CN103194716A - Method for preparing boron carbide coating through reaction plasma spraying - Google Patents

Method for preparing boron carbide coating through reaction plasma spraying Download PDF

Info

Publication number
CN103194716A
CN103194716A CN2012100021140A CN201210002114A CN103194716A CN 103194716 A CN103194716 A CN 103194716A CN 2012100021140 A CN2012100021140 A CN 2012100021140A CN 201210002114 A CN201210002114 A CN 201210002114A CN 103194716 A CN103194716 A CN 103194716A
Authority
CN
China
Prior art keywords
plasma spraying
boron carbide
coating
reaction
plasma
Prior art date
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.)
Granted
Application number
CN2012100021140A
Other languages
Chinese (zh)
Other versions
CN103194716B (en
Inventor
王文东
闫坤坤
黄春
刘邦武
夏洋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ruili Flat Core Microelectronics Guangzhou Co Ltd
Original Assignee
Institute of Microelectronics of CAS
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Institute of Microelectronics of CAS filed Critical Institute of Microelectronics of CAS
Priority to CN201210002114.0A priority Critical patent/CN103194716B/en
Publication of CN103194716A publication Critical patent/CN103194716A/en
Application granted granted Critical
Publication of CN103194716B publication Critical patent/CN103194716B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention provides a method for preparing a boron carbide coating through reaction plasma spraying. The method comprises the steps that: step (1), boron carbide powder is selected and is delivered into a plasma spraying device; step (2), the surface of a substrate requiring spraying is pretreated; and step (3), plasma spraying is carried out upon the surface of the substrate by using the reaction plasma spraying device, such that the boron carbide coating is prepared. According to the invention, spraying is carried out by using methane gas (CH4) which is used for replacing hydrogen as an auxiliary working gas. Methane gas has a reducing performance after ionization, such that B4C can be protected from oxidation. Also, the gas comprises C. Through a reaction of C and B4C, C loss of B4C under high temperature can be reduced or even prevented, such that the B4C coating with good performances can be obtained.

Description

A kind of reaction and plasma spraying prepares the method for boron carbide coating
Technical field
The present invention relates to the plasma spraying technology field, be specifically related to the method that a kind of gas-phase reaction plasma spraying prepares boron carbide coating.
Background technology
At present, the low-temperature plasma fine machining method is the gordian technique of material micro-nano processing, it is the basis of technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optic, particularly in the super large-scale integration manufacturing process, there is nearly 1/3rd operation to finish by means of plasma process, as plasma foil deposition, plasma etching and removing of photoresist by plasma etc.Wherein plasma etching is one of technical process of most critical, is to realize that the Micropicture of super large-scale integration in producing with high fidelity transfer to irreplaceable technology on the silicon chip from Lithographic template.
In etching process, owing to there is a large amount of living radicals with severe corrosive, the internal surface in their article on plasma etching technics chambeies also can produce corrosive nature, causes pollution, influences etching effect, and is lost efficacy in the etching technics chamber.The plasma etching equipment of the early stage nineties takes place to add Al at the aluminum substrate layer under the situation in source at smaller power and single plasma body 2O 3Coating just can satisfy plasma body to the etch damage in etching technics chamber.Enter into 300mm equipment, along with plasma power is increasing, plasma body is also increasing to the damage of etching technics chamber wall, makes in the following problem of the easy generation of the process of etching: (1) particle; (2) process cavity wall disbonding causes plasma body directly and aluminum substrate is had an effect; (3) Al 2O 3The life-span of component is subjected to more high-power restriction.So need to seek a kind of new approach the etching technics inner cavity surface is carried out modification, satisfy the needs of etching technics.
Studies show that Y 2O 3Coating has good protective action to the etching technics chamber.With Al 2O 3Compare Y 2O 3Chemical property highly stable, have excellent anti-plasma etching performance, and and CF be the reaction product YF that gas generates 3Steam forces down, and is difficult to disperse as particle.At present, with Y 2O 3Powder utilizes the air plasma spraying method as spray material, prepares the Y of single structure at the etching technics inner cavity surface 2O 3Corrosion-resistant finishes is a kind of method that generally adopts.
Than Y 2O 3, norbide (B 4C) then have more potentiality.Have a series of good physical such as superhard, high-melting-point, density be low.Also have excellent chemical stability simultaneously, can resist sour, caustic corrosion, and not with most of molten metals wetting with have an effect.Therefore norbide is again good corrosion resistant material, is used for the processing of acid-and base-resisting component.Because boron carbide material and semiconductor technology is compatible good, therefore be suitable as very much the corrosion-resistant finishes of semi-conductor component.
Preparation B 4The main method of C coating has: chemical vapor deposition (CVD), reaction sintering and plasma spraying etc.Air plasma spraying is to use N 2, Ar, H 2And He etc. produces plasma high temperature and high speed jet as ion gas through ionization, and input material fusing or fusion are ejected into the method that working-surface forms coating.Plasma arc extreme temperatures is wherein enough melted all high-melting-point ceramic powder.In the air plasma spraying technology, atmosphere surrounding can have influence significantly to the final performance of coating.The selection principle of gas mainly is to consider practicality and economy.Concrete requirement is: (1) stable performance, not with spray material generation adverse reaction; (2) the heat content height is suitable for refractory material, but does not answer too high and the ablation nozzle; (3) should selection and electrode or nozzle the gas of chemical action does not take place; (4) with low cost, supply is convenient.
Plasma spraying because have jet temperature height, coat-thickness is controlled, bonding strength is high and characteristics such as easy to operate, is preparation B 4The effective ways of C coating.But, B 4There are problems such as high temperature oxidation and gasification in C in spraying process, air plasma spraying can not be prepared well behaved B 4The C coating.There is research to adopt a kind of extraordinary resist technology, under protection of inert gas, carries out plasma spraying, though obtained B 4The C coating, but still there is the small part oxidation products in the coating.Therefore need seeking more suitably, method prepares B 4The C ceramic coating of anti-the erosion.
Summary of the invention
The invention provides a kind of making method of boron carbide coating of abrasion resistant and corrosion resistant performance.
Concrete technical scheme is realized by following steps:
A kind of reaction and plasma spraying prepares the method for boron carbide coating, comprises the steps:
Step (1) is chosen boron carbide powder, and boron carbide powder is sent into plasma spraying equipment;
Step (2) is carried out pre-treatment to the substrate surface that is sprayed;
Step (3) is chosen Ar and CH 4For spraying gas, carry out plasma spraying by described plasma spraying equipment 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, in the described step (2) substrate surface that is sprayed is carried out pre-treatment, specifically comprise the steps: the substrate surface that is sprayed is carried out sandblasting, and clean with acetone.
In such scheme, the sand-blast material that described sandblasting is adopted is white fused alumina, and sand size is 50-100 μ m.
In such scheme, Ar flow 40-90L/min, CH 4Flow 5-20L/min.
In such scheme, the arc voltage 40-50V of described plasma spraying equipment, flame current 800-900A, powder feed rate 15-100g/min, spray distance 80-135mm, 50 °-90 ° of powder feeding angles.
The present invention uses methane gas (CH 4) replace hydrogen to spray as back work gas, have reducing property protection B after the methane gas ionization 4C is not oxidized, simultaneously because contain C in the gas, by itself and B 4The reaction of C can reduce even prevent B 4C C at high temperature runs off.The B that obtained performance is good 4The C coating.
Embodiment
Below in conjunction with embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Present embodiment provides a kind of gas-phase reaction plasma spraying to prepare the method for boron carbide coating, comprises the steps:
(1) selects B 4C powder, size range are 5-40 μ m, have splendid flowability.
(2) the etching technics cavity wall to aluminium base carries out sandblasting, and sand-blast material is white fused alumina, and size range is 50-100 μ m, and cleans with acetone.
(3) adopt Sluzer Metco 9MC plasma spraying equipment to carry out plasma spraying, spray gun type 9MB.The spraying atmosphere surrounding is Ar/CH 4: Ar flow 40-90L/min, CH 4Flow 5-20L/min.50 °-90 ° of arc voltage 40-50V, flame current 800-900A, powder feed rate 15-100g/min, spray distance 80-135mm, powder feeding angles.In spraying process, adopt air blowing method or recirculated water cooling method to cool off matrix.When adopting air blowing method cooling matrix, the flow of cooling gas is 100-2000L/min; When adopting recirculated water cooling method cooling matrix, the flow of water coolant is 10-500L/min.
The above only is preferred embodiment of the present invention, so all equivalences of doing according to the described structure of patent claim of the present invention, feature and principle change or modify, is included in the patent claim of the present invention.

Claims (6)

1. a reaction and plasma spraying prepares the method for boron carbide coating, it is characterized in that, comprises the steps:
Step (1) is chosen boron carbide powder, and boron carbide powder is sent into plasma spraying equipment;
Step (2) is carried out pre-treatment to the substrate surface that is sprayed;
Step (3) is chosen Ar and CH 4For spraying gas, carry out plasma spraying by described plasma spraying equipment at described substrate surface, prepare boron carbide coating.
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, in the described step (2) substrate surface that is sprayed is carried out pre-treatment, specifically comprises the steps: the substrate surface that is sprayed is carried out sandblasting, and cleans with acetone.
4. method according to claim 3 is characterized in that, the sand-blast material that described sandblasting is adopted is white fused alumina, and sand size is 50-100 μ m.
5. method according to claim 1 is characterized in that, described Ar flow 40-90L/min, described CH 4Flow 5-20L/min.
6. method according to claim 1 is characterized in that, the arc voltage 40-50V of described plasma spraying equipment, flame current 800-900A, powder feed rate 15-100g/min, spray distance 80-135mm, 50 °-90 ° of powder feeding angles.
CN201210002114.0A 2012-01-05 2012-01-05 A kind of reaction and plasma spraying is prepared the method for boron carbide coating Active CN103194716B (en)

Priority Applications (1)

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

Applications Claiming Priority (1)

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

Publications (2)

Publication Number Publication Date
CN103194716A true CN103194716A (en) 2013-07-10
CN103194716B CN103194716B (en) 2016-05-18

Family

ID=48717529

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210002114.0A Active CN103194716B (en) 2012-01-05 2012-01-05 A kind of reaction and plasma spraying is prepared the method for boron carbide coating

Country Status (1)

Country Link
CN (1) CN103194716B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711504A (en) * 2013-12-17 2015-06-17 中国科学院微电子研究所 Preparation method of boron carbide coating used for quartz substrate

Citations (1)

* Cited by examiner, † Cited by third party
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
曾毅 等: "等离子喷涂碳化硼涂层的性能研究", 《材料保护》, vol. 32, no. 4, 30 April 1999 (1999-04-30) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104711504A (en) * 2013-12-17 2015-06-17 中国科学院微电子研究所 Preparation method of boron carbide coating used for quartz substrate
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

Also Published As

Publication number Publication date
CN103194716B (en) 2016-05-18

Similar Documents

Publication Publication Date Title
Vardelle et al. The 2016 thermal spray roadmap
CN103194715B (en) Method for preparing amorphous Y3Al5O12 coating through atmospheric plasma spraying technology
WO2015151857A1 (en) Plasma-resistant component, method for manufacturing plasma-resistant component, and film deposition device used to manufacture plasma-resistant component
CN103074566A (en) Method for preparing Y3O3 coating by using supersonic plasma spraying technology
CN103194714B (en) A kind of method of Plasma Spray Boron Carbide Coating
WO2020207089A1 (en) Method for preparing y2o3 ceramic coating by supersonic flame spraying technology
CN102296263B (en) Modification treatment method for inner surface of plasma etching process chamber
CN112830814A (en) Method for coating copper or copper alloy on surface of aluminum nitride ceramic
CN100540511C (en) A kind of compound carbon resisting coating material and on matrix the preparation compound carbon resisting coating method
CN104357785A (en) Method for rapidly preparing high-purity yttrium oxide coating for plasma etching machine
CN103074563B (en) A kind of Y2O3The improved method of resistant to corrosion ceramic coating
CN103132007B (en) A kind of low-voltage plasma spraying technology prepares Y 2o 3the method of ceramic coating
CN103540889A (en) Method for preparing boron carbide coating through low-pressure plasma spraying technology
CN103194716A (en) Method for preparing boron carbide coating through reaction plasma spraying
CN103132003B (en) Black Y in a kind of semiconductor devices 2o 3ceramic coating manufacture method
CN103132002B (en) Preparation method of black yttrium oxide (Y2O3) ceramic coating
CN104711503B (en) A kind of boron carbide gradient coating applied to quartz substrate and preparation method thereof
CN105624602B (en) A kind of Y applied to aluminium base base material3Al5O12The preparation method of coating
CN103074564A (en) Method for preparing Y3O3 coating by using vacuum plasma spraying technology
CN110616397A (en) Preparation of Al/(Y) by atmospheric plasma spraying2O3-ZrO2) Method for composite coating
CN110578143A (en) Preparation of Al-ZrO by atmospheric plasma spraying2/Y2O3method for producing composite coating material
CN103132001B (en) Improvement method for preparing Y2O3 ceramic coating
CN103074568A (en) Preparation method of Y2O3 erosion-resistant ceramic coating
CN103074567A (en) Method for preparing Y3O3 coating by using water-stable plasma spraying technology
CN104711504B (en) A kind of preparation method of boron carbide coating applied to quartz substrate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

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

TR01 Transfer of patent right
TR01 Transfer of patent right

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.