CN103132007B - A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating - Google Patents
A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating Download PDFInfo
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- CN103132007B CN103132007B CN201110396373.1A CN201110396373A CN103132007B CN 103132007 B CN103132007 B CN 103132007B CN 201110396373 A CN201110396373 A CN 201110396373A CN 103132007 B CN103132007 B CN 103132007B
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Abstract
The present invention relates to Y
2o
3ceramic coating manufacturing technology field, is specifically related to a kind of low-voltage plasma spraying technology and prepares Y
2o
3the method of ceramic coating.Describedly prepare black Y
2o
3the method of ceramic coating, comprises the steps: step (1), selects the Y that purity is greater than 99.95%
2o
3powder; Step (2), carries out pre-treatment to substrate surface to be sprayed; Step (3), is first evacuated to 1-10Pa by the vacuum spraying room of described vacuum plasma spray coating equipment when described plasma spraying starts, then is filled with rare gas element Ar, now makes described vacuum spraying room pressure reach 1.3 × 10
3pa; Continue to be filled with H
2, make its pressure reach 10
3~ 10
4spraying operation is carried out after Pa; Prepare Y
2o
3coating.The present invention prepares Y under lower pressure
2o
3coating, uses Y prepared by the present invention
2o
3coating is black, the performance such as have excellent etch resistant, bear dirty, and cost is lower.
Description
Technical field
The present invention relates to Y
2o
3ceramic coating manufacturing technology field, is specifically related to a kind of low-voltage plasma spraying technology and prepares Y
2o
3the method of ceramic coating.
Background technology
At present, low-temperature plasma fine machining method is the gordian technique of material micro-nano processing, it is the basis of the technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optic, particularly in super large-scale integration manufacturing process, the operation of nearly 1/3rd is had to complete by means of plasma process, as plasma foil deposition, plasma etching and removing of photoresist by plasma etc.Wherein plasma etching is one of technical process of most critical, is the Micropicture realized in super large-scale integration production with high fidelity transfers to silicon chip irreplaceable technique from Lithographic template.
In etching process, owing to there is a large amount of living radicals with severe corrosive (as Cl*, Cl
2*, F*, CF* etc.), the internal surface in their article on plasma etching technics chambeies also can produce corrosive nature, causes pollution, affects etching effect, and etching technics chamber can be made to lose efficacy.The plasma etching equipment of the early stage nineties, when smaller power and single plasma-generating source, aluminum substrate layer adds Al
2o
3coating just can meet the etch damage of plasma body to etching technics chamber.Enter into 300mm equipment, along with plasma power is increasing, the damage of plasma body to etching technics chamber wall is also increasing, makes, in the process of etching, following problem easily occurs: (1) particle; (2) process cavity wall disbonding, cause plasma body directly and aluminum substrate have an effect; (3) Al
2o
3the life-span of component is subject to more high-power restriction.So need to find a kind of new approach to carry out modification to etching technics inner cavity surface, meet the needs of etching technics.
Research shows, Y
2o
3coating has good provide protection to etching technics chamber.With Al
2o
3compare, Y
2o
3chemical property highly stable, there is excellent resistant to plasma etching performance, and and the reaction product YF3 steam that generates of CF system gas force down, be difficult to disperse as particle.At present, with Y
2o
3powder, as spray material, utilizes air plasma spraying method, prepares the Y of single structure at etching technics inner cavity surface
2o
3corrosion-resistant finishes is a kind of method generally adopted.
Air plasma spraying uses N
2, Ar, H
2and He etc. is as ion-gas, produce plasma high temperature and high speed jet through ionization, input material fusing or melting are ejected into the method that working-surface forms coating.Plasma arc extreme temperatures wherein, enough melts and comprises Y
2o
3at interior all high-melting-point ceramic powder.In air plasma spraying technique, atmosphere surrounding can have the final performance of coating to be affected significantly.The selection principle of gas mainly considers practicality and economy.Concrete requirement is: (1) stable performance, not with spray material generation adverse reaction; (2) heat content is high, is suitable for refractory material, but should too high and ablation nozzle; (3) gas that chemical action does not occur with electrode or nozzle should be selected; (4) with low cost, supply is convenient.
Erosion resistance and be Y with the bonding strength of matrix
2o
3two critical index of coating.Coating corrosion resistance is not only relevant to the material selected, also relevant with the density of coating.Therefore the lower then corrosion resistance nature of the porosity of coating is better.And the factor such as flight velocity of particle is relevant when the bonding strength of coating and matrix and spraying.For improving the over-all properties of coating further.Need to find more suitably method and prepare Y
2o
3resistant to corrosion ceramic coating.
Summary of the invention
A kind of low-voltage plasma spraying technology is the object of the present invention is to provide to prepare Y
2o
3the method of ceramic coating, can prepare the Y of excellent performance at plasma etching industrial inner cavity surface
2o
3coating.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of low-voltage plasma spraying technology prepares black Y
2o
3the method of ceramic coating, comprises the steps:
Step (1), selects the Y that purity is greater than 99.95%
2o
3powder;
Step (2), carries out pre-treatment to substrate surface to be sprayed;
Step (3), selects Ar and H
2for ionized gas, plasma spraying is carried out at described substrate surface by vacuum plasma spray coating equipment, first the vacuum spraying room of described vacuum plasma spray coating equipment is evacuated to 1-10Pa when described plasma spraying starts, be filled with rare gas element Ar again, now make described vacuum spraying room pressure reach 1.3 × 10
3pa; Continue to be filled with H
2, make its pressure reach 10
3~ 10
4spraying operation is carried out after Pa; Prepare Y
2o
3coating.
In such scheme, the Y in described step (1)
2o
3the granularity of powder is 5 ~ 50 μm.
In such scheme, described step carries out pre-treatment to substrate surface to be sprayed in (2), specifically comprises the steps: to carry out sandblasting to substrate surface to be sprayed, and cleans with acetone.
In such scheme, the sand-blast material that described sandblasting adopts is white fused alumina, and sand size is 50 ~ 100 μm.
In such scheme, in described step (3), the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 10 ~ 30L/min.
In such scheme, in described step (3), the arc voltage of vacuum plasma spray coating equipment is 40 ~ 50V, and flame current is 600 ~ 900A, and powder feed rate is 15 ~ 100g/min, and spray distance is 200 ~ 500mm, and powder feeding angle is 50 ° ~ 90 °.
In such scheme, described step is filled with H in (3)
2preheating carried out to described base material to be sprayed before and described substrate surface carried out to sputtering cleaning.
In such scheme, in described step (3) after spraying operation, described vacuum spraying room continues to maintain low pressure atmosphere 10
3~ 10
4pa is until described base material is cooled to less than 100 DEG C.
Compared with prior art, the beneficial effect that the technical solution used in the present invention produces is as follows:
The present invention prepares Y under lower pressure
2o
3coating, uses Y prepared by the present invention
2o
3coating is black, the performance such as have excellent etch resistant, bear dirty, and cost is lower.
Accompanying drawing explanation
The low-voltage plasma spraying technology that Fig. 1 provides for the embodiment of the present invention prepares black Y
2o
3the schema of the method for coating.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is described in detail.
The present invention adopts low-voltage plasma spraying, prepares black Y under reducing atmosphere
2o
3ceramic coating.Low-voltage plasma spraying (low pressure plasma spraying) is called again vacuum plasma spray coating (vacuum plasma spraying), it plasma gun, workpiece and mechanical manipulator is placed in the sealed chamber of rough vacuum or certain selected controlled atmosphere, controlled the vacuum tightness of chamber by vacuum and filtering system, control the Technology of Plasma Spraying Process Using at chamber outward.
As shown in Figure 1, the embodiment of the present invention provides a kind of low-voltage plasma spraying technology to prepare Y
2o
3the method of ceramic coating, specifically comprises the steps:
(1) Y is selected
2o
3powder, size range is 5 ~ 100 μm, and powder should have single Emission in Cubic structure; The initial size of powder is 40 ~ 60nm, and after secondary granulation, particle diameter is for being 5 ~ 50 μm, and the macrobead powder after granulation is the spherical of vesicular structure, is the hollow micron bead be assembled into by nanometer small-particle, has splendid mobility;
(2) carried out sandblasting to needs by the etching technics cavity wall of the aluminium base sprayed, sand-blast material is white fused alumina, and size range is 50 ~ 100 μm, and cleans with acetone;
(3) Sluzer Metco ChamPro LPPS-TF vacuum plasma spray coating system is adopted to carry out plasma spraying, spray gun class 03CP; First the vacuum spraying room of vacuum plasma spray coating equipment is evacuated to 1-10Pa when plasma spraying starts, then is filled with rare gas element Ar, now make vacuum spraying room pressure reach 1.3 × 10
3pa; Preheating is carried out to base material to be sprayed and to substrate surface carry out sputtering cleaning after, continue to be filled with H
2, make its pressure reach 10
3~ 10
4after Pa, at Ar and H
2spray under atmosphere surrounding, the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 10 ~ 30L/min, and the arc voltage of vacuum plasma spray coating equipment is 40 ~ 50V, and flame current is 600 ~ 900A, and powder feed rate is 15 ~ 100g/min, and spray distance is 200 ~ 500mm, and powder feeding angle is 50 ° ~ 90 °; After spraying operation, vacuum spraying room continues to maintain low pressure atmosphere 10
3~ 10
4pa, until base material is cooled to less than 100 DEG C, finally completes black Y
2o
3the preparation of ceramic coating.
The present invention use Vacuum Plasma Spray Technology there is following characteristics:
(1) low-voltage plasma jet is long, high-temperature zone field width.Under rough vacuum, the 4-5cm of plasma arc Shu Changdu from normal pressure is elongated to 20-50cm, which increases dusty spray particle in arc intrafascicular flight time, thawing of can being heated fully.
(2) flight velocity of dusty spray particle is fast.Because the pressure of vacuum chamber is low, the speed of plasma air-flow can bring up to 3-4 Mach.And the low meeting of pressure reduces the resistance of particle flight greatly, particle is made to have very high kinetic energy.
(3) substrate preheating temperature is high.Under the protection of low pressure and controlled atmosphere, workpiece substrate can allow to be heated to higher temperature (generally can reach 700 DEG C, some superalloy can reach 900 DEG C).This can make matrix surface be in better active state, and the temperature difference of coating and matrix is decreased, and reduces the speed of cooling of coating.Thus reduce the bonding strength of thermal stresses, raising coating and matrix.Make simultaneously molten particles arrive matrix surface time can fully be out of shape, wetting and spreading, eliminating gas, thus reduce porosity.
(4) surface cleaning process can be carried out.Before spraying, plasma transferred arc striking can be adopted, connect negative pole by workpiece substrate, electronics is overflowed from matrix surface, remove surface smut, form surface that is clean, activation.Workpiece just can be combined with coating well without the need to surface coarsening process.
(5) by regulating spraying atmosphere, the composition and structure of coating can be changed.Obtain the coating of ideal performance.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. a low-voltage plasma spraying technology prepares black Y
2o
3the method of ceramic coating, is characterized in that, comprises the steps:
Step (1), selects the Y that purity is greater than 99.95%
2o
3powder;
Step (2), carries out pre-treatment to substrate surface to be sprayed;
Step (3), selects Ar and H
2for ionized gas, plasma spraying is carried out at described substrate surface by vacuum plasma spray coating equipment, first the vacuum spraying room of described vacuum plasma spray coating equipment is evacuated to 1-10Pa when described plasma spraying starts, be filled with rare gas element Ar again, now make described vacuum spraying room pressure reach 1.3 × 10
3pa; Continue to be filled with H
2, make its pressure reach 10
3~ 10
4spraying operation is carried out after Pa; Prepare black Y
2o
3coating;
Wherein, the Y in described step (1)
2o
3the granularity of powder is 5 ~ 50 μm;
Wherein, described step carries out pre-treatment to substrate surface to be sprayed in (2), specifically comprises the steps: to carry out sandblasting to substrate surface to be sprayed, and cleans with acetone;
Wherein, in described step (3), the flow of Ar gas is 40 ~ 90L/min, H
2the flow of gas is 10 ~ 30L/min;
Wherein, in described step (3), the arc voltage of vacuum plasma spray coating equipment is 40 ~ 50V, and flame current is 600 ~ 900A, and powder feed rate is 15 ~ 100g/min, and spray distance is 200 ~ 500mm, and powder feeding angle is 50 ° ~ 90 °.
2. low-voltage plasma spraying technology as claimed in claim 1 prepares black Y
2o
3the method of ceramic coating, is characterized in that, the sand-blast material that described sandblasting adopts is white fused alumina, and sand size is 50 ~ 100 μm.
3. low-voltage plasma spraying technology as claimed in claim 1 prepares black Y
2o
3the method of ceramic coating, is characterized in that, described step is filled with H in (3)
2preheating carried out to described base material to be sprayed before and described substrate surface carried out to sputtering cleaning.
4. low-voltage plasma spraying technology as claimed in claim 1 prepares black Y
2o
3the method of ceramic coating, is characterized in that, in described step (3) after spraying operation, described vacuum spraying room continues to maintain low pressure atmosphere 10
3~ 10
4pa is until described base material is cooled to less than 100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110396373.1A CN103132007B (en) | 2011-12-02 | 2011-12-02 | A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating |
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|---|---|---|---|
| CN201110396373.1A CN103132007B (en) | 2011-12-02 | 2011-12-02 | A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating |
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|---|---|
| CN103132007A CN103132007A (en) | 2013-06-05 |
| CN103132007B true CN103132007B (en) | 2015-09-09 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109839208B (en) * | 2017-11-27 | 2021-01-08 | 深圳航发复合材料有限公司 | Method for characterizing temperature of low-pressure plasma spraying substrate |
| CN111424273A (en) * | 2020-03-30 | 2020-07-17 | 沈阳富创精密设备有限公司 | Method for preparing high-cleanliness coating |
| CN115305433B (en) * | 2022-07-25 | 2024-01-09 | 广东羚光新材料股份有限公司 | Nickel screen and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940119A (en) * | 2005-09-30 | 2007-04-04 | 福吉米株式会社 | Thermal spray powder and forming method of thermal spray coating |
| JP2007227443A (en) * | 2006-02-21 | 2007-09-06 | Hitachi High-Technologies Corp | Plasma etching apparatus and method of forming inner wall in plasma processing chamber |
-
2011
- 2011-12-02 CN CN201110396373.1A patent/CN103132007B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1940119A (en) * | 2005-09-30 | 2007-04-04 | 福吉米株式会社 | Thermal spray powder and forming method of thermal spray coating |
| JP2007227443A (en) * | 2006-02-21 | 2007-09-06 | Hitachi High-Technologies Corp | Plasma etching apparatus and method of forming inner wall in plasma processing chamber |
Non-Patent Citations (1)
| Title |
|---|
| 等离子喷涂氧化钇涂层的组织结构;刘邦武等;《金属热处理》;20101031;第35卷(第10期);第16页左栏第1段至右栏第2段，第17页表1 * |
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Effective date of registration: 20201214 Address after: 510000 601, building a, 136 Kaiyuan Avenue, Huangpu District, Guangzhou City, Guangdong Province Patentee after: AoXin integrated circuit technology (Guangdong) Co.,Ltd. Address before: 3 Tucheng West Road, Chaoyang District, Beijing 100029 Patentee before: Institute of Microelectronics, Chinese Academy of Sciences |
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Effective date of registration: 20220506 Address after: 510000 room 710, Jianshe building, No. 348, Kaifa Avenue, Huangpu District, Guangzhou, Guangdong Patentee after: Ruili flat core Microelectronics (Guangzhou) Co.,Ltd. Address before: 510000 601, building a, 136 Kaiyuan Avenue, Huangpu District, Guangzhou City, Guangdong Province Patentee before: AoXin integrated circuit technology (Guangdong) Co.,Ltd. |
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