CN118086820A - Low-roughness etching-resistant Y2O3Method for producing a coating - Google Patents
Low-roughness etching-resistant Y2O3Method for producing a coating Download PDFInfo
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- 238000000576 coating method Methods 0.000 title claims abstract description 70
- 239000011248 coating agent Substances 0.000 title claims abstract description 63
- 238000005530 etching Methods 0.000 title claims abstract description 16
- 238000005507 spraying Methods 0.000 claims abstract description 137
- 238000010438 heat treatment Methods 0.000 claims abstract description 55
- 239000002002 slurry Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 20
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000758 substrate Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000002203 pretreatment Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 238000007781 pre-processing Methods 0.000 claims abstract description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 42
- 239000000725 suspension Substances 0.000 claims description 29
- 238000002347 injection Methods 0.000 claims description 22
- 239000007924 injection Substances 0.000 claims description 22
- 229910052786 argon Inorganic materials 0.000 claims description 21
- 239000007921 spray Substances 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 238000007750 plasma spraying Methods 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000001020 plasma etching Methods 0.000 abstract description 5
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005524 ceramic coating Methods 0.000 abstract description 2
- 230000003746 surface roughness Effects 0.000 abstract description 2
- 229910052782 aluminium Inorganic materials 0.000 description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- 238000000635 electron micrograph Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
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- 239000002270 dispersing agent Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 239000002518 antifoaming agent Substances 0.000 description 2
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- 229910019142 PO4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
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- Coating By Spraying Or Casting (AREA)
Abstract
The invention discloses a preparation method of a low-roughness etching-resistant Y2O3 coating, and relates to the field of plasma etching-resistant ceramic coatings. The method comprises the following steps: s1, preprocessing a matrix; s2, performing heat treatment on the pretreated substrate; s3, spraying the pretreated spraying powder onto the surface of the substrate treated by the S2 by using APS; s4, SPS spraying the pretreated spraying slurry on the surface of the coating obtained in the S3; wherein, the spraying slurry after pretreatment in S4, the pretreatment method comprises: stirring and heating the spraying slurry to 173-190 ℃, keeping for 10-30min, continuously heating to 220-240 ℃ and keeping for 10-30min. According to the invention, the bonding strength of the yttrium oxide coating is further improved, the porosity and the surface roughness are reduced, and each performance of the obtained coating is superior by carrying out multi-step specific pretreatment or heat treatment steps on the surface of the substrate, the spraying slurry and the coating.
Description
Technical Field
The invention provides a preparation method of a low-roughness etching-resistant Y 2O3 coating, and relates to the field of plasma etching-resistant ceramic coatings.
Background
The increase in silicon wafer size in electronic manufacturing places new demands on all relevant processes, including plasma etching of the wafer. Yttria exhibits excellent resistance to plasma attack and is therefore commonly used as a protective covering for plasma etching chambers. While plasma thermal spray (APS) processes are often used to apply yttria to surfaces that require protection.
The plasma thermal spraying process adopts high-temperature plasma flame to spray carbide, metal ceramic, metal, ceramic and the like. The powder particles used in such thermal spray processes vary in size from 20 microns to 100 microns, thus producing a coarse structured (micron-scale features) coating. With the increasing demand for fine dimensions of very large scale integrated circuits, there is an increasing interest in depositing coatings with submicron and nanometer dimensions, and fine-structured coatings have improved properties in terms of wear, etch resistance, bond strength, voltage resistance, and chemical stability, as compared to conventional coarse-structured coatings. Deposition of fine particles using APS remains a significant challenge because the momentum of the powder particles is insufficient to penetrate the viscous plasma plume and particle agglomeration can result in poor flowability and injector nozzle blockage.
An emerging technology that alleviates the problem of nano-or submicron powder feeding is the Suspension Plasma Spraying (SPS) technology, which involves feeding fine powder in suspension in a suitable liquid medium (aqueous or organic solvent). Coatings produced by suspended atmospheric plasma spraying consist of finer fragments or particles than the counterparts using conventional plasma spraying, and the coatings produced generally exhibit a denser microstructure, showing great potential in producing coatings with high density, low porosity, and greater resistance to plasma etching. However, the SPS method has low powdering rate and takes a lot of time to prepare a coating with ideal thickness.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a Y 2O3 coating used with specific suspension plasma spraying slurry, and the prepared coating has the characteristics of low roughness and etching resistance. The specific scheme is as follows:
A preparation method of a low-roughness etching-resistant Y 2O3 coating comprises the following steps:
S1, preprocessing a matrix;
S2, performing heat treatment on the pretreated substrate;
s3, spraying the pretreated spraying powder onto the surface of the substrate treated by the S2 by using APS;
S4, SPS spraying the pretreated spraying slurry on the surface of the coating obtained in the S3;
Wherein, the spraying slurry after pretreatment in S4, the pretreatment method comprises: stirring and heating the spraying slurry to 173-190 ℃, keeping for 10-30min, continuously heating to 220-240 ℃ and keeping for 10-30min.
Preferably, the pre-treated spraying slurry in S4, the pre-treatment method includes: stirring and heating the spraying slurry to 173-180 ℃, keeping for 10-20min, continuously heating to 220-227 ℃ and keeping for 10-20min.
Preferably, the pre-treated spraying powder in S3, the pre-treatment method includes: mixing yttrium oxide and polyethylene glycol, heating to 80-100deg.C, maintaining for 10-20min, heating to 135-140deg.C, maintaining for 10-20min, and completely removing liquid to obtain powder; wherein the mass ratio of yttrium oxide to polyethylene glycol is (20-25): 1.
The preparation method further comprises the following steps: s5, performing heat treatment on the coating obtained in the step S4.
Preferably, the heat treatment of the coating obtained in the step S4 comprises the steps of treating for 1-2 hours at 300-380 ℃, and cooling to 200-270 ℃ for 3-5 hours.
Preferably, the spraying thickness of S3 is 150-250 μm by APS spraying.
Preferably, the SPS spraying is used for S4, and the spraying thickness is 40-80 mu m.
Preferably, the pretreatment of S1 includes treating the substrate surface to an average roughness of 5.0-7.0 μm.
Preferably, the heat treatment of S2 is carried out, after the substrate is heated to 350-380 ℃, the temperature is reduced to 170-200 ℃. The coating obtained by the heat treatment mode has obviously higher bonding strength than that obtained by directly preheating to 270-300 ℃ through inspection.
And S4, spraying slurry which comprises yttrium oxide, a solvent and a dispersing agent.
Preferably, the yttrium oxide adopts high-purity yttrium oxide powder with the particle size of 1-9um, and the adding percentage of the powder is 20-40 wt%.
Preferably, the solvent is pure water; the dispersing agent comprises one or more than two of ammonium polyacrylate, polyacrylic acid, polyethylene glycol, phosphate, isooctyl alcohol polyoxyethylene ether, BYK-199 modified benzene, DOLAPIX CE and BYK-154, and the addition amount is 0.01-2.00 wt%.
Preferably, the spraying slurry further comprises an antifoaming agent, wherein the antifoaming agent comprises BYK-012 or BYK-16, and the adding amount is 0.05wt% to 2.00wt%.
Preferably, the spraying parameters used for the Atmospheric Plasma Spraying (APS) are: the current is 600-800A, the powder feeding speed is 5-30g/min, the spraying distance is 100-300mm, the flow rate of argon is 35-65NLPM, and the flow rate of hydrogen is 5-15NLPM.
Preferably, the spraying parameters used for the Suspension Plasma Spraying (SPS) are: the voltage is 50-80V, the current is 500-800A, the injection plasma jet of the suspension is 40-70g/min, the incidence angle of the injection plasma jet of the suspension is 50-90 degrees, the main air flow is 35-75NLPM, the spraying distance is 40-100mm, and the moving speed of the spray gun is 500-1500mm/s.
Preferably, the heat treatment according to the invention uses plasma jet air-jet.
Preferably, the main gas is argon with the purity of 99.999 percent.
The invention has the beneficial effects that:
According to the invention, the bonding strength of the yttrium oxide coating is further improved, the porosity and the surface roughness are reduced, and each performance of the obtained coating is superior by carrying out multi-step specific pretreatment or heat treatment steps on the surface of the substrate, the spraying slurry and the coating.
Drawings
FIG. 1 is an electron micrograph of the coating obtained in example 1;
FIG. 2 is an electron micrograph of the coating obtained in example 2;
FIG. 3 is an electron micrograph of the coating obtained in example 3;
FIG. 4 is an electron micrograph of the coating obtained in example 4;
FIG. 5 is an electron micrograph of the coating obtained in example 5;
FIG. 6 is an electron micrograph of the coating obtained in example 6;
FIG. 7 is an electron micrograph of the coating obtained in comparative example 1;
FIG. 8 is an electron micrograph of the coating obtained in comparative example 2;
FIG. 9 is an electron micrograph of the coating obtained in comparative example 3.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art based on the embodiments of the present invention without making any inventive effort are within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
The experimental methods in the following examples are conventional methods unless otherwise specified, and the experimental materials used in the following examples are commercially available unless otherwise specified.
The spray slurries and powders used in the following examples were prepared by the following methods:
Preparation of suspension plasma spraying slurry:
The formula comprises the following components: comprises yttrium oxide and purified water, wherein the purity of the yttrium oxide is more than or equal to 99.9 percent, and D50=2.74. The mass of the yttrium oxide accounts for 20wt% of the sum of the mass of the yttrium oxide and the mass of the purified water; the slurry also comprises dispersant ammonium polyacrylate, wherein the mass fraction of the dispersant ammonium polyacrylate in the slurry is 2.00wt%; the defoamer BYK-012 was 1.50wt% in the slurry.
The preparation process comprises the following steps:
(1) Adding water and polyethylene glycol into yttrium oxide powder, and ball-milling in a ball mill;
(2) Carrying out heat treatment on the obtained slurry;
(3) Taking out the obtained slurry, adding other components except yttrium oxide powder in the formula, and performing ultrasonic dispersion;
(4) And (5) continuing to perform secondary ball milling on the obtained slurry to obtain suspension plasma spraying slurry.
In the step (1), the mass ratio of the yttrium oxide powder to the water to the polyethylene glycol is 1:2:0.2.
And (3) ball milling, wherein the rotational speed of the ball mill is 700rpm, and the ball milling time is 8 hours.
And (3) performing heat treatment, namely heating to 80 ℃, keeping for 2 hours, heating to 170 ℃, keeping for 5 hours, and naturally cooling to room temperature.
And (3) performing ultrasonic dispersion for 30 minutes.
And (3) performing secondary ball milling, wherein the rotating speed of the ball mill is 300rpm, and the ball milling time is 3 hours.
The APS sprayed powder is prepared by the following method:
Mixing yttrium oxide and polyethylene glycol, heating to 100deg.C, maintaining for 20min, heating to 140deg.C, maintaining for 20min, completely removing liquid to obtain powder; wherein the mass ratio of yttrium oxide to polyethylene glycol is 25:1.
Example 1
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8.8 NLPM parts of hydrogen and 160mm of spraying interval. (spraying slurry was stirred and heated to 80 ℃ C., maintained for 20 minutes, heated to 135 ℃ C., and maintained for 20 minutes, and then used.)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (spraying slurry was stirred and heated to 173 ℃ C., maintained for 30 minutes, and then heated to 220 ℃ C., maintained for 30 minutes, and then used.)
Example 2
The average roughness of the aluminum test piece is 6 um, and the aluminum test piece is subjected to air-jet heat treatment (after the substrate is heated to 380 ℃ and cooled to 200 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8.8 NLPM parts of hydrogen and 160mm of spraying interval. (the spraying slurry is stirred and heated to 100 ℃ for 20min, heated to 140 ℃ for 20min and then used)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (spraying slurry was stirred and heated to 190 ℃ C., maintained for 30 minutes, and then heated to 240 ℃ C., maintained for 30 minutes, and then used.)
Example 3
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8. 8NLPM parts of hydrogen and 160mm of spraying interval. (the spraying slurry is stirred and heated to 90 ℃ for 20min, heated to 138 ℃ and used after 20 min)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (the spray slurry was stirred and heated to 180 ℃ C., maintained for 30 minutes, and then heated to 225 ℃ C., maintained for 30 minutes, and then used.)
Example 4
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8. 8NLPM parts of hydrogen and 160mm of spraying interval. (the spraying slurry is stirred and heated to 90 ℃ for 20min, heated to 138 ℃ and used after 20 min)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (the spray slurry was stirred and heated to 180 ℃ C., maintained for 30 minutes, and then heated to 225 ℃ C., maintained for 30 minutes, and then used.)
And (3) carrying out heat treatment on the obtained coating: treating at 300 deg.c for 2 hr, cooling to 200 deg.c and treating for 5 hr.
Example 5
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8. 8NLPM parts of hydrogen and 160mm of spraying interval. (the spraying slurry is stirred and heated to 90 ℃ for 20min, heated to 138 ℃ and used after 20 min)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (the spray slurry was stirred and heated to 180 ℃ C., maintained for 30 minutes, and then heated to 225 ℃ C., maintained for 30 minutes, and then used.)
And (3) carrying out heat treatment on the obtained coating: treating at 380 deg.c for 2 hr, cooling to 270 deg.c and treating for 5 hr.
Example 6
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8. 8NLPM parts of hydrogen and 160mm of spraying interval. (the spraying slurry is stirred and heated to 90 ℃ for 20min, heated to 138 ℃ and used after 20 min)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (the spray slurry was stirred and heated to 180 ℃ C., maintained for 30 minutes, and then heated to 225 ℃ C., maintained for 30 minutes, and then used.)
And (3) carrying out heat treatment on the obtained coating: treating at 380 deg.c for 2 hr, cooling to 270 deg.c and treating for 5 hr.
Comparative example 1 (the difference from example 1 is that the substrate was preheated only)
The average roughness of the aluminum test piece is 6.58um, and a plasma gun is used for air-jet heat treatment (heating to 280 ℃ C.) before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8.8 NLPM parts of hydrogen and 160mm of spraying interval. (spraying slurry was stirred and heated to 80 ℃ C., maintained for 20 minutes, heated to 135 ℃ C., and maintained for 20 minutes, and then used.)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (spraying slurry was stirred and heated to 173 ℃ C., maintained for 30 minutes, and then heated to 220 ℃ C., maintained for 30 minutes, and then used.)
Comparative example 2 (the difference from example 1 is that the APS slurry was not pretreated)
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8.8 NLPM parts of hydrogen and 160mm of spraying interval.
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s. (spraying slurry was stirred and heated to 173 ℃ C., maintained for 30 minutes, and then heated to 220 ℃ C., maintained for 30 minutes, and then used.)
Comparative example 3 (differs from example 1 in that the SPS slurry was not pretreated)
The average roughness of the aluminum test piece is 6.58um, and the aluminum test piece is subjected to air-jet heat treatment (heating to 350 ℃ and cooling to 170 ℃) by using a plasma gun before spraying.
The APS is firstly used for spraying a coating with the thickness of 170um, and the spraying parameters are as follows: 3.5NLPM parts of powder feeding argon, 25g/min of powder feeding quantity, 600A of current, 60n/min of rotating disc rotating speed, 4.0NLPM parts of main argon, 8.8 NLPM parts of hydrogen and 160mm of spraying interval. (spraying slurry was stirred and heated to 80 ℃ C., maintained for 20 minutes, heated to 135 ℃ C., and maintained for 20 minutes, and then used.)
Then SPS is used for spraying a coating with the thickness of 60um, a plasma gun is used for air spraying and preheating before spraying, and the spraying parameters are as follows: the voltage is 65V, the current is 550A, the injection plasma jet of the suspension is 65g/min, the incidence angle of the injection plasma jet of the suspension is 60 degrees, the main air flow is 45NLPM, the spraying distance is 50mm, and the moving speed of the spray gun is 700mm/s.
The coatings obtained in all the above examples and comparative examples were subjected to performance tests, and the results were as follows:
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (10)
1. A preparation method of a low-roughness etching-resistant Y 2O3 coating is characterized by comprising the following steps: the method comprises the following steps:
S1, preprocessing a matrix;
S2, performing heat treatment on the pretreated substrate;
s3, spraying the pretreated spraying powder onto the surface of the substrate treated by the S2 by using APS;
S4, SPS spraying the pretreated spraying slurry on the surface of the coating obtained in the S3;
Wherein, the spraying slurry after pretreatment in S4, the pretreatment method comprises: stirring and heating the spraying slurry to 173-190 ℃, keeping for 10-30min, continuously heating to 220-240 ℃ and keeping for 10-30min.
2. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: s4, spraying the pretreated slurry, wherein the pretreatment method comprises the following steps: stirring and heating the spraying slurry to 173-180 ℃, keeping for 10-20min, continuously heating to 220-227 ℃ and keeping for 10-20min.
3. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: s3, the pretreated spraying powder comprises the following steps: mixing yttrium oxide and polyethylene glycol, heating to 80-100deg.C, maintaining for 10-20min, heating to 135-140deg.C, maintaining for 10-20min, and completely removing liquid to obtain powder; wherein the mass ratio of yttrium oxide to polyethylene glycol is (20-25): 1.
4. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: the preparation method further comprises the following steps: s5, performing heat treatment on the coating obtained in the step S4.
5. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 4, wherein: and (3) performing heat treatment on the coating obtained in the step (S4), wherein the heat treatment comprises the steps of treating for 1-2 hours at 300-380 ℃, and cooling to 200-270 ℃ for treating for 3-5 hours.
6. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: s3, spraying with APS, wherein the spraying thickness is 150-250 mu m.
7. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: s4, SPS spraying is adopted, and the spraying thickness is 40-80 mu m.
8. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: the pretreatment of S1 comprises the step of treating the surface of the substrate to have an average roughness of 5.0-7.0 mu m.
9. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: s2, performing heat treatment, namely heating the substrate to 350-380 ℃, and then cooling to 170-200 ℃.
10. The method for preparing the low-roughness etching-resistant Y 2O3 coating according to claim 1, wherein: the spraying parameters used for the Atmospheric Plasma Spraying (APS) are: the current is 600-800A, the powder feeding speed is 5-30g/min, the spraying distance is 100-300mm, the flow rate of argon is 35-65NLPM, and the flow rate of hydrogen is 5-15NLPM; the spraying parameters used for the Suspension Plasma Spraying (SPS) are: the voltage is 50-80V, the current is 500-800A, the injection plasma jet of the suspension is 40-70g/min, the incidence angle of the injection plasma jet of the suspension is 50-90 degrees, the main air flow is 35-75NLPM, the spraying distance is 40-100mm, and the moving speed of the spray gun is 500-1500mm/s.
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