CN109972101A - A kind of preparation method of low-doped metal nano diamond-like coating - Google Patents

A kind of preparation method of low-doped metal nano diamond-like coating Download PDF

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Publication number
CN109972101A
CN109972101A CN201711452193.4A CN201711452193A CN109972101A CN 109972101 A CN109972101 A CN 109972101A CN 201711452193 A CN201711452193 A CN 201711452193A CN 109972101 A CN109972101 A CN 109972101A
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metal
coating
power supply
magnetron sputtering
sputtering target
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Inventor
唐德礼
杨发展
许传凯
张异华
林剑冰
金凡亚
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Chengdu Co Creation Material Surface Technology Co Ltd
Xiamen Lota International Co Ltd
Southwestern Institute of Physics
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Chengdu Co Creation Material Surface Technology Co Ltd
Xiamen Lota International Co Ltd
Southwestern Institute of Physics
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Priority to CN201711452193.4A priority Critical patent/CN109972101A/en
Publication of CN109972101A publication Critical patent/CN109972101A/en
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0605—Carbon
    • C23C14/0611—Diamond
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/341—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one carbide layer
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates
    • C23C28/343—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one DLC or an amorphous carbon based layer, the layer being doped or not

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention belongs to low temperature plasma material processing technical fields, specially a kind of preparation method of low-doped metal nano diamond-like coating, after workpiece surface cleaning, workpiece is installed on vacuum chamber work rest stationary fixture, carry out vacuum bakeout degasification and plasma clean, it is sequentially depositing metal intermediate layer later, metal carbides middle layer and diamond-like coating, the diamond-like coating particle size is less than 100nm, metallic element degree is lower than 10%, surface color is uniform, high blackness coating can especially be obtained, coating surface even compact simultaneously, film/film-substrate binding strength is big, hardness is high, coefficient of friction is low, excellent anti-corrosion performance, sp3Linkage content is larger, is suitble to large industrialized production requirement.

Description

A kind of preparation method of low-doped metal nano diamond-like coating
Technical field
The invention belongs to low temperature plasma material processing technical fields, and in particular to a kind of preparation side of diamond coatings Method.
Background technique
Diamond-like coating refers to a series of containing sp2(graphite key), sp3The amorphous carbon-film of (diamond key) key.It is permitted More properties also with diamond phase seemingly, such as high rigidity, wear-resistant, low-friction coefficient, chemical inertness, high elastic modulus, electrical isolation Property, thermal conductivity, biocompatibility and optical characteristics etc..Therefore be widely used in machinery, chemical industry, acoustics, electronics, optics and The fields such as biomedicine.Diamond-like coating has the hybrid structure of diamond and graphite, is a kind of metastable longrange disorder Amorphous carbon.Carbon atom therein has sp1、sp2(graphite key), sp3(diamond key) three kinds of bonding configurations, and sp1Key ratio compared with It is small, can usually it ignore.The property of diamond-like coating is mainly by sp2And sp3The relative amount of hydridization is determined, due to sp3Key Changes of contents range it is larger, thus the performance of diamond-like coating of different process preparation is also not quite similar.Generally according to thin The difference of the bonding pattern of carbon ion and various bonding pattern ratios in film, diamond-like coating can be divided into be applied containing hydrogen diamond Layer and non-hydrogen diamond coating two major classes.The wherein content of hydrogen and carbon sp3/sp2The ratio of key is to determine diamond-like coating Two key factors of energy.
Along with the progress of development in science and technology, the requirement to diamond-like coating is also increasingly harsher.In many fields, more It is to need coating with special performance to solve the problems, such as, such as high-grade hardware bath part field workpiece heatproof itself is lower, simultaneously Wear resistant corrosion resistant is required to require color consistent (especially high blackness coating) again.Diamond-like coating has many superior property Can, it considers how to improve the bond strength between film layer and matrix, meet property demand and optimization technique, more preferably broadly It is the most important thing to the urgent need of diamond-like coating applied to each field in actual production, is realized.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of low-doped metal nano diamond-like coating, preparation is arrived Low metal dopen Nano diamond-like coating have excellent performance.
Technical scheme is as follows:
A kind of low-doped metal nano diamond-like coating, including be sequentially depositing from bottom to top metal intermediate layer, metal Carbide middle layer and diamond-like coating, wherein metal intermediate layer is deposited on workpiece surface.
The metal intermediate layer be the aluminium deposited by magnetron sputtering mode, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, Zirconium, molybdenum, tantalum, tungsten or gold pure metal coating.
The metal carbides middle layer is aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten or gold Single metal carbides or aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten and two or more of them golden gold The composite metal carbide of category.
Doped metallic elements in the diamond-like coating, the metallic element be aluminium, magnesium, titanium, vanadium, chromium, manganese, Nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten and golden one or more of them metallic element, and the diamond-like coating particle diameter is small In 100nm, metallic element degree is lower than 10%.
A kind of preparation method of low-doped metal nano diamond-like coating, includes the following steps:
(1) workpiece surface cleans
(2) workpiece is installed on vacuum chamber work rest stationary fixture；
(3) workpiece high vacuum bakeout degassing
(4) plasma clean
(5) deposited metal middle layer
S5.1 opening metal magnetron sputtering target power supply is 20-100nm metal coating a in workpiece surface deposition thickness1；
S5.2 opening metal magnetron sputtering target power supply is in metal coating a1The metal that surface deposition thickness is 150-600nm applies Layer b1；
(6) deposited metal carbide middle layer
S6.1 opening metal magnetron sputtering target power supply in a metal between layer surface deposition thickness be 20-80nm metal carbides Coating a；
S6.2 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating a surface deposition thickness is 20-80nm Belong to carbide coating b；
S6.3 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating b surface deposition thickness is 20-80nm Belong to carbide coating c；
S6.4 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating c surface deposition thickness is 20-80nm Belong to carbide coating d；
S6.5 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating d surface deposition thickness is 20-80nm Belong to carbide coating e；
S6.6 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating e surface deposition thickness is 20-80nm Belong to carbide coating f；
S6.7 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating f surface deposition thickness is 20-80nm Belong to carbide coating g；
S6.8 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating g surface deposition thickness is 20-80nm Belong to carbide coating h；
S6.9 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating h surface deposition thickness is 20-80nm Belong to carbide coating i；
S6.10 opening metal magnetron sputtering target power supply is in the gold that metal-carbide coating i surface deposition thickness is 20-80nm Belong to carbide coating j.
(7) the depositing diamond-like coating on metal-carbide coating j；
(8) workpiece is taken out after vacuum room temperature is cooled to 70 DEG C.
Described step (5) the deposited metal middle layer, specifically:
Argon gas is passed through in S5.1 vacuum chamber, maintaining working vacuum degree is 1.0 × 10-1~6.0 × 10-1It is inclined to adjust pulse by Pa Pressure is 700~1000V, and duty ratio is 60%~80%, and 100~150V of DC voltage, opening metal magnetron sputtering target power supply exists Workpiece surface deposition thickness is 20-100nm metal coating a1；
S5.2 atmosphere and working vacuum degree are constant, adjusting pulsed bias be 200~500V, duty ratio be 15%~ 30%, 30~80V of DC voltage, opening metal magnetron sputtering target power supply is in metal coating a1Surface deposition thickness is 150- The metal coating b of 600nm1。
Described step (6) the deposited metal carbide middle layer, specifically:
A certain proportion of hydrocarbon and argon gas are passed through in S6.1 vacuum chamber, maintaining working vacuum degree is 2.0 × 10-1~ 1Pa, adjusting pulsed bias are 700~1000V, and duty ratio is 60%~80%, 100~150V of DC voltage, opening metal magnetic Layer surface deposition thickness is 20-80nm metal-carbide coating a between control sputters target power supply in a metal；
S6.2 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 500~700V, and duty ratio is 50%~60%, 80~100V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating a deposition of thick Degree is the metal-carbide coating b of 20-80nm；
S6.3 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 400~500V, and duty ratio is 30%~50%, 60~80V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating b deposition of thick Degree is the metal-carbide coating c of 20-80nm；
S6.4 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 300~400V, and duty ratio is 20%~30%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating c deposition of thick Degree is the metal-carbide coating d of 20-80nm；
S6.5 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 200~300V, and duty ratio is 15%~20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating d deposition of thick Degree is the metal-carbide coating e of 20-80nm；
S6.6 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 100~200V, and duty ratio is 15%~20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating e deposition of thick Degree is the metal-carbide coating f of 20-80nm；
S6.7 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, and duty ratio is 15%~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating f deposition of thick Degree is the metal-carbide coating g of 20-80nm；
S6.8 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, and duty ratio is 15%~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating g deposition of thick Degree is the metal-carbide coating h of 20-80nm；
S6.9 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, and duty ratio is 15%~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating h deposition of thick Degree is the metal-carbide coating i of 20-80nm；
S6.10 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, and duty ratio is 15%~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply is in the surface metal-carbide coating i deposition of thick Degree is the metal-carbide coating j of 20-80nm.
The step (1) specifically:
Then workpiece surface used deionized water ultrasonic cleaning 5~10 first with alcohol ultrasonic cleaning 5~20 minutes Minute, then with alcohol ultrasonic cleaning 5~20 minutes, finally use non-woven fabrics wiped clean.
Described step (3) the workpiece high vacuum bakeout degassing, specifically:
When vacuum degree in vacuum chamber reaches 8.0 × 10-3When Pa, vacuum chamber is begun to warm up, and heating temperature is 100-200 DEG C, and Heat preservation 120 minutes.
Described step (4) plasma clean, specifically:
Vacuum chamber is passed through argon gas, and vacuum degree is 2.0 × 10-1~6.0 × 10-1Pa, hall ion source 300~500V of voltage, Time is 15~25 minutes.
The step (7) depositing diamond-like coating on metal-carbide coating j, specifically:
It is passed through working gas, maintaining vacuum degree in vacuum chamber is 2.0 × 10-1~1Pa, pulsed bias are 30~80V, duty ratio It is 15%~30%, 30~120V of DC voltage, while opening hall ion source and metal magnetic controlled sputtering target power supply, Hall ion Source voltage is 1200~3000V, and it is 800~5000nm that hall ion source, which combines deposition thickness with magnetron sputtering technique,.
Remarkable result of the invention is as follows: the depositing diamond-like combined using hall ion source with magnetron sputtering technique The method of coating, can obtain film substrate bond strength is high, coefficient of friction is low, corrosion resistance it is superior it is consistent with color (especially High blackness) high comprehensive performance nanometer diamond-like coating.By the invention it is possible to be prepared under low temperature and hot conditions The nanometer diamond-like coating of excellent combination property.The diamond-like coating particle size is less than 100nm, metallic element percentage Content is lower than 10%, and surface color is uniform, can especially obtain high blackness coating, while coating surface even compact, film/base Bond strength is big, and hardness is high, and coefficient of friction is low, excellent anti-corrosion performance, sp3Linkage content is larger, is suitble to large industrialized production
Detailed description of the invention
Fig. 1 is low-doped metal nano diamond-like coating schematic diagram；
Fig. 2 is low-doped metal nano diamond-like coating preparation method flow chart；
Specific embodiment
Below by the drawings and the specific embodiments, the invention will be further described.
As shown in Figure 1, low-doped metal nano diamond-like coating, successively includes metal intermediate layer, metal from bottom to top Carbide middle layer and diamond-like coating.Wherein metal intermediate layer is attached to workpiece surface.
Metal intermediate layer be the aluminium deposited by magnetron sputtering mode, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, Tantalum, tungsten and golden pure metal coating；
The metal carbides middle layer is to react plated deposition mode system by magnetron sputtering after being passed through hydrocarbon Standby aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten and the corresponding single metal carbides of gold or composition metal Carbide；
The metallic element adulterated in the diamond-like coating, including aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, Molybdenum, tantalum, tungsten and golden one or more of them metallic element, and the diamond-like coating particle size is less than 100nm, metal Element percentage content is lower than 10%.
As shown in Fig. 2, a kind of preparation method of low-doped metal nano diamond-like coating, includes the following steps:
(1) workpiece surface cleans
Then workpiece surface used deionized water ultrasonic cleaning 5~10 first with alcohol ultrasonic cleaning 5~20 minutes Minute, then with alcohol ultrasonic cleaning 5~20 minutes, finally use non-woven fabrics wiped clean.
(2) workpiece is installed
Workpiece is installed on vacuum chamber work rest stationary fixture, and meets work rest revolution, rotation requirement.
(3) workpiece high vacuum bakeout degassing
When vacuum degree in vacuum chamber reaches 8.0 × 10-3When Pa, vacuum chamber is begun to warm up, and heating temperature is 100-200 DEG C, and Heat preservation 120 minutes.
(4) plasma clean
Vacuum chamber is passed through argon gas, and vacuum degree is 2.0 × 10-1~6.0 × 10-1Pa, hall ion source 300~500V of voltage, Time is 15~25 minutes.
(5) deposited metal middle layer
Deposited metal middle layer is divided into following two step:
Argon gas is passed through in S1 vacuum chamber, maintaining working vacuum degree is 1.0 × 10-1~6.0 × 10-1Pa adjusts pulsed bias For 700~1000V, duty ratio is 60%~80%, and 100~150V of DC voltage, opening metal magnetron sputtering target power supply is in work Part surface deposition thickness is 20-100nm metal coating a1；
S2 atmosphere and working vacuum degree are constant, adjusting pulsed bias be 200~500V, duty ratio be 15%~ 30%, 30~80V of DC voltage, opening metal magnetron sputtering target power supply is in metal coating a1Surface deposition thickness is 150- The metal coating b of 600nm1。
(6) deposited metal carbide middle layer
Deposited metal carbide middle layer is divided into the following steps:
A certain proportion of hydrocarbon and argon gas are passed through in S1 vacuum chamber, maintaining working vacuum degree is 2.0 × 10-1~ 1Pa, adjusting pulsed bias are 700~1000V, and duty ratio is 60%~80%, 100~150V of DC voltage, opening metal magnetic Layer surface deposition thickness is 20-80nm metal-carbide coating a between control sputters target power supply in a metal；
S2 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 500~700V, duty ratio 50% ~60%, 80~100V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating a deposition thickness The metal-carbide coating b of 20-80nm；
S3 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 400~500V, duty ratio 30% ~50%, 60~80V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating b deposition thickness The metal-carbide coating c of 20-80nm；
S4 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 300~400V, duty ratio 20% ~30%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating c deposition thickness The metal-carbide coating d of 20-80nm；
S5 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 200~300V, duty ratio 15% ~20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating d deposition thickness The metal-carbide coating e of 20-80nm；
S6 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 100~200V, duty ratio 15% ~20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating e deposition thickness The metal-carbide coating f of 20-80nm；
S7 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, duty ratio 15% ~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating f deposition thickness The metal-carbide coating g of 20-80nm；
S8 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, duty ratio 15% ~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating g deposition thickness The metal-carbide coating h of 20-80nm；
S9 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, duty ratio 15% ~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating h deposition thickness The metal-carbide coating i of 20-80nm；
S10 continues to adjust the ratio of hydrocarbon and argon gas, and adjusting pulsed bias is 80~100V, duty ratio 15% ~20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating i deposition thickness The metal-carbide coating j of 20-80nm.
(7) nanometer diamond-like coating is deposited
The depositing diamond-like coating on metal-carbide coating j；
It is passed through working gas (hydrogen, argon gas and hydrocarbon), the ratio between regulating gas, maintaining vacuum degree is 2.0 ×10-1~1Pa, pulsed bias are 30~80V, and duty ratio is 15%~30%, 30~120V of DC voltage, while opening Hall Ion source and metal magnetic controlled sputtering target power supply, hall ion source voltage are 1200~3000V, hall ion source and magnetron sputtering skill It is 800~5000nm that art, which combines deposition thickness,.
(8) workpiece is taken out
After coating process, keeps vacuum chamber high vacuum state or be passed through appropriate argon gas, it is slow to vacuum room temperature Workpiece is taken out after being cooled to 70 DEG C.
In order to which the technical effect for making the technical solution adopted by the present invention and reaching is clearer, following preferred reality will be passed through Applying example, the present invention is described in further detail.These examples are only to apply the prominent example of technical solution of the present invention, all The technical solution taking equivalent replacement or equivalent transformation and being formed, is within the scope of protection of the claims of the present invention.
Embodiment 1
Using acid bronze alloy hardware bath part surface deposition nanometer diamond-like coating as embodiment, specific preparation process are as follows:
(1) acid bronze alloy hardware part (lower referred to as bath part) is bathed to be put into ultrasonic cleaner, it is first clear with alcohol ultrasonic wave It washes 10 minutes, then with deionized water ultrasonic cleaning 10 minutes, then is dehydrated 10 minutes with alcohol ultrasonic cleaning, finally use nonwoven It is clean that cloth will bathe part surface wipes.
(2) workpiece is installed on vacuum chamber work rest stationary fixture, realizes work rest revolution, rotation requirement.
(3) to vacuum chamber pumping high vacuum, when vacuum degree in vacuum chamber reaches 8.0 × 10-3When Pa, vacuum chamber is begun to warm up, and is added Hot temperature is set as 100 DEG C, when temperature reaches 100 DEG C, keeps the temperature 120 minutes.
(4) argon gas is passed through into vacuum chamber, holding vacuum degree is 0.5Pa, hall ion source voltage 500V, is carried out to bath part Plasma clean, time are 15 minutes.
(5) after the completion of plasma clean, metal intermediate layer deposition is carried out in two steps.
Argon gas is passed through in S1 vacuum chamber, maintaining working vacuum degree is 5.0 × 10-1Pa, adjusting pulsed bias are 1000V, are accounted for Sky than be 80%, DC voltage 150V, open titanium magnetron sputtering target power supply, power 6.4kW, the time 3 minutes；
S2 atmosphere and working vacuum degree are constant, and adjusting pulsed bias is 500V, duty ratio 30%, DC voltage 80V, unlatching titanium magnetron sputtering target power supply, power 6.4kW, the time 5 minutes；
(6) titanium magnetron sputtering target power supply is closed, a certain proportion of argon gas and acetylene gas mixture are passed through, adjusts vacuum Degree and grid bias power supply parameter, are again turned on titanium magnetron sputtering target power supply, carry out following steps deposited metal carbide respectively Middle layer.
Hydrocarbon and argon gas ratio are passed through in S1 vacuum chamber as the mixed gas of 1:1, keeping working vacuum degree is 5.0 ×10-1, adjusting pulsed bias be 1000V, duty ratio 80%, DC voltage 150V, open titanium magnetron sputtering target power supply, Regulation power is 6.4kW, and the time is 3 minutes；
S2 continues to adjust hydrocarbon and argon gas ratio is 1.2:1, and adjusting pulsed bias is 700V, and duty ratio is 60%, DC voltage 100V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S3 continues to adjust hydrocarbon and argon gas ratio is 1.4:1, and adjusting pulsed bias is 500V, and duty ratio is 40%, DC voltage 80V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S4 continues to adjust hydrocarbon and argon gas ratio is 1.6:1, and adjusting pulsed bias is 400V, and duty ratio is 30%, DC voltage 60V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S5 continues to adjust hydrocarbon and argon gas ratio is 1.8:1, and adjusting pulsed bias is 300V, and duty ratio is 20%, DC voltage 60V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S6 continues to adjust hydrocarbon and argon gas ratio is 2.0:1, and adjusting pulsed bias is 200V, and duty ratio is 20%, DC voltage 60V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S7 continues to adjust hydrocarbon and argon gas ratio is 2.2:1, and adjusting pulsed bias is 100V, and duty ratio is 20%, DC voltage 50V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
It is 2.4:1 that S8, which continues to adjust hydrocarbon and argon gas ratio, and adjustings pulsed bias is 90V, duty ratio 20%, DC voltage 50V opens titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
It is 2.6:1 that S9, which continues to adjust hydrocarbon and argon gas ratio, and adjustings pulsed bias is 80V, duty ratio 20%, DC voltage 50V opens titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S10 continues to adjust hydrocarbon and argon gas ratio is 2.8:1, and adjusting pulsed bias is 100V, and duty ratio is 20%, DC voltage 50V open titanium magnetron sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
(7) hydrogen shut-off valve is opened, hydrogen, argon gas and the acetylene ratio in vacuum chamber of adjusting are 3:2:1, vacuum degree 8.0 ×10-1Pa, titanium magnetron sputtering target power output remain unchanged, and are still 6.4kW, pulsed bias 80V, duty ratio 15%, directly Galvanic electricity presses 30V, and hall ion source voltage is 1300V, and it is 110 points that hall ion source, which combines sedimentation time with magnetron sputtering technique, Clock.
(8) after coating process, argon gas is passed through in vacuum chamber, vacuum degree is 2.0 × 10-1Pa is slow to vacuum room temperature Slow cool down takes out bath part to after 70 DEG C.
The bath part of above-described embodiment is tested and analyzed, tissue, structure and constituent analysis, the diamond-like coating are passed through Surface color is consistent, blackness is high, roughness low (Ra=7nm), microscopic particles tiny (﹤ 60nm), diamond-like coating titanium Constituent content ﹤ 6%, SP3Linkage content height (57%), coefficient of friction are low (≈ 0.1), and corrosion resistance (ASTM B 117-02), Adhesion test (ASTM B571-2003) and chemical corrosion resistance etc. are all satisfied the related request of high-grade hardware bath part.
Embodiment 2
Using compressor magnetic guiding loop component inner surface surface deposition nanometer diamond-like coating as embodiment, specific preparation process Are as follows:
(1) compressor magnetic conduction ring component (lower abbreviation magnetic guiding loop) is put into ultrasonic cleaner, first uses alcohol ultrasonic wave Cleaning 15 minutes, then be dehydrated 15 minutes with deionized water ultrasonic cleaning 10 minutes, then with alcohol ultrasonic cleaning, finally use nothing It is clean that woven fabric will bathe part surface wipes.
(2) magnetic guiding loop is installed on vacuum chamber work rest stationary fixture, realizes work rest revolution, rotation requirement.
(3) to vacuum chamber pumping high vacuum, when vacuum degree in vacuum chamber reaches 8.0 × 10-3When Pa, vacuum chamber is begun to warm up, and is added Hot temperature is set as 200 DEG C, when temperature reaches 200 DEG C, keeps the temperature 120 minutes.
(4) argon gas is passed through into vacuum chamber, holding vacuum degree is 0.3Pa, hall ion source voltage 300V, is carried out to bath part Plasma clean, time are 25 minutes.
(5) after the completion of plasma clean, metal intermediate layer deposition is carried out in two steps.
Argon gas is passed through in S1 vacuum chamber, maintenance working vacuum degree is 1Pa, and adjusting pulsed bias is 1000V, and duty ratio is 60%, DC voltage 120V, unlatching tungsten metal magnetic controlled sputtering target power supply, power 7.2kW, the time 3 minutes；
S2 atmosphere and working vacuum degree are constant, and adjusting pulsed bias is 300V, duty ratio 20%, DC voltage 30V, unlatching titanium magnetron sputtering target power supply, power 8.0kW, the time 6 minutes；
(6) tungsten metal magnetic controlled sputtering target power supply is closed, a certain proportion of argon gas and acetylene gas mixture are passed through, adjusts vacuum Degree and grid bias power supply parameter, are again turned on tungsten metal magnetic controlled sputtering target power supply, carry out following steps deposited metal carbide respectively Middle layer.
Hydrocarbon and argon gas ratio are passed through in S1 vacuum chamber as the mixed gas of 1:1, holding working vacuum degree is 1Pa, adjusting pulsed bias are 800V, duty ratio 80%, DC voltage 100V, unlatching tungsten metal magnetic controlled sputtering target power supply, tune Section power is 7.2kW, and the time is 3 minutes；
S2 continues to adjust hydrocarbon and argon gas ratio is 1.2:1, and adjusting pulsed bias is 500V, and duty ratio is 70%, DC voltage 90V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
S3 continues to adjust hydrocarbon and argon gas ratio is 1.4:1, and adjusting pulsed bias is 400V, and duty ratio is 30%, DC voltage 80V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
S4 continues to adjust hydrocarbon and argon gas ratio is 1.6:1, and adjusting pulsed bias is 300V, and duty ratio is 30%, DC voltage 60V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
S5 continues to adjust hydrocarbon and argon gas ratio is 1.8:1, and adjusting pulsed bias is 200V, and duty ratio is 20%, DC voltage 60V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
S6 continues to adjust hydrocarbon and argon gas ratio is 2.0:1, and adjusting pulsed bias is 100V, and duty ratio is 20%, DC voltage 60V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
It is 2.2:1 that S7, which continues to adjust hydrocarbon and argon gas ratio, and adjustings pulsed bias is 80V, duty ratio 20%, DC voltage 50V opens tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
It is 2.4:1 that S8, which continues to adjust hydrocarbon and argon gas ratio, and adjustings pulsed bias is 80V, duty ratio 20%, DC voltage 50V opens tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
It is 2.6:1 that S9, which continues to adjust hydrocarbon and argon gas ratio, and adjustings pulsed bias is 80V, duty ratio 20%, DC voltage 30V opens tungsten metal magnetic controlled sputtering target power supply, regulation power 6.4kW, and the time is 3 minutes；
S10 continues to adjust hydrocarbon and argon gas ratio is 2.8:1, and adjusting pulsed bias is 80V, and duty ratio is 20%, DC voltage 30V open tungsten metal magnetic controlled sputtering target power supply, regulation power 7.2kW, and the time is 3 minutes；
(7) open hydrogen shut-off valve, adjust vacuum chamber in hydrogen, argon gas and acetylene ratio be 4:3:1, vacuum degree 1Pa, Tungsten metal magnetic controlled sputtering target power remains unchanged, and is still 7.2kW, pulsed bias 30V, duty ratio 15%, DC voltage 50V, hall ion source voltage are 1800V, and it is 90 minutes that hall ion source, which combines sedimentation time with magnetron sputtering technique,.
(8) after coating process, argon gas is passed through in vacuum chamber, vacuum degree is 2.0 × 10-1Pa is slow to vacuum room temperature Slow cool down takes out bath part to after 70 DEG C.
The magnetic guiding loop of above-described embodiment is tested and analyzed, by tissue, structure and constituent analysis, which is applied Layer surface color is consistent, roughness is low (Ra=12nm), microscopic particles tiny (﹤ 90nm), diamond-like coating titanium element Content ﹤ 8%, SP3Linkage content height (53%), coefficient of friction are low (≈ 0.1), and corrosion resistance (ASTM B 117-02), adherency Power test (ASTM B571-2003) and chemical corrosion resistance etc. are all satisfied the associated specifications of compressor magnetic guiding loop.

Claims (10)

1. a kind of low-doped metal nano diamond-like coating, it is characterised in that: including in the metal that is sequentially depositing from bottom to top Interbed, metal carbides middle layer and diamond-like coating, wherein metal intermediate layer is deposited on workpiece surface.
2. a kind of low-doped metal nano diamond-like coating as described in claim 1, it is characterised in that: in the metal Interbed is the proof gold of the aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten or the gold that are deposited by magnetron sputtering mode Belong to coating；
The metal carbides middle layer is the single of aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten or gold Metal carbides or aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten and two or more of them golden metal Composite metal carbide.
3. a kind of low-doped metal nano diamond-like coating as described in claim 1, it is characterised in that: the diamond-like Doped metallic elements in stone coating, the metallic element be aluminium, magnesium, titanium, vanadium, chromium, manganese, nickel, copper, zinc, zirconium, molybdenum, tantalum, tungsten and Golden one or more of them metallic element, and the diamond-like coating particle diameter is less than 100nm, metallic element percentage Content is lower than 10%.
4. a kind of preparation method of low-doped metal nano diamond-like coating, which comprises the steps of:
(1) workpiece surface cleans
(2) workpiece is installed on vacuum chamber work rest stationary fixture；
(3) workpiece high vacuum bakeout degassing
(4) plasma clean
(5) deposited metal middle layer
S5.1 opening metal magnetron sputtering target power supply is 20-100nm metal coating a in workpiece surface deposition thickness1；
S5.2 opening metal magnetron sputtering target power supply is in metal coating a1Surface deposition thickness is the metal coating b of 150-600nm1；
(6) deposited metal carbide middle layer
S6.1 opening metal magnetron sputtering target power supply in a metal between layer surface deposition thickness be 20-80nm metal-carbide coating a；
S6.2 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating a surface deposition thickness is 20-80nm Compound coating b；
S6.3 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating b surface deposition thickness is 20-80nm Compound coating c；
S6.4 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating c surface deposition thickness is 20-80nm Compound coating d；
S6.5 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating d surface deposition thickness is 20-80nm Compound coating e；
S6.6 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating e surface deposition thickness is 20-80nm Compound coating f；
S6.7 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating f surface deposition thickness is 20-80nm Compound coating g；
S6.8 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating g surface deposition thickness is 20-80nm Compound coating h；
S6.9 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating h surface deposition thickness is 20-80nm Compound coating i；
S6.10 opening metal magnetron sputtering target power supply is in the metal carbon that metal-carbide coating i surface deposition thickness is 20-80nm Compound coating j.
(7) the depositing diamond-like coating on metal-carbide coating j；
(8) workpiece is taken out after vacuum room temperature is cooled to 70 DEG C.
5. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (5) deposited metal middle layer, specifically:
Argon gas is passed through in S5.1 vacuum chamber, maintaining working vacuum degree is 1.0 × 10-1~6.0 × 10-1Pa, adjusting pulsed bias is 700~1000V, duty ratio are 60%~80%, and 100~150V of DC voltage, opening metal magnetron sputtering target power supply is in workpiece Surface deposition thickness is 20-100nm metal coating a1；
S5.2 atmosphere and working vacuum degree are constant, and adjusting pulsed bias is 200~500V, and duty ratio is 15%~30%, 30~80V of DC voltage, opening metal magnetron sputtering target power supply is in metal coating a1Surface deposition thickness is the gold of 150-600nm Belong to coating b1。
6. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (6) deposited metal carbide middle layer, specifically:
A certain proportion of hydrocarbon and argon gas are passed through in S6.1 vacuum chamber, maintaining working vacuum degree is 2.0 × 10-1~1Pa, Adjusting pulsed bias is 700~1000V, and duty ratio is 60%~80%, and 100~150V of DC voltage, opening metal magnetic control splashes Layer surface deposition thickness is 20-80nm metal-carbide coating a between power supply shoot at the target in a metal；
S6.2 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 500~700V, duty ratio for 50%~ 60%, 80~100V of DC voltage, opening metal magnetron sputtering target power supply are in the surface metal-carbide coating a deposition thickness The metal-carbide coating b of 20-80nm；
S6.3 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 400~500V, duty ratio for 30%~ 50%, 60~80V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating b surface deposition thickness The metal-carbide coating c of 80nm；
S6.4 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 300~400V, duty ratio for 20%~ 30%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating c surface deposition thickness The metal-carbide coating d of 80nm；
S6.5 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 200~300V, duty ratio for 15%~ 20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating d surface deposition thickness The metal-carbide coating e of 80nm；
S6.6 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 100~200V, duty ratio for 15%~ 20%, 50~60V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating e surface deposition thickness The metal-carbide coating f of 80nm；
S6.7 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 80~100V, duty ratio for 15%~ 20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating f surface deposition thickness The metal-carbide coating g of 80nm；
S6.8 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 80~100V, duty ratio for 15%~ 20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating g surface deposition thickness The metal-carbide coating h of 80nm；
S6.9 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 80~100V, duty ratio for 15%~ 20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating h surface deposition thickness The metal-carbide coating i of 80nm；
S6.10 continues to adjust the ratio of hydrocarbon and argon gas, and adjustings pulsed bias is 80~100V, duty ratio for 15%~ 20%, 30~50V of DC voltage, opening metal magnetron sputtering target power supply are 20- in metal-carbide coating i surface deposition thickness The metal-carbide coating j of 80nm.
7. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (1) specifically:
Then workpiece surface used 5~10 points of deionized water ultrasonic cleaning first with alcohol ultrasonic cleaning 5~20 minutes Clock, then with alcohol ultrasonic cleaning 5~20 minutes, finally use non-woven fabrics wiped clean.
8. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (3) workpiece high vacuum bakeout degassing, specifically:
When vacuum degree in vacuum chamber reaches 8.0 × 10-3When Pa, vacuum chamber is begun to warm up, and heating temperature is 100-200 DEG C, and is kept the temperature 120 minutes.
9. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (4) plasma clean, specifically:
Vacuum chamber is passed through argon gas, and vacuum degree is 2.0 × 10-1~6.0 × 10-1Pa, hall ion source 300~500V of voltage, time It is 15~25 minutes.
10. a kind of low-doped metal nano diamond-like coating as claimed in claim 4, which is characterized in that the step (7) the depositing diamond-like coating on metal-carbide coating j, specifically:
It is passed through working gas, maintaining vacuum degree in vacuum chamber is 2.0 × 10-1~1Pa, pulsed bias are 30~80V, and duty ratio is 15%~30%, 30~120V of DC voltage, while opening hall ion source and metal magnetic controlled sputtering target power supply, hall ion source Voltage is 1200~3000V, and it is 800~5000nm that hall ion source, which combines deposition thickness with magnetron sputtering technique,.
CN201711452193.4A 2017-12-28 2017-12-28 A kind of preparation method of low-doped metal nano diamond-like coating Pending CN109972101A (en)

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