CN103160793B - The preparation method of super thick TiN-TiCN multi-layer compound film material - Google Patents
The preparation method of super thick TiN-TiCN multi-layer compound film material Download PDFInfo
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- CN103160793B CN103160793B CN201110425176.8A CN201110425176A CN103160793B CN 103160793 B CN103160793 B CN 103160793B CN 201110425176 A CN201110425176 A CN 201110425176A CN 103160793 B CN103160793 B CN 103160793B
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Abstract
The invention discloses a kind of preparation method of super thick TiN-TiCN multi-layer compound film material. The TiN-TiCN multi-layer compound film material that the present invention adopts magnetically controlled DC sputtering physical gas phase deposition technology to prepare, this film film thickness is 9.5-24.0 μ m, homogeneous densification, smooth surface, elasticity is good, and tack is good, has high hardness and excellent wear resistance. Can be used on the cutter of machine cuts and boring and the mould of machine-shaping.
Description
Technical field
The present invention relates to a kind of TiN-TiCN multi-layer compound film material with high rigidity and good wear resistanceThe method of material.
Background technology
TiN and TiCN thin-film material are owing to all having high hardness, good resistance to wearing and corrosivity, fabulousChemical stability and excellent characteristic such as good electric conductivity and thermal conductivity etc., therefore in machinery, tribology, preventThe fields such as burn into Aero-Space are with a wide range of applications. TiN-TiCN MULTILAYER COMPOSITE membrane material is except comprehensiveOutside the advantage of the two, by layer thickness control and dislocation effect, make TiN-TiCN MULTILAYER COMPOSITE thinMembrane material internal stress aspect is greatly improved, and its thickness and adhesion are all significantly increased.
At present, the main method of preparation TiN-TiCN multi-layer compound film material has physical vapour deposition (PVD), electrificationLearn deposition, chemical vapour deposition technique etc. In these methods, physical vapour deposition (PVD) uses particularly in industryExtensively, comprising vacuum evaporation, sputter, ion beam and epitaxial growth etc. Magnetically controlled DC sputtering is as sputterIn one of relatively conventional, simple to operate system, be often applied in production. In addition, there is high rigidity and goodThe TiN-TiCN multi-layer compound film material of mar proof has potential application prospect aspect cutter, mould.But the use that realizes ultra-long time still has very large challenge, and can make super thick thin-film material haveExcellent performance is of inadequate achievement especially.
Summary of the invention
Main purpose of the present invention is that to utilize magnetically controlled DC sputtering to prepare super thick and have a high rigidity and good wear-resistingDamage the TiN-TiCN multi-layer compound film material of performance.
Principle of the present invention is that transition zone can reduce not matching relationship between layers effectively; At layer and layerBetween suitable Thickness Ratio and many bimolecular numbers of plies can be avoided the undue concentration of internal stress and cause film de-The generation falling.
The TiN-TiCN multi-layer compound film that the present invention adopts magnetically controlled DC sputtering physical gas phase deposition technology to prepareMaterial, the homogeneous densification of this film, smooth surface, elasticity is good, tack is good, have high hardness andExcellent wear resistance.
Technical scheme of the present invention is, application direct magnetic control equipment is in room temperature, and base material is without under any extra heatingDeposition preparation TiN-TiCN multi-layer compound film material.
A preparation method for super thick TiN-TiCN multi-layer compound film material, is characterized in that the method is concreteStep is:
A, in deposition process, adopts DC magnetron sputtering system equipment;
B is fixed on monocrystalline silicon piece or steel disc on underboarding as base material, then underboarding is loaded into depositionIn chamber, vacuumize; When the vacuum of settling chamber reaches 8.0 × 10-4-6.0×10-4When Pa, logical argon gasIn settling chamber, be to use argon under 60-80%, the pulse direct current back bias voltage condition that is 800-1100V in dutycycle(Ar) plasma carries out sputter clean base material 10-20min;
C is 20-40sccm at argon flow amount, and the distance of target and substrate is 10-15cm, initial cavity room temperatureAt 30-40 DEG C, DC current is 2-4sccm, and dutycycle and back bias voltage are respectively 60-80% and 0-100VUnder condition, by gradual change regulate nitrogen and methane flow, the pure titanium target of sputter, makes TiN-TiCN multilayer multipleClose film, sedimentation time is 100-260min;
After D deposition finishes, chamber temp is 125-135 DEG C, while waiting for chamber temp cool to room temperature, takes outMonocrystalline silicon piece or steel disc.
DC magnetron sputtering system equipment used in the present invention is raw by Shenyang scientific instrument Co., Ltd of the Chinese Academy of SciencesProduce, its model is JS-650. This equipment mainly carries target plate, underboarding, by deposition chambers, oneIndividual dc source, a grid bias power supply and a series of vavuum pump composition, wherein carrying target plate and underboarding is justFace is relative, and dc source is connected to and carries on target plate, and grid bias power supply is connected to underboarding.
The performance of the TiN-TiCN multi-layer compound film material that the present invention obtains:
(1) the TiN-TiCN multi-layer compound film thickness that prepared by the method is 9.5-24.0 μ m, with steel ball andSi3N4Ball is antithesis, and in atmospheric environment, rotating speed is the bar that 600rpm and one way coasting distance are 5mmUnder part, can exceed 11 hours its running time, and not worn out;
(2) the TiN-TiCN multi-layer compound film consistency and elasticity modulus that prepared by the method is respectively20.7-30.1GPa and 299.4-389.2GPa;
(3) the TiN-TiCN multi-layer compound film internal stress little (compression < 0.2GPa) that prepared by the method,Tack is good;
(4) it is fast that the method is prepared TiN-TiCN plural layers sedimentation rate, and can carry out Large-Area-Uniform deposition.
The reason that the present invention has above-mentioned performance is: high DC current is carried the ionization level of sputter gasHeight, sedimentation rate increases; Nitrogen and methane slowly increase gradually the transition that is conducive to interlayer, improved layer withMatching between layer, the adhesive force of enhanced film; The suitable Thickness Ratio of TiN layer and TiCN layer is conducive to subtractThe compression that slow high thickness brings; TiCN layer add the great friction coefficient that has improved TiN film with relativeLow hardness, and the raising that is added with the adhesion that is beneficial to TiCN film of TiN layer and entering of tribological propertyOne-step optimization.
The present invention can be used on the cutter of machine cuts and boring and the mould of machine-shaping.
Detailed description of the invention
In order to understand better the present invention, describe by example.
Embodiment 1:
Clean substrate: use respectively absolute ethyl alcohol and acetone soln ultrasonic cleaning ground (N100 type silicon chip and2520-310S high-temperature steel) each 10min, dry up and be placed in reative cell. Vacuumize: with efficient molecular pump to insteadAnswer chamber to vacuumize. Substrate surface treatment: when vacuum is in 6.0 × 10-4When Pa, lead to argon gas in settling chamber,Be that under the condition of 80% pulse direct current back bias voltage 1100V, to carry out sputter with argon (Ar) plasma clear in dutycycleWash base material 10min, to remove surperficial oxide layer and other impurity. Deposition: argon gas, nitrogen and methane is mixedClose gas and pass in reative cell, be adjusted to 1-5 ° holding back flapper valve (control chamber pressure), target and substrateDistance is 10cm, the back bias voltage 100V that dutycycle is 80%, and initial chamber temp remains on the bar of 40 DEG CUnder part, open dc source (electric current is 4A), the pure titanium target of sputter, regulates nitrogen and methane flow by gradual change,Total sedimentation time is 260min, obtains the bimolecular number of plies and be 30 TiN-TiCN multi-layer compound film.
Utilize field emission scanning electron microscope (FESEM) that thin-membrane section is observed and found, film thickness is23.50 μ m, can significantly observe TiCN layer and TiN layer, and even compact, and base material is in conjunction with good.The analysis of application high-resolution-ration transmission electric-lens obtains TiN layer and shows as many crystalline structures, and TiCN layer shows as non-The structure that crystalline state is mixed with crystalline state. Be pressed into experiment by nanometer and show, the consistency and elasticity modulus of this film respectivelyFor 20.7-22.2GPa and 299.4-301.3GPa. Scratch experiment records high-temperature steel (2520-310S) and filmBetween adhesion be about 24-30N. Use UMT tester for friction between, the load applying is 4N, and operation exceedes11 hours, not worn out yet, it was with Si3N4Ball is that the polishing scratch degree of depth of antithesis ball is about 6 μ m, and taking steel ball asThe polishing scratch degree of depth of antithesis ball is about 12 μ m.
Embodiment 2:
As described in Example 1, total sedimentation time is changed to 180min, obtain the bimolecular number of plies and be 20TiN-TiCN multi-layer compound film.
Utilize field emission scanning electron microscope (FESEM) that thin-membrane section is observed and found, film thickness is16.13 μ m, can significantly observe TiCN layer and TiN layer, and even compact, and base material is in conjunction with good.By nanometer be pressed into experiment show, the consistency and elasticity modulus of this film be respectively 24.4-26.7GPa and338.6-367.7GPa. The adhesion that scratch experiment records between high-temperature steel (2520-310S) and film is about24-30N. Know that by the test of UMT tester for friction between film wear resistance is good.
Embodiment 3:
As described in Example 1, total sedimentation time is changed to 100min, obtain the bimolecular number of plies and be 10TiN-TiCN multi-layer compound film.
Utilize field emission scanning electron microscope (FESEM) that thin-membrane section is observed and found, film thickness is9.68 μ m, can significantly observe TiCN layer and TiN layer, and even compact, and base material is in conjunction with good.By nanometer be pressed into experiment show, the consistency and elasticity modulus of this film be respectively 27.0-30.1GPa and355.0-389.2GPa. The adhesion that scratch experiment records between high-temperature steel (2520-310S) and film is about34-38N. Know that by the test of UMT tester for friction between film wear resistance is good.
Claims (1)
1. a preparation method for super thick TiN-TiCN multi-layer compound film material, is characterized in that the methodConcrete steps are:
A, in deposition process, adopts DC magnetron sputtering system equipment;
B is fixed on monocrystalline silicon piece or steel disc on underboarding as base material, then underboarding is loaded into depositionIn chamber, vacuumize; When the vacuum of settling chamber reaches 8.0 × 10-4-6.0×10-4When Pa, logical argon gasIn settling chamber, be to use argon under 60-80%, the pulse direct current back bias voltage condition that is 800-1100V in dutycyclePlasma carries out sputter clean base material 10-20min;
C is 20-40sccm at argon flow amount, and the distance of target and substrate is 10-15cm, initial cavity room temperatureAt 30-40 DEG C, DC current is 2-4sccm, and dutycycle and back bias voltage are respectively 60-80% and 0-100VUnder condition, by gradual change regulate nitrogen and methane flow, the pure titanium target of sputter, making thickness is 9.5-24.0 μ mThe alternately multi-layer compound film of stack of TiN-TiCN, sedimentation time is 100-260min;
After D deposition finishes, chamber temp is 125-135 DEG C, while waiting for chamber temp cool to room temperature, takes outMonocrystalline silicon piece or steel disc.
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| CN105154880B (en) * | 2015-09-08 | 2018-01-26 | 上海应用技术学院 | Turbo rotor groove milling cutter surface TiCN multi-layer composite coatings preparation technologies |
| CN105220120B (en) * | 2015-10-27 | 2017-06-23 | 中国科学院兰州化学物理研究所 | A kind of method of MULTILAYER COMPOSITE fullerene film industrialization in automobile engine |
| CN107488850A (en) * | 2016-06-13 | 2017-12-19 | 沈阳科蓝纳米涂层技术有限公司 | A kind of preparation method of titanium carbonitride coating |
| CN109652764B (en) * | 2019-01-25 | 2021-01-15 | 广东工业大学 | Bulk cermet material based on PVD technology and preparation method and application thereof |
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| CN101081557A (en) * | 2007-06-26 | 2007-12-05 | 广州有色金属研究院 | Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and method for preparing the same |
| CN101787520A (en) * | 2010-03-24 | 2010-07-28 | 中国地质大学（北京） | Tungsten-titanium co-doped diamond coating material and preparation technique thereof |
| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
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| CN101081557A (en) * | 2007-06-26 | 2007-12-05 | 广州有色金属研究院 | Metallic carbide/adamantine (MeC/DLC) nanometer multi-layer film material and method for preparing the same |
| CN101787512A (en) * | 2009-12-31 | 2010-07-28 | 中国地质大学（北京） | Method for preparing multi-metal element doped diamond film |
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