CN106637096B - The multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle - Google Patents

The multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle Download PDF

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CN106637096B
CN106637096B CN201710052985.6A CN201710052985A CN106637096B CN 106637096 B CN106637096 B CN 106637096B CN 201710052985 A CN201710052985 A CN 201710052985A CN 106637096 B CN106637096 B CN 106637096B
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film
arc
magnetic field
porous type
positive bias
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CN106637096A (en
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魏永强
宗晓亚
刘学申
刘源
侯军兴
张华阳
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
    • C23C14/325Electric arc evaporation

Abstract

The multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle, belong to technical field of material surface treatment, the present invention is the loss solved the problems, such as in bulky grain and depositing ions pollute inside pipe wall in multi-stage magnetic field filter device cleaning and arc-plasma transmission process.The method of the present invention includes: one, workpiece to be coated is placed on the indoor sample stage of vacuum, connects line related, opens external water cooling system;Two, film deposits: to the indoor vacuum degree of vacuum less than 10‑4When 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 carries out energy adjustment, bulky grain defect is effectively eliminated by the filtering effect of the blocking shielding of liner positive bias porous type retaining device itself and positively biased piezoelectric field inhibiting effect and multi-stage magnetic field and guarantees the efficiency of transmission of arc-plasma, required technological parameter is set, film preparation is carried out.

Description

The multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle
Technical field
The present invention relates to the multi-stage magnetic field arc ions electroplating methods of liner positive bias porous type baffle, belong at material surface Manage technical field.
Background technique
During arc ion plating prepares film, since arc spot current density is up to 2.5 ~ 5 × 1010A/m2, cause There is the liquid metal melted at the arc spot position of target material surface, under the action of local plasma pressure in droplets Splash comes out, and is attached to film surface or inlays formation " bulky grain " (Macroparticles) defect (Boxman in the film 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, since the movement velocity of electronics is far longer than the movement velocity of ion, big is reached in the unit time The electron number on grain surface is greater than number of ions, makes bulky grain that elecrtonegativity be presented.It is the thin of micron or sub-micron relative to thickness rank Film, size is in 0.1-10 microns of bulky grain defect just as PM2.5 is to the quality and property the pollution of air quality, to film There can be serious harm.With thin-film material and thin film technique apply it is increasingly extensive, 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.
Currently, in order to solve arc ions electroplating method using low melting point pure metal or multicomponent alloy material be also easy to produce greatly Grain defect problem, it is main at present that bulky grain is filtered out using the method for Magnetic filter, as Chinese patent is used for material surface modifying Plasma immersion and ion implantation device (publication number: CN1150180, publication date: on May 21st, 1997) in use 90 ° Magnetic filter is filtered 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 of He'nan University etc. (the filtered cathode arc plasma such as Zhang Yujuan, Wu Zhiguo, Zhang Weiwei prepares TiAlN thin film Middle sedimentary condition to film texture influence China YouSe Acta Metallurgica Sinica 2004,14 (8): 1264-1268.) in article Middle " S " magnetic filter that made is filtered the bulky grain of cathode arc, and there are 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 that proposes Magnetic filter, although these methods have certain effect, the efficiency of transmission damage of plasma in terms of filtering and eliminating bulky grain It loses seriously, substantially reduces ion current density.Based on that can filter on the basis of bulky grain can guarantee efficiency again, Chinese patent is true The side of straight tube filtering is proposed in empty cathode arc straight filter (publication number: CN1632905, publication date: on June 29th, 2005) Method, but which in turn reduces filter effects.In short, relevant researcher is by comparing various Magnetic filter method (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.) find arc ion plating plasma by keeping after magnetic filter High efficiency of transmission and elimination bulky grain is very difficult to take into account, and drastically influences application of the technology in high-quality thin-film deposition. In addition the electric field suppressing method of bias is used on matrix, when applying back bias voltage on matrix, electric field will be to electronegative big Grain generates 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.) use pulse Bias replaces traditional Dc bias, forms 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 substrate temperature mistake caused by Traditional DC bias High, the problems such as stress in thin films is larger.Woods Guoqiang of Dalian University of Technology et al. be (Lin Guoqiang pulsed bias arc ion plating Process ba- sis studies [D] Dalian University of Technology, and 2008. and Huang Meidong, Lin Guoqiang, Dong Chuan, Sun Chao, it is inclined to hear immediately Press Influencing Mechanism [J] Acta Metallurgica Sinica to arc ion plating film surface appearance, 2003,39 (5): 510-515.) needle The mechanism of bulky grain defect reduction is caused to conduct in-depth analysis pulsed bias, 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, big for reducing film surface Grain defect counts, improve the quality of film, are widely used in actual production, but cannot still completely eliminate bulky grain and lack It falls into.Domestic scholars (Wei Yongqiang, Zong Xiaoya, Jiang Zhiqiang, Wen Zhenhua, Chen Liangji multi-stage magnetic field straight tube Magnetic filter and pulse The compound arc ions electroplating method of bias, publication number: CN103276362A, publication date: on September 4th, 2013) propose it is more Grade magnetic field straight tube Magnetic filter and the compound arc ions electroplating method of pulsed bias, big is eliminated by multi-stage magnetic field filter device Grain defect and the efficiency of transmission for promoting 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 period correlation scholar (Wei Yongqiang, Zong Xiaoya, Hou Junxing, Liu Yuan, Liu Xueshen, Jiang Zhiqiang, The multi-stage magnetic field arc ions electroplating method of pallid light liner positive bias straight tube is accorded with, 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.There are also scholars to propose method (Zhao Y, Lin G, Xiao J, Lang W, the Dong C, Gong of dual-layered baffle plate J, Sun C. Synthesis of titanium nitride thin films deposited by a new Shielded arc ion plating [J] Appl Surf Sci, 2011,257 (13): 5694-5697.), research Affecting laws of the baffle spacing to film surface appearance, bulky grain elimination effect and deposition rate.There are also scholar (Zhang Tao, marquis Monarch reaches, Liu Zhiguo, the cathodic arc plasma source and its film preparation [J] China Surface Engineering of Zhang Yicong Magnetic filter, 2002,02): 11-15+20-12.) use for reference Bilek plate method (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), apply positive bias on the bend pipe of 90 degree of bend pipe magnetic filters to improve the transmission effect of plasma Rate.
Summary of the invention
The invention aims to the pure metal or multicomponent alloy of low melting point are used for solution conventional arc ion electroplating method Material and nonmetallic materials (such as graphite) are as target is also easy to produce bulky grain defect, flexure type Magnetic filter technology causes electric arc etc. It gas ions the problems such as transmission efficiency is low, is shielded in conjunction with the mechanical stop of multi-stage magnetic field filter method and porous type baffle self structure And the compound action that positively biased piezoelectric field attracts, while guaranteeing that arc-plasma passes through porous type baffle with higher efficiency of transmission With multi-stage magnetic field filter device, allow workpiece surface it is continuous the case where applying back bias voltage, it is fine and close prepare high-quality thin-film, together Shi Shixian adds control to constituent content in film, the deposition efficiency for reducing the production cost using alloys target, improving film, subtracts Few bulky grain defect is grown to film and the adverse effect of performance, proposes the multi-stage magnetic field electricity of liner positive bias porous type baffle Arc ion electroplating method.
The method of the present invention institute use device includes grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field dress Set 4, multi-stage magnetic field power supply 5, liner positive bias porous type retaining device 6, positively biased voltage source 7, sample stage 8, grid bias power supply waveform Oscillograph 9 and vacuum chamber 10;
Method includes the following steps:
Step 1: substrate work-piece to be processed is placed on the sample stage 8 in vacuum chamber 10, liner positive bias porous type baffle It insulating between device 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect the cathode output end of grid bias power supply 1, Arc ion plating target source 3 is mounted on vacuum chamber 10, connects the cathode output end of arc power 2, the magnetic fields at different levels of multi-stage magnetic field device 4 Each output end of multi-stage magnetic field power supply 5 is connect, positive and negative anodes connection can be determined according to output magnetic direction, liner positive bias Porous type retaining device 6 connects the cathode output end of positively biased voltage source 7, opens external water-cooling circulating system;
Step 2: film deposits: vacuum chamber 10 being vacuumized, to the vacuum degree in vacuum chamber 10 less than 10-4When Pa, it is passed through Working gas opens grid bias power supply 1 and grid bias power supply kymographion 9 to 0.01Pa~10Pa, and adjusts the output of grid bias power supply 1 Bias amplitude, pulse frequency and pulse width, the peak voltage that grid bias power supply 1 exports pulse is 0~1.2kV, pulse frequency Rate 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, adjusting needs The technological parameter wanted, the current value that arc power 2 exports are 10 ~ 300A, adjust multi-stage magnetic field device 4 by multi-stage magnetic field power supply 5, It keeps arc-plasma to stablize generation in arc ion plating target source 3 and be filtered elimination to bulky grain defect, makes electric arc etc. Gas ions reach matrix surface by multi-stage magnetic field device 4 with higher efficiency of transmission, carry out the fast deposition of film, electric arc from Son plates target source 3 and multi-stage magnetic field device 4 and avoids the temperature in the course of work from increasing problem by water-cooling pattern;
Positively biased voltage source 7 is opened, direct current positive bias, adjustment output electricity are kept to liner positive bias porous type retaining device 6 Pressure, attracts liner positive bias porous type retaining device 6 to bulky grain, repels to depositing ions, reduces plasma Loss of the body in pipe in transmission process, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias is more Pass retaining device 6 can cooperate type, the spacing of size and baffle in hole on the design baffle of multi-stage magnetic field device 4, and baffle is logical It crosses to be bolted and carry out position using nut and fix, convenient for dismantling assembling and cleaning pollutant;Liner positive bias porous type gear Activity insulation is assembled together between panel assembly 6 and multi-stage magnetic field device 4, and liner positive bias porous type retaining device 6 can regard Surface pollution degree dismantle in time cleaning and installation, avoid multi-stage magnetic field device 4 under linerless board status inside pipe wall pollution and It is difficult to the problem of clearing up, the perforated baffle spacing of liner positive bias porous type retaining device 6 and the magnetic at different levels of multi-stage magnetic field device 4 Field length matches, and the outer diameter of 6 perforated baffle of liner positive bias porous type retaining device is slightly less than the interior of multi-stage magnetic field device 4 Diameter;Pore size, type in 6 perforated baffle of liner positive bias porous type retaining device according to different targets and technological parameter into Row selection, passes through pore size in 6 perforated baffle of liner positive bias porous type retaining device, Change of types and baffle at different levels The mechanical stop shielding to bulky grain may be implemented in structure combination;The material of liner positive bias porous type retaining device 6 may be selected 304 stainless steel materials of nonmagnetic, resistance to cleaning can select suitable thickness, the size in aperture, type and gear at different levels as needed The topology layout of plate is processed according to actual design parameter;The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is direct current Voltage can generate continual and steady attraction to bulky grain defect during the deposition process, greatly reduce bulky grain and pass through multistage magnetic The probability of the arrival film surface of field device 4.
According to the needs of film preparation, the change that relevant technological parameter carries out pure metal film, different element ratios is adjusted It closes object ceramic membrane, function film and is prepared with the high-quality thin-film of nanometer multilayer or gradient-structure.
Advantages of the present invention: a. liner positive bias porous type retaining device by apply positive bias can to bulky grain into Row effectively attracts, and repels to depositing ions, reduces loss of the plasma in pipe in transmission process, further increases electricity The efficiency of transmission of arc plasma and the deposition velocity of film;B. multi-stage magnetic field filter device can guarantee electricity by the magnetic line of force The high efficiency of transmission of arc plasma changes the motion path of bulky grain defect and lacks to eliminate the bulky grain in arc-plasma It falls into;C. liner positive bias porous type retaining device can realize mechanical stop screen effect by self structure, limit bulky grain The motion path of defect eliminates the bulky grain defect in arc-plasma;D. it is adjusted, is wrapped by pulsed bias parameter Amplitude, pulse width and frequency is included to realize to the adjusting of arc-plasma energy and disappear to remaining bulky grain defect It removes;E. the microstructure and properties of prepared film can be adjusted by pulsed bias parameter, utilize the width of pulsed bias Value, pulse width and frequency realize the pinning effect that energetic ion grows film, improve the texture of film growth and answer Power state improves bond strength;F. prepared film avoids bulky grain defect, and film crystal tissue is finer and close, can be with Further increase the mechanical property of film.
Step 3: can be in conjunction with using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulse Cathode arc and Dc bias, pulsed bias or the compound bias of DC pulse carry out film deposition, to prepare pure metal film, difference Compound ceramic film, function film and the high-quality thin-film with nanometer multilayer or gradient-structure of element ratio.
Detailed description of the invention
Fig. 1 is the scheme of erection of the liner positive bias porous type retaining device of multi-stage magnetic field arc ion plating of the present invention;Fig. 2 It is the structure and 4 kinds of exemplary porous baffle schematic diagrams of liner positive bias porous type retaining device.
Specific embodiment
Specific embodiment 1: illustrating that present embodiment, present embodiment liner positive bias are porous below with reference to Fig. 1 and 2 The multi-stage magnetic field arc ions electroplating method institute use device of type baffle 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, liner positive bias porous type retaining device 6, positively biased voltage source 7, sample stage 8, Grid bias power supply kymographion 9 and vacuum chamber 10;
Method includes the following steps:
Step 1: substrate work-piece to be processed is placed on the sample stage 8 in vacuum chamber 10, liner positive bias porous type baffle It insulating between device 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect the cathode output end of grid bias power supply 1, Arc ion plating target source 3 is mounted on vacuum chamber 10, connects the cathode output end of arc power 2, the magnetic fields at different levels of multi-stage magnetic field device 4 Each output end of multi-stage magnetic field power supply 5 is connect, positive and negative anodes connection can be determined according to output magnetic direction, liner positive bias Porous type retaining device 6 connects the cathode output end of positively biased voltage source 7, opens external water-cooling circulating system;
Step 2: film deposits: vacuum chamber 10 being vacuumized, to the vacuum degree in vacuum chamber 10 less than 10-4When Pa, it is passed through Working gas opens grid bias power supply 1 and grid bias power supply kymographion 9 to 0.01Pa~10Pa, and adjusts the output of grid bias power supply 1 Bias amplitude, pulse frequency and pulse width, the peak voltage that grid bias power supply 1 exports pulse is 0~1.2kV, pulse frequency Rate 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, adjusting needs The technological parameter wanted, the current value that arc power 2 exports are 10 ~ 300A, adjust multi-stage magnetic field device 4 by multi-stage magnetic field power supply 5, It keeps arc-plasma to stablize generation in arc ion plating target source 3 and be filtered elimination to bulky grain defect, makes electric arc etc. Gas ions reach matrix surface by multi-stage magnetic field device 4 with higher efficiency of transmission, carry out the fast deposition of film, electric arc from Son plates target source 3 and multi-stage magnetic field device 4 and avoids the temperature in the course of work from increasing problem by water-cooling pattern;
Positively biased voltage source 7 is opened, and liner positive bias porous type retaining device 6 keeps direct current positive bias, adjusts output voltage, Attract liner positive bias porous type retaining device 6 to bulky grain, depositing ions are repelled, reduces plasma and exist Loss in managing in transmission process, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias porous type Retaining device 6 can cooperate type, the spacing of size and baffle in hole on the design baffle of multi-stage magnetic field device 4, and baffle passes through spiral shell It tethers to connect and carry out position using nut and fix, convenient for dismantling assembling and cleaning pollutant;Liner positive bias porous type baffle dress It sets activity insulation between 6 and multi-stage magnetic field device 4 to be assembled together, liner positive bias porous type retaining device 6 can be with apparent surface Pollution level dismantles cleaning and installation in time, avoids the inside pipe wall pollution of multi-stage magnetic field device 4 under linerless board status and is difficult to The problem of cleaning, the perforated baffle spacing of liner positive bias porous type retaining device 6 and the magnetic fields at different levels of multi-stage magnetic field device 4 are long Degree matches, and the outer diameter of 6 perforated baffle of liner positive bias porous type retaining device is slightly less than the internal diameter of multi-stage magnetic field device 4;It is interior Pore size, type in lining 6 perforated baffle of positive bias porous type retaining device are selected according to different targets and technological parameter It selects, passes through the structure of pore size, Change of types and baffle at different levels in 6 perforated baffle of liner positive bias porous type retaining device The mechanical stop shielding to bulky grain may be implemented in combination;The material of liner positive bias porous type retaining device 6 may be selected without magnetic Property, resistance to cleaning 304 stainless steel materials, suitable thickness, the size in aperture, type and baffle at different levels can be selected as needed Topology layout is processed according to actual design parameter;The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is direct current Pressure, can generate continual and steady attraction to bulky grain defect during the deposition process, greatly reduce bulky grain and pass through multi-stage magnetic field The probability of device 4.
1 output waveform of grid bias power supply is direct current, pulse, DC pulse is compound or multiple-pulse is compound.
The output of arc power 2 direct current, pulse, DC pulse is compound or multiple-pulse is compound.
Arc ion plating target source 3 can be used single using high-melting-point or the pure metal or multicomponent alloy material of low melting point Target, multiple targets or composition target carry out pure metal film, the compound ceramic film of different element ratio, function film, polynary more Layer, superlattices, the high-quality thin-film with nanometer multilayer or gradient-structure.
It is one or more in nitrogen, acetylene, methane, silane or oxygen that working gas selects argon gas or working gas to select Mixed gas, to prepare pure 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 it is proposed of the multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle can be filled in porous type baffle It sets the middle positive bias using application to attract bulky grain, effectively avoids bulky grain problem caused by low melting material;Together When depositing ions are repelled, reduce loss of the plasma between porous type baffle in transmission process, improve plasma Efficiency of transmission and film deposition velocity;The size in liner positive bias porous type retaining device aperture, Change of types and at different levels Structure combination between baffle may be implemented the mechanical stop shielding to bulky grain defect, reduce bulky grain and pass through porous type baffle The probability on device arrival deposited samples surface;Fast quick-detach installation may be implemented in liner positive bias porous type retaining device, avoids The inside pipe wall of multi-stage magnetic field device pollutes the problem of cleaning under linerless board status;By adjusting back bias voltage applied on workpiece ginseng Number, is conducive to the section Potential Distributing for improving plasma between target base, sufficiently attracts compound plasma to workpiece motion s, real The fast deposition of existing film;Also stablize metal plasma lasting, that ionization level is high using the generation of arc ion plating (aip) simultaneously Body is conducive to high ionization level ion in the chemosynthesis reaction of workpiece surface, and the compound ceramic for preparing different element ratios is thin Film, function film, multi-component multi-layer, superlattices and film or pure metal film with gradient-structure.
Specific embodiment 2: present embodiment and embodiment one the difference is that, this method further include:
Step 3: can be in conjunction with using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulse Cathode arc and Dc bias, pulsed bias or the compound bias of DC pulse carry out film deposition, to prepare pure metal film, difference Compound ceramic film, function film and the high-quality thin-film with nanometer multilayer or gradient-structure of element ratio.
Specific embodiment 3: present embodiment and embodiment two the difference is that, execute step 1 extremely repeatedly Step 3 prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment two It is identical.
Specific embodiment 4: present embodiment and embodiment one the difference is that, execute step 1 extremely repeatedly Step 3 prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment two It is identical.
2 sets or above arc ion plating target source 3, multi-stage magnetic field device 4 and liner positively biased can be used in step 2 The multi-stage magnetic field arc ions electroplating method for the liner positive bias porous type baffle for pressing porous type retaining device 6 combined is carried out with various Pure metal element and multicomponent alloy material are that the film of target deposits, and then carry out step 3, then execute repeatedly step 2 and Step 3 prepares the multilayer films with different stress, microstructure and element ratio repeatedly.

Claims (2)

1. the multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle, which is characterized in that this method uses dress It sets including 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), liner positive bias porous type retaining device (6), positively biased voltage source (7), sample stage (8), grid bias power supply kymographion (9) With vacuum chamber (10);
Method includes the following steps:
Step 1: substrate work-piece to be processed is placed on the sample stage (8) in vacuum chamber (10), liner positive bias porous type baffle It insulate between device (6) and vacuum chamber (10) and multi-stage magnetic field device (4), workpiece and sample stage (8) connect the negative of grid bias power supply (1) Pole output end, arc ion plating target source (3) are mounted on vacuum chamber (10), connect the cathode output end of arc power (2), multi-stage magnetic field The magnetic fields at different levels of device (4) connect each output end of multi-stage magnetic field power supply (5), and positive and negative anodes connection can be according to output magnetic direction It is determined, liner positive bias porous type retaining device (6) connects the cathode output end of positively biased voltage source (7), opens external water cooling The circulatory system;
Step 2: film deposits: vacuum chamber (10) being vacuumized, to the vacuum degree in vacuum chamber (10) less than 10-4When Pa, it is passed through Working gas opens grid bias power supply (1) and grid bias power supply kymographion (9) to 0.01Pa~10Pa, and adjusts grid bias power supply (1) the bias amplitude exported, pulse frequency and pulse width, grid bias power supply (1) export the peak voltage of pulse be 0~ 1.2kV, pulse frequency are 0Hz~80kHz, pulse width 1 ~ 90%, and grid bias power supply (1) output waveform is direct current, pulse, straight Stream pulse is compound or multiple-pulse is compound;
It opens arc power (2), the surface in arc ion plating target source (3) is cleaned by the spots moving of electric arc, adjusting needs The technological parameter wanted, arc ion plating target source (3) can be made using high-melting-point or the pure metal or multicomponent alloy material of low melting point With single target, multiple targets or composition target;Carry out pure metal film, the compound ceramic film of different element ratio, function film, Multi-component multi-layer, superlattices, the film with nanometer multilayer or gradient-structure;The current value of arc power (2) output is 10 ~ 300A, Arc power (2) output direct current, pulse, DC pulse is compound or multiple-pulse is compound;It is adjusted by multi-stage magnetic field power supply (5) multistage Magnetic field device (4) keeps arc-plasma to stablize in arc ion plating target source (3) and generates and be filtered to bulky grain defect It eliminates, so that arc-plasma is reached matrix surface by multi-stage magnetic field device (4) with higher efficiency of transmission, carry out film Fast deposition, arc ion plating target source (3) and multi-stage magnetic field device (4) avoid the temperature liter in the course of work by water-cooling pattern High problem;
It opens positively biased voltage source (7), direct current positive bias, adjustment output electricity is kept to liner positive bias porous type retaining device (6) Pressure, attract liner positive bias porous type retaining device (6) to bulky grain, depositing ions repelled, reduce etc. from Loss of the daughter in pipe in transmission process, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias Porous type retaining device (6) can cooperate type, the spacing of size and baffle in hole on multi-stage magnetic field device (4) design baffle, Baffle is bolted and carries out position using nut and fixes, convenient for dismantling assembling and cleaning pollutant;Liner positive bias is more Activity insulation is assembled together between pass retaining device (6) and multi-stage magnetic field device (4), liner positive bias porous type baffle dress Cleaning and installation can be dismantled in time with apparent surface pollution level by setting (6), avoid multi-stage magnetic field device (4) under linerless board status Inside pipe wall is polluted and is difficult to the problem of clearing up, the perforated baffle spacing of liner positive bias porous type retaining device (6) and multistage magnetic The length of magnetic field at different levels of field device (4) match, and the outer diameter of liner positive bias porous type retaining device (6) perforated baffle is slightly less than The internal diameter of multi-stage magnetic field device (4);Pore size, type root in liner positive bias porous type retaining device (6) perforated baffle It is selected according to different targets and technological parameter, passes through the aperture in liner positive bias porous type retaining device (6) perforated baffle The structure of size, Change of types and baffle at different levels combines, and the mechanical stop shielding to bulky grain may be implemented;Liner positive bias is more 304 stainless steel materials of nonmagnetic, resistance to cleaning may be selected in the material of pass retaining device (6), and it is suitable to select as needed The topology layout of thickness, the size in aperture, type and baffle at different levels is processed according to actual design parameter;Positively biased voltage source (7) voltage parameter is 0 ~+200V, is DC voltage, can be generated during the deposition process to bulky grain defect continual and steady Attraction, greatly reduce bulky grain by multi-stage magnetic field device (4) reach film surface probability;
The multi-stage magnetic field arc ions electroplating method institute use device of liner positive bias porous type baffle further includes grid bias power supply waveform Oscillograph (9) is used to show the pulse voltage and current waveform that grid bias power supply (1) issues, by adjusting the defeated of grid bias power supply (1) Waveform out effectively attracts plated film ion, carries out the ratio of the deposition and control deposition targets of film in the film, real The adjusting of existing plasma energy;
Liner positive bias porous type retaining device (6) can effectively attract bulky grain by applying positive bias, to deposition Ion is repelled, and is reduced loss of the plasma in pipe in transmission process, is further increased the transmission of arc-plasma The deposition velocity of efficiency and film;Multi-stage magnetic field filter device can guarantee the efficient biography of arc-plasma by the magnetic line of force It is defeated, change the motion path of bulky grain defect to eliminate the bulky grain defect in arc-plasma;Liner positive bias porous type Retaining device (6) can realize mechanical stop screen effect by self structure, limit the motion path of bulky grain defect to disappear Except the bulky grain defect in arc-plasma;It is adjusted by pulsed bias parameter, including amplitude, pulse width and frequency It realizes to the adjusting of arc-plasma energy and remaining bulky grain defect is eliminated;The microstructure of prepared film It can be adjusted by pulsed bias parameter with performance, realize high energy using the amplitude, pulse width and frequency of pulsed bias The pinning effect of ion pair film growth, improves the texture and stress state of film growth, improves bond strength;It is prepared Film avoid bulky grain defect, film crystal tissue is finer and close, can be further improved the mechanical property of film;
Step 3: can be in conjunction with using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating and pulsed cathode Arc and Dc bias, pulsed bias or the compound bias of DC pulse carry out film deposition, to prepare pure metal film, different elements Compound ceramic film, function film and the film with nanometer multilayer or gradient-structure of ratio;
Step 1 is executed repeatedly to step 2, and it is thin to prepare pure metal film, the compound ceramic film of different element ratios, function Film and film with nanometer multilayer or gradient-structure;
The multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle can be in porous type retaining device using applying The positive bias added attracts bulky grain, effectively avoids bulky grain problem caused by low melting material;Simultaneously to deposition from Son is repelled, and is reduced loss of the plasma between porous type baffle in transmission process, is improved the efficiency of transmission of plasma With the deposition velocity of film;Between the size in liner positive bias porous type retaining device (6) aperture, Change of types and baffle at different levels Structure combination may be implemented the mechanical stop shielding to bulky grain defect, reduce bulky grain and be reached by porous type retaining device The probability on deposited samples surface;Fast quick-detach installation may be implemented in liner positive bias porous type retaining device (6), avoids linerless The inside pipe wall of multi-stage magnetic field device (4) pollutes the problem of cleaning under board status;By adjusting back bias voltage parameter applied on workpiece, Be conducive to improve the section Potential Distributing of plasma between target base, sufficiently attract compound plasma to workpiece motion s, realize The fast deposition of film;Also stablize metallic plasma lasting, that ionization level is high using the generation of arc ion plating (aip) simultaneously, Be conducive to high ionization level ion in the chemosynthesis reaction of workpiece surface, prepare different element ratios compound ceramic film, Function film, multi-component multi-layer, superlattices and film or pure metal film with gradient-structure.
2. the multi-stage magnetic field arc ions electroplating method of liner positive bias porous type baffle according to claim 1, feature It is, working gas selects argon gas or working gas to select one or more in nitrogen, acetylene, methane, silane or oxygen mix Close gas, this method can singly cover or 2 sets or more arc ion plating target source (3), multi-stage magnetic field device (4) and liner just Bias porous type retaining device (6) combination liner positive bias porous type baffle multi-stage magnetic field arc ions electroplating method combine into Row is deposited using various pure metal elements and multicomponent alloy material as the film of target, then executes step 2 and step 3 repeatedly, Repeatedly, prepare pure metal film, the compound ceramic film of different element ratio, function film and have nanometer multilayer or The film of gradient-structure.
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