CN108385082A - A method of depositing DLC protection films in accessory inner surface - Google Patents
A method of depositing DLC protection films in accessory inner surface Download PDFInfo
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- CN108385082A CN108385082A CN201611190578.3A CN201611190578A CN108385082A CN 108385082 A CN108385082 A CN 108385082A CN 201611190578 A CN201611190578 A CN 201611190578A CN 108385082 A CN108385082 A CN 108385082A
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- protection films
- microwave
- plasma
- depositing dlc
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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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical 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
- C23C16/26—Deposition of carbon only
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical 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
- C23C16/50—Chemical 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
- C23C16/511—Chemical 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 microwave 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 kind of methods depositing DLC protection films in accessory inner surface of the present invention; this method is based on Linear extended microwave plasma equipment and realizes coating process; the present invention, which proposes, introduces the new method that Linear extended microwave plasma plates protection film in part inner wall; this method can prepare uniform protection film in inner cavity of component; the protective film plated is fine and close, uniform, and adhesive strength is good；Plasma when the thinner inner surface of pipe fitting of internal diameter is handled has been well solved to be difficult to enter the problem in pipe fitting.
Description
Technical field
The present invention relates to field of surface technology, are a kind of sides depositing DLC protection films in accessory inner surface specifically
Method.
Background technology
The workpiece such as the earthen pipe of engine and the umbrella tooth internal splines of transmission portion are using its inner surface as groundwork
The invalidation period in face, inner surface decides the service life of whole part.Due to table in the factors pipe fitting such as burn into fretting wear
Face serious destruction frequent occurrence, causes these part lifes shorter, replaces frequent.And these parts due to diameter it is smaller（It is logical
Often less than 150mm）Using conventional method it is difficult to carry out anticorrosion and anti abrasive technique to it.Part inner working face is carried out
Protective treatment is that many companies and research institution have been devoted to solve the problems, such as, people ask to solve the abrasion of part inner wall
Topic also proposed many methods.It is directed to inner surface of pipe fitting modification at present, some scientific research institutions and university all do in the world
A large amount of research work, the method mainly used have plating, laser reinforcing processing, plasma surface modification etc..
Currently, the protection processing method of inner surface mainly has the methods of plating, laser reinforcing processing and plasma treatment.But
It is that there is deficiencies in performance for electroplated coating, and plating solution has serious pollution to environment, and laser reinforcing processing needs laser
Generator, equipment is huge, and cost is higher.Steel are to infrared energy simultaneously（Wavelength is 10.6 μm）Absorptivity it is very low, only
10% or so, the waste of energy is caused, therefore laser is only applicable in some special occasions, application is greatly limited.Gas
Body plasma discharging has very extensive application in terms of material surface modifying and processing, can generate various work(in piece surface
Energy film, can play the application of wear-and corrosion-resistant etc., and the plasma treatment master method to be applied of inner surface is empty at present
The methods of the heart-yin pole charging method, center auxiliary electrode and microwave ECR plasma source, since first two method has electric discharge not
Uniform defect, and microwave ECR plasma source needs externally-applied magnetic field processing that can not handle ferrimagnet.Therefore inner surface
Corona treatment is always the difficult point of surface modification treatment.
Linear extended microwave plasma be using between microwave and plasma interaction, generation and maintain plasma
A kind of device.In this device, it is 800 W by magnetron generation power, the microwave that frequency is 2.45 GHz.By waveguide
Pipe, circulator, power match load after, microwave by Waveguide coaxial mode converter, it is heavy to be coupled into from the both ends of equipment
Product room.On the axis of settling chamber, device has the coaxial line type transmitting antenna as microwave rf generator.In the outer of transmitting antenna
Side is equipped with quartz ampoule.After feed-in microwave energy, a plasma column for surrounding quartz ampoule can be generated within the deposition chamber,
By changing the microwave power of feed-in and the type and pressure of gas, the radius of plasma column can be adjusted.
Invention content
It is a kind of in accessory inner surface deposition DLC protection films the purpose of the present invention is overcoming the deficiencies of the prior art and provide
（The method of diamond-like carbon film-coating (Diamond-like carbon) solves the thinner inner surface of pipe fitting of pipe fitting, especially internal diameter
Plasma is difficult to enter the problem in pipe fitting when processing.
In order to solve the above technical problems, a kind of method depositing DLC protection films in accessory inner surface of the present invention, is based on line
Shape microwave plasma device realizes coating process, the described method comprises the following steps：
The inner surface of part is subjected to blast or polishing treatment, is cleaned 5 minutes with deionized water, is then placed in ultrasonic wave acetone
Cleaning.
More than one part is sleeved on to the quartz round tube periphery of built-in coaxial microwave antenna, when installation keeps in all parts
The heart is coaxial with quartz ampoule.All parts connect back bias voltage and insulate with chamber.
After electricity consumption blowing drying, it is put into vacuum chamber, is passed through argon gas, adjusts argon flow amount between 5 ~ 8sccm, gas
Voltage-controlled system opens gas ion source between 0.05 ~ 0.08Pa, and power setting is 200 ~ 300W, and it is clear to carry out argon ion bombardment
It washes, scavenging period controls between 30 ~ 60min.
C2H2 flows are adjusted to 100 ~ 150sccm, argon flow amount is adjusted to 100 ~ 200sccm, pressure control 0.1 ~
Between 0.2Pa, opening pulsed bias power supply, adjusting frequency values to 30k ~ 50kHz, duty ratio 30% ~ 50%, bias -50V ~ -
100V adjusts microwave power to 300W ~ 500W, in the inner wall coating diamond-like film of part.
Preferably, the acetone scavenging period is 60min.
Preferably, before icon bombardment cleaning, it is evacuated to 0.001 ~ 0.004Pa.
After adopting the above technical scheme, the present invention propose introduce Linear extended microwave plasma part inner wall plating protection it is thin
The new method of film, this method can prepare uniform protection film in inner cavity of component, and the protective film plated is fine and close, uniform, attached
It is good intensity.Plasma when the thinner inner surface of pipe fitting of internal diameter is handled has been well solved to be difficult to enter the problem in pipe fitting.
Description of the drawings
Fig. 1 is linear microwave source inner cavity plasma treatment appts structural schematic diagram in one embodiment of the invention；
Fig. 2 is the Cross Section Morphology testing result schematic diagram of inner surface DLC film；
Fig. 3 is the XPS testing result schematic diagrames after the swarming of inner surface DLC film.
Specific implementation mode
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.It is described below and is only used for solving
The present invention is released, is not intended to limit the present invention.
A kind of method depositing DLC protection films in accessory inner surface of the present invention, is based on Linear extended microwave plasma equipment
Realize that coating process, Fig. 1 are linear microwave source inner cavity plasma treatment appts structural schematic diagram in one embodiment of the invention.Line
Property microwave source inner cavity plasma treatment appts include vacuum chamber and vacuum pump 4, further include microwave and plasma generator, wherein
Quartz ampoule 6 etc. including the pulse power, built-in coaxial microwave antenna 5, vacuum chamber are equipped with gas outlet 3, air inlet 2, should also be equipped with
More than one part 7 need to be sleeved on the quartz round tube 6 of built-in coaxial microwave antenna 5 by the fixture 8 of retaining element 7 before starting plated film
Periphery, when installation, keep all Central of the parts and quartz ampoule 6 coaxial, and all parts connect back bias voltage and insulate with chamber.First with
The electric discharge of microwave excitation working gas generates the plasma of circular tube shaped, then profit around the quartz round tube of built-in coaxial microwave antenna
With plasma chemical vapor deposition technique internal spline inner wall coating diamond-like film.The present invention is based on the productions of linear microwave source
Life can generate the characteristics of annular ion column, and the quartz ampoule equipped with transmitting antenna is penetrated and is fixed on deposit cavity by cantilever fixture
In pipe-shaped parts among, as gas ionization source, the reaction gas of within the deposition chamber is ionized into plasma, surround quartz ampoule
Around, then by applying back bias voltage to part, ion can be made to deposit on part inner wall and reacted to generate phase
The protective film answered, to play wear-resisting or corrosion resistant function.
Below with reference to one embodiment to a kind of side depositing DLC protection films in accessory inner surface of the present invention
Method is further described：
Embodiment 1：Certain inner spline parts
1）The polished and cleaned of part
Internal spline inner surface is subjected to blast or polishing treatment, is cleaned 5 minutes with deionized water, is then placed in ultrasonic wave acetone
After cleaning 60min.
2）Part is loaded
Internal spline is installed by state as shown in Figure 1, part and quartz ampoule are coaxial when installation.Part connects back bias voltage and and chamber
It insulate room.
3）Ion Cleaning
After electricity consumption blowing drying, be put into vacuum chamber, be evacuated to 0.001 ~ 0.004Pa, be passed through argon gas, adjust argon flow amount 5 ~
Between 8sccm, pressure control opens gas ion source between 0.05 ~ 0.08Pa, and power setting is 200 ~ 300W, is carried out
Argon ion bombardment cleans, and scavenging period controls between 30 ~ 60min.
3）Depositing Ti layer is as transition zone
Adjust TiCl3Flow is to 100 ~ 150sccm, and argon flow amount is adjusted to 100 ~ 200sccm, and pressure control is in 0.1 ~ 0.2Pa
Between, pulsed bias power supply is opened, adjusts frequency values to 30k ~ 50kHz, duty ratio 30% ~ 50%, bias -50V ~ -100V, tune
Microwave power is saved to 300W ~ 500W, carries out Ti layers of deposition, total sedimentation time 2 hours.
4）Deposit DLC
Adjust C2H2For flow to 100 ~ 150sccm, argon flow amount is adjusted to 100 ~ 200sccm, pressure control 0.1 ~ 0.2Pa it
Between, pulsed bias power supply 9 is opened, adjusts frequency values to 30k ~ 50kHz, duty ratio 30% ~ 50%, bias -50V ~ -100V, adjusting
Microwave power carries out DLC layer deposition, total sedimentation time 3 hours to 300W ~ 500W.
It is as Figure 2-3 to the detection result of sample after the completion of the embodiment, SP in Fig. 33Content 30%.
The coating performance index is ideal it can be seen from inspection result.
It these are only preferred embodiments of the present invention, do not constitute any limitation of the invention, all essences in the present invention
Any modification, improvement and the equivalent replacement etc. made in refreshing and principle, should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of method depositing DLC protection films in accessory inner surface, which is characterized in that set based on Linear extended microwave plasma
It is standby to realize coating process, it the described method comprises the following steps：
The inner surface of part is subjected to blast or polishing treatment, is cleaned 5 minutes with deionized water, is then placed in ultrasonic wave acetone
Cleaning；
More than one part is sleeved on to the quartz round tube periphery of built-in coaxial microwave antenna, when installation keep all Central of the parts with
Quartz ampoule is coaxial, and all parts connect back bias voltage and insulate with chamber；
Part is put into vacuum chamber, is passed through argon gas, adjusts argon flow amount between 5 ~ 8sccm, pressure control 0.05 ~
Between 0.08Pa, gas ion source is opened, power setting is 200 ~ 300W, carries out argon ion bombardment cleaning, scavenging period control
System is between 30 ~ 60min；
C2H2 flows are adjusted to 100 ~ 150sccm, argon flow amount is adjusted to 100 ~ 200sccm, pressure control 0.1 ~ 0.2Pa it
Between, pulsed bias power supply is opened, adjusts frequency values to 30k ~ 50kHz, duty ratio 30% ~ 50%, bias -50V ~ -100V, adjusting
Microwave power is to 300W ~ 500W, in the inner wall coating diamond-like film of part.
2. the method for depositing DLC protection films in accessory inner surface according to claim 1, which is characterized in that the acetone
Scavenging period is 60min.
3. the method for depositing DLC protection films in accessory inner surface according to claim 1, which is characterized in that banged in ion
Before hitting cleaning, it is evacuated to 0.001 ~ 0.004Pa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190578.3A CN108385082A (en) | 2016-12-21 | 2016-12-21 | A method of depositing DLC protection films in accessory inner surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190578.3A CN108385082A (en) | 2016-12-21 | 2016-12-21 | A method of depositing DLC protection films in accessory inner surface |
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| Publication Number | Publication Date |
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| CN108385082A true CN108385082A (en) | 2018-08-10 |
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| CN201611190578.3A Pending CN108385082A (en) | 2016-12-21 | 2016-12-21 | A method of depositing DLC protection films in accessory inner surface |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109302791A (en) * | 2018-10-26 | 2019-02-01 | 中国科学院合肥物质科学研究院 | Microwave antenna, which regulates and controls magnetic, enhances linear plasma source generation system |
| CN110512195A (en) * | 2019-09-20 | 2019-11-29 | 武汉工程大学 | A kind of tubular material inner surface carries out the method and device of MPCVD |
| CN114293144A (en) * | 2022-01-12 | 2022-04-08 | 松山湖材料实验室 | Cutter coating process and equipment |
| CN114334589A (en) * | 2021-11-26 | 2022-04-12 | 北京大学 | Miniature 2.45GHzECR electron source and electron cyclotron resonance electron source system |
| CN114855143A (en) * | 2022-05-10 | 2022-08-05 | 西南石油大学 | Solid film coating for oil pump plunger |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037768A (en) * | 2007-04-10 | 2007-09-19 | 武汉工程大学 | Method and device for plating diamond like film on inner-outer wall of quartz round tube |
| CN102358940A (en) * | 2011-10-12 | 2012-02-22 | 湖北久之洋红外系统有限公司 | Method for depositing anti-corrosion diamond-like film on object substrate |
-
2016
- 2016-12-21 CN CN201611190578.3A patent/CN108385082A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037768A (en) * | 2007-04-10 | 2007-09-19 | 武汉工程大学 | Method and device for plating diamond like film on inner-outer wall of quartz round tube |
| CN102358940A (en) * | 2011-10-12 | 2012-02-22 | 湖北久之洋红外系统有限公司 | Method for depositing anti-corrosion diamond-like film on object substrate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109302791A (en) * | 2018-10-26 | 2019-02-01 | 中国科学院合肥物质科学研究院 | Microwave antenna, which regulates and controls magnetic, enhances linear plasma source generation system |
| CN109302791B (en) * | 2018-10-26 | 2023-08-22 | 中国科学院合肥物质科学研究院 | Microwave antenna regulation and control magnetic enhancement linear plasma source generation system |
| CN110512195A (en) * | 2019-09-20 | 2019-11-29 | 武汉工程大学 | A kind of tubular material inner surface carries out the method and device of MPCVD |
| CN114334589A (en) * | 2021-11-26 | 2022-04-12 | 北京大学 | Miniature 2.45GHzECR electron source and electron cyclotron resonance electron source system |
| CN114293144A (en) * | 2022-01-12 | 2022-04-08 | 松山湖材料实验室 | Cutter coating process and equipment |
| CN114855143A (en) * | 2022-05-10 | 2022-08-05 | 西南石油大学 | Solid film coating for oil pump plunger |
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Application publication date: 20180810 |