CN106835034A - A kind of multi-layer nano composite coating - Google Patents

A kind of multi-layer nano composite coating Download PDF

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Publication number
CN106835034A
CN106835034A CN201710125514.3A CN201710125514A CN106835034A CN 106835034 A CN106835034 A CN 106835034A CN 201710125514 A CN201710125514 A CN 201710125514A CN 106835034 A CN106835034 A CN 106835034A
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CN
China
Prior art keywords
target
substrate
coating
composite coating
nano composite
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Pending
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CN201710125514.3A
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Chinese (zh)
Inventor
刘和勇
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ANHUI ZHILIAN INVESTMENT GROUP Co Ltd
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ANHUI ZHILIAN INVESTMENT GROUP Co Ltd
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Priority to CN201710125514.3A priority Critical patent/CN106835034A/en
Publication of CN106835034A publication Critical patent/CN106835034A/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
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • 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
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • 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
    • 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
    • C23C14/3485—Sputtering using pulsed power to the target

Abstract

The invention discloses a kind of coating, the coating is a kind of multi-layer nano composite coating, including transition zone and top coat, and wherein top coat is TiCN nano coatings；The transition zone is Ti, TiC, TiN or Ti/TiN nanometer layer.Wherein transition region thickness is 100 200nm, and top coat is 600 800nm.Method present invention also offers above-mentioned nano-composite coating is prepared, the sputtering equipment of selection work target can be rotated using many target position, target pedestal；Specimen holder substrate being fixed on before sputtering target, is installed on target and target position, and cavity temperature is heated, vacuumized, being passed through Ar gas, and aura etching is carried out to substrate；Open high power pulsed source deposition transition zone；Finally, N2, depositing Ti CN coatings are passed through.The Nanoalloy composite coating that the present invention is provided, the design of its multi-layer nano structure causes that this coating comprehensively has the advantages that film-substrate cohesion is strong, coating is fine and close, so as to reach the coating advantage such as high rigidity, high tenacity, high abrasion and high-temperature oxidation resistance.

Description

A kind of multi-layer nano composite coating
Technical field
The present invention relates to coatings art, more particularly to a kind of composite coating used on machine tool, belong to mechanical neck Domain.
Background technology
Hard coat is mainly by CVD method, the high hardness wear-resisting protective coating deposited on tool matrix. At present, hard coat is widely used to the protection of drill bit, screw tap, slotting cutter, reamer, milling cutter blade capable of rotating positions, brazed shank tool etc. Treatment, and mould, wear-resisting component of machine etc. field of surface treatment.Generally, this type coating has extreme hardness, high resistance to The advantages of mill property, high intensity, high tenacity with reference to tool matrix, coating treatment is remarkably improved the wearability of cutter without reducing Its toughness, assigns cutter excellent comprehensive mechanical performance, and then extends cutting tool service life, greatly improves machining effect Rate.Additionally, hard coat is coated on parts can be effectively reduced mechanical wear and the high-temperature oxydation tendency of each parts, from And the service life of prolonged mechanical parts, these good combination properties cause hard coat in industrial materials especially cutter There is important application prospect in material.
Cutting-Tool Coating Technology preferably solves cutter material hardness and wearability is higher and toughness and the poorer lance of intensity Shield, substantially increases durability, applicability and the operating efficiency of cutting tool.Since being employed from coated cutting tool, cutter coat Technology achieves very fast development, and coat type is also more and more.TiC and TiN systems are the earliest cutting tool coating materials for occurring. TiC coating hardness is high, but fragility is big, not impact resistance, and temperature in use is no more than 500 DEG C.TiCN good toughness, temperature in use is reachable It is also current technique maturation and the cutting tool coating material being most widely used the most to 600 DEG C, but coating membranous layer binding force is poor.
The content of the invention
In order to solve the above problems, the present invention devises a kind of hard alloy, using nano composite multiple layer structure, to reach Improve the goal of the invention of the membranous layer binding force of hard alloy.
For achieving the above object, the technical scheme that the present invention takes is as follows：
The invention provides a kind of coating, the coating is a kind of multi-layer nano composite coating, including transition zone and top coat, its Middle top coat is TiCN nano coatings；The transition zone is Ti, TiC, TiN or Ti/TiN nanometer layer；Wherein transition region thickness is 100-200nm, top coat is 600-800nm.
Method present invention also offers above-mentioned nano-composite coating is prepared, choosing can be rotated using many target position, target pedestal Select the sputtering equipment of work target；
Substrate uses monocrystalline silicon piece, sheet glass or steel disc；First substrate is processed, by substrate respectively in acetone and ethanol it is each It is cleaned by ultrasonic 20min, drying；
Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, target is installed on target position, target-substrate distance is 16cm； Cavity temperature is heated to 300 DEG C, is evacuated to 4.0 × 10-3Below Pa, be passed through air pressure be 1.0Pa Ar gas, substrate bias- 350V, aura etching 25min is carried out to substrate；
High power pulsed source deposition transition zone is opened, film layer is 100-200nm；
Finally, N2, flow 20sccm are passed through, cavity air pressure 0.35Pa is kept, bias -50--300V is adjusted, frequency is 350kHz, depositing Ti CN coatings, using pulsed sputter, pulse voltage 700V, pulsewidth 180 μ s, frequency 100Hz, target power output 850W；Sedimentation time is 80-100min, thicknesses of layers 600-700nm.
Beneficial effects of the present invention：The Nanoalloy composite coating that the present invention is provided, the design of its multi-layer nano structure makes This coating comprehensively has the advantages that film-substrate cohesion is strong, coating is fine and close, so as to reach high rigidity, high tenacity, high abrasion and height The coating advantage such as warm inoxidizability.
Specific embodiment
Further illustrated to of the invention with reference to specific embodiment.The depositing system for using for cavity size：Φ 800×800mm；Vacuum can be less than 1 × 10-5torr；Heating-up temperature is up to 500 DEG C；Gas flow 0-100sccm；Sputtering target base Seat：：2 rotating disks of sputtering target material can be carried, it is rotatable.
Embodiment 1
Substrate uses p-type (100) monocrystalline silicon piece, sheet glass, steel disc；Substrate is processed, by substrate respectively in acetone and second It is each in alcohol to be cleaned by ultrasonic 20min, drying；
Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, target is alloys target target TiC, target-substrate distance is 16cm；Cavity temperature is heated to 300 DEG C, is evacuated to 4.0 × 10-3Below Pa, is passed through the Ar gas that air pressure is 1.0Pa, and matrix is inclined Pressure -350V, aura etching 25min is carried out to substrate；
Open high power pulsed source depositing Ti C transition zones, film layer about 200nm；
Finally, N2, flow 20sccm are passed through, cavity air pressure 0.35Pa is kept, bias -50--300V is adjusted, frequency are 350kHz, Pulse reversing time is 2 μ s, depositing Ti CN coatings, using pulsed sputter, pulse voltage 700V, pulsewidth 180 μ s, frequency 100Hz, Coupling DC current 1.0A, target power output 850W；Sedimentation time is 80-100min, thicknesses of layers 600-700nm.
Embodiment 2
Substrate uses steel disc；Substrate is processed, substrate is respectively cleaned by ultrasonic 20min, drying in acetone and ethanol respectively；
Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, by target simple metal target Ti and alloys target TiC point On two different target position that An Zhuan be on target pedestal, target-substrate distance is 16cm；
Cavity temperature is heated to 300 DEG C, is evacuated to 3.0 × 10-3Below Pa, is passed through the Ar gas that air pressure is 1.0Pa, and matrix is inclined Pressure -300V, aura etching 20min is carried out to substrate；Remove the impurity and oxide layer of substrate surface；
Ti targets are placed in operating position, high power pulsed source depositing Ti transition zone, film layer about 200nm is opened；
Finally, rotary target material pedestal, operating position is placed in by TiC targets；N2, flow 20sccm are passed through, cavity air pressure is kept 0.35Pa, adjusts bias -300V, and frequency is 350kHz, and pulse reversing time is 2 μ s, and depositing Ti CN coatings use pulsed sputter, Pulse voltage 700V, pulsewidth 200 μ s, frequency 100Hz, couple DC current 1.0A, target power output 850W；Sedimentation time is 100- 120min, thicknesses of layers about 700-800nm.
Embodiment 3
Substrate uses sheet glass；Substrate is processed, substrate is respectively cleaned by ultrasonic 20min in acetone and ethanol respectively, dried It is dry；
Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, by target simple metal target Ti and alloys target TiC point On two different target position that An Zhuan be on target pedestal, target-substrate distance is 16cm；
Cavity temperature is heated to 300 DEG C, is evacuated to 4.0 × 10-3Below Pa, is passed through the Ar gas that air pressure is 1.0Pa, and matrix is inclined Pressure -300V, aura etching 20min is carried out to substrate；Remove the impurity and oxide layer of substrate surface；
Ti targets are placed in operating position, N2, flow 10sccm is passed through, cavity air pressure 0.35Pa is kept, high power pulse electricity is opened Source, pulsed negative bias -300V, frequency is 350KHz, depositing TiN transition zone, film layer about 200nm；
Finally, rotary target material pedestal, operating position is placed in by TiC targets；N2, flow 20sccm are passed through, cavity air pressure is kept 0.35Pa, adjusts bias -300V, and frequency is 350kHz, and pulse reversing time is 2 μ s, and depositing Ti CN coatings use pulsed sputter, Pulse voltage 700V, pulsewidth 200 μ s, frequency 100Hz, couple DC current 1.0A, target power output 850W；Sedimentation time is 80- 120min, thicknesses of layers about 600-800nm.
Embodiment 4
Substrate uses steel disc；Substrate is processed, substrate is respectively cleaned by ultrasonic 20min, drying in acetone and ethanol respectively；
Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, by target simple metal target Ti and alloys target TiC point On two different target position that An Zhuan be on target pedestal, target-substrate distance is 16cm；
Cavity temperature is heated to 300 DEG C, is evacuated to 3.0 × 10-3Below Pa, is passed through the Ar gas that air pressure is 1.0Pa, and matrix is inclined Pressure -300V, aura etching 20min is carried out to substrate；Remove the impurity and oxide layer of substrate surface；
Ti targets are placed in operating position, high power pulsed source depositing Ti transition zone, film layer about 100nm is opened；N2 is passed through afterwards, Flow 10sccm, keeps cavity air pressure 0.35Pa, opens high power pulsed source, pulsed negative bias -300V, and frequency is 350KHz, depositing TiN transition zone, film layer about 100nm；
Finally, rotary target material pedestal, operating position is placed in by TiC targets；N2, flow 20sccm are passed through, cavity air pressure is kept 0.35Pa, adjusts bias -300V, and frequency is 350kHz, and pulse reversing time is 2 μ s, and depositing Ti CN coatings use pulsed sputter, Pulse voltage 700V, pulsewidth 200 μ s, frequency 100Hz, couple DC current 1.0A, target power output 850W；Sedimentation time is 120min, thicknesses of layers about 700-800nm.
Finally, it is noted that the foregoing is only the preferred embodiments of the present invention, it is not intended to limit the invention. For those skilled in the art, still it is referred to the technical scheme described in various embodiments of the present invention and modifies, is equal to Replace.All any modification, equivalent substitution and improvements done within spirit of the invention or principle etc., should be included in this hair Within bright protection domain.

Claims (6)

1. a kind of coating, the coating is a kind of multi-layer nano composite coating, including transition zone and top coat, and wherein top coat is TiCN nano coatings；The transition zone is Ti, TiC, TiN or Ti/TiN nanometer layer.
2. a kind of multi-layer nano composite coating according to claim 1, it is characterised in that：The transition region thickness is 100- 200nm, top coat is 600-800nm.
3. a kind of multi-layer nano composite coating according to claim 1 and 2, it is characterised in that：Using many target position, target base Seat can rotate the sputtering equipment of selection work target；Preparation process includes：
1）Substrate is respectively cleaned by ultrasonic 20min, drying in acetone and ethanol respectively；
2）Substrate is fixed on before being placed in sputtering target on the specimen holder of sputtering equipment, target is installed on target position, target-substrate distance is 16cm；Cavity temperature is heated to 300 DEG C, is evacuated to 4.0 × 10-3Below Pa, is passed through the Ar gas that air pressure is 1.0Pa, and matrix is inclined Pressure -350V, aura etching 25min is carried out to substrate；
3）High power pulsed source deposition transition zone is opened, film layer is 100-200nm；
4）N2, flow 20sccm are passed through, cavity air pressure 0.35Pa is kept, bias -50--300V is adjusted, frequency are 350kHz, sink Product TiCN coatings, using pulsed sputter, pulse voltage 700V, pulsewidth 180 μ s, frequency 100Hz, target power output 850W；Sedimentation time It is 80-100min, thicknesses of layers 600-700nm.
4. a kind of multi-layer nano composite coating according to claim 3, it is characterised in that：Substrate uses monocrystalline silicon piece, glass Glass piece or steel disc.
5. a kind of multi-layer nano composite coating according to claim 4, it is characterised in that：The target at least includes alloy TiC targets.
6. a kind of multi-layer nano composite coating according to claim 5, it is characterised in that：The target also includes simple metal Target Ti.
CN201710125514.3A 2017-03-04 2017-03-04 A kind of multi-layer nano composite coating Pending CN106835034A (en)

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Application Number Priority Date Filing Date Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111455311A (en) * 2020-04-12 2020-07-28 江苏利宇剃须刀有限公司 Preparation process of multilayer nano composite tetrahedral amorphous carbon film
CN114059018A (en) * 2021-11-23 2022-02-18 嘉兴学院 Super-wear-resistant multilayer combined broadband absorption film and preparation method thereof
CN115928009A (en) * 2022-06-23 2023-04-07 广东华升纳米科技股份有限公司 TiCN coating and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831616A (en) * 2010-05-11 2010-09-15 广东工业大学 Nano composite titanium-chromium-silicon nitride cutter coat and preparation method thereof
CN101831608A (en) * 2010-05-11 2010-09-15 广东工业大学 Nano composite titanium-aluminum-silicon nitride cutter coating and preparation method thereof
CN102011090A (en) * 2010-12-09 2011-04-13 中国科学院宁波材料技术与工程研究所 TiAlN/TiAlCN multilayer coating of substrate surface and preparing method thereof
CN102392217A (en) * 2011-11-23 2012-03-28 西北工业大学 Blade surface pitting corrosion resistant coating and preparation method thereof
CN103668058A (en) * 2012-09-21 2014-03-26 现代自动车株式会社 Coating material for intake/exhaust valve and method for manufacturing thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831616A (en) * 2010-05-11 2010-09-15 广东工业大学 Nano composite titanium-chromium-silicon nitride cutter coat and preparation method thereof
CN101831608A (en) * 2010-05-11 2010-09-15 广东工业大学 Nano composite titanium-aluminum-silicon nitride cutter coating and preparation method thereof
CN102011090A (en) * 2010-12-09 2011-04-13 中国科学院宁波材料技术与工程研究所 TiAlN/TiAlCN multilayer coating of substrate surface and preparing method thereof
CN102392217A (en) * 2011-11-23 2012-03-28 西北工业大学 Blade surface pitting corrosion resistant coating and preparation method thereof
CN103668058A (en) * 2012-09-21 2014-03-26 现代自动车株式会社 Coating material for intake/exhaust valve and method for manufacturing thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111455311A (en) * 2020-04-12 2020-07-28 江苏利宇剃须刀有限公司 Preparation process of multilayer nano composite tetrahedral amorphous carbon film
CN114059018A (en) * 2021-11-23 2022-02-18 嘉兴学院 Super-wear-resistant multilayer combined broadband absorption film and preparation method thereof
CN115928009A (en) * 2022-06-23 2023-04-07 广东华升纳米科技股份有限公司 TiCN coating and preparation method thereof

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