CN106591820B - A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating - Google Patents
A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating Download PDFInfo
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- CN106591820B CN106591820B CN201510676326.0A CN201510676326A CN106591820B CN 106591820 B CN106591820 B CN 106591820B CN 201510676326 A CN201510676326 A CN 201510676326A CN 106591820 B CN106591820 B CN 106591820B
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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
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Abstract
The present invention relates to cold sprayings to prepare field of ceramic coatings, especially a kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating.This method mainly includes following operating procedure: (1) protection in the uncoated region of part；(2) surface preparation of part spraying area；(3) high-purity yttrium oxide powder is used, purity >=99.9wt%, average particle size are 2~50 μm；(4) fast spraying is carried out using low pressure cold spraying system, obtains high-purity yttrium oxide coating.Compared to traditional thermal spraying, cold spraying can efficiently reduce and reduce the heat input to matrix, therefore, be suitable in the IC equipment key components and parts surface spraying coating such as aluminium and aluminium alloy.The cold spraying method that the present invention uses, spraying temperature are only 100~1000 DEG C, well below temperature needed for plasma spraying (i.e. 2410 DEG C of melting temperature of yttrium oxide or more)；The yttria coating quality of cold spraying preparation is stable, thickness is uniform.
Description
Technical field
The present invention relates to cold sprayings to prepare field of ceramic coatings, and especially a kind of IC equips the high pure zirconia of key components and parts
The preparation method of yttrium coating.
Background technique
For IC equipment enterprise, the supply of components determines the process of its research and development and industrialization.Do not meet IC to set
The components supplying that standby enterprise's technique requires, the development that IC equips industry is inconceivable.Break through representational IC equipment
The Integrated-manufacturing Techniques of high-end components and key components and parts can solve the localization of 70% components of IC equipment.Establish me
State IC equips special precision components public service platform, and research and development and industrialization process to China's IC equipment have most important
Effect.
With 22nm technology gradually be used for chip volume production, the world's integrated circuit line width research and development come into 14nm so that
The equipment and technique of 7nm are tackled key problems, at this time the integrated circuits critical equipment such as etching, ion implanting, PVD, CVD be faced with it is many newly
Challenge.It is on the one hand higher and higher to the indoor purity requirements of etch chamber by taking etching machine reaction chamber as an example；On the other hand, it etches
With the collective effect of the higher and higher plasma bombardment of strong corrosive gas and energy, the industry being currently known is produced most
Strong corrosive environment can generate serious corrosion in metal parts therein, release metal ion or particle pollution cavity,
Cause chip circuit short-circuit.
Traditional IC equipment components mostly use anode oxidation alumina coating to be protected.Since components are in strong
Corrosive environment and ion bombardment interacting state, once digestion of metallic ion is generated because of corrosion causes systemic contamination, damage
Mistake will be unable to estimate.Studies have shown that yttria coating has better plasma resistant erosion property than aluminium oxide, and have more
Long service life, therefore become IC and equip the defensive new coating of components.Other than etching machine, yttria coating exists
Also there is huge application value in other IC equipment components.
Yttria coating belongs to ceramic coating, is prepared usually using plasma spraying.Plasma spray is coated with plasma
Body is heat source, and yttrium oxide is heated to fusing (2410 DEG C) or semi-molten state and is then sprayed on matrix.This high temperature can not
Cause the oxidation, phase transformation or other chemical reactions of sprayed particle with avoiding, while high temperature may also to aluminum matrix alloy material
It causes to damage.
Summary of the invention
The high pure zirconia of key components and parts is equipped using cold spray technique preparation IC the purpose of the present invention is to provide a kind of
The preparation method of yttrium coating, solve the plasma spray technologies such as existing plasma preparation yttria coating when existing coating quality it is poor,
Problem that is oxidizable, and causing aluminium alloy spraying matrix heat input excessive is opened up the new high-purity yttrium oxide for preparing of one kind and is applied
The effective way of layer, to expand practical ranges early.
Technical solution of the present invention is as follows:
A kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating, comprising the following steps:
1) spraying matrix is thoroughly cleaned before spraying, and region of the matrix other than to be sprayed is effectively protected
Shield；
2) high-purity yttrium oxide powder to be sprayed is added in the powder feeder of cold spray apparatus；
3) cold spray apparatus is used, is sprayed at matrix position to be sprayed, high-purity yttrium oxide coating is obtained.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, cold spray process parameter are as follows:
100~1000 DEG C of the gas temperature of powder feeding, 0.5~5MPa of gas pressure of powder feeding, 50~1500m/ of movement speed of powder
Min, 10~40mm of spray distance, 10~150g/min of powder feeding rate.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, preferred cold spray process parameter
It is as follows: 200~600 DEG C of the gas temperature of powder feeding, 1~4MPa of gas pressure of powder feeding, 500~1000m/ of movement speed of powder
Min, 20~30mm of spray distance, 50~100g/min of powder feeding rate.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, the thickness of high-purity yttrium oxide coating
It is 50~500 μm.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, preferred high-purity yttrium oxide coating
With a thickness of 100~300 μm.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, the chemistry of high-purity yttrium oxide powder
Ingredient is by weight percentage are as follows: Y2O3≤ 99.9%, particle size range is 2~50 μm.
The preparation method of the IC equipment key components and parts high-purity yttrium oxide coating, the granularity of high-purity yttrium oxide powder
It is required that are as follows: the powder of granularity < 35 μm, mass percentage are greater than 95%；The powder that 35 μm~45 μm of granularity, quality percentage
Content is less than 3%；Surplus is the powder of granularity > 45 μm.
Design philosophy of the invention is:
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), is to use
The pre- hot compressed gas of heating facility, compressed gas generate ultrahigh speed air-flow by scaling type Laval nozzle, and driving metallic makes
It, with high velocity collision substrate, makes particle that violent plastic deformation occur under complete solid-state, and deposits in matrix surface
For a kind of novel spraying technology of coating.Since temperature is lower than its fusing point to powder particle in entire deposition process, thus it is referred to as cold
Spraying.In actual operation, common working gas has N2, He and air or their mixed gas.Working gas preheating
Temperature be usually no more than 1000 DEG C.Cold spraying has the characteristics that solid deposited under low temperature, can be significantly reduced or even disappears completely
Except oxidation, phase transformation, segregation, residual tension and crystal grain such as are grown up at the adverse effect in traditional thermal spraying.It is prepared using cold spraying high
The method of pure zirconia yttrium ceramic coating has not been reported.
The invention has the advantages and beneficial effects that:
1, the present invention has the characteristics that solid deposited under low temperature using cold spraying, can be significantly reduced and even completely eliminates biography
Oxidation, phase transformation, segregation, residual tension and crystal grain, which are grown up etc., in system thermal spraying adversely affects, and is got over by academia and industry
Carry out more concerns.Compared to traditional thermal spraying, cold spraying can efficiently reduce and reduce the heat input to matrix.Cause
This, is suitable in the IC equipment key components and parts surface spraying coating such as aluminium and aluminium alloy.
2, the cold spraying method that the present invention uses, spraying temperature is only 100~1000 DEG C, well below plasma spraying
Required temperature (i.e. 2410 DEG C of melting temperature of yttrium oxide or more)；The yttria coating quality stabilization of cold spraying preparation, thickness
Uniformly, the yttria coating with a thickness of 200 μm can be prepared, and coating is fine and close, greatly improves IC equipment components
The corrosivity of anti-high energy plasma and strong corrosive gas, while improving the service life and preparation efficiency of part.
Detailed description of the invention
Fig. 1 is the XRD analysis map 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.Wherein, 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 12O3Coating/6061 matrixes section metallograph.Wherein, Fig. 3 (a)
For 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)
For the SEM photograph of 6061 aluminium alloy matrix surfaces；Fig. 4 (b) is Y2O3Coating/6061 matrixes section metallograph.
Specific embodiment
In a specific embodiment, cold spraying of the present invention prepares the side of IC equipment key components and parts high-purity yttrium oxide coating
Method mainly comprises the steps that
1) spraying matrix is thoroughly cleaned before spraying, and region of the matrix other than to be sprayed is effectively protected
Shield；
2) high-purity yttrium oxide powder to be sprayed is added in the powder feeder of cold spray apparatus；
3) use cold spray apparatus, sprayed at matrix position to be sprayed, high-purity yttrium oxide coating with a thickness of 50~
500μm。
Wherein, cold spray apparatus refer to Chinese invention patent (patent No.: 01128130.8, Authorization Notice No.:
CN1161188C a kind of cold air driven spray painter) mentioned.During preparing high-purity coating using cold spray technique, spraying
When gas heating temperature be 100~1000 DEG C (preferably 200~600 DEG C), air, nitrogen or argon gas can be used in spray gas.
High-purity yttrium oxide powder is the commercial yttrium oxide powder sold on the market, and chemical component is by weight percentage are as follows: Y2O3≧
99.9% (particle size range is 2~50 μm), granularity requirements are as follows: the powder of granularity < 35 μm, mass percentage are greater than
95%；The powder that 35 μm~45 μm of granularity, mass percentage is less than 3%；Surplus is the powder of granularity > 45 μm.Typically
The cold spray process parameter of spraying high-purity yttrium oxide coating is shown in Table 1.
Table 1
To keep technical solution of the present invention and advantage clearer, it is described in detail below in conjunction with specific embodiment.
Embodiment 1
Cold spray process parameter: 600 DEG C of the gas temperature of powder feeding, the gas pressure 2MPa of powder feeding, powder movement speed
1000m/min, spray distance 20mm, powder feeding rate 100g/min, 4 passages；Matrix: 6061 aluminium alloys；It is obtained after spraying
About 120 μm of coating layer thickness.
(1) XRD analysis:
As shown in Figure 1, the Y after spraying2O3Compared with original powder composition transfer does not occur for coating.
(2) surface roughness measurement:
Ra=9.090 μm of the roughness average 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 Y2O3Coating/6061 matrix sections metallograph can be seen that coating and matrix
It is well combined, 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 movement speed
800m/min, spray distance 20mm, powder feeding rate 80g/min, 6 passages；Matrix: 6061 aluminium alloys；The painting obtained after spraying
About 100 μm of thickness degree.
As shown in Fig. 4 (a), the surface topography of 6061 alloy matrix aluminums；As shown in Fig. 4 (b), from Y2O3Coating/6061 matrixes
The metallograph in section can be seen that coating and be well combined with matrix, and institutional framework is evenly distributed.
Claims (3)
1. a kind of preparation method of IC equipment key components and parts high-purity yttrium oxide coating, which comprises the following steps:
1) spraying matrix is thoroughly cleaned before spraying, and region of the matrix other than to be sprayed is effectively protected；
2) high-purity yttrium oxide powder to be sprayed is added in the powder feeder of cold spray apparatus；
3) cold spray apparatus is used, is sprayed at matrix position to be sprayed, high-purity yttrium oxide coating is obtained；
Cold spray process parameter is as follows: 100~1000 DEG C of the gas temperature of powder feeding, 0.5~5MPa of gas pressure of powder feeding, powder
50~1500m/min of movement speed, 10~40mm of spray distance, 10~150g/min of powder feeding rate；
High-purity yttrium oxide coating with a thickness of 50~500 μm；The chemical component of high-purity yttrium oxide powder is by weight percentage are as follows:
Y2O3≤ 99.9%, particle size range is 2~50 μm；The granularity requirements of high-purity yttrium oxide powder are as follows: the powder of granularity < 35 μm, matter
It measures percentage composition and is greater than 95%；The powder that 35 μm~45 μm of granularity, mass percentage is less than 3%；Surplus is granularity > 45 μm
Powder.
2. the preparation method of IC equipment key components and parts high-purity yttrium oxide coating according to claim 1, feature exist
In preferred cold spray process parameter is as follows: 200~600 DEG C of the gas temperature of powder feeding, 1~4MPa of gas pressure of powder feeding, powder
500~1000m/min of movement speed of body, 20~30mm of spray distance, 50~100g/min of powder feeding rate.
3. the preparation method of IC equipment key components and parts high-purity yttrium oxide coating according to claim 1, feature exist
In, preferred high-purity yttrium oxide coating with a thickness of 100~300 μm.
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| 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 |
| 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 |
| CN109825827A (en) * | 2019-02-22 | 2019-05-31 | 沈阳富创精密设备有限公司 | A kind of preparation method of IC equipment plasma etch chamber protective coating |
| CN109957748B (en) * | 2019-04-02 | 2021-03-26 | 沈阳富创精密设备股份有限公司 | Preparation method of surface protective coating for IC equipment key parts |
| CN110468367A (en) * | 2019-08-05 | 2019-11-19 | 中国科学院金属研究所 | Preparation method based on the IC of plasma spraying and cold spray technique equipment key components and parts surface protection coating |
| 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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| CN104357785A (en) * | 2014-11-14 | 2015-02-18 | 北京矿冶研究总院 | Method for rapidly preparing high-purity yttrium oxide coating for plasma etching machine |
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