CN102912298B - 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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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 coated material preparation field, be specifically related to a kind of preparation method with the diamond-like coating of mixing Cr (hereinafter to be referred as DLC coating) of anticorrosive and antifriction performance.
Background technology
Hard coat is as TiN, TiAlN, and TiSiN etc., generally have high rigidity, the performance such as wear-resistant and anti-oxidant, in cutting tool, forming mould and component of machine surfacecti proteon field, have wide application prospect.
In recent years in order to reduce the fuel oil consumption of automobile and motorcycle engine, solve engine slide unit and just becoming more and more important as antifriction and the etching problem of piston, piston ring and cylinder etc.In addition, various mechanical bearing transmission systems and at a high speed all need to there is erosion-resisting friction coat without oily sewing machine component 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 in use there is cracking and peel off, can not effectively bring into play its effect.Although mix, the DLC coating of Ti is wear-resisting to increase with antifriction performance, and its corrosive nature is also undesirable.So exploitation has anticorrosive and DLC coating antifriction performance and just seems very important.For this reason, applicant utilizes the good corrosion resistance of Metal Cr, and the lattice match relation good with steel matrix, has 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 higher (≤500 ℃ of the general temperature of chemical vapor deposited coatings technology), base material is had to certain limitation.Current, physical vapor deposition is the mainstream technology of preparing 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 surface smoothness advantages of higher, is mainly used at present decorating on workpiece and 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, be difficult to meet the workpiece surface strengthening requirement under harsh service condition.The 2nd, electric arc ion-plating deposition technology, arc ion plating has that sedimentation rate is fast, bonding force advantages of higher, is mainly used at present on the cutter and mould of various body materials.But the drop in electric arc ion coating plating, due to the restriction of preparation principle itself, cannot thoroughly be eliminated all the time, cause that coating structure is comparatively loose, 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 the DLC coating of mixing Cr of anticorrosive and antifriction performance is provided, the DLC coating of mixing Cr prepared by the method, smooth surface is fine and close, coating hardness is 20GPa, is expected to meet 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:
A method prepared by the anticorrosive and DLC coating of mixing Cr antifriction, is characterized in that.The method comprises the following steps:
1) the good matrix of pre-treatment is put in the rotating stand rod of electric arc and magnetron sputtering composite coating equipment, this rotating stand rod is rotated with pivoted frame platform, or rotation, to guarantee the homogeneity of coating process;
2) using post arc Cr target as Cr source, the three pairs of plane C targets are as the source of C, and three pairs of plane C targets are to be placed on inboard wall of furnace body the mode of target; Adopt high-purity Ar as main ionization of gas, guarantee effective glow discharging process; Adopt high-purity N
2for reactant gases, make its ionization and be combined with Cr, C element, at matrix surface formation of deposits, mix the DLC coating of Cr;
3) preparation process condition:
A) matrix plasma clean:
Matrix packs into after 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 the matrix surface of vacuum chamber is carried out to Bombardment and cleaning, continue 30min;
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is adjusted to 0.3Pa, then open post arc Cr target, post arc current is 50A, and be biased into-300V of adjustment also keeps 10min, at matrix surface, prepares Cr bottom;
C) CrC transition layer preparation:
After prepared by Cr bottom, 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 adjusted to 3KW, on Cr bottom, prepare CrC transition layer, continue 10min;
D) mix the DLC coating preparation of Cr:
After prepared by CrC transition layer, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is adjusted to 5KW, the DLC coating that on CrC transition layer, Cr is mixed in preparation again, 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, the corrosion potential 700mv of the DLC coating of mixing Cr in electrolytic solution phosphoric acid salt (PH=7.4), passive current density 4.76 * 10
-6/ Acm
-2.Show that the DLC coating of mixing Cr has good corrosion resistance and antifriction performance.
Accompanying drawing explanation
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 for the embodiment providing below in conjunction with accompanying drawing and contriver.
Embodiment
The present embodiment provides a kind of method of preparing the DLC coating of mixing Cr of anticorrosive and antifriction performance at surface of high speed steel, it should be noted that, the DLC coating of mixing Cr prepared by method of the present invention, on the material that can select at any cutter, mould and mechanical wear-resisting spare part, carry out, be not limited to this embodiment.
The concrete preparation process of the present embodiment is:
(1) adopt through 1170 ℃ of quenchings the high speed steel substrate that the hardness after 550 ℃ of tempering is HRC=60 (material: W18Cr4V) as sample, immerse ultrasonic cleaning in acetone, dehydration of alcohol after surface degreasing, polishing.
(2) the good sample of pre-treatment is put into electric arc and magnetron sputtering composite coating equipment.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, plane C target 5, permanent magnet 6, post arc Cr target 7, well heater 8, pump group 9, sample is placed in rotating stand rod 4, rotating stand rod 4 can be rotated with turntable frame 2, also can rotation, so just avoid the film can only one side 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 Cr source, effectively improve film-substrate cohesion, 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 inboard wall of furnace body in the mode to target, and by adjusting the power of medium-frequency pulse power supply, controls the sputtering raste of above-mentioned plane C target; Adopt high-purity Ar as main ionization of gas, guarantee effective glow discharging process; Adopt high-purity N
2as reactant gases, its ionization the Cr in target, C element are combined, at sample surfaces formation of deposits, mix the DLC coating of Cr.
(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 packs into after 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 vacuum chamber workpiece surface is carried out to Bombardment and cleaning, continue 30min.
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is adjusted to 0.3Pa, then open post arc Cr target, post arc current is 50A, and be biased into-300V of adjustment also keeps 10min, at matrix surface, prepares Cr bottom.
C) CrC transition layer preparation:
After prepared by Cr bottom, 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 adjusted to 3KW, on Cr bottom, prepare CrC transition layer.Continue 10min.
D) mix the DLC coating preparation of Cr:
After prepared by CrC transition layer, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is adjusted to 5KW, the DLC coating that Cr is mixed in preparation on 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 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 is 80N, 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, the corrosion potential 700mv of the DLC coating of mixing Cr in electrolytic solution phosphoric acid salt (PH=7.4), passive current density 4.76 * 10
-6/ Acm
-2.Show that the DLC coating of mixing Cr has good corrosion resistance and antifriction performance.
Claims (2)
1. the method that prepared by the anticorrosive and DLC coating of mixing Cr antifriction, is characterized in that, the method comprises the following steps:
1) the good matrix of pre-treatment is put in the rotating stand rod of electric arc and magnetron sputtering composite coating equipment, this rotating stand rod is rotated with pivoted frame platform, or rotation, to guarantee the homogeneity of coating process;
2) using post arc Cr target as Cr source, the three pairs of plane C targets are as the source of C, and three pairs of plane C targets are to be placed on inboard wall of furnace body the mode of 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, at matrix surface formation of deposits, mix the DLC coating of Cr;
3) preparation process condition:
A) matrix plasma clean:
Matrix packs into after 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 the matrix surface of vacuum chamber carried out to Bombardment and cleaning, continue 30min;
B) Cr bottom preparation:
Regulate argon flow amount to 30ml/min, gas pressure in vacuum is adjusted to 0.3Pa, then open post arc Cr target, post arc current is 50A, and be biased into-300V of adjustment also keeps 10min, at matrix surface, prepares Cr bottom;
C) CrC transition layer preparation:
After prepared by Cr bottom, 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 adjusted to 3KW, on Cr bottom, prepare CrC transition layer, continue 10min;
D) mix the DLC coating preparation of Cr:
After prepared by CrC transition layer, the post arc current of post arc Cr target is reduced to 30A, the power of plane C target is adjusted to 5KW, the DLC coating that on CrC transition layer, Cr is mixed in preparation again, 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 acetone after comprising surface degreasing, polishing.
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| CN201210421250.3A CN102912298B (en) | 2012-10-29 | 2012-10-29 | Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method |
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| CN201210421250.3A CN102912298B (en) | 2012-10-29 | 2012-10-29 | Cr-doped DLC (diamond-like carbon) coating with anticorrosion and antifriction properties and preparation method |
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| CN102912298B true CN102912298B (en) | 2014-02-26 |
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| KR20170118737A (en) * | 2015-02-24 | 2017-10-25 | 오를리콘 서피스 솔루션스 아크티엔게젤샤프트, 페피콘 | Method of coating piston for internal combustion engine |
| 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 |
| 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 |
| CN108286037A (en) * | 2017-12-29 | 2018-07-17 | 昆山米泰克精密电子组件有限公司 | A kind of preparation method of Kato surface insulation nanoscale coating |
| 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 |
| CN108359938B (en) * | 2018-05-22 | 2020-04-07 | 南京飞燕活塞环股份有限公司 | Preparation method of super-thick diamond-like carbon film coating on surface of piston ring |
| 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 |
| 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 |
| 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 |
| CN116240492A (en) * | 2023-03-06 | 2023-06-09 | 中国科学院宁波材料技术与工程研究所 | Friction structural member for polymer matching pair, preparation method and application thereof |
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| 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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| 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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