CN102912298A - Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method - Google Patents
Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method Download PDFInfo
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- CN102912298A CN102912298A CN2012104212503A CN201210421250A CN102912298A CN 102912298 A CN102912298 A CN 102912298A CN 2012104212503 A CN2012104212503 A CN 2012104212503A CN 201210421250 A CN201210421250 A CN 201210421250A CN 102912298 A CN102912298 A CN 102912298A
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Abstract
The invention discloses a method for preparing a corrosion-resistant antifriction Cr-doped DLC (diamond-like carbon) coating. The method comprises the steps of placing a pretreated substrate on a rotating stand rod of arc and magnetron sputtering composite deposition equipment, taking a post arc Cr target as a Cr source and three pairs of flat targets C targets as C sources, and installing the three pairs of flat targets C on the inner wall of a furnace body in an opposite manner; adopting high-purity Ar as a main ionization gas to guarantee an effective glow discharge process; and adopting high-purity N2 as a reacting gas, ionizing the reacting gas and combining the reacting gas with Cr and C elements to deposit on the surface of the substrate so as to form the Cr-doped DLC coating. The prepared Cr-doped DLC coating has a smooth and compact surface, hardness of 20 GPa, binding force with the substrate of 80N, coating thickness of 2.0 micrometers, and excellent corrosion resistance and antifriction performance.
Description
Technical field
The invention belongs to the coated material preparation field, be specifically related to a kind of preparation method with diamond-like coating of mixing Cr (hereinafter to be referred as the DLC coating) of anticorrosive and antifriction performance.
Background technology
Hard coat such as TiN, TiAlN, TiSiN etc. generally have high rigidity, the performance such as wear-resistant and anti-oxidant, have wide application prospect in cutting tool, forming mould and component of machine surfacecti proteon field.
In order to reduce the fuel oil consumption of automobile and motorcycle engine, the antifriction and the etching problem that solve engine slide unit such as piston, piston ring and cylinder etc. are just becoming more and more important in recent years.In addition, various mechanical bearing transmission systems and at a high speed all need to have erosion-resisting friction coat without oily sewing machine component such as bearing enclose, retainer, rolling body, shank, line-choosing connecting rod, axle sleeve, rotating shuttle etc.Obviously, above-mentioned traditional hard coat is difficult to meet the demands.Diamond-like coating DLC (Diamond-like Carbon) causes people's extensive concern with its high rigidity, low-friction coefficient and good chemical stability, but DLC coating self internal stress is large, bonding force is poor, often cracking and peeling off in use can not effectively be brought into play its effect.The DLC coating of Ti is wear-resisting to increase with antifriction performance although mix, and its corrosive nature is also undesirable.So exploitation has anticorrosive and DLC coating antifriction performance just seems very important.For this reason, the applicant utilizes the good corrosion resistance of Metal Cr, and with the good lattice match of steel matrix relation, designed a kind of DLC coating with better bonding force and antifriction, the erosion-resisting Cr of mixing.
At present, the preparation method of hard coat mainly contains physical gas phase deposition technology and chemical vapour deposition technique, and wherein, physical gas phase deposition technology comprises the methods such as the ion plating of heated filament arc, arc ion plating, magnetic controlled sputtering ion plating; Chemical vapour deposition technique comprises that high temperature chemical vapor deposition, pulsed dc plasma strengthen chemical vapour deposition, microwave plasma enhanced chemical vapour deposition and radio-frequency plasma and strengthen chemical vapour deposition etc.But the higher (of the general temperature of chemical vapor deposited coatings technology>=500 ℃), base material there is certain limitation.Current, physical vapor deposition is the mainstream technology of preparation hard coat, mainly comprise two class technology, the one, magnetron sputtered deposition technology, the method has composition regulation and control and composition optimizes convenience, and rete is fine and close and the surface smoothness advantages of higher, is mainly used at present decorating on workpiece and the part tool and mould.But it is not high that the main drawback of magnetron sputtering is coating binding force, and sedimentation rate is slower, and the workpiece surface that is difficult to satisfy under the harsh service condition is strengthened requirement.The 2nd, the electric arc ion-plating deposition technology, arc ion plating has fast, the bonding force advantages of higher of sedimentation rate, is mainly used at present on the cutter and mould of various body materials.But the drop in the electric arc ion coating plating causes coating structure comparatively loose because the restriction of preparation principle itself can't thoroughly be eliminated all the time, and surfaceness is poor etc.
Summary of the invention
Deficiency based on above-mentioned various coating productions, the object of the invention is to, a kind of preparation method with DLC coating of mixing Cr of anticorrosive and antifriction performance is provided, the DLC coating of mixing Cr of the method preparation, smooth surface is fine and close, coating hardness is 20GPa, is expected to satisfy the anticorrosive and antifriction requirement of the engine component of automobile and motorcycle.
In order to realize above-mentioned task, the present invention takes following solution:
The method that a kind of DLC coating of mixing Cr anticorrosive and antifriction prepares is characterized in that.The method comprises the following steps:
1) matrix that pre-treatment is good is put on the turret shaft of electric arc and magnetron sputtering composite coating equipment, and this turret shaft is rotated with the pivoted frame platform, and perhaps rotation is to guarantee the homogeneity of coating process;
2) with post arc Cr target as the Cr source, the three pairs of plane C targets are as the source of C, three pairs of plane C targets are placed on the inboard wall of furnace body in the mode to target; Adopt high-purity Ar as main ionization of gas, guarantee effective glow discharging process; Adopt high-purity N
2Be reactant gases, make its ionization and be combined with Cr, C element, mix the DLC coating of Cr at the matrix surface formation of deposits;
3) preparation process condition:
A) matrix plasma clean:
Matrix is packed into behind the vacuum chamber, vacuumize and be heated to be 300 ℃ constant.Pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V carries out Bombardment and cleaning to the matrix surface of vacuum chamber, continues 30min;
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is transferred to 0.3Pa, then open post arc Cr target, the post arc current is 50A, adjustment is biased into-and 300V and keep 10min, prepare the Cr bottom at matrix surface;
C) CrC transition layer preparation:
After Cr bottom preparation is finished, keep post arc current 50A and the bias voltage-300V of post arc Cr target constant, open the control power supply of plane C target, the power of plane C target is transferred to 3KW, at Cr bottom preparation CrC transition layer, continue 10min;
D) mix the DLC coating preparation of Cr:
After the preparation of CrC transition layer is finished, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is transferred to 5KW, prepare again the DLC coating of mixing Cr on the CrC transition layer, mix in the DLC coating preparation process of Cr 300 ℃ of vacuum chamber temperature, plated film bias voltage-200V, air pressure 0.3Pa, DLC coating depositing time 120min.
The present invention adopts electric arc and magnetron sputtering composite film coating technology HAMSD(Hybrid Arc-Magnetron Sputtering Deposition), utilized the advantage of magnetron sputtering rete densification, and the high advantage of arc ion plating rete bonding force, and bottom and transition layer method of design have been adopted, the prepared DLC coating of mixing Cr, smooth surface is fine and close, the hardness 20GPa of coating, film-substrate cohesion reaches 80N, and coat-thickness is 2.0 μ m.When friction pair is Al
2O
3During ball, the dry friction coefficient of mixing the DLC coating of Cr is 0.16, mixes the corrosion potential 700mv of DLC coating in electrolytic solution phosphoric acid salt (PH=7.4) of Cr, passive current density 4.76 * 10
-6/ Acm
-2Show that the DLC coating of mixing Cr has good corrosion resistance and antifriction performance.
Description of drawings
Fig. 1 is electric arc of the present invention and magnetron sputtering composite coating equipment structural representation.
The present invention is described in further detail below in conjunction with embodiment that accompanying drawing and contriver provide.
Embodiment
Present embodiment provides a kind of method for preparing the DLC coating of mixing Cr of anticorrosive and antifriction performance at surface of high speed steel, need to prove, the DLC coating of mixing Cr of method preparation of the present invention, can carry out at the material that any cutter, mould and mechanical wear-resisting spare part are selected, be not limited to this embodiment.
The concrete preparation process of present embodiment is:
(1) adopt through 1170 ℃ of quenchings, the hardness after 550 ℃ of tempering is the high speed steel substrate (material: W18Cr4V) as sample, immerse ultrasonic cleaning in the acetone, dehydration of alcohol after surface degreasing, polishing of HRC=60.
(2) sample that pre-treatment is good is put into electric arc and magnetron sputtering composite coating equipment.As shown in Figure 1, electric arc and magnetron sputtering composite coating equipment comprise vacuum chamber 1, turntable frame 2, bias voltage 3, turret shaft 4, plane C target 5, permanent magnet 6, post arc Cr target 7, well heater 8, pump group 9 at least, sample places on the turret shaft 4, turret shaft 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 φ 60 * 495mm post arc Cr target 7 as the Cr source, the Effective Raise film-substrate cohesion is by the sputtering raste of post arc power current control post arc Cr target 7; Target adopts three pairs of plane C target 5 sources as corresponding C element that are of a size of 435 * 95 * 10mm, as shown in Figure 1, plane C target 5 is placed on the inboard wall of furnace body in the mode to target, and controls the sputtering raste of above-mentioned plane C target by the power of adjusting the medium-frequency pulse power supply; Adopt high-purity Ar as main ionization of gas, guarantee effective glow discharging process; Adopt high-purity N
2As reactant gases, its ionization and the Cr in target, C element are combined, mix the DLC coating of Cr at the sample surfaces formation of deposits.
(4) electric arc and magnetron sputtering compound ion are coated with for the Optimizing Technical of mixing the DLC coating of Cr and are:
A) sample plasma cleans:
Sample is packed into behind the vacuum chamber, vacuumize and be heated to be 300 ℃ constant.Pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V carries out Bombardment and cleaning to the vacuum chamber workpiece surface, continues 30min.
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is transferred to 0.3Pa, then open post arc Cr target, the post arc current is 50A, adjustment is biased into-and 300V and keep 10min, prepare the Cr bottom at matrix surface.
C) CrC transition layer preparation:
After Cr bottom preparation is finished, keep post arc current 50A and the bias voltage-300V of post arc Cr target constant, open the control power supply of plane C target, the power of plane C target is transferred to 3KW, at Cr bottom preparation CrC transition layer.Continue 10min.
D) mix the DLC coating preparation of Cr:
After CrC transition layer preparation is finished, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is transferred to 5KW, the DLC coating of mixing Cr in the preparation of CrC transition layer.Mix in the DLC coating preparation process of Cr 300 ℃ of vacuum chamber temperature, plated film bias voltage-200V, air pressure 0.3Pa, DLC coating depositing time 120min.
Under above-mentioned processing condition, can obtain the smooth surface densification, coat-thickness is the DLC coating of mixing Cr of the anticorrosive and antifriction performance of 2.0 μ m.
After tested, the hardness 20GPa of coating, film-substrate cohesion are 80N, and coat-thickness is 2.0 μ m, when friction pair is Al
2O
3During ball, the dry friction coefficient of mixing the DLC coating of Cr is 0.16, mixes the corrosion potential 700mv of DLC coating in electrolytic solution phosphoric acid salt (PH=7.4) of Cr, passive current density 4.76 * 10
-6/ Acm
-2Show that the DLC coating of mixing Cr has good corrosion resistance and antifriction performance.
Claims (2)
1. the method that the DLC coating of mixing Cr anticorrosive and antifriction prepares is characterized in that.The method comprises the following steps:
1) matrix that pre-treatment is good is put on the turret shaft of electric arc and magnetron sputtering composite coating equipment, and this turret shaft is rotated with the pivoted frame platform, and perhaps rotation is to guarantee the homogeneity of coating process;
2) with post arc Cr target as the Cr source, the three pairs of plane C targets are as the source of C, three pairs of plane C targets are placed on the inboard wall of furnace body in the mode to target; Adopt high-purity Ar as main ionization of gas, guarantee effective glow discharging process; Adopt high-purity N
2As reactant gases, make its ionization and be combined with Cr, C element, mix the DLC coating of Cr at the matrix surface formation of deposits;
3) preparation process condition:
A) matrix plasma clean:
Matrix is packed into behind the vacuum chamber, vacuumize and be heated to be 300 ℃ constant.Pass into the Ar of 10ml/min to vacuum chamber, when gas pressure in vacuum reaches 6Pa, open be biased into-1000V carries out Bombardment and cleaning to the matrix surface of vacuum chamber, continues 30min;
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is transferred to 0.3Pa, then open post arc Cr target, the post arc current is 50A, adjustment is biased into-and 300V and keep 10min, prepare the Cr bottom at matrix surface;
C) CrC transition layer preparation:
After Cr bottom preparation is finished, keep post arc current 50A and the bias voltage-300V of post arc Cr target constant, open the control power supply of plane C target, the power of plane C target is transferred to 3KW, at Cr bottom preparation CrC transition layer, continue 10min;
D) mix the DLC coating preparation of Cr:
After the preparation of CrC transition layer is finished, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is transferred to 5KW, prepare again the DLC coating of mixing Cr on the CrC transition layer, mix in the DLC coating preparation process of Cr 300 ℃ of vacuum chamber temperature, plated film bias voltage-200V, air pressure 0.3Pa, DLC coating depositing time 120min.
2. the method for claim 1 is characterized in that, described substrate pretreated immerses ultrasonic cleaning and dehydration of alcohol in the acetone after comprising surface degreasing, polishing.
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CN108330459A (en) * | 2018-02-26 | 2018-07-27 | 温州职业技术学院 | A kind of application of symmetrical magnetron sputtering technique and its diamond-like coating |
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CN110306153A (en) * | 2019-07-22 | 2019-10-08 | 河南科技大学 | A kind of preparation method for the DLC coating adulterating Cr |
CN112048702A (en) * | 2020-09-10 | 2020-12-08 | 中国航发沈阳黎明航空发动机有限责任公司 | Preparation method of coating for aeroengine parts |
CN114836715A (en) * | 2022-03-21 | 2022-08-02 | 华南理工大学 | Metal surface Cr/CrN/CrCN/Cr-DLC multilayer composite self-lubricating film and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101823353A (en) * | 2010-04-30 | 2010-09-08 | 广州有色金属研究院 | Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof |
CN102653855A (en) * | 2012-05-05 | 2012-09-05 | 马胜利 | Preparation method of abrasion-resistant and oxidation-resisting TiAlSiN nanometer composite superhard coating |
-
2012
- 2012-10-29 CN CN201210421250.3A patent/CN102912298B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101823353A (en) * | 2010-04-30 | 2010-09-08 | 广州有色金属研究院 | Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof |
CN102653855A (en) * | 2012-05-05 | 2012-09-05 | 马胜利 | Preparation method of abrasion-resistant and oxidation-resisting TiAlSiN nanometer composite superhard coating |
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CN106399952A (en) * | 2016-05-31 | 2017-02-15 | 西安浩元航空科技有限公司 | Preparation method of hot die-casting die surface coating |
CN106399952B (en) * | 2016-05-31 | 2019-01-11 | 西安浩元航空科技有限公司 | The preparation method of injection moulding mold facecoat |
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CN107881468B (en) * | 2017-12-06 | 2018-12-25 | 周口师范学院 | A kind of printed circuit board processing micro- drill of coating and preparation method thereof |
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CN108330459A (en) * | 2018-02-26 | 2018-07-27 | 温州职业技术学院 | A kind of application of symmetrical magnetron sputtering technique and its diamond-like coating |
CN108359938A (en) * | 2018-05-22 | 2018-08-03 | 南京飞燕活塞环股份有限公司 | A kind of piston ring surface super thick DLC film coating production |
CN110306153A (en) * | 2019-07-22 | 2019-10-08 | 河南科技大学 | A kind of preparation method for the DLC coating adulterating Cr |
CN112048702A (en) * | 2020-09-10 | 2020-12-08 | 中国航发沈阳黎明航空发动机有限责任公司 | Preparation method of coating for aeroengine parts |
CN112048702B (en) * | 2020-09-10 | 2022-07-01 | 中国航发沈阳黎明航空发动机有限责任公司 | Preparation method of coating for aeroengine parts |
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