CN100387754C - Diamond film containing chronium and its preparing method - Google Patents
Diamond film containing chronium and its preparing method Download PDFInfo
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- CN100387754C CN100387754C CNB2005101127231A CN200510112723A CN100387754C CN 100387754 C CN100387754 C CN 100387754C CN B2005101127231 A CNB2005101127231 A CN B2005101127231A CN 200510112723 A CN200510112723 A CN 200510112723A CN 100387754 C CN100387754 C CN 100387754C
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Abstract
The present invention discloses a quasi-diamond film containing chrome and the preparing method of the quasi-diamond film. The film is a quasi-diamond film which is vapor deposited on the surface of a basal body, is without hydrogen and contains chrome. The quasi-diamond film has an alternating compact multilayer gradient structure of a Cr layer, a Cr N < x > layer, a Cr < y > C< z > layer, a Cr layer, a Cr N< x > layer, a Cr< y > C < z > layer, etc. which are orderly arranged along the vertical direction of the surface of the basal body from inside to outside. The thickness of the film is not smaller than 2 mum. The quasi-diamond film has the advantages of high hardness, strong bonding force between the film and the basal body and favorable abrasion-proof property. The present invention has the preparing method that a magnetically controlled sputtering system is used to carry out filming. Magnetically controlled targets are a pair of unbalanced magnetically controlled Cr targets and one to four pairs of unbalanced magnetically controlled C targets. A target power supply is a medium frequency alternating current power supply between 20k Hz and 250k Hz. A single-level pulse direct current power supply is used to control the application of a pulse basal body negative bias voltage applied on a filmed basal body. The sputtering gas is argon gas. The preparing method overcomes a target poisoning defect existing in a direct current reaction magnetically controlled sputtering method which is used for forming quasi-diamond films.
Description
[technical field]
The present invention relates to a kind of cr-doped dlc film and preparation method thereof, specifically, relate to a kind of magnetron sputtering cr-doped dlc film and preparation method thereof.
[background technology]
Because diamond like carbon film (Diamond-like carbon, DLC film) has high rigidity, low-friction coefficient and over-all properties such as wear-resistant, as the wear-resistant protection film of cutter and mould, diamond-film-like has obtained researchist's extensive concern.
DLC film commonly used is divided into hydrogeneous DLC film and no hydrogen DLC film.The main drawback of no hydrogen DLC film is: 1, performance does not match between film and the matrix, causes between film and matrix bonding force bad, particularly steel matrix; 2, have high internal stress in the DLC film, cause the fragility height of film, therefore general film thickness is difficult to surpass 1 μ m.Simultaneously, the no hydrogen DLC film of general single structure, single component is difficult to possess good comprehensive performances, particularly the film wear resistance.For this reason, have the people once to add to contain at film base interface B and Ti uniformly-spaced layer to improve the bonding force between DLC film and matrix; Or employing contains TiN, TiCN and TiC layer in the DLC film, improve its mechanical property, but effect is all not satisfactory.
The required part film of industrialization requires film thickness can meet or exceed 2 μ m and have good film and the bonding force between matrix; wear-resistant protective film so not only may be used for the various surface abrasion resistance parts of mechanical manufacturing field; for example: gear, pump, plunger, bearing and their parts, and can be used for the cutter and the mould of material processing field.
Therefore general no hydrogen DLC film is difficult to reach the requirement of industrialization part film.
Therefore, synthetic possess good comprehensive performances, and the DLC film that promptly has high rigidity and good combination power and wear resisting property simultaneously becomes the new problem in film field.
People adopt several different methods to synthesize the DLC film, and for example: multi-arc ion coating, radio frequency (RF) PCVD and non-balance magnetically controlled sputter, the synthetic DLC film of general magnetron sputtering is to adopt direct current reaction magnetron sputtering.
When the direct current reaction magnetron sputtering dielectric substance, the subject matter that runs into is when sedimentation rate reduces, to produce because the defective that the starting the arc causes is referred to as " target poisoning " or " anode extinction tests " at film surface.Its reason is, along with deposition process continues, on the magnetic controlling target surface, progressively forms dielectric layer and causes that ionic charge gathers, until gathering electric charge and discharge playing an arc form.The starting the arc can cause that the target surface droplets of materials splashes, and forms defective in growing film.Have, the target surface damage field may become the arc discharge source again, has caused radian frequency to increase and the sedimentation rate reduction, and influences the stoichiometric ratio of technology stability and growing film.
[summary of the invention]
The technical issues that need to address of the present invention just are to overcome existing single structure, bonding force is bad between single component DLC film and matrix, the fragility height of film, the target poisoning defective that the synthetic DLC film of the defective of film wear resisting property difference and dc reactive magnetron sputtering technique exists, a kind of cr-doped dlc film and preparation method thereof is provided, it is that the hard that a kind of thickness with the preparation of non-balance magnetically controlled sputter method can surpass 2 μ m contains chromium (Cr) DLC film, it has fine and close multi-gradient structure, and has comprehensive excellent properties: high rigidity, Vickers' hardness surpasses 20GPa, bonding force between good film/base, between its film base under bonding force critical load＞50N and the atmospheric environment frictional coefficient be no more than 0.2.
For addressing the above problem, the present invention adopts following technical scheme:
Cr-doped dlc film of the present invention, it is the no hydrogen cr-doped dlc film in the matrix surface vapour deposition, described film has along the matrix surface vertical direction and outwards is followed successively by Cr layer, CrN from the lining
xLayer, Cr
yC
zLayer, Cr layer, CrN
xLayer, Cr
yC
zLayer ... the fine and close multi-gradient structure of alternative.
The thickness of film of the present invention is not less than 2 μ m, and wherein the X span is 0.10-1.00, and the Y span is 0.10-1.00, and the Z span is 0.10-1.00.
Wherein, described Cr layer thickness is 0.05-0.30 μ m.Described CrN
xLayer thickness is 0.05-0.80 μ m.Described Cr
yC
zLayer thickness is 0.10-1.50 μ m.
Film of the present invention has bonding force and good abrasion resistance between high rigidity, good film/base, and its Vickers' hardness is not less than 20GPa, and the critical load of bonding force is not less than 50N between its film/base, and its frictional coefficient under atmospheric environment is no more than 0.2.
The present invention discloses a kind of preparation method of described cr-doped dlc film, it utilizes magnetic control sputtering system to carry out plated film, on the vacuum chamber work rest, be furnished with rotatable matrix to be coated, matrix arranged around magnetic controlling target and ion source, described magnetic controlling target are that 1 pair of non-equilibrium magnetic controlled Cr target and 1-4 are to non-equilibrium magnetic controlled C target; Target power supply is the midfrequent AC power supply of 20-250kHz; Utilize the single-stage pulse dc power to be controlled at and apply pulse matrix negative bias on the matrix to be plated; Sputter gas is an argon gas, and argon gas directly adds by magnetic controlling target; Be evacuated to 1.0 * 10 by pumped vacuum systems
-3～5.0 * 10
-3Pa, vacuum chamber are preheating to 100-150 ℃, deposition Cr layer and CrN
xDuring layer, start the Cr target; Deposition Cr
yC
zDuring layer, start Cr target and C target simultaneously, Cr target power output or target current reduce to low from height, and C target power output or target current increase from low to high; At deposition CrN
xDuring layer, add reactant gases nitrogen by gas-adding pipe.
In the inventive method, described magnetic controlling target can be 1 pair of non-equilibrium magnetic controlled Cr target and 3 pairs of non-equilibrium magnetic controlled C targets.
In the inventive method, sputter gas pressure is no more than 0.32Pa.The matrix pulsed negative bias is-100V is to-200V.Target current is 1-10A.
The present invention utilizes intermediate frequency facing-target magnetron sputtering system system, and by regulating processing parameter, sputter gas pressure is no more than 0.32Pa.The matrix pulsed negative bias is-100V is to-200V, target current is that 1-10A or target power output are 2-8kW, utilize the selectivity sputter of C and Cr target and cosputtering in pure argon atmosphere on metallic matrix synthetic hard with multi-gradient structure contain chromium DLC film, the gradient multilayered structure is a significant benefit to be eliminated because the internal stress that DLC and steel matrix physicals do not match and cause; Wherein, utilize chromium layer and chrome-containing layer can obviously improve bonding force between film/base, CrN
xLayer also plays important supporting role.Therefore synthetic film has comprehensive excellent properties: high rigidity, and Vickers' hardness surpasses 20GPa, bonding force between good film/base, bonding force critical load＞50N between its film/base, frictional coefficient is no more than 0.2 under atmospheric environment.
The present invention utilizes the glow discharge of pulse intermediate frequency can change the magnetron sputtering plasma characteristics; Utilize single-stage pulse dc power control matrix negative bias and matrix bias current, the ion energy of matrix negative bias may command bombardment matrix; Can significantly improve the performance of film in conjunction with utilizing these two kinds of pulsed techniques.Utilize and many magnetic control is improved spatter film forming speed to target; Argon gas directly adds to strengthen sputter by magnetic controlling target to be renderd a service.Overcome the defective that the synthetic DLC film of dc reactive magnetron sputtering technique exists target to poison.
Utilize AFM (atomic force microscope), SEM (scanning electronic microscope) to investigate surface topography and the microstructure that contains chromium composite multi-layer DLC film.Utilize microhardness tester to measure the Vickers' hardness of synthetic film.Utilize the bonding force between full-automatic scratching instrument measurement steel matrix and the DLC film.Utilize ball-dish trier to investigate the friction and wear behavior of synthetic film: DLC film sample is bonded on the dish, and the antithesis ball is Al
2O
3Ball is in atmospheric environment.
Experimental result shows that the chromium DLC film that contains with fine and close multi-gradient structure that utilizes magnetron sputtering technique of the present invention to obtain has comprehensive excellent properties: its thickness surpasses 2 μ m, has high rigidity, and Vickers' hardness surpasses 20GPa; Bonding force between good film/base, the bonding force critical load is greater than 50N between film/base; Good abrasion resistance, frictional coefficient is no more than 0.2 under its atmospheric environment.
[description of drawings]
Fig. 1 is the cross sectional representation of SP8050 coating equipment.
Wherein, 1--work rest; The 2--magnetic controlling target; The 3--pumped vacuum systems;
Fig. 2 is the section SEM photo that contains chromium DLC film.
Wherein, A--Cr layer; B--CrN
xLayer; C--Cr
yC
zLayer;
[embodiment]
Embodiment 1
1) film coating apparatus
Adopting SP8050 coating equipment (manufacturings of strength source, Beijing science and technology limited Company) to utilize non-balance magnetically controlled sputter method to synthesize to contain chromium does not have hydrogen DLC film, the cross sectional representation of this coating equipment as shown in Figure 1, four pairs of magnetic controls in cylindrical vacuum chamber, have been placed to target, comprising two Cr targets and six C targets, wherein the C target is a graphite target.The specification of target is 420mm * 8mm, and purity is 99.99%.Every pair of magnetic control is arranged with 70cm in vacuum chamber at interval Face to face to two plane magnetic control targets of target.Work rest places the vacuum chamber central zone.Utilization is applied to a pulse dc power of waiting to deposit on the workpiece and is added in every pair respectively to four 40kHz pulse midfrequent AC power supply control matrix negative biass, matrix bias current and magnetic controlling target parameters on the target.On intermediate frequency power supply, control with constant current mode.In deposition process, magnetic controlling target is by regulating target voltage to control, and the target voltage working range is 200V to 800V, adopts constant current mode, for example is set to 2A, 4A and 6A respectively.Adopt argon gas from each magnetic controlling target, directly to feed, render a service to strengthen magnetic control.The processing parameter of each operation can be controlled automatically by PLC (programmable logic controller).
2) preparation process
A) waiting to deposit workpiece prepares
Cr12Mo4V rapid steel workpiece surface is polished to minute surface in advance, and its surface average roughness Ra is about 0.05 μ m; The ultrasonic cleaning 20min in the acetone container that then all workpiece packed into cleans the back workpiece and dries up with drying nitrogen.
B) the Ar ion cleans
With molecular pump or diffusion pump vacuum chamber is evacuated to 1.0 * 10
-3～5.0 * 10
-3Behind the Pa, under-500V bias voltage and 3.0Pa argon gas condition, utilize Ar ion bombardment substrate surface further to clean, remove the impurity that substrate surface adheres to.
C) coating process
Vacuum chamber is heated to 120 ℃, and pressure remains on 0.30Pa in argon gas atmosphere, and the major sedimentary process comprised for three steps: (1) deposition Cr layer: start the Cr adhesion layer that two Cr targets deposit thickness on substrate surface is about 0.20 μ m.(2) deposition CrN
xLayer: feeding under the condition of nitrogen gas, utilizing two Cr targets to sputter at the CrN that deposit thickness on the Cr layer is about 0.50 μ m
xLayer.(3) deposition Cr
yC
zLayer: start two Cr targets and six C targets simultaneously, at CrN
xCosputtering thickness is about the Cr of 1.00 μ m on the layer
yC
zLayer, wherein the Cr target current is progressively reduced to 1A from 10A, and the C target current progressively is increased to 6A from 2A.(4) repeat above-mentioned deposition procedures (1), (2) and (3) successively.
3) contain the surface topography and the cross-sectional structure of chromium DLC film
The AFM measuring result shows that the average surface roughness Ra of synthetic film is 9.6nm, and the median size of projection is 94nm, and center line average difference is 20nm.Synthetic film has level and smooth surface topography, the visible loose particles that from target, does not sputter out, and this smooth-flat-surface makes synthetic DLC film be applicable to the demanding mould of surface treatment.Fig. 2 in dutycycle be 70%-120V unipolar pulse negative bias under the synthetic SEM photo that contains the compound DLC film of chromium.Can see that in Fig. 2 containing the compound DLC film of chromium has very fine and close gradient multilayered structure, wherein A is that Cr layer, B are CrN
xLayer, C are Cr
yC
z, thickness is about 5.1 μ m, and its structural group becomes: Cr layer, CrN
xLayer, CryCz layer, Cr layer, CrN
xLayer, Cr
yC
zLayer, Cr layer, CrN
xLayer, Cr
yC
zLayer mutually alternately.The Raman test result of DLC film conforms to the amorphous carbon-film feature: the characteristic peak D peak of DLC film and G peak intensity ratio I
D/ I
GBe 1.78.The interface does not have visible defects in conjunction with good between compound each layer of DLC film.Utilize this gradient multilayered structure can eliminate because the high internal stress that physicals does not match and causes between DLC film and the matrix, wherein CrN
xLayer can also play important supporting role on the steel matrix surface.
4) film performance
The microhardness tester measuring result shows, is between 21GPa and the 38GPa in DLC film microhardness under the 20g load.
The scratching instrument test result show between film/base bonding force be improved significantly, the critical load in the DLC film cut process is between 50N and the 65N.
Adopt ball-dish trier to investigate the friction and wear behavior of synthetic film.Under 10N, 20N and the effect of 50N load, the average friction coefficient of film is between 0.08 to 0.19.
Prepare the following example by embodiment 1 described method
Film is a three-decker, from matrix surface outwards is: the Cr layer: 0.25 μ m; CrN
0.1Layer: 0.45 μ m; Cr
0.1C layer: 1.45 μ m.
Film is six layers of structure, from matrix surface outwards is: the Cr layer: 0.20 μ m; CrN
0.6Layer: 0.40 μ m; Cr
0.55C
0.1Layer: 0.85 μ m; Cr layer: 0.25 μ m; CrN
0.6Layer: 0.45 μ m; Cr
0.55C
0.1Layer: 0.80 μ m;
Embodiment 4
Film is nine layers of structure, from matrix surface outwards is: the Cr layer: 0.17 μ m; CrN layer: 0.42 μ m; CrC
0.5Layer: 0.96 μ m; Cr layer: 0.25 μ m; CrN layer: 0.45 μ m; CrC
0.5Layer: 0.95 μ m; Cr layer: 0.23 μ m; CrN layer: 0.47 μ m; CrC
0.5Layer: 0.93 μ m.
Claims (9)
1. the preparation method of a cr-doped dlc film, described cr-doped dlc film is the no hydrogen cr-doped dlc film in the matrix surface vapour deposition, described film has along the matrix surface vertical direction and outwards is followed successively by Cr layer, CrN from the lining
xLayer, Cr
yC
zLayer, Cr layer, CrN
xLayer, Cr
yC
zLayer ... the fine and close multi-gradient structure of alternative; It is to utilize magnetic control sputtering system to carry out plated film, on the vacuum chamber work rest, be furnished with rotatable matrix to be coated, matrix arranged around magnetic controlling target and ion source is characterized in that: described magnetic controlling target is that 1 pair of non-equilibrium magnetic controlled Cr target and 1-4 are to non-equilibrium magnetic controlled C target; Target power supply is the midfrequent AC power supply of 20-250kHz; Utilize the single-stage pulse dc power to be controlled at and apply pulse matrix negative bias on the matrix to be plated; Sputter gas is an argon gas, and argon gas directly adds by magnetic controlling target; Vacuum chamber is preheating to 100-150 ℃, deposition Cr layer and CrN
xDuring layer, start the Cr target; Deposition Cr
yC
zDuring layer, start Cr target and C target simultaneously, Cr target power output or target current reduce from high to low, and C target power output or target current increase from low to high; At deposition CrN
xDuring layer, add reactant gases nitrogen by gas-adding pipe.
2. the preparation method of cr-doped dlc film as claimed in claim 1, it is characterized in that: described magnetic controlling target is 1 pair of non-equilibrium magnetic controlled Cr target and 3 pairs of non-equilibrium magnetic controlled C targets.
3. the preparation method of cr-doped dlc film as claimed in claim 2 is characterized in that: the matrix pulsed negative bias for-100V to-200V.
4. as the preparation method of arbitrary described cr-doped dlc film of claim 1-3, it is characterized in that: target current is that 1-10A or target power output are 2-8kW.
5. the preparation method of cr-doped dlc film as claimed in claim 4, it is characterized in that: the thickness of described film is not less than 2 μ m, and the span of described X is 0.10-1.00, and the span of Y is 0.10-1.00, and the span of Z is 0.10-1.00.
6. the preparation method of cr-doped dlc film as claimed in claim 5, it is characterized in that: described Cr layer thickness is 0.05-0.30 μ m.
7. the preparation method of cr-doped dlc film as claimed in claim 6 is characterized in that: described CrN
xLayer thickness is 0.05-0.80 μ m.
8. the preparation method of cr-doped dlc film as claimed in claim 7 is characterized in that: described Cr
yC
zLayer thickness is 0.10-1.50 μ m.
9. the preparation method of cr-doped dlc film as claimed in claim 8, it is characterized in that: described film has high rigidity, and its Vickers' hardness is not less than 20GPa; Bonding force between good film/base, the critical load of bonding force is not less than 50N between its film/base; And good abrasion resistance, its frictional coefficient under atmospheric environment is no more than 0.2.
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|---|---|---|---|
| CNB2005101127231A CN100387754C (en) | 2005-10-12 | 2005-10-12 | Diamond film containing chronium and its preparing method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101127231A CN100387754C (en) | 2005-10-12 | 2005-10-12 | Diamond film containing chronium and its preparing method |
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| Publication Number | Publication Date |
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| CN1743503A CN1743503A (en) | 2006-03-08 |
| CN100387754C true CN100387754C (en) | 2008-05-14 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4704950B2 (en) | 2006-04-27 | 2011-06-22 | 株式会社神戸製鋼所 | Amorphous carbon-based hard multilayer film and hard surface member having this film on the surface |
| CN101608299B (en) * | 2009-07-13 | 2010-12-29 | 四川大学 | High hardness and low friction Cr/CrCN gradient coating technology applicable to surface of profiled reed |
| US9617654B2 (en) | 2012-12-21 | 2017-04-11 | Exxonmobil Research And Engineering Company | Low friction coatings with improved abrasion and wear properties and methods of making |
| CN105597149B (en) * | 2015-10-08 | 2018-08-17 | 西南交通大学 | C film biomaterial preparation method with wear self-repair function in a kind of environment in vivo |
| KR102257499B1 (en) * | 2016-05-03 | 2021-05-31 | 엘지전자 주식회사 | Linear compressor and a method for manufacturing the same |
| US11364705B2 (en) | 2017-10-17 | 2022-06-21 | Exxonmobil Upstream Research Company | Diamond-like-carbon based friction reducing tapes |
| CN108611613B (en) * | 2018-06-09 | 2020-06-30 | 中国科学院兰州化学物理研究所 | Preparation method of nano multilayer structure carbon-based film |
| CN111218656A (en) * | 2019-11-25 | 2020-06-02 | 江苏氢电新能源有限公司 | High-corrosion-resistance high-conductivity fuel cell metal bipolar plate protective film and preparation method thereof |
| CN111748789B (en) * | 2020-07-10 | 2022-06-24 | 哈尔滨工业大学 | Device and method for depositing pure DLC (Diamond like carbon) by enhancing glow discharge through graphite cathode arc |
| CN112647040B (en) * | 2021-01-04 | 2022-06-21 | 中国科学院兰州化学物理研究所 | Ta-c base multilayer wear-resistant cutter coating and preparation method thereof |
| CN114836715A (en) * | 2022-03-21 | 2022-08-02 | 华南理工大学 | Metal surface Cr/CrN/CrCN/Cr-DLC multilayer composite self-lubricating film and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004204311A (en) * | 2002-12-26 | 2004-07-22 | Nachi Fujikoshi Corp | Sliding member coated with cr carbide |
| WO2005014882A1 (en) * | 2003-07-25 | 2005-02-17 | Nv Bekaert Sa | Substrate covered with an intermediate coating and a hard carbon coating |
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2005
- 2005-10-12 CN CNB2005101127231A patent/CN100387754C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004204311A (en) * | 2002-12-26 | 2004-07-22 | Nachi Fujikoshi Corp | Sliding member coated with cr carbide |
| WO2005014882A1 (en) * | 2003-07-25 | 2005-02-17 | Nv Bekaert Sa | Substrate covered with an intermediate coating and a hard carbon coating |
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