CN101748381A - Method for preparing high-performance doped diamond-like film - Google Patents
Method for preparing high-performance doped diamond-like film Download PDFInfo
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- CN101748381A CN101748381A CN200910217545A CN200910217545A CN101748381A CN 101748381 A CN101748381 A CN 101748381A CN 200910217545 A CN200910217545 A CN 200910217545A CN 200910217545 A CN200910217545 A CN 200910217545A CN 101748381 A CN101748381 A CN 101748381A
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Abstract
The invention discloses a method for preparing a high-performance doped diamond-like film. The method is characterized by comprising the following steps: firstly, utilizing ultrasonic cleaning technology to remove a polluted layer on the surface of a substrate; utilizing ion beam assisted deposition technology to prepare a gradient transition layer; and finally utilizing ion beam deposition and magnetron sputtering to synthesize a multi-element doped DLC film, wherein except any one of carbonaceous gases, such as methane, acetylene, benzene, ethanol, acetone and the like, any gas containing non-carbon elements, such as silicon hydride, boron hydride, phosphorane, carbon tetrafluoride and the like, is simultaneously introduced, and a metal sputtering source is opened for the doping of metal elements. The method has the advantages of synthesizing the multi-element doped DLC film which is simultaneously doped with the metal elements and the nonmetal elements, fully developing the complementary advantages of the doped metal elements and the doped nonmetal elements and remarkably improving the combination properties of the DLC film.
Description
Affiliated technical field:
Patent of the present invention relates to a kind of technology of preparing of high-performance quasi-diamond (DLC) film of the multiple element that mixes, and belongs to the compound technology of preparing of DLC mould material.
Background technology:
Diamond-film-like has friction and wear behavior, chemical stability and the biocompatibility of high rigidity, high elastic coefficient, excellence, has very application prospects.Limited the application of DLC film under harsh service condition but internal stress is big, film/basic bonding force is poor, poor heat stability, fragility are big etc.
Adopt the gradient transitional lay of optimizing to alleviate the internal stress of DLC film and the film/basic bonding force of raising DLC film; Forming with the amorphous carbon-film by doped metallic elements is the over-all properties that the multiphase structure of matrix can improve the DLC film, but doping metals can cause the frictional coefficient of DLC film higher, can not obtain low frictional coefficient.Doped with non-metals element F, H can significantly reduce the frictional coefficient of DLC film under extraordinary condition, doping Si, SiO
2Structure and performance Deng the adjustable DLC film of nonmetallic ingredient.Mixing metallic element and non-metallic element simultaneously in the DLC film, realize learning from other's strong points to offset one's weaknesses of different doped elements, be an effective way that obtains high-performance DLC film, but the research of this respect yet there are no all reports at present.
Summary of the invention:
In order to overcome the deficiency that present DLC membrane preparation technology and doped scheme exist, patent of the present invention has proposed a kind of novel DLC film composite deposition technology, it is characterized in that: in the process of the synthetic DLC film of ion beam depositing, except in ion source, feeding any carbonaceous gass such as methane, acetylene, benzene, ethanol, acetone, also feed simultaneously and comprise that silane, borine, phosphine, tetrafluoro-methane etc. contain any gas of non-carbon gas source, and opening metal sputtering source doped metallic elements, synthetic multi-element doping DLC film said method comprising the steps of:
(1) at first utilize ultrasonic cleaning technology to remove the matrix surface pollution layer;
(2) utilize ion beam assisted deposition to prepare gradient transitional lay then;
(3) on gradient transitional lay, utilize ion beam depositing+magnetron sputtering to synthesize multi-element doping DLC film at last.
In above-mentioned preparation method, step (2) ion source can adopt any ion source in anode layer ion source, the graceful ion source of Kraft, hall ion source, radio-frequency induction coupling ion source, the electron cyclotron resonace ion source.
In above-mentioned preparation method, the ionic fluid that step (2) ion source produces consist of argon ion, argon/nitrogen hybrid ionic, argon/carbon hybrid ionic or argon/nitrogen/carbon hybrid ionic, the ratio of different ions is controlled as required.
In above-mentioned preparation method, the ion energy of step (2) ionic fluid is 50eV～500eV.
In above-mentioned preparation method, the evaporation/sputtering source of step (2) can adopt any in magnetron sputtering target, cathodic arc evaporation source, the hollow cathode arc evaporation source.
In above-mentioned preparation method, the evaporation of step (2)/sputtering source target is any metal of Ti, Cr, Zr, W, Nb.
In above-mentioned preparation method, according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the described transition layer of step (2) comprises Ti/TiN/TiCN/TiC, Cr/CrN/CrCN/CrC, Zr/ZrN/ZrCN/ZrC, W/WC, Nb/NbN/NbC constant gradient transition layer.
In above-mentioned preparation method, the ion source of step (3) can adopt any ion source in anode layer ion source, the graceful ion source of Kraft, hall ion source, radio-frequency induction coupling ion source, the electron cyclotron resonace ion source.
In above-mentioned preparation method, step (3) is except feeding any carbonaceous gass such as methane, acetylene, benzene, ethanol, acetone in ion source, also feeding comprises that silane, borine, phosphine, tetrafluoro-methane etc. contain any gas of non-carbon gas source simultaneously.
In above-mentioned preparation method, step (3) feeds the non-metallic element incorporation that the ionogenic throughput ratio that contains non-carbon gas source and carbonaceous gas is adjusted the DLC film by control.
In above-mentioned preparation method, the ion energy of step (3) ionic fluid is 50eV～1000eV.
In above-mentioned preparation method, the controlled sputtering source of step (3) can adopt any magnetron sputtering mode in magnetically controlled DC sputtering, medium frequency magnetron sputtering, the rf magnetron sputtering.
In above-mentioned preparation method, the described controlled sputtering source target of step (3) is any of metallic elements such as W, Cr, Ti, Nb, Mo, Zr, Ag, Cu, Co.
In above-mentioned preparation method, step (3) is adjusted the metallic element incorporation of DLC film by the power of control magnetron sputtering target.
The advantage of patent of the present invention is to give full play to ion beam assisted depositing combination, the ion beam depositing of multi component mixed gas body, the advantage of magnetron sputtering, the multi-element doping DLC film of synthetic doped metallic elements simultaneously and non-metallic element on the gradient transitional lay basis of ion beam assisted depositing gradient preparation, realize the mutual supplement with each other's advantages of metallic element and non-metallic element, significantly improve the over-all properties of DLC film; By changing regulation and control doped element kind such as the factor that feeds ionogenic gaseous species and flow, sputter target material and target power output and content, obtain high performance multi-element doping DLC film.
Embodiment:
Below in conjunction with specific embodiment patent of the present invention is described in further detail, but not as the qualification to patent of the present invention.
Embodiment 1
At first utilize ultrasonic cleaning technology to remove GCr15 bearing surface grease contamination layer; Utilize the auxiliary magnetically controlled DC sputtering deposition of anode layer ion source Cr/CrN/CrCN/CrC gradient transitional lay then, the magnetron sputtering target material is Cr, the gas that feeds anode layer ion source comprises argon gas, nitrogen, acetylene, by the flow that changes argon gas, nitrogen, acetylene gradually realize the gradient transition of transition layer, ion energy be-100～-800eV; Utilize the DLC film of ion beam depositing+magnetron sputtering technique synthetic mix simultaneously Cr, Si, F on the Cr/CrN/CrCN/CrC gradient transitional lay at last, ion source adopts anode layer ion source, the gas that feeds anode layer ion source comprises argon gas, acetylene, silane and tetrafluoro-methane, controlled sputtering source adopts the magnetically controlled DC sputtering mode, and target is Cr; Control Cr, Si, the F content of multi-element doping DLC film by the flow that changes argon gas, acetylene, silane and tetrafluoro-methane, the sputtering power of chromium sputtering target.
Embodiment 2
At first utilize ultrasonic cleaning technology to remove the grease contamination layer of engine plunger surface; Utilize the auxiliary magnetically controlled DC sputtering deposition of anode layer ion source Cr/CrN/CrCN/CrC gradient transitional lay then, the magnetron sputtering target material is Cr, the gas that feeds anode layer ion source comprises argon gas, nitrogen, benzene, by the flow that changes argon gas, nitrogen, benzene gradually realize the gradient transition of transition layer, ion energy be-100～-800eV; Utilize the DLC film of ion beam depositing+magnetron sputtering technique synthetic mix simultaneously Cr, F, N on the Cr/CrN/CrCN/CrC gradient transitional lay at last, ion source adopts anode layer ion source, the gas that feeds anode layer ion source comprises argon gas, benzene, tetrafluoro-methane, nitrogen, magnetron sputtering adopts the magnetically controlled DC sputtering mode, and target is Cr; Control Cr, F, the N content of multi-element doping DLC film by the flow that changes argon gas, acetylene, tetrafluoro-methane, nitrogen, the sputtering power of chromium sputtering target.
Embodiment 3
At first utilize ultrasonic cleaning technology to remove speedy steel cutting-tool surface grease pollution layer; Utilize anode layer ion source auxiliary cathode arc deposited to prepare the Ti/TiN/TiCN/TiC gradient transitional lay then, the cathode arc target material is Ti, the gas that feeds anode layer ion source comprises argon gas, nitrogen, methane, by the flow that changes argon gas, nitrogen, methane gradually realize the gradient transition of transition layer, ion energy be-100～-800eV; Utilize ion beam depositing+magnetron sputtering technique synthetic doped Ti, Si, F, SiO simultaneously on the Ti/TiN/TiCN/TiC gradient transitional lay at last
2The DLC film, ion source adopts anode layer ion source, the gas that feeds anode layer ion source comprises hydrogen, methane, silane, tetrafluoro-methane, water vapour, magnetron sputtering adopts the magnetically controlled DC sputtering mode, target is Ti; Control Ti, Si, F, the SiO of multi-element doping DLC film by the flow that changes hydrogen, methane, silane, tetrafluoro-methane, water vapour, the sputtering power of titanium sputtering target
2Content.
Claims (8)
1. the preparation method of a multi-element doping quasi-diamond (DLC) film, it is characterized in that: in the process of the synthetic DLC film of ion beam depositing, except in ion source, feeding any carbonaceous gass such as methane, acetylene, benzene, ethanol, acetone, also feed simultaneously and comprise that silane, borine, phosphine, tetrafluoro-methane etc. contain any gas of non-carbon gas source, and opening metal sputtering source doped metallic elements, synthetic multi-element doping DLC film said method comprising the steps of:
(1) at first utilize ultrasonic cleaning technology to remove the matrix surface pollution layer;
(2) utilize ion beam assisted deposition to prepare gradient transitional lay then;
(3) on gradient transitional lay, utilize ion beam depositing+magnetron sputtering to synthesize multi-element doping DLC film at last.
2. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the ion source of step (2) can adopt any ion source in anode layer ion source, the graceful ion source of Kraft, hall ion source, radio-frequency induction coupling ion source, the electron cyclotron resonace ion source; The ionic fluid that ion source produces consist of argon ion, argon/nitrogen hybrid ionic, argon/carbon hybrid ionic or argon/nitrogen/carbon hybrid ionic, the ratio of different ions is controlled as required; The ion energy of ionic fluid is 50eV～500eV.
3, according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the evaporation/sputtering source of step (2) can adopt any in magnetron sputtering target, cathodic arc evaporation source, the hollow cathode arc evaporation source; Evaporation/sputtering source target is any metal of Ti, Cr, Zr, W, Nb.
4. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the described transition layer of step (2) comprises Ti/TiN/TiCN/TiC, Cr/CrN/CrCN/CrC, Zr/ZrN/ZrCN/ZrC, W/WC, Nb/NbN/NbC constant gradient transition layer.
5. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the ion source of step (3) can adopt any ion source in anode layer ion source, the graceful ion source of Kraft, hall ion source, radio-frequency induction coupling ion source, the electron cyclotron resonace ion source.
6. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: step (3) is except feeding any carbonaceous gass such as methane, acetylene, benzene, ethanol, acetone in ion source, also feeding comprises that silane, borine, phosphine, tetrafluoro-methane etc. contain any gas of non-carbon gas source simultaneously; Feed the non-metallic element incorporation that the ionogenic throughput ratio that contains non-carbon gas source and carbonaceous gas is adjusted the DLC film by control.
7. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the ion energy of step (2) ionic fluid is 50eV～1000eV.
8. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the controlled sputtering source of step (3) can adopt any magnetron sputtering mode in magnetically controlled DC sputtering, medium frequency magnetron sputtering, the rf magnetron sputtering.
9. according to the described multi-element doping DLC of claim 1 membrane preparation method, it is characterized in that: the described controlled sputtering source target of step (3) is any of metallic elements such as W, Cr, Ti, Nb, Mo, Zr, Ag, Cu, Co; Adjust the metallic element incorporation of DLC film by the power of control magnetron sputtering target.
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| CN102337497A (en) * | 2010-07-22 | 2012-02-01 | 中国科学院兰州化学物理研究所 | Method for preparing multi-element doped carbon-based nano composite film integrating functions of antiwear and lubrication |
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Application publication date: 20100623 |