CN104141107B - A kind of Al-Cu-N abrasion-resistant hardcoat and its preparation method - Google Patents
A kind of Al-Cu-N abrasion-resistant hardcoat and its preparation method Download PDFInfo
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Abstract
The present invention discloses a kind of Al-Cu-N abrasion-resistant hardcoat, is made up of mutually with Cu crystal AlN crystal phase, and wherein, Cu crystal is dispersed in AlN crystal mutually, and the interface between Cu crystal phase and AlN crystal phase is bonded with Cu-Al key; Described Al-Cu-N abrasion-resistant hardcoat is made up of the Cu element of atomic percentage conc 74.6%��89%Al and N and 11%��25.4%. Al-Cu-N abrasion-resistant hardcoat of the present invention has good hardness and excellent abrasion resistance properties, and wear rate is lower than 4.0 �� 10-16m3/ Nm, reaches the requirement of high-wearing feature, can extensively for the field such as mould, mechanical component. The invention also discloses the preparation method of a kind of Al-Cu-N abrasion-resistant hardcoat, adopt reaction magnetocontrol sputtering method, workable, controllability is good, is easy to suitability for industrialized production, has broad application prospects and good economic benefit.
Description
Technical field
The present invention relates to wear-resistant coating and preparation field thereof, it is specifically related to a kind of Al-Cu-N abrasion-resistant hardcoat and its preparation method.
Background technology
Friction is the phenomenon that we often run into, have in the world the energy of 1/1 to two/3rds by rubbing consumption fall, and damage machine and engineering structure, reduce working efficiency. Surface-coated wear-resistant coating at machine and device becomes a kind of effective way reducing frictional dissipation. So far, find and develop the important task that wear-resistant coating is material technology expert always.
Researchist finds the metallic element (such as: Ni, Ag, Cu etc.) by doping appropriate amount in metal nitride (such as: CrN, TiN, AlN etc.), preparing hard phase/soft matter phase nano-composite coating, the mechanical property such as the hardness of coating, wear resistance and toughness obtains improvement in various degree. The coatings such as common transition metal nitride, carbide, boride have high hardness, but toughness is relatively low. Metal has good plasticity and toughness, but hardness is lower.
The hardness of block AlN is about 12GPa only, is not used as wear-resistant coating traditionally. But, adding appropriate metallographic phase at AlN, it is possible to improve the over-all properties of AlN coating, existing research mainly concentrates in the hardness improving coating. If the people such as J.Musil are at 573K, prepare Al-Cu-N coating when direct current (DC) bias is-100V, worked as PN2When being less than 0.09Pa, coating is by Al2Cu with AlN phase is formed, and when P is increased to 0.12Pa or higher, formation be amorphous coating, coating hardness reduces.
By document being done further retrieval and analysis, also do not find that wear rate is lower than 4.0 �� 10-16m3The Al-Cu-N abrasion-resistant hardcoat of/Nm nano composite structure.
Application publication number is V-Al-N hard coat and its preparation method that the Chinese invention patent application of CN102534493A discloses a kind of nano composite structure, wherein, the V-Al-N hard coat of nano composite structure comprises AlN phase and some the VN crystal grains continuously of crystalline structure, each VN crystal grain is wrapped up continuously mutually by the AlN of crystalline structure, VN crystal grain forms coherent interface continuously mutually with the AlN of crystalline structure, and its composition represents for (V1-xAlx) N, wherein, 1-x is 0.41��0.6, x is 0.4��0.59. This nano composite structure V-Al-N hard coat preparation: adopt magnetron sputtering technique, by DC cathode splash-proofing sputtering metal V, intermediate frequency negative electrode sputters Al, and with N in vacuum chamber2Solid/liquid/gas reactions generates the V-Al-N hard coat of nano composite structure. But the hardness of the V-Al-N hard coat of this nano composite structure and frictional behaviour need to improve further.
Summary of the invention
In order to overcome the deficiency that prior art exists, the present invention provides a kind of Al-Cu-N abrasion-resistant hardcoat, and wear resistance is good.
A kind of Al-Cu-N abrasion-resistant hardcoat, is made up of with Cu crystal mutually AlN crystal phase, and wherein, Cu crystal is dispersed in AlN crystal mutually, and the interface between Cu crystal phase and AlN crystal phase is bonded with Cu-Al key;
In described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N74.6%��89%;
Cu11%��25.4%;
Wherein, the atomic ratio of Al and N is 0.9��1:1.
When the atomic percentage conc of Cu is lower than 11%, in coating, Cu exists with non-crystalline state, in use, owing to crystallisation procedure can occur the amorphous Cu of rising of temperature, therefore, affect the stable of coating, the wear resisting property of Al-Cu-N abrasion-resistant hardcoat is not good, and when the atomic percentage conc of Cu is higher than 25.4%, the hardness of coating significantly reduces, affect the abrasion resistance properties of coating, when the atomic percentage conc of Cu is 11.0%��25.4%, the atomic ratio of Al and N is 0.9��1:1, and Al-Cu-N abrasion-resistant hardcoat of the present invention has high-wearing feature.
As preferably, in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N80%��89%;
Cu11%��20%.
The atomic percentage conc of Cu controls 11%��20%, the Al-Cu-N abrasion-resistant hardcoat formed under this atomic percentage conc, and its defective reduces, and reduces the internal stress of Al-Cu-N abrasion-resistant hardcoat, it is to increase the hardness of Al-Cu-N abrasion-resistant hardcoat.
Further preferably, in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N82.1%��85.3%;
Cu14.7%��17.9%;
Wherein, the atomic ratio of Al and N is 1:1.
Al-Cu-N abrasion-resistant hardcoat according to embodiment 2,3,6,7,12 preparation is it will be seen that the Al-Cu-N abrasion-resistant hardcoat under this condition has very excellent abrasion resistance properties, and has good hardness.
More a step is preferred, and in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al41.15%;
N41.15%;
Cu17.7%��
The Al-Cu-N abrasion-resistant hardcoat prepared according to embodiment 7 is it will be seen that the wear rate of Al-Cu-N abrasion-resistant hardcoat under this condition is 1.2 �� 10-16m3/ Nm, has abrasion resistance properties the most excellent, and can keep good hardness, and its hardness is close to 30GPa, and this hardness has been enough to meet user demand such that it is able to greatly extend the work-ing life of mould, mechanical component etc.
In Al-Cu-N abrasion-resistant hardcoat of the present invention, Cu and N not easily occurs reaction to generate nitride, AlN and Cu is formed with the hard phase/soft matter phase nano composite structure of Cu-Al key bonding after certain interaction occurs at two-phase interface place, it is to increase the hardness of Al-Cu-N abrasion-resistant hardcoat of the present invention and wear resistance. As preferably, the diffraction surfaces of described AlN crystal phase is 0002, also (0002) face is claimed, the diffraction surfaces of described Cu crystal phase is 111, also (111) face is claimed, interface between the Cu crystal phase of above-mentioned crystalline state and AlN crystal phase, with Cu-Al key bonding, forms more stable hard phase/soft matter phase nano composite structure, it is possible to improve hardness and the wear resistance of Al-Cu-N abrasion-resistant hardcoat of the present invention better.
As preferably, the particle diameter of described Cu crystal phase is 1��10nm, the Cu crystal of this particle diameter can be dispersed in better mutually AlN crystal mutually in, Cu crystal phase can form stable interface with AlN crystal phase, thus can further improve hardness and the wear resistance of Al-Cu-N abrasion-resistant hardcoat of the present invention.
Al-Cu-N abrasion-resistant hardcoat of the present invention, has the growth structure without column crystal densification, and its surfaceness, lower than 6.1nm, substantially increases the abrasion resistance properties of Al-Cu-N abrasion-resistant hardcoat of the present invention.
Present invention also offers the preparation method of a kind of Al-Cu-N abrasion-resistant hardcoat, adopt reaction magnetocontrol sputtering method, workable, controllability is good, is easy to suitability for industrialized production.
A preparation method for Al-Cu-N abrasion-resistant hardcoat, comprises the following steps:
Al target is arranged on intermediate frequency negative electrode, Cu target is arranged on DC cathode, matrix is arranged on anode, the temperature of matrix is 200 DEG C��400 DEG C, lead to into nitrogen, adopt the method for two target reaction magnetocontrol sputtering, by the dividing potential drop of adjustment nitrogen, the power density of Al target and the power density of Cu target, matrix is carried out sputtering sedimentation, obtains Al-Cu-N abrasion-resistant hardcoat.
In the present invention, two target reaction magnetocontrol sputtering adopts Al target and Cu target sputter simultaneously, ensure that the homogeneity of composition in the rete of preparation, avoid the problem that in machinery combination target, composition is wayward. In addition, Cu not easily reacts with N, and thus the final coating formed is the nano-composite coating that AlN phase is formed with Cu phase.
As preferably, the dividing potential drop of described nitrogen is 0.2Pa��0.5Pa, the power density of described Al target is 4.5��5.5W/cm2, the power density of described Cu target is 0.1��0.5W/cm2The power density of the power density of the dividing potential drop of nitrogen, Al target and Cu target is controlled in above-mentioned scope, the elementary composition Al-Cu-N abrasion-resistant hardcoat of specific atoms percentage composition can be obtained, and Al-Cu-N abrasion-resistant hardcoat is made up of with Cu crystal mutually AlN crystal phase, Cu crystal is dispersed in AlN crystal mutually, interface between Cu crystal phase and AlN crystal phase is with Cu-Al key bonding, and the Al-Cu-N abrasion-resistant hardcoat of above-mentioned preparation has excellent abrasion resistance properties and good hardness.
As preferably, intermediate frequency negative electrode applies the intermediate frequency bias voltage of-50V��-90V, suitably apply bias voltage, prepared Al-Cu-N abrasion-resistant hardcoat structure can be impelled more fine and close, there is the growth structure without column crystal densification, greatly improve the wear resistance of Al-Cu-N abrasion-resistant hardcoat of the present invention.
Compared with prior art, tool of the present invention has the following advantages:
One, Al-Cu-N abrasion-resistant hardcoat of the present invention, AlN crystal phase and Cu crystal are formed with the hard phase/soft matter phase nano composite structure of Cu-Al key bonding after certain interaction occurs at two-phase interface place, substantially increase hardness and the wear resistance of Al-Cu-N abrasion-resistant hardcoat of the present invention.Al-Cu-N abrasion-resistant hardcoat of the present invention is the growth structure without column crystal densification, and Coating Surface Roughness is little, and the hardness of rete and wear resisting property are good.
Two, the ratio H/E* of hardness and modulus can as the index weighing material wear-resistant performance, high H/E* ratio correspond to low wear rate, but it is not that H/E* ratio its wear rate more high is more low, when the H/E* ratio of Al-Cu-N abrasion-resistant hardcoat of the present invention is close to 0.1, can obtaining excellent abrasion resistance properties, its wear rate is 4.0 �� 10-16m3/ below Nm. In addition, also being considered and the mating (such as rapid steel) of matrix modulus in actual application, namely the modulus of coating will with matrix modulus close to just be of practical significance. Can by improving hardness H, the method reducing E* improves H/E*, but high rigidity often correspond to high-modulus, accordingly, it is desirable to while modulus reduces, hardness still remains in a higher scope, and the H/E* value of Al-Cu-N abrasion-resistant hardcoat of the present invention wants high relative to not adding coating lower than 11.0% of the coating of Cu and Cu atomic percentage conc, its value is about 0.1, and therefore, Al-Cu-N abrasion-resistant hardcoat of the present invention demonstrates excellent abrasion resistance properties.
Three, relative to prior art, Al-Cu-N abrasion-resistant hardcoat of the present invention has excellent abrasion resistance properties, and wear rate is lower than 4.0 �� 10-16m3/ Nm, reaches the requirement of high-wearing feature, can extensively for the field such as surfacecti proteon of mould, mechanical component, other frictional wear.
Four, the preparation method of Al-Cu-N abrasion-resistant hardcoat of the present invention, adopts reaction magnetocontrol sputtering method, and it is workable, controllability good, be easy to suitability for industrialized production, has broad application prospects and good economic benefit.
Accompanying drawing explanation
Fig. 1 is the structural representation of Al-Cu-N abrasion-resistant hardcoat of the present invention;
Fig. 2 is the coating of comparative example 1 and comparative example 2 preparation and X-ray diffraction (XRD) figure of the Al-Cu-N abrasion-resistant hardcoat of embodiment 5, embodiment 6, embodiment 7 and embodiment 9 preparation;
In Fig. 3, scanning electronic microscope (SEM) sectional view of the coating that (a) is prepared for comparative example 1 in Fig. 3, scanning electronic microscope (SEM) sectional view of the Al-Cu-N abrasion-resistant hardcoat that (b) is prepared for embodiment 7 in Fig. 3;
In Fig. 4, x-ray photoelectron power spectrum (XPS) figure that Fig. 4 (a) is pure Cu, x-ray photoelectron power spectrum (XPS) figure of the Al-Cu-N abrasion-resistant hardcoat that Fig. 4 (b) is prepared for embodiment 7.
Embodiment
Comparative example 1��2 and embodiment 1��13
First matrix (M42 rapid steel 15mm �� 16mm �� 3mm) is cleaned, the model that matrix is first put into the production of Borer company is washing composition ultrasonic cleaning 3 minutes at the temperature of 60 DEG C of HT1401, then the model putting into the production of Borer company is washing composition ultrasonic cleaning 3 minutes at the temperature of 50 DEG C of HT1233,0.5 minute is cleaned again the deionized water for ultrasonic of 45 DEG C, the vacuum drying oven finally matrix after cleaning being put into 95 DEG C toasts 3 minutes, puts on the rotatable base frame of vacuum chamber after oven dry.
Al target is arranged on intermediate frequency negative electrode, and apply the intermediate frequency bias voltage of-50V��-90V, Cu target is arranged on DC cathode, M42 matrix is arranged in sample table and is connected with anode, sample table temperature is 200 DEG C��400 DEG C, namely it is 200 DEG C��400 DEG C by the temperature of matrix after thermal conduction, leads to into nitrogen, regulate N2Dividing potential drop be 0.2Pa��0.5Pa, adopt the method for two target reaction magnetocontrol sputtering, by regulating the Sputtering power density of Al target and Cu, regulate the content of Cu in coating, matrix is deposited, obtains Al-Cu-N abrasion-resistant hardcoat.The Sputtering power density of Al target is 4.5��5.5W/cm2, the Sputtering power density of Cu target is 0.1��0.5W/cm2��
In the method for two target reaction magnetocontrol sputtering, the experiment parameter of comparative example 1��2 and embodiment 1��13 is as shown in table 1, and wherein, Cu content is Cu atomic percentage conc, and the atomic percentage conc of Al and N is 100%-Cu atomic percentage conc.
Table 1
Adopt structural parameter and the physicals of the coating in following experimental technique assessment comparative example and embodiment.
The composition of coating
Adopting EDS to measure the composition of each film system, its configuration EDAXSi (Li) probe, is calibrated by ZAF, and the selected area of each sample is not less than 4000 ��m2Region, measures the mean value of its composition.
The crystalline structure of coating
Adopting Germany's BrukerD8Advance diffractometer, utilize CuK alpha-ray incident, X-ray tube controls at 40KV and 40mA, measures the crystalline structure of each film system, utilizes nickel filtering device to filter out K��Ray, arranging detection angle is 20 �㡫80 ��.
The measurement of hardness and modulus
The model adopting American MTS to produce is hardness and the Young's modulus that NANOG200 nano-hardness tester measures each film system, it configures tetrahedron Berkvich pressure head, by the setting press-in degree of depth (80��100nm), load changes with the press-in degree of depth, and each sample is averaged after measuring 6 matrix points.
Chemical state
Adopting the AxisULTRADLDX X-ray photoelectron spectroscopy X (XPS) of Kratos company to analyze the internal chemical environment of coating, wherein light source is monochromatic AlKa (1486.6eV), and when work, in chamber, air pressure is better than 5 �� 10-9Torr��
Wear rate
Frictional wear experiment adopts CETRUMT-3 frictional wear instrument, and temperature is room temperature (25 DEG C), and relative humidity is 50 �� 5%, and antithesis ball is the WC-Co ball of 6.0mm, and loading force is 2N, planing speed 0.05m/s, slides distance 1000m.
The structural representation of Al-Cu-N abrasion-resistant hardcoat of the present invention, as shown in Figure 1, Al-Cu-N abrasion-resistant hardcoat is made up of with Cu crystal mutually AlN crystal phase, wherein, Cu crystal is dispersed in AlN crystal mutually, and the interface between Cu crystal phase and AlN crystal is bonded with Cu-Al key.
X-ray diffraction (XRD) figure of coating prepared by comparative example 1 and comparative example 2 and Al-Cu-N abrasion-resistant hardcoat prepared by embodiment 5, embodiment 6, embodiment 7 and embodiment 9, as shown in Figure 2, when the content of Cu is 0, namely, in comparative example 1, coating is mainly diffraction surfaces for the AlN in (0002) face and (10-11) face; When the atomic percentage conc of Cu is 7.3%, namely in comparative example 2, AlN(10-11 in coating) peak disappear, and XRD does not have the peak of Cu, this illustrate Cu be non-crystal structure, this coating in use, owing to crystallisation procedure can occur the amorphous Cu of rising of temperature, therefore, the stability of coating can be affected. And in the XRD figure of the Al-Cu-N abrasion-resistant hardcoat of embodiments of the invention 5,6,7,9 preparation, Al-Cu-N abrasion-resistant hardcoat only exists Cu(111) peak and AlN(0002) peak, illustrate that Al-Cu-N abrasion-resistant hardcoat is made up of with the AlN phase of crystalline state the Cu phase of crystalline state.
Fig. 3 is the coating of comparative example 1 preparation and scanning electronic microscope (SEM) sectional view of the Al-Cu-N abrasion-resistant hardcoat of embodiment 7 preparation, wherein, scanning electronic microscope (SEM) sectional view of the coating that (a) is prepared for comparative example 1 in Fig. 3, scanning electronic microscope (SEM) sectional view of the Al-Cu-N abrasion-resistant hardcoat that (b) is prepared for embodiment 7 in Fig. 3, as shown in Figure 3, in Fig. 3 (a), when the content of Cu is 0, namely in comparative example 1, coating is the columnar crystal structure of short texture, its hardness and wear resisting property are very low, in Fig. 3 (b), Al-Cu-N abrasion-resistant hardcoat of the present invention is the growth structure without column crystal densification, and surfaceness is little, hardness and the wear resisting property of Al-Cu-N abrasion-resistant hardcoat of the present invention are good.
In Fig. 4, x-ray photoelectron power spectrum (XPS) figure that Fig. 4 (a) is pure Cu, x-ray photoelectron power spectrum (XPS) figure of the Al-Cu-N abrasion-resistant hardcoat that Fig. 4 (b) is prepared for embodiment 7. As shown in Figure 4, there is Cu-Al key in Al-Cu-N abrasion-resistant hardcoat prepared by embodiment 7, this illustrates that AlN and Cu two-phase exists chemical action in interface, and namely interface between Cu crystal phase and AlN crystal is bonded with Cu-Al key.
By electron scanning micrograph it will be seen that in the Al-Cu-N abrasion-resistant hardcoat of embodiment 1��13 preparation, the particle diameter of Cu crystal phase is 1��10nm.
The part-structure parameter of coating prepared by the Al-Cu-N abrasion-resistant hardcoat of the embodiment of the present invention 1��13 and comparative example 1,2 and physicals are as shown in table 2.
Table 2
As known from Table 2, Al-Cu-N abrasion-resistant hardcoat of the present invention, its hardness is far above the coating (comparative example 1) not adding Cu, H/E* value is basic close to 0.1, and what this H/E* value was corresponding is low wear rate and low roughness, such as embodiment 7, when the content of Cu is 17.7%, its hardness is 0.11 close to 30GPa, H/E* value, and wear rate and roughness only have 1.2 �� 10- 16m3/ Nm and 3.4nm, has very excellent abrasion resistance properties.
Claims (9)
1. an Al-Cu-N abrasion-resistant hardcoat, it is characterised in that, be made up of mutually with Cu crystal AlN crystal phase, wherein, Cu crystal be dispersed in mutually AlN crystal mutually in, Cu crystal phase and AlN crystal mutually between interface be bonded with Cu-Al key;
In described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N74.6%��89%;
Cu11%��25.4%;
Wherein, the atomic ratio of Al and N is 0.9��1:1.
2. Al-Cu-N abrasion-resistant hardcoat according to claim 1, it is characterised in that, in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N80%��89%;
Cu11%��20%.
3. Al-Cu-N abrasion-resistant hardcoat according to claim 2, it is characterised in that, in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al and N82.1%��85.3%;
Cu14.7%��17.9%;
Wherein, the atomic ratio of Al and N is 1:1.
4. Al-Cu-N abrasion-resistant hardcoat according to claim 3, it is characterised in that, in described Al-Cu-N abrasion-resistant hardcoat, the atomic percentage conc of each element is as follows:
Al41.15%;
N41.15%;
Cu17.7%.
5. Al-Cu-N abrasion-resistant hardcoat according to the arbitrary item of Claims 1 to 4, it is characterised in that, the diffraction surfaces of described AlN crystal phase is 0002, and the diffraction surfaces of described Cu crystal phase is 111.
6. Al-Cu-N abrasion-resistant hardcoat according to the arbitrary item of Claims 1 to 4, it is characterised in that, the particle diameter of described Cu crystal phase is 1��10nm.
7. the preparation method of Al-Cu-N abrasion-resistant hardcoat according to the arbitrary item of claim 1��6, it is characterised in that, comprise the following steps:
Al target is arranged on intermediate frequency negative electrode, Cu target is arranged on DC cathode, matrix is arranged on anode, the temperature of matrix is 200 DEG C��400 DEG C, lead to into nitrogen, adopt the method for two target reaction magnetocontrol sputtering, by the dividing potential drop of adjustment nitrogen, the power density of Al target and the power density of Cu target, matrix is carried out sputtering sedimentation, obtains Al-Cu-N abrasion-resistant hardcoat.
8. the preparation method of Al-Cu-N abrasion-resistant hardcoat according to claim 7, it is characterised in that, the dividing potential drop of described nitrogen is 0.2Pa��0.5Pa, and the power density of described Al target is 4.5��5.5W/cm2, the power density of described Cu target is 0.1��0.5W/cm2��
9. the preparation method of Al-Cu-N abrasion-resistant hardcoat according to claim 7, it is characterised in that, intermediate frequency negative electrode applies the intermediate frequency bias voltage of-50V��-90V.
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| CN101660160A (en) * | 2009-09-14 | 2010-03-03 | 南昌航空大学 | Nitride compound protective coating with high hardness and high thermal shock stability |
| TW201226601A (en) * | 2010-12-20 | 2012-07-01 | Hon Hai Prec Ind Co Ltd | Housing and method for making the same |
| CN102534493A (en) * | 2012-01-13 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | V-Al-N hard coating with nano composite structure and preparation method thereof |
| CN102560355A (en) * | 2012-01-11 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | V-Si-N nanometer composite hard coating and preparation method thereof |
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| CN101660160A (en) * | 2009-09-14 | 2010-03-03 | 南昌航空大学 | Nitride compound protective coating with high hardness and high thermal shock stability |
| TW201226601A (en) * | 2010-12-20 | 2012-07-01 | Hon Hai Prec Ind Co Ltd | Housing and method for making the same |
| CN102560355A (en) * | 2012-01-11 | 2012-07-11 | 中国科学院宁波材料技术与工程研究所 | V-Si-N nanometer composite hard coating and preparation method thereof |
| CN102534493A (en) * | 2012-01-13 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | V-Al-N hard coating with nano composite structure and preparation method thereof |
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| Hard and superhard nanocomposite Al-Cu-N films prepared by magnetron sputtering;J.Musil et al.;《Surface and Coatings Technology》;20011231;第142-144卷;第603-609页 * |
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