CN107287555B - A kind of self-assembled nanometer oxynitride coating and its preparation method and application - Google Patents

A kind of self-assembled nanometer oxynitride coating and its preparation method and application Download PDF

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CN107287555B
CN107287555B CN201710340300.8A CN201710340300A CN107287555B CN 107287555 B CN107287555 B CN 107287555B CN 201710340300 A CN201710340300 A CN 201710340300A CN 107287555 B CN107287555 B CN 107287555B
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nitrogen
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CN107287555A (en
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王启民
耿东森
代伟
吴正涛
黎海旭
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Guangdong University of Technology
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0676Oxynitrides
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    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
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    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/0021Reactive sputtering or evaporation
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    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
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    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
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    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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Abstract

The present invention discloses a kind of preparation method of self-assembled nanometer oxynitride coating, it is prepared using traditional PVD technique, according to the phenomenon different with Density Distribution of energy of plasma within the scope of target different distance, by adjusting the rotation of sample pivoted frame and revolution speed, change sample in different plasma region residence time, to prepare self-assembled nanometer multilayer oxygen nitride coatings.The coating includes oxygen-rich layer and nitrogen-enriched layer, and on matrix, coating composition is Al:20~35at.%, Cr:10~25at.%, Si:0~15at.%, O:5~50at.%, N:10~50at.% for oxygen-rich layer and nitrogen-enriched layer alternating deposit.Preparation process of the invention is simple, low in cost, and adaptability is good, takes into account the advantage of nitride and oxide coating, there is very big application potentiality.

Description

A kind of self-assembled nanometer oxynitride coating and its preparation method and application
Technical field
The invention belongs to material coating fields, more particularly, to a kind of self-assembled nanometer oxynitride coating and its system Preparation Method and application.
Background technique
In recent years, metal nitride, oxide, carbon are coated on the products such as tool and mould, component of machine using PVD technique Compound etc. has become a kind of widely applied process for modifying surface come the method for improving product surface performance and used life, Middle metal nitride coatings are cutter coat mainstreams.With the development of processing technology, high speed cutting tool and hot-work die are contour Warm application environment requires the high-temperature behavior of coating higher and higher.The conventional carbons such as TiC, HfC and TiN, CrN, TiCN (nitrogen) compound Coating high-temp oxidation resistance temperature is at 600 DEG C hereinafter, being unable to satisfy the requirement of high-speed cutting.To improve heat resistance, Al, Cr, Si etc. It protects the rare earth elements such as element and Y that nitride coatings, such as AlTiN, AlCrN, AlTiSiN, AlTiYN are added, improves coating High-temperature behavior, but room for promotion is limited, and the best AlCrN coating of high-temperature behavior, heat resisting temperature also can only achieve 900-1000 DEG C or so.To further increase hard coat high-temperature behavior, it is necessary to develop new coating system.Compared with nitride coatings, Oxide coating thermo-chemical stability is more preferable, if aluminum oxide coating layer heat resistance can be to 1200 DEG C or more, but oxide coating brittleness Height, hardness are low (being lower than 20GPa).TiCN/Al2O3The composite coatings such as/TiN improve the high-temperature behavior of coating to a certain extent, lead to (10-400 layers) of peroxide/nitride alternate multiple designs, TiAlN/Al2O3Multilayer cutter coat has both nitride hardness, tough Property good and oxide excellent high temperature chemical stability the advantages of, it is good to process the performances such as aluminium in high-speed cutting and hot-work die;By In the high-insulativity of aluminium oxide, which need to be using special RF (radio frequency) sputtering and BP-DMS (sputtering of bipolar pulse twin target) Technology increases equipment cost, and deposition rate is relatively low, limits its popularization and application.Therefore, development process simply has both oxide Become current urgent problem with the new coating of nitride advantage.
Summary of the invention
The purpose of the invention is to overcome the deficiencies of existing technologies, a kind of self-assembled nanometer oxynitride coating is provided Preparation method, this method is prepared using conventional arc ion plating and magnetron sputtering, according to plasma within the scope of target different distance The physical efficiency amount phenomenon different with Density Distribution, by adjusting the rotation of sample pivoted frame and revolution speed, change sample it is different it is equal from Daughter region residence time, to realize that the self assembly of nanometer multilayer in coating generates.The preparation technology of coating is simple, cost Cheap, adaptability is good, and takes into account the advantage of nitride and oxide coating, there is very big application potentiality.
It is a further object of the present invention to provide a kind of self assembly AlCr (Si) ON nanoscale oxynitride compounds of above method preparation Coating.
Another object of the present invention is to provide the application of above-mentioned self-assembled nanometer oxynitride coating.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A kind of preparation method of self-assembled nanometer oxynitride coating, comprises the following specific steps that:
S1. metallic matrix cleans: by matrix polishing treatment, then successively it is cleaned by ultrasonic 10~20min with acetone, alcohol, It is packed into vacuum chamber with after being dried with nitrogen again;
S2.Ar and metal ion bombardment: being installed into equipment for target Cr target and AlCr (Si) target, opens heater and is warming up to 300~500 DEG C, by vacuum chamber to vacuum degree 1.0~8.0 × 10-3Pa;The Ar gas of 200~300sccm is then passed to, - 800~-1000V of work support bias is set, sputter clean, 10~20min of bombardment time are carried out to matrix surface;It again will be inclined Pressure drop lights Cr target, 60~150A of target current, with high energy Cr ion bombardment 3~15min of matrix, activation to -600~-800V Metal base surface is to improve film-base junction resultant force;
S3. it deposits nano laminated coating: being passed through O2And N2, adjust sample pivoted frame rotational velocity and revolution speed, control pressure In 1.0~3.0Pa, AlCr (Si) target, 60~150A of target current, bias -60~-200V, 0.5~2h of sedimentation time are lighted;
S4. arc power is closed, is down to room temperature to vacuum room temperature, vacuum chamber is opened and takes out matrix, in matrix surface shape At coating, as self-assembled nanometer oxynitride coating.
Preferably, rotational velocity described in step S3 is 1~6r/min, and the revolution speed is 0~5r/min.
Preferably, each element atomic percent of AlCrSi target described in step S3 be Al:55~70at.%, Cr:20~ 35at.%, Si:0~20at.%.
Preferably, O described in step S32Account for O2And N2The 1~25% of total volume.
Preferably, matrix described in step S1-S4 is metal, hard alloy or ceramics.
The self-assembled nanometer oxynitride coating of above method preparation, the self-assembled nanometer oxynitride coating include richness Oxygen layer and nitrogen-enriched layer, the oxygen-rich layer and nitrogen-enriched layer alternating deposit are on matrix.
Wherein, the ingredient of the self-assembled nanometer oxynitride coating be Al:20~35at.%, Cr:10~25at.%, Si:0~15at.%, O:5~50at.%, N:10~50at.%.
Preferably, the overall thickness of the self-assembled nanometer oxynitride coating is 2~10 μm.
Preferably, the thickness in monolayer of the oxygen-rich layer is 2~20nm, and the thickness in monolayer of the nitrogen-enriched layer is 5~100nm.
Preferably, described matrix is metal, hard alloy or ceramics.
Above-mentioned self-assembled nanometer oxynitride coating is in the protection field of component of machine and knife mold product surface Using.
Compared with prior art, the invention has the following advantages:
1. the present invention prepares self-assembled nanometer multilayer oxygen nitride coatings, the coating using arc ion plating and magnetron sputtering The advantage for taking into account nitride and oxide coating, overcomes the difficult disadvantage of oxide coating manufacture, and simple process can operate Property is strong, and controllability is good, and low in cost, adaptability is good, suitable for the protection of the product surfaces such as component of machine, knife mold, has Preferable economic benefit.
2. the present invention phenomenon different with Density Distribution according to energy of plasma within the scope of target different distance, passes through tune Whole sample pivoted frame rotation and revolution speed change sample in different plasma region residence time, prepare it is novel from Assemble nanometer multilayer oxygen nitride coatings, can be adapted for the working environment under mal-condition.
Detailed description of the invention
Fig. 1 is the schematic diagram that the present invention uses arc deposited device.
Fig. 2 is SEM the and TEM photo of self-assembled nanometer oxynitride coating prepared by embodiment 1.
Fig. 3 is the structural schematic diagram of self-assembled nanometer oxynitride coating.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention. Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
A kind of self-assembled nanometer oxynitride coating, including oxygen-rich layer AlCrSiON and nitrogen-enriched layer AlCrSiON.Wherein, rich Oxygen layer with a thickness of 2nm, nitrogen-enriched layer with a thickness of 5nm, the atom percentage content of each element in coating are as follows: Al:20at.%, Cr:10at.%, Si:15at.%, O:50at.%, N:5at.%.
By high speed steel substrate polishing treatment, it is cleaned by ultrasonic 10min through acetone, alcohol, then is packed into vacuum with after being dried with nitrogen It is indoor.Target Cr target and AlCrSi target are installed into equipment, heater is opened and is warming up to 300 DEG C, vacuum chamber to vacuum Degree 1.0 × 10-3Pa or less.It is passed through the Ar gas of 300sccm, work support bias -1000V is set, matrix surface is sputtered Cleaning, bombardment time 10min.Bias is down to -600V later, lights Cr target, target current 150A, with high energy Cr ion bombardment Matrix 15min.Bias is adjusted to -200V, is passed through the N of 300sccm2Gas and O2, control pressure is in 3.0Pa, O2/O2+N2Ratio is 25%, CrAlSi target is lighted, target current 60A, sedimentation time 0.5 hour, transfer rack revolution speed was 0r/min, from revolving speed Degree is 6r/min.After completing plated film, it is down to room temperature to vacuum room temperature, vacuum chamber is opened and takes out matrix, obtain self-assembled nanometer Multilayer oxygen nitride coatings.
Fig. 1 is the schematic diagram that the present invention uses arc deposited device.Matrix rotates during depositing coating, and matrix is just Energy of plasma and density are higher when to target, react more abundant, nitrogen content is higher, and layer is also thicker;And in matrix far from target Plasma density is lower when material, and the oxygen and metal for being easier to reaction generate oxygen-enriched layer, and the nanometer layer is relatively thin, therefore prepared by coating Cheng Zhonghui self assembly generates nano-multilayered structures.
Fig. 2 is the TEM and SEM photograph of self-assembled nanometer multilayer oxygen nitride coatings.Wherein, Fig. 2 (a) is TEM photo, figure 2 (b) be SEM photograph.As can be seen that coating structure densification fails to obviously distinguish multilayered structure from Fig. 2 (b), and to painting Layer part finds that there are nano-multilayered structures in coating after carrying out TEM test observation, and wherein the brighter thinner thickness of color is richness Oxygen layer, and color is thicker compared with deep thickness for nitrogen-enriched layer.
Embodiment 2
A kind of self-assembled nanometer multilayer oxygen nitride coatings, including oxygen-rich layer AlCrSiON and nitrogen-enriched layer AlCrSiON.Its In, oxygen-rich layer with a thickness of 8nm, nitrogen-enriched layer with a thickness of 30nm, the atom percentage content of each element in coating are as follows: Al: 25at.%, Cr:15at.%, Si:5at.%, O:5at.%, N:50at.%.
By hard alloy substrate polishing treatment, it is cleaned by ultrasonic 15min through acetone, alcohol, then is packed into very with after being dried with nitrogen In empty room.Target Cr target and AlCrSi target are installed into equipment, heater is opened and is warming up to 350 DEG C, vacuum chamber is to true Reciprocal of duty cycle 5.0 × 10-3Pa or less.It is passed through the Ar gas of 250sccm, work support bias -800V is set, matrix surface is sputtered Cleaning, bombardment time 20min.Bias is down to -800V later, lights Cr target, target current 120A, with high energy Cr ion bombardment Matrix 3min.Bias is adjusted to -150V, is passed through the N of 300sccm2Gas and O2, control pressure is in 1.5Pa, O2/O2+N2Ratio is 2%, CrAlSi target is lighted, target current 80A, sedimentation time 1 hour, transfer rack revolution speed was 2r/min, rotational velocity For 4r/min.After completing plated film, it is down to room temperature to vacuum room temperature, vacuum chamber is opened and takes out matrix, obtain self-assembled nanometer oxygen Nitride coatings.
Embodiment 3
A kind of self-assembled nanometer multilayer oxygen nitride coatings, including oxygen-rich layer AlCrSiON and nitrogen-enriched layer AlCrSiON.Its In, oxygen-rich layer with a thickness of 12nm, nitrogen-enriched layer with a thickness of 60nm, the atom percentage content of each element in coating are as follows: Al: 30at.%, Cr:20at.%, Si:10at.%, O:15at.%, N:25at.%.
High speed steel substrate polishing treatment is cleaned by ultrasonic 15min through acetone, alcohol, then is packed into vacuum chamber with after being dried with nitrogen It is interior.Target Cr target and AlCrSi target are installed into equipment, heater is opened and is warming up to 400 DEG C, vacuum chamber to vacuum degree 5.0×10-3Pa or less.It is passed through the Ar gas of 300sccm, work support bias -900V is set, matrix surface sputter clear It washes, bombardment time 15min.Bias is down to -700V later, lights Cr target, target current 100A, with high energy Cr ion bombardment base Body 10min.Bias is adjusted to -120V, is passed through the N of 250sccm2And O2, control pressure is in 1.5Pa, O2/O2+N2Ratio is 10%, AlCrSi target is lighted, target current 100A, sedimentation time 1.5 hours, transfer rack revolution speed was 3r/min, and rotational velocity is 3r/min.After completing plated film, it is down to room temperature to vacuum room temperature, vacuum chamber is opened and takes out matrix, obtain self-assembled nanometer oxygen nitrogen Compound coating.
Embodiment 4
A kind of self-assembled nanometer multilayer oxygen nitride coatings, including oxygen-rich layer AlCrON and nitrogen-enriched layer AlCrON.Wherein, rich Oxygen layer with a thickness of 20nm, nitrogen-enriched layer with a thickness of 100nm, the atom percentage content of each element in coating are as follows: Al: 35at.%, Cr:25at.%, Si:0at.%, O:30at.%, N:10at.%.
By ceramic matrix polishing treatment, it is cleaned by ultrasonic 20min through acetone, alcohol, then is packed into vacuum chamber with after being dried with nitrogen It is interior.Target Cr target and AlCr target are installed into equipment, heater is opened and is warming up to 450 DEG C, vacuum chamber to vacuum degree 8.0 ×10-3Pa or less.It is passed through the Ar gas of 200sccm, -900~-1000V of work support bias is set, matrix surface is sputtered Cleaning, bombardment time 20min.Bias is down to -800V later, lights Cr target, target current 60A, with high energy Cr ion bombardment Matrix 15min.Bias is adjusted to -100V, is passed through the N of 200sccm2Gas adjusts air pressure to 1.0Pa, deposits CrN transition 5min. It is passed through O2, control pressure is in 3.0Pa, O2/O2+N2Ratio is 1%, lights AlCr target, and target current 150A, bias -150V sink Product time 2 h, transfer rack revolution speed are 5r/min, rotational velocity 1r/min.After completing plated film, to vacuum room temperature It is down to room temperature, vacuum chamber is opened and takes out matrix, obtain self-assembled nanometer oxynitride coating.
Fig. 3 is the structural schematic diagram of self-assembled nanometer oxynitride coating.It can be seen that self-assembled nanometer oxynitride applies The structure of layer is made of oxygen-rich layer and nitrogen-enriched layer, which takes into account the advantage of nitride and oxide coating, overcomes oxidation The difficult disadvantage of object coating manufacture, in the process of depositing coating, the energy of plasma and close when matrix turns to face target Degree is higher, reacts more abundant, nitrogen content is higher, and layer is also thicker;And when matrix is far from target, plasma density is lower, is easier to anti- The oxygen and metal answered generate oxygen-enriched layer, and the nanometer layer is relatively thin.Simple process, strong operability, controllability is good, low in cost, Adaptability is good, suitable for the protection of the product surfaces such as component of machine, knife mold, has preferable economic benefit.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of preparation method of self-assembled nanometer oxynitride coating, which is characterized in that comprise the following specific steps that:
S1. metallic matrix cleans: by matrix polishing treatment, being then successively cleaned by ultrasonic 10~20min with acetone, alcohol, then is used It is packed into vacuum chamber after being dried with nitrogen;
S2.Ar and metal ion bombardment: being installed into equipment for target Cr target and AlCrSi target, open heater be warming up to 300~ 500 DEG C, by vacuum chamber to vacuum degree 1.0~8.0 × 10-3Pa;The Ar gas of 200~300sccm is then passed to, work is set Part bracket -800~-1000V of bias carries out sputter clean, 10~20min of bombardment time to matrix surface;Bias is down to again- 600~-800V lights Cr target, 60~150A of target current, with high energy Cr ion bombardment 3~15min of matrix, activated metal base Body surface face is to improve film-base junction resultant force;
S3. it deposits nano laminated coating: being passed through O2And N2, adjust sample pivoted frame rotational velocity and revolution speed, control pressure exist 1.0~3.0Pa lights AlCrSi target, 60~150A of target current, bias -60~-200V, 0.5~2h of sedimentation time;
S4. arc power is closed, is down to room temperature to vacuum room temperature, vacuum chamber is opened and takes out matrix, formed in matrix surface Coating, as self-assembled nanometer oxynitride coating;The self-assembled nanometer oxynitride coating includes oxygen-rich layer and nitrogen-enriched layer, The oxygen-rich layer and nitrogen-enriched layer alternating deposit are on matrix;The ingredient of the self-assembled nanometer oxynitride coating be Al:20~ 35at.%, Cr:10~25at.%, Si:0~15at.%, O:5~50at.%, N:10~50at.%;The self assembly is received The overall thickness of rice oxynitride coating is 2~10 μm, and the thickness in monolayer of the oxygen-rich layer is 2~20nm, the list of the nitrogen-enriched layer Layer is with a thickness of 5~100nm.
2. the preparation method of self-assembled nanometer oxynitride coating according to claim 1, which is characterized in that institute in step S3 Stating rotational velocity is 1~6r/min, and the revolution speed is 0~5r/min.
3. the preparation method of self-assembled nanometer oxynitride coating according to claim 1, which is characterized in that institute in step S3 The each element atomic percent for stating AlCrSi target is Al:55~70at.%, Cr:20~35at.%, Si:0~20at.%.
4. the preparation method of self-assembled nanometer oxynitride coating according to claim 1, which is characterized in that institute in step S3 State O2Account for O2And N2The 1~25% of total volume.
5. the preparation method of self-assembled nanometer oxynitride coating according to claim 1, which is characterized in that step S1-S4 Described in matrix be metal, hard alloy or ceramics.
6. the self-assembled nanometer oxynitride coating of any one of -5 the method preparations according to claim 1, which is characterized in that institute Stating self-assembled nanometer oxynitride coating includes oxygen-rich layer and nitrogen-enriched layer, and the oxygen-rich layer and nitrogen-enriched layer alternating deposit are in matrix On.
7. self-assembled nanometer oxynitride coating according to claim 6, which is characterized in that the self-assembled nanometer oxynitriding The ingredient of object coating be Al:20~35at.%, Cr:10~25at.%, Si:0~15at.%, O:5~50at.%, N:10~ 50at.%.
8. self-assembled nanometer oxynitride coating according to claim 6, which is characterized in that the self-assembled nanometer oxynitriding The overall thickness of object coating is 2~10 μm, and the thickness in monolayer of the oxygen-rich layer is 2~20nm, and the thickness in monolayer of the nitrogen-enriched layer is 5 ~100nm.
9. self-assembled nanometer oxynitride coating according to claim 6, which is characterized in that described matrix is metal, hard Alloy or ceramics.
10. the described in any item self-assembled nanometer oxynitride coatings of claim 6-9 are in component of machine and knife mold product Application in the protection field on surface.
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