CN102605324A - 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 of 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 characteristic: 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 advantages such as its higher hardness and wear resistance have preferably obtained application widely on mould and cutting tool.
Along with developing rapidly of processing manufacturing industry, mould has been proposed increasingly high requirement, also huge power is provided for its development.In recent years; Die industry structural adjustment paces are accelerated; Mainly show as overall development speed, especially IT that large-scale, accurate, complicated, long lifetime mould standard spare, mould standard spare tempo be higher than industry, automobile, hi-tech industry to precision die require increasingly high.The method of precision die surface-treated mainly contains nitriding, carburizing and hardening film deposition at present; Wherein the surface reforming layer hardness of carburizing and nitridation technique formation is lower, the abrasion resistance performance not enough, high temperature resistant property is 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 firmness, 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 the 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 ternary or quaternary coatings such as Ti-B-N, Ti-Cr-N, Ti-Si-N, Ti-Al-Si-N, 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 package; Promptly by the superstructure that forms less than the nanocrystalline or amorphous two phase material layer alternating growths of 15nm, and, the modulation period of this structure be evenly, fixed.Experimental study shows: the fine structure multilayer film by two phase metaboly formation of deposits of nanoscale has the unusual superhard property effect that increases of hardness; In addition, this particular structural 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 to improve superhard thin film flexible important means.On the one hand, the nanometer multilayerization of superhard thin film mainly is a 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, 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 to the research of nitrogenize ti-based coating.
Summary of the invention
The objective of the invention is to overcome the deficiency of 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 on precision die and high speed cutting instrument, be able to industrial applications.
The present invention realizes through following technical scheme; 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 said cubic structure and hexagonal structure is on the nanometer transition layer; Said nanometer transition layer is the composite layer of Ti/TiN, and the interface of the AlSiN layer of said hexagonal structure is provided with the AlSiN layer of cubic structure.
Be 7～9nm the modulation period of the TiN layer of said cubic structure and the AlSiN layer of hexagonal structure.
The total thickness of said 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 said 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 Vakuumkammer
2Insert in the Vakuumkammer 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 Vakuumkammer;
(3) feed Ar gas in the Vakuumkammer, 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 Vakuumkammer 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 said step (1), the target of the first intermediate frequency arc source is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source is processed 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 said step (2), the vacuum tightness of Vakuumkammer is 7 * 10
-3Pa, Heating temperature is 300～500 ℃, workpiece rotational frequency is 3～5 commentaries on classics/min.
In the said 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 said cubic structure and the AlSiN layer of hexagonal structure is 40～90min.
The present invention compares prior art and has the following advantages: 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 decrease of hardness that the appearance owing to six side AlN causes, 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 the 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 on precision die and high speed cutting instrument, has good application prospects.
Description of drawings
Fig. 1 is the structural representation of Vakuumkammer of the present invention;
Fig. 2 is a 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 deposited;
Fig. 6 is the diffraction pattern in transverse section of the TiN/AlSiN superlattice nano-composite coating of deposited;
Fig. 7 is the transverse section high resolution transmission view of the TiN/AlSiN superlattice nano-composite coating of deposited;
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 ability spectrogram of deposited Si;
Figure 11 is the ability 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 the variation synoptic diagram of TiN/AlSiN superlattice coating hardness with annealing temperature;
Figure 15 is the variation synoptic diagram of TiN/AlSiN superlattice anchoring strength of coating with 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
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
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 Vakuumkammer 1
2Insert in the Vakuumkammer 1 with Ar gas, the target of the first intermediate frequency arc source 2 is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is processed 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 UW 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 Vakuumkammer 1, and Vakuumkammer 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 Vakuumkammer 1, feed Ar gas, make that the pressure in the Vakuumkammer 1 is 2Pa, add negative bias 1000V workpiece surface is carried 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 samples 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 Vakuumkammer 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 obtains through the TEM check and analysis; 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; The TiN layer 8 of said cubic structure and AlSiN layer 9 alternating deposit of hexagonal structure are on nanometer transition layer 7, and said 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.
Like Fig. 7, shown in 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 with hexagonal structure of cubic structure.
Like Figure 10 and shown in Figure 11, after the XPS spectrum check and analysis, Si2p key bound energy mainly comprises 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.
Shown in figure 12, utilize XRD that superlattice TiN/AlSiN is carried out the thermal stability analysis, still to form after the annealing of superlattice nano coating by TiN, six sides' AlN phase has appearred 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 Vakuumkammer 1
2Insert in the Vakuumkammer 1 with Ar gas, the target of the first intermediate frequency arc source 2 is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is processed 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 UW 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 Vakuumkammer 1, and Vakuumkammer 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 Vakuumkammer 1, feed Ar gas, make that the pressure in the Vakuumkammer 1 is 2Pa, add negative bias 900V workpiece surface is carried 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 samples 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 Vakuumkammer 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.
Embodiment 3
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 Vakuumkammer 1
2Insert in the Vakuumkammer 1 with Ar gas, the target of the first intermediate frequency arc source 2 is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is processed 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 UW 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 Vakuumkammer 1, and Vakuumkammer 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 Vakuumkammer 1, feed Ar gas, make that the pressure in the Vakuumkammer 1 is 2Pa, add negative bias 1100V workpiece surface is carried 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 samples 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 Vakuumkammer 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.
Embodiment 4
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 Vakuumkammer 1
2Insert in the Vakuumkammer 1 with Ar gas, the target of the first intermediate frequency arc source 2 is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source 3 is processed 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 UW 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 Vakuumkammer 1, and Vakuumkammer 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 Vakuumkammer 1, feed Ar gas, make that the pressure in the Vakuumkammer 1 is 2Pa, add negative bias 1000V workpiece surface is carried 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 samples 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 Vakuumkammer 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.
Shown in figure 13; Comparative example 1～embodiment 4; Utilize dsc DSC to superlattice TiN/AlSiN coating thermokinetics behavior analyze, the superlattice nano coating exothermic peak occurs, the curve among the figure between 1 and 2 in 850 ℃～1030 ℃ scopes; Six corresponding side AlSiN decompose, and form the Si of crystallization
3N
4AlN with six sides.
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, and the hardness value of the superlattice coating of deposited is 52GPa, and the hardness value of superlattice nano-composite coating is 47GPa after through 1100 ℃ of vacuum annealings.
Shown in figure 15; Comparative example 1～embodiment 4 analyzes the bonding strength before and after the annealing of superlattice coating with scratch method, 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, pairing load when promptly coating and matrix take place to peel off in a large number) reaches 44N.
Shown in figure 16; Comparing traditional nitriding handles with TiN coating processing automobile component manufacturing and uses 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 (10)
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 said cubic structure and hexagonal structure is on the nanometer transition layer, and said nanometer transition layer is the composite layer of Ti/TiN, and the interface of the AlSiN layer of said hexagonal structure is provided with the AlSiN layer of cubic structure.
2. a kind of multi-arc ion coating superlattice nano-composite coating according to claim 1 is characterized in that: be 7～9nm the modulation period of the TiN layer of said 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 is characterized in that: the total thickness of said nano-composite coating is 4～6 μ m, and the thickness of nanometer transition layer is 1～2 μ m.
4. a kind of multi-arc ion coating superlattice nano-composite coating according to claim 1 is characterized in that: the Si that contains crystallization in the said nano-composite coating
3N
4Phase.
5. according to the preparation method of each described a kind of multi-arc ion coating superlattice nano-composite coating in the claim 1～4, 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 Vakuumkammer
2Insert in the Vakuumkammer 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 Vakuumkammer;
(3) feed Ar gas in the Vakuumkammer, 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 Vakuumkammer cool to room temperature gets final product.
6. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 5 is characterized in that, comprises that also step (6) anneals to post-depositional nano-composite coating, and annealing temperature is 700～1200 ℃.
7. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 5 is characterized in that, in the said step (1), the target of the first intermediate frequency arc source is processed by Ti simple substance, and purity is 99.9%; The target of the second intermediate frequency arc source is processed by AlSi powder metallurgy, and the atomic percent of Al and Si is 88: 12, and the purity of AlSi target is 99.9%.
8. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 5 is characterized in that, in the said step (2), the vacuum tightness of Vakuumkammer is 7 * 10
-3Pa, Heating temperature is 300～500 ℃, workpiece rotational frequency is 3～5 commentaries on classics/min.
9. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 5 is characterized in that, in the said step (4), the depositing time of Ti layer is 10～20min, and the depositing time of TiN layer is 40～60min.
10. the preparation method of a kind of multi-arc ion coating superlattice nano-composite coating according to claim 5 is characterized in that, the depositing time of the TiN layer of said cubic structure and the AlSiN layer of hexagonal structure is 40～90min.
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| CN103757597A (en) * | 2014-02-07 | 2014-04-30 | 上海理工大学 | TiN/CrAlSiN nano composite multilayer coating and preparation method thereof |
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| CN105971617A (en) * | 2016-05-12 | 2016-09-28 | 西安热工研究院有限公司 | Multi-layer film of tool ring of tunnel boring machine and preparation method thereof |
| CN108588715A (en) * | 2018-04-28 | 2018-09-28 | 九江职业技术学院 | A kind of nano combined cutter coat and preparation method thereof containing cobalt titanium nitrogen aluminium |
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| CN103757597A (en) * | 2014-02-07 | 2014-04-30 | 上海理工大学 | TiN/CrAlSiN nano composite multilayer coating and preparation method thereof |
| CN103757597B (en) * | 2014-02-07 | 2016-03-23 | 上海理工大学 | A kind of TiN/CrAlSiN nanocomposite laminated coating and preparation method thereof |
| CN103952671A (en) * | 2014-04-29 | 2014-07-30 | 马鞍山多晶金属材料科技有限公司 | Multi-arc ion plated hard coating prepared by adopting frequency-modulation electromagnetic coil, and method |
| CN104073770A (en) * | 2014-06-23 | 2014-10-01 | 江苏科技大学 | Tiwaln hard thin film and preparation method thereof |
| CN104674167A (en) * | 2015-02-09 | 2015-06-03 | 苏州涂冠镀膜科技有限公司 | Screw rod with PVD coating and surface treatment method thereof |
| CN105971617A (en) * | 2016-05-12 | 2016-09-28 | 西安热工研究院有限公司 | Multi-layer film of tool ring of tunnel boring machine and preparation method thereof |
| CN108588715A (en) * | 2018-04-28 | 2018-09-28 | 九江职业技术学院 | A kind of nano combined cutter coat and preparation method thereof containing cobalt titanium nitrogen aluminium |
| 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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