CN106756823A - Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube - Google Patents

Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube Download PDF

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CN106756823A
CN106756823A CN201710053016.2A CN201710053016A CN106756823A CN 106756823 A CN106756823 A CN 106756823A CN 201710053016 A CN201710053016 A CN 201710053016A CN 106756823 A CN106756823 A CN 106756823A
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magnetic field
straight tube
arc
film
stage magnetic
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CN106756823B (en
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魏永强
宗晓亚
张华阳
刘学申
刘源
侯军兴
蒋志强
冯宪章
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Zhengzhou University of Aeronautics
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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
    • C23C14/24Vacuum evaporation
    • C23C14/32Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, belong to technical field of material surface treatment, the present invention is to solve the problems, such as the loss in bulky grain and depositing ions pollute to inside pipe wall in multi-stage magnetic field filter cleaning and arc-plasma transmitting procedure.The inventive method includes:First, on the sample stage that workpiece to be coated is placed in vacuum chamber, line related is connected, opens external water cooling system;2nd, thin film deposition:Treat that the vacuum in vacuum chamber is less than 10‑4During Pa, it is passed through working gas and adjusts air pressure, open plated film power supply, attract the arc-plasma in exit using grid bias power supply simultaneously and carry out energy adjustment, bulky grain defect is effectively eliminated by the stop shielding of liner positive bias conical pipe and straight tube set composite itself and the filtering effect of positively biased piezoelectric field inhibitory action and multi-stage magnetic field and ensures the efficiency of transmission of arc-plasma, technological parameter needed for setting, carries out film preparation.

Description

Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube
Technical field
The present invention relates to liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, belong to material Technical field of surface.
Background technology
During arc ion plating prepares film, because arc spot current density is up to 2.5 ~ 5 × 1010A/m2, cause Occurs the liquid metal of melting at the arc spot position of target material surface, in the presence of local plasma pressure in droplets Splash out, is attached to film surface or inlays formation " bulky grain " in the film(Macroparticles)Defect(Boxman R L, Goldsmith S. Macroparticle contamination in cathodic arc coatings: generation, transport and control [J]. Surf Coat Tech, 1992, 52(1): 39-50.). In arc-plasma, it is far longer than due to the movement velocity of electronics and big is reached in the movement velocity of ion, unit interval The electron number on grain surface is more than number of ions, makes bulky grain that elecrtonegativity is presented.It is the thin of micron or sub-micron relative to thickness rank Film, pollution of the size in 0.1-10 microns of bulky grain defect just as PM2.5 to air quality, quality and property to film There can be serious harm.It is increasingly extensive with thin-film material and thin film technique application, the solution of bulky grain defect problem with The no bottleneck further developed as arc ions electroplating method, seriously constrains its answering in thin-film material of new generation preparation With.
At present, it is also easy to produce greatly in the simple metal using low melting point or multicomponent alloy material to solve arc ions electroplating method Grain defect problem, the method for using Magnetic filter main at present filters out bulky grain, and such as Chinese patent is used for material surface modifying Plasma immersion and ion implantation device(Publication number:CN1150180, publication date:On May 21st, 1997)It is middle to use 90 ° Magnetic filter is filtered to the bulky grain of pulsed cathode arc, 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.) and the Zhang Yujuan etc. of He'nan University (such as Zhang Yujuan, Wu Zhiguo, Zhang Weiwei filtered cathode arc plasmas prepare TiAlN thin film Influence China YouSe Acta Metallurgica Sinica 2004,14 (8) of the middle sedimentary condition to film texture:1264-1268.) in article Middle " S " magnetic filter that made is filtered to the bulky grain of cathode arc, also American scholar Anders et al.(Anders A, MacGill R A. Twist filter for the removal of macroparticles from cathodic arc plasmas [J]. Surf Coat Tech, 2000, 133-134: 96-100.)The Twist filter's of proposition Magnetic filter, although the efficiency of transmission that these methods have certain effect, plasma in terms of filtering and eliminating bulky grain is damaged Lose seriously, substantially reduce ion current density.Based on that can filter on the basis of bulky grain can guarantee that efficiency again, Chinese patent is true Empty cathode arc straight filter (publication number:CN1632905, publication date:On June 29th, 2005) the middle side for proposing straight tube filtering Method, but which in turn reduces filter effect.In a word, related researcher is by contrasting various Magnetic filter methods(Anders A. Approaches to rid cathodic arc plasmas of macro- and nanoparticles: a review [J] Surf Coat Tech, 1999,120-121319-330. and Takikawa H, Tanoue H. Review of cathodic arc deposition for preparing droplet-free thin films [J]. IEEE Trans Plasma Sci, 2007, 35(4): 992-999.)It was found that arc ion plating plasma after magnetic filter by keeping Efficiency of transmission and elimination bulky grain high is very difficult to take into account, and drastically influence application of the technology in high-quality thin-film deposition. In addition using the electric field suppressing method of bias on matrix, when back bias voltage is applied on matrix, electric field will be to electronegative big Grain produces repulsive interaction, and then reduces the generation of film surface bulky grain defect.German scholar Olbrich et al.(Olbrich W, Fessmann J, Kampschulte G, Ebberink J. Improved control of TiN coating properties using cathodic arc evaporation with a pulsed bias [J]. Surf Coat Tech, 1991, 49(1-3):258-262. and Fessmann J, Olbrich W, Kampschulte G, Ebberink J. Cathodic arc deposition of TiN and Zr(C, N) at low substrate temperature using a pulsed bias voltage [J]. Mat Sci Eng A, 1991, 140: 830-837.)Using pulse Bias to replace traditional Dc bias, form a kind of new physical gas phase deposition technology --- pulsed bias arc ion plating Technology, not only greatly reduces the number of film surface bulky grain, also overcomes the substrate temperature mistake that Traditional DC bias causes It is high, the problems such as stress in thin films is larger.Woods Guoqiang of Dalian University of Technology et al.(Woods Guoqiang pulsed bias arc ion platings Process ba- sis research [D] Dalian University of Technology, 2008. and Huang Meidong, woods Guoqiang, Dong Chuan, Sun Chao hear immediately inclined Press Influencing Mechanism [J] the Acta Metallurgica Sinicas to arc ion plating film surface appearance, 2003,39 (5): 510-515.)Pin The mechanism for causing bulky grain defect to reduce to pulsed bias conducts in-depth analysis, by pulsed bias amplitude, frequency and arteries and veins The adjustment of width and other processes parameter is rushed, the sheaths kinetic characteristic of arc-plasma can be improved, reduce film surface big Grain defect counts, improve the quality of film, are widely used in actual production, but bulky grain can not be still completely eliminated and lack Fall into.Domestic scholars(Wei Yongqiang, Zong Xiaoya, Jiang Zhiqiang, literary Zhenhua, Chen Liang thoroughbred horse multi-stage magnetic field straight tube Magnetic filters and pulse The compound arc ions electroplating method of bias, publication number:CN103276362A, publication date:On September 4th, 2013)Propose many The arc ions electroplating method that level magnetic field straight tube Magnetic filter is combined with pulsed bias, big is eliminated by multi-stage magnetic field filter Grain defect simultaneously lifts the efficiency of transmission of plasma, but the pollution problem of inside pipe wall and the loss of inside pipe wall plasma do not have It is well solved, later stage correlation scholar(Wei Yongqiang, Zong Xiaoya, Hou Junxing, Liu Yuan, Liu Xueshen, Jiang Zhiqiang, Accord with the multi-stage magnetic field arc ions electroplating method of pallid light liner positive bias straight tubes, publication number:CN105925940A, publication date: On September 7th, 2016)The multi-stage magnetic field arc ions electroplating method of liner positive bias straight tube is proposed to solve the pollution to inside pipe wall Problem.Also scholar(The cathodic arc plasma source and its film of Zhang Tao, Hou Junda, Liu Zhiguo, Zhang Yicong Magnetic filters Prepare [J] China Surface Engineering, 2002,02): 11-15+20-12.)The method for using for reference Bilek plates(Bilek M M M, Yin Y, McKenzie D R, Milne W I A M W I. Ion transport mechanisms in a filtered cathodic vacuum arc (FCVA) system [C]. Proceedings of the Discharges and Electrical Insulation in Vacuum, 1996 Proceedings ISDEIV, XVIIth International Symposium on, 1996: 962-966 vol.2), on 90 degree of bend pipes of bend pipe magnetic filter Apply positive bias to improve the efficiency of transmission of plasma.
The content of the invention
The invention aims to be the simple metal or multicomponent alloy for solving conventional arc ion electroplating method using low melting point Material and nonmetallic materials(Such as graphite)Bulky grain defect, flexure type Magnetic filter technology are also easy to produce as target cause electric arc etc. The low problem of gas ions efficiency of transmission, with reference to multi-stage magnetic field filter method and conical pipe own form mechanical stop shielding and just The compound action that biasing electric field attracts, while ensureing arc-plasma with efficiency of transmission higher by conical pipe and multistage magnetic Filter, allow workpiece surface the situation for applying back bias voltage it is continuous, fine and close prepare high-quality thin-film, while realize it is right Constituent content addition control, reduction use the production cost of alloys target, improve the deposition efficiency of film, reduce bulky grain in film Defect is to film growth and the adverse effect of performance, it is proposed that liner positive bias conical pipe and the compound multi-stage magnetic field electric arc of straight tube Ion electroplating method.
The inventive method institute use device includes grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field dress Put 4, multi-stage magnetic field power supply 5, liner positive bias conical pipe and straight tube set composite 6, positively biased voltage source 7, sample stage 8, bias plasma Source waveform oscillograph 9 and vacuum chamber 10;
The method is comprised the following steps:
On step one, the sample stage 8 that pending substrate work-piece is placed in vacuum chamber 10, liner positive bias conical pipe and straight tube are multiple Attach together and put insulation between 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect the negative pole output of grid bias power supply 1 End, arc ion plating target source 3 is arranged on vacuum chamber 10, connects the cathode output end of arc power 2, multi-stage magnetic field device 4 it is at different levels Magnetic field connects each output end of multi-stage magnetic field power supply 5, and both positive and negative polarity connection can be determined according to output magnetic direction, and liner is just Bias conical pipe and straight tube set composite 6 connect the cathode output end of positively biased voltage source 7, open outside water-cooling circulating system;
Step 2, thin film deposition:Vacuum chamber 10 is vacuumized, treats that the vacuum in vacuum chamber 10 is less than 10-4During Pa, work is passed through Make gas to 0.01Pa~10Pa, open grid bias power supply 1 and grid bias power supply kymographion 9, and adjust the output of grid bias power supply 1 Bias amplitude, pulse frequency and pulse width, the peak voltage of the output pulse of grid bias power supply 1 is 0~1.2kV, pulse frequency It is 0Hz~80kHz, pulse width 1 ~ 90%;
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, what regulation needed Technological parameter, the current value of the output of arc power 2 is 10 ~ 300A, and multi-stage magnetic field device 4 is adjusted by multi-stage magnetic field power supply 5, is kept Arc-plasma is produced in the stabilization of arc ion plating target source 3 and carries out filtering elimination to bulky grain defect, makes arc plasma Body reaches matrix surface with efficiency of transmission higher by multi-stage magnetic field device 4, carries out the fast deposition of film, arc ion plating Target source 3 and multi-stage magnetic field device 4 avoid the temperature in the course of work from raising problem by water-cooling pattern;
Positively biased voltage source 7 is opened, direct current positive bias, adjustment output are kept to liner positive bias conical pipe and straight tube set composite 6 Voltage, makes liner positive bias conical pipe and straight tube set composite 6 attract bulky grain, and depositing ions are repelled, and subtracts Loss of few plasma in transmitting procedure in pipe, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner Positive bias conical pipe and straight tube set composite 6 can coordinate multi-stage magnetic field device 4 to design various structures and import and export layout, each pipe Between be connected by bolt and nut, be easy to disassemble assembling and cleaning pollutant;Liner positive bias conical pipe and straight tube are compound Activity insulation connection between device 6 and multi-stage magnetic field device 4, liner positive bias conical pipe and straight tube set composite 6 can regard table Face pollution level is dismantled cleaning and is installed in time, it is to avoid the inside pipe wall pollution of multi-stage magnetic field device 4 and difficult under linerless board status In the problem of cleaning, the length of liner positive bias conical pipe and straight tube set composite 6HLength with multi-stage magnetic field device 4 is identical, Internal diameter at liner positive bias conical pipe and the right side import of straight tube set composite 6D EnterIt is interior more than the external diameter in arc ion plating target source 3 Lining positive bias conical pipe and the internal diameter of the external diameter less than multi-stage magnetic field device 4 on the right side of straight tube set composite 6, liner positive bias taper Internal diameter at pipe and the left side outlet of straight tube set composite 6D Go outSelected according to different targets and technological parameter, at import Internal diameter change and the textural association of set composite with exit, it is possible to achieve the mechanical stop shielding to bulky grain, liner is just The material of bias conical pipe and straight tube set composite 6 may be selected 304 stainless steel materials of nonmagnetic, resistance to cleaning, can be according to taper The length and rigidity of pipe and straight tube set composite need to select suitable thickness, are processed according to actual design parameter;Positively biased The voltage parameter of voltage source 7 is 0 ~+200V, is DC voltage, bulky grain defect can be produced in deposition process and continued The attraction of stabilization, greatly reduces the probability that bulky grain reaches film surface by multi-stage magnetic field device 4.
The need for film preparation, adjusting related technological parameter carries out simple metal film, the change of different element ratios It is prepared by compound ceramic membrane, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
Advantages of the present invention:A. liner positive bias conical pipe and straight tube set composite can be to big by applying positive bias Particle is effectively attracted, and depositing ions are repelled, and reduces loss of the plasma in transmitting procedure in pipe, further Improve the efficiency of transmission of arc-plasma and the deposition velocity of film;B. multi-stage magnetic field filter can be by the magnetic line of force Ensure the high efficiency of transmission of arc-plasma, change the motion path of bulky grain defect to eliminate big in arc-plasma Grain defect;C. liner positive bias conical pipe and straight tube set composite can realize mechanical stop screen effect by own form, The motion path of bulky grain defect is limited to eliminate the bulky grain defect in arc-plasma;D. pulsed bias parameter is passed through It is adjusted, including amplitude, pulse width and frequency are realized to the regulation of arc-plasma energy and the bulky grain to remaining Defect is eliminated;E. the microstructure and properties of prepared film can be adjusted by pulsed bias parameter, using arteries and veins Amplitude, pulse width and the frequency for rushing bias realize the pinning effect that energetic ion grows to film, improve the crystalline substance of film growth Body tissue and stress state, improve bond strength;F. prepared film avoids bulky grain defect, and film crystal tissue is more Plus it is fine and close, can further improve the mechanical property of film.
Step 3, can combine using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulse Cathode arc carries out thin film deposition to prepare simple metal film, difference with the compound bias of Dc bias, pulsed bias or DC pulse The compound ceramic film of element ratio, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
Brief description of the drawings
Fig. 1 is the liner positive bias conical pipe of multi-stage magnetic field arc ion plating of the present invention and a kind of dress of straight tube set composite With sketch;Fig. 2 is 4 kinds of typical structure sketches of liner positive bias conical pipe and straight tube set composite.
Specific embodiment
Specific embodiment one:Present embodiment, present embodiment liner positive bias taper are illustrated with reference to Fig. 1 and 2 The multi-stage magnetic field arc ions electroplating method institute use device that pipe and straight tube are combined includes grid bias power supply 1, arc power 2, arc ions Plating target source 3, multi-stage magnetic field device 4, multi-stage magnetic field power supply 5, liner positive bias conical pipe and straight tube set composite 6, positively biased piezoelectricity Source 7, sample stage 8, grid bias power supply kymographion 9 and vacuum chamber 10;
The method is comprised the following steps:
On step one, the sample stage 8 that pending substrate work-piece is placed in vacuum chamber 10, liner positive bias conical pipe and straight tube are multiple Attach together and put insulation between 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect the negative pole output of grid bias power supply 1 End, arc ion plating target source 3 is arranged on vacuum chamber 10, connects the cathode output end of arc power 2, multi-stage magnetic field device 4 it is at different levels Magnetic field connects each output end of multi-stage magnetic field power supply 5, and both positive and negative polarity connection can be determined according to output magnetic direction, and liner is just Bias conical pipe and straight tube set composite 6 connect the cathode output end of positively biased voltage source 7, open outside water-cooling circulating system;
Step 2, thin film deposition:Vacuum chamber 10 is vacuumized, treats that the vacuum in vacuum chamber 10 is less than 10-4During Pa, work is passed through Make gas to 0.01Pa~10Pa, open grid bias power supply 1 and grid bias power supply kymographion 9, and adjust the output of grid bias power supply 1 Bias amplitude, pulse frequency and pulse width, the peak voltage of the output pulse of grid bias power supply 1 is 0~1.2kV, pulse frequency It is 0Hz~80kHz, pulse width 1 ~ 90%;
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, what regulation needed Technological parameter, the current value of the output of arc power 2 is 10 ~ 300A, and multi-stage magnetic field device 4 is adjusted by multi-stage magnetic field power supply 5, is kept Arc-plasma is produced in the stabilization of arc ion plating target source 3 and carries out filtering elimination to bulky grain defect, makes arc plasma Body reaches matrix surface with efficiency of transmission higher by multi-stage magnetic field device 4, carries out the fast deposition of film, arc ion plating Target source 3 and multi-stage magnetic field device 4 avoid the temperature in the course of work from raising problem by water-cooling pattern;
Positively biased voltage source 7 is opened, and liner positive bias conical pipe and straight tube set composite 6 keep direct current positive bias, adjustment output electricity Pressure, makes liner positive bias conical pipe and straight tube set composite 6 attract bulky grain, and depositing ions are repelled, and reduces Loss of the plasma in transmitting procedure in pipe, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner is just Bias conical pipe and straight tube set composite 6 can coordinate multi-stage magnetic field device 4 to design various structures and import and export layout, respectively manage it Between be connected by bolt and nut, be easy to disassemble assembling and cleaning pollutant;Liner positive bias conical pipe and the compound dress of straight tube To put 6 can realize quickly removing and installing, it is to avoid the inside pipe wall pollution cleaning of multi-stage magnetic field device 4 asks under linerless board status Topic, the internal diameter at liner positive bias conical pipe and the right side import of straight tube set composite 6D EnterIt is outer more than arc ion plating target source 3 The internal diameter of the external diameter less than multi-stage magnetic field device 4 on footpath, liner positive bias conical pipe and the right side of straight tube set composite 6, liner positively biased Internal diameter at pressure conical pipe and the left side outlet of straight tube set composite 6D Go outSelected according to different targets and technological parameter, passed through The internal diameter ratio change at import and exit and the textural association of set composite, it is possible to achieve to the mechanical stop screen of bulky grain Cover, the material of liner positive bias conical pipe and straight tube set composite 6 may be selected 304 stainless steel materials of nonmagnetic, resistance to cleaning, can Length and rigidity according to conical pipe and straight tube set composite need to select suitable thickness, are according to the processing of actual design parameter Can;The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is DC voltage, and bulky grain defect can be produced in deposition process The continual and steady attraction of life, greatly reduces probability of the bulky grain by multi-stage magnetic field device 4.
The output waveform of grid bias power supply 1 is direct current, pulse, DC pulse is compound or multiple-pulse is compound.
The output of arc power 2 direct current, pulse, DC pulse are compound or multiple-pulse is compound.
Arc ion plating target source 3 is using high-melting-point or the simple metal or multicomponent alloy material of low melting point, it is possible to use single Target, multiple target or composition target, carry out simple metal film, the compound ceramic film of different element ratios, function film, polynary many Layer, superlattices, the high-quality thin-film with nanometer multilayer or gradient-structure.
Working gas selects argon gas, or working gas from one or more in nitrogen, acetylene, methane, silane or oxygen Mixed gas prepare simple metal film, the compound ceramic film of different element ratio, function film, multi-component multi-layer, super Lattice, the film with nanometer multilayer or gradient-structure.
The proposition of liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, can be in conical pipe Bulky grain is attracted using the positive bias for applying with straight tube set composite, is prevented effectively from big produced by low melting material Particle issues;Depositing ions are repelled simultaneously, reduces loss of the plasma in transmitting procedure in pipe, improve plasma The efficiency of transmission of body and the deposition velocity of film;Liner positive bias conical pipe and straight tube set composite pass through textural association and outlet The internal diameter at placeD Go outRegulation, it is possible to achieve the mechanical stop shielding to bulky grain defect, reduces bulky grain and reaches heavy by exit The probability of product sample surfaces;Liner positive bias conical pipe and straight tube set composite can realize quickly removing and installing, it is to avoid nothing The problem of the inside pipe wall pollution cleaning of multi-stage magnetic field device under liner plate state;Apply on workpiece back bias voltage parameter by adjusting, Be conducive to improving the interval Potential Distributing of plasma between target base, fully attract compound plasma to workpiece motion s, realize The fast deposition of film;Simultaneously also using the metallic plasma that the stable lasting, ionization level of generation of arc ion plating (aip) is high, Be conducive to ionization level ion high in the chemosynthesis reaction of workpiece surface, prepare different element ratios compound ceramic film, Function film, multi-component multi-layer, superlattices and the film with gradient-structure or simple metal film.
Specific embodiment two:Present embodiment is that the method also includes with the difference of implementation method one:
Step 3, can combine using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulsed cathode Arc carries out thin film deposition to prepare simple metal film, different elements with the compound bias of Dc bias, pulsed bias or DC pulse The compound ceramic film of ratio, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
Specific embodiment three:Present embodiment is with the difference of implementation method two, perform repeatedly step one to Step 3, prepares the multilayer films with different stress, microstructure and element ratio, other and implementation method two It is identical.
Specific embodiment four:Present embodiment is with the difference of implementation method one, perform repeatedly step one to Step 3, prepares the multilayer films with different stress, microstructure and element ratio, other and implementation method two It is identical.
2 sets or arc ion plating target source 3, multi-stage magnetic field device 4 and the liner positively biased of the above can be used in step 2 The liner positive bias conical pipe and the compound multi-stage magnetic field arc ion plating side of straight tube of pressure conical pipe and the combination of straight tube set composite 6 Method carries out the thin film deposition with various simple metal elements and multicomponent alloy material as target, then carries out step 3, then repeatedly Step 2 and step 3 are performed, so repeatedly, the sandwich construction with different stress, microstructure and element ratio is prepared Film.

Claims (7)

1. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe and straight tube are combined, it is characterised in that the method institute Use device includes grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field device 4, multi-stage magnetic field power supply 5, interior Lining positive bias conical pipe and straight tube set composite 6, positively biased voltage source 7, sample stage 8, grid bias power supply kymographion 9 and vacuum chamber 10;
The method is comprised the following steps:
On step one, the sample stage 8 that pending substrate work-piece is placed in vacuum chamber 10, liner positive bias conical pipe and straight tube are multiple Attach together and put insulation between 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect the negative pole output of grid bias power supply 1 End, arc ion plating target source 3 is arranged on vacuum chamber 10, connects the cathode output end of arc power 2, multi-stage magnetic field device 4 it is at different levels Magnetic field connects each output end of multi-stage magnetic field power supply 5, and both positive and negative polarity connection can be determined according to output magnetic direction, and liner is just Bias conical pipe and straight tube set composite 6 connect the cathode output end of positively biased voltage source 7, open outside water-cooling circulating system;
Step 2, thin film deposition:Vacuum chamber 10 is vacuumized, treats that the vacuum in vacuum chamber 10 is less than 10-4During Pa, work is passed through Gas opens grid bias power supply 1 and grid bias power supply kymographion 9, and adjust the inclined of the output of grid bias power supply 1 to 0.01Pa~10Pa Pressure amplitude value, pulse frequency and pulse width, the peak voltage of the output pulse of grid bias power supply 1 is 0~1.2kV, and pulse frequency is 0Hz~80kHz, pulse width 1 ~ 90%;
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, what regulation needed Technological parameter, the current value of the output of arc power 2 is 10 ~ 300A, and multi-stage magnetic field device 4 is adjusted by multi-stage magnetic field power supply 5, is kept Arc-plasma is produced in the stabilization of arc ion plating target source 3 and carries out filtering elimination to bulky grain defect, makes arc plasma Body reaches matrix surface with efficiency of transmission higher by multi-stage magnetic field device 4, carries out the fast deposition of film, arc ion plating Target source 3 and multi-stage magnetic field device 4 avoid the temperature in the course of work from raising problem by water-cooling pattern;
Positively biased voltage source 7 is opened, direct current positive bias, adjustment output are kept to liner positive bias conical pipe and straight tube set composite 6 Voltage, makes liner positive bias conical pipe and straight tube set composite 6 attract bulky grain, and depositing ions are repelled, and subtracts Loss of few plasma in transmitting procedure in pipe, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner Positive bias conical pipe and straight tube set composite 6 can coordinate multi-stage magnetic field device 4 to design various structures and import and export layout, each pipe Between be connected by bolt and nut, be easy to disassemble assembling and cleaning pollutant;Liner positive bias conical pipe and straight tube are compound Activity insulation connection between device 6 and multi-stage magnetic field device 4, liner positive bias conical pipe and straight tube set composite 6 can regard table Face pollution level is dismantled cleaning and is installed in time, it is to avoid the inside pipe wall pollution of multi-stage magnetic field device 4 and difficult under linerless board status In the problem of cleaning, the length of liner positive bias conical pipe and straight tube set composite 6HLength with multi-stage magnetic field device 4 is identical, Internal diameter at liner positive bias conical pipe and the right side import of straight tube set composite 6D EnterIt is interior more than the external diameter in arc ion plating target source 3 Lining positive bias conical pipe and the internal diameter of the external diameter less than multi-stage magnetic field device 4 on the right side of straight tube set composite 6, liner positive bias taper Internal diameter at pipe and the left side outlet of straight tube set composite 6D Go outSelected according to different targets and technological parameter, at import Internal diameter change and the textural association of set composite with exit, it is possible to achieve the mechanical stop shielding to bulky grain, liner is just The material of bias conical pipe and straight tube set composite 6 may be selected 304 stainless steel materials of nonmagnetic, resistance to cleaning, can be according to taper The length and rigidity of pipe and straight tube set composite need to select suitable thickness, are processed according to actual design parameter;Positively biased The voltage parameter of voltage source 7 is 0 ~+200V, is DC voltage, bulky grain defect can be produced in deposition process and continued The attraction of stabilization, greatly reduces the probability that bulky grain reaches film surface by multi-stage magnetic field device 4.
2. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, the method institute use device also includes that grid bias power supply kymographion 9 is used to show the arteries and veins that grid bias power supply 1 sends Voltage and current waveform is rushed, by adjusting the output waveform of grid bias power supply 1, effective attraction is carried out to plated film ion, carried out thin The deposition and control deposition targets of film ratio in the film, realize the regulation of plasma energy.
3. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, grid bias power supply 1 is exported, pulse is pulse, DC pulse is compound or multiple-pulse is compound.
4. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, the method can singly cover or set combination prepares simple metal film, the compound ceramic of different element ratios more Film, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
5. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, the method also includes:
Step 3, can combine using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulsed cathode Arc carries out thin film deposition to prepare simple metal film, different elements with the compound bias of Dc bias, pulsed bias or DC pulse The compound ceramic film of ratio, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
6. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, performing step one repeatedly to step 2, using 2 sets or cover the system to prepare simple metal film, different units more The compound ceramic film of plain ratio, function film and the high-quality thin-film with nanometer multilayer or gradient-structure.
7. the multi-stage magnetic field arc ions electroplating method that liner positive bias conical pipe according to claim 1 and straight tube are combined, Characterized in that, working gas selects argon gas, or working gas from a kind of or many in nitrogen, acetylene, methane, silane or oxygen Kind mixed gas prepare simple metal film, the compound ceramic film of different element ratio, function film and with nanometer The high-quality thin-film of multilayer or gradient-structure.
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CN111748777B (en) * 2020-06-08 2022-07-15 季华实验室 Variable-angle variable-diameter magnetic filtration cathode arc film deposition equipment and method
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