CN101701332B - Method for preparing compound diamond-like carbon coating by using medium-frequency magnetic-control glow discharge method - Google Patents
Method for preparing compound diamond-like carbon coating by using medium-frequency magnetic-control glow discharge method Download PDFInfo
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- CN101701332B CN101701332B CN2009102727950A CN200910272795A CN101701332B CN 101701332 B CN101701332 B CN 101701332B CN 2009102727950 A CN2009102727950 A CN 2009102727950A CN 200910272795 A CN200910272795 A CN 200910272795A CN 101701332 B CN101701332 B CN 101701332B
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Abstract
The invention relates to a method for preparing a nano compound diamond-like carbon coating, which is realized in a way that: glow discharge is produced by using a medium-frequency magnetic-control sputtering target; argon and excessive hydrocarbon gases are introduced, so that the metal on the target surface reacts with the hydrocarbon gases to produce metallic carbides; when the argon ions bombard the target surface, the target surface sputters the metallic carbides; strong plasma produced by the glow discharge of the target surface ionize the hydrocarbon gases, so that the hydrocarbon gases produce highly-ionized carbon ions; and the carbides sputtered from the target surface and the highly-ionized carbon ions produced from the hydrocarbon gases form a high-hardness carbide-doped nano compound diamond-like carbon coating on a workpiece surface. The coating prepared by the invention has the characteristics of high hardness, strong adhesive force, high growth speed, high production efficiency, low depositing temperature, low production cost, simple equipment structure and the like; and diamond-like carbon coatings with different thicknesses can be prepared on hard alloy, high-speed steel and various other workpieces.
Description
Technical field
The present invention relates to a kind of method for preparing nano composite diamond coating, belong to the thin-film material technical field.
Background technology
Quasi-diamond (DLC) film has low-friction coefficient, high rigidity, high elastic coefficient, high-wearing feature and thermal conductivity, a series of particular performances such as good chemical stability and resistance to corrosion.The focus of whole world research since the eighties always.The DLC technology of preparing comprises two kinds of CVD (chemical vapour deposition) and PVD (physical vapor deposition), the CVD method as the treatment temp of plasma-assisted chemical deposition (PECVD), electron cyclotron resonace (ECR-CVD) more than 400 ℃, hydrogeneous in the coating simultaneously, coating stress is bigger, and growth velocity is lower, and body material is had relatively high expectations.Characteristics such as it is lower that PVD method such as magnetron sputtering, arc ion plating then have treatment temp, and preparation technology is flexible and changeable are adapted to the workpiece of various differing materials, have obtained application more and more widely at present, and the trend of further replacement CVD is arranged.
Internal stress and sticking power problem that PVD prepares the DLC coating are the problems of primary study in the DLC coatings applications always.In order to reduce the internal stress of DLC coating, various solutions have been proposed both at home and abroad, as gradient cladding, doping etc., gradient cladding is because the restriction use at present of complicated process of preparation and preparation equipment is less, and mixing then is to use the main method that reduces DLC coating internal stress more widely at present.The doped element of DLC has Si, N, B and transition metal.Doping DLC has lower stress and good wear-resisting and lubricity.For common diamond-like coating PVD preparation method, the hardness of coating generally below the 15GPa, thickness generally below 500 nanometers, if surpass thickness 500 nanometers, then cause disbonding at short notice because internal stress is excessive; Prepared effective coating film area is very little, and the plated film homogeneity can not guarantee, can not mass industrialized production, and the coating cost is very high.
Among the diamond-like coating PVD preparation method, mainly comprise magnetron sputtering and arc-over at present.In magnetron sputtering, sputtering target material adopts graphite target, utilizing the Ar ion that carbon atom is sputtered out from target flies to workpiece and forms diamond-like coating, because the carbon ionization level low (less than 5%) of sputtering method, the hardness that causes coating generally below HV15GPa, coating growth velocity lower (less than 0.3 μ m/h) simultaneously.Because the sputter energy is lower, cause the sticking power of coating and matrix relatively poor in addition.Although technology such as gradient cladding, doping are widely used at present,, then cause disbonding at short notice because internal stress is excessive if surpass thickness 500 nanometers, effective coating film area of equipment is very little, the plated film homogeneity can not guarantee, can not mass industrialized production, and the coating cost is very high.Relative magnetron sputtering technique, the ionization level of arc discharge method very high (greater than 90%), but when using graphite as target, because the temperature factor that graphite is negative, cause arc spot speed when target surface moves very slow, the graphite of regional area is erupted in a large number, directly fly to film forming on the workpiece, cause the graphite that has particle bigger in the coating, cause particle contamination.In order to adopt the quasi-diamond of the no particle contamination of arc discharge method preparation, generally all adopt the filtering method of magnetic at present, that is to say a bend pipe is set before target surface, filter out bigger graphite granule.The use of bend pipe makes the sedimentation rate of coating reduce (less than 0.5 micron/hour) significantly, and device structure complexity, poor stability, maintenance difficult are unfavorable for industrial batch production.
In order to overcome the shortcoming that above-mentioned arc process prepares diamond-like coating, it is 200710053095.3 Chinese patent application that the applicant has once submitted number of patent application to China national Department of Intellectual Property, and this application discloses a kind of method for preparing nano composite diamond coating.Acetylene gas was excessive before this scheme utilized the acetylene gas that feeds different flow in the cathode arc discharge process to make metallic target, target surface forms metal carbide layer poisons target surface, when arc motion, evaporate metallic carbide, utilize the high-melting-point characteristic of carbide to eliminate the metallic particles pollution that the conventional cathode arc-over causes from target surface.This external electric arc target the place ahead configuration auxiliary magnetic field, the strong plasma body ionization acetylene gas that utilizes magnetic focusing effect and arc-over to produce, produce the carbon ion of height ionization, under the effect of bias voltage, form carbide doped diamond coating from the metallic carbide of target surface evaporation and the carbon ion of acetylene ionization generation at workpiece surface, by adjusting the size and the content of carbide grain in the different acetylene flow control coatings.The carbon ionization level height that this method produces, the growth velocity of coating is higher, and because the nanocrystalline and amorphous strengthening effect of carbide under the condition of low coating stress, also has higher hardness when keeping the good lubrication performance, its hardness can reach 27Gpa simultaneously.
But find from practical situations, because the energy of arc-over is very high, cause causing in the coating process that temperature raises, generally more than 100 ℃, carry out to cause certain damage to material when diamond-like coating prepares with this method at the low relatively poor material surface of heatproof of fusing points such as plastics, aluminium alloy and copper alloy, limited its use occasion.In addition, because high-energy and certain temperature rise in the arc process preparation process cause the diamond-like coating surfaceness higher, the workpiece surface finish of institute's coating is not enough, cause behind the surface coating that surface smoothness descends, on mould of having relatively high expectations and instrument, can not satisfy the requirement of application and limited its use range.
Summary of the invention
The objective of the invention is to the higher and higher problem that can not on low melting material such as plastics and non-ferrous metal, prepare of preparation temperature of particle contamination, coating roughness in order to overcome arc process and to prepare diamond-like coating, a kind of method for preparing nano composite diamond coating of suitable industrialized production is provided.This preparation method has characteristics such as principle advanced person, coating apparatus is simple in structure, sedimentation rate is fast, adopts the diamond-like coating of this method preparation to have higher hardness and good lubricating property and good surface smoothness; Can on all kinds of basic materials such as Wimet, rapid steel, stainless steel, carbon steel, die steel and non-ferrous metal and plastics, carry out the low temperature preparation of coating.
For achieving the above object, technical scheme provided by the invention is: a kind of method for preparing nano composite diamond coating, it is characterized in that: at 0.05-1Pa ,-50 under the condition of-300V bias voltage, utilize medium frequency magnetron sputtering (twin target sputter) technology in argon atmosphere, to prepare the 30-50nm intermediate metal, feed excessive hydrocarbon gas and a small amount of argon gas then, hydrocarbon gas and the target surface formation metallic carbide that react under the glow discharge effect of medium frequency magnetron sputtering target surface, when argon ion sputtering target surface, sputter metallic carbide; The strong plasma body ionization hydrocarbon gas that the glow discharge that utilizes target surface intermediate frequency to drive produces makes hydrocarbon gas produce the carbon ion of height ionization; The carbon ion of the height ionization that produces from the carbide and the hydrocarbon gas of target surface evaporation forms the carbide dopen Nano composite diamond coating of high rigidity at workpiece surface.
Produce the used medium frequency magnetron sputtering target of glow discharge and be also referred to as twin target, promptly by two independently target form jointly, drive by intermediate frequency power supply, two targets are anode and cathode each other, the intermediate frequency power supply frequency is 30KHz; Target back magnetic field of magnets intensity is 300-500 Gauss in 3500-4000 Gauss after decaying to target surface; The field pole of two targets of twin target is opposite.Two target target surface angles that constitute twin target are 120 degree or face-to-face parallel arrangement.
Metallic target target of the present invention is Ti, Cr or Zr target, and the quantity of target is that 2-8 is right, target size be width at 100-300mm, length is at 400-1200mm; The electric current of metallic target is at the 5-50 ampere.
Described hydrocarbon gas is methane, acetylene or propane.
It is 100-1000sccm that the present invention feeds the hydrocarbon gas flow.Argon flow amount is 30-50sccm.
It is that magnetron sputtering method prepares a phenomenon of doing one's utmost in the coating to avoid that target is poisoned; target is poisoned and is caused coating quality to descend through regular meeting; sedimentation rate reduces; in order to overcome the target intoxicating phenomenon; adopted complicated watch-dog monitor closely reactant gases in the conventional magnetron sputtering equipment; reduce the input of reactant gases if gas is excessive, cause the equipment overall structure more complicated at once.The present invention is then opposite, makes full use of the target intoxicating phenomenon and makes target surface form carbide, because the sputtering yield of carbide well below the sputtering yield of pure metal, has reduced the sputter rate of target surface significantly for this reason, glow discharge voltage is raise.Conventional DC shielding power supply cisco unity malfunction adopts the intermediate frequency power supply power supply for this reason among the present invention.Because intermediate frequency power supply is Alternating Current Power Supply, can overcome " target poisonings " phenomenon, have good sputter ability to conducting electricity relatively poor metal target surface carbide, work that can long-term stability.The present invention makes full use of the medium frequency magnetron sputtering technology can overcome " target poisoning " and " anode disappearance " and the high advantage of sputter energy, make twin target under intermediate frequency power supply drives, produce glow discharge, feed excessive hydrocarbon gas (methane, acetylene or propane etc.), make target surface metal and gas reaction generate metallic carbide, target surface is poisoned.When the argon ion bombardment target surface, not to sputter metal ion, but sputter metallic carbide, because the metallic target carbide surface is a ceramic phase, impedance discharge is than metallic target height, cause target surface glow discharge voltage to increase substantially, in addition, because anode and cathode each other between two targets of intermediate frequency magnetic controlling target, the glow discharge that adds target surface is controlled by magnetic field, and plasma body is vibration back and forth between two targets, and plasma density is very high, make the hydrocarbon gas height ionization in target surface annex zone, produce the active carbon ion of a large amount of high-energy.The carbide of target surface increases sparking voltage simultaneously, and the carbon ion energy increases when further making glow discharge.In the glow discharging process, argon ion is except the sputter target surface produces carbide, also can bump with hydrocarbon gas, make hydrocarbon gas decompose ionization and become carbon ion or hydrocarbon polymer ion, under the effect of negative bias, the carbon of ionization and hydrocarbon polymer ion are adsorbed to workpiece surface and form diamond-film-like, and the metallic carbide that the while target surface sputters also can be doped in the film, by the flow of control hydrocarbon gas, then can form the diamond-like composite coating of different carbide dopings.Conventional quasi-diamond uses graphite as carbon source, and ionization level is very low in the sputter procedure, causes coating based on class graphite mutually, and hardness is lower.Can there be particle contamination in the electric arc rule, causes that roughness raises; Though the target poisoned technique can overcome particle contamination problems, preparation temperature is higher, causes that coatingsurface smooth finish descends; And the present invention adopts hydrocarbon gas to do carbon source, utilizes the ionization of intermediate frequency magnetic-control glow discharge simultaneously, can obtain the carbon ion of height ionization, has avoided adopting arc discharge method graphite to spray the shortcoming of big drop and the decline of target poisoned technique workpiece surface finish.Can obtain the diamond-like coating of high-quality no particle contamination.Utilize the work characteristics of magnetron sputtering for this reason among the present invention but overcome the low shortcoming of magnetically controlled DC sputtering ionization level, obtained the carbon ion of the height ionization that arc-discharge technique just can reach.Preparation temperature is low simultaneously, and workpiece surface finish is good, and prepared diamond-like coating has the hardness height that produces near arc ion plating but coating is very fine and close, does not have particle contamination, simultaneously coating sedimentation rate higher (near 3 microns/hour).
Because the high-performance that diamond-like coating has, make it in fields such as aerospace, machinery, biomedicine, computers, have a good application prospect, intermediate frequency magnetic-control glow discharge method is because its technical superiority makes it not only can overcome the particle issues of arc process for this reason, inherit simultaneously characteristics such as common magnetic sputtering coating densification and arc ion plating ionization level height again, make the hardness, sticking power, homogeneity etc. of coating be better than conventional magnetron sputtering and arc discharge method, in the DLC coating preparation, have a good application prospect.
Description of drawings
The coating system synoptic diagram of Fig. 1 for being adopted among the present invention;
Fig. 2 makes coating layer of Nano composite diamond surface scan Electronic Speculum pattern for the present invention;
Fig. 3 makes coating layer of Nano composite diamond surface atom power shape appearance figure for the present invention;
The microhardness of coating layer of Nano composite diamond under the different methane flow conditions that Fig. 4 makes for the present invention;
Embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further:
Embodiment 1: utilize the medium frequency magnetron sputtering target to prepare the Ti intermediate metal in argon atmosphere under the condition of 0.5Pa, negative 100V bias voltage, the deposit thickness of intermediate metal is 300 nanometers; Feed excessive acetylene gas and argon gas then, acetylene and the metal Ti target surface formation titanium carbide that reacts when argon ion sputtering target surface, sputters titanium carbide from target surface; The strong plasma body ionization acetylene gas that the glow discharge that utilizes target surface intermediate frequency to drive produces produces the carbon ion of height ionization; Form titanium carbide dopen Nano composite diamond coating from the titanium carbide of target surface evaporation and the carbon ion of acetylene generation at workpiece surface.Wherein feeding the acetylene gas flow is 200sccm, and argon flow amount is 30sccm; The total current of metal Ti target is at 80 amperes.Titanium carbide content is 20-22at.% in the prepared diamond-like composite coating, and the carbide particle diameter is the 20-30 nanometer, and coating hardness is 35-40GPa.
Embodiment 2: utilize the medium frequency magnetron sputtering target to prepare the Cr intermediate metal in argon atmosphere under the condition of 0.4Pa, negative 100V bias voltage, the deposit thickness of intermediate metal is 200 nanometers; Feed excessive methane gas and argon gas then, acetylene and the Metal Cr target surface formation chromium carbide that reacts when argon ion sputtering target surface, sputters chromium carbide from target surface; The strong plasma body ionization methane gas that the glow discharge that utilizes target surface intermediate frequency to drive produces produces the carbon ion of height ionization; Form chromium carbide dopen Nano composite diamond coating from the chromium carbide of target surface evaporation and the carbon ion of methane generation at workpiece surface.Wherein feeding the methane gas flow is 300sccm, and argon flow amount is 40sccm; The total current of Metal Cr target is at 100 amperes.Chromium carbide content is 13-15at.% in the prepared diamond-like composite coating, and the chromium carbide particle diameter is the 10-15 nanometer, and coating hardness is 30-32GPa.
Embodiment 3: utilize magnetic controlling target to prepare the Zr intermediate metal under the condition of 0.6Pa, negative 100V bias voltage, the deposit thickness of intermediate metal is 400 nanometers; Feed excessive propane gas and argon gas then, propane and the metallic Z r target surface formation zirconium carbide that reacts when argon ion sputtering target surface, sputters zirconium carbide from target surface; The strong plasma body ionization propane gas that the glow discharge that utilizes target surface intermediate frequency to drive produces produces the carbon ion of height ionization; Form zirconium carbide dopen Nano composite diamond coating from the zirconium carbide of target surface evaporation and the carbon ion of propane generation at workpiece surface.Wherein feeding the propane gas flow is 400sccm, and argon flow amount is 50sccm; The total current of metal zirconium target is at 120 amperes.Zirconium carbide content is 8-10at.% in the prepared diamond-like composite coating, and the zirconium carbide particle diameter is the 5-10 nanometer, and coating hardness is 35-40GPa.
Fig. 1 is a coating system structural representation of the present invention, this equipment opening door vacuum apparatus, and vacuum-chamber dimensions is Φ 800 * 800mm
2The unit of bleeding is bled by 6 pairs of vacuum chambers of bleeding point.Be provided with four pairs of the same twin magnetic controlling target 3 and work rests 5 in the vacuum chamber, metal magnetic control target size is 140 * 600mm
2, by intermediate frequency power supply 2 power supplies.Work rest 5 is positioned at the middle part of vacuum chamber and carries out Three dimensional rotation, and well heater 1 is positioned at the positive center of vacuum chamber, is used for bake out and coating process and heats up.In vacuum chamber, layout has a certain degree between the twin magnetic controlling target target surface.Operate by door 4 during maintenance of equipment.The homogeneity of this equipment coating has obtained good assurance, has improved coating quality, has improved coating adhesion.
Fig. 2 is the surface topography sem photograph of the prepared TiC-DLC nano-composite coating of the present invention, and as can be seen from the figure coatingsurface does not have particle and cavity, and is very smooth.
Fig. 3 is the atomic power shape appearance figure of the prepared TiC-DLC nano-composite coating of the present invention, and coatingsurface is more even as can be seen, has very low surfaceness, and its roughness Ra value is 0.5nm, belongs to extremely slick surface.
The microhardness of coating layer of Nano composite diamond under the different methane flow conditions that Fig. 4 makes for the present invention, as can be seen from the figure, coating hardness is higher, is up to 36GPa.
Claims (6)
1. method for preparing nano composite diamond coating, it is characterized in that: at 0.05-1Pa ,-50 under the condition of-300V bias voltage, utilize the medium frequency magnetron sputtering technology in argon atmosphere, to prepare the 30-50nm intermediate metal, feed argon gas and excessive hydrocarbon gas then, under the glow discharge effect of medium frequency magnetron sputtering target surface, make hydrocarbon gas and the target surface formation metallic carbide that react, when argon ion sputtering target surface, sputter metallic carbide; The strong plasma body ionization hydrocarbon gas that utilizes target surface glow discharge to produce makes hydrocarbon gas produce the carbon ion of height ionization; The carbon ion of the height ionization that metallic carbide that sputter from target surface and hydrocarbon gas produce forms the metallic carbide dopen Nano composite diamond coating of high rigidity at workpiece surface; Produce the used medium frequency magnetron sputtering target of glow discharge and be also referred to as twin target, promptly by two independently target form jointly, drive by intermediate frequency power supply, two targets are anode and cathode each other, the intermediate frequency power supply frequency is 30KHz; Target back magnetic field of magnets intensity is 300-500 Gauss in 3500-4000 Gauss after decaying to target surface; The field pole of two targets of twin target is opposite; The medium frequency magnetron sputtering target is Ti, Cr or Zr target, target size be width at 100-300mm, length is at 400-1200mm; The electric current of metallic target is at the 5-50 ampere.。
2. preparation method according to claim 1 is characterized in that: the field pole of two targets of twin target is opposite; Two target target surface angles that constitute twin target are 120 degree or face-to-face parallel arrangement.
3. preparation method according to claim 1 and 2 is characterized in that: the quantity of twin target is that 2-8 is right.
4. preparation method according to claim 1 and 2 is characterized in that: described hydrocarbon gas is methane, acetylene or propane.
5. preparation method according to claim 1 and 2 is characterized in that: feeding the hydrocarbon gas flow is 100-1000sccm, and argon flow amount is 30-50sccm.
6. preparation method according to claim 1 and 2 is characterized in that: the metal transfer layer thickness is 30-50nm.
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| CN103129023B (en) * | 2013-02-27 | 2015-08-19 | 武汉大学 | Wear-resisting Si/Si/Si-DLC/DLC self-lubricating coat in use of a kind of inner-walls of duct anticorrosion and preparation method thereof |
| CN105714256A (en) * | 2014-12-05 | 2016-06-29 | 中国科学院大连化学物理研究所 | Method for low-temperature preparation of DLC film through magnetron sputtering |
| CN105420673A (en) * | 2015-12-09 | 2016-03-23 | 上海应用技术学院 | Diamond-like micro-nano coating for rubber mold and preparation method |
| CN107287567B (en) * | 2017-07-11 | 2019-09-27 | 成都天府新区河川科技有限公司 | Droplet ion sputtering technique and hydraulic turbine preparation method |
| CN107937877B (en) * | 2017-11-15 | 2019-11-08 | 温州职业技术学院 | DLC coating apparatus based on anode technology |
| CN109913798B (en) * | 2017-12-13 | 2022-12-23 | 维达力实业(深圳)有限公司 | Surface-hardened graphite mold and surface hardening method thereof |
| CN108251819A (en) * | 2018-01-23 | 2018-07-06 | 温州职业技术学院 | The method of twin load midfrequent AC PECVD deposition DLC coatings |
| CN108330464B (en) * | 2018-02-26 | 2023-10-31 | 温州职业技术学院 | Wire rod diamond-like coating processingequipment |
| CN112791225A (en) * | 2019-11-14 | 2021-05-14 | 美国发现集团有限公司 | Nano robot for tumor treatment and preparation method thereof |
| CN112795880A (en) * | 2019-11-14 | 2021-05-14 | 美国发现集团有限公司 | Preparation method of anti-tumor nano robot |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US5620754A (en) * | 1994-01-21 | 1997-04-15 | Qqc, Inc. | Method of treating and coating substrates |
| CN101113516A (en) * | 2007-08-31 | 2008-01-30 | 武汉大学 | Method for preparing nano composite diamond coating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5620754A (en) * | 1994-01-21 | 1997-04-15 | Qqc, Inc. | Method of treating and coating substrates |
| CN101113516A (en) * | 2007-08-31 | 2008-01-30 | 武汉大学 | Method for preparing nano composite diamond coating |
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