CN104878359B - High rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings and preparation method thereof - Google Patents
High rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings and preparation method thereof Download PDFInfo
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Abstract
The present invention provides high rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings and preparation method thereof, belong to protective coating technical field.TiAlN layer and ZrSiN layer of the coating including several alternating deposits；When making the coating, substrate TiAl targets and ZrSi targets alternating sputtering are made several times.The coating of the present invention has many advantages, such as that hardness is high, high-wearing feature, and the preparation method of coating has controllable, deposition rate height at low cost, simple for process and environmentally safe.
Description
Technical field
The present invention relates to a kind of novel protective coating, more particularly to a kind of height with TiAlN and ZrSiN alternating deposits
It is resistance to be mainly used in high-mechanic, height for hardness and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings and preparation method thereof
The piece surface of mill, so as to improve the service life of part.
Background technology
With the development of advanced manufacturing industry, increasingly higher demands are proposed to the surface property of material, it is desirable that material table
Face has higher hardness, wear-resisting, corrosion-resistant and high temperature resistance.It is to improve material to coat one layer of superhard coating in material surface
A kind of effective way of surface property, its development have adapted to high-tech requirement of the modern manufacturing industry to metal cutting tool, can
It is widely used in the fields such as machine-building, auto industry, geological drilling, mould industry.With high-speed cutting, DRY CUTTING etc.
The continuous development of advanced cutting technology, also proposed the performance of coating higher requirement, traditional coating, as TiN, TiCN,
CrN, TiAlN coating cannot gradually be met the requirements.
With the development of nanometer science and technology, nano-structured coating becomes the important development direction of hard coating material.
So-called nano-structured coating includes nanometer multilayer and nano combined two kinds of structures.Laminated coating is by two or more ingredient
Or the different material of structure is in the two-dimentional multilayer material that growth is alternateed on coating surface direction and is formed, for two
The laminated coating of kind different structure or composition forms a basic unit per adjacent two layers, and thickness is known as modulation period, usually
Laminated coating of the modulation period less than 100nm is known as nano laminated coating, research shows that, it is specific thickness when modulation period
When, nano laminated coating is extremely raised " super-hardness effect " by presentation hardness, and nano laminated coating is made to have high mechanical property.
In addition, as a kind of Two-dimensional Composites, the advantages of nano laminated coating can make full use of each material, make the comprehensive of its
It can get a promotion.Therefore, nano laminated coating is the important development direction of novel protected type hard coat.Nano-composite coating is
Refer to the composite structure coating that matrix phase is mutually coated by interface, since the crystallite dimension of matrix phase is generally several to tens nanometers, because
This is called nano-composite coating, which equally has super-hardness effect, it has also become the important development direction in superhard coating field.
It is learnt by reading up the literature, nanometer multilayer and nano composite structure coating have successfully been made at present by a variety of methods
, obtain many beneficial achievements, such as TiZrAlSiON, AlTiN/AlCrN, TiAlZrN/CrN, AlN/Si3N4.By looking into
It askes, retrieves the following Chinese patent in relation to preparing nanostructured superhard coating：
Application No. is CN201410170158 patent be related to a kind of TiZrAlSiON nano composite super-hards coated cutting tool and
Preparation method, coated cutting tool include hard alloy cutter ontology, coating TiZrAlSiON nano-composite coatings on cutter body,
TiZrAlSiON coatings include 50-100 nanometer thickness metal prime coat Zr metal layers, 100-200 nanometer thickness nitride transition layers
ZrN, 1000-4000 nanometer thickness functional layer TiZrAlSiON are formed, and it is non-that which there is nano-crystalline granule to be embedded in
The nano composite structure of brilliant matrix, nano particle is TiN and ZrN, and noncrystal substrate includes Al2O3 and Si3N4；Prepared
TiZrAlSiON composite coatings are with hardness is high, friction coefficient is low, toughness and binding force are strong, the spies such as excellent high temperature resistance oxygen
Point.
Patent application No. is CN201210368027 is related to a kind of AlTiN-AlCrN super hard nanos multi-layer composite coatings rolling
Serrated knife and preparation method thereof.It is generated in hobcutter using arc ion plating (aip) by Cr, CrN, AlTiN/CrN, AlTiN/AlCrN
The nano-composite coating formed successively.AlTiN/AlCrN coatings and high-speed steel or hard alloy gear hobbing prepared by the invention
Cutter has good binding force, good hardness and superior heat resistance.
Application No. is CN201410398736 patent be related to a kind of high rigidity TiAlZrN/CrN nano laminated coatings and its
Preparation method；The nano laminated coating is formed by multiple TiAlZrN layers and CrN layers, and each TiAlZrN layers and CrN layers alternately heavy
Product forms nanometer scale multilayered structure on matrix, and overall thickness is 2.4~5.8 μm；The preparation side of the nano laminated coating
Method is first by matrix surface polishing treatment, after ultrasonic cleaning and Ion Cleaning, then using reactive sputtering on matrix
TiAlZrN layers and CrN layers of alternating sputtering.
Patent application No. is CN200710135578 is related to a kind of nano-structured coating and preparation method thereof, described
AlN/Si3N4 nano-multilayer films are formed in by AlN and Si3N4 on the matrix of metal or ceramics, are alternating deposit nanometer scale
Multilayered structure, each layer thickness range are：AlN layer thickness is 2.0-12nm, and Si3N4 layers are 0.4-12.0nm, and overall thickness is arrived for 1.0
5.0 micron.During preparation, metal or ceramic matrix surface are made into mirror finish processing first, then by metal or ceramics
Si3N4 layers and AlN layers of double-target radio frequency reactive sputtering method alternating deposit is carried out using pure Al and Si targets on matrix, is passed through high-purity
Ar and N2 produces AlN/Si3N4 nano-multilayer films.The thickness of AlN/Si3N4 multilayer films is by increasing the modulation period of multilayer film
Number obtains.
However, in studied for superhard coating in the past, there are problems that mechanical property is contradicted with coating cost, some
The mechanical properties such as coating hardness are not high, it is impossible to meet worsening part Service Environment；And the coating material of certain better performances
Material, preparation process is again relative complex, and so as to cause coating, the production cost increases.Therefore, simple for process, production cost is developed
It is low, have high rigidity, the nano-structured coating material of high-wearing feature and its technology of preparing modern material Surface Engineering field urgently
The critical issue of solution.
Invention content
Regarding the issue above, the present invention provides a kind of TiAlN/ZrSiN with high rigidity and high-wearing feature
Nanostructured protective coating.
It is a further object of the present invention to provide a kind of TiAlN/ZrSiN nanostructured protectiveness simple for process, at low cost
The preparation method of coating.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings, the coating are deposited on substrate,
Substrate is metal, hard alloy or ceramics, the TiAlN layers of the coating including several alternating deposits with ZrSiN layers.
In above-mentioned coating, the overall thickness of the coating is 2.0-5.0 μm.
In above-mentioned coating, ZrSiN layers have ZrN and SiNx two phase structures.
In above-mentioned coating, the ZrSiN layer thickness is less than 1.6nm, and ZrSiN layers are made in TiAlN layers of template
Face-centred cubic structure is converted under.
In above-mentioned coating, the TiAlN layers of the coating bottom are deposited on TiN transition zones.
The preparation method of a kind of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings, including following
Step：
Step A, TiAlN layers are sputtered：Reactive sputtering is carried out the substrate face TiAl targets of splash coating are needed；
Step B, ZrSiN layers are sputtered：After completing step A, rotation substrate makes substrate face ZrSi targets carry out reactive sputtering；
Step C, alternating sputtering：Step A-B is repeated several times, so as to form the TiAlN layers including several alternating deposits
With ZrSiN layers of coating.
In above-mentioned preparation method, in step, the Ti contents of TiAl targets are 50at%, in stepb, ZrSi targets
In Si contents be 16-32at%.
In above-mentioned preparation method, in step, substrate residence time above TiAl targets is 16s, in stepb,
Substrate residence time above ZrSi targets is 6s, and in step C, the modulation period of coating is by accurately controlling Si substrates in TiAl
Residence time before target and ZrSi targets realizes that the rotation period of substrate is 150 times, and the thickness of coating is 2.0-5.0 μm.
In above-mentioned preparation method, in step, before reactive sputtering is carried out to substrate, further include and clean substrate
The step of with depositing TiN transition zone, wherein, substrate cleaning is that the substrate after polishing is sent into supersonic wave cleaning machine, and use is anhydrous
Alcohol and/or acetone clean 5-10min under 15-30kHz, and substrate then is put into vacuum chamber, is evacuated down to 6 × 10-4After Pa
It is passed through Ar gas, maintains vacuum degree in 2-4Pa, with intermediate frequency to substrate into the ion bombardment of 30min during behavior, power 80-100W；
Depositing TiN transition zone is to put the substrate after ion bombardment in sputtering chamber into, is reacted using pure Ti targets (99.99at.%)
Sputtering, by DC power control Ti targets, power 120W passes through Ar and N2Flow is respectively 32sccm and 2sccm, and substrate is not
Heating, sedimentation time 5min.
In above-mentioned preparation method, the sputtering of step A and step B are using multi-target magnetic control sputtering instrument, wherein DC power supply
Control TiAl targets, radio-frequency power supply control ZrSi targets, ZrSiN layers of sputtering power 300W, time 6s；TiAlN layers of sputtering power 120W,
Time 20s；Ar throughputs are 38sccm；N2Throughput is 5sccm；Target-substrate distance is 5-7cm；Total gas pressure is 0.2-0.6Pa；Sputtering
Temperature is -300 DEG C of room temperature.
Compared with prior art, the advantage of the invention is that：The coating that the present invention develops is replaced by TiAlN and ZrSiN
The high rigidity of deposition and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings, wherein ZrSiN is by ZrN and SiNx two-phases
Composition is formed the multilayered structure coating of nanometer scale by TiAlN and ZrSiN alternating deposits on matrix, superhard so as to enrich
Coating material research field content proposes a kind of design method of novel super-hard protective coating material in engineering practice, because
This has important meaning and value in science and engineering practice field.
The preparation method of the present invention, using physical gas-phase deposition to TiAlN/ZrSiN nano-structured coating systems
It is standby, have many advantages, such as coating it is at low cost, it is simple for process it is controllable, deposition rate is high and environmentally safe.
Description of the drawings
Fig. 1 is the structure diagram of coating provided by the invention.
In figure：ZrSiN layers 1, TiAlN layers 2, TiN transition zones 3, substrate 4.
Specific embodiment
Embodiment 1
(1) matrix is cleaned
Polished treated matrix is sent into supersonic wave cleaning machine first, it is sharp in analytically pure absolute alcohol and acetone
Cleaning 5-10min is carried out with 15-30kHz ultrasonic waves；Then Ion Cleaning is carried out, i.e., matrix is put into vacuum chamber, is evacuated down to 6
×10-4It is passed through Ar gas after Pa, maintains vacuum degree in 2-4Pa, with intermediate frequency to matrix into the ion bombardment of 30min during behavior, power
For 80-100W；
(2) depositing TiN transition zone
Substrate after ion bombardment is put into sputtering chamber, depositing TiN transition zone is strong to improve the combination of coating and matrix
Degree.In our current research, reactive sputtering is carried out using pure Ti targets (99.99at%), by DC power control Ti targets, power is
120W passes through Ar and N2Flow is respectively 32sccm and 2sccm, and substrate does not heat, sedimentation time 5min；
(3) alternating sputtering TiAlN layers and ZrSiN layers
By rotating substrate frame, substrate face TiAl (Ti successively are allowed:Al=50at%:50at%) target and ZrSi targets (Si
Content is 16-32at.%) obtain TiAlN/ZrSiN nano-structured coatings, the modulation period of coating is by accurately controlling Si bases
Residence time of the piece before TiAl targets and ZrSi targets is realized.In the present embodiment, substrate residence time above TiAl targets is
16s；Substrate residence time above ZrSi targets is 6s.The rotation period of substrate is 150 times when preparing nano-multilayer film, and deposition applies
The thickness of layer is 2.0-5.0 μm.
The process control parameter of above-mentioned sputtering process is：DC power control TiAl targets, radio-frequency power supply control ZrSi targets；
ZrSiN layers of sputtering power 300W, time 6s；TiAlN layers of sputtering power 120W, time 20s；Si contents are in 16- in ZrSi targets
32at%；Ar throughputs are 38sccm；N2Throughput is 5sccm；Target-substrate distance is 5-7cm；Total gas pressure range 0.2-0.6Pa；It splashes
Temperature is penetrated as -300 DEG C of room temperature.
Preparation, characterization and measuring instrument used in the present invention：JGP-450 type magnetic control sputtering systems, Chinese Academy of Sciences's Shenyang science
Instrument development centered finite company；2550 VB/PC type X-ray diffractometers of D/MAX, Rigaku Co., Ltd.；NANO
Indenter G200 type nano-hardness testers, Agilent Technologies of the U.S..
Embodiment 2
The present embodiment and the preparation process of embodiment 1 are essentially identical, and the difference lies in Ar throughputs are 38sccm, N2
Throughput is 5sccm；In ZrSi targets Si contents in 16at%, ZrSiN Si contents in 8at%；Total gas pressure is 0.4Pa；ZrSiN
Sputtering power 300W, time 6s；TiAlN sputtering power 120W, time 20s；Substrate temperature is room temperature, and matrix is metal.
After testing, the hardness of TiAlN/ZrSiN nanostructured protective coatings is 35.9GPa under this technique.
Embodiment 3
The present embodiment and the preparation process of embodiment 1 are essentially identical, and the difference lies in Ar throughputs are 38sccm, N2
Throughput is 5sccm；In ZrSi targets Si contents in 20at%, ZrSiN Si contents in 10at%；Total gas pressure is 0.2Pa；
ZrSiN sputtering power 300W, time 6s；TiAlN sputtering power 120W, time 20s；Substrate temperature is 100 DEG C.
After testing, the hardness of TiAlN/ZrSiN nanostructured protective coatings is 39.4GPa under this technique.
Embodiment 4
The present embodiment and the preparation process of embodiment 1 are essentially identical, and the difference lies in Ar throughputs are 38sccm, N2
Throughput is 5sccm；In ZrSi targets Si contents in 24at%, ZrSiN Si contents in 12at%；Total gas pressure is 0.6Pa；
ZrSiN sputtering power 300W, time 6s；TiAlN sputtering power 120W, time 20s；Substrate temperature is 200 DEG C.
After testing, the hardness of TiAlN/ZrSiN nanostructured protective coatings is 43.5GPa under this technique.
Embodiment 5
The present embodiment and the preparation process of embodiment 1 are essentially identical, and the difference lies in Ar throughputs are 38sccm, N2
Throughput is 5sccm；In ZrSi targets Si contents in 32at%, ZrSiN Si contents in 14at.%；Total gas pressure is 0.4Pa；
ZrSiN sputtering power 300W, time 6s；TiAlN sputtering power 120W, time 20s；Substrate temperature is 300 DEG C.
Embodiment 6
As shown in Figure 1, present embodiments provide a kind of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protectiveness
Coating, the coating are prepared by method described in embodiment 1.
The coating is deposited on substrate 4, which includes one layer of TiN transition zone 3 for being deposited on 4 surface of substrate, in TiN mistakes
Crossing alternating deposit on layer 3 has several TiAlN layers 2 and ZrSiN layers 1.Substrate 4 be metal, hard alloy or ceramics, coating it is total
Thickness is 2.0-5.0 μm.
Preferred embodiment, 1 thickness of ZrSiN layers are less than 1.6nm, and ZrSiN layers 1 have ZrN and SiNx two phase structures, and
ZrSiN layers 1 are converted into face-centred cubic structure under the template action of TiAlN layers 2.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or additions to described specific embodiment or replace in a similar way
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (2)
1. a kind of preparation method of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructured protective coatings, which is characterized in that
Include the following steps：
(1) matrix is cleaned
Polished treated matrix is sent into supersonic wave cleaning machine first, is utilized in analytically pure absolute alcohol and acetone
15-30kHz ultrasonic waves carry out cleaning 5-10min；Then Ion Cleaning is carried out, i.e., matrix is put into vacuum chamber, it is evacuated down to 6 ×
10-4It is passed through Ar gas after Pa, maintaining vacuum degree, with intermediate frequency to matrix into the ion bombardment of 30min during behavior, power is in 2-4Pa
80-100W；
(2) depositing TiN transition zone
Substrate after ion bombardment is put into sputtering chamber, depositing TiN transition zone is to improve the bond strength of coating and matrix.
In this research, reactive sputtering is carried out using pure Ti targets, by DC power control Ti targets, power 120W passes through Ar and N2Stream
Amount is respectively 32sccm and 2sccm, and substrate does not heat, sedimentation time 5min；
(3) alternating sputtering TiAlN layers and ZrSiN layers
By rotating substrate frame, allowing substrate, face TiAl targets and ZrSi targets obtain TiAlN/ZrSiN nano-structured coatings successively,
In ZrSi targets Si contents in 24at%, ZrSiN Si contents in 12at%；Total gas pressure is 0.6Pa；ZrSiN sputtering power 300W,
Time 6s；TiAlN sputtering power 120W, time 20s；Substrate temperature is 200 DEG C.
2. the preparation method of coating according to claim 1, which is characterized in that the thickness of coating is 2.0-5.0 μm.
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| CN105925946B (en) * | 2016-05-06 | 2018-11-06 | 辽宁科技大学 | A method of using magnetron sputtering method TiN or CrN films are prepared in aluminum alloy surface |
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|---|---|---|---|---|
| CN102337499A (en) * | 2011-11-03 | 2012-02-01 | 上海理工大学 | TiAlN/SiO2 nanometer multilayer coating of high-hardness and high elastic modulus and preparation method thereof |
| CN103273687A (en) * | 2013-05-13 | 2013-09-04 | 山东大学 | TiSiN+ZrSiN composite nanometer coated cutting tool and preparation method thereof |
| CN104204275A (en) * | 2012-03-07 | 2014-12-10 | 山高刀具公司 | Nanolaminated coated cutting tool |
| CN204752842U (en) * | 2015-06-12 | 2015-11-11 | 浙江金盾链条制造有限公司 | High rigidity and high wearing feature tiAlNZrSiN nanostructured protective coating |
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| JP5003947B2 (en) * | 2007-06-07 | 2012-08-22 | 住友電工ハードメタル株式会社 | Surface coated cutting tool |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102337499A (en) * | 2011-11-03 | 2012-02-01 | 上海理工大学 | TiAlN/SiO2 nanometer multilayer coating of high-hardness and high elastic modulus and preparation method thereof |
| CN104204275A (en) * | 2012-03-07 | 2014-12-10 | 山高刀具公司 | Nanolaminated coated cutting tool |
| CN103273687A (en) * | 2013-05-13 | 2013-09-04 | 山东大学 | TiSiN+ZrSiN composite nanometer coated cutting tool and preparation method thereof |
| CN204752842U (en) * | 2015-06-12 | 2015-11-11 | 浙江金盾链条制造有限公司 | High rigidity and high wearing feature tiAlNZrSiN nanostructured protective coating |
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