CN103484809B - The making method of corrosion-resistant coating, corrosion-resistant coating, plasma processing device - Google Patents
The making method of corrosion-resistant coating, corrosion-resistant coating, plasma processing device Download PDFInfo
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- CN103484809B CN103484809B CN201210195700.1A CN201210195700A CN103484809B CN 103484809 B CN103484809 B CN 103484809B CN 201210195700 A CN201210195700 A CN 201210195700A CN 103484809 B CN103484809 B CN 103484809B
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Abstract
The invention provides a kind of making method of corrosion-resistant coating, corrosion-resistant coating, plasma processing device, wherein, the making method of corrosion-resistant coating comprises the following steps: yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1: 1 are mixed acquisition composite granule; Described composite granule is coated in the surface of described metal parts, thus obtains erosion-resisting compound coating on the surface of described metal parts.The making method of this corrosion-resistant coating can obtain the lower corrosion-resistant coating of porosity, thus can improve the plasma etch resistance energy of coating.
Description
Technical field
The invention belongs to microelectronic processing technique field, particularly, relate to a kind of making method of corrosion-resistant coating, corrosion-resistant coating and plasma processing device.
Background technology
Plasma processing device is the common equipment of processing semiconductor device, and it is mainly used in implementing the techniques such as etching, sputtering and deposition.In the process of implementing process, the reactant gases ionization that plasma processing device will pass in reaction chamber, to form plasma body in reaction chamber, and utilizes plasma processor part.Because plasma body has very strong corrodibility to metal, therefore, the metal parts (as by metal chamber inner walls such as aluminium alloys) the being positioned at reaction chamber easily corrosion of subject plasma and service life reduction, thus add the use cost of plasma processing device.In addition, the metallic particles that plasma etching produces not only can pollute reaction chamber, thus increases the difficulty of cleaning reaction chamber, but also can pollute the surface of workpiece to be machined, thus affects the processing quality of workpiece to be machined.
In order to improve the plasma etch resistance energy of metal parts, usually spray one deck yttria coating in its surface, to improve the work-ing life of metal parts.But because the porosity (that is, the ratio of interstitial surface area and the coating total area) of yttria coating is comparatively large, generally at about 4%-5%, plasma body easily penetrates yttria coating and corroding metal substrate.
Disclose in the document of " development of high-purity yttrium oxide compound coating " that " hot-spraying techniques " was published in volume the 2nd phase December the 1st in 2009 the 31st page to the 33rd page another kind of plasma etch resistance can coating, i.e. alumina-yttria compound coating, this compound coating comprises the bottom and top layer that are successively set on substrate surface, wherein, bottom is aluminum oxide coating layer; Top layer is yttria coating.Compared with mono-layer oxidized yttrium coating; alumina-yttria compound coating adds aluminum oxide coating layer; the effect of temporary protection metal base can be played by aluminum oxide coating layer after yttria coating failures, thus improve the corrosive nature of the plasma resistant of metal parts.But inevitably there is following problem in actual applications in alumina-yttria compound coating:
One, due to different from the thermal expansivity on yttrium oxide top layer at aluminum oxide bottom, in use, easily ftracture and even come off in aluminum oxide bottom and yttrium oxide top layer, this not only lowers the corrosive nature of the plasma resistant of coating, and the coating come off also can pollute reaction chamber.
Its two, alumina-yttria compound coating only increases the thickness of coating, and porosity is still comparatively large, and therefore, the corrosive nature of the plasma resistant of coating does not improve significantly.
Summary of the invention
The present invention is intended at least to solve one of technical problem existed in prior art, and propose a kind of corrosion-resistant coating and making method, it has lower porosity, improves the plasma etch resistance energy of coating.
In addition, the invention allows for a kind of plasma processing device, the coating being arranged on metal part surface has lower porosity, and plasma etch resistance can be higher, thus improves the work-ing life of metal parts.
A kind of making method of corrosion-resistant coating being provided for realizing object of the present invention, for preparing corrosion-resistant coating on the surface of metal parts, comprising the following steps:
Yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are mixed acquisition composite granule;
The surface of described metal parts is cleaned and sandblasting;
Adopt spraying coating process alumina powder jointed in the surface-coated of described metal parts, to obtain aluminum oxide coating layer;
By spraying coating process, described composite granule is coated in the surface of described aluminum oxide coating layer, thus obtains erosion-resisting compound coating;
Adopt spraying coating process at the surface-coated yttrium oxide powder of described compound coating, to obtain yttria coating.
Wherein, yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are being mixed in the step obtaining composite granule, in described yttrium oxide powder, the purity of yttrium oxide is more than 99.9%.
Wherein, yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are being mixed obtain composite granule step in, described alumina powder jointed in, the purity of aluminum oxide is more than 99.9%.
Wherein, the size range of described composite granule is at 20 ~ 40 μm.
Wherein, the thickness range of described erosion-resisting compound coating is at 150 ~ 200 μm.
Wherein, sandblasting is carried out to the surface of described metal parts, make the surface roughness Ra of described metal parts be 6 ~ 8 μm.
Wherein, employing spraying coating process in the step that the surface-coated of described metal parts is alumina powder jointed, described alumina powder jointed size range at 20 ~ 40 μm, and described alumina powder jointed in, the purity of aluminum oxide is more than 99.9%; The thickness range of described aluminum oxide coating layer is at 150 ~ 200 μm.
Wherein, at employing spraying coating process in the step of the surface-coated yttrium oxide powder of described compound coating, the size range of described yttrium oxide powder is at 20 ~ 40 μm, and in described yttrium oxide powder, the purity of described yttrium oxide is more than 99.9%; The thickness range of described yttria coating is at 150 ~ 200 μm.
The present invention also provides a kind of corrosion-resistant coating, for improving the plasma etch resistance energy of metal parts, the aluminum oxide coating layer that the thickness direction that described corrosion-resistant coating is included in described metal parts sets gradually, compound coating and yttria coating; Described compound coating includes yttrium oxide and aluminum oxide, and the weight ratio of yttrium oxide and aluminum oxide is 1:1.
Wherein, the thickness range of described compound coating is 150 ~ 200 μm.
The present invention also provides a kind of plasma processing device, comprises reaction chamber, in described reaction chamber, be provided with corrosion-resistant coating with the surface of the metal parts of Plasma contact, and described corrosion-resistant coating is corrosion-resistant coating provided by the invention.
The present invention has following beneficial effect:
The making method of corrosion-resistant coating provided by the invention, its by the surface-coated at metal parts by yttrium oxide powder and the alumina powder jointed composite granule mixed according to the ratio of weight ratio 1:1, thus obtain the anticorrosive compound coating had compared with low porosity, and then improve the plasma etch resistance energy of coating.
In a preferred embodiment of the present invention, adopt spraying coating process on the surface of metal parts successively coating alumina powder, composite granule and yttrium oxide powder, thus obtain aluminum oxide coating layer, compound coating and yttria coating successively from inside to outside on the surface of metal parts.Due to above-mentioned composite granule be by purity be more than 99.9% yttrium oxide powder and the alumina powder jointed ratio according to weight ratio 1: 1 mix, thus obtained compound coating has lower porosity, thus improves the corrosive nature of the plasma resistant of coating.In addition, because compound coating has the coefficient of thermal expansion all close with yttria coating with aluminum oxide coating layer, thus it solves coating because there is the difference of coefficient of thermal expansion and the problem ftractureing or come off as middle layer, thus further increases the corrosive nature of the plasma resistant of coating.
The present invention also provides a kind of corrosion-resistant coating, comprise compound coating, described compound coating includes yttrium oxide and aluminum oxide, and the weight ratio of yttrium oxide and aluminum oxide is 1: 1, this corrosion-resistant coating has lower porosity, thus the plasma etch resistance energy of metal parts can be improved, and then the work-ing life of metal parts can be improved.
The present invention also provides a kind of plasma processing device, and it, by applying corrosion-resistant coating provided by the invention on metal parts, can improve the plasma etch resistance energy of metal parts, thus improve the work-ing life of metal parts.
Accompanying drawing explanation
The FB(flow block) of the making method of the corrosion-resistant coating that Fig. 1 provides for the embodiment of the present invention;
Fig. 2 a is for adopting the cross section microstructure morphology of the corrosion-resistant coating of the making method acquisition shown in Fig. 1;
The chart of percentage comparison that Fig. 2 b is the corrosion-resistant coating cross section mesoporosity area shown in Fig. 2 a and non-interstitial surface area;
The FB(flow block) of the making method of the corrosion-resistant coating that Fig. 3 provides for the embodiment of the present invention; And
Fig. 4 is for adopting the sectional view of the corrosion-resistant coating of the making method acquisition shown in Fig. 3.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the making method of corrosion-resistant coating provided by the invention, corrosion-resistant coating and plasma processing device are described in detail.
The FB(flow block) of the making method of the corrosion-resistant coating that Fig. 1 provides for the embodiment of the present invention.Refer to Fig. 1, the making method of corrosion-resistant coating is that it comprises the following steps for preparing corrosion-resistant coating on the surface of metal parts:
Step S1, mixes acquisition composite granule by yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1: 1.
Step S2, is coated in the surface of metal parts by composite granule, thus obtains erosion-resisting compound coating on the surface of metal parts.
Utilize weight ratio to be the yttrium oxide powder of 1: 1 and the anticorrosive compound coating of alumina powder jointed acquisition, there is lower porosity, thus the plasma etch resistance energy of corrosion-resistant coating can be improved.
Preferably, in step S 1, in yttrium oxide powder, the purity of yttrium oxide is more than 99.9%; In alumina powder jointed, the purity of aluminum oxide is more than 99.9%.In actual applications, the purity of yttrium oxide and aluminum oxide is higher, and the quality of corrosion-resistant coating is better.In addition, tackle alumina powder jointed and yttrium oxide powder and carry out ball milling mixing fully, mix to make the two.And the size range of the mixed composite granule of ball milling is 20 ~ 40 μm.
Preferably, in step s 2, adopt spraying coating process composite granule to be coated in the surface of metal parts, thus obtain erosion-resisting compound coating on the surface of metal parts.
Step S2 specifically comprises:
Step S21, cleans and sandblasting the surface of described metal parts.
Before surface composite granule being coated in metal parts, can clean and sandblasting the surface of metal parts in advance, to improve the surface smoothness of metal parts.Clean can adopt washed with de-ionized water, also first can adopt alcohol or acetone cleaning, then use deionized water rinsing, with the bonding force avoiding the materials such as the greasy dirt of metal part surface, dust to affect composite granule and metal parts.Sandblasting is the roughness in order to increase metal part surface, to improve the bonding force of composite granule and metal parts.The surface roughness Ra (profile arithmetic mean deviation) of the present embodiment metal parts after sandblasting is 6 ~ 8 μm.
Step S22, is coated in the surface of described metal parts by described composite granule by spraying coating process, thus obtain erosion-resisting compound coating.
The present embodiment applies composite granule by spraying coating process, thus obtain erosion-resisting compound coating on the surface of metal parts.The thickness of erosion-resisting compound coating is 150 ~ 200 μm.
In actual applications, spraying coating process can select suitable spraying equipment as the case may be, and according to processing parameters such as the setting of adopted spraying equipment airshed, spray distance and electric currents.Such as, when adopting German GTV company plasma spray system spraying compound coating, the processing parameter of spraying compound coating can be set as: main air stream amount is 35 ~ 40L/min, and auxiliary airshed is 10 ~ 15L/min, and electric current is 600 ~ 650A and spray distance is 200 ~ 240 μm.
Below the compound coating that the making method of the corrosion-resistant coating adopting the present embodiment to provide obtains is tested, to obtain the porosity of this compound coating.The concrete grammar of the porosity of test compound coating is: adopt the microstructure morphology of scanning electron microscope to compound coating cross section to observe, and adopt Survey Software to measure non-interstitial surface area in observed compound coating cross section and interstitial surface area respectively, to calculate the porosity of compound coating according to non-interstitial surface area and interstitial surface area.The test result adopting aforesaid method to obtain is specially: Fig. 2 a is for adopting the cross section microstructure morphology of the corrosion-resistant coating of the making method acquisition shown in Fig. 1.The chart of percentage comparison that Fig. 2 b is the corrosion-resistant coating cross section mesoporosity area shown in Fig. 2 a and non-interstitial surface area.As shown in Figure 2 a, in figure, yellow area is compound coating, and red area is hole.As can be seen from Fig. 2 a, the comparatively small amt of compound coating mesoporosity, and the area of single hole is less, thus the integrity of compound coating is better, thus effectively can prevent plasma penetration coating corrosion metal parts.
As shown in Figure 2 b, in figure, yellow tetragonal body is the summation of the non-interstitial surface area in compound coating cross section in Fig. 2 a, and red tetragonal body is the summation of the interstitial surface area in compound coating cross section.From Fig. 2 b, the ratio of non-interstitial surface area and the total area is 97.5%, the ratio of interstitial surface area and the total area is 2.5%, namely, the porosity of this compound coating is 2.5%, and the porosity of existing yttria coating is 4%-5%, therefore, the porosity of the compound coating of the making method acquisition of the corrosion-resistant coating adopting the present embodiment to provide obviously reduces, thus improves the plasma etch resistance energy of coating.
Fig. 3 is the FB(flow block) of the making method of corrosion-resistant coating provided by the invention.Fig. 4 is for adopting the sectional view of the corrosion-resistant coating of the making method acquisition shown in Fig. 3.See also Fig. 3 and Fig. 4, the making method of corrosion-resistant coating comprises the following steps:
Step S100, adopts spraying coating process alumina powder jointed in the surface-coated of metal parts 1, to obtain aluminum oxide coating layer 2.
In the step s 100, adopt purity be more than 99.9% alumina powder jointed, and alumina powder jointed size range is at 20 ~ 40 μm.The thickness range of the aluminum oxide coating layer 2 obtained is at 150 ~ 200 μm.When adopting German GTV company plasma spray system spraying compound coating, the processing parameter of spray aluminum oxide coating 2 is: main air stream amount is 30 ~ 35L/min, auxiliary airshed is 15 ~ 20L/min, and electric current is 600 ~ 620A and spray distance is 220 ~ 250 μm.In actual applications, spraying coating process can select suitable spraying equipment as the case may be, and according to processing parameters such as the setting of adopted spraying equipment airshed, spray distance and electric currents.
In addition, by alumina powder jointed be coated in the surface of metal parts before, first the surface of metal parts is cleaned and sandblasting, cleans identical with sandblasting with the cleaning in embodiment with the concrete technology parameter of sandblasting, in this no longer repeated description.
Step S200, at the surface-coated composite granule of aluminum oxide coating layer 2, thus obtains compound coating 3 on the surface of aluminum oxide coating layer 2.
Step S200 is identical with the step S2 in embodiment, does not repeat them here.
Step S300, adopts spraying coating process at the surface-coated yttrium oxide powder of compound coating 3, to obtain yttria coating 4.
In step S300, adopt purity to be the yttrium oxide powder of more than 99.9%, and the size range of yttrium oxide powder is at 20 ~ 40 μm.The thickness range of the yttria coating obtained is at 150 ~ 200 μm.When adopting German GTV company plasma spray system spraying compound coating, the processing parameter of spraying yttria coating 4 is: main air stream amount is 35 ~ 38L/min, auxiliary airshed is 15 ~ 18L/min, and electric current is 600 ~ 650A and spray distance is 240 ~ 250 μm.In actual applications, spraying coating process can select suitable spraying equipment as the case may be, and according to processing parameters such as the setting of adopted spraying equipment airshed, spray distance and electric currents.
As from the foregoing, the making method that the present embodiment provides is that yttria coating is as top layer using aluminum oxide coating layer as bottom, compound coating as middle layer.Because the porosity of compound coating is lower, thus improve the corrosive nature of the plasma resistant of whole corrosion-resistant coating.In addition, because compound coating has the coefficient of thermal expansion all close with yttria coating with aluminum oxide coating layer, thus it solves coating because there is the difference of coefficient of thermal expansion and the problem ftractureing or come off as middle layer, thus further increases the corrosive nature of the plasma resistant of coating.
It should be noted that, although the present embodiment is coating alumina powder, composite granule and yttrium oxide powder successively on the surface of metal parts, the present invention is not limited thereto.In actual applications, corrosion-resistant coating also can using compound coating as bottom, and yttria coating is as top layer; Or using aluminum oxide coating layer as bottom, compound coating is as top layer, or using yttria coating as bottom, compound coating as middle layer, aluminum oxide coating layer is as top layer.
In sum, the making method of the corrosion-resistant coating that the present embodiment provides, its by the surface-coated at metal parts by yttrium oxide powder and the alumina powder jointed composite granule mixed according to the ratio of weight ratio 1: 1, the anticorrosive compound coating had compared with low porosity can be obtained, thus improve the plasma etch resistance energy of coating.
The present invention also provides a kind of corrosion-resistant coating, for improving the plasma etch resistance energy of metal parts.In the present embodiment, corrosion-resistant coating comprises one deck compound coating, and this compound coating includes yttrium oxide and alumina component, and the weight ratio of yttrium oxide and aluminum oxide is 1: 1.Utilize weight ratio to be the yttrium oxide powder of 1: 1 and the anticorrosive compound coating of alumina powder jointed acquisition, there is lower porosity, thus improve the plasma etch resistance energy of anticorrosive compound coating.
It should be noted that, in the present embodiment, corrosion-resistant coating is one deck compound coating, but the present invention is not limited thereto, in actual applications, aluminum oxide coating layer, compound coating and yttria coating that the thickness direction that corrosion-resistant coating is included in metal parts sets gradually; Or be the compound coating that is successively set on metal part surface and yttria coating; Or be the aluminum oxide coating layer that is successively set on metal part surface and compound coating.
Preferably, the thickness range of compound coating is 150 ~ 200 μm, so both can improve the plasma etch resistance energy of corrosion-resistant coating, can reduce again the cost of corrosion-resistant coating.
In sum, corrosion-resistant coating provided by the invention, it comprises compound coating, it is 1: 1 yttrium oxide and aluminum oxide that compound coating includes weight ratio, such corrosion-resistant coating has lower porosity, thus the plasma etch resistance energy of metal parts can be improved, and then the work-ing life of metal parts can be improved.
The present invention also provides a kind of plasma processing device, it comprises reaction chamber, and be provided with corrosion-resistant coating on the locular wall of reaction chamber and/or with the surface of the metal parts of Plasma contact, this corrosion-resistant coating is the coating structure described in above-described embodiment, does not repeat them here.
Plasma processing device provided by the invention, by the metal parts in the chamber of itself and Plasma contact applying the above-mentioned corrosion-resistant coating had compared with low porosity, the plasma etch resistance energy of metal parts can be improved, thus improve the work-ing life of metal parts, and then improve the working (machining) efficiency of plasma processing device.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (11)
1. a making method for corrosion-resistant coating, for preparing corrosion-resistant coating on the surface of metal parts, is characterized in that, comprising the following steps:
Yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are mixed acquisition composite granule;
The surface of described metal parts is cleaned and sandblasting;
Adopt spraying coating process alumina powder jointed in the surface-coated of described metal parts, to obtain aluminum oxide coating layer;
By spraying coating process, described composite granule is coated in the surface of described aluminum oxide coating layer, thus obtains erosion-resisting compound coating;
Adopt spraying coating process at the surface-coated yttrium oxide powder of described compound coating, to obtain yttria coating.
2. the making method of corrosion-resistant coating according to claim 1, it is characterized in that, yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are being mixed in the step obtaining composite granule, in described yttrium oxide powder, the purity of yttrium oxide is more than 99.9%.
3. the making method of corrosion-resistant coating according to claim 1, it is characterized in that, yttrium oxide powder and the alumina powder jointed ratio ball milling according to weight ratio 1:1 are being mixed obtain composite granule step in, described alumina powder jointed in, the purity of aluminum oxide is more than 99.9%.
4. the making method of corrosion-resistant coating according to claim 1, is characterized in that, the size range of described composite granule is at 20 ~ 40 μm.
5. the making method of corrosion-resistant coating according to claim 1, is characterized in that, the thickness range of described erosion-resisting compound coating is at 150 ~ 200 μm.
6. the making method of corrosion-resistant coating according to claim 1, is characterized in that, carries out sandblasting to the surface of described metal parts, makes the surface roughness Ra of described metal parts be 6 ~ 8 μm.
7. the making method of corrosion-resistant coating according to claim 1, it is characterized in that, at employing spraying coating process in the step that the surface-coated of described metal parts is alumina powder jointed, described alumina powder jointed size range is at 20 ~ 40 μm, and described alumina powder jointed in, the purity of aluminum oxide is more than 99.9%; The thickness range of described aluminum oxide coating layer is at 150 ~ 200 μm.
8. the making method of corrosion-resistant coating according to claim 1, it is characterized in that, at employing spraying coating process in the step of the surface-coated yttrium oxide powder of described compound coating, the size range of described yttrium oxide powder is at 20 ~ 40 μm, and in described yttrium oxide powder, the purity of described yttrium oxide is more than 99.9%; The thickness range of described yttria coating is at 150 ~ 200 μm.
9. a corrosion-resistant coating, for improving the plasma etch resistance energy of metal parts, is characterized in that, the aluminum oxide coating layer that the thickness direction that described corrosion-resistant coating is included in described metal parts sets gradually, compound coating and yttria coating;
Described compound coating includes yttrium oxide and aluminum oxide, and the weight ratio of yttrium oxide and aluminum oxide is 1:1.
10. corrosion-resistant coating according to claim 9, is characterized in that, the thickness range of described compound coating is 150 ~ 200 μm.
11. 1 kinds of plasma processing devices, comprise reaction chamber, in described reaction chamber, be provided with corrosion-resistant coating with the surface of the metal parts of Plasma contact, it is characterized in that, described corrosion-resistant coating is the corrosion-resistant coating described in claim 9-10 any one.
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| CN116092909A (en) * | 2017-12-12 | 2023-05-09 | 中微半导体设备(上海)股份有限公司 | Plasma etching reactor |
| CN110246738A (en) * | 2018-03-08 | 2019-09-17 | 北京北方华创微电子装备有限公司 | Reaction chamber modular construction and preparation method thereof, reaction chamber |
| JP7066868B2 (en) * | 2018-03-08 | 2022-05-13 | ベイジン・ナウラ・マイクロエレクトロニクス・イクイップメント・カンパニー・リミテッド | Reaction chamber components, fabrication methods, and reaction chambers |
| CN110634723B (en) * | 2018-06-21 | 2022-07-05 | 中微半导体设备(上海)股份有限公司 | Corrosion-resistant gas mixing device and plasma treatment equipment |
| CN109081605A (en) * | 2018-08-13 | 2018-12-25 | 长兴微羽智能科技有限公司 | A kind of preparation method and applications of Ce3+/Y3+ codope TiO2 film |
| CN110331362A (en) * | 2019-08-21 | 2019-10-15 | 重庆臻宝实业有限公司 | The composite coating and preparation method of resisting plasma corrosion |
| CN114256047B (en) * | 2020-09-25 | 2023-12-22 | 中微半导体设备(上海)股份有限公司 | Semiconductor component, coating forming method and plasma reaction apparatus |
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| US7220497B2 (en) * | 2003-12-18 | 2007-05-22 | Lam Research Corporation | Yttria-coated ceramic components of semiconductor material processing apparatuses and methods of manufacturing the components |
| KR100863456B1 (en) * | 2008-01-14 | 2008-11-18 | 주식회사 코미코 | Spray coating powder and method of manufacturing the spray coating powder |
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