CN104878359A - High-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating and preparation method thereof - Google Patents
High-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating and a preparation method thereof and belongs to the technical field of protective coatings. The protective coating comprises a plurality of alternatively deposited TiA1N layers and ZrSiN layers. When the coating is manufactured, a substrate is prepared by a plurality of times of alternative sputtering conducted on a TiA1N target and a ZrSiN target. The high-hardness and high-abrasion-resisting TiA1N/ZrSiN nano-structure protective coating has the advantages of being high in hardness and abrasion resistance, and the preparation method of the coating has the advantages of being low in cost, simple and controllable in process, high in deposition speed, free of environment pollution and the like.
Description
Technical field
The present invention relates to a kind of novel protective coating; in particular to a kind of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructure protective coating and preparation method thereof with TiAlN and ZrSiN alternating deposit; be mainly used in the piece surface of high-mechanic, high abrasion, thus improve the work-ing life of part.
Background technology
Along with the development of advanced manufacturing industry, more and more higher requirement is proposed to the surface property of material, require that material surface has higher hardness, wear-resisting, corrosion-resistant and resistance to elevated temperatures.Applying one deck superhard coating at material surface is a kind of effective way improving material surface performance, its development has adapted to the hi-tech requirement of modern manufacturing industry to metal cutting tool, can be widely used in the fields such as machinofacture, automotive industry, geological drilling, mould industry.Along with the development of the advanced cutting technology such as high speed cutting, DRY CUTTING, higher requirement be it is also proposed to the performance of coating, traditional coating, as TiN, TiCN, CrN, TiAlN coating can not meet the demands gradually.
Along 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 comprises nanometer multilayer and nano combined two kinds of structures.Laminated coating is at the two-dimentional multilayer material formed perpendicular to alternating growth mutual on coatingsurface direction by two or more composition or the different material of structure, for the laminated coating of two kinds of different structures or composition, every adjacent two layers forms an elementary cell, its thickness is called modulation period, usually the laminated coating being less than 100nm modulation period is called nano laminated coating, research shows, when modulation period is specific thickness, nano laminated coating, by presenting abnormal " super-hardness effect " raised of hardness, makes nano laminated coating have high mechanical property.In addition, as a kind of Two-dimensional Composites, nano laminated coating can make full use of the advantage of often kind of material, and its over-all properties is got a promotion.Therefore, nano laminated coating is the important development direction of novel protected type hard coat.Nano-composite coating refers to the composite structure coating by the coated matrix phase of interfacial phase, grain-size due to matrix phase is generally several to tens nanometers, therefore be called nano-composite coating, this coating has super-hardness effect equally, has become the important development direction in superhard coating field.
Learn by reading up the literature, nanometer multilayer and nano composite structure coating are successfully obtained by multiple method at present, obtain much useful achievement, as TiZrAlSiON, AlTiN/AlCrN, TiAlZrN/CrN, AlN/Si3N4 etc.By inquiry, retrieve as follows about the Chinese patent of preparation nanostructure superhard coating:
Application number is that the patent of CN201410170158 relates to a kind of TiZrAlSiON nano composite super-hard coated cutting tool and preparation method thereof, coated cutting tool comprises inserted tool body, coating TiZrAlSiON nano-composite coating on cutter body, TiZrAlSiON coating comprises 50-100 nanometer thickness metal prime coat Zr metal level, 100-200 nanometer thickness nitride transition layer ZrN, 1000-4000 nanometer thickness functional layer TiZrAlSiON is formed, this nano-composite coating has the nano composite structure that nano-crystalline granule is embedded in noncrystal substrate, nano particle is TiN and ZrN, and noncrystal substrate comprises Al2O3 and Si3N4, prepared TiZrAlSiON compound coating has that hardness is high, frictional coefficient is low, toughness and bonding force strong, the features such as excellent high temperature resistance oxygen.
Application number is that the patent of CN201210368027 relates to a kind of AlTiN-AlCrN super hard nano multi-layer composite coatings hobcutter and preparation method thereof.Arc ion plating (aip) is adopted to generate the nano-composite coating be made up of successively Cr, CrN, AlTiN/CrN, AlTiN/AlCrN at hobcutter.AlTiN/AlCrN coating prepared by this invention and rapid steel or Wimet hobcutter have good bonding force, good hardness and superior heat resistance.
Application number is that the patent of CN201410398736 relates to a kind of high rigidity TiAlZrN/CrN nano laminated coating and preparation method thereof; Described nano laminated coating is made up of multiple TiAlZrN layer and CrN layer, and each TiAlZrN layer and CrN layer alternating deposit form nanometer scale multilayered structure on matrix, and its total thickness is 2.4 ~ 5.8 μm; The preparation method of described nano laminated coating is first by matrix surface polished finish, after ultrasonic cleaning and Ion Cleaning, then adopts reactive sputtering to replace sputtered with Ti AlZrN layer and CrN layer on matrix.
Application number is that the patent of CN200710135578 relates to a kind of nano-structured coating and preparation method thereof, described AlN/Si3N4 nano-multilayer film is formed in by AlN and Si3N4 on the matrix of metal or pottery, for the multilayered structure of alternating deposit nanometer scale, each layer thickness scope is: AlN layer thickness is 2.0-12nm, Si3N4 layer is 0.4-12.0nm, and total thickness is 1.0 to 5.0 microns.During preparation, first metal or ceramic matrix surface are done mirror polish process, then by adopting pure Al and Si target to carry out double-target radio frequency reactive sputtering method alternating deposit Si3N4 layer and AlN layer on the matrix of metal or pottery, passing into high-purity Ar and N2, producing AlN/Si3N4 nano-multilayer film.The thickness of AlN/Si3N4 multilayer film is obtained by number modulation period increasing multilayer film.
But in studying for superhard coating, there is mechanical property and the conflicting problem of coating cost, the mechanical properties such as some coating hardness are not high, can not meet the part Service Environment gone from bad to worse in the past; And the coated material of some better performances, preparation technology's relative complex again, thus cause the production cost of coating to increase.Therefore, develop that technique is simple, production cost is low, there is high rigidity, the nano-structured coating material of high-wearing feature and technology of preparing modern material Surface Engineering field thereof key issue urgently to be resolved hurrily.
Summary of the invention
The object of the invention is for the problems referred to above, a kind of TiAlN/ZrSiN nanostructure protective coating with high rigidity and high-wearing feature is provided.
Another object of the present invention is to provide the preparation method of the TiAlN/ZrSiN nanostructure protective coating that a kind of technique is simple, cost is low.
For achieving the above object, the present invention adopts following technical proposals:
A kind of high rigidity and high-wearing feature TiAlN/ZrSiN nanostructure protective coating, this painting is deposited upon on substrate, and substrate is metal, Wimet or pottery, and this coating comprises TiAlN layer and the ZrSiN layer of several alternating deposits.
In above-mentioned coating, the total thickness of this coating is 2.0-5.0 μm.
In above-mentioned coating, described ZrSiN layer has ZrN and SiNx two phase structure.
In above-mentioned coating, described ZrSiN layer thickness is less than 1.6nm, and ZrSiN layer is converted into face-centred cubic structure under the template action of TiAlN layer.
In above-mentioned coating, the TiAlN of this coating bottom is deposited upon on TiN transition layer.
A preparation method for high rigidity and high-wearing feature TiAlN/ZrSiN nanostructure protective coating, comprises the following steps:
Steps A, sputtered with Ti AlN layer: just reactive sputtering is carried out to TiAl target needing the substrate of splash coating;
Step B, sputtering ZrSiN layer: after completing steps A, rotate substrate and make substrate just carry out reactive sputtering to ZrSi target;
Step C, alternating sputtering: repeating step A-B several times, thus formation comprises the TiAlN layer of several alternating deposits and the coating of ZrSiN layer.
In above-mentioned preparation method, in step, the Ti content of TiAl target is 50at%, and in stepb, the Si content in ZrSi target is 16-32at%.
In above-mentioned preparation method, in step, substrate residence time above TiAl target is 16s, in stepb, substrate residence time above ZrSi target is 6s, and in step C, the modulation period of coating is by accurately the residence time of control Si substrate before TiAl target and ZrSi target realizes, 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, also comprise the step by substrate cleaning and depositing TiN transition layer, wherein, substrate cleaning be by polishing after substrate send in Ultrasonic Cleaners, under 15-30kHz, clean 5-10min with raw spirit and/or acetone, then substrate is put into vacuum chamber, be evacuated down to 6 × 10
-4pass into Ar gas after Pa, maintain vacuum tightness at 2-4Pa, with intermediate frequency to substrate carry out for time 30min ion bombardment, power is 80-100W; Depositing TiN transition layer be by ion bombardment after substrate put in sputtering chamber, utilize pure Ti target (99.99at.%) to carry out reactive sputtering, by DC power control Ti target, power is 120W, by Ar and N
2flow is respectively 32sccm and 2sccm, and substrate does not heat, and depositing time is 5min.
In above-mentioned preparation method, the sputtering of steps A and step B adopts multi-target magnetic control sputtering instrument, wherein DC power control TiAl target, radio-frequency power supply control ZrSi target, ZrSiN layer sputtering power 300W, time 6s; TiAlN layer sputtering power 120W, time 20s; Ar airshed is 38sccm; N
2airshed is 5sccm; Target-substrate distance is 5-7cm; Total gas pressure is 0.2-0.6Pa; Sputter temperature is room temperature-300 DEG C.
Compared with prior art; the invention has the advantages that: the coating of the present invention's exploitation is by the high rigidity of TiAlN and ZrSiN alternating deposit and high-wearing feature TiAlN/ZrSiN nanostructure protective coating; wherein ZrSiN is by ZrN and SiNx two phase composite; on matrix, the multilayered structure coating of nanometer scale is formed by TiAlN and ZrSiN alternating deposit; thus enriched superhard coating investigation of materials field content; engineering practice proposes a kind of method of design of novel super-hard supercoat material, therefore all has important meaning and value at Science and engineering practise area.
Preparation method of the present invention, adopts physical gas-phase deposition to be prepared TiAlN/ZrSiN nano-structured coating, has that coating cost is low, technique is simply controlled, sedimentation rate is high and the advantage such as environmentally safe.
Accompanying drawing explanation
Fig. 1 is the structural representation of coating provided by the invention.
In figure: ZrSiN layer 1, TiAlN layer 2, TiN transition layer 3, substrate 4.
Embodiment
Embodiment 1
(1) matrix is cleaned
First the matrix after polished finish is sent into Ultrasonic Cleaners, in analytically pure raw spirit and acetone, utilize 15-30kHz ultrasonic wave to carry out cleaning 5-10min; Then carry out Ion Cleaning, put into vacuum chamber by matrix, be evacuated down to 6 × 10
-4pass into Ar gas after Pa, maintain vacuum tightness at 2-4Pa, with intermediate frequency to matrix carry out for time 30min ion bombardment, power is 80-100W;
(2) depositing TiN transition layer
Put in sputtering chamber by the substrate after ion bombardment, depositing TiN transition layer is to improve the bonding strength of coating and matrix.In this research, utilize pure Ti target (99.99at%) to carry out reactive sputtering, by DC power control Ti target, power is 120W, by Ar and N
2flow is respectively 32sccm and 2sccm, and substrate does not heat, and depositing time is 5min;
(3) alternating sputtering TiAlN layer and ZrSiN layer
By rotation base horse, allow substrate just obtain TiAlN/ZrSiN nano-structured coating to TiAl (Ti:Al=50at%:50at%) target and ZrSi target (Si content is 16-32at.%) successively, the modulation period of coating is by accurately the residence time of control Si substrate before TiAl target and ZrSi target realizes.In the present embodiment, substrate residence time above TiAl target is 16s; Substrate residence time above ZrSi target is 6s.During preparation nano-multilayer film, the rotation period of substrate is 150 times, and the thickness of deposited coatings is 2.0-5.0 μm.
The process control parameter of above-mentioned sputter procedure is: DC power control TiAl target, radio-frequency power supply control ZrSi target; ZrSiN layer sputtering power 300W, time 6s; TiAlN layer sputtering power 120W, time 20s; In ZrSi target, Si content is at 16-32at%; Ar airshed is 38sccm; N
2airshed is 5sccm; Target-substrate distance is 5-7cm; Total gas pressure scope 0.2-0.6Pa; Sputter temperature is room temperature-300 DEG C.
The present invention's preparation used, sign and surveying instrument: JGP-450 type magnetic control sputtering system, Chinese Academy of Sciences Shenyang scientific instrument development center company limited; D/MAX 2550 VB/PC type X-ray diffractometer, Rigaku Co., Ltd.; NANO Indenter G200 type nano-hardness tester, Agilent Technologies of the U.S..
Embodiment 2
The present embodiment is substantially identical with the preparation process of embodiment 1, and difference is, Ar airshed is 38sccm, N
2airshed is 5sccm; In ZrSi target Si content in 16at%, ZrSiN Si content at 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, under this technique, the hardness of TiAlN/ZrSiN nanostructure protective coating is 35.9GPa.
Embodiment 3
The present embodiment is substantially identical with the preparation process of embodiment 1, and difference is, Ar airshed is 38sccm, N
2airshed is 5sccm; In ZrSi target Si content in 20at%, ZrSiN Si content at 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, under this technique, the hardness of TiAlN/ZrSiN nanostructure protective coating is 39.4GPa.
Embodiment 4
The present embodiment is substantially identical with the preparation process of embodiment 1, and difference is, Ar airshed is 38sccm, N
2airshed is 5sccm; In ZrSi target Si content in 24at%, ZrSiN Si content at 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, under this technique, the hardness of TiAlN/ZrSiN nanostructure protective coating is 43.5GPa.
Embodiment 5
The present embodiment is substantially identical with the preparation process of embodiment 1, and difference is, Ar airshed is 38sccm, N
2airshed is 5sccm; In ZrSi target Si content in 32at%, ZrSiN Si content at 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 nanostructure protective coating, this coating is prepared by the method described in embodiment 1.
This painting is deposited upon on substrate 4, and this coating comprises one deck TiN transition layer 3 being deposited on substrate 4 surface, and TiN transition layer 3 alternately deposits several TiAlN layers 2 and ZrSiN layer 1.Substrate 4 is metal, Wimet or pottery, and the total thickness of coating is 2.0-5.0 μm.
Preferred version, ZrSiN layer 1 thickness is less than 1.6nm, and described ZrSiN layer 1 has ZrN and SiNx two phase structure, and ZrSiN layer 1 is converted into face-centred cubic structure under the template action of TiAlN layer 2.
Specific embodiment described herein is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various amendment or supplement or adopt similar mode to substitute to described specific embodiment, but can't depart from spirit of the present invention or surmount the scope that appended claims defines.
Claims (10)
1. high rigidity and a high-wearing feature TiAlN/ZrSiN nanostructure protective coating, is characterized in that, this coating comprises TiAlN layer and the ZrSiN layer of several alternating deposits.
2. coating according to claim 1, is characterized in that, the total thickness of this coating is 2.0-5.0 μm.
3. coating according to claim 1 and 2, is characterized in that, described ZrSiN layer has ZrN and SiNx two phase structure.
4. coating according to claim 3, is characterized in that, described ZrSiN layer thickness is less than 1.6nm, and ZrSiN layer is converted into face-centred cubic structure under the template action of TiAlN layer.
5. coating according to claim 1 and 2, is characterized in that, the TiAlN of this coating bottom is deposited upon on TiN transition layer.
6. a preparation method for high rigidity and high-wearing feature TiAlN/ZrSiN nanostructure protective coating, is characterized in that, comprise the following steps:
Steps A, sputtered with Ti AlN layer: just reactive sputtering is carried out to TiAl target needing the substrate of splash coating;
Step B, sputtering ZrSiN layer: after completing steps A, rotate substrate and make substrate just carry out reactive sputtering to ZrSi target;
Step C, alternating sputtering: repeating step A-B several times, thus formation comprises the TiAlN layer of several alternating deposits and the coating of ZrSiN layer.
7. the preparation method of coating according to claim 6, is characterized in that, in step, the Ti content of TiAl target is 50at%, and in stepb, the Si content in ZrSi target is 16-32at%.
8. the preparation method of the coating according to claim 6 or 7, is characterized in that, in step, substrate residence time above TiAl target is 16s, and in stepb, substrate residence time above ZrSi target is 6s, in step C, the thickness of coating is 2.0-5.0 μm.
9. the preparation method of the coating according to claim 6 or 7, it is characterized in that, in step, before reactive sputtering is carried out to substrate, also comprise the step by substrate cleaning and depositing TiN transition layer, wherein, substrate cleaning be by polishing after substrate send in Ultrasonic Cleaners, under 15-30kHz, clean 5-10min with raw spirit and/or acetone, then substrate is put into vacuum chamber, be evacuated down to 6 × 10
-4pass into Ar gas after Pa, maintain vacuum tightness at 2-4Pa, with intermediate frequency to substrate carry out for time 30min ion bombardment, power is 80-100W; Depositing TiN transition layer be by ion bombardment after substrate put in sputtering chamber, utilize pure Ti target to carry out reactive sputtering, by DC power control Ti target, power is 120W, by Ar and N
2flow is respectively 32sccm and 2sccm, and substrate does not heat, and depositing time is 5min.
10. the preparation method of the coating according to claim 6 or 7, is characterized in that, the sputtering of steps A and step B adopts multi-target magnetic control sputtering instrument, wherein DC power control TiAl target, radio-frequency power supply control ZrSi target, ZrSiN layer sputtering power 300W, time 6s; TiAlN layer sputtering power 120W, time 20s; Ar airshed is 38sccm; N
2airshed is 5sccm; Target-substrate distance is 5-7cm; Total gas pressure is 0.2-0.6Pa; Sputter temperature is room temperature-300 DEG C.
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