CN103194716B - A kind of reaction and plasma spraying is prepared the method for boron carbide coating - Google Patents
A kind of reaction and plasma spraying is prepared the method for boron carbide coating Download PDFInfo
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- CN103194716B CN103194716B CN201210002114.0A CN201210002114A CN103194716B CN 103194716 B CN103194716 B CN 103194716B CN 201210002114 A CN201210002114 A CN 201210002114A CN 103194716 B CN103194716 B CN 103194716B
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Abstract
The invention provides a kind of reaction and plasma spraying and prepare the method for boron carbide coating, comprise the steps: step (1), choose boron carbide powder, and boron carbide powder is sent into plasma-spraying device; Step (2), carries out pretreatment to the substrate surface being sprayed; Step (3), carries out plasma spraying by reactive plasma spraying equipment at described substrate surface, prepares boron carbide coating. The present invention uses methane gas (CH4) replace hydrogen to spray as back work gas, after methane gas ionization, there is reducing property protection B4C is not oxidized, simultaneously because contain C in gas, by itself and B4The reaction of C, can reduce and even prevent B4C C at high temperature runs off, and obtains well behaved B4C coating.
Description
Technical field
The present invention relates to plasma spraying technology field, be specifically related to a kind of gas-phase reaction plasmaThe method of boron carbide coating is prepared in spraying.
Background technology
At present, low temperature plasma fine machining method is the key technology of material micro-nano processing,It is the basis of the technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optics, particularly existsIn super large-scale integration manufacturing process, having nearly 1/3rd operation is by means of plasmaBody machines, as plasma foil deposition, plasma etching and removing of photoresist by plasmaDeng. One of technological process that wherein plasma etching is most critical is to realize ultra-large collectionBecome circuit produce in Micropicture with high fidelity from Lithographic template transfer to silicon chip can notAlternative technique.
In etching process, owing to having a large amount of activity with severe corrosive freelyBase, the inner surface in their article on plasma etching technics chambeies also can produce corrosiveness, causes pollution,Affect etching effect, and can make etching technics chamber lose efficacy. The plasma of the early stage ninetiesEtching apparatus, the in the situation that of smaller power and single plasma-generating source, at aluminum substrate layerOn add Al2O3Coating just can meet the etch damage of plasma to etching technics chamber. EnterTo 300mm equipment, along with plasma power is increasing, plasma is to etching technics chamberThe damage of wall is also increasing, makes, in the process of etching, following problem easily occurs: (1)Grain; (2) process cavity wall disbonding, causes plasma directly and aluminum substrate is had an effect;(3)Al2O3The life-span of parts is subject to more high-power restriction. So need to find a kind ofNew approach carries out modification to etching technics inner cavity surface, meets the needs of etching technics.
Research shows, Y2O3Coating has good protective effect to etching technics chamber. With Al2O3Compare Y2O3Chemical property highly stable, there is excellent resistance to plasma etching performance,And and CF is the product YF that gas generates3Steam forces down, and is difficult to disperse as particle.At present, with Y2O3Powder, as sprayed on material, utilizes air plasma spraying method, is carvingEtching technique inner cavity surface is prepared the Y of single structure2O3Corrosion-resistant finishes is that one generally adoptsMethod.
Than Y2O3, boron carbide (B4C) have more potentiality. Have superhard, high-melting-point,The a series of good physical such as density is low. Also have excellent chemical stability simultaneously, can supportAntiacid, caustic corrosion, and do not soak and have an effect with most of motlten metals. Therefore carbonizationBoron is again good corrosion-resistant material, for the processing of acid and alkali resistance parts. Due to boron carbideThe compatibility of material and semiconductor technology is good, is therefore suitable as very much the resistance to of semiconductor partsCorrosion resistant coating.
Preparation B4The main method of C coating has: chemical vapour deposition (CVD) (CVD), reaction-sintered andPlasma spraying etc. Air plasma spraying is to use N2、Ar、H2And He etc. is as ionGas, produces plasma high temperature and high speed jet through ionization, and input material fusing or melting are ejected intoWorking surface forms the method for coating. Plasma-arc extreme temperatures wherein, enough melts instituteSome high-melting-point ceramic powders. In air plasma spraying technique, gaseous environment can be to coatingFinal performance has impact significantly. The selection principle of gas is mainly to consider practicality and warpJi property. Concrete requirement is: (1) stable performance, not with sprayed on material generation adverse reaction;(2) heat content is high, is suitable for refractory material, but should be too high and ablation nozzle; (3) shouldThere is not the gas of chemical action in selection and electrode or nozzle; (4) with low cost, supply is convenient.
Jet temperature is high, coating layer thickness is controlled owing to having for plasma spraying, bond strength high withAnd the feature such as easy to operate, be preparation B4The effective ways of C coating. But, B4C is in sprayingIn process, have the problem such as high-temperature oxydation and gasification, air plasma spraying can not be prepared performanceGood B4C coating. There is research to adopt a kind of extraordinary resist technology, under inert gas shieldingCarry out plasma spraying, although obtained B4C coating, but in coating, still there is small partOxidation product. Therefore need the more suitably method of finding to prepare B4The C ceramic coating of resistance to erosion.
Summary of the invention
The invention provides a kind of preparation method of boron carbide coating of abrasion resistant and corrosion resistant performance.
Concrete technical scheme is realized by following steps:
Reaction and plasma spraying is prepared a method for boron carbide coating, comprises the steps:
Step (1), chooses boron carbide powder, and boron carbide powder is sent into plasma-spraying device;
Step (2), carries out pretreatment to the substrate surface being sprayed;
Step (3), chooses Ar and CH4For spraying gas, establish by described plasma spray coatingFor carrying out plasma spraying at described substrate surface, prepare boron carbide coating.
In such scheme, the granularity of described boron carbide powder is 5-40 μ m.
In such scheme, described step is located in advance to the substrate surface being sprayed in (2)Reason, specifically comprises the steps: that the substrate surface to being sprayed carries out blasting treatment, and with thirdKetone cleans.
In such scheme, the sand-blast material that described blasting treatment adopts is white fused alumina, sandblast grainDegree is 50-100 μ m.
In such scheme, Ar flow 40-90L/min, CH4Flow 5-20L/min.
In such scheme, the arc voltage 40-50V of described plasma spraying equipment, electric arcElectric current 800-900A, powder feed rate 15-100g/min, spray distance 80-135mm, powder feeding50 °-90 ° of angles.
The present invention uses methane gas (CH4) replace hydrogen to spray as back work gas,After methane gas ionization, there is reducing property protection B4C is not oxidized, simultaneously because contain in gasC, by itself and B4The reaction of C, can reduce and even prevent B4C C at high temperature runs off.Obtain well behaved B4C coating.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is further described in detail, providesEmbodiment is only in order to illustrate the present invention, instead of in order to limit the scope of the invention.
The present embodiment provides a kind of method of gas-phase reaction Plasma Spray Boron Carbide Coating,Comprise the steps:
(1) select B4C powder, particle size range is 5-40 μ m, has splendid mobility.
(2) the etching technics cavity wall of aluminium base is carried out to blasting treatment, sand-blast material is whiteCorundum, particle size range is 50-100 μ m, and cleans with acetone.
(3) adopt SluzerMetco9MC plasma spraying equipment to carry out plasma spraying,Spray gun type 9MB. Spraying gaseous environment is Ar/CH4: Ar flow 40-90L/min, CH4Flow 5-20L/min. Arc voltage 40-50V, arc current 800-900A, powder feed rate50 °-90 ° of 15-100g/min, spray distance 80-135mm, powder feeding angles. At spraying processIn, adopt air blowing method or recirculated water cooling method to carry out cooling matrix. When adopting air sprayWhile blowing the cooling matrix of method, the flow of refrigerating gas is 100-2000L/min; When adopting circulationWhen the cooling matrix of water-cooling method, the flow of cooling water is 10-500L/min.
The above is only preferred embodiment of the present invention, therefore all according to patent claim of the present inventionThe equivalence that described structure, feature and principle done changes or modifies, and is included in the present invention specialIn profit application range.
Claims (4)
1. reaction and plasma spraying is prepared a method for boron carbide coating, it is characterized in that, comprises the steps:
Step (1), chooses boron carbide powder, and boron carbide powder is sent into plasma-spraying device;
Step (2), carries out pretreatment to the substrate surface being sprayed;
Step (3), chooses Ar and CH4For spraying gas, carry out plasma spraying by described plasma-spraying device at described substrate surface, prepare boron carbide coating;
Wherein, described Ar flow 40-90L/min, described CH4Flow 5-20L/min; The arc voltage of described plasma-spraying device is 40-50V, arc current 800-900A, powder feed rate 15-100g/min, spray distance 80-135mm, 50 °-90 ° of powder feeding angles.
2. method according to claim 1, is characterized in that, the granularity of described boron carbide powder is 5-40 μ m.
3. method according to claim 1, is characterized in that, described step is carried out pretreatment to the substrate surface being sprayed in (2), specifically comprises the steps: that the substrate surface to being sprayed carries out blasting treatment, and cleans with acetone.
4. method according to claim 3, is characterized in that, the sand-blast material that described blasting treatment adopts is white fused alumina, and sand size is 50-100 μ m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210002114.0A CN103194716B (en) | 2012-01-05 | 2012-01-05 | A kind of reaction and plasma spraying is prepared the method for boron carbide coating |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210002114.0A CN103194716B (en) | 2012-01-05 | 2012-01-05 | A kind of reaction and plasma spraying is prepared the method for boron carbide coating |
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| CN103194716A CN103194716A (en) | 2013-07-10 |
| CN103194716B true CN103194716B (en) | 2016-05-18 |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104711504B (en) * | 2013-12-17 | 2018-07-13 | 中国科学院微电子研究所 | A kind of preparation method of boron carbide coating applied to quartz substrate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6054187A (en) * | 1997-12-15 | 2000-04-25 | Ngk Insulators, Ltd. | Method of manufacturing a boron carbide film on a substrate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6054187A (en) * | 1997-12-15 | 2000-04-25 | Ngk Insulators, Ltd. | Method of manufacturing a boron carbide film on a substrate |
Non-Patent Citations (1)
| Title |
|---|
| 等离子喷涂碳化硼涂层的性能研究;曾毅 等;《材料保护》;19990430;第32卷(第4期);33-34,36 * |
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Effective date of registration: 20201223 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: 100029 Beijing city Chaoyang District Beitucheng West Road No. 3 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. |