma spraying technology, the spraying distance is 5-50mm, the used fuel gas is propane, the combustion-supporting gas is oxygen, the powder feeding gas is nitrogen, and the gas flow rates of the fuel gas, the combustion-supporting gas and the powder feeding gas are respectively 20-80mL/min, 200-400mL/min and 20-80 mL/min.
5. The Al-ZrO produced by the atmospheric plasma spraying technique according to claim 1 or 42/Y2O3A method of compounding a coating material, characterized by: in step (4), in Al-ZrO2Y prepared on the coating2O3The thickness of the coating is 80-200 μm.
6. The Al-ZrO prepared by the atmospheric plasma spraying technique according to claim 42/Y2O3A method of compounding a coating material, characterized by: the spraying distance of the used atmosphere plasma spraying equipment is 40-120mm, and the length of a spray pipe is 60-200 mm.
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