CN103255373B - A kind of TaVN compound coating and preparation method thereof - Google Patents
A kind of TaVN compound coating and preparation method thereof Download PDFInfo
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- CN103255373B CN103255373B CN201310138383.4A CN201310138383A CN103255373B CN 103255373 B CN103255373 B CN 103255373B CN 201310138383 A CN201310138383 A CN 201310138383A CN 103255373 B CN103255373 B CN 103255373B
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- tavn
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- frictional coefficient
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- 238000000576 coating method Methods 0.000 title claims abstract description 29
- 239000011248 coating agent Substances 0.000 title claims abstract description 28
- 150000001875 compounds Chemical class 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims description 13
- 238000004544 sputter deposition Methods 0.000 claims abstract description 19
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000005516 engineering process Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229910052715 tantalum Inorganic materials 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 20
- 239000002131 composite material Substances 0.000 abstract description 14
- 239000012528 membrane Substances 0.000 abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000758 substrate Substances 0.000 abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- 238000005520 cutting process Methods 0.000 abstract description 7
- 229910052786 argon Inorganic materials 0.000 abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007704 transition Effects 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000003754 machining Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005546 reactive sputtering Methods 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910001315 Tool steel Inorganic materials 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Landscapes
- Cutting Tools, Boring Holders, And Turrets (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of TaVN compound coating, it is characterized in that under the mixed gas atmosphere of nitrogen and argon gas, with metal, Wimet or pottery for matrix, adopt high-purity Ta target and high-purity V target co-sputtering, the atomic percent of V element is 0 ~ 46.7at% and is greater than 0, first at the pure Ta layer of deposition on substrate as transition layer, and then deposit the TaVN composite membrane of 1.5-2 μm.Gained TaVN film hardness is 30-34GPa, and the frictional coefficient under normal temperature is minimum is 0.56, and the frictional coefficient under high temperature is minimum is 0.5.Can be used as the coating of high speed cutting tool and other wear-resisting workpiece of being on active service under the high temperature conditions.
Description
Technical field
What the present invention relates to is a kind of film and preparation method thereof, and specifically the TaVN compound coating of a kind of high rigidity, low-friction coefficient, belongs to ceramic coating technical field.
Background technology
In manufacturing, one of top-priority problem how to improve the efficiency of machining process, under the extreme service condition of such as dry-type processing etc., remains a challenge to the machining of the difficult-to-machine materials such as such as hard tool steel.The principal character of high-performance machining be with the friction surface of workpiece generation adhesion reaction on there is higher temperature and stress, and be easy to the vigorous oxidation be subject to from environment and corrode, and during high speed cutting, temperature can rise to 800 ~ 1000 DEG C, these harsh and extreme external conditions, make to produce the comprehensive phenomenon such as violent local plastic deformation, phase in version, mass transfer and chemical reaction at the tool surface of friction, these extreme working conditions cause the premature failure of cutting tool.Therefore, how to design a kind of thin-film material and can meet extreme service condition, be the target that scholars pursues always.
TaN, as a kind of transition metal nitride, has higher fusing point (3380 DEG C) and higher hardness (1450HV), is suitable as high-abrasive material, can be applicable to the surfaces such as tool and mould as reinforced wear-resistant friction coat.But in order to improve the over-all properties of TaN film surface further, as hardness, oxidation-resistance and wear resistance etc., in its raw material, generally adding another kind of transition metal again form multi-component film, as TiCrN, TiZrN and TaZrN etc.
Through finding the literature search of prior art, the research of TaN base film is mainly concentrated at present to the performance of its electricity aspect.Through the further retrieval to prior art, not yet find the report identical or similar with the technology of the present invention theme at present.
Summary of the invention
The object of the invention is to overcome the above-mentioned problems in the prior art, the TaVN compound coating of a kind of high rigidity, low-friction coefficient is provided, make it be applicable to high speed cutting and DRY CUTTING, and preparation method is convenient to efficient enforcement.
The present invention is achieved by the following technical solutions:
TaVN compound coating, adopts Ta target (purity 99.9%) and V target (purity 99.9%) cosputtering, and the matrix being deposited on metal, Wimet or pottery obtains, and the thickness of TaVN rete is 1 ~ 3 μm.The hardness of this coating is 30 ~ 34GPa, and the frictional coefficient under normal temperature is minimum is 0.56, and the frictional coefficient under high temperature is minimum is 0.5.
Wherein the atomic percent of V element is 0 ~ 46.7at%, show that more excellent scope is 18.25 ~ 46.7at%, be more preferred from 18.25 ~ 32.8at% in conjunction with hardness and frictional coefficient.
TaVN compound coating provided by the invention can adopt reactive sputtering method to prepare, and is specially: adopt reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta and V, and with Ar gas and N in vacuum chamber
2n in oxygen mixture
2solid/liquid/gas reactions generates TaVN, by regulating the sputtering power being added in V target, prepares the TaVN film of different V content, easily controls the content of each component in coating, is convenient to the preparation of coating.
Specifically:
(1) with metal, Wimet or pottery for substrate, clean, ultrasonic, dry in rear fixing rotatable substrate frame in a vacuum chamber;
(2) high-purity Ta target and V target are arranged on two radio-frequency sputtering rifles respectively;
(3) vacuum chamber, passes into highly purified Ar and N in vacuum chamber
2mixed gas, wherein partial pressure of ar gas is (0.5-1.5) × 10
-1pa, nitrogen partial pressure is (2-4) × 10
-2pa, operating air pressure remains on 0.3Pa;
(4) Ta target power output is fixed as 100W, and V target power output is respectively 40-100W, first at the pure Ta layer of deposition on substrate as transition layer, and then deposit the TaVN composite membrane of 1 ~ 3 μm.
The TaVN compound coating obtained has the performance of high rigidity and low-friction coefficient concurrently, for the cutter protection coating and other wear-resistant coatings that are used as high speed cutting and DRY CUTTING in suitability for industrialized production, has very large using value.
Accompanying drawing explanation
Fig. 1 is the microstructure of TaVN composite membrane of the present invention and the graph of a relation of V content; Single TaN film is δ-NaCl face-centred cubic structure, along (200) face preferentially.TaVN film has the face-centred cubic structure similar to individual layer TaN film, and each diffraction peak of the increase along with V content is overall to the skew of wide-angle direction, and preferred orientation is changed into (111) by (200) gradually;
Fig. 2 is the hardness of TaVN composite membrane of the present invention and the graph of a relation of V content; The hardness of the TaVN composite membrane formed after adding V element is all higher than individual layer TaN film, and the lattice distortion that solution strengthening produces is the reason that TaVN composite membrane microhardness increases;
Fig. 3 is under normal temperature, the average friction coefficient of TaVN composite membrane of the present invention and the graph of a relation of V content.Visible, at normal temperatures along with the increase of V content, the frictional coefficient of TaVN composite membrane reduces;
Fig. 4 is that in TaVN composite membrane of the present invention, V content is the average friction coefficient of the composite membrane of 18.25at% and the graph of a relation of experimental temperature.Visible, more than 400 DEG C, along with the rising of temperature, the frictional coefficient of composite membrane also reduces.Major cause defines the Magn é li phase V with self-lubricating function in friction contact
2o
5.
Embodiment
Adopt JGP-450 type multi-target magnetic control sputtering instrument to prepare film, monocrystalline silicon piece and stainless steel substrate deposit TaVN laminated film.Be arranged on two radio-frequency sputtering rifles respectively by Ta target (purity 99.9%) and V target (purity 99.9%), the spacing of substrate frame and sputter gun is 78mm.Substrate is after acetone and raw spirit ultrasonic cleaning, and flash baking loads in the rotatable substrate frame in vacuum chamber.Vacuum chamber base vacuum is better than 6 × 10
-4pa.Ar and N that purity is 99.999% is passed in vacuum chamber
2mixed gas, wherein partial pressure of ar gas is 1 × 10
-1pa, nitrogen partial pressure is 3 × 10
-2pa, operating air pressure remains on 0.3Pa.In the process of preparation TaVN film, Ta target power output is fixed as 100W, and V target power output is respectively 40,70 and 100W, thus prepares the TaVN composite membrane of a series of different V content.Before preparation TaN unitary film and TaVN composite membrane, on substrate, deposit the pure Ta of about 100nm in advance as transition layer, and then deposit the unitary film of TaN and the TaVN composite membrane of about 1 ~ 3 μm.
TaVN compound coating provided by the invention can adopt at Ar, N
2the method preparation of reactant physical vapor deposition in mixed gas.Such as two targets (being respectively Ta target, V target) are prepared from by reactive sputtering method.
Embodiment is provided below in conjunction with content of the present invention:
Example one
Ta target power output 100W, V target power output 0W, preparation TaN single coating.
Adopt reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta, and with Ar gas and N in vacuum chamber
2n in oxygen mixture
2solid/liquid/gas reactions generates Ta-N coating.The hardness of coating is 27.8GPa, and thickness is 1 ~ 3 μm, and when frictional coefficient when normal temperature frictional coefficient is 0.66,600 DEG C is 0.8,800 DEG C, frictional coefficient is 0.7.
Example two
Ta target power output 100W, V target power output 40W, preparation Ta
0.82v
0.18n compound coating.
Adopt reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta and V, and with Ar gas and N in vacuum chamber
2n in oxygen mixture
2solid/liquid/gas reactions generates TaVN compound coating.The hardness of coating is 32.305GPa, and thickness is 1 ~ 3 μm, and when frictional coefficient when normal temperature frictional coefficient is 0.64,600 DEG C is 0.65,800 DEG C, frictional coefficient is 0.5.
Example three
Ta target power output 100W, V target power output 70W, preparation Ta
0.67v
0.33n compound coating.
Adopt reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta and V, and with Ar gas and N in vacuum chamber
2n in oxygen mixture
2solid/liquid/gas reactions generates TaVN compound coating.The hardness of coating is 30.215GPa, and thickness is 1-3 μm, and when normal temperature frictional coefficient is 0.58,800 DEG C, frictional coefficient is 0.56.
Example four
Ta target power output 100W, V target power output 100W, preparation Ta
0.53v
0.47n compound coating.
Adopt reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta and V, and with Ar gas and N in vacuum chamber
2n in oxygen mixture
2solid/liquid/gas reactions generates TaVN compound coating.The hardness of coating is 29.472GPa, and thickness is 1 ~ 3 μm, and when normal temperature frictional coefficient is 0.56,800 DEG C, frictional coefficient is 0.51.
Through contriver's practice, in the mixed gas of argon gas and nitrogen, partial pressure of ar gas is (0.5-1.5) × 10
-1pa, nitrogen partial pressure is (2-4) × 10
-2within the scope of Pa, operating air pressure remains on 0.3Pa, all can realize above-mentioned experimentation, and the thickness all meeting gained TaVN rete is 1 ~ 3 μm, and hardness is 30-34GPa, and the frictional coefficient under normal temperature is minimum is 0.56, and the frictional coefficient under high temperature is minimum is 0.5.
Claims (2)
1.TaVN compound coating, it is characterized in that adopting high-purity Ta target and high-purity V target co-sputtering, the matrix being deposited on metal, Wimet or pottery obtains, the thickness of TaVN rete is 1-3 μm, hardness is 30-34GPa, frictional coefficient under normal temperature is minimum is 0.56, and the frictional coefficient under high temperature is minimum is 0.5; Wherein the atomic percent of V element is 18.25 ~ 32.8at%; The purity of high-purity Ta target and high-purity V target is 99.9%.
2. the preparation method of TaVN compound coating according to claim 1, it is characterized in that adopting reaction magnetocontrol sputtering technology by radio frequency cathode sputtering metal Ta and V, and with Ar gas and N in vacuum chamber
2n in mixed gas
2solid/liquid/gas reactions generates TaVN, by regulating the sputtering power being added in V target, prepares the TaVN film of different V content.
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| CN201310138383.4A CN103255373B (en) | 2013-04-19 | 2013-04-19 | A kind of TaVN compound coating and preparation method thereof |
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| CN201310138383.4A CN103255373B (en) | 2013-04-19 | 2013-04-19 | A kind of TaVN compound coating and preparation method thereof |
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| CN103255373B true CN103255373B (en) | 2015-08-12 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952672B (en) * | 2014-03-12 | 2016-10-12 | 江苏科技大学 | TaCN hard nanometer structural membrane and preparation method |
| CN104060231A (en) * | 2014-06-13 | 2014-09-24 | 江苏科技大学 | TaN-Ag hard thin film and preparation method |
| CN105695933A (en) * | 2016-01-29 | 2016-06-22 | 江苏科技大学 | Niobium-vanadium-silicon-nitrogen nano hard film and preparation method |
| CN107841719A (en) * | 2017-11-03 | 2018-03-27 | 江苏科技大学 | A kind of TaMgN composite coatings and its preparation method and application |
| CN107841720A (en) * | 2017-11-03 | 2018-03-27 | 江苏科技大学 | A kind of ZrMgN nano structure membranes and its preparation method and application |
| CN107794504A (en) * | 2017-11-07 | 2018-03-13 | 东南大学 | TiZrTaN coated cutting tools and preparation method thereof |
| CN112481591B (en) * | 2020-11-11 | 2023-03-24 | 中国科学院宁波材料技术与工程研究所 | Self-adaptive high-low temperature cycle resistant low-friction functional protective coating and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102994945A (en) * | 2012-11-19 | 2013-03-27 | 江苏科技大学 | ZrVN nano composite membrane and preparation method thereof |
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| CN102994945A (en) * | 2012-11-19 | 2013-03-27 | 江苏科技大学 | ZrVN nano composite membrane and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 调制周期对TaN/VN纳米多层膜的影响;张学华等;《真空科学与技术学报》;20071031;第27卷(第5期);第367页-369页 * |
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Address after: 212028 Zhenjiang, Dantu Metro Industrial Park Rui East Road, No. 9 Patentee after: JIANGSU University OF SCIENCE AND TECHNOLOGY Address before: 212003 Zhenjiang City, Jiangsu province dream Creek Road, No. 2 Patentee before: Jiangsu University of Science and Technology |
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Granted publication date: 20150812 |