CN110373640A - A kind of preparation method of CrAlXN base PVD coated cemented carbide material - Google Patents

A kind of preparation method of CrAlXN base PVD coated cemented carbide material Download PDF

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Publication number
CN110373640A
CN110373640A CN201910838921.8A CN201910838921A CN110373640A CN 110373640 A CN110373640 A CN 110373640A CN 201910838921 A CN201910838921 A CN 201910838921A CN 110373640 A CN110373640 A CN 110373640A
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China
Prior art keywords
cralxn
matrix
alloys target
deposited
cemented carbide
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Pending
Application number
CN201910838921.8A
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Chinese (zh)
Inventor
孙浩斌
张华�
姚海滨
司守佶
李昌业
刘欣
付道龙
李晓艳
常江
王焕涛
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PENGLAI SUPERHARD COMPOUND MATERIAL CO Ltd
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PENGLAI SUPERHARD COMPOUND MATERIAL CO Ltd
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Priority to CN201910838921.8A priority Critical patent/CN110373640A/en
Publication of CN110373640A publication Critical patent/CN110373640A/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
    • C23C14/0021—Reactive sputtering or evaporation
    • 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
    • C23C14/0641—Nitrides
    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation

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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)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a kind of preparation methods of CrAlXN base PVD coated cemented carbide material, comprising the following steps: step 1 is put into Deposited By Vacuum Cathodic Arc equipment after being cleaned and dried matrix；Step 2 opens Deposited By Vacuum Cathodic Arc equipment, uses CrAl alloys target and CrAlX alloys target, N2As reaction gas, CrAlX alloys target, CrAl alloys target are alternately opened, rotates base station alternating deposit CrAlXN/CrAlN composite layer, the CrAlXN/CrAlN composite layer is deposited on matrix surface；Step 3 heats the matrix for being deposited with high-ductility abrasion-proof composite coating in step 2 under background vacuum, and rear cooling obtains matrix.CrAlXN base PVD coating of the present invention and cemented carbide material surface binding force are good, and hardness is high, and coating stress is low, the high-temperature oxidation resistant temperature of coating is higher than 1000 DEG C or more, hardness is higher than 35GPa, and after 1000 DEG C of high temperings of high temperature, coating hardness will not be substantially reduced.

Description

A kind of preparation method of CrAlXN base PVD coated cemented carbide material
Technical field
The invention belongs to technical field of material, are directed primarily to a kind of CrAlXN base PVD coated cemented carbide material Preparation method.
Background technique
Currently, being therefore widely used in intermetallic composite coating, electronics since ultra-fine cemented carbide has excellent mechanical property The fields such as industry, medicine, for example, be used as printed circuit board microbit, milling cutter, whole aperture knife tool, accurate tool and mould, Difficult-to-machine material cutter etc..And surface covering can greatly improve surface hardness, wearability and heat resistance of cutting tool etc., mesh Before, coating technology has become one of three big key technologies of modern cutting tools.With Machining Technology for Cutting to high speed, it is high-precision, Efficiently, intelligence and environmentally friendly direction are developed, and the difficult-to-machine materials such as high intensity, high tenacity emerge one after another, coating material and coating Technology must be continuously improved and develop, to meet the needs that the comprehensive cutting ability of cutter coat system is promoted.
In recent years, using physical gas phase deposition technology (PVD) work, die surface prepare advanced hard coat application by To extensive concern.Composite multilayer membrane, nano composite multiple layer film become the important directions of current superhard coating technology development.These are applied Layer is not only applicable to cutting tool field, also obtains a degree of application in die industry.The hardness of coating, high temperature resistant property And coating becomes the important indicator of assessment coating quality with the bond strength of matrix.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of CrAlXN base PVD that wear-resisting, heat-resisting, antioxygenic property collaboration is promoted The preparation method of coated cemented carbide material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of CrAlXN base PVD coated carbides The preparation method of material, comprising the following steps:
Step 1 is put into Deposited By Vacuum Cathodic Arc equipment after being cleaned and dried matrix；
Step 2 opens Deposited By Vacuum Cathodic Arc equipment, uses CrAl alloys target and CrAlX alloys target, N2As reaction Gas alternately opens CrAlX alloys target, CrAl alloys target, rotates base station alternating deposit CrAlXN/CrAlN composite layer, described CrAlXN/CrAlN composite layer is deposited on matrix surface；
Step 3 heats the matrix for being deposited with high-ductility abrasion-proof composite coating in step 2 under background vacuum, rear cooling Obtain matrix.
In step 2, one group of CrAlX alloys target and one group alternately CrAlXN/CrAlN composite layer preparation parameter: are opened CrAl alloys target, every group of target are three pieces of a column, remaining position target is in off state, the time interval that rotation is opened is 2~ 5min, 50~90A of electric current, is passed through N2, control pressure is in 3.0~5.0Pa, 50~120V of back bias voltage, duty ratio 30~80%, base 450~600 DEG C of temperature, base station keeps rotation, 1~2rpm when opening CrAlX alloys target, 2 when opening CrAl alloys target~ 3rpm, cycle period are 3~5, total 10~50min of sedimentation time, and overall thickness is 200~1000nm.
In step 3, after alternating deposit CrAlXN/CrAlN composite layer, turn off all target position, turn off all gas stream Measure valve；Vacuum chamber is adjusted to background vacuum, and heating, vacuum furnace body keeps the temperature 3~5h to 650 DEG C；Turn off furnace body heating, allows heat to make convex The matrix of mold is cooled to 100 DEG C hereinafter, blow-on, takes out matrix.
Described matrix is hard alloy substrate.
The X is nonmetalloid.
CrAlXN/CrAlN composite layer coating of the invention, effectively raises the hardness, toughness and chemical stabilization of coating Property, the wearability and thermal fatigue resistance of carbide surface are enhanced, deformation is advantageously reduced, the fatigue for eliminating coating is lost Effect, improves service life.
CrAlXN base PVD coating of the present invention and cemented carbide material surface binding force are good, and hardness is high, and coating stress is low, apply The high-temperature oxidation resistant temperature of layer is higher than 1000 DEG C or more, and hardness is higher than 35GPa, and after 1000 DEG C of high temperings of high temperature, Coating hardness will not be substantially reduced.
Specific embodiment
The present invention is further discussed below below with reference to embodiment:
A kind of embodiment 1: preparation method of CrAlXN base PVD coated cemented carbide material, comprising the following steps:
Step 1 is put into Deposited By Vacuum Cathodic Arc equipment after being cleaned and dried hard alloy substrate；
Step 2 opens Deposited By Vacuum Cathodic Arc equipment, uses CrAl alloys target and CrAlSi alloys target, N2As anti- Gas is answered, CrAlSi alloys target, CrAl alloys target are alternately opened, rotates base station alternating deposit CrAlSiN/CrAlN composite layer, institute It states CrAlSiN/CrAlN composite layer and is deposited on matrix surface；
Step 3 heats the matrix for being deposited with high-ductility abrasion-proof composite coating in step 2 under background vacuum, rear cooling Obtain matrix.
In step 2, one group of CrAlSi alloys target and one group alternately CrAlSiN/CrAlN composite layer preparation parameter: are opened CrAl alloys target, every group of target is three pieces of a column, remaining position target is in off state, and the time interval that rotation is opened is 3min, electric current 70A, is passed through N2, control pressure is in 4.0Pa, back bias voltage 100V, duty ratio 50%, and 500 DEG C of substrate temperature, base station Rotation is kept, 2rpm when opening CrAlSi alloys target, 3rpm when opening CrAl alloys target, cycle period are 4, total sedimentation time 30min, overall thickness 800nm.
In step 3, after alternating deposit CrAlSiN/CrAlN composite layer, turn off all target position, turn off all gas stream Measure valve；Vacuum chamber is adjusted to background vacuum, and heating, vacuum furnace body keeps the temperature 4h to 650 DEG C；Turn off furnace body heating, heat is allowed to make punch-pin The matrix of tool is cooled to 100 DEG C hereinafter, blow-on, takes out matrix.
CrAlXN base PVD coating of the present invention and cemented carbide material surface binding force are good, and hardness is high, and coating stress is low, apply The high-temperature oxidation resistant temperature of layer is higher than 1000 DEG C or more, hardness 40GPa, and after 1000 DEG C of high temperings of high temperature, applies Layer hardness will not be substantially reduced.
A kind of embodiment 2: preparation method of CrAlXN base PVD coated cemented carbide material, comprising the following steps:
Step 1 is put into Deposited By Vacuum Cathodic Arc equipment after being cleaned and dried hard alloy substrate；
Step 2 opens Deposited By Vacuum Cathodic Arc equipment, uses CrAl alloys target and CrAlSi alloys target, N2As anti- Gas is answered, CrAlSi alloys target, CrAl alloys target are alternately opened, rotates base station alternating deposit CrAlSiN/CrAlN composite layer, institute It states CrAlSiN/CrAlN composite layer and is deposited on matrix surface；
Step 3 heats the matrix for being deposited with high-ductility abrasion-proof composite coating in step 2 under background vacuum, rear cooling Obtain matrix.
In step 2, one group of CrAlSi alloys target and one group alternately CrAlSiN/CrAlN composite layer preparation parameter: are opened CrAl alloys target, every group of target is three pieces of a column, remaining position target is in off state, and the time interval that rotation is opened is 4min, electric current 50A, is passed through N2, control pressure is in 3.0Pa, and back bias voltage 70V, duty ratio 60%, 450 DEG C of substrate temperature, base station is protected Rotation is held, 1rpm when opening CrAlSi alloys target, 2rpm when opening CrAl alloys target, cycle period are 3, total sedimentation time 30min, overall thickness 700nm.
In step 3, after alternating deposit CrAlSiN/CrAlN composite layer, turn off all target position, turn off all gas stream Measure valve；Vacuum chamber is adjusted to background vacuum, and heating, vacuum furnace body keeps the temperature 5h to 650 DEG C；Turn off furnace body heating, heat is allowed to make punch-pin The matrix of tool is cooled to 100 DEG C hereinafter, blow-on, takes out matrix.
CrAlXN base PVD coating of the present invention and cemented carbide material surface binding force are good, and hardness is high, and coating stress is low, apply The high-temperature oxidation resistant temperature of layer is higher than 1000 DEG C or more, hardness 38GPa, and after 1000 DEG C of high temperings of high temperature, applies Layer hardness will not be substantially reduced.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention, It should not be considered as limiting the scope of the invention.All changes and improvements made in accordance with the scope of the present invention, should all It still belongs within this patent covering scope.

Claims (5)

1. a kind of preparation method of CrAlXN base PVD coated cemented carbide material, it is characterised in that: the following steps are included:
Step 1 is put into Deposited By Vacuum Cathodic Arc equipment after being cleaned and dried matrix；
Step 2 opens Deposited By Vacuum Cathodic Arc equipment, uses CrAl alloys target and CrAlX alloys target, N2As reaction gas, CrAlX alloys target, CrAl alloys target are alternately opened, base station alternating deposit CrAlXN/CrAlN composite layer, the CrAlXN/ are rotated CrAlN composite layer is deposited on matrix surface；
Step 3 heats the matrix for being deposited with high-ductility abrasion-proof composite coating in step 2 under background vacuum, and rear cooling obtains Matrix.
2. the preparation method of CrAlXN base PVD coated cemented carbide material according to claim 1, it is characterised in that: In step 2, CrAlXN/CrAlN composite layer preparation parameter: one group of CrAlX alloys target and one group of CrAl alloys target are alternately opened, often Group target is three pieces of a column, remaining position target is in off state, and the time interval that rotation is opened is 2~5min, electric current 50~ 90A is passed through N2, control pressure is in 3.0~5.0Pa, 50~120V of back bias voltage, duty ratio 30~80%, and substrate temperature 450~ 600 DEG C, base station keeps rotation, 1~2rpm when opening CrAlX alloys target, 2~3rpm when opening CrAl alloys target, cycle period It is 3~5, total 10~50min of sedimentation time, overall thickness is 200~1000nm.
3. the preparation method of CrAlXN base PVD coated cemented carbide material according to claim 1, it is characterised in that: In step 3, after alternating deposit CrAlXN/CrAlN composite layer, turns off all target position, turn off all gas flow valve；Vacuum chamber It is adjusted to background vacuum, heating, vacuum furnace body keeps the temperature 3~5h to 650 DEG C；Turn off furnace body heating, heat is allowed to make the matrix of convex mold 100 DEG C are cooled to hereinafter, blow-on, takes out matrix.
4. the preparation method of CrAlXN base PVD coated cemented carbide material according to claim 1, it is characterised in that: institute Stating matrix is hard alloy substrate.
5. the preparation method of CrAlXN base PVD coated cemented carbide material according to claim 1, it is characterised in that: institute Stating X is nonmetalloid.
CN201910838921.8A 2019-09-05 2019-09-05 A kind of preparation method of CrAlXN base PVD coated cemented carbide material Pending CN110373640A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959574A (en) * 2022-05-25 2022-08-30 宜昌永鑫精工科技股份有限公司 CrAlN coating of PCB milling cutter and processing method thereof

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EP2832479A4 (en) * 2012-03-29 2015-11-11 Osg Corp Hard coating for cutting tool and cutting tool coated with hard coating
KR20170128675A (en) * 2016-05-12 2017-11-23 디티알주식회사 A method of forming a multi-element alloy thin film composite
CN108396292A (en) * 2018-03-12 2018-08-14 中国科学院力学研究所 A kind of die casting composite coating and preparation method thereof
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CN104441828A (en) * 2014-12-04 2015-03-25 马鞍山多晶金属材料科技有限公司 AlCrSiN film with resistance to seawater corrosion and multilayer compound structure and preparation method of AlCrSiN film
KR20170128675A (en) * 2016-05-12 2017-11-23 디티알주식회사 A method of forming a multi-element alloy thin film composite
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CN109161841A (en) * 2018-07-27 2019-01-08 广东工业大学 A kind of AlCrN/AlCrSiN super hard nano composite laminated coating and its preparation method and application

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959574A (en) * 2022-05-25 2022-08-30 宜昌永鑫精工科技股份有限公司 CrAlN coating of PCB milling cutter and processing method thereof

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