CN103088307B - Method for obtaining a plurality of W-Ti-N films with different W/Ti ratios by one time sputtering - Google Patents
Method for obtaining a plurality of W-Ti-N films with different W/Ti ratios by one time sputtering Download PDFInfo
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- CN103088307B CN103088307B CN200910180698.9A CN200910180698A CN103088307B CN 103088307 B CN103088307 B CN 103088307B CN 200910180698 A CN200910180698 A CN 200910180698A CN 103088307 B CN103088307 B CN 103088307B
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Abstract
The invention discloses a method for obtaining a plurality of W-Ti-N films with different W/Ti ratios by one time sputtering. According to the method, 40 Cr stainless steel is selected as a substrate, W and Ti with a purity higher than 99.99% are selected as sputtering target materials, and the plurality of the W-Ti-N films with different W/Ti ratios are obtained in one time sputtering process by changing positions between the substrate and the target materials (the angle between the sputtering bench and each of the two targets is 45 degrees). The method has easily available raw materials, low cost, simple process and easily controllable parameters, and the obtained W-Ti-N films have a plurality of microstructures, has excellent comprehensive properties in the aspects of wear resistance, corrosion resistance, high-temperature oxidation resistance and the like, can be widely applied in the fields of cutting tools, circuits and frictions and is suitable for large-scale industrialized production.
Description
Technical field
The present invention relates to the preparation method of W-Ti-N film, particularly a kind of once sputtering obtains the multiple method with the W-Ti-N film of different W/Ti ratio.
Background technology
W-Ti-N film is because having higher hardness and good high-temperature oxidation resistant corrosive nature and being widely used as the supercoat of various cutting tool and the diffusion barrier layers of circuit card; significantly improve the surface property of body material; thus obviously extend the work-ing life of cutting tool and circuit electroplax, reduce industrial cost.Research shows, in W-Ti-N film, the ratio of W/Ti all has material impact to the microtexture of film, pattern, high-temperature oxidation resistance and various mechanical property, its performance of film with different W/Ti ratio also has difference, such as the corrosion resistance nature of the film that W/Ti ratio is higher is more outstanding, and the mechanical performance compare of the lower film of W/Ti ratio is given prominence to, if the multiple W-Ti-N film with different W/Ti ratio can be obtained by a kind of method, the over-all properties of W-Ti-N film will be made to significantly improve.In order to obtain the W-Ti-N film with different W/Ti ratio, usually adopt composition target at present or inlay target, but the chemical composition of the W-Ti-N film prepared by these methods is close with target and change that is W/Ti ratio is very limited, for improving the effect of W-Ti-N film over-all properties and not obvious.
Summary of the invention
A kind of once sputtering is the object of the present invention is to provide to obtain the multiple method with the W-Ti-N film of different W/Ti ratio, the method can in a sputter procedure, by changing the position of target, a large amount of synthesis have the W-Ti-N film of multiple different W/Ti ratio.
Above-mentioned purpose is achieved by the following technical solution:
Once sputtering obtains a multiple method with the W-Ti-N film of different W/Ti ratio, comprises the steps:
(1) sputtering equipment adopts the comprehensive injection device of the two electric discharge control microwave ECR plasma of PSII type, sputtering target material selects pure metal W target (purity >=99.99%) and pure metal Ti target (purity >=99.99%), the two is mutually 90 ° and all and between sputtering unit places in 45 °, two pinwheel line is apart from sample bench 83mm, 40Cr stainless steel (being of a size of 10mm × 10mm × 3mm) selected by base material, and it put successively according to by left and right order;
(2) reverse sputtering cleaning is carried out to stainless steel sample, power 100W, cleaning 10min;
(3) send in main sputtering chamber by stainless steel sample, target and sample all adopt recirculated water water-cooled;
(4) in main sputtering chamber, reactant gases N is added
2(purity>=99.99%) and sputter gas Ar (purity>=99.99%), the ratio of the two is 1: 2 ~ 1: 5 (preferably 1: 3), initial depression>=5 × 10
-4pa, double target co-sputtering, power is 100W ~ 300W (preferred 200W), sputtering 1h ~ 3h;
(5) sputter complete, stainless steel sample is cooled to room temperature, place it in again in porcelain boat and send in high temperature box furnace, according to the temperature rise rate of 10 DEG C/min, in-furnace temperature is increased to 800 DEG C and keeps 1h, after cool to room temperature with the furnace and namely obtain the W-Ti-N film with multiple different W/Ti ratio.
Utilize frictional coefficient and the wear rate of UMT-3 type Tribological Test machine being evaluated the film of heterogeneity, frictional experiment 25 DEG C, relative humidity RH=30%, to carry out under oil-free environment, adopt ball-dish reciprocating contact mode, couple of rubbing is selected to the Stainless Steel Ball of Φ 4mm, planing speed 0.1m/s, load 5N, fraction time 30min.Can find out, the friction and wear behavior of the Ti-Al-N film of the heterogeneity prepared is also different.
The inventive method raw material is easy to get, with low cost, technique is simple, parameter is easily controlled; By means of only once sputtering, namely the W-Ti-N film with multiple different W/Ti ratio has been synthesized in a large number, and the composition of W-Ti-N film can control, the W-Ti-N film prepared has multiple microtexture, very excellent in many-sided over-all propertieies such as wear resistance, erosion resistance, high-temperature oxidation resistances, can be widely used in cutting tool, circuit field and friction field, be applicable to large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the W-Ti-N film of embodiment 1.
Fig. 2 is the microscopic appearance picture of the W-Ti-N film of embodiment 1.
Fig. 3 is the frictional coefficient change curve of the W-Ti-N film of embodiment 1.
Fig. 4 is the wear rate change curve of the W-Ti-N film of embodiment 1.
Fig. 5 is the grinding defect morphology figure of the W-Ti-N film of embodiment 1.
Embodiment
The present invention is further described below by way of embodiment, as known by the technical knowledge, the present invention also describes by other the scheme not departing from the technology of the present invention feature, and the change therefore within the scope of the present invention all or equivalent scope of the invention is all included in the invention.
Embodiment 1:
(1) sputtering equipment adopts the comprehensive injection device of the two electric discharge control microwave ECR plasma of PSII type, sputtering target material selects pure metal W target (purity >=99.99%) and pure metal Ti target (purity >=99.99%), the two is mutually 90 ° and all and between sputtering unit places in 45 °, two pinwheel line is apart from sample bench 83mm, 40Cr stainless steel (being of a size of 10mm × 10mm × 3mm) selected by base material, and it put successively according to by left and right order;
(2) reverse sputtering cleaning is carried out to stainless steel sample, power 100W, cleaning 10min;
(3) send in main sputtering chamber by stainless steel sample, target and sample all adopt recirculated water water-cooled;
(4) in main sputtering chamber, reactant gases N is added
2(purity>=99.99%) and sputter gas Ar (purity>=99.99%), the ratio of the two is 1: 3, initial depression>=5 × 10
-4pa, double target co-sputtering, power is 200W, sputtering 2h;
(5) sputter complete, stainless steel sample is cooled to room temperature, place it in again in porcelain boat and send in high temperature box furnace, according to the temperature rise rate of 10 DEG C/min, in-furnace temperature is increased to 800 DEG C and keeps 1h, after cool to room temperature with the furnace and namely obtain the W-Ti-N film with multiple different W/Ti ratio.
Measure the various performance parameters of the W-Ti-N film prepared according to the present embodiment method, result is as shown in Fig. 1 ~ Fig. 5.The film thing that Fig. 1 indicates the heterogeneity of preparation is mutually different, and has occurred TiN, TiN
0.6o
0.4, WN, W
2n, TiO
2etc. multiple thing phase.The film prepared as seen from Figure 2 is based on granular texture, and crystal grain is even compact comparatively.The film friction coefficient that Fig. 3 shows heterogeneity is also different, and reaches minimum value 0.12 at the frictional coefficient of mid-way film.Fig. 4 is presented at the film prepared in mid-way and has the most outstanding wear resistant friction reducing performance in whole system.Fig. 5 shows film wearing and tearing for typical abrasive wear, clearly can observe a large amount of very dark ditch dug with a plow and scratch phenomenon in polishing scratch.
Embodiment 2:
(1) sputtering equipment adopts the comprehensive injection device of the two electric discharge control microwave ECR plasma of PSII type, sputtering target material selects pure metal W target (purity >=99.99%) and pure metal Ti target (purity >=99.99%), the two is mutually 90 ° and all and between sputtering unit places in 45 °, two pinwheel line is apart from sample bench 83mm, 40Cr stainless steel (being of a size of 10mm × 10mm × 3mm) selected by base material, and it put successively according to by left and right order;
(2) reverse sputtering cleaning is carried out to stainless steel sample, power 100W, cleaning 10min;
(3) send in main sputtering chamber by stainless steel sample, target and sample all adopt recirculated water water-cooled;
(4) in main sputtering chamber, reactant gases N is added
2(purity>=99.99%) and sputter gas Ar (purity>=99.99%), the ratio of the two is 1: 3, initial depression>=5 × 10
-4pa, double target co-sputtering, power is 100W, sputtering 3h;
(5) sputter complete, stainless steel sample is cooled to room temperature, place it in again in porcelain boat and send in high temperature box furnace, according to the temperature rise rate of 10 DEG C/min, in-furnace temperature is increased to 800 DEG C and keeps 1h, after cool to room temperature with the furnace and namely obtain the W-Ti-N film with multiple different W/Ti ratio.
Embodiment 3:
(1) sputtering equipment adopts the comprehensive injection device of the two electric discharge control microwave ECR plasma of P SII type, sputtering target material selects pure metal W target (purity >=99.99%) and pure metal Ti target (purity >=99.99%), the two is mutually 90 ° and all and between sputtering unit places in 45 °, two pinwheel line is apart from sample bench 83mm, 40Cr stainless steel (being of a size of 10mm × 10mm × 3mm) selected by base material, and it put successively according to by left and right order;
(2) reverse sputtering cleaning is carried out to stainless steel sample, power 100W, cleaning 10min;
(3) send in main sputtering chamber by stainless steel sample, target and sample all adopt recirculated water water-cooled;
(4) in main sputtering chamber, reactant gases N is added
2(purity>=99.99%) and sputter gas Ar (purity>=99.99%), the ratio of the two is 1: 4, initial depression>=5 × 10
-4pa, double target co-sputtering, power is 200W, sputtering 3h;
(5) sputter complete, stainless steel sample is cooled to room temperature, place it in again in porcelain boat and send in high temperature box furnace, according to the temperature rise rate of 10 DEG C/min, in-furnace temperature is increased to 800 DEG C and keeps 1h, after cool to room temperature with the furnace and namely obtain the W-Ti-N film with multiple different W/Ti ratio.
Claims (3)
1. once sputtering obtains a multiple method with the W-Ti-N film of different W/Ti ratio, it is characterized in that comprising the steps:
(1) sputtering equipment adopts the comprehensive injection device of the two electric discharge control microwave ECR plasma of PSII type, sputtering target material selects the pure metal W target of purity >=99.99% and the pure metal Ti target of purity >=99.99%, the two is mutually 90 ° and all and between sputtering unit places in 45 °, two pinwheel line is apart from sample bench 83mm, base material preferred dimension is the 40Cr stainless steel of 10mm × 10mm × 3mm, and it is put successively according to by left and right order;
(2) reverse sputtering cleaning is carried out to stainless steel sample, power 100W, cleaning 10min;
(3) send in main sputtering chamber by stainless steel sample, target and sample all adopt recirculated water water-cooled;
(4) in main sputtering chamber, add the reactant gases N of purity>=99.99%
2with the sputter gas Ar of purity>=99.99%, the ratio of the two is 1: 2 ~ 1: 5, initial depression>=5 × 10
-4pa, double target co-sputtering, power is 100W ~ 300W, sputtering 1h ~ 3h;
(5) sputter complete, stainless steel sample is cooled to room temperature, place it in again in porcelain boat and send in high temperature box furnace, according to the temperature rise rate of 10 DEG C/min, in-furnace temperature is increased to 800 DEG C and keeps 1h, after cool to room temperature with the furnace and namely obtain the W-Ti-N film with multiple different W/Ti ratio.
2. in accordance with the method for claim 1, it is characterized in that, N in described step (4)
2be 1: 3 with the ratio of Ar.
3. in accordance with the method for claim 1, it is characterized in that, the power in described step (4) is 200W.
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| CN104947055A (en) * | 2015-05-20 | 2015-09-30 | 常州机电职业技术学院 | Process for preparing Ti-Al-N series high-temperature wear-resistant films with different ingredients by virtue of single sputtering |
| CN106555162B (en) * | 2016-10-18 | 2019-01-15 | 麦福枝 | A kind of preparation method of high rigidity sterilization PVD film |
| CN113305463B (en) * | 2021-06-15 | 2022-07-22 | 广东谛思纳为新材料科技有限公司 | Process for preventing stainless steel from discoloring during welding |
Citations (3)
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|---|---|---|---|---|
| US6471830B1 (en) * | 2000-10-03 | 2002-10-29 | Veeco/Cvc, Inc. | Inductively-coupled-plasma ionized physical-vapor deposition apparatus, method and system |
| US6596133B1 (en) * | 2001-06-14 | 2003-07-22 | Cvc Products, Inc. | Method and system for physically-assisted chemical-vapor deposition |
| CN100363530C (en) * | 2005-02-16 | 2008-01-23 | 吴大维 | Nano super-lattice structured superhard composite film cutting tool and deposition method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6471830B1 (en) * | 2000-10-03 | 2002-10-29 | Veeco/Cvc, Inc. | Inductively-coupled-plasma ionized physical-vapor deposition apparatus, method and system |
| US6596133B1 (en) * | 2001-06-14 | 2003-07-22 | Cvc Products, Inc. | Method and system for physically-assisted chemical-vapor deposition |
| CN100363530C (en) * | 2005-02-16 | 2008-01-23 | 吴大维 | Nano super-lattice structured superhard composite film cutting tool and deposition method therefor |
Non-Patent Citations (1)
| Title |
|---|
| Deposition and characterization of Ti- and W-containing diamond-like carbon films by plasma source ion implantation;Koumei Baba 等;《Surface and Coatings Technology》;20030630;第169－170卷;第287－290页 * |
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Application publication date: 20130508 Assignee: Liyang Turbovap Machinery Co., Ltd. Assignor: Wuxi Runpeng Composite Materials Co., Ltd. Contract record no.: 2016320000032 Denomination of invention: Method for obtaining a plurality of W-Ti-N films with different W/Ti ratios by primary sputtering Granted publication date: 20150624 License type: Exclusive License Record date: 20160226 |
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