CN103451608A - Wolframium (W) doped diamond-like coating and preparation method thereof - Google Patents
Wolframium (W) doped diamond-like coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a wolframium (W) doped diamond-like coating and a preparation method thereof. The coating comprises a Cr bottom layer, a CrC transition layer and a W doped diamond-like layer, wherein the Cr bottom layer is deposited on the surface of a substrate, the CrC transition layer is prepared on the Cr bottom layer, and the W doped diamond-like layer is prepared on the CrC transition layer. The preparation method comprises the following steps: firstly carrying out plasma cleaning on the substrate, opening a column electric arc Cr target to prepare the Cr bottom layer on the surface of the substrate, opening a plane magnetron sputtering C target to prepare the CrC transition layer on the Cr bottom layer, and finally closing the column electric arc Cr target and opening a plane magnetron sputtering W target to prepare the W doped diamond-like layer on the CrC transition layer. According to the preparation method provided by the invention, the electric arc and magnetron sputtering composite coating technology is adopted, so that the prepared coating is smooth and compact in surface, high in hardness, high in film bonding strength, low in friction coefficient and good in oxidization resistance and chemical stability, and can meet relatively high requirements for oxidization resistance, wear resistance and antifriction performance, therefore the coating has wide application prospects.
Description
Technical field
The invention belongs to the coated material preparation field, be specifically related to a kind of quasi-diamond (DLC) coating of mixing tungsten and preparation method thereof.
Background technology
Traditional carbon back superhard coating, as mix Ti or mix quasi-diamond (the Diamond-like Carbon of Cr, abbreviation DLC) coating has the excellent properties such as high rigidity, low-friction coefficient, there is wide application prospect in component of machine surfacecti proteon field, but the antioxidant property deficiency of these coatings, limited their further application.In order to reduce the fuel oil consumption of automobile and motorcycle engine, solve the engine slide unit and just becoming more and more important as wearing and tearing and oxidation deactivations under the hot operation condition such as piston, piston ring and cylinders in recent years.In addition, the component surface that crankshaft of cooler compressor, slide block etc. move at a high speed also needs coating to have oxidation resistant wear resistant friction reducing coating.Obviously, above-mentioned traditional carbon-base coating is difficult to meet the demands.
At present, the carbon back superhard coating mainly adopts the magnetron sputtered deposition technology preparation, the method has composition regulation and control and composition optimizes convenience, and rete is fine and close and the surface smoothness advantages of higher, but it is not high that the main drawback of magnetron sputtering technique is coating binding force, sedimentation rate is slower, is difficult to meet the workpiece surface strengthening requirement under harsh service condition.The electric arc ion coating plating technology of preparing has that sedimentation rate is fast, the bonding force advantages of higher, is mainly used at present in cutter and the preparation of die surface coating.Yet the drop in electric arc ion coating plating, due to the restriction of preparation principle itself, can't thoroughly be eliminated all the time, cause coating structure comparatively loose, surfaceness is poor etc.
Summary of the invention
The object of the present invention is to provide a kind of diamond-like coating of mixing tungsten and preparation method thereof, this mixes the diamond-like coating smooth surface densification of tungsten, and coating hardness is strong, can meet the anti-oxidant and requirement wear resistant friction reducing performance.
In order to achieve the above object, the technical solution used in the present invention is:
A kind of diamond-like coating of mixing tungsten, comprise the Cr bottom that is deposited on matrix surface, be prepared in the CrC transition layer on the Cr bottom and be prepared in the quasi-diamond layer of mixing W on the CrC transition layer.
Described Cr bottom is made by the electric arc ion coating plating method, and the CrC transition layer is made by electric arc ion coating plating method and magnetically controlled sputter method, and the quasi-diamond layer of mixing W is made by magnetically controlled sputter method.
Its thickness is 2.0 μ m, and hardness is 28GPa, and film-substrate cohesion is 70N, and oxidation resistance temperature reaches 800 ℃; When friction pair is Si
3n
4during ball, its dry friction coefficient is 0.1.
A kind of preparation method who mixes the diamond-like coating of tungsten comprises the following steps:
1) matrix plasma clean: by pre-treatment, good matrix is put into the vacuum chamber of electric arc and magnetron sputtering composite coating equipment, passes into Ar after vacuumizing matrix surface is carried out to Bombardment and cleaning;
2) preparation of Cr bottom: after step 1) completes, it is 0.3Pa that the adjusting argon flow amount makes gas pressure in vacuum, then opens column type electric arc Cr target, at matrix surface, prepares the Cr bottom;
3) preparation of CrC transition layer: in step 2) after completing, column type electric arc Cr target is held open state, opens planar magnetic control sputtering C target, preparation CrC transition layer on the Cr bottom;
4) mix the preparation of the quasi-diamond layer of W: after step 3) completes, column type electric arc Cr target is closed, the power of planar magnetic control sputtering C target is adjusted to 5KW, the power of planar magnetic control sputtering W target is increased to 3KW by 0, on the CrC transition layer, the quasi-diamond layer of W is mixed in preparation, obtains mixing the diamond-like coating of tungsten.
Described matrix is through 1170 ℃ of quenchings, the high speed steel substrate that the hardness after 550 ℃ of tempering is HRC=60, and its material is W
18cr
4v.
The pre-treatment of described matrix is: will immerse ultrasonic cleaning, then dehydration of alcohol in acetone after matrix surface oil removing, polishing.
Vacuumize in described step 1) and first be heated to 300 ℃ afterwards, pass into again Ar matrix surface is carried out to Bombardment and cleaning, the concrete operations of Bombardment and cleaning are: pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V the matrix surface in vacuum chamber is carried out to Bombardment and cleaning, continue 30min.
Described step 2) thus in regulate argon flow amount be 30ml/min to make gas pressure in vacuum be 0.3Pa, the concrete operations that prepare the Cr bottom at matrix surface are: the electric current of column type electric arc Cr target is 50A, bias voltage be-300V, maintenance 10min.
The concrete operations that prepare the CrC transition layer in described step 3) on the Cr bottom are: the electric current that maintains column type electric arc Cr target is 50A, and bias voltage is-300V that the power of planar magnetic control sputtering C target is 3KW, continues 30min.
The vacuum chamber temperature of mixing in described step 4) in the preparation process of quasi-diamond layer of W is 150 ℃, and bias voltage is-300V, and air pressure is 1.5Pa, and depositing time is 150min.
With respect to prior art, beneficial effect of the present invention is:
The present invention has utilized the good antioxidant property of refractory metal tungsten (W), a kind of diamond-like coating of mixing tungsten with transition layer structure is provided, this is mixed, and the diamond-like coating smooth surface of tungsten is fine and close, coating hardness is high, film-substrate cohesion is high, frictional coefficient is low, also there is good anti-oxidant and chemical stability, can meet the requirement of higher anti-oxidant and wear resistant friction reducing performance, be expected to realize the anti-oxidant and wear resistant friction reducing performance requriements of the engine component of automobile and motorcycle, be with a wide range of applications.
The present invention adopts electric arc and magnetron sputtering composite film coating technology HAMSD(Hybrid Arc-Magnetron Sputtering Deposition), utilize the advantage of magnetron sputtering rete densification, and arc ion plating rete bonding force is high and the advantage of fast growth, and adopted the method for design of bottom and transition layer, first on matrix, deposit the Cr bottom, prepare again the CrC transition layer on the Cr bottom, the last quasi-diamond layer of mixing W for preparing on the CrC transition layer, finally obtain mixing the diamond-like coating of tungsten, the prepared diamond-like coating smooth surface densification of mixing tungsten, the hardness of coating is high, film-substrate cohesion is strong, dry friction coefficient is low, oxidation resistance temperature is high.Show that the diamond-like coating of mixing tungsten has good antioxidant property and wear resistant friction reducing performance.
Further, the diamond-like coating of mixing tungsten that adopts method of the present invention to prepare, its thickness is 2.0 μ m after measured, and hardness is 28GPa, and film-substrate cohesion is 70N, and oxidation resistance temperature reaches 800 ℃;
When friction pair is Si
3n
4during ball, its dry friction coefficient is 0.1.
The accompanying drawing explanation
The structural representation that Fig. 1 is electric arc of the present invention and magnetron sputtering composite coating equipment;
The scanning cross-section pattern SEM figure that Fig. 2 is the diamond-like coating of mixing tungsten for preparing of the present invention;
Wherein: 1 is that vacuum chamber, 2 is that turntable frame, 3 is that bias voltage, 4 is that rotating stand rod, 5 is that planar magnetic control sputtering C target or planar magnetic control sputtering W target, 6 are that permanent magnet, 7 is that column type electric arc Cr target, 8 is that well heater, 9 is the pump group.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
The diamond-like coating of mixing tungsten provided by the invention, comprise the Cr bottom that is deposited on matrix surface, be prepared in the CrC transition layer on the Cr bottom and be prepared in the quasi-diamond layer of mixing W on the CrC transition layer.The Cr bottom is made by column type electric arc Cr target (electric arc ion coating plating method), the CrC transition layer is made by column type electric arc Cr target and plane magnetron sputtering C target (electric arc ion coating plating method and magnetically controlled sputter method), and the quasi-diamond layer of mixing W is made by planar magnetic control sputtering W target and plane magnetron sputtering C target (magnetically controlled sputter method).
(1) substrate pretreated: adopt through 1170 ℃ of quenchings the high speed steel substrate (material: W that the hardness after 550 ℃ of tempering is HRC=60
18cr
4v), as matrix, ultrasonic cleaning, then dehydration of alcohol in acetone will be immersed after its surface degreasing, polishing.
(2) by pre-treatment good matrix put into electric arc and magnetron sputtering composite coating equipment vacuum chamber rotating stand rod on.As shown in Figure 1, electric arc and magnetron sputtering composite coating equipment at least comprise vacuum chamber 1, turntable frame 2, bias voltage 3, rotating stand rod 4, planar magnetic control sputtering C target or planar magnetic control sputtering W target 5, permanent magnet 6, column type electric arc Cr target 7, well heater 8, pump group 9, rotating stand rod 4 can be rotated with turntable frame 2, also can rotation, so just avoid the film can only the single face plating and the problem of plated film inequality, guaranteed the homogeneity of coating process.
(3) adopt the Cr source of φ 60 * 495mm column type electric arc Cr target 7 as prime coat and transition layer, effectively improve film-substrate cohesion, the sputtering raste of the current control post arc Cr target 7 by column type electric arc Cr target; It is (wherein a pair of for planar magnetic control sputtering W target that employing is of a size of three pairs of plane magnetic controlled sputtering targets of 435 * 95 * 10mm, two pairs is planar magnetic control sputtering C target) as the source of corresponding W or C element, as shown in Figure 1, three pairs of plane magnetic controlled sputtering targets 5 are placed on the inwall of electric arc and magnetron sputtering composite coating equipment in the mode to target, and pass through the sputtering raste of the power control plane magnetron sputtering target of adjustment medium-frequency pulse power supply; Adopt high-purity Ar as ionization of gas, guarantee effective glow discharging process, mix the diamond-like coating of tungsten at the matrix surface formation of deposits.
(4) mix the preparation process condition of the diamond-like coating of tungsten:
A) matrix plasma clean:
Matrix is packed into after vacuum chamber, vacuumize and be heated to keep 300 ℃ constant, then pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V the matrix surface in vacuum chamber carried out to Bombardment and cleaning, continue 30min.
B) preparation of Cr bottom:
In steps A) complete after, regulate argon flow amount to 30ml/min, thereby gas pressure in vacuum be adjusted to 0.3Pa, then open column type electric arc Cr target, the electric current of column type electric arc Cr target is 50A, be biased into-300V of adjustment also keeps 10min, at matrix surface, prepares the Cr bottom.
C) preparation of CrC transition layer:
After prepared by the Cr bottom, the electric current that keeps column type electric arc Cr target be 50A and bias voltage for-300V is constant, opens the control power supply of planar magnetic control sputtering C target, and the power of planar magnetic control sputtering C target is adjusted to 3KW, on the Cr bottom, preparation CrC transition layer, continue 30min.
D) mix the preparation of the quasi-diamond layer of W:
After prepared by the CrC transition layer, column type electric arc Cr target is closed, the power of planar magnetic control sputtering C target is adjusted to 5KW, the power of planar magnetic control sputtering W target is increased to 3KW by 0 gradually, on the CrC transition layer, the quasi-diamond layer of W is mixed in preparation, and mixing vacuum chamber temperature in the quasi-diamond layer preparation process of W is 150 ℃, and bias voltage is-300V, air pressure is 1.5Pa, and depositing time is 150min.
Under above-mentioned processing condition, can obtain the smooth surface densification, the diamond-like coating of mixing tungsten that coat-thickness is 2.0 μ m.The scanning electron microscope morphology of this coating vertical section as shown in Figure 2, can be found out, the coating structure densification is obvious with the line of delimitation of matrix.After tested, the hardness 28GPa of the diamond-like coating of mixing tungsten of preparing, film-substrate cohesion 70N, coat-thickness 2.0 μ m.When friction pair is Si
3n
4during ball, the dry friction coefficient of mixing the diamond-like coating of tungsten is 0.1, and the oxidation resistance temperature of mixing the diamond-like coating of tungsten reaches 800 ℃, shows that the diamond-like coating of mixing tungsten has good antioxidant property and wear resistant friction reducing performance.
Claims (10)
1. a diamond-like coating of mixing tungsten is characterized in that: comprise the Cr bottom that is deposited on matrix surface, be prepared in the CrC transition layer on the Cr bottom and be prepared in the quasi-diamond layer of mixing W on the CrC transition layer.
2. the diamond-like coating of mixing tungsten according to claim 1, it is characterized in that: described Cr bottom is made by the electric arc ion coating plating method, the CrC transition layer is made by electric arc ion coating plating method and magnetically controlled sputter method, and the quasi-diamond layer of mixing W is made by magnetically controlled sputter method.
3. the diamond-like coating of mixing tungsten according to claim 1 and 2, it is characterized in that: its thickness is 2.0 μ m, and hardness is 28GPa, and film-substrate cohesion is 70N, and oxidation resistance temperature reaches 800 ℃; When friction pair is Si
3n
4during ball, its dry friction coefficient is 0.1.
4. a preparation method who mixes the diamond-like coating of tungsten, is characterized in that, comprises the following steps:
1) matrix plasma clean: by pre-treatment, good matrix is put into the vacuum chamber of electric arc and magnetron sputtering composite coating equipment, passes into Ar after vacuumizing matrix surface is carried out to Bombardment and cleaning;
2) preparation of Cr bottom: after step 1) completes, it is 0.3Pa that the adjusting argon flow amount makes gas pressure in vacuum, then opens column type electric arc Cr target, at matrix surface, prepares the Cr bottom;
3) preparation of CrC transition layer: in step 2) after completing, column type electric arc Cr target is held open state, opens planar magnetic control sputtering C target, preparation CrC transition layer on the Cr bottom;
4) mix the preparation of the quasi-diamond layer of W: after step 3) completes, column type electric arc Cr target is closed, the power of planar magnetic control sputtering C target is adjusted to 5KW, the power of planar magnetic control sputtering W target is increased to 3KW by 0, on the CrC transition layer, the quasi-diamond layer of W is mixed in preparation, obtains mixing the diamond-like coating of tungsten.
5. the preparation method who mixes the diamond-like coating of tungsten according to claim 4 is characterized in that: described matrix is for through 1170 ℃ of quenchings, the high speed steel substrate that the hardness after 550 ℃ of tempering is HRC=60, and its material is W
18cr
4v.
6. the preparation method who mixes the diamond-like coating of tungsten according to claim 4, it is characterized in that: the pre-treatment of described matrix is: will after matrix surface oil removing, polishing, immerse ultrasonic cleaning, then dehydration of alcohol in acetone.
7. according to the described preparation method who mixes the diamond-like coating of tungsten of any one in claim 4-6, it is characterized in that: vacuumize in described step 1) and first be heated to 300 ℃ afterwards, pass into again Ar matrix surface is carried out to Bombardment and cleaning, the concrete operations of Bombardment and cleaning are: pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V the matrix surface in vacuum chamber is carried out to Bombardment and cleaning, continue 30min.
8. according to the described preparation method who mixes the diamond-like coating of tungsten of any one in claim 4-6, it is characterized in that: described step 2) thus in to regulate argon flow amount be that to make gas pressure in vacuum be 0.3Pa to 30ml/min, the concrete operations that prepare the Cr bottom at matrix surface are: the electric current of column type electric arc Cr target is 50A, bias voltage is-300V to keep 10min.
9. according to the described preparation method who mixes the diamond-like coating of tungsten of any one in claim 4-6, it is characterized in that: the concrete operations that prepare the CrC transition layer in described step 3) on the Cr bottom are: the electric current that maintains column type electric arc Cr target is 50A, bias voltage is-300V, the power of planar magnetic control sputtering C target is 3KW, continues 30min.
10. according to the described preparation method who mixes the diamond-like coating of tungsten of any one in claim 4-6, it is characterized in that: the vacuum chamber temperature of mixing in described step 4) in the preparation process of quasi-diamond layer of W is 150 ℃, bias voltage is-300V, and air pressure is 1.5Pa, and depositing time is 150min.
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| CN103903670A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Nickel-based electrical connector and manufacture method thereof |
| CN103903669A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Copper-based electrical connector and manufacturing method thereof |
| CN104630708A (en) * | 2015-03-06 | 2015-05-20 | 重庆大学 | Diamond-like thick film, preparation method of diamond-like thick film and work-piece |
| CN105386049A (en) * | 2015-11-21 | 2016-03-09 | 太原理工大学 | Method for manufacturing gradient hard composite coating on surface of hard alloy |
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| CN103903669A (en) * | 2014-03-24 | 2014-07-02 | 大连理工常州研究院有限公司 | Copper-based electrical connector and manufacturing method thereof |
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| CN104630708A (en) * | 2015-03-06 | 2015-05-20 | 重庆大学 | Diamond-like thick film, preparation method of diamond-like thick film and work-piece |
| CN104630708B (en) * | 2015-03-06 | 2017-04-12 | 重庆大学 | Diamond-like thick film, preparation method of diamond-like thick film and work-piece |
| CN106282935A (en) * | 2015-05-15 | 2017-01-04 | 新科实业有限公司 | Material with diamond-like coating and preparation method thereof |
| CN105386049A (en) * | 2015-11-21 | 2016-03-09 | 太原理工大学 | Method for manufacturing gradient hard composite coating on surface of hard alloy |
| CN105386049B (en) * | 2015-11-21 | 2017-10-10 | 太原理工大学 | A kind of method for preparing gradient hard composite coating in carbide surface |
| CN106756847A (en) * | 2016-12-21 | 2017-05-31 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
| CN106756847B (en) * | 2016-12-21 | 2019-03-22 | 蚌埠玻璃工业设计研究院 | A kind of preparation method of witch culture DLC film |
| CN106835040B (en) * | 2017-01-04 | 2019-01-15 | 西安交通大学 | A kind of preparation method for the diamond-like coating that gold doping belongs to |
| CN106835040A (en) * | 2017-01-04 | 2017-06-13 | 西安交通大学 | A kind of preparation method of the diamond-like coating of gold doping category |
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| CN107287571A (en) * | 2017-07-17 | 2017-10-24 | 维达力实业(深圳)有限公司 | DLC film |
| CN107287571B (en) * | 2017-07-17 | 2019-11-12 | 维达力实业(深圳)有限公司 | DLC film |
| CN107502868A (en) * | 2017-09-06 | 2017-12-22 | 蚌埠玻璃工业设计研究院 | A kind of high, high resistant W doping CN films preparation method |
| CN108118294A (en) * | 2017-12-25 | 2018-06-05 | 珠海格力节能环保制冷技术研究中心有限公司 | Air cylinder structure and with its compressor |
| CN109972101A (en) * | 2017-12-28 | 2019-07-05 | 核工业西南物理研究院 | A kind of preparation method of low-doped metal nano diamond-like coating |
| CN111991621A (en) * | 2020-08-27 | 2020-11-27 | 广州大学 | Medical instrument and preparation method thereof |
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