CN118086815A - Suspension plasma spraying slurry and preparation method and application thereof - Google Patents
Suspension plasma spraying slurry and preparation method and application thereof Download PDFInfo
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- CN118086815A CN118086815A CN202410143752.7A CN202410143752A CN118086815A CN 118086815 A CN118086815 A CN 118086815A CN 202410143752 A CN202410143752 A CN 202410143752A CN 118086815 A CN118086815 A CN 118086815A
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- 239000002002 slurry Substances 0.000 title claims abstract description 148
- 239000000725 suspension Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000007750 plasma spraying Methods 0.000 title claims abstract description 26
- 238000007613 slurry method Methods 0.000 title description 2
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 99
- 238000010438 heat treatment Methods 0.000 claims abstract description 63
- 238000000576 coating method Methods 0.000 claims abstract description 36
- 239000011248 coating agent Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims description 74
- 239000000843 powder Substances 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 239000002270 dispersing agent Substances 0.000 claims description 30
- 239000002202 Polyethylene glycol Substances 0.000 claims description 28
- 229920001223 polyethylene glycol Polymers 0.000 claims description 28
- 239000007921 spray Substances 0.000 claims description 27
- 239000008213 purified water Substances 0.000 claims description 26
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 26
- 229920002125 Sokalan® Polymers 0.000 claims description 21
- 239000004584 polyacrylic acid Substances 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 14
- 238000007780 powder milling Methods 0.000 claims description 12
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 7
- 239000002518 antifoaming agent Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 7
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 150000001555 benzenes Chemical class 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 abstract description 37
- 239000000758 substrate Substances 0.000 abstract description 7
- 238000001020 plasma etching Methods 0.000 abstract description 5
- 238000002203 pretreatment Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 3
- 238000005524 ceramic coating Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 230000003746 surface roughness Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 239000013530 defoamer Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000007751 thermal spraying Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses suspension plasma spraying slurry, a preparation method and application thereof, 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 slurry on 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 suspension plasma spraying slurry, a preparation method and application thereof, and relates to the field of plasma etching resistant ceramic coatings.
Background
The increase in silicon wafer size in sub-fabrication 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, 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 features, which have improved properties in terms of wear, etch resistance, bond strength, voltage resistance, and chemical stability 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 suspension plasma spraying slurry matched with a specific coating preparation method, a preparation method and application thereof, and the prepared coating has the characteristics of low roughness and etching resistance by adopting the slurry matched with the specific coating preparation method. The specific scheme is as follows:
A suspension plasma spraying slurry comprises yttrium oxide and purified water, wherein the purity of the yttrium oxide is more than or equal to 99.9%, the particle size is 1-9 mu m, and the mass of the yttrium oxide accounts for 20-30wt% of the sum of the mass of the yttrium oxide and the mass of the purified water; the slurry also comprises one or more than two of dispersing agent and defoaming agent.
Preferably, 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 mass fraction of the dispersing agent in the slurry is 0.01-2.50 wt%.
Preferably, the defoamer comprises one or two of BYK-016 and BYK-012, and the mass fraction in the slurry is 0.05wt% to 2.00wt%.
The preparation method of the suspension plasma spraying slurry 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.
Preferably, the components of step (1) are formulated as a suspension plasma spray slurry as described above.
Preferably, the mass ratio of the yttrium oxide powder, the water and the polyethylene glycol in the step (1) is 1 (1-2): 0.1-0.3.
Preferably, the ball milling is carried out in the step (1), the rotating speed of the ball mill is 500-700rpm, and the ball milling time is 4-8h.
Preferably, in the heat treatment in the step (2), the temperature is raised to 60-80 ℃ firstly, kept for 1-2h, then raised to 150-170 ℃ and kept for 3-5h, and naturally cooled to room temperature.
Preferably, the ultrasonic dispersion in the step (3) is carried out for 10-30 minutes.
Preferably, the secondary ball milling in the step (4) is carried out, the rotating speed of the ball mill is 200-300rpm, and the ball milling time is 2-3h.
The application of the suspension plasma spraying slurry in preparing the 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 performed by heating the substrate to 450-480 ℃ and then cooling to 270-300 ℃. 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 yttrium oxide powder used in the slurry is subjected to pretreatment, so that when the slurry is applied to the preparation of the yttrium oxide coating, a denser coating can be formed, and lower roughness and higher etching resistance can be obtained.
Drawings
FIG. 1 is an electron microscope image of a coating prepared from the slurry obtained in example 1 in a performance testing step;
FIG. 2 is an electron microscope image of a coating prepared from the slurry obtained in example 2 in a performance testing step;
FIG. 3 is an electron microscope image of a coating prepared from the slurry obtained in example 3 in a performance testing step;
FIG. 4 is an electron microscope image of a coating prepared from the slurry obtained in example 4 in a performance testing step;
FIG. 5 is an electron microscopic image of a coating prepared from the slurry obtained in comparative example 1 in a performance testing step;
FIG. 6 is an electron micrograph of a coating prepared from the slurry of comparative example 2 in a performance testing step;
FIG. 7 is an electron microscopic image of a coating prepared from the slurry obtained in comparative example 3 in a performance testing step;
FIG. 8 is an electron micrograph of a coating prepared from the slurry of comparative example 4 during a performance test procedure;
FIG. 9 is an electron micrograph of a coating prepared from the slurry of comparative example 5 at a performance test procedure;
FIG. 10 is an electron microscopic image of a coating prepared from the slurry of comparative example 6 in a performance testing step;
FIG. 11 is an electron micrograph of the resulting slurry of comparative example 7 at a performance test procedure.
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. Yttrium oxide powder, d50=2.74, used in the following examples.
Example 1 preparation of suspension plasma spray 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. 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 0.50wt%; the defoaming agent BYK-016 accounts for 0.5wt% of 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 1:1:0.1.
And (3) ball milling, wherein the rotational speed of the ball mill is 500rpm, and the ball milling time is 4 hours.
And (3) performing heat treatment, namely heating to 60 ℃, keeping the temperature for 1h, heating to 150 ℃, keeping the temperature for 3h, and naturally cooling to room temperature.
And (3) performing ultrasonic dispersion for 10 minutes.
And (3) performing secondary ball milling, wherein the rotating speed of the ball mill is 200rpm, and the ball milling time is 2 hours.
Example 2 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:1:0.1.
And (3) ball milling, wherein the rotational speed of the ball mill is 500rpm, and the ball milling time is 4 hours.
And (3) performing heat treatment, namely heating to 60-80 ℃, keeping the temperature for 1h, heating to 150 ℃, keeping the temperature for 3h, and naturally cooling to room temperature.
And (3) performing ultrasonic dispersion for 10 minutes.
And (3) performing secondary ball milling, wherein the rotating speed of the ball mill is 200rpm, and the ball milling time is 2 hours.
Example 3 preparation of suspension plasma spray 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. 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 isooctyl alcohol polyoxyethylene ether, and the mass fraction of the dispersant isooctyl alcohol polyoxyethylene ether in the slurry is 2.50wt%; the defoamer BYK-016 accounts for 2.00wt% of 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 1:1:0.1.
And (3) ball milling, wherein the rotational speed of the ball mill is 500rpm, and the ball milling time is 4 hours.
And (3) performing heat treatment, namely heating to 60 ℃, keeping the temperature for 1h, heating to 150 ℃, keeping the temperature for 3h, and naturally cooling to room temperature.
And (3) performing ultrasonic dispersion for 10 minutes.
And (3) performing secondary ball milling, wherein the rotating speed of the ball mill is 200rpm, and the ball milling time is 2 hours.
Example 4 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:2:0.3.
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.
Comparative example 1 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid in the slurry is 2.00wt%; the defoamer BYK-012 was 1.50wt% in the slurry.
The preparation process comprises the following steps:
(1) Mixing all the components in the formula, and performing ultrasonic dispersion;
(2) And (5) continuing ball milling of the obtained slurry to obtain suspension plasma spraying slurry.
The ultrasonic dispersion time is 30 minutes.
The ball milling is carried out at the rotating speed of 300rpm for 3 hours.
Comparative example 2 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 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.
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.
Comparative example 3 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 isooctyl alcohol polyoxyethylene ether 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 isooctyl alcohol polyoxyethylene ether is 1:2:2.
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.
Comparative example 4 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:2:2.
And (3) ball milling, wherein the rotational speed of the ball mill is 700rpm, and the ball milling time is 8 hours.
And (3) carrying out heat treatment, namely heating to 80 ℃, keeping for 2 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.
Comparative example 5 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:2:2.
And (3) ball milling, wherein the rotational speed of the ball mill is 700rpm, and the ball milling time is 8 hours.
And (3) carrying out heat treatment, namely heating to 80 ℃, keeping for 7 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.
Comparative example 6 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:2:2.
And (3) ball milling, wherein the rotational speed of the ball mill is 700rpm, and the ball milling time is 8 hours.
And (3) carrying out heat treatment, namely heating to 170 ℃, maintaining 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.
Comparative example 7 preparation of suspension plasma spray 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. 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 polyacrylic acid, and the mass fraction of the dispersant polyacrylic acid 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 1:2:2.
And (3) ball milling, wherein the rotational speed of the ball mill is 700rpm, and the ball milling time is 8 hours.
And (3) carrying out heat treatment, namely heating to 170 ℃, keeping for 7 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 slurries obtained in all the above examples and comparative examples were used to prepare low roughness etch resistant Y2O3 coatings, respectively:
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.
Firstly, spraying a coating with the thickness of 120um by using APS, wherein 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 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. )
And then spraying slurry by using SPS spraying suspension plasma, spraying a coating with the thickness of 60um, and preheating by using a plasma gun in an empty spraying mode before spraying, wherein 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 prepared from the slurries 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 suspension plasma spray slurry characterized by: comprises yttrium oxide and purified water, wherein the purity of the yttrium oxide is more than or equal to 99.9 percent, the particle size is 1-9 mu m, and the mass of the yttrium oxide accounts for 20-40 weight percent of the sum of the mass of the yttrium oxide and the mass of the purified water; the slurry also comprises one or more than two of dispersing agent and defoaming agent.
2. The suspension plasma spray slurry according to claim 1, wherein: 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 mass fraction of the dispersing agent in the slurry is 0.01-2.50 wt%.
3. The suspension plasma spray slurry according to claim 1, wherein: the defoaming agent comprises one or two of BYK-016 and BYK-012, and the mass fraction of the defoaming agent in the slurry is 0.05-2.00 wt%.
4. A method of preparing a suspension plasma spray slurry according to any one of claims 1 to 3, characterized in that: the method 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.
5. The method of preparing a suspension plasma spray slurry according to claim 4, wherein: in the step (1), the mass ratio of the yttrium oxide powder to the water to the polyethylene glycol is 1 (1-2) to 0.1-0.3.
6. The method of preparing a suspension plasma spray slurry according to claim 4, wherein: the ball milling is carried out in the step (1), the rotating speed of the ball mill is 500-700rpm, and the ball milling time is 4-8h.
7. The method of preparing a suspension plasma spray slurry according to claim 4, wherein: and (3) performing heat treatment, namely heating to 60-80 ℃, maintaining for 1-2h, heating to 150-170 ℃ again, maintaining for 3-5h, and naturally cooling to room temperature.
8. The method of preparing a suspension plasma spray slurry according to claim 4, wherein: and (3) performing ultrasonic dispersion for 10-30 minutes.
9. The method of preparing a suspension plasma spray slurry according to claim 4, wherein: and (3) performing secondary ball milling, wherein the rotating speed of the ball mill is 200-300rpm, and the ball milling time is 2-3h.
10. Use of a suspension plasma spray slurry according to any of claims 1-3 for the preparation of a low roughness etch resistant Y 2O3 coating.
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