CN105803411A - Combined method of arc ion plating and twin target bipolar high-power pulsed magnetron sputtering - Google Patents

Combined method of arc ion plating and twin target bipolar high-power pulsed magnetron sputtering Download PDF

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CN105803411A
CN105803411A CN201610310484.9A CN201610310484A CN105803411A CN 105803411 A CN105803411 A CN 105803411A CN 201610310484 A CN201610310484 A CN 201610310484A CN 105803411 A CN105803411 A CN 105803411A
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magnetron sputtering
target
power supply
power
ion plating
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魏永强
宗晓亚
魏永辉
侯军兴
蒋志强
符寒光
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325Electric arc evaporation

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  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a combined method of arc ion plating and twin target bipolar high-power pulsed magnetron sputtering, and belongs to the technical field of material surface treatment. The method aims to solve the problem of large particles due to use of low-melting-point pure metal (like aluminum) or multicomponent alloy materials and non-metallic materials (like graphite) in arc ion plating and the limitation of semiconductor material silicon, and discharge arcing in the unipolar high-power pulsed magnetron sputtering technique and the limit in using of high-melting-point and difficult-to-ionize target materials (like zirconium) are eliminated. The method includes the steps that first, workpieces are placed on a sample table inside a vacuum chamber and connected with related equipment; second, thin film deposition is performed, working gas is introduced when vacuumizing is executed to 10<-4> Pa, and a film coating power supply is switched on; and the large-particle defect in arc ion plating is overcome through high-power pulsed magnetron sputtering, the high-melting-point and difficult-to-ionize materials are ionized through arc ion plating, twin targets generate multi-component plasma and further adjust the content of the plasma in a thin film, plasma energy is regulated through a grid bias power supply, and accordingly the thin film can be prepared.

Description

Arc ion plating and twin target bipolarity high-power impulse magnetron sputtering complex method
Technical field
The present invention relates to arc ion plating and twin target bipolarity high-power impulse magnetron sputtering complex method, belong to material Technical field of surface.
Background technology
Arc ion plating (aip) can obtain the nearly all metal ion including carbon ion, simultaneously with high ionization Rate, diffractive good, the advantage such as film-substrate cohesion is good, coating quality is good, deposition efficiency is high and equipment is easy and simple to handle and come into one's own, It it is one of current physical vapour deposition (PVD) technology of preparing being used widely in the industry.It can be not only used for preparing metal and prevents Protect coating, it is also possible to by the regulation of process, it is achieved the preparation of the high-temperature ceramic coating such as nitride, carbide, exist simultaneously Also there is application in function film field.Even for the parts that shape is irregular, arc ion plating can also realize the fast of thin film Speed deposition, even also serves as nanometer multilayer and superlattice film preparation method (Tay B K, Zhao Z W, Chua D H C. Review of metal oxide films deposited by filtered cathodic vacuum arc Technique [J]. Mater Sci Eng R, 2006,52 (1-3): 1-48.).But prepare thin at arc ion plating During film, owing to arc speckle electric current density is up to 2.5 ~ 5 × 1010A/m2, cause the arc speckle position of target material surface to occur molten The liquid metal melted, under the effect of local plasma pressure in droplets splash out, be attached to film surface or Inlay in the film formed " bulky grain " (Macroparticles) defect (Wei Yongqiang, literary composition Zhenhua, Jiang Zhiqiang, Tian Xiubo. The distribution research [J] in thin film prepared by arc ion plating of the bulky grain defect. vacuum, 2013,50 (6): 7- 10.).Just as the PM2.5 pollution to air quality, relative to the thin film that thickness rank is micron or submicron, size exists The bulky grain defect of 0.1-10 micron has serious harm to quality and the performance of thin film.Along with thin-film material and thin film technique That applies is increasingly extensive, and whether the solution of bulky grain defect problem becomes the bottleneck that arc ions electroplating method develops further, sternly Heavily constrain its application in a new generation's thin-film material preparation.The way of Magnetic filter is the most generally used to filter out bulky grain, If Chinese patent is for plasma immersion and ion implantation device (publication number: CN1150180, the publication date of material surface modifying Phase: on May 21st, 1997) in use 90 ° of magnetic filters the bulky grain of pulsed cathode arc is filtered, American scholar Anders et al. (Anders S, Anders A, Dickinson M R, MacGill R A, Brown I G. S- shaped magnetic macroparticle filter for cathodic arc deposition [J]. IEEE Trans Plasma Sci, 1997,25 (4): 670-674.) make " S " magnetic filter under study for action to cathode arc Bulky grain filters, although these methods have certain effect in terms of bulky grain filtering and eliminate, but the biography of plasma Defeated loss in efficiency is serious, makes ion current density be substantially reduced.
1999, V. Kouznetsov of Linkoping,Sweden university et al. (Kouznetsov V, Mac á k K, Schneider J M, Helmersson U, Petrov I. A novel pulsed magnetron sputter technique utilizing very high target power densities [J]. Surf Coat Tech, 1999,122 (2-3): 290-293.) high-power impulse magnetron sputtering technology (HPPMS) is proposed, it utilizes higher pulse peak Value power and relatively low pulse width improve the ionization level of sputter material, and will not to increase target because of overheated cold for target cathode simultaneously But requirement.Its peak power improves 100 times compared to conventional DC magnetron sputtering, about 1000 ~ 3000W/cm2, wait from The density of daughter reaches 1018m-3The order of magnitude, its central region ion concentration is up to 1019m-3The order of magnitude, simultaneously sputter material Ionization level reaches as high as more than 90%, and without the bulky grain defect in the arc ions electroplating method the highest present off rate.2008 After Nian, at home each colleges and universities also begin to launch for high-power impulse magnetron sputtering technology research (Li Xiping. Gao Gong Rate composite pulse magnetron sputtering plasma characteristics and TiAlN thin film prepare [D];Harbin Institute of Technology, 2008. Wuzhongs Shake, Zhu Zongtao, Gong Chunzhi, Tian Xiubo, Yang Shiqin, Li Xiping. the development of high-power impulse magnetron sputtering technology with grind Study carefully [J]. vacuum, 2009,46 (3): 18-22. and Mu Zongxin, Mu Xiaodong, Wang Chun, Jia Li, Dong Chuan. DC source Coupling high power pulse non-balance magnetically controlled sputter ionization property [J]. Acta Physica Sinica, 2011,60 (1): 422-428.), but Being owing to the pulsed discharge of high-power impulse magnetron sputtering technology is unstable, and target current potential is relatively low, target metal is after ionization Substantial amounts of metal ion is sucked back into target surface, fails to arrive matrix surface and realizes the deposition of thin film, causes the effect of thin film deposition Rate is substantially reduced, and affects it and is further substituted with common magnetron sputtering and the paces of arc ion plating, in follow-up popularization and application side Face receives a definite limitation.Although also there being scholar to be improved the application of high-power impulse magnetron sputtering, such as China is specially Profit high power combined pulsed magnetron sputtering ion implantation and deposition method (publication number: CN101838795A, publication date: 2010 On JIUYUE 22) advantage utilizing high pressure and impulsive synchronization coalignment to make full use of high-power impulse magnetron sputtering that proposed, Realize the breakthrough at field ion implantation of the high-power impulse magnetron sputtering technology, but due to the restriction of high voltage power supply, arrive base The density of surface depositing ions can not be the highest, otherwise can cause the damage of high voltage power supply.And twin target bipolarity high power arteries and veins Rush magnetron sputtering technique and on double targets, obtain the alternating voltage of opposite in phase respectively by alternating current power supply, double targets replace into anode and Negative electrode, can be substantially improved the stability that hipims electric discharge runs, and the accumulation of target surface charge can be avoided to draw simultaneously The sparking problem risen, is substantially improved the stability that high-power impulse magnetron sputtering electric discharge runs.(Wang Lang puts down, and Lin Tiegui, king is little Peak. a kind of high power bipolar pulse magnetically controlled sputter method [P]. publication number: CN104195515A, publication date: 2014-12- 10.).
At present, the simple metal of low melting point or multicomponent alloy material is being used to be easily generated greatly in order to solve arc ions electroplating method There is the problem being difficult to ionization in grain defect and magnetron sputtering technique in terms of using high-melting-point target, extends existing arc ions Plating and two kinds of methods of magnetron sputtering, in the respective limitation of target use, make full use of twin target bipolarity high power pulse Low melting point metal material (such as aluminum) that magnetron sputtering should not be able to use with sputtering sedimentation arc ions electroplating method or multicomponent alloy Target (such as aluminum silicon), nonmetallic materials (such as graphite) and semi-conducting material (such as silicon) (prosperous. Al2O3Thermal control coating High-power impulse magnetron sputtering Study on Preparation Technology [D];Harbin Institute of Technology, 2014. He Jia. ABS plastic is aluminized table Face high power pulse r. f. magnetron sputtering SiO2Thin film study [D];Dalian University of Technology, 2013. and Cui Shaoqiang. class The high-power impulse magnetron sputtering of diamond carbon thin-film material prepares [D];Shandong University, 2015.), utilize simultaneously electric arc from Son is plated in the advantage in terms of high-melting-point and difficult ionization target, realizes preparing multicomponent material, component ratio and microstructure adjustable Thin film.
Summary of the invention
The invention aims to for solve conventional arc ion electroplating method is easily generated bulky grain defect, Magnetic filter technology is drawn Play arc-plasma efficiency of transmission low and use the simple metal (such as aluminum) of low melting point or multicomponent alloy material (such as aluminum silicon closes Gold), nonmetallic materials (such as graphite) and semi-conducting material (such as silicon) deposit in conventional arc ion electroplating method as target Bulky grain, conventional magnetron sputtering technology ionization level and thin film deposition efficiency is low, high-melting-point target use limitation, with eutectic The simple metal (such as aluminum) of point or multicomponent alloy material (such as alusil alloy) and nonmetallic materials (such as graphite and quasiconductor material Material silicon etc.) as the target of twin target bipolarity high-power impulse magnetron sputtering, recycling arc ions electroplating method make difficult ionization, Materials with high melting point (such as zirconium and alloy material thereof) produces the arc-plasma of ionization level continual and steady, high, makes surface of the work Apply back bias voltage situation can be continuous, fine and close prepare high-quality thin-film, realize simultaneously in thin film constituent content add control System, reduction use the production cost of alloys target, the deposition efficiency of raising thin film, minimizing high-power impulse magnetron sputtering sparking to discharge In unstability and arc ion plating bulky grain defect to thin film growth and the adverse effect of performance, it is proposed that arc ion plating and Twin target bipolarity high-power impulse magnetron sputtering complex method.
The used device of the inventive method includes that grid bias power supply 1, arc power 2, arc ion plating target source 3, twin target are bipolar Property high-power impulse magnetron sputtering power supply 4, twin target bipolarity high-power impulse magnetron sputtering target source 5, twin target bipolarity high Power Impulse Magnetron shielding power supply kymographion 6, grid bias power supply kymographion 7, vacuum chamber 8 and sample stage 9;
The method comprises the following steps:
Step one, being placed on the sample stage 9 in vacuum chamber 8 by pending substrate work-piece, workpiece connects the outfan of grid bias power supply 1, The arc ion plating target source 3 being arranged on vacuum chamber 8 connects the outfan of arc power 2, twin target bipolarity high power pulse magnetic control Sputtering target source 5 connects the high power pulse outfan of twin target bipolarity high-power impulse magnetron sputtering power supply 4;
Step 2, thin film deposition: by vacuum chamber 8 evacuation, treat that the vacuum in vacuum chamber 8 is less than 10-4During Pa, it is passed through work Gas, to 0.01Pa~10Pa, is opened grid bias power supply 1 and grid bias power supply kymographion 7, and is regulated the inclined of grid bias power supply 1 output Pressure amplitude value, pulse frequency and pulse width, it is 0~1.2kV that grid bias power supply 1 exports the peak voltage of pulse, and pulse frequency is 0 ~80kHz, pulse width 1 ~ 90%, can be according to the output frequency of twin target bipolarity high-power impulse magnetron sputtering power supply 4 and defeated Go out waveform and carry out Matching and modification;
After the surface in arc ion plating target source 3 is carried out by unlatching arc power 2 by the spots moving of electric arc, regulation needs Technological parameter, the current value of arc power 2 output is 10A ~ 300A, makes high-melting-point, difficult ionization target (such as zirconium and alloy material thereof Material) produce high ionization level, highdensity arc-plasma, it is achieved the fast deposition of thin film;
Open twin target bipolarity high-power impulse magnetron sputtering power supply 4, adjust suitable output services power, running voltage and After operating current, make twin target bipolarity high-power impulse magnetron sputtering target source 5 build-up of luminance, to twin target bipolarity high power pulse Surface, magnetic controlled sputtering target source 5 carries out film preparation after being carried out, twin target bipolarity high-power impulse magnetron sputtering power supply 4 Output 100W ~ 120kW, frequency 0 ~ 10kHz, peak point current 10A ~ 4000A, positive negative pulse stuffing width 5 μ s~300 μ s, work Voltage 100V ~ 4000V, positive negative pulse stuffing is set to 5 μ s~3000 μ s, then according to target kind, size and depositing operation choosing Select twin target bipolarity high-power impulse magnetron sputtering power supply 4 output running voltage, peak point current, positive negative pulse stuffing width and Every, produce stable multiple elements design plasma, adjust twin target element ratio in the film.
According to the needs of film preparation, adjust relevant technological parameter and carry out simple metal thin film, the change of different element ratio Compound ceramic membrane, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure prepare.
Advantages of the present invention: a. uses pure for low melting point of twin target bipolarity high-power impulse magnetron sputtering technology Metal or multicomponent alloy material do not produce bulky grain defect, therefore need not defecator, it is possible to achieve ionization ion efficient Transmission;B. utilize twin target bipolarity high-power impulse magnetron sputtering technology, can use two kinds of different unit targets or The combination such as unit and polynary and two kinds of multicomponent target materials, it is achieved the plasma of multiple elements design produces, and then can deposit various Unit, polynary and type of compounds and the thin film of different element ratio;C. can to make up twin target bipolar in arc ion plating target source Property high-power impulse magnetron sputtering high-melting-point target (such as zirconium and alloy material thereof) is difficult to the restriction of ionization, it is ensured that deposit from The high density of son persistently produces;D. owing to have employed pulsed bias Waveform output device, matrix can be made effectively to attract twin Multiple elements design ion produced by target bipolarity high-power impulse magnetron sputtering and arc ion plating target source, it is ensured that thin film deposition Speed, makes the energy of depositing ions obtain optimizing regulation;E. by regulation twin target bipolarity high-power impulse magnetron sputtering target The technological parameter in source, in conjunction with the technological parameter in arc ion plating target source, it is possible to achieve in compound plasma various elements from Sub-ratio, it is achieved the thin film deposition of different element ratios;The microstructure and properties of the most prepared thin film can be inclined by pulse Pressure parameter is adjusted, and utilizes the amplitude of pulsed bias, pulse width and frequency to realize the pinning that thin film is grown by energetic ion Effect, improves texture and the stress state of thin film growth, improves bond strength;G. due to twin target bipolarity high power Pulsed magnetron sputtering eliminates the simple metal (such as aluminum) of low melting point or multicomponent alloy material (such as alusil alloy) and nonmetal The material (such as graphite and Semiconducting Silicon Materials etc.) application in arc ion plating limits, it is possible to achieve originally multi-element film system The thin film that during Bei, the interpolation of these elements and ratio adjust;H. prepared thin film avoids eutectic in arc ion plating High-melting-point, difficult ionization material (such as zirconium and alloy material thereof) in the bulky grain defect of some target and high-power impulse magnetron sputtering The problem that ionization level is low, the texture of thin film is finer and close, further increases the mechanical property of thin film.
Step 3, can individually use Traditional DC magnetron sputtering, pulsed magnetron sputtering, twin target medium frequency magnetron sputtering, Twin target bipolarity high-power impulse magnetron sputtering, conventional arc ion plating, pulsed cathode arc or multi-stage magnetic field arc ion plating Carry out thin film deposition in conjunction with the compound bias of Dc bias, pulsed bias or DC pulse is compound, prepare simple metal thin film, difference The compound ceramic thin film of element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Step 3, can individually use Traditional DC magnetron sputtering, pulsed magnetron sputtering, twin target medium frequency magnetron sputtering, Twin target bipolarity high-power impulse magnetron sputtering, conventional arc ion plating, pulsed cathode arc or Magnetic filter arc ion plating knot Close Dc bias, the compound bias of pulsed bias or DC pulse is compound carries out thin film deposition, prepares simple metal thin film, different unit The element compound ceramic thin film of ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Accompanying drawing explanation
Fig. 1 is arc ion plating of the present invention and twin target bipolarity high-power impulse magnetron sputtering complex method sketch.
Detailed description of the invention
Detailed description of the invention one: present embodiment, present embodiment arc ion plating and twin target are described below in conjunction with Fig. 1 The used device of bipolarity high-power impulse magnetron sputtering complex method includes grid bias power supply 1, arc power 2, arc ion plating target Source 3, twin target bipolarity high-power impulse magnetron sputtering power supply 4, twin target bipolarity high-power impulse magnetron sputtering target source 5, Twin target bipolarity high-power impulse magnetron sputtering power supply wave shape oscillograph 6, grid bias power supply kymographion 7, vacuum chamber 8 and sample Sample platform 9;
The method comprises the following steps:
Step one, being placed on the sample stage 9 in vacuum chamber 8 by pending substrate work-piece, workpiece connects the outfan of grid bias power supply 1, The arc ion plating target source 3 being arranged on vacuum chamber 8 connects the outfan of arc power 2, twin target bipolarity high power pulse magnetic control Sputtering target source 5 connects the high power pulse outfan of twin target bipolarity high-power impulse magnetron sputtering power supply 4;
Step 2, thin film deposition: by vacuum chamber 8 evacuation, treat that the vacuum in vacuum chamber 8 is less than 10-4During Pa, it is passed through work Gas, to 0.01Pa~10Pa, is opened grid bias power supply 1 and grid bias power supply kymographion 7, and is regulated the inclined of grid bias power supply 1 output Pressure amplitude value, pulse frequency and pulse width, it is 0~1.2kV that grid bias power supply 1 exports the peak voltage of pulse, and pulse frequency is 0 ~80kHz, pulse width 1 ~ 90%, can be according to the output frequency of twin target bipolarity high-power impulse magnetron sputtering power supply 4 and defeated Go out waveform and carry out Matching and modification;
After the surface in arc ion plating target source 3 is carried out by unlatching arc power 2 by the spots moving of electric arc, regulation needs Technological parameter, the current value of arc power 2 output is 10A ~ 300A, makes high-melting-point, difficult ionization target (such as zirconium) produce high ionization Rate, highdensity arc-plasma, it is achieved the fast deposition of thin film;
Open twin target bipolarity high-power impulse magnetron sputtering power supply 4, adjust suitable output services power, running voltage and After operating current, make twin target bipolarity high-power impulse magnetron sputtering target source 5 build-up of luminance, to twin target bipolarity high power pulse Surface, magnetic controlled sputtering target source 5 carries out film preparation after being carried out, twin target bipolarity high-power impulse magnetron sputtering power supply 4 Output 100W ~ 120kW, frequency 0 ~ 10kHz, peak point current 10A ~ 4000A, positive negative pulse stuffing width 5 μ s~300 μ s, work Voltage 100V ~ 4000V, positive negative pulse stuffing is set to 5 μ s~3000 μ s, then according to target kind, size and depositing operation choosing Select twin target bipolarity high-power impulse magnetron sputtering power supply 4 output running voltage, peak point current, positive negative pulse stuffing width and Every, produce stable multiple elements design plasma, adjust twin target element ratio in the film.
Grid bias power supply 1 output waveform is direct current, pulse, DC pulse is compound or multiple-pulse is combined.
Arc power 2 exports direct current, pulse, DC pulse is compound or multiple-pulse is combined.
Arc ion plating target source 3 uses high-melting-point, the simple metal of difficult ionization or multicomponent alloy material (such as zirconium and alloy thereof Material), twin target bipolarity high-power impulse magnetron sputtering target source 5 uses simple metal (such as aluminum) or the multicomponent alloy of low melting point Material (such as alusil alloy) and nonmetallic materials (such as graphite and Semiconducting Silicon Materials etc.), it is possible to use single target, multiple Target or composition target, carry out simple metal thin film, the different compound ceramic thin film of element ratio, function film, multi-component multi-layer, super brilliant Lattice, there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Working gas selects argon, or working gas selects one or more in nitrogen, acetylene, methane, silane or oxygen Mixed gas, prepare simple metal thin film, the different compound ceramic thin film of element ratio, function film, multi-component multi-layer, super Lattice, there is the thin film of nanometer multilayer or gradient-structure.
Arc ion plating and the proposition of twin target bipolarity high-power impulse magnetron sputtering complex method, make full use of twin Target bipolarity high-power impulse magnetron sputtering achieves the simple metal of low melting point or multicomponent alloy material and nonmetallic materials (such as Graphite and Semiconducting Silicon Materials etc.) application in arc ion plating, it is prevented effectively from arc ion plating target and uses low melting point material Produced bulky grain problem during material, breaches again nonmetallic materials (such as graphite and Semiconducting Silicon Materials etc.) in arc ions Application in plating limits, and twin target can use two kinds of different unit targets or unit and polynary and two kinds of polynary targets Materials etc. combine, it is achieved the plasma of multiple elements design produces, deposition all kinds and the thin film of element ratio;Utilize waveform simultaneously Output device adjusts applied back bias voltage parameter on workpiece in time, is conducive to improving the interval electromotive force of plasma between target base and divides Cloth, fully attracts compound plasma to workpiece motion s, it is achieved the fast deposition of thin film;The most also utilize arc ion plating (aip) Produce stable continue, metallic plasma that ionization level is high, decrease high-melting-point, difficult ionization metal material in twin target Frequently the restriction used in magnetron sputtering, the highest ionization level ion is at the chemosynthesis reaction of surface of the work, and preparation is different first The element compound ceramic thin film of ratio, function film, multi-component multi-layer, superlattices and there is the thin film of gradient-structure or simple metal is thin Film.
Detailed description of the invention two: present embodiment is with the difference of embodiment one, and the method also includes:
Step 3, can individually use Traditional DC magnetron sputtering, pulsed magnetron sputtering, twin target medium frequency magnetron sputtering, twin Target bipolarity high-power impulse magnetron sputtering, conventional arc ion plating, pulsed cathode arc or Magnetic filter arc ion plating combine straight The compound bias of stream bias, pulsed bias or DC pulse is compound carries out thin film deposition, prepares simple metal thin film, different element ratio The compound ceramic thin film of example, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Step 2 can first use twin target bipolarity high-power impulse magnetron sputtering power supply 4 carry out magnetron sputtering combination High-tension pulsed bias power supply carries out the pinning effect that thin film is grown by energetic ion, improves the adhesion of thin film and matrix, Then step 3 is carried out, it is thus achieved that certain thickness thin film.
Detailed description of the invention three: present embodiment is with the difference of embodiment two, repeatedly perform step one to Step 3, preparation has the multilayer films of different stress, microstructure and element ratio, other and embodiment two Identical;
Step 2 can first use twin target bipolarity high-power impulse magnetron sputtering power supply 4 carry out magnetron sputtering and combine high electricity Pressure carries out the pinning effect that thin film is grown by energetic ion, improves the adhesion of thin film and matrix, then carries out step 3, then Repeatedly performing step 2 and step 3, the most repeatedly, preparation has the multilamellar of different stress, microstructure and element ratio Structural membrane.
Detailed description of the invention four: present embodiment is with the difference of embodiment one, repeatedly perform step one to Step 3, preparation has the multilayer films of different stress, microstructure and element ratio, other and embodiment two Identical.
Step 2 can use 2 sets or 2 overlap above twin target bipolarity high-power impulse magnetron sputtering target source 5 to enter Row (compares with the simple metal element (such as aluminum) of various low melting points or multicomponent alloy material (such as alusil alloy) and nonmetallic materials Such as graphite and Semiconducting Silicon Materials etc.) it is the thin film deposition of target, then carry out step 3, the most repeatedly perform step 2 and step Rapid three, the most repeatedly, preparation has the multilayer films of different stress, microstructure and element ratio.

Claims (7)

1. arc ion plating and twin target bipolarity high-power impulse magnetron sputtering complex method, it is characterised in that the method institute Device is used to include grid bias power supply 1, arc power 2, arc ion plating target source 3, twin target bipolarity high-power impulse magnetron sputtering Power supply 4, twin target bipolarity high-power impulse magnetron sputtering target source 5, twin target bipolarity high-power impulse magnetron sputtering power supply Kymographion 6, grid bias power supply kymographion 7, vacuum chamber 8 and sample stage 9;
The method comprises the following steps:
Step one, being placed on the sample stage 9 in vacuum chamber 8 by pending substrate work-piece, workpiece connects the outfan of grid bias power supply 1, The arc ion plating target source 3 being arranged on vacuum chamber 8 connects the outfan of arc power 2, twin target bipolarity high power pulse magnetic control Sputtering target source 5 connects the high power pulse outfan of twin target bipolarity high-power impulse magnetron sputtering power supply 4;
Step 2, thin film deposition: by vacuum chamber 8 evacuation, treat that the vacuum in vacuum chamber 8 is less than 10-4During Pa, it is passed through work gas Body, to 0.01Pa~10Pa, is opened grid bias power supply 1 and grid bias power supply kymographion 7, and is regulated the bias of grid bias power supply 1 output Amplitude, pulse frequency and pulse width, it is 0~1.2kV that grid bias power supply 1 exports the peak voltage of pulse, pulse frequency be 0~ 80kHz, pulse width 1 ~ 90%, can be according to the output frequency of twin target bipolarity high-power impulse magnetron sputtering power supply 4 and output Waveform carries out Matching and modification;
After the surface in arc ion plating target source 3 is carried out by unlatching arc power 2 by the spots moving of electric arc, regulation needs Technological parameter, the current value of arc power 2 output is 10A ~ 300A, makes high-melting-point, difficult ionization target (such as zirconium) produce high ionization Rate, highdensity arc-plasma, it is achieved the fast deposition of thin film;
Open twin target bipolarity high-power impulse magnetron sputtering power supply 4, adjust suitable output services power, running voltage and After operating current, make twin target bipolarity high-power impulse magnetron sputtering target source 5 build-up of luminance, to twin target bipolarity high power pulse Surface, magnetic controlled sputtering target source 5 carries out film preparation after being carried out, twin target bipolarity high-power impulse magnetron sputtering power supply 4 Output 100W ~ 120kW, frequency 0 ~ 10kHz, peak point current 10A ~ 4000A, positive negative pulse stuffing width 5 μ s~300 μ s, work Voltage 100V ~ 4000V, positive negative pulse stuffing is set to 5 μ s~3000 μ s, then according to target kind, size and depositing operation choosing Select twin target bipolarity high-power impulse magnetron sputtering power supply 4 output running voltage, peak point current, positive negative pulse stuffing width and Every, produce stable multiple elements design plasma, adjust twin target element ratio in the film.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, the used device of the method also includes that grid bias power supply kymographion 7 is for showing the arteries and veins that grid bias power supply 1 sends Rush voltage and current waveform, by adjusting the output waveform of grid bias power supply 1, plated film ion is effectively attracted, it is achieved right The regulation of energy of plasma;Utilize twin target bipolarity high-power impulse magnetron sputtering power supply wave shape oscillograph 6 for showing The bipolar voltage of twin target bipolarity high-power impulse magnetron sputtering power supply 4 and current waveform, bipolar by adjusting twin target Property high-power impulse magnetron sputtering power supply 4 make twin target bipolarity high-power impulse magnetron sputtering target source 5 produce stable, continue and The multiple elements design plasma of high ionization level, carries out the deposition of thin film and controls low melting point simple metal (such as aluminum) or alloy material (such as alusil alloy) and nonmetallic materials (such as graphite and Semiconducting Silicon Materials etc.) element ratio in the film.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, grid bias power supply 1 export pulse be pulse, DC pulse is compound or multiple-pulse is combined.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, the method also includes:
Step 3, can individually use Traditional DC magnetron sputtering, pulsed magnetron sputtering, twin target medium frequency magnetron sputtering, twin Target bipolarity high-power impulse magnetron sputtering, conventional arc ion plating, pulsed cathode arc or Magnetic filter arc ion plating combine straight The compound bias of stream bias, pulsed bias or DC pulse is compound carries out thin film deposition, prepares simple metal thin film, different element ratio The compound ceramic thin film of example, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, repeatedly perform step one to step 2, prepare simple metal thin film, different element ratio compound ceramic thin Film, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, the target body material that twin target bipolarity high-power impulse magnetron sputtering target source 5 uses can be the pure of low melting point Metal (such as aluminum) or multicomponent alloy target (such as aluminum silicon), and arc ion plating target source 3 should not use nonmetal (such as Graphite) and semi-conducting material (such as silicon), and arc ion plating target source 3 can be the height using magnetron sputtering technique to be difficult to ionization Fusing point simple metal or multicomponent alloy material (such as zirconium and alloy material thereof), it is also possible to effectively utilize twin target technology to realize eutectic The simple metal of point or multicomponent alloy target and nonmetalloid element ratio in the film.
Arc ion plating the most according to claim 1 and twin target bipolarity high-power impulse magnetron sputtering complex method, It is characterized in that, working gas selects argon, or working gas is selected in nitrogen, acetylene, methane, silane or oxygen a kind of or many The mixed gas planted, prepares simple metal thin film, compound ceramic thin film, the function film of different element ratio and has nanometer Multilamellar or the high-quality thin-film of gradient-structure.
CN201610310484.9A 2016-05-11 2016-05-11 Combined method of arc ion plating and twin target bipolar high-power pulsed magnetron sputtering Pending CN105803411A (en)

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CN108220901A (en) * 2018-02-06 2018-06-29 中国工程物理研究院流体物理研究所 A kind of novel plasma sputtering film coating method
CN108441832A (en) * 2018-03-28 2018-08-24 北京师范大学 A kind of centrifugal pump impeller surface treatment method and equipment
CN109136871A (en) * 2018-09-04 2019-01-04 北京航空航天大学 A kind of bipolar pulse magnetically controlled sputter method
CN112030117A (en) * 2020-07-28 2020-12-04 温州职业技术学院 Method for preparing aluminum oxide coating by modulating high-current pulse arc

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CN108220901A (en) * 2018-02-06 2018-06-29 中国工程物理研究院流体物理研究所 A kind of novel plasma sputtering film coating method
CN108441832A (en) * 2018-03-28 2018-08-24 北京师范大学 A kind of centrifugal pump impeller surface treatment method and equipment
CN109136871A (en) * 2018-09-04 2019-01-04 北京航空航天大学 A kind of bipolar pulse magnetically controlled sputter method
CN112030117A (en) * 2020-07-28 2020-12-04 温州职业技术学院 Method for preparing aluminum oxide coating by modulating high-current pulse arc
CN112030117B (en) * 2020-07-28 2022-08-12 温州职业技术学院 Method for preparing aluminum oxide coating by modulating high-current pulse arc

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