CN106498344B - A kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film - Google Patents

A kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film Download PDF

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CN106498344B
CN106498344B CN201610894584.0A CN201610894584A CN106498344B CN 106498344 B CN106498344 B CN 106498344B CN 201610894584 A CN201610894584 A CN 201610894584A CN 106498344 B CN106498344 B CN 106498344B
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carbon
argon gas
film
sputtering
power supply
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CN106498344A (en
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郝俊英
韩�熙
郑建云
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

Abstract

The invention discloses a kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film, the specific steps are：Plasma sputtering cleaning is carried out to monocrystalline silicon piece and stainless steel thin slice；Transition zone deposits, using multifunction composite magnetic controlled sputtering sputtering equipment, within the deposition chamber initial temperature is 25 ~ 35 DEG C, and target is set as 7 ~ 14 cm with substrate spacing, using high-purity titanium target, it is passed through sputter gas argon gas, argon gas/nitrogen and argon gas/methane/nitrogen successively, opens DC power supply, is 0.2 ~ 1.0 Pa in operating pressure, 2.0 ~ 4.0 A of electric current, substrate bias is 100 V, under conditions of duty ratio is 80%, sputters Ti, TiN, TiCN multilayer film successively as transition zone；Argon gas and nitrogen are closed, methane is retained, closes DC power supply, opens radio-frequency power supply, is 20 ~ 40 W in power, operating pressure is 2.5 ~ 3.5 Pa, and substrate bias is 1000 ~ 1200 V, sputtering target material Ti, Al or Si, the carbon-base film of deposition single-element doping.Membrane structure prepared by the present invention is fine and close, surface roughness is low, has lower friction coefficient in atmospheric environment.

Description

A kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film
Technical field
The invention belongs to technology of thin film material preparation fields, are related to one kind in room temperature（Without any extra heat source）With no benzene The method that excellent toughness and nanometer carbon/agraphitic carbon composite film material of lubrication are prepared under ring organic reagent.
Background technology
Carbon material plays important function in the development of human history, even to this day, excellent physics and chemically Matter still attracts the attention of researcher.In various carbon materials, agraphitic carbon is by sp of the carbon without grain boundary3With sp2The arbitrary covalent networks structure of hydridization site composition.Numerous studies are it has been shown that agraphitic carbon can be used as solid lubrication material Material, for fields such as space flight and aviation, machine-building.Heterogeneous element is adulterated in amorphous carbon-base film（Ti, Si, Al etc.）It can change It is apt to its comprehensive performance.Therefore, in order to obtain ultra-low friction and improve its tribology adaptability under severe service condition, accelerate Its practicalization, researcher have been carried out numerous studies to heterogeneous element doping agraphitic carbon base film.In addition, as carbon materials One of important composition of material, carbon nanotube have the elasticity modulus of superelevation（About 1 TPa）With extraordinary tensile strength（20~100 Within the scope of GPa）.In existing report, the block materials of carbon nanotube toughness enhancing show outstanding Resisting fractre behavior. But due to large volume fraction, interfacial reaction and alignment problem, the film of carbon nanotube toughness enhancing so far can not be real It is existing.Basic component units of the carbon nano ring as carbon nanotube have property similar with carbon nanotube.Compared with carbon nanotube For, carbon nano ring has smaller volume and simple structure, is expected to show its unique engineering properties in involvement film.
Although carbon nano ring has simple structure, its synthesis is still a huge challenge.In numerous studies Under the effort of work, has part scientific research personnel and the chemical synthesis process with innovative significance is used to prepare carbon nano ring. It should be noted that in these methods, the synthesis of carbon nano ring is directed to the organic chemical reagent containing phenyl ring（Such as hexamethylene two Alkene）, and the use of these reagents finally will produce some by-products of pollution environment.Therefore, develop a kind of no organic examination of phenyl ring The synthetic method of agent is very necessary, it can be effectively facilitated the development and application of carbon nano ring.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of elastic lubrication nanometer carbon/agraphitic carbon laminated film.
The present invention uses CH4The method of plasma self assembly, by forcing band under conditions of higher pressure and bias The C of chargexHy n+Between mutually collide, form the phenyl ring of electrification（C6Hz n+）.And when the phenyl ring of two electrifications is in plasma It meets in group, series connection Suzuki couplings/big cyclization sequence reaction will occur.This reaction will be with other electrically charged phenyl ring It is added and sustained response, until the generation of carbon nano ring.Meanwhile in this process, most of C for not participating in cyclizationxHy n+Directly It connects and is converted to agraphitic carbon.Nanometer carbon prepared by the present invention/agraphitic carbon complex thin film structure is fine and close, and surface is smooth, tool There are good elasticity and greasy property.
A kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film, it is characterised in that adopt at room temperature With multifunction composite magnetic controlled sputtering equipment, utilize CH4Plasma self-assembling technique prepares nanometer carbon/agraphitic carbon THIN COMPOSITE Film, concrete operation step are as follows：
1）It is cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with absolute ethyl alcohol and acetone, drying process is placed on settling chamber It is interior, it is evacuated to 3 × 10-3 Pa is hereinafter, using argon gas as sputter gas, pulsed bias is -1100 V, pressure is 1.0 ~ 2.0 The plasma sputtering cleaning of 20 ~ 30 min is carried out under conditions of Pa；
2）Transition zone deposits, and within the deposition chamber initial temperature is 25 ~ 35 DEG C, and target is set as 7 ~ 14 cm with substrate spacing, Using high-purity titanium target, it is passed through sputter gas argon gas, argon gas/nitrogen and argon gas/methane/nitrogen successively, opens DC power supply, Operating pressure is 0.2 ~ 1.0 Pa, and 2.0 ~ 4.0 A of electric current, substrate bias is -100 V, under conditions of duty ratio is 80 %, according to Secondary sputtering Ti, TiN, TiCN multilayer film is as transition zone, 15 ~ 20 min of sputtering time；
3）Argon gas and nitrogen are closed, retains methane as sputter gas, closes DC power supply, radio-frequency power supply is opened, in work( Rate be 20 ~ 40 W, operating pressure be 2.5 ~ 3.5 Pa, substrate bias be -1000 ~ -1200 V, sputtering target material Ti, Al or Si, The carbon-base film of single-element doping is deposited, after 3.0 ~ 3.5 h, deposition, within the deposition chamber temperature is not higher than sedimentation time 90 ℃。
The thickness of the transition zone is 1.0 ± 0.2 μm；The thickness of carbon-base film is 1.0 ± 0.3 μm, laminated film Overall thickness is 2.0 ± 0.3 μm.
Elastic lubrication nanometer carbon prepared by the present invention/agraphitic carbon laminated film has the following structure and performance：
1, the elastic lubrication nanometer carbon/agraphitic carbon laminated film mainly consists of two parts：Thickness be 1.0 ± The carbon-base film that 0.2 μm of Ti/TiN/TiCN multilayer transition layers and thickness is 1.0 ± 0.3 μm；
2, the compact structure of the film and substrate are firmly combined with, surface roughness is less than 1.5 nm, elastic restoration ratio （W e ）More than 65 %；
3, the film has excellent tribological property in atmospheric environment, and friction coefficient is down to 0.028, wear rate Less than 4 × 10-7 mm3/（Nm）.
Nanometer carbon/agraphitic carbon laminated film prepared by the present invention has the advantages that the reason of above is：It is depositing Higher pressure makes intermolecular distance reduce in the process, and plasma and molecular collision probability are significantly increased, the work of film forming Property ion increase so that film growth rate increase, and caused by the reduction of ion energy makes high-energy ion bombardment etch rate drop Low, therefore, film has higher deposition rate；Apply high back bias voltage to substrate, improve atom film surface diffusion and The ability for participating in chemical reaction, improves the consistency and film forming ability of film；Meanwhile being self-assembly of in deposition process Nanometer carbon has excellent toughness and very weak shear strength, and incorporating can be with the toughness and tribology of enhanced film in film Energy.
Description of the drawings
Fig. 1 is the transmission electron microscope and its enlarged drawing of laminated film described in the embodiment of the present invention 1.
Fig. 2 is laminated film Raman collection of illustrative plates described in the embodiment of the present invention 1.
Fig. 3 is the displacement-load curves figure of laminated film described in the embodiment of the present invention 2.
Fig. 4 is the aerial friction coefficient curve of laminated film described in the embodiment of the present invention 3.
Specific implementation mode
For a better understanding of the present invention, it is further illustrated the present invention in conjunction with following embodiments.
Embodiment 1
Clean substrate：It is cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with absolute ethyl alcohol and acetone soln, after drying process It is positioned within the deposition chamber.Deposit pre-treatment：It is evacuated to 2 × 10-3 Pa is 80 in duty ratio hereinafter, using argon gas as sputter gas %, pulsed bias carries out plasma sputtering to substrate under conditions of being -1100 V and cleans 20 min, to remove surface oxide layer And impurity.Deposition：Using high-purity titanium target, it is passed through sputter gas argon gas, argon gas+nitrogen and argon gas+nitrogen+methane successively, opens DC power supply is opened, is 0.4 ~ 1.0 Pa, 2 A of DC current, -100 V of substrate bias in operating pressure, duty ratio is the item of 80 % Multilayer transition layer Ti/TiN/TiCN is deposited under part, transition zone sedimentation time is 15 min.After transition zone deposits, argon is closed Gas and nitrogen retain methane as sputter gas, close DC power supply, opens radio-frequency power supply, and power setting is 20 W, is being worked Pressure is 3.0 Pa, and substrate bias is -1100 V, and duty ratio carries out the heavy of the carbon-base film of Ti doping under conditions of being 80 % Product, sedimentation time are 3.2 h, obtain a series of nanometer carbon/agraphitic carbon laminated film.
The section of laminated film and surface are observed using field emission scanning electron microscope, film thickness（Including mistake Cross layer）It it is 1.7 μm, surface is smooth, compact structure.Its transmission electron microscope image and its enlarged drawing are as shown in Figure 1, multiple It closes film and shows typical undefined structure, the presence of some cyclic structures can be obviously observed in its enlarged drawing. The Raman collection of illustrative plates of laminated film is as shown in Fig. 2, the characteristic peak of carbon nano ring and agraphitic carbon is clearly present in such film.It is former It is 1.051 nm that sub- force microscope, which measures laminated film surface roughness,.Nano-indentation experiment is the result shows that its hardness（H）And bullet Property modulus（E）Respectively 10.04 and 89.0 GPa, elastic restoration ratio（W e ）For 66.0 %.It is such thin in air friction testing The average friction coefficient 0.028 of film, wear rate are 3.5 × 10-7 mm3/（Nm）.
Embodiment 2
As described in Example 1, radio-frequency power is adjusted to 40 W in carbon layer deposition.
Film sections and surface are observed using field emission scanning electron microscope, thickness is 2.07 μm, surface is smooth, Compact structure.Raman results show that laminated film has the characteristic peak of carbon nano ring and agraphitic carbon.Utilize atomic force microscope It is 0.389 nm to measure roughness of film.According to nano-indentation experiment as a result, the consistency and elasticity mould of gained laminated film Amount is respectively 11.36 and 87.8 GPa, elastic restoration ratio（W e ）For 69.0 %, displacement-load curves are as shown in Figure 3.Big Gas rubs in test, and the average friction coefficient of such laminated film is 0.048, and wear rate is 7.32 × 10-7 mm3/（Nm）.
Embodiment 3
As described in Example 1, sputtering target material is changed to silicon target by titanium target after depositing transition zone, opens radio-frequency power supply, work( Rate is adjusted to 20 W, prepares a series of carbon-base film of Si doping.
Film sections and surface to be observed with field emission scanning electron microscope, laminated film thickness is 2.0 μm, Surface is smooth, compact structure.It is 0.261 nm to measure roughness of film using atomic force microscope.Raman collection of illustrative plates shows, Laminated film has the characteristic peak of carbon nano ring and agraphitic carbon.In air friction testing, such laminated film average friction Coefficient is 0.03, and wear rate is 2.04 × 10-7 mm3/（Nm）, the aerial friction coefficient curve of film is as shown in Figure 4.

Claims (2)

1. a kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film, it is characterised in that use at room temperature Multifunction composite magnetic controlled sputtering equipment utilizes CH4Plasma self-assembling technique prepares nanometer carbon/agraphitic carbon THIN COMPOSITE Film, concrete operation step are as follows：
1）It is cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with absolute ethyl alcohol and acetone, drying process is placed within the deposition chamber, takes out Vacuum is to 3 × 10-3 Pa is hereinafter, using argon gas as sputter gas, in the item that pulsed bias is -1100 V, pressure is 1.0 ~ 2.0 Pa The plasma sputtering cleaning of 20 ~ 30 min is carried out under part；
2）Transition zone deposits, and within the deposition chamber initial temperature is 25 ~ 35 DEG C, and target is set as 7 ~ 14 cm with substrate spacing, is used High-purity titanium target is passed through sputter gas argon gas, argon gas/nitrogen and argon gas/methane/nitrogen successively, opens DC power supply, is working Pressure is 0.2 ~ 1.0 Pa, and 2.0 ~ 4.0 A of electric current, substrate bias is that -100 V splash successively under conditions of duty ratio is 80 % Ti, TiN, TiCN multilayer film are penetrated as transition zone, 15 ~ 20 min of sputtering time；
3）Argon gas and nitrogen are closed, retains methane as sputter gas, closes DC power supply, open radio-frequency power supply, be in power 20 ~ 40 W, operating pressure are 2.5 ~ 3.5 Pa, and substrate bias is -1000 ~ -1200 V, sputtering target material Ti, Al or Si, deposition The carbon-base film of single-element doping, for sedimentation time after 3.0 ~ 3.5 h, deposition, within the deposition chamber temperature is not higher than 90 ℃。
2. preparation method as described in claim 1, it is characterised in that the thickness of the transition zone is 1.0 ± 0.2 μm；It is carbon-based The thickness of film is 1.0 ± 0.3 μm, and the overall thickness of laminated film is 2.0 ± 0.3 μm.
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CN109423612A (en) * 2017-08-31 2019-03-05 南京理工大学 Wear-resisting hydrophobic carbon-based laminated film, preparation method and applications
CN108517499B (en) * 2018-03-28 2019-12-27 中国科学院兰州化学物理研究所 Lubricating/conductive double-function NbSe2Low-temperature preparation method of film

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