CN110408880A - A kind of atmospheric plasma spraying technology preparation Y+Y2O3/Y2O3The method of composite coating - Google Patents
A kind of atmospheric plasma spraying technology preparation Y+Y2O3/Y2O3The method of composite coating Download PDFInfo
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- CN110408880A CN110408880A CN201910823123.8A CN201910823123A CN110408880A CN 110408880 A CN110408880 A CN 110408880A CN 201910823123 A CN201910823123 A CN 201910823123A CN 110408880 A CN110408880 A CN 110408880A
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- coating
- plasma spraying
- composite coating
- powder
- atmospheric plasma
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Classifications
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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
- C23C4/06—Metallic material
-
- 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 present invention relates to the preparation technical field of ceramic coating, specially a kind of atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating.This method comprises the following steps: (1) Y for selecting purity to be greater than 99.9wt%2O3Powder and Y powder carry out with when mixed processing powder；(2) surface of spraying sample is pre-processed；(3) it is sprayed by atmospheric plasma spraying technology in matrix surface, prepares Y+Y2O3Coating is as intermediate layer；(4) using atmospheric plasma spraying technology in Y+Y2O3Coating outer layer deposits high-purity Y2O3Coating forms Y+Y2O3/Y2O3Composite coating；(5) by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, and temperature is 160~180 DEG C, 4~6h of time.Y+Y prepared by the present invention2O3/Y2O3Composite coating structure is fine and close, and porosity is low, and between 0.5%~2%, the bond strength of coating and matrix reaches 30~70MPa.
Description
Technical field
The present invention relates to the preparation technical field of ceramic coating, specially a kind of atmospheric plasma spraying technology prepares Y+
Y2O3/Y2O3The method of composite coating is suitable for IC and equips plasma etch chamber protective coating.
Background technique
In previous research, plasma spray technology preparation yttria coating is mostly used to be used to make table in IC equipment key components and parts
The protective coating in face.When depositing coating, it usually needs yttrium powder is heated to melting or semi-molten state, condition are severe
It carves, and expense is more expensive.If technological parameter selection is improper, the coating of preparation just will appear outer layer transversal crack, not enough
Densification, quality need to be further increased.
Current international trend is the synthesis for studying yttrium oxide and yttria-stabilized zirconia ceramic coating to improve coating
Performance.There are some new work successively in the research that plasma spray technology prepares yttrium oxide protective coating in the country.In for example,
State patent publication No. CN104357785A discloses a kind of method for quickly preparing plasma etching machine high-purity yttrium oxide coating,
The high-purity yttrium oxide powder produced using Beijing Mine and Metallurgy General Inst, using three anode plasma spray systems and multi-spindle machining hand
Scheme sprayed, matrix heat input can be effectively reduced by being compared with the traditional method, and improve the purity and uniformity of coating, quickly
It prepares with a thickness of 120~180 μm, purity >=99wt% high-purity yttrium oxide coating greatly improves large scale integrated circuit
Etch the plasma resistant erosion property and service life of machine part.
China Patent Publication No. CN109440052A and publication number CN109609888A is related to a kind of atmosphere plasma spray
The method that painting prepares yttrium oxide composite coating, the technology are sprayed using atmospheric plasma equipment, first carry out piece surface
Then hard anodizing carries out masking protection and blasting treatment to piece surface, next in treated piece surface
Plasma oxidation yttrium coating is prepared, the yttria coating that this method obtains has high rigidity, high compactness, high tensile, resistance to
Corrosion and reactance voltage have very excellent performance indicator, and also there is good binding force on yttria coating boundary, will not take off
Fall phenomenon.
China Patent Publication No. CN105648386A is related to thermal spraying alumina-yttria composite ceramic coat and its preparation
Method, the alumina-yttria composite ceramic coat is formed on metal base or the transition of stress of metallic substrate surface
On layer.In the world, Seok etc. is prepared for several etch resistant coatings, such as Al using the method for air plasma spraying2O3Coating,
Y2O3The Y of coating, different yttria levels2O3-ZrO2Coating, Y2O3-ZrO2-A12O3Coating etc., and test their etching
Rate, it was therefore concluded that: Y2O3-ZrO2The etch rate of coating is approximately less than yttria coating, and works as Y2O3: ZrO2When for 70:30,
The etch rate of coating is minimum, about 5nm/min, i.e. resistant to plasma etching performance preferably (Seok H W, Kim Y C, Chol E
Y, et a1.Multi-component thermal spray coating material and production method
And coating method therefore:US, 13/915976 [P] .2013-06-12.).
Summary of the invention
Aiming at the above shortcomings existing in the prior art, mesh of the invention is to provide a kind of atmospheric plasma spraying technology system
Standby Y+Y2O3/Y2O3It is etched in high power to solve current IC equipment plasma etch chamber protective coating for the method for composite coating
The problem of failure is easy in journey opens up a kind of new effective way for preparing IC equipment plasma etch chamber protective coating, with
Phase obtains practical application early.
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of atmospheric plasma spraying technology preparation Y+Y2O3/Y2O3The method of composite coating, includes the following steps:
Step (1) selects purity to be greater than the Y of 99.9wt%2O3Powder and Y powder weigh the powder of different quality proportion respectively
End is mixed；
Step (2) is sprayed using atmospheric plasma spraying technology in matrix surface, and Y+Y is prepared2O3Coating；
Step (3), by atmospheric plasma spraying technology in Y+Y2O3Y is deposited outside coating2O3Coating forms Y+Y2O3/
Y2O3Composite coating；
Step (4), by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, temperature 160
~180 DEG C, 4~6h of time.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, in step (1), Y2O3Powder
The granularity at end is 10~60 μm.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, in step (1), Y powder
With Y2O3The mass ratio range of powder is 1:1~1:50.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating is right before step (2) spraying
Spraying substrate surface is pre-processed, and specifically comprises the following steps: respectively to carry out spraying substrate surface using acetone and alcohol
Pretreatment and blasting treatment, blast media used are white fused alumina, and particle size range is 50~100 μm.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, step (2) and step (3)
In, the air plasma spraying equipment used, combustion gas used is propane, and combustion-supporting gas is oxygen, and powder feeding gas is nitrogen.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, when combustion gas used is third
Alkane, combustion-supporting gas is oxygen, and when powder feeding gas is nitrogen, gas flow is respectively 20~80mL/min, 200~400mL/min and
20~80mL/min.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, atmospheric plasma used
Spraying equipment, spray distance are 40~120mm, and jet pipe length is 60~200mm.
The atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, Y+Y2O3/Y2O3Compound painting
The porosity of layer is 2% hereinafter, Y+Y2O3/Y2O3The interface bond strength of composite coating and basis material is 30~70MPa, is applied
Layer is with a thickness of 10~400 μm.
Design philosophy of the invention is:
Since thermal expansion coefficient differs greatly between ceramics and metal, simple Y2O3Coating is past in conjunction with metallic matrix
It is past not sufficiently tight, requirement is not able to satisfy under some special operation conditions.Using metallic yttrium as compatibility metal and Y2O3Mixing
Prepare Y+Y2O3On the one hand metal-cermic coating can reduce thermal expansion coefficient, enhancing Y+ between ceramics and metal as bottom
Y2O3Binding force between metal-cermic coating and metallic matrix；On the other hand, the use of Y can not introduce other kinds of impurity
Metal.
It advantages of the present invention and has the beneficial effect that:
The Y+Y that the present invention is prepared using atmospheric plasma spraying technology with a thickness of 10~400 μm2O3/Y2O3Composite coating,
Plasma etch chamber protective materials is equipped as IC.This method deposition efficiency is high, and the composite coating of double-layer structure is than single
Yttrium coating be easier in conjunction with metallic matrix, alleviate and there is thermal expansion between yttrium coating and metallic matrix
The problem that difference of coefficients is larger, binding force is lower.Meanwhile coating layer thickness can be adjusted according to actual use situation, to prepare
Thick IC equips plasma etch chamber protective coating.
Detailed description of the invention
Fig. 1 is Y+Y2O3/Y2O3Composite coating structure schematic diagram.In figure, 1- matrix, 2- intermediate layer, the high-purity Y of 3-2O3
Coating.
Specific embodiment
In the specific implementation process, the present invention is by Y powder and Y2O3Powder is according to pure Y powder and Y2O3The weight ratio of powder
Example is that 1:1~1:50 (preferably 1:1~1:10) is mixed, and is dried to obtain micron order mixed-powder, 10~60 μm of powder size.
By above-mentioned Y+Y2O3Mixed-powder is deposited on etch chamber material inner surface through atmospheric plasma spraying technology, obtains plasma etching
Inner cavity surface protective coating.Y+Y prepared by the present invention2O3/Y2O3Composite coating structure is fine and close, and the porosity of the composite coating exists
The bond strength at 2% or less (generally 0.5%~2%), coating and basis material interface is 30~70MPa, and coating layer thickness is
10~400 μm.
Hereinafter, the present invention is described in further detail in conjunction with the embodiments.
Embodiment 1
In the present embodiment, IC is prepared on 6061 alloy substrates and equips plasma etch chamber protective coating, i.e. atmosphere etc.
Plasma-spray technique is in Y+Y2O3Specific step is as follows for coating production:
(1) Y of 20g pure Y powder and 160g is weighed2O3Powder, drying for standby after mixing；Weigh the high-purity (purity of 100g
99.99wt%) Y2O3Powder, drying for standby.
(2) spraying substrate surface is pre-processed, is specifically comprised the following steps: using acetone and alcohol respectively to spraying
Substrate surface is pre-processed and blasting treatment, and blast media used is white fused alumina, and particle size range is 50~100 μm.With
The micron order Y+Y prepared in step (1)2O3Mixed-powder is prepared on 6061 alloy substrates using atmospheric plasma spraying technology
Y+Y2O3Composite coating is about 80 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 50mL/min, oxygen 300mL/min and nitrogen 50mL/min.Spray distance is 80mm, spray
Length of tube is 120mm.
(3) Y+Y prepared in step (2)2O3Composite coating surface prepares high-purity Y using air plasma spraying2O3
Coating is about 100 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 50mL/min, oxygen 300mL/min and nitrogen 50mL/min.Spray distance is 80mm, spray
Length of tube is 120mm.
(4) by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, and temperature is 180 DEG C, when
Between 4h.
As shown in Figure 1, air plasma spraying Y+Y on matrix 12O3Coating is as intermediate layer 2, on intermediate layer 2
The high-purity Y of air plasma spraying2O3Coating 3 forms Y+Y2O3/Y2O3Composite coating.The Y+Y of this implementation preparation2O3/Y2O3It is compound
The interface bond strength of coating, porosity 2.0%, coating and basis material is 45MPa.
Embodiment 2
In the present embodiment, IC is prepared on 6061 alloy substrates and equips plasma etch chamber protective coating, i.e. atmosphere etc.
Plasma-spray technique is in Y+Y2O3Specific step is as follows for coating production:
(1) Y of 30g pure Y powder and 120g is weighed2O3Powder, drying for standby after mixing.Weigh the high-purity (purity of 50g
99.99wt%) Y2O3Powder, drying for standby.
(2) spraying substrate surface is pre-processed, is specifically comprised the following steps: using acetone and alcohol respectively to spraying
Substrate surface is pre-processed and blasting treatment, and blast media used is white fused alumina, and particle size range is 50~100 μm.With
The micron order Y+Y prepared in step (1)2O3Mixed-powder is prepared on 6061 alloy substrates using atmospheric plasma spraying technology
Y+Y2O3Composite coating is about 100 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 30mL/min, oxygen 200mL/min and nitrogen 30mL/min.Spray distance is 60mm, spray
Length of tube is 80mm.
(3) Y+Y prepared in step (2)2O3Composite coating surface prepares high-purity Y using air plasma spraying2O3
Coating is about 100 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 30mL/min, oxygen 200mL/min and nitrogen 30mL/min.Spray distance is 60mm, spray
Length of tube is 80mm.
(4) by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, and temperature is 180 DEG C, when
Between 6h.
As shown in Figure 1, air plasma spraying Y+Y on matrix 12O3Coating is as intermediate layer 2, on intermediate layer 2
The high-purity Y of air plasma spraying2O3Coating 3 forms Y+Y2O3/Y2O3Composite coating.The Y+Y of this implementation preparation2O3/Y2O3It is compound
The interface bond strength of coating, porosity 2.0%, coating and basis material is 55MPa.
Embodiment 3
In the present embodiment, IC is prepared on 6061 alloy substrates and equips plasma etch chamber protective coating, i.e. atmosphere etc.
Plasma-spray technique is in Y+Y2O3Specific step is as follows for coating production:
(1) Y of 20g pure Y powder and 160g is weighed2O3Powder, drying for standby after mixing；Weigh the high-purity (purity of 60g
99.99wt%) Y2O3Powder, drying for standby.
(2) spraying substrate surface is pre-processed, is specifically comprised the following steps: using acetone and alcohol respectively to spraying
Substrate surface is pre-processed and blasting treatment, and blast media used is white fused alumina, and particle size range is 50~100 μm.With
The micron order Y+Y prepared in step (1)2O3Mixed-powder is prepared on 6061 alloy substrates using atmospheric plasma spraying technology
Y+Y2O3Composite coating is about 80 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 60mL/min, oxygen 400mL/min and nitrogen 60mL/min.Spray distance is 100mm,
Jet pipe length is 160mm.
(3) Y+Y prepared in step (2)2O3Composite coating surface prepares high-purity Y using air plasma spraying2O3
Coating is about 100 μm thick.
Wherein, the air plasma spraying equipment used, combustion gas used are propane, and combustion-supporting gas is oxygen, and powder feeding gas is
Nitrogen, gas flow are respectively propane 60mL/min, oxygen 400mL/min and nitrogen 60mL/min.Spray distance is 100mm,
Jet pipe length is 160mm.
(4) by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, and temperature is 180 DEG C, when
Between 4h.
As shown in Figure 1, air plasma spraying Y+Y on matrix 12O3Coating is as intermediate layer 2, on intermediate layer 2
The high-purity Y of air plasma spraying2O3Coating 3 forms Y+Y2O3/Y2O3Composite coating.The Y+Y of this implementation preparation2O3/Y2O3It is compound
The interface bond strength of coating, porosity 2.0%, coating and basis material is 45MPa.
Above embodiments the result shows that, IC prepared by the present invention equips plasma etch chamber Y+Y2O3/Y2O3It is compound anti-
Coating is protected, is well combined with matrix, 2% hereinafter, interface bond strength is 30~70MPa, coating layer thickness is coating porosity
10~400 μm.
Be above premised on inventive technique scheme under provide detailed embodiment and specific operation process, but the present invention
Protection scope be not limited to above embodiment.
Claims (8)
1. a kind of atmospheric plasma spraying technology prepares Y+Y2O3/Y2O3The method of composite coating, which is characterized in that including walking as follows
It is rapid:
Step (1) selects purity to be greater than the Y of 99.9wt%2O3Powder and Y powder, weigh respectively different quality proportion powder into
Row mixing；
Step (2) is sprayed using atmospheric plasma spraying technology in matrix surface, and Y+Y is prepared2O3Coating；
Step (3), by atmospheric plasma spraying technology in Y+Y2O3Y is deposited outside coating2O3Coating forms Y+Y2O3/Y2O3It is multiple
Close coating；
Step (4), by plasma spraying Y+Y2O3/Y2O3Composite coating is roasted under vacuum conditions, and temperature is 160~180
DEG C, 4~6h of time.
2. atmospheric plasma spraying technology as described in claim 1 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In, in step (1), Y2O3The granularity of powder is 10~60 μm.
3. atmospheric plasma spraying technology as described in claim 1 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In, in step (1), Y powder and Y2O3The mass ratio range of powder is 1:1~1:50.
4. atmospheric plasma spraying technology as described in claim 1 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
Before the spraying of, step (2), spraying substrate surface is pre-processed, specifically comprises the following steps: to distinguish using acetone and alcohol
Spraying substrate surface is pre-processed and blasting treatment, blast media used is white fused alumina, particle size range is 50~
100μm。
5. atmospheric plasma spraying technology as described in claim 1 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In, in step (2) and step (3), the air plasma spraying equipment used, combustion gas used is propane, and combustion-supporting gas is oxygen,
Powder feeding gas is nitrogen.
6. atmospheric plasma spraying technology as claimed in claim 5 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In, when combustion gas used is propane, combustion-supporting gas is oxygen, and when powder feeding gas is nitrogen, gas flow is respectively 20~80mL/min,
200~400mL/min and 20~80mL/min.
7. atmospheric plasma spraying technology as claimed in claim 5 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In air plasma spraying equipment used, spray distance is 40~120mm, and jet pipe length is 60~200mm.
8. atmospheric plasma spraying technology as claimed in claim 5 prepares Y+Y2O3/Y2O3The method of composite coating, feature exist
In Y+Y2O3/Y2O3The porosity of composite coating is 2% hereinafter, Y+Y2O3/Y2O3The interface cohesion of composite coating and basis material
Intensity is 30~70MPa, and coating layer thickness is 10~400 μm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114592162A (en) * | 2020-11-30 | 2022-06-07 | 中国科学院金属研究所 | Method for preparing yttrium coating by supersonic flame spraying technology |
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| CN109355612A (en) * | 2018-11-29 | 2019-02-19 | 沈阳富创精密设备有限公司 | A method of yttria coating is prepared with air plasma spraying |
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| DE69516566T2 (en) * | 1994-03-01 | 2001-02-08 | Citroen Sa(Automobiles) | Casting mold and process for its manufacture |
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