CN104372304A - Diamond-like carbon film preparation process - Google Patents

Diamond-like carbon film preparation process Download PDF

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Publication number
CN104372304A
CN104372304A CN201410702591.7A CN201410702591A CN104372304A CN 104372304 A CN104372304 A CN 104372304A CN 201410702591 A CN201410702591 A CN 201410702591A CN 104372304 A CN104372304 A CN 104372304A
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CN
China
Prior art keywords
vacuum chamber
substrate
vacuum
diamond
preparation technology
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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.)
Pending
Application number
CN201410702591.7A
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Chinese (zh)
Inventor
李俊
梁天也
李斌商
李徐兵
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ANHUI WEIWEI VEHICLE RUBBER Co Ltd
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ANHUI WEIWEI VEHICLE RUBBER Co Ltd
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Application filed by ANHUI WEIWEI VEHICLE RUBBER Co Ltd filed Critical ANHUI WEIWEI VEHICLE RUBBER Co Ltd
Priority to CN201410702591.7A priority Critical patent/CN104372304A/en
Publication of CN104372304A publication Critical patent/CN104372304A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26Deposition of carbon only
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02Pretreatment of the material to be coated
    • C23C16/0227Pretreatment of the material to be coated by cleaning or etching
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4407Cleaning of reactor or reactor parts by using wet or mechanical methods
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
    • C23C16/505Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using radio frequency discharges

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Vapour Deposition (AREA)

Abstract

The invention discloses a diamond-like carbon film preparation process. Pretreatment of the preparation process includes the steps: (1) vacuum chamber pretreatment: before a substrate is put in a vacuum chamber, using a dust collector to suck dust and attachments of the vacuum chamber, putting on disposable gloves, and using absolute ethyl alcohol and medical gauze to wipe a sample stage and inner walls of the vacuum chamber; (2) substrate pretreatment: taking part of alcohol and diethyl ether to uniformly mix in a small dropping bottle according to a certain proportion, and taking petroleum ether in a certain quantity to put into another small dropping bottle; dripping alcohol and diethyl ether mixed solution for cleaning a Si substrate, and after cleaning is finished, using petroleum ether to clean the substrate again.

Description

A kind of diamond like carbon film preparation technology
Technical field
The invention belongs to automobile rubber film applications, more particularly, the present invention relates to a kind of diamond like carbon film preparation technology.
Background technology
Quasi-diamond (DLC) film is a kind of amorphous carbon-film; it is high that it has hardness; infrared region is transparent; high-wearing feature, low-friction coefficient, high heat conductance, high resistivity, high chemical stability and specific refractory power can between 1.7 to 2.3 a series of excellent properties such as adjustable; compared with there is the diamond thin of same excellent properties; the cost performance of diamond like carbon film is higher, depositing temperature is low, depositional area is large, face flat smooth, is the ideal material of the desirable anti-reflection protective film of large-scale infrared window.Since utilizing carbon ion and argon ion to prepare diamond like carbon film first in vacuum system from 1971, it is as new function thin-film material, not only there is huge application prospect at optical field, and having tempting development and application space too as automobile mechanical wear-resistant coating, microelectromechanical-systems and semiconductor applications, receive the concern of many researchists.
Summary of the invention
Problem to be solved by this invention is to provide one and has high rigidity, high elastic coefficient, low, the anti abrasive diamond like carbon film preparation technology of frictional coefficient.
To achieve these goals, the technical scheme that the present invention takes is: a kind of diamond like carbon film preparation technology, the pre-treatment of described preparation technology, comprises the steps:
(1) vacuum chamber pre-treatment: before substrate is put into vacuum chamber, first with the suction cleaner exhaustion dust of vacuum chamber and dirt settling, then brings disposable gloves, and by dehydrated alcohol and hospital gauze wiping vacuum chamber inwall and sample table.
(2) substrate pre-treatment: get a part of alcohol and mix in small droplet bottles according to certain proportioning with ether, gets a certain amount of sherwood oil in another small droplet bottles; Fine-still alcohol and ether mixing solutions clean Si substrate, after having cleaned, more again clean substrate with sherwood oil; After having cleaned, with rubber pipette bulb, substrate is dried up, then put in the sample table of the vacuum chamber processed fast, close vacuum chamber.
Preferably, its preparation technology's concrete steps are as follows:
(1) by the sample table that is put into through pretreated sample in vacuum chamber.
(2) close vacuum room cover, open vacuum system, vacuumize the vacuum tightness being extracted into needs.
(3) drive flow director, be filled with argon gas, pressure in vacuum tank is adjusted to the pressure of needs, then opens radio-frequency power supply, produce glow discharge, substrate is cleaned, remove the adsorption particle of substrate surface further.
(4) drive flow director, be filled with reactant gases according to design requirements ratio, then set deposition pressure.
(5) open radio-frequency power supply, carry out plated film work, until complete technological process.
(6) vacuum chamber is exitted.
(7) sample processed is taken out.
Preferably, in described step (3) cleaning process, background vacuum is 3 × 10 -3,radio frequency power is 860W, and cleaning pressure is 2Pa, and scavenging period is 200S, Ar is 30sccm.
Beneficial effect: this diamond like carbon film preparation technology reactant gases employing purity is the normal butane (C of 99.9% 4h 10) and 99.999% argon gas (Ar), owing to being conducive to the growth of graphite-phase under high-temperature condition, substrate is not toasted in the process preparing sample, in experimentation, bottom crown is connected with water coolant, making the temperature of substrate when being subject to plasma bombardment also can not be too high, using RF-PECVD to prepare DLC film and there is the advantages such as thickness is even, production efficiency is high, sedimentation rate is high, stability, repeatability, adjustability are good.
Embodiment
The invention provides a kind of diamond like carbon film preparation technology, for realizing object of the present invention, technical scheme of the present invention is as follows: a kind of diamond like carbon film preparation technology, the pre-treatment of described preparation technology, comprise the steps: (1) vacuum chamber pre-treatment: before substrate is put into vacuum chamber, first with the suction cleaner exhaustion dust of vacuum chamber and dirt settling, then bring disposable gloves, and by dehydrated alcohol and hospital gauze wiping vacuum chamber inwall and sample table.(2) substrate pre-treatment: get a part of alcohol and mix in small droplet bottles according to certain proportioning with ether, gets a certain amount of sherwood oil in another small droplet bottles; Fine-still alcohol and ether mixing solutions clean Si substrate, after having cleaned, more again clean substrate with sherwood oil; After having cleaned, with rubber pipette bulb, substrate is dried up, then put in the sample table of the vacuum chamber processed fast, close vacuum chamber.Its preparation technology's concrete steps are as follows: (1) is by the sample table that is put into through pretreated sample in vacuum chamber.2) close vacuum room cover, open vacuum system, vacuumize the vacuum tightness being extracted into needs.(3) drive flow director, be filled with argon gas, pressure in vacuum tank is adjusted to the pressure of needs, then opens radio-frequency power supply, produce glow discharge, substrate is cleaned, remove the adsorption particle of substrate surface further.(4) drive flow director, be filled with reactant gases according to design requirements ratio, then set deposition pressure.(5) open radio-frequency power supply, carry out plated film work, until complete technological process.(6) vacuum chamber is exitted.(7) take out the sample processed, in described step (3) cleaning process, background vacuum is 3 × 10 -3,radio frequency power is 860W, and cleaning pressure is 2Pa, and scavenging period is 200S, Ar is 30sccm.
After above art breading, this diamond like carbon film preparation technology reactant gases employing purity is the normal butane (C of 99.9% 4h 10) and 99.999% argon gas (Ar), owing to being conducive to the growth of graphite-phase under high-temperature condition, substrate is not toasted in the process preparing sample, in experimentation, bottom crown is connected with water coolant, making the temperature of substrate when being subject to plasma bombardment also can not be too high, using RF-PECVD to prepare DLC film and there is the advantages such as thickness is even, production efficiency is high, sedimentation rate is high, stability, repeatability, adjustability are good.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize specification sheets of the present invention and embodiment content to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.

Claims (3)

1. a diamond like carbon film preparation technology, is characterized in that, the pre-treatment of described preparation technology, comprises the steps:
(1) vacuum chamber pre-treatment: before substrate is put into vacuum chamber, first with the suction cleaner exhaustion dust of vacuum chamber and dirt settling, then brings disposable gloves, and by dehydrated alcohol and hospital gauze wiping vacuum chamber inwall and sample table;
(2) substrate pre-treatment: get a part of alcohol and mix in small droplet bottles according to certain proportioning with ether, gets a certain amount of sherwood oil in another small droplet bottles; Fine-still alcohol and ether mixing solutions clean Si substrate, after having cleaned, more again clean substrate with sherwood oil; After having cleaned, with rubber pipette bulb, substrate is dried up, then put in the sample table of the vacuum chamber processed fast, close vacuum chamber.
2. according to a kind of diamond like carbon film preparation technology according to claim 1, it is characterized in that: its preparation technology's concrete steps are as follows:
(1) by the sample table that is put into through pretreated sample in vacuum chamber;
(2) close vacuum room cover, open vacuum system, vacuumize the vacuum tightness being extracted into needs;
(3) drive flow director, be filled with argon gas, pressure in vacuum tank is adjusted to the pressure of needs, then opens radio-frequency power supply, produce glow discharge, substrate is cleaned, remove the adsorption particle of substrate surface further;
(4) drive flow director, be filled with reactant gases according to design requirements ratio, then set deposition pressure;
(5) open radio-frequency power supply, carry out plated film work, until complete technological process;
(6) vacuum chamber is exitted;
(7) sample processed is taken out.
3. according to a kind of diamond like carbon film preparation technology according to claim 2, it is characterized in that: in described step (3) cleaning process, background vacuum is 3 × 10 -3,radio frequency power is 860W, and cleaning pressure is 2Pa, and scavenging period is 200S, Ar is 30sccm.
CN201410702591.7A 2014-11-29 2014-11-29 Diamond-like carbon film preparation process Pending CN104372304A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410702591.7A CN104372304A (en) 2014-11-29 2014-11-29 Diamond-like carbon film preparation process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410702591.7A CN104372304A (en) 2014-11-29 2014-11-29 Diamond-like carbon film preparation process

Publications (1)

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CN104372304A true CN104372304A (en) 2015-02-25

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108459361A (en) * 2018-04-12 2018-08-28 无锡奥夫特光学技术有限公司 A kind of infrared optical window and preparation method thereof
CN108962730A (en) * 2018-07-11 2018-12-07 无锡奥夫特光学技术有限公司 A kind of preparation method of infrared optical window
CN112951707A (en) * 2019-12-11 2021-06-11 株洲中车时代电气股份有限公司 Film and preparation method and application thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈林林: "类金刚石薄膜制备工艺与特性研究", 《中国优秀硕士学位论文全文数据库 基础科学辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108459361A (en) * 2018-04-12 2018-08-28 无锡奥夫特光学技术有限公司 A kind of infrared optical window and preparation method thereof
CN108962730A (en) * 2018-07-11 2018-12-07 无锡奥夫特光学技术有限公司 A kind of preparation method of infrared optical window
CN112951707A (en) * 2019-12-11 2021-06-11 株洲中车时代电气股份有限公司 Film and preparation method and application thereof

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Application publication date: 20150225