CN110218965A - A kind of preparation method of advanced ceramics layer - Google Patents
A kind of preparation method of advanced ceramics layer Download PDFInfo
- Publication number
- CN110218965A CN110218965A CN201910453200.5A CN201910453200A CN110218965A CN 110218965 A CN110218965 A CN 110218965A CN 201910453200 A CN201910453200 A CN 201910453200A CN 110218965 A CN110218965 A CN 110218965A
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- CN
- China
- Prior art keywords
- particle
- ceramic layer
- preparation
- spraying
- advanced ceramics
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
Abstract
The present invention relates to a kind of preparation method of advanced ceramics layer, the ceramic layer of technology preparation is mainly used in corrosion resistant environment.This method mainly comprises the steps that (1) carries out pre-treatment to the component that needs spray；(2) fine particle even nano-scale particle is dissolved in liquid, forms suspension；(3) atmospheric plasma spraying technology is utilized, in conjunction with suspension, prepares one layer of ceramic layer in piece surface.The advanced ceramics layer prepared using this method has apparent technical advantage.This method remains excellent performance of fine particle itself to the maximum extent, and coating compactness obtained is fabulous, and porosity is low, and corrosion resistance is very good, and hardness is high.There is function outstanding in terms of preventing components corrosion resistance.
Description
Technical field
The invention belongs to thermal spraying modes to prepare ceramic layer field, especially lead the ceramic layer applied to semiconductor equipment
Domain.
Background technique
Along with the fast development of semiconductor equipment, the etching gas in etch chamber requires to get over to the extent of corrosion of components
Come higher, this also requires the corrosion resistance of semiconductor components more and more stronger.And in semiconductor equipment etch chamber, it is most of
Part is aluminum hardware, in order to improve the corrosion resistance of aluminum components, most starts to improve it by the way of anodic oxidation
Corrosion resistance.Later, with the development of technology, it is found that the corrosion resistance of yttrium is more preferable than aluminium, thermal spraying oxidation then occur
The mode of yttrium ceramic layer improves its corrosion resistance.But thermal spraying yttrium layer, can only sprayed particle diameter at 10 μm
Above yttrium oxide powder due to too small in particle, can not converge in flame flow center for fine particle in spraying process,
Coating cannot be formed, not only limits the application of fine powder in this way, the coating obtained is also made to have lacked the excellent of fine powder
Performance.
On the other hand, ceramic layer is finer and close, and etching gas is more difficult to invade coat inside, and the corrosion resistance of coating is got over
By force.And fine particle is since its particle diameter is small, so the coating formed is finer and close.In order to obtain finer and close ceramic layer, energy
Enough realize that the spraying of fine particle is necessary.Therefore, the purpose of the present invention is in order to solve spraying fine particle
Problem obtains finer and close advanced ceramics layer, to solve the problems, such as that aluminum components corrosion resistance is inadequate.
Summary of the invention
It is an object of the invention to prepare a kind of advanced ceramics layer, mainly fine particle even nano-scale particle is dissolved in
In liquid, and anti-solid agent is added, prevents particle agglomeration, form suspension.Recycle atmospheric plasma spraying technology and suspension
Slurry device connection is sent, sending in slurry device has stirring rod, and constantly stirred suspension, prevents particle from sinking to solution bottom, by fine particle
Even nano particle sprays to piece surface, forms one layer of advanced ceramic layer.The ceramic layer can be the pottery based on yttrium
Enamel coating or alumina ceramic layer.The method for preparing the advanced ceramics layer advantageously, on the one hand breaches 10 μ of spraying
M once even nano particle technological difficulties；On the other hand, ceramic layer compactness obtained is higher, possessed corrosion-resistant
Property is stronger.Therefore, there is high-densit, low latitude gap, high rigidity excellent performance using the advanced ceramics layer of the technology of the present invention preparation,
It applies in aluminum component surface, the service life of aluminum components can be significantly increased, advanced half can be met
Conductor device will go the corrosion-resistant of components.
To achieve the goals above, the technical solution adopted by the present invention is that:
(1) before spraying, the place for not needing spraying is subjected to masking protection, the place for needing to spray is subjected to sandblasting or is swashed
Light texture processing, to increase Part Surface Roughness；
(2) the even nano-scale particle of the fine particle by particle diameter less than 10 μm is dissolved in liquid, and is added anti-condensation
Gu agent prevents particle agglomeration；
(3) again with atmospheric plasma spraying technology by the particle spray coating in suspension to piece surface, one layer of densification is formed
Advanced ceramics layer；The ceramic layer can be alumina ceramic layer or the ceramic layer based on yttrium.
(4) after spraying, ceramic layer thickness is measured, masking protection is removed.
(5) the fine particle even Optimality of nano particle are remained using the advanced ceramics layer of the method for the present invention preparation
Can, the coating densification of preparation is high, and rotproofness is strong, good characteristics with high hardness.
The invention has the advantages that
1. fine particle even nano-scale particle is dissolved in liquid by the present invention, realizes and spray tiny or even nano particle
Technology.
2. the advanced ceramics layer that the present invention sprays, compactness is high, and porosity is low, and porosity is lower than 1%, can effectively prevent
Only etching gas invades coat inside, so that the corrosion resistance of coating is higher.
3. ceramic layer of the invention is applied in aluminum component surface, it is insufficient to can solve existing components corrosion resistance
Problem substantially increases the service life of aluminum components.
Detailed description of the invention
Fig. 1 is usual spray yttria coating, the SEM photograph in the section of 400 times of amplification；
Fig. 2 is advanced oxidation yttrium coating prepared by the present invention, the sectional view SEM photograph of 400 times of amplification.
Fig. 3 is usual spray yttria coating, the SEM photograph of the surface topography of 1000 times of amplification；
Fig. 4 is advanced oxidation yttrium coating prepared by the present invention, the surface topography SEM photograph of 1000 times of amplification.
Specific embodiment
The present invention program is described in detail in conjunction with attached drawing 1-4 and example.
A kind of preparation method of advanced ceramics layer, includes the following steps:
(1) before spraying, the place for not needing spraying is subjected to masking protection, will need the place that sprays increase it is coarse
The pretreatment work of degree；
(2) fine particle even nano-scale particle is dissolved in liquid, and adds Anti-solidification agent, prevent particle agglomeration；
(3) again with atmospheric plasma spraying technology by the particle spray coating in suspension to piece surface, one layer of densification is formed
Advanced ceramics layer；
(4) after spraying, ceramic layer thickness is measured, masking protection is removed.
The method that the step (1) blocks protection can be specific using masking glue using soft occlusion method；Or hard screening
Gear method specifically uses shielding module；The method for increasing spraying area roughness can be using sandblasting, the method for laser texture.
In the step (2), fine particle refer to 10 μm hereinafter, the granular size that conventional thermal spray technology cannot achieve,
And nanoscale particle；The liquid being dissolved in can be water, methanol or ethyl alcohol；According to different grain types, can add not
Same Anti-solidification agent.
Atmospheric plasma spraying technology in the step (3) send suspension to slurry device connection, realizes that spraying is tiny even
The method of nano-scale particle, in spraying process, stirring rod constantly agitating solution will be had by sending in slurry device, prevent fine particle heavy
Enter solution bottom；The ceramic layer can be alumina ceramic layer or using yttrium as the ceramic layer of base, such as yttria coating.
In the step (4), after spraying, ceramic layer thickness is measured, if its thickness can reach requirement, can be removed
Masking protection.
The ceramic layer has tiny or even nano particle excellent performance, and compactness is high, leads to the corrosion resistant of ceramic layer
Corrosion, hardness are very high.Applied on the components required with corrosion resistance in semiconductor equipment, components can be improved
Service life.
Embodiment one
Firstly, the place that part does not need spraying is covered with masking tape, then will need the part that sprays into
Row sandblasting, so that the surface roughness of Spray Application is up to Ra6.4 or so.
Secondly, by particle diameter be 2.5 μm or so, powder concn be >=99.9% yttrium oxide powder it is soluble in water,
The concentration of middle particle is 35% or so, in a small amount of anti-solid agent of addition, prevents particle agglomeration.
Again, slurry device is sent using atmospheric plasma spraying technology connection suspension, sprays advanced oxidation yttrium coating, is spraying
During, sending in slurry device has stirring rod, and constantly agitating solution, prevents particle to be sunken to solution bottom.Spray-on coating with a thickness of
200-230 μm or so of ceramic layer, coating surface mean roughness are Ra4 or so.
Finally, the yttrium oxide layer thickness of measurement part each section, meets drawing requirement, remove masking protection.
Fig. 1 is the sectional view for spraying common yttrium oxide, and Fig. 2 is the sectional view for spraying advanced oxidation yttrium, black approach in figure
It is gap in circular part, compares two figures as can be seen that having apparent gap distribution in Fig. 1, gap is big and more, passes through
Measurement, porosity is 4% or so.And gap in Fig. 2 is small and distribution is few, by measurement, porosity < 1%.Due to porosity
Low, coating compactness is high, and etching gas is difficult to invade coat inside from the gap of coating, therefore, advanced oxidation yttrium coating by
In its extremely low porosity, and there is very high corrosion resistance, and then improves the service life of components.
Embodiment two
Firstly, being covered the place that part does not need spraying with masking glue and hard masking, then will need to spray
Part carry out laser texture processing so that the surface roughness of Spray Application is up to Ra4.8 or so.
Secondly, being 1 μm or so by particle diameter, powder concn is that >=99.95% yttrium oxide powder is dissolved in ethyl alcohol,
The concentration of middle particle is 40% or so, in a small amount of anti-solid agent of addition, prevents particle agglomeration.
Again, slurry device is sent using atmospheric plasma spraying technology connection suspension, sprays advanced oxidation yttrium coating, is spraying
During, sending in slurry device has stirring rod, and constantly agitating solution, prevents particle to be sunken to solution bottom.Spray-on coating with a thickness of
170-200 μm or so of ceramic layer, coating surface mean roughness are Ra3 or so.
Finally, the yttrium oxide layer thickness of measurement part each section, meets drawing requirement, remove masking protection.
Fig. 3 is common yttria coating surface pattern schematic diagram, and Fig. 4 is the surface topography signal of advanced oxidation yttrium coating
Figure, compares two figures as can be seen that advanced oxidation yttrium coating is since sprayed particle diameter is small, without apparent gap, and it is common
The gap of yttria coating is then obvious.It can be seen that the compactness of advanced oxidation yttrium coating is higher, corrosion resistance is more preferable！
The foregoing is only a preferred embodiment of the present invention, is not limited to well-behaved invention, for this field skill
For art personnel, the present invention may have various change and combination.Present invention is mainly used in every field, corrosion resistance is wanted
The components asked, such as some aluminum components in semiconductor field, semiconductor equipment etch chamber.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of advanced ceramics layer, which comprises the steps of:
(1) before spraying, the place for not needing spraying is subjected to masking protection, the place sprayed will be needed to carry out increasing roughness
Pretreatment work；
(2) fine particle even nano-scale particle is dissolved in liquid, and adds Anti-solidification agent, prevent particle agglomeration；
(3) again with atmospheric plasma spraying technology by the particle spray coating in suspension to piece surface, one layer of fine and close elder generation is formed
Into ceramic layer；
(4) after spraying, ceramic layer thickness is measured, masking protection is removed.
2. a kind of preparation method of advanced ceramics layer according to claim 1, which is characterized in that the step (1) is blocked
The method of protection can use soft occlusion method, specific using masking glue；Or hard occlusion method, it is specific using masking mould
Block；The method for increasing spraying area roughness can be using sandblasting, the method for laser texture.
3. a kind of preparation method of advanced ceramics layer according to claim 1, which is characterized in that in the step (2), carefully
Little particle refer to 10 μm hereinafter, the granular size and nanoscale particle that conventional thermal spray technology cannot achieve；The liquid being dissolved in
Body can be water, methanol or ethyl alcohol；According to different grain types, different Anti-solidification agent can be added.
4. a kind of preparation method of advanced ceramics layer according to claim 1, which is characterized in that in the step (3)
Atmospheric plasma spraying technology send suspension to slurry device connection, realizes and sprays tiny or even nano-scale particle method, is spraying
In the process, stirring rod constantly agitating solution will be had by sending in slurry device, prevent fine particle from sinking to solution bottom；The ceramic layer can be with
It is alumina ceramic layer or using yttrium as the ceramic layer of base, such as yttria coating.
5. a kind of preparation method of advanced ceramics layer according to claim 1, which is characterized in that in the step (4), spray
Tu Hou will measure ceramic layer thickness, if its thickness can reach requirement, can remove masking protection.
6. a kind of preparation method of advanced ceramics layer according to claim 1, which is characterized in that the ceramic layer has tiny
The even excellent performance of nano particle, compactness is high, causes the corrosion resistance of ceramic layer, hardness very high.Applied to partly leading
On the components required with corrosion resistance in body equipment, the service life of components can be improved.
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| CN201910453200.5A CN110218965A (en) | 2019-05-28 | 2019-05-28 | A kind of preparation method of advanced ceramics layer |
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Cited By (3)
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| CN112501539A (en) * | 2020-10-27 | 2021-03-16 | 沈阳富创精密设备股份有限公司 | Preparation method of corrosion-resistant coating |
| CN114507837A (en) * | 2022-01-17 | 2022-05-17 | 北京富创精密半导体有限公司 | Preparation method of high-compactness voltage-resistant plasma spraying yttrium oxide coating |
| CN115852293A (en) * | 2022-10-13 | 2023-03-28 | 扬州大学 | Preparation method of metal ceramic self-lubricating composite wear-resistant coating |
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Address after: No.18a-1, Feiyun Road, Hunnan District, Shenyang City, Liaoning Province Applicant after: Shenyang fuchuang precision equipment Co.,Ltd. Address before: No.18a-1, Feiyun Road, Dongling District, Shenyang, Liaoning Province, 110000 Applicant before: Shenyang Fortune Precision Equipment Co.,Ltd. |
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Application publication date: 20190910 |