CN104862648B - A kind of excellent MoS of wear Characteristics2Ti composite membranes and preparation method thereof - Google Patents
A kind of excellent MoS of wear Characteristics2Ti composite membranes and preparation method thereof Download PDFInfo
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- CN104862648B CN104862648B CN201510331855.7A CN201510331855A CN104862648B CN 104862648 B CN104862648 B CN 104862648B CN 201510331855 A CN201510331855 A CN 201510331855A CN 104862648 B CN104862648 B CN 104862648B
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Abstract
The invention belongs to metal material surface lubricating modification solid lubricant coating technical field, and in particular to a kind of excellent MoS of wear Characteristics2Ti composite membranes and preparation method thereof, i.e., it is a kind of to significantly improve the MoS of composite membrane wear Characteristics in atmospheric environment2‑TiL/MoS2‑TiHNano-stack composite membrane.MoS of the present invention2‑TiL/MoS2‑TiHThe low MoS of nano-stack composite membrane amount containing Ti2‑TiLFilm and the high MoS of amount containing Ti2‑TiHWhat the alternating deposit of film was constituted, it can not only prevent film from being in the form of a column growth, but also MoS can be made2‑TiLWith MoS2‑TiHIt is mutually mixed, the growing of column crystal, scattered stress in thin film can be suppressed, suppress film layer bulk and come off, improve consistency, so as to improve the wear Characteristics of composite membrane.
Description
Technical field
The invention belongs to metal material surface lubricating modification solid lubricant coating technical field, and in particular to a kind of anti-friction
MoS2-Ti composite membranes of excellent performance and preparation method thereof are damaged in scouring.
Background technology
It is used as the transition metal sulfide with layer structure, MoS2It is a kind of extensive with good greasy property
The solid lubricant of application.MoS2Lubricant effect is more notable in vacuum environment, and its Magnetron Sputtering Thin Film material is usually used in
The surface lubrication modification of spacecraft precision movable part such as bearing.The pure MoS prepared using magnetron sputtering2Film is in the form of a column
Grow and with loose vermiform surface texture, hardness also than relatively low, easily occurs in atmospheric environment with oxygen and water
Reaction generation MoO3, change film crystal structure, ultimately result in film and lose greasy property, thus it is moist in air to limit it
Application in environment.For pure MoS2The defect of film, researcher is by mixing PbO, Sb2O3Deng oxide and Ti, Au,
The metals such as Nb, Pb, Cr, Zr, Ni, W improve MoS2Greasy property of the film in air wet environment.In MoS2Group compound film
In numerous ameliorative ways of moisture-resistance, magnetron sputtering MoS2- Ti composite membranes are one of which excellent performances and had extensive
The solid lubricant of application prospect, the surface available for mechanical movable part such as gear, bearing etc. is modified.
For MoS2The research that-Ti composite membranes are carried out is more, according to the difference of preparation method, mainly there is alternating deposit
MoS2/ Ti formation sandwich construction composite membranes and cosputtering MoS2The two ways such as target, Ti targets formation compound composite membrane.For
MoS2/ Ti multilayer complex films, multi-layer film structure can effectively prevent composite membrane from being in the form of a column growth, simultaneously because interfacial effect can
To improve the hardness of composite membrane, thus anti-wear performance of the composite membrane in air wet environment can be improved.For MoS2- Tiization
Compound composite membrane, the addition of Ti elements can not only improve the consistency of composite membrane, but also can improve the hardness of composite membrane,
Ti oxidations generate TiO in composite membrane simultaneously2Diaphragm is formed on surface afterwards and prevents further diffusion of the oxygen in composite membrane, so that
Improve its wear Characteristics in wet environment.It also found simultaneously, the content of Ti elements is to composite membrane in composite membrane
Properties also have large effect.With the increase of Ti constituent contents, structure of composite membrane is finer and close, surface more light
Clean, stronger with substrate adhesion, hardness, wear Characteristics, antioxygenic property and the moisture resistance performance of composite membrane are also obtained
Improve.But, MoS2- Ti composite membranes wear Characteristics do not improve always with the increase of Ti constituent contents.Work as Ti
Element increases to after certain value, and its wear Characteristics declines.Research shows, with the continuation increase of Ti constituent contents, meeting
Generate more TiO2, although composite membrane antioxygenic property in wet environment can be improved, but can contain lubricant component simultaneously
Quantitative change is few so that composite membrane coefficient of friction rises, and ultimately results in composite membrane and loses greasy property.The building ring of mechanical movable part
Border is often complicated and changeable, and this requires lubriation material to possess good environmental suitability, to ensure mechanical part not
With normal work in environment.In MoS2In-Ti composite membranes, although the incorporation of Ti elements can improve its resisting in atmospheric environment
Friction and wear behavior, but with the increase of Ti elements, greasy property is but lost while combination property is improved, can not
Meet requirement of the mechanical movable part working environment complicated and changeable to solid lubricant coating.Therefore, how further to improve
MoS2Wear Characteristics of-Ti the composite membranes in atmospheric environment, are that composite membrane realizes wide variety of key.
The content of the invention
The present invention is exactly to solve MoS2There is provided a kind of wear Characteristics are excellent for the deficiency of the compound film properties of-Ti
MoS2- Ti composite membranes and preparation method thereof, i.e., a kind of MoS2-TiL/MoS2-TiHNano-stack composite membrane, can be significantly improved
Wear Characteristics of the composite membrane in atmospheric environment.
The present invention relates to the MoS that a kind of wear Characteristics are excellent2- Ti composite membranes, adopt and prepare with the following method:First
Matrix is successively placed on progress ultrasonic wave cleaning in acetone, alcohol;Then, using magnetron sputtering technique, work is used as using argon gas
Gas, in advance in substrate deposit transition zone;Then, cosputtering Ti targets, MoS are passed through2Target, changes Ti target power outputs, realizes and contains Ti
The low MoS of amount2-TiLFilm and the high MoS of amount containing Ti2-TiHFilm(That is MoS2-TiL/MoS2-TiH)Alternating deposit, adjust work
Make the parameters such as pressure, depositing temperature and total sedimentation time, the excellent MoS of wear Characteristics is prepared on matrix2-
TiL/MoS2-TiHNano-stack composite membrane.
Described matrix is metal material, usually mechanical movable part.
Described ultrasonic wave scavenging period is generally 10-30min, specifically depending on matrix situation.
Described magnetron sputtering technique includes other deriving technologies such as ion arc plating, the closed Nonequilibrium magnetic of sputtering technology
Control sputtering, the injection of gas ions immersion ion and the technology such as deposition, high-power impulse magnetron sputtering.
Described transition zone is metal and its alloy firm transition zones such as Ti, Al, and thickness is typically between 100-1000nm.
Described Ti target power outputs, in the low MoS of deposition amount containing Ti2-TiLCorrespondence Ti target power outputs are low during film, deposit amount containing Ti
High MoS2-TiHCorrespondence Ti target power outputs are high during film, depending on specific performance number is according to equipment situation.
Described operating pressure, sets according to distinct device and technology, typically between 0.5-2Pa.
Described depositing temperature can be room temperature or hyperthermia temperature range between 20-600 degrees Celsius.
MoS in described nano-stack composite membrane2-TiL、MoS2-TiHThickness and thickness ratio can be by controlling individual layer
Sedimentation time is controlled, and the thickness of composite membrane is by sedimentation time control, thickness is typically between 300-2000nm.
MoS of the present invention2-TiL/MoS2-TiHThe low MoS of nano-stack composite membrane amount containing Ti2-TiLFilm and containing Ti
The high MoS of amount2-TiHWhat the alternating deposit of film was constituted, it can not only prevent film from being in the form of a column growth, but also can make
MoS2-TiLWith MoS2-TiHBe mutually mixed, can suppress the growing of column crystal, scattered stress in thin film, suppress film layer bulk come off,
Consistency is improved, so as to improve the wear Characteristics of composite membrane.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention;
As illustrated, in figure:1 is that matrix 2 is that transition zone 3 is MoS2-TiLFilm 4 is MoS2-THFilm;
Fig. 2 is composite film surface shape appearance figure prepared by the present invention;
Fig. 3 is composite membrane and MoS prepared by the present invention2-TiLCoefficient of friction of the composite membrane under the conditions of same test;
As illustrated, in figure:1 is that the coefficient of friction 2 of composite membrane prepared by the present invention is MoS2-TiLThe friction of composite membrane
Coefficient.
Fig. 4 is composite membrane and MoS prepared by the present invention2-TiLWear trace of the composite membrane under the conditions of same test;
As illustrated, in figure:1 is that the wear trace 2 of composite membrane prepared by the present invention is MoS2-TiLThe abrasion of composite membrane
Vestige.
Embodiment
Following embodiment is further illustrating for the present invention, rather than limits the application of the present invention.
Embodiment 1
Each ultrasonic wave that carries out is successively placed in acetone, alcohol to stainless steel base first and cleans 10min;Then, using magnetic
Sputtering technology is controlled, using argon gas as working gas, it is 100W to set Ti target power outputs, in 0.8Pa operating pressure and room temperature condition
Under, 20min is deposited, one layer of Ti transition zone is deposited on stainless steel in advance;Then, Ti target power outputs are arranged to 50W, 100W alternating
Change, MoS2Target is 100W, passes through cosputtering Ti targets, MoS2Target, under 0.8Pa operating pressure and room temperature condition, deposition
120min, prepares the excellent MoS of wear Characteristics on stainless steel2-TiL/MoS2-TiHNano-stack composite membrane.For
The composite membrane wear Characteristics relatively more of the invention that prepare, are 50W, MoS in Ti target power outputs2Target is 100W sputtering power
Under, it is prepared for custom doped MoS2- Ti composite membranes, in order to distinguish the high MoS of amount containing Ti for having lost greasy property2-TiHIt is multiple
Film is closed, such composite membrane is designated as MoS2-TiLComposite membrane.Composite film surface shape appearance figure prepared by the present invention is shown in Fig. 2, present invention system
Standby composite membrane and MoS2-TiLPVvalue testing data of the composite membrane under the conditions of same test are shown in Fig. 3, prepared by the present invention
Composite membrane and MoS2-TiLWear trace wear trace of the composite membrane under the conditions of same test is shown in Fig. 4.
Claims (1)
1. a kind of excellent MoS of wear Characteristics2- Ti is combined membrane preparation method, it is characterised in that described preparation method tool
There is following process:Each ultrasonic wave that carries out is successively placed in acetone, alcohol to stainless steel base first and cleans 10min;Then, use
Magnetron sputtering technique, using argon gas as working gas, it is 100W to set Ti target power outputs, in 0.8Pa operating pressure and room temperature bar
Under part, 20min is deposited, one layer of Ti transition zone is deposited on stainless steel in advance;Then, Ti target power outputs are arranged into 50W, 100W to hand over
For change, MoS2Target is 100W, passes through cosputtering Ti targets, MoS2Target, under 0.8Pa operating pressure and room temperature condition, deposition
120min, prepares the excellent MoS of wear Characteristics on stainless steel2-TiL/MoS2-TiHNano-stack composite membrane.
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CN106086990B (en) * | 2016-08-04 | 2019-02-01 | 北京工业大学 | A kind of method of the immobilized molybdenum disulfide of porous titania thin films |
CN106521441B (en) * | 2016-11-16 | 2018-10-19 | 中国科学院宁波材料技术与工程研究所 | A kind of molybdenum disulfide/lead titanium alloy nano plural layers and preparation method thereof |
CN107841717B (en) * | 2017-10-18 | 2019-08-02 | 吉林大学 | A kind of low-friction coefficient MoS2Base Metal-oxide composite solid lubrication film preparation method |
CN110331370A (en) * | 2019-07-25 | 2019-10-15 | 清华大学 | A kind of molybdenum-disulfide radical complex multi layer films and preparation method thereof |
CN114086137B (en) * | 2021-11-18 | 2022-07-15 | 中国地质大学(北京) | Rotating joint pin applied to spacecraft mechanism and preparation method thereof |
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US6423419B1 (en) * | 1995-07-19 | 2002-07-23 | Teer Coatings Limited | Molybdenum-sulphur coatings |
CN1718857A (en) * | 2005-08-11 | 2006-01-11 | 上海交通大学 | Friction reducing MoS2/Ti composite coating layer |
CN1846990A (en) * | 2005-04-13 | 2006-10-18 | 日立金属株式会社 | Multi-layer coating having excellent adhesion and sliding properties and production method thereof |
CN102161106A (en) * | 2011-04-01 | 2011-08-24 | 山推工程机械股份有限公司 | Ti-TiN & Ti-MoS2/Ti double-cutting-surface coated cutting tool and preparation process thereof |
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JPH0443380A (en) * | 1990-06-11 | 1992-02-13 | Canon Inc | Developing device |
KR20050063463A (en) * | 2003-12-22 | 2005-06-28 | 재단법인 포항산업과학연구원 | Manufacturing method and structure of hard coatings with lubrication properties |
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Patent Citations (4)
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---|---|---|---|---|
US6423419B1 (en) * | 1995-07-19 | 2002-07-23 | Teer Coatings Limited | Molybdenum-sulphur coatings |
CN1846990A (en) * | 2005-04-13 | 2006-10-18 | 日立金属株式会社 | Multi-layer coating having excellent adhesion and sliding properties and production method thereof |
CN1718857A (en) * | 2005-08-11 | 2006-01-11 | 上海交通大学 | Friction reducing MoS2/Ti composite coating layer |
CN102161106A (en) * | 2011-04-01 | 2011-08-24 | 山推工程机械股份有限公司 | Ti-TiN & Ti-MoS2/Ti double-cutting-surface coated cutting tool and preparation process thereof |
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