CN107190233A - A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness - Google Patents

A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness Download PDF

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Publication number
CN107190233A
CN107190233A CN201610351226.5A CN201610351226A CN107190233A CN 107190233 A CN107190233 A CN 107190233A CN 201610351226 A CN201610351226 A CN 201610351226A CN 107190233 A CN107190233 A CN 107190233A
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matrix
composite coatings
preparation technology
tialsin
coatings
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张笑
李伟
刘京京
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SHANGHAI ZENIX VACUUM COATING TECHNOLOGY Co Ltd
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SHANGHAI ZENIX VACUUM COATING TECHNOLOGY Co Ltd
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Priority to CN201610351226.5A priority Critical patent/CN107190233A/en
Publication of CN107190233A publication Critical patent/CN107190233A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • 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
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641Nitrides
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • 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
    • C23C14/0021Reactive sputtering or evaporation
    • C23C14/0036Reactive sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • 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
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

Abstract

The invention discloses a kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness, comprise the following steps:(1)Matrix is cleaned, including ultrasonic wave cleaning and Ion Cleaning;(2)It is prepared by TiN transition zones:By step(1)Matrix after processing is sent to the TiN transition zones that sputtering chamber carries out 100~200nm of deposition;(3)It is prepared by TiAlSiN nano-composite coatings:The base material after TiN transition zones will be coated, using the TiAlSi composite target materials of radio frequency cathodic control, deposit the TiAlSiN nano-composite coatings of 2~5 μ m thicks.Gained TiAlSiN coatings of the invention not only have the hardness higher than 40GPa; and with excellent high temperature oxidation resistance and decay resistance; coating production of the present invention not only has the features such as technique is simple, deposition velocity is fast, cost is low, bond strength is high simultaneously; and it is low with production efficiency height, energy consumption; the advantages of relatively low to equipment requirement, can as at a high speed, the protective coating of the cutter coat of DRY CUTTING and other field.

Description

A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness
Technical field
The present invention relates to surface modification engineering technical field, more particularly to a kind of cutter coat for being applicable to cutting tool With the preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness of the protective coating of other field.
Background technology
Cutting tool not only needs very high hardness and wearability, and needs preferable bending strength and impact tough Property.The performance of these two aspects is conflicting, it is difficult to take into account.Cutting-Tool Coating Technology is that recent decades grow up in response to the market demand Material surface modifying technology, hardness, wearability and bending strength, the impact of cutter material can be effectively solved using coating technology Contradiction between toughness, effectively improves cutting tool service life, cutter is obtained excellent comprehensive mechanical performance, so that significantly Degree improves machining efficiency.
Coating material be applied to it is on tool matrix and in conjunction, what the wearability and cutting ability of cutter were enhanced Meanwhile, the toughness of matrix in itself will not be lowered, so as to reduce the coefficient of friction between workpiece and cutter, extend the work of cutter Make the life-span.The other obvious action of cutter coat is exactly heat-insulated, due to the coefficient of heat conduction ratio quilt of most of coatings itself Processing component and tool matrix will be low it is many, cause processing in produce heat impact scatter and disappear approach change, formed heat shielding, Tool matrix is effectively protected, improves its service efficiency.
However, as cutting technology develops to high-speed cutting and DRY CUTTING direction, traditional coating, such as TiN, CrN are very The performance requirement of harshness can not gradually have been met to TiAlN coatings.With the development of Surface Science technology, by conventional Ti N, The coatings such as TiAlN incorporation Si elements can make new coating of the coating formation with nano composite structure, nano-composite coating technology It is the coating new technology developed rapidly in recent years, the grain size of its coating material is general all in below 100nm, with the hard of superelevation Degree and good combination property.Such as, the TiAlSiN coatings of Si elements formation nano composite structure are added in TiAlN, its is hard Degree can reach more than 40GPa, and its high temperature oxidation resistance is significantly improved compared with TiAlN coatings.TiAlSiN is currently advanced Protective coating material, from occur just into domestic and international research focus, in the world many enterprises also actively carry out industry answer With its topmost feature is exactly ultrahigh hardness and good heat resistance.
At present, understand that TiAlSiN coatings are successfully made by different deposition process by inquiring about document.By looking into New retrieve prepares the relevant patent of TiAlSiN coatings as follows:
The patent of Application No. 201510237876.2 discloses a kind of preparation method of the superhard gradient coatings of TiAlSiN, including One is carried out the step of sandblasting and cleaning to workpiece surface, and one is coated with TiAlSiN to workpiece using cathode ion depositing process and surpasses The step of hard gradient coating, including six stages, the first stage prepare Ti prime coat layers;Second stage prepares TiN gradient coatings, Phase III prepares TiAl gradient coatings, and fourth stage prepares TiAlN gradient coatings, and the 5th stage prepared SiN gradient coatings, the Six stages prepared TiSiN gradient coatings, and finally coating surface is processed by shot blasting.Prepared by the method for the present invention The modulus of elasticity of TiAlSiN gradient coatings is up to 340GPa, and high temperature oxidation resisting temperature is up to 1200 DEG C.
The patent of Application No. 201110439124.6 discloses a kind of TiAlSiN-DLC laminated films, including is attached to The TiAlSiN layers of metal base surface, the TiAlSiN layers for the C doping being attached on TiAlSiN layers, and it is attached to C doping DLC layer on TiAlSiN layers;Described TiAlSiN layers thickness is 0.8 μm~2 μm, the thickness of the TiAlSiN layers of the C doping For 0.3 μm~1 μm, the thickness of the DLC layer is 1 μm~2.5 μm.Between metallic matrix of the present invention and film layer, film layer inside into Point and micro-structural seamlessly transit, without obvious physical interface, realize TiAlSiN layer " no interface " combination between DLC layer, It ensure that laminated film has good high temperature oxidation resistance and self-lubricating abrasion-resistant antifriction performance concurrently.
The patent of Application No. 201210139265.0 discloses a kind of wear-resistant and oxidation resistant nanometer composite Ti AlSiN The preparation method of superhard coating, will be put into electric arc and magnetron sputtering composite coating equipment after substrate pretreated, with post arc Ti targets As Ti sources, pass through the sputtering raste of post arc power current control post arc Ti targets;Come using plane Si targets, Al targets as respective element Source, plane Si targets and Al targets are placed on inboard wall of furnace body in the way of to target, by the Power Control for adjusting medium-frequency pulse power supply The sputtering raste of target;Main ionization of gas is used as using high-purity Ar, it is ensured that effective glow discharging process;Using high-purity N2As anti- Gas is answered, makes its ionization and is combined with Ti, Si, Al element, deposit to form TiAlSiN coatings in matrix surface, it is prepared TiAlSiN coating layer thicknesses are 3.5 microns, and coating microhardness 40GPa, coefficient of friction is about that 0.7, TiAlSiN coatings are anti-oxidant Temperature can reach 1000 DEG C, with excellent antioxygenic property and abrasion resistance properties.
The patent of Application No. 201510808060.0, which is disclosed, a kind of superhard receives micron multi-layer composite coatings and its preparation Method, the superhard micron multi-layer composite coatings of receiving are made up of TiAlSiN layers, TiCN layer, TiN layer, and its coating structure is from inside to outside TiN layer, TiCN layer, TiAlSiN layer are followed successively by, the preparation method of the coating is physical vapour deposition (PVD), and each layer coating structure is Nano-micron compound structure, TiAlSiN/TiCN/TiN laminated coatings thickness prepared by the present invention is 2.5~3.5um, with high Hardness, wearability and high temperature oxidation resistance, its transition layer structure improve the adhesion of coating and matrix, reduce coatings growth Intrinsic stress and thermal stress, it is possible to increase the performance and working life of tool and mould.
The patent of Application No. 201010192207.5, which discloses a kind of CrTiAlSiN nano-composite coatings, deposition, this Cutter of coating and preparation method thereof.The composite coating includes tack coat, supporting layer and main wearing layer, and tack coat is Cr, support Layer is CrN, and main wearing layer is to replace the compound painting of the CrSiN/TiAlSiN nanometer multilayers constituted with TiAlSiN layers by CrSiN layers Layer.Above-mentioned tack coat is deposited on tool matrix, redeposited supporting layer and main wearing layer obtain depositing the knife of the coating Tool.Gained CrTiAlSiN nano-composite coatings of the invention have the advantages that hardness is high, coefficient of friction is low, adhesive force is strong.
The patent of Application No. 201510756629.3 discloses a kind of nitrogen boron titanium/nitrogen sial titanium nanocomposite laminated coating knife Tool, is attached with transition zone and wearing layer on tool matrix successively from the inside to the outside, and transition zone is TiN, wearing layer by TiBN layer with TiAlSiN layers are alternately combined composition.The present invention additionally provides the preparation method of above-mentioned cutter simultaneously, is first sunk before coating is carried out One layer of transition zone of product, transition zone can greatly improve the adhesive force of coating;Then deposit under certain condition nano combined many Layer coating, by controlling work rest rotating speed and nitrogen pressure, to realize the change of multi-layer compound film modulation period, to adjust one The thickness in individual double-deck cycle.TiBN/TiAlSiN nanocomposite laminated coating cutters of the invention prepared have good adhesion and Wear-resisting, resistance to elevated temperatures, it is ensured that cutter long-term stable operation.
However, in the above documents, there is the problem of coating mechanical property is contradicted with coating cost, some coating hardness It is not high etc. mechanical property, it is impossible to meet the part Service Environment gone from bad to worse;And the coating material of some better performances, prepare work Skill is again relative complex, so that causing the production cost of coating increases.Therefore, develop that technique is simple, production cost is low, with height Hardness, the TiAlSiN nano-composite coatings of high-wearing feature and its technology of preparing are key issues urgently to be resolved hurrily.
The content of the invention
In order to solve the problems of the prior art, it is an object of the invention to provide a kind of technique is simple, deposition velocity fast, into The preparation technology of this Si dopen Nano composite coating with ultrahigh hardness that low, production efficiency is high, energy consumption is low, this technique pair is set It is standby to require relatively low, can as high speed, the cutter coat of DRY CUTTING and other field protective coating.Made using this technique Coating has higher hardness, and with excellent high temperature oxidation resistance and decay resistance, bond strength is high.
To achieve these goals, the technical solution adopted by the present invention is:
A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness, it comprises the following steps:
S1, matrix cleaning:The cleaning of described matrix includes the ultrasonic wave cleaning successively carried out successively and Ion Cleaning;
The preparation of S2, TiN transition zone:Once purged matrix is sent to sputtering chamber, passes through DC power control Ti targets, vacuum chamber Background vacuum be better than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power be 80~120W, sputtering Time is 5~10min, makes the thick TiN transition zones of 100~200nm of substrate deposit by sputtering;
The preparation of S3, TiAlSiN nano-composite coating:Matrix after handling through step S2 is continued to deposit, Ti-Si composite target materials By radio frequency cathodic control, the background vacuum of vacuum chamber is better than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, splash Power is penetrated for 200~350W, sputtering time is 90~120min, is heated during matrix deposition, as obtained by sputtering makes step S2 The TiN of matrix crosses on layer the TiAlSiN nano-composite coatings for depositing 2~5 μ m-thicks.
It is preferred that scheme, described in step S1 ultrasonic wave cleaning be by through polish mirror finish processing after matrix anhydrous In ethanol and acetone 5~10min is cleaned using ultrasonic wave.
Further preferred scheme, the method for the Ion Cleaning described in step S1 is:By the sample after being cleaned through ultrasonic wave Sample Room is inserted after installing, Ar is opened after vacuumizing, maintenance vacuum is 2~4Pa, carries out 30min ion to matrix with intermediate frequency Bombardment, the power of Ions Bombardment is 80~100W.
Scheme still more preferably, the matrix described in the step S1 is metal, hard alloy or ceramics.
Scheme still further preferably, have described in step S3 the TiAlSiN nano-composite coatings of nano composite structure by The TiAlN phases and Si of NaCl structures is presented3N4Phase composition.
Ar and N described in step S2 and S32Mixed gas in, N2Flow be 5~10sccm, Ar flows be 30~ 50sccm, N2Scope with Ar flow-rate ratio is:3/38~7/38.
The distance between Ti-Si composite target materials in Ti targets and step S3 in step S2 and matrix scope is 5~ 7cm。
The air pressure range that TiAlSiN nano-composite coatings described in step S3 are deposited is 0.2~0.6Pa.
The cleaning frequency of ultrasonic wave is 15~30kHz in the step S1, and intermediate frequency is 13.56Hz.
The temperature range that step S3 described matrixes are heated when depositing is 200~400 DEG C.
By using above technical scheme, a kind of preparation of the Si dopen Nano composite coatings with ultrahigh hardness of the present invention Compared with prior art, its advantage is technique:
1st, the TiAlSiN coated bodies that the present invention is obtained are by TiAlN phases and Si3N4The phase composition of interface phase two, and in coating Portion forms nano composite structure, i.e. Si3N4The mutually crystallite-cladded size in interface is 5~10nm TiAlN nanocrystals, in the nanometer Under composite construction, dislocation motion is difficult to carry out, therefore, and this coating can obtain higher hardness, and its hardness can be higher than 40GPa.
2nd, the coating that the present invention is obtained has excellent high temperature oxidation resistance and decay resistance.
3rd, not only manufacture craft is simple, deposition velocity is fast, cost is low, bond strength is high by the present invention, and with production effect Rate is high, energy consumption is low, it is relatively low to equipment requirement the advantages of, can as high speed, the cutter coat of DRY CUTTING and other field guarantor Protect coating.
Brief description of the drawings
Fig. 1 is a kind of process chart of the preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness of the present invention.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to instantiation and with reference to attached Figure, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the present invention's Scope.In addition, in the following description, the description to known features and technology is eliminated, to avoid unnecessarily obscuring the present invention Concept.
Used instrument is respectively in the preparation method of the present invention:
The many target dual chamber magnetic control sputtering systems of JGP-450 types;
M308457 supersonic wave cleaning machines.
Method of testing of the present invention:
EDAX energy disperse spectroscopies(EDS)Analysis ingredient;
The VB/PC type X-ray diffractometers of D/MAX 2550(XRD)Determine thing phase composition;
NANO Indenter G200 types nano-hardness tester measures consistency and elasticity modulus.
A kind of Si dopen Nanos composite coating material and its preparation technology with ultrahigh hardness, as shown in attached body 1, it is wrapped Include following preparation process:
(1)Matrix is cleaned
Matrix after mirror finish processing of polishing is cleaned into 5~10min in absolute ethyl alcohol and acetone using ultrasonic wave;
Then Ion Cleaning is carried out:Load Sample Room after sample is installed, open Ar gas after vacuumizing, maintain vacuum 2~ 4Pa, 30min Ions Bombardment is carried out with intermediate frequency to described matrix, and power is 80~100W;
(2)It is prepared by TiN transition zones
By step(1)Matrix after processing is sent to sputtering chamber, and by DC power control Ti targets, the background vacuum of vacuum chamber is excellent In 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power be 80~120W, sputtering time be 5~10min, Carry out 100~200nm of deposition TiN transition zones;
(3)It is prepared by TiAlSiN nano-composite coatings
By step(2)Matrix after processing continues to deposit, and Ti-Si composite target materials are by radio frequency cathodic control, and the background of vacuum chamber is true Reciprocal of duty cycle is better than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power be 200~350W, sputtering time is 90 ~120min, is heated during matrix deposition, the TiAlSiN nano-composite coatings of 2~5 μm of deposition.
This patent floating coat is prepared on JGP-450 type multi-target magnetic control sputtering instrument using reactive sputtering.Using high-speed steel, Hard alloy etc. is as matrix, and the ion that progress 30min in vacuum chamber is loaded after acetone and the cleaning of absolute ethyl alcohol ultrasonic wave is clear Wash, then deposited using direct current or RF-reactively sputtered titanium method.
Prepared in following embodiment also according to above-mentioned steps, simply design parameter is slightly varied, it is specific as follows:
Embodiment 1
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:5cm;N2Stream Amount:5sccm;Ar flows:38sccm;Total gas pressure:0.4Pa;Temperature:300℃;Radio-frequency power supply power:350W, sedimentation time: 90min.After tested, it is 42.4GPa to obtain coating hardness, and coating layer thickness is 2.5 μm.
Embodiment 2
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:6cm;N2Stream Amount:10sccm;Ar throughputs:48sccm;Total gas pressure:0.6Pa;Temperature:250℃;Radio-frequency power supply power:300W, sedimentation time: 120min.After tested, it is 40.4GPa to obtain coating hardness, and coating layer thickness is 4.6 μm.
Embodiment 3
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:7cm;N2Stream Amount:6sccm;Ar throughputs:40sccm;Total gas pressure:0.5Pa;Temperature:350℃;Radio-frequency power supply power:320W, sedimentation time: 100min.After tested, it is 41.6GPa to obtain coating hardness, and coating layer thickness is 3.7 μm.
Embodiment 4
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:5cm;N2Stream Amount:5sccm;Ar throughputs:30sccm;Total gas pressure:0.2Pa;Temperature:200℃;Radio-frequency power supply power:280W, sedimentation time: 110min.After tested, it is 42.8GPa to obtain coating hardness, and coating layer thickness is 3.2 μm.
Embodiment 5
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:6cm;N2Stream Amount:7sccm;Ar throughputs:45sccm;Total gas pressure:0.4Pa;Temperature:250℃;Radio-frequency power supply power:300W, sedimentation time: 100min.After tested, it is 40.7GPa to obtain coating hardness, and coating layer thickness is 2.6 μm.
Embodiment 6
The specific process parameter of TiAlSiN nano-composite coatings preparation method proposed by the present invention is:Target-substrate distance:7cm;N2Stream Amount:9sccm;Ar throughputs:42sccm;Total gas pressure:0.4Pa;Temperature:300℃;Radio-frequency power supply power:330W, sedimentation time: 90min.After tested, it is 40.4GPa to obtain coating hardness, and coating layer thickness is 3.0 μm.
Above-mentioned embodiment is exemplary, be in order to preferably make skilled artisans appreciate that this Patent, it is impossible to be not understood as including this patent the limitation of scope;As long as times made of spirit according to disclosed in this patent How with change or modification, the scope that this patent includes is each fallen within.

Claims (10)

1. a kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness, it is characterised in that it includes following step Suddenly:
S1, matrix cleaning:The cleaning of described matrix includes the ultrasonic wave cleaning successively carried out successively and Ion Cleaning;
The preparation of S2, TiN transition zone:
Once purged matrix is sent to sputtering chamber, by DC power control Ti targets, the background vacuum of vacuum chamber is better than 5 10-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power be 80~120W, sputtering time be 5~10min, pass through Sputtering makes the thick TiN transition zones of 100~200nm of substrate deposit;
The preparation of S3, TiAlSiN nano-composite coating:
Matrix after handling through step S2 is continued to deposit, Ti-Si composite target materials are by radio frequency cathodic control, and the background of vacuum chamber is true Reciprocal of duty cycle is better than 510-3Pa, sputtering atmosphere uses Ar and N2Mixed gas, sputtering power be 200~350W, sputtering time is 90 ~120min, is heated during matrix deposition, and the TiN of the matrix as obtained by sputtering makes step S2, which is crossed, deposits 2~5 μ m-thicks on layer TiAlSiN nano-composite coatings.
2. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the cleaning of ultrasonic wave described in step S1 be by the matrix after mirror finish processing of polishing in absolute ethyl alcohol and acetone 5~10min is cleaned using ultrasonic wave.
3. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the method for the Ion Cleaning described in step S1 is:Sample Room is inserted after sample after being cleaned through ultrasonic wave is installed, is taken out Ar is opened after vacuum, maintenance vacuum is 2~4Pa, carries out 30min Ions Bombardment, the power of Ions Bombardment to matrix with intermediate frequency For 80~100W.
4. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the matrix described in the step S1 is metal, hard alloy or ceramics.
5. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, there is the TiAlSiN nano-composite coatings of nano composite structure by the TiAlN phases of presentation NaCl structures described in step S3 And Si3N4Phase composition.
6. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, Ar and N described in step S2 and S32Mixed gas in, N2Flow be 5~10sccm, Ar flows be 30~ 50sccm, N2Scope with Ar flow-rate ratio is:3/38~7/38.
7. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the distance between the Ti-Si composite target materials in Ti targets and step S3 in step S2 and matrix scope are 5~7cm.
8. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the air pressure range that TiAlSiN nano-composite coatings described in step S3 are deposited is 0.2~0.6Pa.
9. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the cleaning frequency of ultrasonic wave is 15~30kHz in the step S1, and intermediate frequency is 13.56Hz.
10. a kind of preparation technology of Si dopen Nano composite coatings with ultrahigh hardness according to claim 1, it is special Levy and be, the temperature range that step S3 described matrixes are heated when depositing is 200~400 DEG C.
CN201610351226.5A 2016-05-25 2016-05-25 A kind of preparation technology of the Si dopen Nano composite coatings with ultrahigh hardness Pending CN107190233A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN109930106A (en) * 2019-05-08 2019-06-25 哈尔滨工业大学 A kind of preparation method of the TiAlSi/TiAlSiN multilayer alternate coatings with high wear resistance ability
CN111254401A (en) * 2020-03-09 2020-06-09 浙江申吉钛业股份有限公司 Method for improving adhesion strength of hard wear-resistant nano coating of titanium alloy plate
CN111455338A (en) * 2020-05-08 2020-07-28 上海新弧源涂层技术有限公司 Nano multilayer coating, preparation method thereof and cutter with nano multilayer coating coated on surface
CN111926292A (en) * 2020-09-09 2020-11-13 上海仟纳真空镀膜科技有限公司 Composite coating and preparation method and application thereof
CN112391591A (en) * 2020-11-11 2021-02-23 中国科学院合肥物质科学研究院 WCrSiN superhard coating and preparation method thereof
CN113564526A (en) * 2021-07-27 2021-10-29 上海工具厂有限公司 Composite coating film and preparation method and application thereof

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