CN102605324B - Multi-arc ion plating superlattice nanometer composite coating and preparation method of multi-arc ion plating superlattice nanometer composite coating - Google Patents
Multi-arc ion plating superlattice nanometer composite coating and preparation method of multi-arc ion plating superlattice nanometer composite coating Download PDFInfo
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Abstract
The invention discloses a multi-arc ion plating superlattice nanometer composite coating and a preparation method of the multi-arc ion plating superlattice nanometer composite coating. A TiN layer in a cubic structure and an AlSiN layer in an orthohexagonal structure of the costing disclosed by the invention are alternately deposited on a nanometer transition layer, the nanometer transition layer is a Ti/TiN compound layer, and an AlSiN layer in the cubic structure is arranged on an interface of the AlSiN layer in the orthohexagonal structure. According to the preparation method, polished and cleaned workpieces are clamped on a clamp, the clamp is arranged on a turntable, the turntable is positioned in a vacuum chamber, Ar gas is introduced into the vacuum chamber, negative bias pressure is added for carrying out Ar ion bombardment cleaning on the surfaces of the workpeices, residues on the surfaces of the workpieces are removed, the negative bias pressure is reduced, a first medium frequency electric arc source is started, a Ti layer is generated through deposition, then, N2 gas is introduced, a TiN layer is generated through deposition, a second medium frequency electric arc source is started, N2 gas is introduced, the TiN layer in the cubic structure and the AlSiN layer in the orthohexagonal structure are alternately deposited and formed, and the coating is cooled to the room temperature in the vacuum chamber.
Description
Technical field
What the present invention relates to is a kind of precision die and high speed cutting tool surfaces plated film strengthening treatment process, in particular a kind of multi-arc ion coating superlattice nano-composite coating and preparation method thereof.
Background technology
The magnesium-yttrium-transition metal nitride coatings is because having higher hardness and wear resistance preferably, and it is material modified to be widely used as die surface.The gained coating must have following feature: good bonding force, enough thickness, suitable mechanical property (hardness and intensity), heat resistanceheat resistant disturbance performance and high-temperature stability.The titanium nitride base film is because its higher hardness and advantage such as wear resistance have preferably obtained application widely at mould and cutting tool.
Along with developing rapidly of processing manufacturing industry, mould has been proposed more and more higher requirement, also provide huge power for its development.In recent years, die industry structural adjustment paces are accelerated, mainly showing as large-scale, accurate, complicated, long lifetime mould standard spare, mould standard spare tempo, to be higher than overall development speed, especially IT, automobile, the hi-tech industry of industry more and more higher to the requirement of precision die.The method of precision die surface modification mainly contains nitriding, carburizing and hardening film deposition at present, wherein lower, the abrasion resistance performance deficiency of the surface reforming layer hardness that forms of carburizing and nitridation technique, high temperature resistant property are relatively poor, far can not reach the requirement that improves the precision die life-span.The hard coat of hardening film deposition technique preparation can satisfy high rigidity, good resistance to wearing and high temperature resistant property, become the most promising precision die process for modifying surface it
TiN has been widely used in mould and cutting tool industry as prevailing hard coat, but the TiN coating is because lower wear resistance, relatively poor antioxidant property and low hot red hardness shortcomings such as (500 ℃ of its hardness just begin rapid decline) have limited its further application on precision die and high speed cutting instrument.In recent years, constantly be devoted to high-performance coating and strengthen further exploitation and the application of precision die and high speed cutting instrument, as on TiN base coating basis, add B, Si, Cr, W, etc. element form Ti-B-N, Ti-Cr-N, Ti-Si-N, Ti-Al-Si-N, ternary or quaternary coatings such as Ti-Si-C-N, Ti-W-Al-N.
In nineteen ninety-five, people such as Germany scientist Stan Veprek have proposed the design concept of new super hard nano composite membrane, namely by the superstructure that forms less than the nanocrystalline of 15nm or amorphous two-phase material layer alternating growth, and, the modulation period of this structure be evenly, fixing.Experimental study shows: the fine structure multilayer film by the two-phase metaboly formation of deposits of nanoscale has the unusual superhard property effect that increases of hardness; In addition, this special structure also has good effect to improving the coating tribological property.But this coating is owing to have higher internal stress and the adding of Si3N4 mutually of crisp matter, reduced film toughness and and high base strength, limited its application on precision die.Nanometer multilayerization (superlattice) and aftertreatment (thermal treatment) are the important means of improving superhard thin film toughness.On the one hand, the nanometer multilayerization of superhard thin film mainly is magnetron sputtering technique at present, but the deposition techniques inefficiency of this preparation film is difficult to large-scale industrial production; On the other hand, though vacuum annealing can reduce the internal stress in the superhard thin film, along with the rising of temperature, when especially surpassing more than 1000 ℃, mechanical property reduces.
In general, although at present more to the research of nitrogenize ti-based coating, utilize multi-arc ion coating to obtain ultrahigh hardness, high heat stability performance and the basic nano-composite coating precision die of TiN with excellent toughness does not appear in the newspapers.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of multi-arc ion coating superlattice nano-composite coating and preparation method thereof is provided, make polycrystalline lattice titanium nitride base nano-composite coating be able to industrial applications at precision die and high speed cutting instrument.
The present invention is achieved by the following technical solutions, the present invention includes the TiN layer of nanometer transition layer, cubic structure and the AlSiN layer of hexagonal structure, the AlSiN layer alternating deposit of the TiN layer of described cubic structure and hexagonal structure is on the nanometer transition layer, described nanometer transition layer is the composite layer of Ti/TiN, and the interface of the AlSiN layer of described hexagonal structure is provided with the AlSiN layer of cubic structure.
Be 7～9nm the modulation period of the TiN layer of described cubic structure and the AlSiN layer of hexagonal structure.
The total thickness of described nano-composite coating is 4～6 μ m, and the thickness of nanometer transition layer is 1～2 μ m.
The Si that contains crystallization in the described nano-composite coating
3N
4Phase.
A kind of preparation method of multi-arc ion coating superlattice nano-composite coating may further comprise the steps:
(1) the first intermediate frequency arc source and the second intermediate frequency arc source, N are set respectively in the both sides of vacuum chamber
2Insert in the vacuum chamber with Ar gas;
(2) piece-holder after will polishing, cleaning is on anchor clamps, and anchor clamps are arranged on the turntable, and turntable is arranged in vacuum chamber;
(3) feed Ar gas in the vacuum chamber, add negative bias workpiece surface is carried out reducing negative bias after the Ar icon bombardment cleaning removes the workpiece surface resistates;
(4) start the first intermediate frequency arc source, deposition generates the Ti layer, feeds N then
2Gas, deposition generates the TiN layer;
(5) start the second intermediate frequency arc source, at first depositing Al SiN layer rotates sample then, makes being exposed between two intermediate frequency arc sources of sample gap, and alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and the vacuum chamber cool to room temperature gets final product.
Be to improve coating performance, comprise that also step (6) anneals to post-depositional nano-composite coating, annealing temperature is 700～1200 ℃.
In the described step (1), the target of the first intermediate frequency arc source is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%.
In the described step (2), the vacuum tightness of vacuum chamber is 7 * 10
-3Pa, Heating temperature is 300～500 ℃, workpiece rotational frequency is 3～5 commentaries on classics/min.
In the described step (4), the depositing time of Ti layer is 10～20min, and the depositing time of TiN layer is 40～60min.
The depositing time of the TiN layer of described cubic structure and the AlSiN layer of hexagonal structure is 40～90min.
The present invention has the following advantages compared to existing technology: the present invention has realized the TiN of nanocrystalline cube mechanism and the uniform alternating growth of AlSiN of hexagonal structure, has formed the superstructure with accurate modulation period; There is the cubic structure AlSiN of one deck small thickness in place, six side AlSiN bed interfaces, causes cube TiN layer and the even alternating growth of six side AlSiN layers, and its hardness is up to 52GPa; In vacuum annealing process, the AlSiN phase decomposition of hexagonal structure becomes the Si of crystallization
3N
4Phase, coherence epitaxy under the template action of cube TiN has compensated the hardness that the appearance owing to six side AlN causes and has descended, and in addition, the AlSiN of cubic structure can suppress the generation of six side AlN; Simultaneously, after this superlattice nano composite material annealing, bonding strength increases substantially.This superstructure has hardness and the thermal stability of superelevation, therefore enlarged TiN base hard films through engineering approaches range of application, for the exploitation that utilizes multi-arc ion coating to prepare similar high-end product provides new method, and has good application prospects at precision die and high speed cutting instrument.
Description of drawings
Fig. 1 is the structural representation of vacuum chamber of the present invention;
Fig. 2 is process flow sheet of the present invention;
Fig. 3 is the transmission photo of TiN transition layer on the TiN/AlSiN film;
Fig. 4 is the photo of the diffraction pattern in TiN/AlSiN layer region transverse section;
Fig. 5 is the transverse section transmission view of the TiN/AlSiN superlattice nano-composite coating of deposition attitude;
Fig. 6 is the diffraction pattern in transverse section of the TiN/AlSiN superlattice nano-composite coating of deposition attitude;
Fig. 7 is the transverse section high resolution transmission view of the TiN/AlSiN superlattice nano-composite coating of deposition attitude;
Fig. 8 is the local diffraction pattern of (a) among Fig. 7;
Fig. 9 is the local diffraction pattern of (b) among Fig. 7;
Figure 10 is the energy spectrogram of deposition attitude Si;
Figure 11 is the energy spectrogram of the Si after the annealing;
Figure 12 is the XRD figure spectrum before and after the annealing of TiN/AlSiN superlattice Coatings in Vacuum;
Figure 13 is the dsc analysis synoptic diagram of TiN/AlSiN superlattice coating;
Figure 14 is that TiN/AlSiN superlattice coating hardness is with the variation synoptic diagram of annealing temperature;
Figure 15 is that TiN/AlSiN superlattice anchoring strength of coating is with the variation synoptic diagram of annealing temperature;
Figure 16 is that the manufacturing of different surface treatment automobile component is with comparing synoptic diagram the work-ing life of precise punching die.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As depicted in figs. 1 and 2, the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating of present embodiment may further comprise the steps:
(1) the first intermediate frequency arc source 2 and the second intermediate frequency arc source 3, N are set respectively in the both sides of vacuum chamber 1
2Insert in the vacuum chamber 1 with Ar gas, the target of the first intermediate frequency arc source 2 is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%;
(2) workpiece after the polished finish is respectively cleaned 15min with acetone and alcohol ultrasonic wave successively, be clamped in after the oven dry on the anchor clamps 4, anchor clamps 4 are arranged on the turntable 5, and turntable 5 is arranged in vacuum chamber 1, and vacuum chamber 1 is vacuumized, and making its vacuum tightness is 7 * 10
-3Pa, Heating temperature is 400 ℃, and workpiece rotational frequency is 4 commentaries on classics/min, chooses monocrystalline silicon piece as workpiece, and workpiece is of a size of 20mm * 10mm * 0.5mm;
(3) in vacuum chamber 1, feed Ar gas, make that the pressure in the vacuum chamber 1 is 2Pa, add the workpiece surface of negative bias 1000V and carry out Ar icon bombardment cleaning 10min, behind removal workpiece surface resistates such as adsorptive and the oxide compound, reduce negative bias to 800V;
(4) start the first intermediate frequency arc source 2, deposition generates the Ti layer, and depositing time 10min feeds N then
2Gas, deposition generates the TiN layer, and depositing time is 40min;
(5) start the second intermediate frequency arc source 3, depositing Al SiN layer at first, revolving-turret 5 drives the sample rotation then, make being exposed between two intermediate frequency arc sources of sample gap, alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and depositing time is 40min, and vacuum chamber 1 cool to room temperature gets final product, open fire door then, take out workpiece;
(6) post-depositional nano-composite coating is carried out vacuum annealing, annealing temperature is 700 ℃.
Shown in Fig. 3～6, workpiece behind the present embodiment plated film detects to analyze through TEM and obtains, multi-arc ion coating superlattice nano-composite coating comprises the TiN layer 8 of nanometer transition layer 7, cubic structure and the AlSiN layer 9 of hexagonal structure, AlSiN layer 9 alternating deposit of the TiN layer 8 of described cubic structure and hexagonal structure are on nanometer transition layer 7, and described nanometer transition layer 7 is composite layers of Ti/TiN.The bed interface of the AlSiN layer 9 of hexagonal structure is provided with the AlSiN layer of cubic structure.The AlSiN layer of cubic structure plays a transition role between the AlSiN layer 9 of the TiN of cubic structure layer 8 and hexagonal structure, makes the TiN layer 8 of cubic structure and the AlSiN layer 9 of hexagonal structure replace the coherence growth.
Be 8nm the modulation period of the TiN layer 8 of the cubic structure of present embodiment and the AlSiN layer 9 of hexagonal structure.
The total thickness of nano-composite coating is 5 μ m, and the thickness of nanometer transition layer 7 is 1 μ m.
Shown in Fig. 7,8 and 9, the fast Fourier conversion FFT result show, the AlSiN layer that has the cubic structure of one deck small thickness on the bed interface of the AlSiN layer 9 of the hexagonal structure of present embodiment makes the AlSiN layer 9 coherence epitaxy of TiN layer 8 and hexagonal structure of cubic structure.
As shown in Figure 10 and Figure 11, after XPS spectrum detected analysis, Si2p key bound energy mainly comprised 101.6eV and 102.1eV in the superlattice nano-composite coating by the workpiece of plated film, and the key bound energy is the Si of the corresponding crystallization of 102.1eV
3N
4, the Si of crystallization
3N
4Annealing back content increases the Si of crystallization
3N
4Can under the effect of the TiN of cubic structure template, form the TiN/Si of coherence
3N
4, can compensate owing to the coating hardness decline that six side AlN cause mutually occurring.
As shown in figure 12, utilize the superlattice TiN/AlSiN of XRD to carry out the thermal stability analysis, still formed by TiN after the annealing of superlattice nano coating, occurred six sides' AlN phase in the time of 1100 ℃.
The preparation method of the superlattice nano-composite coating of present embodiment may further comprise the steps:
(1) the first intermediate frequency arc source 2 and the second intermediate frequency arc source 3, N are set respectively in the both sides of vacuum chamber 1
2Insert in the vacuum chamber 1 with Ar gas, the target of the first intermediate frequency arc source 2 is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%;
(2) workpiece after the polished finish is respectively cleaned 15min with acetone and alcohol ultrasonic wave successively, be clamped in after the oven dry on the anchor clamps 4, anchor clamps 4 are arranged on the turntable 5, and turntable 5 is arranged in vacuum chamber 1, and vacuum chamber 1 is vacuumized, and making its vacuum tightness is 7 * 10
-3Pa, Heating temperature is 300 ℃, and workpiece rotational frequency is 3 commentaries on classics/min, chooses monocrystalline silicon piece as workpiece, and workpiece is of a size of 20mm * 10mm * 0.5mm;
(3) in vacuum chamber 1, feed Ar gas, make that the pressure in the vacuum chamber 1 is 2Pa, add the workpiece surface of negative bias 900V and carry out Ar icon bombardment cleaning 10min, behind removal workpiece surface resistates such as adsorptive and the oxide compound, reduce negative bias to 700V;
(4) start the first intermediate frequency arc source 2, deposition generates the Ti layer, and depositing time 15min feeds N then
2Gas, deposition generates the TiN layer, and depositing time is 50min;
(5) start the second intermediate frequency arc source 3, depositing Al SiN layer at first, revolving-turret 5 drives the sample rotation then, make being exposed between two intermediate frequency arc sources of sample gap, alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and depositing time is 40min, and vacuum chamber 1 cool to room temperature gets final product, open fire door then, take out workpiece;
(6) post-depositional nano-composite coating is carried out vacuum annealing, annealing temperature is 900 ℃.
The total thickness of the nano-composite coating for preparing is 4 μ m, and the thickness of nanometer transition layer 7 is 2 μ m.
Other embodiments are identical with embodiment 1.
The preparation method of the superlattice nano-composite coating of present embodiment may further comprise the steps:
(1) the first intermediate frequency arc source 2 and the second intermediate frequency arc source 3, N are set respectively in the both sides of vacuum chamber 1
2Insert in the vacuum chamber 1 with Ar gas, the target of the first intermediate frequency arc source 2 is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%;
(2) workpiece after the polished finish is respectively cleaned 15min with acetone and alcohol ultrasonic wave successively, be clamped in after the oven dry on the anchor clamps 4, anchor clamps 4 are arranged on the turntable 5, and turntable 5 is arranged in vacuum chamber 1, and vacuum chamber 1 is vacuumized, and making its vacuum tightness is 7 * 10
-3Pa, Heating temperature is 500 ℃, and workpiece rotational frequency is 5 commentaries on classics/min, chooses monocrystalline silicon piece as workpiece, and workpiece is of a size of 20mm * 10mm * 0.5mm;
(3) in vacuum chamber 1, feed Ar gas, make that the pressure in the vacuum chamber 1 is 2Pa, add the workpiece surface of negative bias 1100V and carry out Ar icon bombardment cleaning 10min, behind removal workpiece surface resistates such as adsorptive and the oxide compound, reduce negative bias to 900V;
(4) start the first intermediate frequency arc source 2, deposition generates the Ti layer, and depositing time 20min feeds N then
2Gas, deposition generates the TiN layer, and depositing time is 60min;
(5) start the second intermediate frequency arc source 3, depositing Al SiN layer at first, revolving-turret 5 drives the sample rotation then, make being exposed between two intermediate frequency arc sources of sample gap, alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and depositing time is 40min, and vacuum chamber 1 cool to room temperature gets final product, open fire door then, take out workpiece;
(6) post-depositional nano-composite coating is carried out vacuum annealing, annealing temperature is 1100 ℃.
The total thickness of the nano-composite coating for preparing is 4 μ m, and the thickness of nanometer transition layer 7 is 1 μ m.
Other embodiments are identical with embodiment 1.
The preparation method of the superlattice nano-composite coating of present embodiment may further comprise the steps:
(1) the first intermediate frequency arc source 2 and the second intermediate frequency arc source 3, N are set respectively in the both sides of vacuum chamber 1
2Insert in the vacuum chamber 1 with Ar gas, the target of the first intermediate frequency arc source 2 is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%;
(2) workpiece after the polished finish is respectively cleaned 15min with acetone and alcohol ultrasonic wave successively, be clamped in after the oven dry on the anchor clamps 4, anchor clamps 4 are arranged on the turntable 5, and turntable 5 is arranged in vacuum chamber 1, and vacuum chamber 1 is vacuumized, and making its vacuum tightness is 7 * 10
-3Pa, Heating temperature is 300 ℃, and workpiece rotational frequency is 4 commentaries on classics/min, chooses monocrystalline silicon piece as workpiece, and workpiece is of a size of 20mm * 10mm * 0.5mm;
(3) in vacuum chamber 1, feed Ar gas, make that the pressure in the vacuum chamber 1 is 2Pa, add the workpiece surface of negative bias 1000V and carry out Ar icon bombardment cleaning 10min, behind removal workpiece surface resistates such as adsorptive and the oxide compound, reduce negative bias to 800V;
(4) start the first intermediate frequency arc source 2, deposition generates the Ti layer, and depositing time 20min feeds N then
2Gas, deposition generates the TiN layer, and depositing time is 60min;
(5) start the second intermediate frequency arc source 3, depositing Al SiN layer at first, revolving-turret 5 drives the sample rotation then, make being exposed between two intermediate frequency arc sources of sample gap, alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and depositing time is 40min, and vacuum chamber 1 cool to room temperature gets final product, open fire door then, take out workpiece;
(6) post-depositional nano-composite coating is carried out vacuum annealing, annealing temperature is 1200 ℃.
The total thickness of the nano-composite coating for preparing is 4 μ m, and the thickness of nanometer transition layer 7 is 1 μ m.
Other embodiments are identical with embodiment 1.
As shown in figure 13, comparative example 1～embodiment 4, utilize the behavior of the superlattice TiN/AlSiN of dsc DSC coating thermokinetics to analyze, the superlattice nano coating exothermic peak occurs in 850 ℃～1030 ℃ scopes, curve among the figure between 1 and 2, six corresponding side AlSiN decompose, and form the Si of crystallization
3N
4AlN with six sides.
As shown in figure 14, comparative example 1～embodiment 4, with the nano impress method hardness before and after the annealing of superlattice nano-composite coating is analyzed, maximum load is 650mN, the hardness value of the superlattice coating of deposition attitude is 52GPa, and the hardness value of superlattice nano-composite coating is 47GPa after through 1100 ℃ of vacuum annealings.
As shown in figure 15, comparative example 1～embodiment 4, with scratch method the bonding strength before and after the annealing of superlattice coating is analyzed, after the annealing, the superlattice Bond Strength of Coating significantly improves, in the time of 900 ℃, the Lc2 value of characterizing coating bonding strength (second critical load, corresponding load when namely coating and matrix take place to peel off in a large number) reaches 44N.
As shown in figure 16, compare traditional nitriding processing and TiN coating and handle automobile component manufacturing press tool, the automobile component manufacturing that superlattice TiN/AlSiN multi-player super-hard nano film in the present embodiment is handled is with increasing considerably the work-ing life of press tool, this mainly is because the press tool that present embodiment is handled has excellent high-temperature stability and comprehensive mechanical property, and especially the high temperature of ultrahigh hardness keeps and the realization of bonding force by force.
Claims (9)
1. multi-arc ion coating superlattice nano-composite coating, it is characterized in that, comprise the TiN layer of nanometer transition layer, cubic structure and the AlSiN layer of hexagonal structure, the AlSiN layer alternating deposit of the TiN layer of described cubic structure and hexagonal structure is on the nanometer transition layer, described nanometer transition layer is the composite layer of Ti/TiN, and the interface of the AlSiN layer of described hexagonal structure is provided with the AlSiN layer of cubic structure; The Si that contains crystallization in the described nano-composite coating
3N
4Phase.
2. a kind of multi-arc ion coating superlattice nano-composite coating according to claim 1, it is characterized in that: be 7～9nm the modulation period of the TiN layer of described cubic structure and the AlSiN layer of hexagonal structure.
3. a kind of multi-arc ion coating superlattice nano-composite coating according to claim 1, it is characterized in that: the total thickness of described nano-composite coating is 4～6 μ m, the thickness of nanometer transition layer is 1～2 μ m.
4. according to the preparation method of each described a kind of multi-arc ion coating superlattice nano-composite coating in the claim 1～3, it is characterized in that, may further comprise the steps:
(1) the first intermediate frequency arc source and the second intermediate frequency arc source, N are set respectively in the both sides of vacuum chamber
2Insert in the vacuum chamber with Ar gas;
(2) piece-holder after will polishing, cleaning is on anchor clamps, and anchor clamps are arranged on the turntable, and turntable is arranged in vacuum chamber;
(3) feed Ar gas in the vacuum chamber, add negative bias workpiece surface is carried out reducing negative bias after the Ar icon bombardment cleaning removes the workpiece surface resistates;
(4) start the first intermediate frequency arc source, deposition generates the Ti layer, feeds N then
2Gas, deposition generates the TiN layer;
(5) start the second intermediate frequency arc source, at first depositing Al SiN layer rotates sample then, makes being exposed between two intermediate frequency arc sources of sample gap, alternating deposit generates the TiN layer of cubic structure and the AlSiN layer of hexagonal structure, and the vacuum chamber cool to room temperature gets final product.
5. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 4 is characterized in that, comprises that also step (6) anneals to post-depositional nano-composite coating, and annealing temperature is 700～1200 ℃.
6. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 4 is characterized in that, in the described step (1), the target of the first intermediate frequency arc source is made by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source is made by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%.
7. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 4 is characterized in that, in the described step (2), the vacuum tightness of vacuum chamber is 7 * 10
-3Pa, Heating temperature is 300～500 ℃, workpiece rotational frequency is 3～5 commentaries on classics/min.
8. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 4 is characterized in that, in the described step (4), the depositing time of Ti layer is 10～20min, and the depositing time of TiN layer is 40～60min.
9. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 4 is characterized in that, the depositing time of the TiN layer of described cubic structure and the AlSiN layer of hexagonal structure is 40～90min.
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| CN103952671B (en) * | 2014-04-29 | 2016-03-23 | 安徽多晶涂层科技有限公司 | A kind of FM electromagnetic coil that adopts prepares multi-arc ion coating hard coat and method |
| CN104073770B (en) * | 2014-06-23 | 2016-10-19 | 江苏科技大学 | TiWAlN ganoine thin film and preparation method |
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| CN105971617B (en) * | 2016-05-12 | 2018-08-31 | 西安热工研究院有限公司 | A kind of plural layers and preparation method thereof of tunnel piercing rounding machine cutter cutter ring |
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| CN108866491A (en) * | 2018-07-24 | 2018-11-23 | 山东大学 | TiAlN/CrAlSiN nanocomposite laminated coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202037930U (en) * | 2011-04-06 | 2011-11-16 | 武汉大学苏州研究院 | Cutter with nanometer multi-layer superhard composite coating |
Non-Patent Citations (2)
| Title |
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| "刀具表面超晶格TiN/AlN纳米多层膜的制备及性能的研究";潘应君等;《热加工工艺》;20051130(第11期);第23-25页 * |
| 潘应君等."刀具表面超晶格TiN/AlN纳米多层膜的制备及性能的研究".《热加工工艺》.2005,(第11期),第23-25页. |
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