CN106498344A - 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 PDFInfo
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- CN106498344A CN106498344A CN201610894584.0A CN201610894584A CN106498344A CN 106498344 A CN106498344 A CN 106498344A CN 201610894584 A CN201610894584 A CN 201610894584A CN 106498344 A CN106498344 A CN 106498344A
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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
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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
- C23C14/02—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
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
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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
- C23C14/22—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
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Abstract
The invention discloses a kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film, concretely comprises the following steps:Plasma sputtering cleaning is carried out to monocrystalline silicon piece and stainless steel thin slice;Transition zone is deposited, using multifunction composite magnetic controlled sputtering sputtering equipment, the indoor initial temperature of deposition is 25 ~ 35 DEG C, and target is set to 7 ~ 14 cm with basal spacing, using high-purity titanium target, it is passed through sputter gas argon, argon/nitrogen and argon/methane/nitrogen successively, opens DC source, is 0.2 ~ 1.0 Pa in operating pressure, 2.0 ~ 4.0 A of electric current, substrate bias are 100 V, and under conditions of dutycycle is 80 %, sputtering Ti, TiN, TiCN multilayer film is used as transition zone successively;Argon and nitrogen is closed, retains methane, close DC source, open radio-frequency power supply, be 20 ~ 40 W in power, operating pressure is 2.5 ~ 3.5 Pa, and substrate bias are 1000 ~ 1200 V, and sputtering target material is Ti, Al or Si, deposits the carbon-base film of single-element doping.The membrane structure densification of present invention preparation, surface roughness are low, and there is in atmospheric environment relatively low coefficient of friction.
Description
Technical field
The invention belongs to technology of thin film material preparation field, is related to one kind in room temperature(Without the need for any extra heat source)With without benzene
The method for preparing the nanometer carbon/agraphitic carbon composite film material of excellent toughness and lubrication under ring organic reagent.
Background technology
Material with carbon element serves important function in the development of human history, even to this day, its excellent physics and chemical
Matter still attracts the attention of researcher.In various material with carbon elements, agraphitic carbon is the sp by carbon without grain boundary3With
sp2Any 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.Adulterate in amorphous carbon-base film heterogeneous element(Ti, Si, Al etc.)Can change
It is apt to its combination property.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.Additionally, as carbon materials
One of important composition of material, CNT, the elastic modelling quantity for having superelevation(About 1 TPa)With extraordinary tensile strength(20~100
In the range of GPa).In existing report, the enhanced block materials of CNT toughness show outstanding Resisting fractre behavior.
But, due to large volume fraction, interfacial reaction and alignment problem, the enhanced thin film of CNT toughness so far cannot be real
Existing.Basic component units of the carbon nano ring as CNT, with the property similar to CNT.Compared with CNT
For, carbon nano ring has less volume and simple structure, is expected to incorporate the engineering propertiess for showing in thin film which is unique.
Although carbon nano ring has simple structure, its synthesis remains a huge challenge.In numerous studies
Under the effort of work, existing part scientific research personnel has prepared carbon nano ring using the chemical synthesis process with innovative significance.
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 eventually produces some by-products of pollution environment.Therefore, develop one kind without the organic examination of phenyl ring
The synthetic method of agent is very necessary, and it can be effectively facilitated the development and application of carbon nano ring.
Content of the invention
It is an object of the invention to provide a kind of preparation method of elastic lubrication nanometer carbon/agraphitic carbon laminated film.
The present invention adopts CH4The method of plasma self assembly, by forcing band under conditions of higher pressure and bias
The C of electric chargexHy n+Between mutually collide, form powered phenyl ring(C6Hz n+).And when two powered phenyl ring are in plasma
Meet in colony, series connection Suzuki couplings/big cyclization sequence reaction will occur.This reaction will be with other charged phenyl ring
Add and sustained response, until the generation of carbon nano ring.Meanwhile, in this process, major part does not participate in the C of cyclizationxHy n+Directly
Connect and be converted to agraphitic carbon.Nanometer carbon prepared by the present invention/agraphitic carbon complex thin film structure is fine and close, smooth surface, 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)Be cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with dehydrated alcohol and acetone, deposition interior is placed in after dried, is taken out
Vacuum is to 3 × 10-3Below Pa, with argon as sputter gas, in the bar that pulsed bias are -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 is deposited, and the indoor initial temperature of deposition is 25 ~ 35 DEG C, and target is set to 7 ~ 14 cm with basal spacing, adopts
High-purity titanium target, is passed through sputter gas argon, argon/nitrogen and argon/methane/nitrogen successively, opens DC source, in work
Pressure is 0.2 ~ 1.0 Pa, and 2.0 ~ 4.0 A of electric current, substrate bias are -100 V, under conditions of dutycycle is 80 %, splash successively
Ti, TiN, TiCN multilayer film is penetrated as transition zone, 15 ~ 20 min of sputtering time;
3)Argon and nitrogen is closed, is retained methane as sputter gas, is closed DC source, open radio-frequency power supply, in power be
20 ~ 40 W, operating pressure are 2.5 ~ 3.5 Pa, and substrate bias are -1000 ~ -1200 V, and sputtering target material is Ti, Al or Si, deposits
The carbon-base film of single-element doping, in 3.0 ~ 3.5 h, after deposition terminates, deposition indoor temperature is not higher than 90 to sedimentation time
℃.
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
Gross thickness is 2.0 ± 0.3 μm.
Elastic lubrication nanometer carbon/agraphitic carbon laminated film prepared by the present invention has following structure and performance:
1st, the elastic lubrication nanometer carbon/agraphitic carbon laminated film is mainly made up of two parts:Thickness is 1.0 ± 0.2 μm
Ti/TiN/TiCN multilayer transition layers and thickness be 1.0 ± 0.3 μm of carbon-base film;
2nd, the compact structure of the thin film and substrate are firmly combined with, surface roughness is less than 1.5 nm, elastic restoration ratio(W e )
It is more than 65 %;
3rd, there is in atmospheric environment the thin film excellent tribological property, coefficient of friction as little as 0.028, wear rate to be less than 4
×10-7mm3/(Nm).
Nanometer carbon prepared by the present invention/agraphitic carbon laminated film is the reason for there is above advantage:In deposition
During higher pressure intermolecular distance is reduced, plasma and molecular collision probability are significantly increased, the work of film forming
Property ion increase film growth rate increased, and reductions of ion energy drops the etch rate that high-energy ion bombardment causes
Low, therefore, thin film has higher sedimentation rate;High back bias voltage is applied to substrate, improve atom in film surface diffusion and
The ability of chemical reaction is participated in, consistency and the film forming ability of thin film is improve;Meanwhile, it is self-assembly of in deposition process
Nanometer carbon has excellent toughness and very weak shear strength, and incorporating can be with the toughness of enhanced film and tribology in thin film
Energy.
Description of the drawings
Transmission electron microscope and its enlarged drawing of the Fig. 1 for 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.
Displacement-load curves figures of the Fig. 3 for laminated film described in the embodiment of the present invention 2.
Aerial friction coefficient curves of the Fig. 4 for laminated film described in the embodiment of the present invention 3.
Specific embodiment
For a better understanding of the present invention, the present invention is further illustrated in conjunction with following embodiments.
Embodiment 1
Cleaning substrate:It is cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with dehydrated alcohol and acetone soln, places after dried
Indoor in deposition.Deposition pre-treatment:It is evacuated to 2 × 10-3Below Pa, with argon as sputter gas, is 80 % in dutycycle,
Pulsed bias be -1100 V under conditions of substrate is carried out plasma sputtering clean 20 min, with remove surface oxide layer and
Impurity.Deposition:Using high-purity titanium target, sputter gas argon, argon+nitrogen and argon+nitrogen+methane is passed through successively, open
DC source, is 0.4 ~ 1.0 Pa, 2 A of DC current in operating pressure, and -100 V of substrate bias, dutycycle are the condition of 80 %
Lower deposition multilayer transition layer Ti/TiN/TiCN, transition zone sedimentation time is 15 min.After transition zone deposition terminates, argon is closed
And nitrogen, retaining methane as sputter gas, close DC source, open radio-frequency power supply, power setting is 20 W, in work pressure
It is by force 3.0 Pa, substrate bias are -1100 V, dutycycle is the deposition of the carbon-base film for carrying out Ti doping under conditions of 80 %,
Sedimentation time is 3.2 h, obtains a series of nanometer carbon/agraphitic carbon laminated film.
The section and surface of laminated film are observed using Flied emission Scanning Electron microscope, its thickness(Including
Cross layer)For 1.7 μm, smooth surface, compact structure.Its transmission electron microscope image and its enlarged drawing are as shown in figure 1, multiple
Closing thin film and showing typical undefined structure, the presence of some circuluses can be substantially 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 thin film.Former
Sub- force microscope measures laminated film surface roughness for 1.051 nm.Nano-indentation experiment result shows its hardness(H)And bullet
Property modulus(E)Respectively 10.04 and 89.0 GPa, elastic restoration ratio(W e )For 66.0 %.In air friction testing, such thin
The average friction coefficient 0.028 of film, wear rate are 3.5 × 10-7mm3/(Nm).
Embodiment 2
As described in Example 1, radio-frequency power is adjusted to 40 W in carbon layer deposition.
Using Flied emission Scanning Electron microscope viewing film section and surface, its thickness is 2.07 μm, smooth surface,
Compact structure.Raman results show that laminated film has the characteristic peak of carbon nano ring and agraphitic carbon.Using atomic force microscope
Roughness of film is measured for 0.389 nm.According to nano-indentation experiment 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 %, its displacement-load curves is 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 × 10-7mm3/(Nm).
Embodiment 3
As described in Example 1, sputtering target material is changed to silicon target by titanium target after deposition transition zone, opens radio-frequency power supply, power is adjusted
Save as 20 W, prepare a series of carbon-base film of Si doping.
Film sections and surface are observed with field emission scanning electron microscope, laminated film thickness is 2.0 μm,
Smooth surface, compact structure.Roughness of film is measured for 0.261 nm 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 × 10-7mm3/(Nm), the aerial friction coefficient curve of thin 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 adopt at room temperature
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)Be cleaned by ultrasonic monocrystalline silicon piece and stainless steel thin slice with dehydrated alcohol and acetone, deposition interior is placed in after dried, is taken out
Vacuum is to 3 × 10-3Below Pa, with argon as sputter gas, in the bar that pulsed bias are -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 is deposited, and the indoor initial temperature of deposition is 25 ~ 35 DEG C, and target is set to 7 ~ 14 cm with basal spacing, adopts
High-purity titanium target, is passed through sputter gas argon, argon/nitrogen and argon/methane/nitrogen successively, opens DC source, in work
Pressure is 0.2 ~ 1.0 Pa, and 2.0 ~ 4.0 A of electric current, substrate bias are -100 V, under conditions of dutycycle is 80 %, splash successively
Ti, TiN, TiCN multilayer film is penetrated as transition zone, 15 ~ 20 min of sputtering time;
3)Argon and nitrogen is closed, is retained methane as sputter gas, is closed DC source, open radio-frequency power supply, in power be
20 ~ 40 W, operating pressure are 2.5 ~ 3.5 Pa, and substrate bias are -1000 ~ -1200 V, and sputtering target material is Ti, Al or Si, deposits
The carbon-base film of single-element doping, in 3.0 ~ 3.5 h, after deposition terminates, deposition indoor temperature is not higher than 90 to sedimentation time
℃.
2. preparation method as claimed in claim 1, it is characterised in that the thickness of the transition zone is 1.0 ± 0.2 μm;Carbon-based
The thickness of thin film is 1.0 ± 0.3 μm, and the gross thickness of laminated film is 2.0 ± 0.3 μm.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108517499A (en) * | 2018-03-28 | 2018-09-11 | 中国科学院兰州化学物理研究所 | A kind of difunctional NbSe of lubrication/conduction2The low temperature preparation method of film |
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 |
Citations (1)
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CN1354276A (en) * | 2000-10-17 | 2002-06-19 | 日新电机株式会社 | Carbon film and its forming method |
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CN1354276A (en) * | 2000-10-17 | 2002-06-19 | 日新电机株式会社 | Carbon film and its forming method |
Non-Patent Citations (4)
Title |
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JIANYUN ZHENG等: "Properties of TiN/TiCN multilayer films by direct current magnetron sputtering", 《JOURNAL OF PHYSICS D: APPLIED PHYSICS》 * |
JINLONG JIANG等: "Structure and characteristics of amorphous (Ti,Si)–C:H films deposited by reactive magnetron sputtering", 《DIAMOND & RELATED MATERIALS》 * |
R. G. LACERDA等: "Hard hydrogenated carbon films with low stress", 《APPLIED PHYSICS LETTERS》 * |
XIAOQIANG LIU等: "A Near-Frictionless and Extremely Elastic Hydrogenated Amorphous Carbon Film with Self-Assembled Dual Nanostructure", 《ADVANCED MATERIALS》 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN108517499A (en) * | 2018-03-28 | 2018-09-11 | 中国科学院兰州化学物理研究所 | A kind of difunctional NbSe of lubrication/conduction2The low temperature preparation method of film |
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