CN102650030A - TiMoN hard nanostructure film and preparation method thereof - Google Patents
TiMoN hard nanostructure film and preparation method thereof Download PDFInfo
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- CN102650030A CN102650030A CN2012101515824A CN201210151582A CN102650030A CN 102650030 A CN102650030 A CN 102650030A CN 2012101515824 A CN2012101515824 A CN 2012101515824A CN 201210151582 A CN201210151582 A CN 201210151582A CN 102650030 A CN102650030 A CN 102650030A
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- timon
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- nanostructure film
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- 241000946381 Timon Species 0.000 title claims abstract description 29
- 239000002086 nanomaterial Substances 0.000 title abstract description 8
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 16
- 238000004544 sputter deposition Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000919 ceramic Substances 0.000 claims abstract description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 5
- 229910052786 argon Inorganic materials 0.000 claims abstract description 4
- 239000012495 reaction gas Substances 0.000 claims abstract description 3
- 239000010936 titanium Substances 0.000 claims description 40
- 239000010408 film Substances 0.000 claims description 36
- 238000002474 experimental method Methods 0.000 claims description 20
- 239000000758 substrate Substances 0.000 claims description 20
- 239000012528 membrane Substances 0.000 claims description 16
- 239000011159 matrix material Substances 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- 229910052719 titanium Inorganic materials 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 5
- 230000007704 transition Effects 0.000 claims description 4
- PWKWDCOTNGQLID-UHFFFAOYSA-N [N].[Ar] Chemical compound [N].[Ar] PWKWDCOTNGQLID-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 239000000956 alloy Substances 0.000 abstract 2
- 229910045601 alloy Inorganic materials 0.000 abstract 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- QFUKUPZJJSMEGE-UHFFFAOYSA-N 5-(hydroxymethyl)-1-(3-methylbutyl)pyrrole-2-carbaldehyde Chemical compound CC(C)CCN1C(CO)=CC=C1C=O QFUKUPZJJSMEGE-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910010037 TiAlN Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
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Abstract
The invention discloses a TiMoN hard nanostructure film and a preparation method thereof. The TiMoN hard nanostructure film is prepared by being deposited onto hard alloy or a ceramic basal body through a double target confocal radio frequency reaction sputtering method. The molecular formula of the TiMoN hard nanostructure film is represented by (TixMo1-x)N, wherein x is 25.67-70.13 at.%. The thickness of the TiMoN hard nanostructure film is 2-3 mu m. The maximum hardness of the TiMoN hard nanostructure film is 36.37 GPa. In a dry cutting test, the minimum friction coefficient is 0.3917 and the minimum wear rate is 1.270*10<-8> mm<3>/Nmm. The TiMoN hard nanostructure film is deposited on the hard alloy or the ceramic basal body through the double target confocal radio frequency reaction sputtering method, the vacuum degree is less than 6.0*10<-4> Pa in the depositing process, and the depositing process is carried out by taking argon gas as starting arc and nitrogen gas as reaction gas.
Description
Technical field
The present invention relates to a kind of coating and preparation method thereof, particularly a kind of TiMoN hard nanometer structural membrane and preparation method thereof belongs to the ceramic coating technical field.
Background technology
The development of modern processing; Cutter coat has been proposed such as higher service demand such as " high-speed and high-temperature ", " high precision ", " high reliability ", " long lifetives "; Except requiring coating to have the high-temperature oxidation resistance of the due high firmness of ordinary cutting tool coating, excellence, more need coating to have the excellent friction polishing machine.Yet though existing cutter coat all has higher hardness, their friction and wear behavior is undesirable, is difficult to satisfy the service condition harsh like high speed, DRY CUTTING etc.Traditional binary coating such as TiN can not be competent at the requirement of contemporary processing manufacturing industry to the cutter service condition fully.For example, the hardness of at present the most frequently used TiN coating is about 23GPa, and its frictional coefficient is about 0.9; Though the TiAlN coating hardness is up to 40GPa, friction and wear behavior is relatively poor, and its frictional coefficient is about 1.0.Therefore, compare with the desired desirable high firmness anti-attrition wear-resistant coating of contemporary processing manufacturing industry, the friction and wear behavior of this type of hard coat still has gap.Produce at present to go up and be badly in need of a kind of instrument coating that can have high firmness and good friction and wear behavior concurrently.
Recently research shows that the MoN film has higher hardness, stable mechanical property, and the Mo element forms in frictional wear experiment easily has the low Magn é li phase MoO of modulus that clips and pastes
3, have good Wear-resistant effect, in the frictional wear element, have industrial application value.Yet, there are some researches show that the nitride of the Mo for preparing under the PVD condition exists like γ-Mo
2N, B1-MoN, many kinds of phase structures of δ-MoN, its phase structure changes noticeably with the difference of preparation technology parameter.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of TiMoN hard nanometer structural membrane and preparation method thereof is provided.It is shortcomings such as hard nanometer structure composite package and multilayer film friction and wear behavior be undesirable that the present invention has overcome existing TiN; Have than high efficiency; Have high firmness and excellent friction and wear behavior concurrently, can be used as the nanostructure ganoine thin film of high speed, DRY CUTTING.
The present invention realizes through following technical scheme: a kind of TiMoN hard nanometer structural membrane, film adopt two confocal RF-reactively sputtered titanium methods of target to be deposited on wimet or the ceramic matrix and prepare, and described divided thin film minor is expressed as (Ti
xMo
1-x) N, x=25.67～70.13at. ﹪ wherein, film thickness is at 2-3 μ m, and the film maximum hardness is 36.37GPa, and under the dried cutting experiment, minimum frictional coefficient is 0.3917, and the minimal wear rate is 1.270 * 10
-8Mm
3/ Nmm.
The relative content 1-x of film Mo is 29.87～74.33at.%.
The method for preparing described TiMoN hard nanometer structural membrane is utilized the two confocal RF-reactively sputtered titanium method of target depositing Ti MoN hard nanometer structural membranes on wimet or ceramic matrix, and during deposition, vacuum tightness is＜6.0 * 10
-4Pa, with the argon gas starting the arc, nitrogen is that reaction gas deposits.
The Ti of deposition 200nm is a transition layer earlier on matrix.
Substrate temperature is set on demand, from room temperature to 200 ℃, sputtering pressure 0.3Pa, argon nitrogen throughput ratio 10/3, and Ti target sputtering power 250W, Mo target sputtering power is 30～250W.
Ti target power output 250W, Mo target power output 150W.
Beneficial effect:
1.TiMoN film is a face-centred cubic structure, and is similar with the TiN phase structure.With the rising of Mo content, preferred orientation changes (200) into by (111).Its microhardness significantly raises with the increase of Mo content, is up to 36.37GPa.
2.TiMoN the rising of the The friction coefficient Mo content of film and reducing, last frictional coefficient reaches a stationary value, and roughly about 0.4, the wear resisting property of TiMoN film is excellent, and the minimal wear rate is 8 * 10
-8Mm
3/ Nmm.
Description of drawings
Fig. 1 is the variation relation of TiMoN film microhardness of the present invention with Mo content;
Fig. 2 concerns with the Mo content for average friction coefficient under the dried cutting experiment of TiMoN film of the present invention;
Fig. 3 concerns with the Mo content for wear rate under the dried cutting experiment of TiMoN film of the present invention.
Embodiment:
TiMoN hard nanometer structural membrane molecular formula of the present invention is expressed as (Ti
xMo
1-x) N.Adopt high-purity Ti target and the confocal RF-reactively sputtered titanium of Mo target; Be deposited on wimet such as rapid steel or the ceramic matrix; The thickness of TiMoN hard nanometer structural membrane is 2～3 μ m; Ti content (x) is between 25.67～70.13at. ﹪ in the film, and Mo content (1-x) is between 29.87～74.33at. ﹪.This hard coat can obtain the high firmness of 36.37GPa, has excellent friction and wear behavior concurrently, and under the dried cutting experiment, its minimum frictional coefficient is 0.3917, and the minimal wear rate is 1.270 * 10
-8Mm
3/ Nmm.
Preparing method of the present invention, specific as follows:
The preparation of TiMoN film is accomplished on the compound high-vacuum multi-target magnetic control sputtering equipment of JGP450.This magnetic control sputtering device has three sputtering targets, is installed in respectively on the target support of three water-cooleds, and three stainless steel baffle plates are placed in three target fronts respectively, control automatically through computer.Mo target (purity is 99.95%) and Ti target (purity is 99.9%) are installed in respectively independently on the radio frequency negative electrode, and the target diameter is 75mm.Mirror polish is made on wimet such as rapid steel or ceramic matrix surface handled, feed high-purity Ar (99.999%) and N
2(99.999%), generates TiMoN hard nanometer structural membrane through on the matrix of wimet such as rapid steel or pottery, adopting pure Ti and pure Mo target to carry out the confocal RF-reactively sputtered titanium method deposition of two targets.Before the depositing Ti MoN film, isolate substrate and ion district through baffle plate, Ti target and Mo target carry out 10 minutes preparatory sputter.Then on substrate in advance deposit thickness be about the Ti transition layer of 200nm.Sputtering time is fixed as 2h, and film thickness is 2-3 μ m.
Wherein, selecting substrate for use is that the film of monocrystalline silicon piece carries out the research of composition, phase structure; Selecting substrate for use is that stainless composite package carries out microhardness and Study on Friction and Wear.Substrate material is used absolute ethyl alcohol and acetone ultrasonic cleaning 15min respectively, on the rotatable substrate frame in the Vakuumkammer of packing into after drying up with warm air.Target is 11cm to the fixed distance of substrate.Vakuumkammer base vacuum degree is superior to 6.0 * 10
-4In Vakuumkammer, feed earlier purity behind the Pa and be 99.999% the argon gas starting the arc; Isolate substrate and ion district through baffle plate; Each target carries out the preparatory sputter of 10min to remove the oxide impurity of target material surface, feeds purity then and is 99.999% nitrogen and deposit as reactant gases.At the Ti transition layer about preparatory sputter 200nm on the substrate, to strengthen film-substrate cohesion.Substrate temperature remains 200 ℃.Fixedly sputtering pressure (0.3Pa), argon nitrogen throughput ratio (10/3) and Ti target sputtering power (250W), Mo target sputtering power is 30～250W, through changing the TiMoN film that Mo target sputtering power prepares a series of different Mo content.
Below in conjunction with content of the present invention embodiment is provided:
Embodiment 1
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 30W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 70.13at.% in the film at this moment, and Mo content is 29.87at.%.The film microhardness is 22.20GPa.Under the dried cutting experiment, average friction coefficient is 0.5754, and wear rate is 1.335 * 10
-6Mm
3/ Nmm.
Embodiment 2
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 50W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 57.30at.% in the film at this moment, and Mo content is 42.70at.%.The film microhardness is 24.76GPa.Under the dried cutting experiment, average friction coefficient is 0.5736, and wear rate is 1.270 * 10
-8Mm
3/ Nmm.
Embodiment 3
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 70W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 48.57at.% in the film at this moment, and Mo content is 51.43at.%.The film microhardness is 23.60GPa.Under the dried cutting experiment, average friction coefficient is 0.5733, and wear rate is 2.110 * 10
-8Mm
3/ Nmm.
Embodiment 4
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 90W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 35.89at.% in the film at this moment, and Mo content is 64.11at.%.The film microhardness is 23.80GPa.Under the dried cutting experiment, average friction coefficient is 0.5347, and wear rate is 3.170 * 10
-8Mm
3/ Nmm.
Embodiment 5
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 150W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 31.65at.% in the film at this moment, and Mo content is 68.35at.%.The film microhardness is 28.37GPa.Under the dried cutting experiment, average friction coefficient is 0.3933, and wear rate is 5.900 * 10
-8Mm
3/ Nmm.
Embodiment 6
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 200W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 26.85at.% in the film at this moment, and Mo content is 73.15at.%.The film microhardness is 36.30GPa.Under the dried cutting experiment, average friction coefficient is 0.3917, and wear rate is 7.110 * 10
-7Mm
3/ Nmm.
Embodiment 7
The main experiment parameter of the present invention is Ti target power output 250W, and the Mo target power output is 230W, and substrate temperature remains under 200 ℃ of conditions.Ti content is 25.67at.% in the film at this moment, and Mo content is 74.33at.%.The film microhardness is 34.80GPa.Under the dried cutting experiment, average friction coefficient is 0.3950, and wear rate is 3.244 * 10
-6Mm
3/ Nmm.
Claims (6)
1. TiMoN hard nanometer structural membrane, film adopt two confocal RF-reactively sputtered titanium methods of target to be deposited on wimet or the ceramic matrix and prepare, and it is characterized in that described divided thin film minor is expressed as (Ti
xMo
1-x) N, x=25.67～70.13at. ﹪ wherein, film thickness is at 2-3 μ m, and the film maximum hardness is 36.37GPa, and under the dried cutting experiment, minimum frictional coefficient is 0.3917, and the minimal wear rate is 1.270 * 10
-8Mm
3/ Nmm.
2. TiMoN hard nanometer structural membrane according to claim 1 is characterized in that the relative content 1-x of film Mo is 29.87～74.33at.%.
3. prepare the method for the described TiMoN hard nanometer of claim 1 structural membrane, it is characterized in that, utilize the two confocal RF-reactively sputtered titanium method of target depositing Ti MoN hard nanometer structural membranes on wimet or ceramic matrix, during deposition, vacuum tightness is＜6.0 * 10
-4Pa, with the argon gas starting the arc, nitrogen is that reaction gas deposits.
4. the method for preparing TiMoN hard nanometer structural membrane according to claim 3 is characterized in that, the Ti of deposition 200nm is a transition layer earlier on matrix.
5. the method for preparing TiMoN hard nanometer structural membrane according to claim 3 is characterized in that substrate temperature is set on demand; From room temperature to 200 ℃; Sputtering pressure 0.3Pa, argon nitrogen throughput ratio 10/3, Ti target sputtering power 250W, Mo target sputtering power is 30～250W.
6. the method for preparing TiMoN hard nanometer structural membrane according to claim 5 is characterized in that, Ti target power output 250W, Mo target power output 150W.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101519252B1 (en) * | 2013-12-05 | 2015-05-11 | 현대자동차주식회사 | METHOD FOR COATING TiAgMoN LAYER |
| KR101583882B1 (en) * | 2013-12-13 | 2016-01-12 | 현대자동차주식회사 | METHOD FOR COATING TiAgMoN LAYER |
| CN105695932A (en) * | 2016-01-29 | 2016-06-22 | 江苏科技大学 | Titanium-yttrium-nitrogen nano-hard film and preparation method thereof |
| RU2644094C1 (en) * | 2016-12-13 | 2018-02-07 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | METHOD OF OBTAINING ADAPTIVE WEAR-RESISTANT Ti-Al-Mo-N COATING FOR PROTECTING FROM WEARING IN VARIABLE FREQUENCY CONDITIONS |
| CN108884553A (en) * | 2016-03-29 | 2018-11-23 | 大同特殊钢株式会社 | Titanium alloy overlay film and titanium alloy target |
| US20180369927A1 (en) * | 2017-06-27 | 2018-12-27 | Tungaloy Corporation | Coated cutting tool |
| CN111455318A (en) * | 2020-06-01 | 2020-07-28 | 中国科学院兰州化学物理研究所 | A kind of molybdenum nitride/molybdenum disulfide/silver ternary composite high temperature solid lubricating film and preparation method thereof |
-
2012
- 2012-05-15 CN CN2012101515824A patent/CN102650030A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 王秀贤: "Ti-Mo-N纳米结构复合膜的微结构与性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101519252B1 (en) * | 2013-12-05 | 2015-05-11 | 현대자동차주식회사 | METHOD FOR COATING TiAgMoN LAYER |
| KR101583882B1 (en) * | 2013-12-13 | 2016-01-12 | 현대자동차주식회사 | METHOD FOR COATING TiAgMoN LAYER |
| CN105695932A (en) * | 2016-01-29 | 2016-06-22 | 江苏科技大学 | Titanium-yttrium-nitrogen nano-hard film and preparation method thereof |
| CN108884553A (en) * | 2016-03-29 | 2018-11-23 | 大同特殊钢株式会社 | Titanium alloy overlay film and titanium alloy target |
| RU2644094C1 (en) * | 2016-12-13 | 2018-02-07 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | METHOD OF OBTAINING ADAPTIVE WEAR-RESISTANT Ti-Al-Mo-N COATING FOR PROTECTING FROM WEARING IN VARIABLE FREQUENCY CONDITIONS |
| US20180369927A1 (en) * | 2017-06-27 | 2018-12-27 | Tungaloy Corporation | Coated cutting tool |
| US10751805B2 (en) * | 2017-06-27 | 2020-08-25 | Tungaloy Corporation | Coated cutting tool |
| CN111455318A (en) * | 2020-06-01 | 2020-07-28 | 中国科学院兰州化学物理研究所 | A kind of molybdenum nitride/molybdenum disulfide/silver ternary composite high temperature solid lubricating film and preparation method thereof |
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Application publication date: 20120829 |