CN101671811A - Method for preparing high-load tribology DLC membrane on surface of titanium - Google Patents
Method for preparing high-load tribology DLC membrane on surface of titanium Download PDFInfo
- Publication number
- CN101671811A CN101671811A CN200910036095A CN200910036095A CN101671811A CN 101671811 A CN101671811 A CN 101671811A CN 200910036095 A CN200910036095 A CN 200910036095A CN 200910036095 A CN200910036095 A CN 200910036095A CN 101671811 A CN101671811 A CN 101671811A
- Authority
- CN
- China
- Prior art keywords
- dlc
- base material
- sic
- membrane
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a method for preparing a high-load tribology DLC membrane on the surface of titanium, which is characterized by comprising the following steps: firstly, cleaning the titanium used as the base material and SiC used as the target; secondly, settling SiC on the surface of the base material by an RF magnetron sputtering method to form an SiC membrane middle layer; and at last,forming a DLC membrane on the SiC membrane middle layer by a DC magnetron sputtering method. The SiC membrane has obvious gradient element diffusion with the base material and the DLC membrane, thereby well solving the technical difficulty that the DLC membrane and the titanium have poor cohesion, and greatly enhancing the carrying capacity of an interface; at the same time, the invention enablesthe DLC membrane to have graphite phase with high mass fraction by optimizing the preparation technology, and greatly enhances the self carrying capacity of the DLC membrane. The invention well solvesthe preparation difficulty of the high-load tribology DLC membrane on the surface of titanium and has simple technology, thereby having wide application prospects in fields such as biology, medicine,and the like.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance surface film, especially a kind ofly utilize physical vaporous deposition to form in surface of metal titanium to have the method for DLC (quasi-diamond) film of good friction characteristic, specifically a kind of method for preparing high-load tribology DLC membrane in surface of metal titanium.
Background technology
As everyone knows, titanium metal has many excellent characteristic such as intensity height, proportion be little, anticorrosive, high temperature resistant, low temperature resistant, is widely used in many fields such as aerospace, weaponry, people's implants in vivo.But its frictional coefficient is big, wear resisting property is relatively poor, seriously affects their use properties.
Many good performances such as DLC (quasi-diamond) film is low with its friction, wearing and tearing and corrosion resistance height, bio-medical performance are good and become the research focus of metal surface protection, functional film in recent years.Although domestic and international many research institutions have obtained remarkable progress and produced a collection of relevant patent with regard to the research of metal surface protection, functional DLC film with the scholar, the DLC film that can have fine friction and wear behavior under high-load is still a very big challenge.The research of this theme has great importance for carrying occasion such as artificial hip joint etc.
Restriction metallic surface DLC film still has fine friction and wear behavior under high-load factor is many-sided, as the interface in conjunction with the toughness of, film etc.Up to the present, surface of metal titanium does not have as yet that a kind of to carry the DLC film that still has down fine tribological property at height available.
Summary of the invention
The objective of the invention is at DLC (quasi-diamond) film to invent a kind of method for preparing high-load tribology DLC membrane in surface of metal titanium in the relatively poor problem of the friction and wear behavior under the high-load.
Technical scheme of the present invention is:
A kind ofly prepare the method for high-load tribology DLC membrane, it is characterized in that it may further comprise the steps in surface of metal titanium:
At first, to cleaning as the titanium metal of base material and the SiC of target (silicon carbide);
Secondly, utilize the surface deposition SiC of radio-frequency magnetron sputter method, form the SiC membrane middle layer at base material;
At last, utilize direct current magnetron sputtering process on the SiC membrane middle layer, to form class DLC film.
Refer to remove the substrate surface dirt with the method for sand paper, polishing earlier during described cleaning to target and base material, immerse then and use ultrasonic cleaning in the organic solvent; Target with put into main sputtering chamber and Sample Room respectively through the base material that cleans and carry out the radio frequency backwash and clean target and base material; The side is taken out and respectively two Room is vacuumized after two Room air pressure are lower than 20 handkerchiefs, when main sputtering chamber, Sample Room air pressure reach 10
-5Behind the handkerchief, stop to vacuumize, feed argon gas, carry out the radio frequency backwash and clean; The basic technology parameter that main sputtering chamber cleans target is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 70W, time 15～20min, and the processing parameter that Sample Room radio frequency backwash cleans base material is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 100W, time 15～20min.
Described intermediate layer film deposition is meant: after cleaning SiC target and base material with the radio frequency backwash earlier two Room are vacuumized respectively, when Sample Room air pressure is lower than 10
-4Handkerchief, main sputtering chamber air pressure are lower than 10
-5Behind the handkerchief, open valve Sample Room is communicated with main sputtering chamber, base material is sent into main sputtering chamber from Sample Room; After having sent sample, shut-off valve vacuumizes main sputtering chamber, makes air pressure be lower than 5 * 10
-5Stop behind the handkerchief vacuumizing, feed working gas, ordering parameter carries out magnetron sputtering, adopts magnetron sputtering technique with radio frequency (RF) mode formation of deposits middle layer SiC film on base material.
The deposition of described diamond like carbon film is meant and adopts direct current (DC) mode to deposit quasi-diamond (DLC) film with high-load tribology performance on the SiC film of middle layer.
Beneficial effect of the present invention:
(1) but the present invention provides a kind of preparation method of the DLC film that also has fine friction resistant polishing machine under high-load of suitability for industrialized production for surface of metal titanium.
(2) by utilizing magnetron sputtering technique to prepare the characteristics of chemical ingredients consistency between the high characteristics of the energy of film and titanium metal, SiC, the DLC, make and taken place between membrane-membrane-Ji obviously and gradient element diffusion, thereby make the physics of film and base material and mechanical property be in asymptotic change state, cause finally having formed the combination of good interface, improved the supporting capacity at interface greatly.
(3) by controlling the processing parameter that magnetron sputtering prepares the DLC film, make the DLC film have the graphite phase of high level, guaranteed that the DLC film self has high toughness, improved the supporting capacity of DLC film self greatly.
(4) film that utilizes the present invention to make has following good physical and chemical performance: sp
3/ sp
2Than be 0.2～0.24, nano hardness is that 6.3～10.5GPa, Young's modulus are 86.2～109.2GPa, test actual measurement: work as sp
3/ sp
2Than being 0.2 o'clock, (when initial Hertzian contact stress was about 685～930MPa), wear rate was 10 under to the part that rubs, simulated body fluid or air conditions at 200～500g load, silicon nitride ball (radius is 2mm)
-6～10
-7Mm
3/ Nm level, frictional coefficient is about 0.1, and breaking and peeling phenomenon of film do not occur.
(5) all have tangible and gradient element diffusion between SiC film of the present invention and base material and DLC film, solved the technical barrier of bonding state difference between DLC film and titanium metal well, improved the supporting capacity at interface greatly, the present invention has simultaneously solved the preparation difficult problem of surface of metal titanium high-load tribology DLC membrane well, and technology is simple, is with a wide range of applications in fields such as bio-medicals.
Description of drawings
Fig. 1 utilizes method of the present invention to prepare the surface topography photo of DLC (quasi-diamond) film of gained.
Fig. 2 is the section microscopic appearance of film of the present invention, matrix and the X-ray energy spectrum analytical line scanning spectrogram of element distribution.
Fig. 3 utilizes method of the present invention to prepare the Raman spectrogram of the DLC film of gained.
Fig. 4 utilizes method of the present invention to prepare the nano impress load-displacement curve figure of the DLC film of gained.
Fig. 5 is the curve that the The friction coefficient wearing-in period of utilizing method of the present invention to prepare the DLC film of gained changes.
Fig. 6 utilizes method of the present invention to prepare the profilograph on polishing scratch surface of the DLC film of gained.
Fig. 7 utilizes method of the present invention to prepare the frictional abrasion surface pattern photo of the DLC film of gained.
Embodiment
The present invention is further illustrated below in conjunction with drawings and Examples.
Embodiment one.
Shown in Fig. 1-7.
A kind ofly prepare the method for high-load tribology DLC (quasi-diamond) film in surface of metal titanium, it may further comprise the steps:
At first, to cleaning as the titanium metal of base material and the SiC of target (silicon carbide);
Secondly, utilize the surface deposition SiC of radio-frequency magnetron sputter method, form the SiC membrane middle layer at base material;
At last, utilize direct current magnetron sputtering process on the SiC membrane middle layer, to form the DLC film.
Described cleaning to target and base material is meant removes the substrate surface dirt with the method for sand paper, polishing earlier, immerses then to use ultrasonic cleaning in the organic solvent (as acetone, dehydrated alcohol etc.); Target with put into main sputtering chamber and Sample Room respectively through the base material that cleans and carry out the radio frequency backwash and clean target and base material; The side is taken out and respectively two Room is vacuumized after two Room air pressure are lower than 20 handkerchiefs, when main sputtering chamber, Sample Room air pressure reach 10
-5Behind the handkerchief, stop to vacuumize, feed argon gas, carry out the radio frequency backwash and clean; The basic technology parameter that main sputtering chamber cleans target is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 70W, time 15～20min, and the processing parameter that Sample Room radio frequency backwash cleans base material is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 100W, time 15～20min.
Described intermediate layer film deposition is meant: after cleaning SiC target and base material with the radio frequency backwash earlier two Room are vacuumized respectively, when Sample Room air pressure is lower than 10
-4Handkerchief, main sputtering chamber air pressure are lower than 10
-5Behind the handkerchief, open valve Sample Room is communicated with main sputtering chamber, base material is sent into main sputtering chamber from Sample Room; After having sent sample, shut-off valve vacuumizes main sputtering chamber, makes air pressure be lower than 5 * 10
-5Stop behind the handkerchief vacuumizing, feed working gas, ordering parameter carries out magnetron sputtering, adopts magnetron sputtering technique with radio frequency (RF) mode formation of deposits middle layer SiC film on base material.
Described DLC depositing of thin film is meant and adopts direct current (DC) mode to deposit the DLC film with high-load tribology performance on the SiC film of middle layer.
Embodiment two.
Base material Ti, intermediate layer film SiC, surface film DLC.When being undertaken, adopt JGP560CVI type ultra-high vacuum multifunctional magnetic control sputtering device to prepare film by embodiment one.Background pressure when preparation SiC film and DLC film all is 2.5 * 10
-5Pa, base material temperature all are that room temperature, target-base material distance are 70mm all.Used technology is radio frequency (RF) magnetron sputtering technique during deposition SiC film, and target is SiC, the pressure 2.1Pa of working gas (argon gas), and the argon stream amount is 55sccm, and sputtering power is 200W, and sputtering time is 120min.Used technology is direct current (DC) magnetron sputtering technique during preparation DLC film, and target is graphite (Gr), the pressure 1.1Pa of working gas (argon gas), and the argon stream amount is 65sccm, and sputtering power is 100W, and sputtering time is 120min.
Adopt the DLC film of above-mentioned prepared: have " submicron-scale farmland " surface appearance feature, in conjunction with closely, do not have defectives such as hole (Fig. 1) between " farmland "; Obvious and gradient element diffusion are arranged between base material, intermediate layer film, surface film, and its interface is in conjunction with fine (Fig. 2); Ratio (the I of the G peak of DLC film and the integral area at D peak
G/ I
D) be sp
3/ sp
2Lower, be about 0.2, i.e. the content of graphite of film higher (Fig. 3); The DLC film has low hardness (6.3GPa), low Young's modulus (86.2GPa) (Fig. 4); For to the part that rubs, Kokubo human body simulation body fluid or air conditions following time, the wear rate of this DLC film is 10 in 200～500g load, silicon nitride ball (radius is 2mm)
-6～10
-7Mm
3/ Nm level (seeing Table 1, the average friction coefficient of DLC film and wear rate), frictional coefficient is about 0.1 (Fig. 5), and the maximum polishing scratch degree of depth is less than 0.5 micron (Fig. 6), and breaking of film and peeling phenomenon (Fig. 7) do not appear in wear surface.
The average friction coefficient and the wear rate of table 1DLC film
(radius is that the silicon nitride ball of 2mm is to the part that rubs)
Embodiment three.
Base material Ti, intermediate layer film SiC, surface film DLC.When being undertaken, adopt JGP560CVI type ultra-high vacuum multifunctional magnetic control sputtering device to prepare film by embodiment one described step.Background pressure when preparation SiC film and DLC film all is 2.5 * 10
-5Pa, base material temperature all are that room temperature, target-base material distance are 70mm all.Used technology is radio frequency (RF) magnetron sputtering technique during deposition SiC film, and target is SiC, the pressure 2.0Pa of working gas (argon gas), and the argon stream amount is 65sccm, and sputtering power is 200W, and sputtering time is 120min.Used technology is direct current (DC) magnetron sputtering technique during preparation DLC film, and target is graphite (Gr), the pressure 1.0Pa of working gas (argon gas), and the argon stream amount is 65sccm, and sputtering power is 100W, and sputtering time is 120min.
Adopt the DLC film of above-mentioned prepared: have " nanoscale farmland " surface appearance feature, in conjunction with closely, do not have defectives such as hole between " farmland "; Have between base material, intermediate layer film, surface film obviously and gradient element diffusion, the interface its in conjunction with fine; The DLC film has the ratio (I of the integral area at low G peak and D peak
G/ I
D) be about 0.24; The hardness of DLC film is that 10.5GPa, Young's modulus are 109.2GPa; For to the part that rubs, Kokubo human body simulation body fluid following time, this DLC film wear rate is 5.19 * 10 in 200g load, silicon nitride ball (radius is 2mm)
-6Mm
3/ Nm level, frictional coefficient is about 0.108,1.3 microns of the maximum polishing scratch degree of depth, breaking of obvious film and peeling phenomenon do not appear in wear surface.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (4)
1, a kind ofly prepare the method for high-load tribology DLC membrane, it is characterized in that it may further comprise the steps in surface of metal titanium:
At first, to cleaning as the titanium metal of base material and the silicon carbide of target (SiC);
Secondly, utilize the surface deposition SiC of radio-frequency magnetron sputter method, form the SiC membrane middle layer at base material;
At last, utilize direct current magnetron sputtering process on the SiC membrane middle layer, to form quasi-diamond (DLC) film.
2, the method for preparing high-load tribology DLC membrane in surface of metal titanium according to claim 1, refer to remove the substrate surface dirt with the method for sand paper, polishing earlier when it is characterized in that described cleaning to target and base material, immerse then and use ultrasonic cleaning in the organic solvent; Target with put into main sputtering chamber and Sample Room respectively through the base material that cleans and carry out the radio frequency backwash and clean target and base material; The side is taken out and respectively two Room is vacuumized after two Room air pressure are lower than 20 handkerchiefs, when main sputtering chamber, Sample Room air pressure reach 10
-5Behind the handkerchief, stop to vacuumize, feed argon gas, carry out the radio frequency backwash and clean; The basic technology parameter that main sputtering chamber cleans target is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 70W, time 15～20min, and the processing parameter that Sample Room radio frequency backwash cleans base material is argon flow amount 60sccm, build-up of luminance air pressure 3～5Pa, power 100W, time 15～20min.
3, the method for preparing high-load tribology DLC membrane in surface of metal titanium according to claim 1, it is characterized in that described intermediate layer film deposition is meant: after cleaning SiC target and base material with the radio frequency backwash earlier two Room are vacuumized respectively, when Sample Room air pressure is lower than 10
-4Handkerchief, main sputtering chamber air pressure are lower than 10
-5Behind the handkerchief, open valve Sample Room is communicated with main sputtering chamber, base material is sent into main sputtering chamber from Sample Room; After having sent sample, shut-off valve vacuumizes main sputtering chamber, makes air pressure be lower than 5 * 10
-5Stop behind the handkerchief vacuumizing, feed working gas, ordering parameter carries out magnetron sputtering, adopts magnetron sputtering technique with radio frequency (RF) mode formation of deposits middle layer SiC film on base material.
4, according to claim 1ly prepare high-load tribology DLC in surface of metal titanium) method of film, it is characterized in that described DLC depositing of thin film is meant to adopt direct current (DC) mode on the SiC film of middle layer, to deposit DLC film with high-load tribology performance.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100360951A CN101671811B (en) | 2009-10-16 | 2009-10-16 | Method for preparing high-load tribology DLC membrane on surface of titanium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100360951A CN101671811B (en) | 2009-10-16 | 2009-10-16 | Method for preparing high-load tribology DLC membrane on surface of titanium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101671811A true CN101671811A (en) | 2010-03-17 |
| CN101671811B CN101671811B (en) | 2011-07-20 |
Family
ID=42019223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100360951A Expired - Fee Related CN101671811B (en) | 2009-10-16 | 2009-10-16 | Method for preparing high-load tribology DLC membrane on surface of titanium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101671811B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285422A (en) * | 2013-06-03 | 2013-09-11 | 浙江理工大学 | SiC/TiO2 structure&function bionic nano skeleton material and preparation method thereof |
| CN103710677A (en) * | 2013-12-31 | 2014-04-09 | 东华大学 | Method for improving wear resistance of surface of steel collar |
| CN103849847A (en) * | 2014-03-24 | 2014-06-11 | 西南科技大学 | Method of preparing diamond-like membrane by film sputtering in SiNx middle layer |
| CN111621757A (en) * | 2020-05-21 | 2020-09-04 | 沈阳中北通磁科技股份有限公司 | Neodymium-iron-boron permanent magnet with anti-corrosion wear-resistant coating and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1776027A (en) * | 2005-12-01 | 2006-05-24 | 苏州大学 | Diamond coating-like biological material and its preparing method |
-
2009
- 2009-10-16 CN CN2009100360951A patent/CN101671811B/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285422A (en) * | 2013-06-03 | 2013-09-11 | 浙江理工大学 | SiC/TiO2 structure&function bionic nano skeleton material and preparation method thereof |
| CN103710677A (en) * | 2013-12-31 | 2014-04-09 | 东华大学 | Method for improving wear resistance of surface of steel collar |
| CN103849847A (en) * | 2014-03-24 | 2014-06-11 | 西南科技大学 | Method of preparing diamond-like membrane by film sputtering in SiNx middle layer |
| CN111621757A (en) * | 2020-05-21 | 2020-09-04 | 沈阳中北通磁科技股份有限公司 | Neodymium-iron-boron permanent magnet with anti-corrosion wear-resistant coating and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101671811B (en) | 2011-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106835011B (en) | A kind of structural member and preparation method thereof with diamond-like array | |
| CN103920185B (en) | A kind of metal-doped composite diamond coating titanium alloy artificial Bones and joints of Mo and preparation method thereof | |
| Wang et al. | Synthesis and characterization of titanium-containing graphite-like carbon films with low internal stress and superior tribological properties | |
| CN105755442B (en) | A kind of efficient filtered arc cathodic plasma deposition preparation DLC thick-film methods | |
| CN101487121B (en) | Diamond / W-C gradient structure composite coating and preparing method thereof | |
| CN101298656B (en) | Preparation of high-hardness diamond-like multi-layer film | |
| CN106191807B (en) | A kind of hard alloy piece and preparation method thereof with diamond coatings | |
| CN101671811B (en) | Method for preparing high-load tribology DLC membrane on surface of titanium | |
| CN101798678B (en) | Novel super-hard TiB2/c-BN nano multi-layer film prepared by magnetron sputtering technique | |
| CN108823526B (en) | Nano multilayer composite superhard cutter coating and preparation method thereof | |
| CN104862657B (en) | Titanium alloy surface nano Ti/TiN gradient film and preparation method thereof | |
| CN106086886B (en) | A kind of self-lubricating titanium diboride/diamond-like coating and its preparation method and application | |
| CN109183020A (en) | A kind of preparation method of aluminum alloy surface complex gradient modified layer | |
| CN105839070B (en) | A kind of preparation method of low friction nanometer TaC enhancings charcoal base complex phase film | |
| CN107557784A (en) | A kind of textured surfaces lubrication matrix for coating magnetic fluid and its processing method | |
| Dhandapani et al. | Enhancement of tribological properties of DLC by incorporation of amorphous titanium using magnetron sputtering process | |
| CN106498362B (en) | In the method that titanium alloy surface prepares antifriction antiwear F-DLC film | |
| Xiang et al. | Study of tribological properties of textured boron-doped diamond film under water lubrication | |
| CN101671808B (en) | Method for preparing ultralow elasticity modulus high-wearing feature shell microstructural membrane on surface of titanium | |
| CN107058949B (en) | A kind of preparation method of wear-resisting tungsten disulfide film | |
| Tang et al. | Surface morphology of α-SIC coatings deposited by RF magnetron sputtering | |
| Zhou et al. | Novel carbon-based nc-MoC/aC (Al) nanocomposite coating towards low internal stress and low-friction | |
| CN106319518B (en) | Diamond/metal carbides composite coating and its preparation method and application | |
| CN102580154A (en) | Antifriction and toughening metal/ceramic bionic multilayer-film artificial joint | |
| CN105773462B (en) | A kind of method and apparatus in the skive stick service life that polishing optical glass is improved based on ion beam technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110720 Termination date: 20181016 |