CN104002516A - CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and preparation method thereof - Google Patents
CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a CrAlN/MoS2 multi-layered coating layer with high rigidity and low friction coefficient and a preparation method thereof. According to the CrAlN/MoS2 multi-layered coating layer, CrAlN nano-layers and MoS2 nano-layers are formed on a matrix by alternatively sputtering and depositing through a multi-target magnetron sputtering manner, wherein the CrAlN nano-layers are close to the matrix; the upmost layer is the one MoS2 nano-layer; the total thickness of the CrAlN/MoS2 multi-layered coating layer is 2.0-4.5 micrometers; the thickness of each CrAlN nano-layer is 5.0 nanometers and the thickness of each MoS2 nano-layer is 0.2-1.4 nanometers. The preparation method comprises the following steps: arranging the washed matrix in a multi-target magnetron sputtering instrument; alternatively staying in the front of a CrAl alloy target and an MoS2 alloy target in argon-nitrogen mixed atmosphere; controlling the thickness of each coating layer by adjusting the powers and deposition times of the CrAl target and the MoS2 target to finally obtain the CrAlN/MoS2 multi-layered coating layer.
Description
Technical field
The present invention relates to a kind of New Rigid protective finish, particularly a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating and preparation method thereof, the military service occasion that be mainly used in and require high rigidity, there is again high friction resistance energy.
Background technology
Along with social development and scientific and technological progress, material surface performance has been proposed to more and more higher requirement, not only require it to there is higher hardness, decay resistance, more require it to there is higher wear resistance, to meet more and more higher requirement of engineering.At material surface, applying protective hard coat is a kind of economical and practical effective way that improves material surface performance; protective coating is as an important branch of mechanical function film; in machine tools application very wide, particularly in metal cutting, accounted for leading position.Hard coat can improve the surface property of material, and the friction and wear of minimizing and workpiece, effectively improves material surface hardness, toughness, wearability and high-temperature stability, increases substantially the service life of coating product.Its development has adapted to the high-tech requirement of modern manufacturing industry to metal cutting tool, has caused the great change of cutter material and performance, can be widely used in the fields such as machine-building, auto industry, textile industry, geological drilling, mould industry, Aero-Space.
For many years; ternary nitride is widely used in protectiveness hard coating material owing to having high hardness, wearability, corrosion resistance, the higher advantages such as antioxygenic property; as TiAlN, CrAlN, ZrAlN and TiSiN etc., improving the serviceability of part and on the life-span, obtaining good effect.Yet more severe along with current material military service environment, has higher requirement to performances such as the hardness of coating material, wear resistances.Therefore traditional signal layer coating can not meet the requirement of severe service condition gradually, in the urgent need to the protective coating material of development of new.Along with the development of nanometer science and technology, nano laminated coating becomes the important development direction of hard coating material.So-called laminated coating is by two or more composition or the different material of structure alternating growth and the two-dimentional multilayer material that forms mutually on perpendicular to coating surface direction, laminated coating for two kinds of different structures or composition, every adjacent two layers forms an elementary cell, its thickness is called modulation period, conventionally the laminated coating that is less than to 100nm modulation period becomes nano laminated coating, research shows, when be specific thickness modulation period, nano laminated coating will present abnormal " the superhard effect " raising of hardness, make nano laminated coating there is high mechanical property.In addition, as a kind of Two-dimensional Composites, nano laminated coating can make full use of the advantage of every kind of material, and its combination property is got a promotion.Therefore, nano laminated coating is the important development direction of novel protected type hard coat.
By reading up the literature, learn, nano laminated coating successfully makes by several different methods at present, obtains many useful achievements, as TiN/CrAlSiN, Ti/TiCrN, ZrO
2/ TiN etc.By inquiry, retrieve the following relevant Chinese patent of preparing nano laminated coating:
Application number is that 201410044737.3 patent has related to a kind of TiN/CrAlSiN nanocomposite laminated coating and preparation method.Described TiN/CrAlSiN nanocomposite laminated coating is formed on matrix by CrAlSiN layer and the TiN layer alternating deposit of nano composite structure, and one deck of close matrix is TiN layer, the CrAlSiN layer that the superiors are nano composite structure; Described TiN/CrAlSiN nanocomposite laminated coating thickness is 2.0-3.2 μ m, and the CrAlSiN layer thickness of described nano composite structure is 1.2nm, and described TiN layer thickness is 6.0nm.Its preparation method comprises 2 steps such as cleaning matrix and alternating sputtering CrAlSiN layer and TiN layer.This TiN/CrAlSiN nanocomposite laminated coating hardness is higher, and when the atomic ratio of Si and CrAl, when Si:CrAl is 5:20, its hardness is up to 39.7GPa.
Application number is that 201310129525.0 patent has related to a kind of nano laminated coating, it is characterized in that this coating at least comprises sedimentary deposit, this sedimentary deposit is formed by comprised TiAlSiN subgrade and CrAlN subgrade alternating deposit, and, in described TiAlSiN subgrade, the atom content of Si is 2～12%, the nanocrystalline CrAlN microscopic structure that described CrAlN subgrade contains B1 structure.The invention also discloses the preparation method of this nano laminated coating.Compared with prior art, the present invention obtains nano laminated coating and has advantages of high rigidity, high tenacity, high thermal stability and high antioxidant.
Application number is that 201310082478.9 patent relates to a kind of Ti/TiCrN nano laminated coating impeller and preparation technology thereof, impeller matrix material is 25 steel, impeller matrix surface is that the multilayer of nano TiC rN, CrTiN, TiN and CrN is mixed phase structure high hardness spray coating, between impeller matrix and high surface hardness coating, contains one deck ti interlayer.Concrete technology comprises the multilayer mixing phase structure high hardness spray coating of pre-treatment, Ion Cleaning, titanium deposition transition zone, deposition surface nano TiC rN, CrTiN, TiN and CrN.Ti/TiCrN nano laminated coating impeller when can keep higher hardness, improve coating toughness and and matrix between bond strength, thereby improve resistance to impact and the wearability of coating, extend the service life of impeller.The impeller of preparing by the method, compares with the impeller of coating not, and wearability and decay resistance are improved largely.
Application number is that 201210193969.6 patent relates to the technique that a kind of PVD technology is prepared super hard nano composite laminated coating, and this PVD technology is prepared the technique of super hard nano composite laminated coating, comprises the following steps: the pretreatment on a, tool and mould surface; Preheating of b, tool and mould; The etching on c, tool and mould surface; Being coated with of d, TiN rete; Being coated with of e, (TiN+CrN) rete; Being coated with of f, CrAlN rete.The internal stress of the super hard nano composite laminated coating that this technique is prepared is little, thereby makes the bond strength on be coated with super hard nano composite laminated coating and tool and mould surface good, adhesion >75N; And the tool and mould that has been coated with super hard nano composite laminated coating has the advantages that red hardness is high, non-oxidizability is high, wearability is high and price is low.
Application number is that 201110082001.1 patent has related to a kind of Ti-Zr/ZrN nano laminated coating cutter and preparation technology thereof, tool matrix material is carbide alloy or high-speed steel, tool matrix surface is ZrN high hardness spray coating, between tool matrix and ZrN high hardness spray coating, have Ti transition zone, be the sandwich construction that Zr and ZrN replace between Ti transition zone and surperficial ZrN high hardness spray coating.Concrete technology comprises pre-treatment, Ion Cleaning, depositing Ti transition zone, repeatedly deposits the step of Zr layer and ZrN layer, deposition surface ZrN layer.Ti-Zr/ZrN nano laminated coating cutter contains high rigidity ZrN coating and ductile metal Zr, when can keep higher hardness, improve coating toughness and and matrix between bond strength, thereby improve the wearability of coating.
Application number is that 200610029133.7 patent has related to a kind of ZrO
2/ TiN hard nanometer laminated coating, belongs to field of ceramic coatings.The present invention is by ZrO
2layer and TiN layer alternating deposit form in carbide alloy, pottery or metallic substrates, ZrO
2the thickness of layer is 2～8nm, and TiN bed thickness is 0.4～1.2nm, and total coating thickness is 2～5mm.ZrO of the present invention
2the dual-target sputtering technology of/TIN nano laminated coating employing in argon atmospher is at metal or the ceramic matrix surface alternating deposit ZrO of polishing
2layer and TiN layer obtain.The ZrO of gained of the present invention
2/ TiN nano laminated coating not only has excellent high-temperature oxidation resistance, and has the hardness of 19.1GPa to 23GPa.The present invention, as high speed cutting tool and other coating wear-resisting, corrosion-resistant workpiece of being on active service under hot conditions, has very high using value and the possibility of popularization.
Yet above-mentioned existing coating still exists the problem that hardness, friction and wear behavior, deposition efficiency and cost cannot be taken into account, there is hardness and wear Characteristics and have to be hoisted, production efficiency and the more high a series of shortcomings of cost.
Summary of the invention
The object of the invention is, in order to overcome the deficiencies in the prior art, provides a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, this CrAlN/MoS
2laminated coating, adopts the combination of ternary nitride and sulfide, by CrAlN layer and MoS
2the sandwich construction of the nanometer scale with high rigidity and high friction resistance energy that layer alternating deposit forms on matrix.
An other object of the present invention is to provide above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, this preparation method has that production efficiency is high, energy consumption is low, to advantages such as equipment requirement are lower.
technical scheme of the present invention
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, on matrix, the mode alternating sputtering deposition by multi-target magnetic control sputtering forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 2.0-4.5 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 0.2～1.4nm;
Described matrix is metal, carbide alloy, pottery or plastics.
The described CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating is worked as MoS
2when nanometer layer thickness is less than 1.0nm, MoS
2nanometer layer is forced to be converted into face-centred cubic structure under the template action of CrAlN layer.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of nano laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.2Pa-0.6Pa; Ar throughput is 20-50sccm, N
2throughput is 20-50sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 2-10s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
useful technique effect of the present invention
A kind of CrAlN/MoS with high rigidity and low-friction coefficient of the present invention
2laminated coating, owing to adopting higher CrAlN nanometer layer and the lower MoS of coefficient of friction of hardness
2nanometer layer replaces laminated coating prepared by magnetron sputtering, utilizes the coherence epitaxial growth structure of nano laminated coating to suppress dislocation motion, makes the CrAlN/MoS of final gained
2the hardness of laminated coating gets a promotion, and its highest hardness reaches 39.2 GPa;
Further, a kind of CrAlN/MoS with high rigidity and low-friction coefficient of the present invention
2laminated coating, due to MoS
2adding of nanometer layer makes this CrAlN/MoS
2laminated coating has lower coefficient of friction, and the coefficient of friction of itself and GCr15 steel ball is lower than 0.30, thereby shows excellent crocking resistance.Therefore, this has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating can be used as protective finish, for require high rigidity, again have high friction resistance can military service occasion.
Further, a kind of CrAlN/MoS with high rigidity and low-friction coefficient of the present invention
2the preparation method of laminated coating, owing to adopting reaction magnetocontrol sputtering preparation technology, has the advantages that preparation technology is simple, deposition velocity is fast, production efficiency is high, production cost is low.
Accompanying drawing explanation
The CrAlN/MoS with high rigidity and low-friction coefficient of Fig. 1, embodiment 3 gained
2the transmission electron microscope picture of the cross section of laminated coating.
The specific embodiment
Below by specific embodiments and the drawings, the present invention is described in further detail, but do not limit the present invention.
Preparation, sign and measuring instrument that the present invention is used:
JGP-450 type magnetic control sputtering system, Chinese Academy of Sciences Shenyang scientific instrument development center Co., Ltd
D/MAX 2550 VB/PC type X-ray diffractometers, Rigaku Co., Ltd.
NANO Indenter G200 type nano-hardness tester, U.S. Agilent Technologies
Tecnai G
220 type high resolution transmission electron microscopies, U.S. FEI Co.
HSR-2M coating friction wear testing machine, Ke Kaihua Science and Technology Development Co., Ltd. in Lanzhou
embodiment 1
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, on matrix, the mode alternating sputtering deposition by multi-target magnetic control sputtering forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 2.5 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 0.2nm;
Described matrix is carbide alloy.
The above-mentioned CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, MoS
2nanometer layer thickness is 0.2nm, MoS
2layer, by CrAlN institute crystallization, is face-centred cubic structure.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.4Pa; Ar throughput is 32sccm, N
2throughput is 32sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 2s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
Above-mentioned gained has the CrAlN/MoS of high rigidity and low-friction coefficient
2after testing, CrAlN nanometer layer thickness is 5nm to laminated coating, MoS
2nanometer layer thickness is 0.2nm, has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating gross thickness is 2.5 μ m, and hardness is 36.8GPa, and the coefficient of friction in rubbing with GCr15 steel ball is 0.27.
embodiment 2
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, the mode alternating sputtering deposition by multi-target magnetic control sputtering on matrix forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 2.9 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 0.6nm;
Described matrix is high-speed steel.
The above-mentioned CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, MoS
2nanometer layer thickness is 0.2nm, MoS
2layer, by CrAlN institute crystallization, is face-centred cubic structure.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.2Pa; Ar throughput is 20sccm, N
2throughput is 20sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 4s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
Above-mentioned gained has the CrAlN/MoS of high rigidity and low-friction coefficient
2after testing, CrAlN nanometer layer thickness is 5nm to laminated coating, MoS
2nanometer layer thickness is 0.6nm, has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating gross thickness is 2.9 μ m, and hardness is 37.1GPa, and the coefficient of friction in rubbing with GCr15 steel ball is 0.24.
embodiment 3
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, the mode alternating sputtering deposition by multi-target magnetic control sputtering on matrix forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 3.4 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 1.0nm;
Described matrix is carbide alloy.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.5Pa; Ar throughput is 36sccm, N
2throughput is 36sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 6s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
Above-mentioned gained has the CrAlN/MoS of high rigidity and low-friction coefficient
2after testing, CrAlN nanometer layer thickness is 5.0nm to laminated coating, MoS
2nanometer layer thickness is 1.0nm, has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating gross thickness is 3.4 μ m, and hardness is 39.2GPa, and the coefficient of friction in rubbing with GCr15 steel ball is 0.28.
Adopt Tecnai G
220 type high resolution transmission electron microscopies (U.S. FEI Co.) are to above-mentioned gained CrAlN/MoS
2the cross section of nano laminated coating is observed, the microstructure of the painting layer cross section of gained as shown in Figure 1, as can be seen from Figure 1 CrAlN nanometer layer and MoS
2between nanometer layer, there is sandwich construction, each CrAlN layer and MoS
2layer thickness is respectively 5.0nm and 1.0nm, and can find out lattice fringe continuous run through a plurality of nanometer layer, show MoS
2nanometer layer, by CrAlN institute crystallization, is face-centred cubic structure, CrAlN nanometer layer and MoS
2between nanometer layer, form coherence epitaxial growth structure, this coherent growth interface On Dislocation Motion has inhibition, makes CrAlN/MoS
2coating is strengthened.
embodiment 4
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, the mode alternating sputtering deposition by multi-target magnetic control sputtering on matrix forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 3.9 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 1.2nm;
Described matrix is high-speed steel.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.6Pa; Ar throughput is 50sccm, N
2throughput is 50sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 8s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
Above-mentioned gained has the CrAlN/MoS of high rigidity and low-friction coefficient
2after testing, CrAlN nanometer layer thickness is 5nm to laminated coating, MoS
2nanometer layer thickness is 1.2nm, has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating gross thickness is 3.9 μ m, and hardness is 37.6GPa, and the coefficient of friction in rubbing with GCr15 steel ball is 0.30.
embodiment 5
A kind of CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, the mode alternating sputtering deposition by multi-target magnetic control sputtering on matrix forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
The described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is about 4.5 μ m, and the thickness of each CrAlN nanometer layer is about 5.0nm, each MoS
2the thickness of nanometer layer is 1.4nm;
Described matrix is silicon oxide ceramics.
Above-mentioned a kind of CrAlN/MoS with high rigidity and low-friction coefficient
2the preparation method of laminated coating, specifically comprises the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.4Pa; Ar throughput is 40sccm, N
2throughput is 28sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 10s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
Above-mentioned gained has the CrAlN/MoS of high rigidity and low-friction coefficient
2after testing, CrAlN nanometer layer thickness is 5nm to laminated coating, MoS
2nanometer layer thickness is 1.4nm, has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating gross thickness is 4.5 μ m, and hardness is 37.2GPa, and the coefficient of friction in rubbing with GCr15 steel ball is 0.26.
In sum, a kind of CrAlN/MoS with high rigidity and low-friction coefficient of the present invention
2laminated coating, owing to adopting higher CrAlN nanometer layer and the lower MoS of coefficient of friction of hardness
2nanometer layer replaces laminated coating prepared by magnetron sputtering, MoS
2layer can be presented face-centred cubic structure by CrAlN institute crystallization, and keeps coherence epitaxial growth structure with CrAlN, utilizes this OILS STRUCTURE DEPRESSION dislocation motion, makes the CrAlN/MoS of final gained
2the hardness of laminated coating gets a promotion, and its highest hardness reaches 39.2 GPa; In addition, due to MoS
2adding of nanometer layer makes this CrAlN/MoS
2laminated coating has lower coefficient of friction, and the coefficient of friction of itself and GCr15 steel ball is lower than 0.30, thereby shows excellent crocking resistance.Therefore, this has the CrAlN/MoS of high rigidity and low-friction coefficient
2laminated coating can be used as protective finish, for require high rigidity, again have high friction resistance can military service occasion.
The above is only giving an example of embodiments of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (5)
1. a CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, is characterized in that the described CrAlN/MoS with high rigidity and low-friction coefficient
2laminated coating, on matrix, the mode alternating sputtering deposition by multi-target magnetic control sputtering forms CrAlN nanometer layer and MoS
2nanometer layer, one deck of close matrix is CrAlN nanometer layer, the superiors are MoS
2nanometer layer;
Described matrix is metal, carbide alloy or pottery.
2. the CrAlN/MoS with high rigidity and low-friction coefficient as claimed in claim 1
2laminated coating, is characterized in that the described CrAlN/MoS with high rigidity and low-friction coefficient
2the gross thickness of laminated coating is 2.0-4.5 μ m, and the thickness of each CrAlN nanometer layer is 5.0nm, each MoS
2the thickness of nanometer layer is 0.2～1.4nm.
3. the CrAlN/MoS with high rigidity and low-friction coefficient as claimed in claim 2
2laminated coating, is characterized in that described MoS
2when nanometer layer thickness is less than 1.0nm, MoS
2nanometer layer is face-centred cubic structure.
4. the CrAlN/MoS with high rigidity and low-friction coefficient as claimed in claim 1
2the preparation method of laminated coating, is characterized in that specifically comprising the steps:
(1), clean matrix
First, the matrix after polishing is sent into supersonic wave cleaning machine, with acetone and absolute ethyl alcohol, with 15～30kHz, carry out respectively Ultrasonic Cleaning 10min successively;
Then, the matrix after Ultrasonic Cleaning is put into vacuum chamber, be evacuated down to 6 * 10
-4after Pa, passing into Ar gas, maintain vacuum at 2-4Pa, is that 80-100W radio-frequency power supply carries out Ions Bombardment 30min to matrix and carries out Ion Cleaning with power;
(2), alternating sputtering CrAlN layer and MoS
2layer
Matrix by step (1) after Ion Cleaning is inserted in multi-target magnetic control sputtering instrument, in argon, nitrogen mixed gas atmosphere, alternately rests on CrAl alloys target and MoS
2before target, by sputter, obtain by a plurality of CrAlN nanometer layer and MoS
2nanometer layer is the nanometer scale laminated coating of stack alternately, adjusts CrAl target and MoS in process
2the power of target and sedimentation time to be to control the thickness of each coating, the final CrAlN/MoS must with high rigidity and low-friction coefficient
2laminated coating;
The control ginseng technique number of above-mentioned sputter procedure is:
In described CrAl alloys target, Cr and Al are 1:1 by atomic ratio, MoS
2the purity of target is 99.99%;
CrAl alloys target and MoS
2the diameter of target is 75mm;
Described argon, nitrogen mixed gas atmosphere, total gas pressure is 0.2Pa-0.6Pa; Ar throughput is 20-50sccm, N
2throughput is 20-50sccm;
CrAlN nanometer layer sputtering power 120W, time 10s;
MoS
2nanometer layer sputtering power 80W, time 2-10s;
Target-substrate distance 3-7cm;
Substrate temperature is 300 ℃.
5. the NbN/WS with high rigidity and low-friction coefficient as claimed in claim 4
2the preparation method of laminated coating, is characterized in that the JGP-450 type magnetic control sputtering system that the multi-target magnetic control sputtering Yi Wei Chinese Academy of Sciences Shenyang scientific instrument development center Co., Ltd described in step (2) produces.
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