CN106591820A - Preparation method of high-purity yttrium oxide coating for IC equipment critical parts - Google Patents
Preparation method of high-purity yttrium oxide coating for IC equipment critical parts Download PDFInfo
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- CN106591820A CN106591820A CN201510676326.0A CN201510676326A CN106591820A CN 106591820 A CN106591820 A CN 106591820A CN 201510676326 A CN201510676326 A CN 201510676326A CN 106591820 A CN106591820 A CN 106591820A
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- yttrium oxide
- powder
- purity yttrium
- coating
- oxide coating
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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
- C23C24/00—Coating starting from inorganic powder
- C23C24/02—Coating starting from inorganic powder by application of pressure only
- C23C24/04—Impact or kinetic deposition of particles
Abstract
The present invention relates to the field of cold spraying preparation of ceramic coatings, more particularly to a preparation method of a high-purity yttrium oxide coating for IC equipment critical parts. The method mainly comprises: (1) protecting the coating-free area on a part; (2) carrying out surface pretreatment on the sprayed area of the part; (3) using high-purity yttrium oxide powder, wherein the purity is more than or equal to 99.9 wt%, and the average particle size is 2-50 [mu]m; and (4) carrying out rapid spray coating by using a low-pressure cold spray coating system to obtain the high-purity yttrium oxide coating. Compared to the traditional hot spray coating, the cold spray coating of the present invention can effectively reduce and decrease the heat input to the substrate, such that the cold spray coating is suitable for the spraying of the coating on the surface of the aluminum, the aluminum alloy and other IC equipment critical parts. According to the present invention, the spray coating temperature of the used cold spray coating method is only 100-1000 DEG C, and is much lower than the temperature required by the plasma spraying (the melting temperature of the yttrium oxide is more than 2410 DEG C); and the yttrium oxide coating prepared through the cold spraying has characteristics of stable quality and uniform thickness.
Description
Technical field
The present invention relates to cold spraying prepares field of ceramic coatings, a kind of particularly IC equipment key components and partss are with high-purity
The preparation method of yttria coating.
Background technology
For IC equipment enterprise, the supply of parts determines the process of its research and development and industrialization.Without full
The components supplying of sufficient IC equipment enterprise technological requirement, the development of IC equipment industries is inconceivable.Break through
The Integrated-manufacturing Techniques of the high-end parts of representational IC equipment and key components and partss, can solve IC equipment
The localization of 70% parts.China IC equipment special precision parts public service platforms are set up, to China
The research and development of IC equipment and industrialization process have vital effect.
As 22nm technologies have progressively been used for chip volume production, world's integrated circuit live width research and development come into 14nm
So that the equipment and technique of 7nm are tackled key problems, now the integrated circuit such as etching, ion implanting, PVD, CVD is closed
Key equipment is faced with many new challenges.By taking etching machine reaction chamber as an example, on the one hand to the cleaning in etching cavity
Degree requires more and more higher；On the other hand, etching is banged with severe corrosive gas and the higher and higher plasma of energy
The collective effect hit, produces the most strong corrosive environment of the industrial quarters being currently known, in metal parts therein
Serious corrosion can be produced, metal ion or particle pollution cavity is discharged, causes chip circuit short circuit.
Protected using anode oxidation alumina coating more than traditional IC equipment parts.Because parts are in
Strong corrosive atmosphere and ion bom bardment interacting state, once produce digestion of metallic ion because of corrosion cause
Systemic contamination, loss will be unable to estimate.Research shows, yttria coating than aluminium oxide have more preferable anti-grade from
Daughter erosion property, and with longer service life, therefore it is defensive new to become IC equipment parts
Coating.In addition to etching machine, yttria coating also has huge using value in other IC equipment parts.
Yttria coating belongs to ceramic coating, plasma spraying is usually used and is prepared.Plasma spray is coated with
Gas ions are thermal source, and yittrium oxide is heated to melt (2410 DEG C) or semi-molten state and then is sprayed on matrix.
This high temperature has inevitably resulted in oxidation, phase transformation or other chemical reactions of sprayed particle, while high temperature pair
Aluminum matrix alloy material is likely to cause to damage.
The content of the invention
It is an object of the invention to provide a kind of prepare IC equipment key components and partss with high-purity using cold spray technique
The preparation method of yttria coating, solves the plasma spray technologies such as existing plasma and prepares what is existed during yttria coating
Coating quality is poor, oxidizable, and causes the excessive problem of aluminium alloy spraying matrix heat input, opens up one kind
The new effective way for preparing high-purity yttrium oxide coating, to expanding practical ranges early.
Technical solution of the present invention is as follows：
A kind of IC equips the key components and partss preparation method of high-purity yttrium oxide coating, comprises the following steps：
1) thoroughly cleaning is carried out to spraying matrix before spraying, and region of the matrix beyond to be sprayed is carried out effectively
Protection；
2) high-purity yttrium oxide powder body to be sprayed is added in the powder feeder of cold spray apparatus；
3) cold spray apparatus are adopted, is sprayed at matrix position to be sprayed, obtain high-purity yttrium oxide coating.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, and cold spray process parameter is such as
Under：100～1000 DEG C of the gas temperature of powder feeding, the 0.5～5MPa of gas pressure of powder feeding, the mobile speed of powder body
Degree 50～1500m/min, 10～40mm of spray distance, 10～150g/min of powder feeding rate.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, preferred cold spray process
Parameter is as follows：200～600 DEG C of the gas temperature of powder feeding, the 1～4MPa of gas pressure of powder feeding, the movement of powder body
500～1000m/min of speed, 20～30mm of spray distance, 50～100g/min of powder feeding rate.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, high-purity yttrium oxide coating
Thickness is 50～500 μm.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, preferred high-purity yttrium oxide
The thickness of coating is 100～300 μm.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, high-purity yttrium oxide powder
Chemical composition is by weight percentage：Y2O3≤ 99.9%, particle size range is 2～50 μm.
Described IC equips the preparation method of key components and partss high-purity yttrium oxide coating, high-purity yttrium oxide powder
Granularity requirements are：Granularity<35 μm of powder, its weight/mass percentage composition is more than 95%；35 μm～45 μm of granularity
Powder, its weight/mass percentage composition be less than 3%；Balance of granularity>45 μm of powder.
The present invention design philosophy be：
The present invention is a kind of technology for being totally different from thermal spraying using cold spraying (also known as cold air power spraying and coating),
It is that, using the pre- hot compressed gas of heating facility, compressed gas produce ultrahigh speed gas by scaling type Laval nozzles
Stream, drives metallic to make it under complete solid-state with high velocity collision substrate, particle occurs violent
Plastic deformation, and it is deposited as a kind of novel spraying technology of coating in matrix surface.Because powder particle is whole
Temperature is less than its fusing point, therefore referred to as cold spraying in deposition process.In real work, conventional working gas has
N2, He and air, or their mixed gas.The temperature of working gas preheating is usually no more than 1000 DEG C.
The characteristics of cold spraying has solid deposited under low temperature, can significantly reduce and even completely eliminate oxygen in traditional thermal spraying
Change, phase transformation, segregation, residual tension and crystal grain such as are grown up at the adverse effect.High pure zirconia is prepared using cold spraying
The method of yttrium ceramic coating has not been reported.
Advantages of the present invention and beneficial effect are：
1st, the characteristics of present invention has solid deposited under low temperature using cold spraying, can significantly reduce or even disappear completely
Except oxidation, phase transformation, segregation, residual tension and crystal grain such as are grown up at the adverse effect in traditional thermal spraying, learned
Art circle and industrial quarters are more and more paid close attention to.Compared to traditional thermal spraying, cold spraying can efficiently reduce and
Reduce the heat input to matrix.Therefore, it is suitable for being sprayed on the IC equipment key components and partss such as aluminum and aluminium alloy surface
Coating layer.
2nd, the present invention adopt cold spray-coating method, its spraying temperature is only 100～1000 DEG C, well below wait from
Temperature (i.e. more than 2410 DEG C of the melting temperature of yittrium oxide) needed for son spraying；Yittrium oxide prepared by cold spraying is applied
Layer steady quality, thickness are uniform, can prepare the yttria coating that thickness is 200 μm, and coating is fine and close,
The corrosivity of the anti-high energy plasma of IC equipment parts and severe corrosive gas are drastically increased, while improve
The service life and preparation efficiency of part.
Description of the drawings
Fig. 1 is the XRD analysis collection of illustrative plates of the embodiment of the present invention 1.
Fig. 2 (a)-(b) is the SEM photograph of 6061 aluminium alloy matrix surfaces in the embodiment of the present invention 1.Its
In, Fig. 2 (a) is 500 times of amplification；Fig. 2 (b) is 10000 times of amplification.
Fig. 3 (a)-(b) is Y in the embodiment of the present invention 12O3The section metallograph of coating/6061 matrix.
Wherein, Fig. 3 (a) is section metallograph I；Fig. 3 (b) is section metallograph II.
Fig. 4 (a)-(b) is the matrix surface SEM photograph and section metallograph of the embodiment of the present invention 2.
Wherein, Fig. 4 (a) is the SEM photograph of 6061 aluminium alloy matrix surfaces；Fig. 4 (b) is Y2O3Coating/6061
The section metallograph of matrix.
Specific embodiment
In a specific embodiment, cold spraying of the present invention prepares IC equipment key components and partss high-purity yttrium oxide coatings
Method, mainly include the following steps that：
1) thoroughly cleaning is carried out to spraying matrix before spraying, and region of the matrix beyond to be sprayed is carried out effectively
Protection；
2) high-purity yttrium oxide powder body to be sprayed is added in the powder feeder of cold spray apparatus；
3) cold spray apparatus are adopted, is sprayed at matrix position to be sprayed, the thickness of high-purity yttrium oxide coating is
50～500 μm.
Wherein, cold spray apparatus refer to the Chinese invention patent (patent No.：01128130.8, Authorization Notice No.：
CN1161188C a kind of cold air driven spray painter) mentioned.High-purity coating is prepared using cold spray technique
During, gas heating-up temperature is 100～1000 DEG C (preferably 200～600 DEG C) during spraying, and spray gas can
Using air, nitrogen or argon.High-purity yttrium oxide powder is the commercial yttrium oxide powder sold on the market, its change
Study and point be by weight percentage：Y2O3≤ 99.9% (particle size range is 2～50 μm), its granularity requirements is：
Granularity<35 μm of powder, its weight/mass percentage composition is more than 95%；The powder that 35 μm～45 μm of granularity, its matter
Amount percentage composition is less than 3%；Balance of granularity>45 μm of powder.Typical spraying high-purity yttrium oxide coating
Cold spray process parameter is shown in Table 1.
Table 1
To make technical scheme and advantage clearer, retouched in detail below in conjunction with specific embodiment
State.
Embodiment 1
Cold spray process parameter：600 DEG C of the gas temperature of powder feeding, the gas pressure 2MPa of powder feeding, powder body movement
Speed 1000m/min, spray distance 20mm, powder feeding rate 100g/min, 4 passages；Matrix：6061 aluminum
Alloy；About 120 μm of the coating layer thickness obtained after spraying.
(1) XRD analysis：
As shown in figure 1, the Y after spraying2O3There is no composition transfer compared with original powder body in coating.
(2) surface roughness measurement：
Roughness average Ra=9.090 μm of cold spraying coating on 6061 alloy matrix aluminums；
(3) surface topography SEM photograph：
As shown in Fig. 2 (a)-(b), the surface topography of 6061 alloy matrix aluminums；
(4) section metallograph：
As shown in Fig. 3 (a)-(b), from Y2O3The metallograph in coating/6061 matrix section can be seen that painting
Layer is well combined with matrix, coating densification tight.
Embodiment 2
Difference from Example 1 is,
Cold spray process parameter：500 DEG C of the gas temperature of powder feeding, the gas pressure 4MPa of powder feeding, powder body movement
Speed 800m/min, spray distance 20mm, powder feeding rate 80g/min, 6 passages；Matrix：6061 aluminum are closed
Gold；About 100 μm of the coating layer thickness obtained after spraying.
As shown in Fig. 4 (a), the surface topography of 6061 alloy matrix aluminums；As shown in Fig. 4 (b), from Y2O3Apply
The metallograph in layer/6061 matrix sections can be seen that coating and be well combined with matrix, and organizational structure is evenly distributed.
Claims (7)
1. a kind of IC equips the preparation method of key components and partss high-purity yttrium oxide coating, it is characterised in that bag
Include following steps：
1) thoroughly cleaning is carried out to spraying matrix before spraying, and region of the matrix beyond to be sprayed is carried out effectively
Protection；
2) high-purity yttrium oxide powder body to be sprayed is added in the powder feeder of cold spray apparatus；
3) cold spray apparatus are adopted, is sprayed at matrix position to be sprayed, obtain high-purity yttrium oxide coating.
2. IC according to claim 1 equips the preparation method of key components and partss high-purity yttrium oxide coating,
Characterized in that, cold spray process parameter is as follows：100～1000 DEG C of the gas temperature of powder feeding, the gas of powder feeding
0.5～5MPa of pressure, the 50～1500m/min of translational speed of powder body, 10～40mm of spray distance, powder feeding
10～150g/min of speed.
3. IC according to claim 2 equips the preparation method of key components and partss high-purity yttrium oxide coating,
Characterized in that, preferred cold spray process parameter is as follows：200～600 DEG C of the gas temperature of powder feeding, powder feeding
1～4MPa of gas pressure, the 500～1000m/min of translational speed of powder body, 20～30mm of spray distance, send
Powder 50～100g/min of speed.
4. the IC according to one of claims 1 to 3 equips key components and partss high-purity yttrium oxide coating
Preparation method, it is characterised in that the thickness of high-purity yttrium oxide coating is 50～500 μm.
5. IC according to claim 4 equips the preparation method of key components and partss high-purity yttrium oxide coating,
Characterized in that, the thickness of preferred high-purity yttrium oxide coating is 100～300 μm.
6. IC according to claim 1 equips the preparation method of key components and partss high-purity yttrium oxide coating,
Characterized in that, the chemical composition of high-purity yttrium oxide powder is by weight percentage：Y2O3≤ 99.9%, granularity
Scope is 2～50 μm.
7. IC according to claim 6 equips the preparation method of key components and partss high-purity yttrium oxide coating,
Characterized in that, the granularity requirements of high-purity yttrium oxide powder are：Granularity<35 μm of powder, its quality percentage contains
Amount is more than 95%；The powder that 35 μm～45 μm of granularity, its weight/mass percentage composition is less than 3%；Balance of granularity
>45 μm of powder.
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| CN201510676326.0A CN106591820B (en) | 2015-10-15 | 2015-10-15 | A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating |
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| CN201510676326.0A CN106591820B (en) | 2015-10-15 | 2015-10-15 | A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109957748A (en) * | 2019-04-02 | 2019-07-02 | 沈阳富创精密设备有限公司 | A kind of preparation method of IC equipment key components and parts surface protection coating |
| WO2019214075A1 (en) * | 2018-05-11 | 2019-11-14 | 沈阳富创精密设备有限公司 | Improved method for preparing y2o3 ceramic coating using cold spraying |
| CN110578143A (en) * | 2019-09-30 | 2019-12-17 | 中国科学院金属研究所 | Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3method for producing composite coating material |
| WO2020042287A1 (en) * | 2018-08-29 | 2020-03-05 | 沈阳富创精密设备有限公司 | Cold-spraying preparation method for y / y2o3 metal ceramic protective coating |
| WO2020168679A1 (en) * | 2019-02-22 | 2020-08-27 | 沈阳富创精密设备有限公司 | Method for preparing protective coating for plasma etching chamber of ic equipment |
| WO2021022791A1 (en) * | 2019-08-05 | 2021-02-11 | 沈阳富创精密设备有限公司 | Plasma spraying and cold spraying technology-based method for preparing a protective coating for surface of key components and parts of ic equipment |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019214075A1 (en) * | 2018-05-11 | 2019-11-14 | 沈阳富创精密设备有限公司 | Improved method for preparing y2o3 ceramic coating using cold spraying |
| CN110468402A (en) * | 2018-05-11 | 2019-11-19 | 中国科学院金属研究所 | A kind of cold spraying preparation Y2O3The improved method of ceramic coating |
| WO2020042287A1 (en) * | 2018-08-29 | 2020-03-05 | 沈阳富创精密设备有限公司 | Cold-spraying preparation method for y / y2o3 metal ceramic protective coating |
| CN110872713A (en) * | 2018-08-29 | 2020-03-10 | 中国科学院金属研究所 | Y/Y2O3Cold spraying preparation method of metal ceramic protective coating |
| CN110872713B (en) * | 2018-08-29 | 2022-04-05 | 中国科学院金属研究所 | Y/Y2O3Cold spraying preparation method of metal ceramic protective coating |
| WO2020168679A1 (en) * | 2019-02-22 | 2020-08-27 | 沈阳富创精密设备有限公司 | Method for preparing protective coating for plasma etching chamber of ic equipment |
| CN109957748A (en) * | 2019-04-02 | 2019-07-02 | 沈阳富创精密设备有限公司 | A kind of preparation method of IC equipment key components and parts surface protection coating |
| WO2021022791A1 (en) * | 2019-08-05 | 2021-02-11 | 沈阳富创精密设备有限公司 | Plasma spraying and cold spraying technology-based method for preparing a protective coating for surface of key components and parts of ic equipment |
| JP2022542655A (en) * | 2019-08-05 | 2022-10-06 | 沈陽富創精密設備股▲フン▼有限公司 | Manufacturing method of surface protective coating for main parts of IC device based on plasma spraying and low temperature spraying technology |
| JP7288548B2 (en) | 2019-08-05 | 2023-06-07 | 沈陽富創精密設備股▲フン▼有限公司 | Method for producing surface protective coatings for plasma etching chambers based on plasma spraying and low-temperature spraying technology |
| CN110578143A (en) * | 2019-09-30 | 2019-12-17 | 中国科学院金属研究所 | Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3method for producing composite coating material |
| CN110578143B (en) * | 2019-09-30 | 2021-10-22 | 中国科学院金属研究所 | Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3Method for producing composite coating material |
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