CN106676482B - Liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle - Google Patents

Liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle Download PDF

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CN106676482B
CN106676482B CN201710052993.0A CN201710052993A CN106676482B CN 106676482 B CN106676482 B CN 106676482B CN 201710052993 A CN201710052993 A CN 201710052993A CN 106676482 B CN106676482 B CN 106676482B
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film
magnetic field
arc
perforated baffle
ladder pipe
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CN106676482A (en
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魏永强
宗晓亚
陈小霞
侯军兴
张华阳
刘源
刘学申
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

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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)
  • Plasma Technology (AREA)

Abstract

Liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle, belong to technical field of material surface treatment, the present invention is to solve the problems, such as that bulky grain and depositing ions are to the loss in inside pipe wall pollution and arc-plasma transmission process in multi-stage magnetic field filter device.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, to effectively eliminate bulky grain defect and guarantee the efficiency of transmission of arc-plasma by the blocking shielding and positively biased piezoelectric field inhibiting effect of liner positive bias ladder pipe and perforated baffle hybrid device own form and structure combination and the filtering effect of multi-stage magnetic field, technological parameter is set, film preparation is carried out.

Description

Liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle
Technical field
The present invention relates to the compound multi-stage magnetic field arc ions electroplating methods of liner ladder pipe and perforated baffle, belong to material Technical field of surface.
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 is gas ions the problems such as transmission efficiency is low, compound in conjunction with multi-stage magnetic field filter method and liner positive bias ladder pipe and perforated baffle The compound action that the mechanical stop shielding and positively biased piezoelectric field of device own form and structure combination attract, while guaranteeing electric arc Plasma is compound by multi-stage magnetic field filter device and liner positive bias ladder pipe and perforated baffle with higher efficiency of transmission Type device, allow workpiece surface it is continuous the case where applying back bias voltage, it is fine and close prepare high-quality thin-film, while realizing to film Middle constituent content addition control, reduces bulky grain defect at the deposition efficiency for reducing the production cost using alloys target, improving film To the adverse effect of film growth and performance, liner ladder pipe and the compound multi-stage magnetic field arc ions of perforated baffle are proposed 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 ladder pipe and perforated baffle hybrid 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 ladder pipe and more It insulate between hole baffle hybrid device 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect grid bias power supply 1 Cathode 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 device 4 magnetic fields at different levels connect each output end of multi-stage magnetic field power supply 5, and positive and negative anodes connection can carry out true according to output magnetic direction Calmly, liner positive bias ladder pipe and perforated baffle hybrid device 6 connect the cathode output end of positively biased voltage source 7, open external water SAPMAC method 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 positively biased is kept to liner positive bias ladder pipe and perforated baffle hybrid device 6 Pressure adjusts output voltage, attracts liner positive bias ladder pipe and perforated baffle hybrid device 6 to bulky grain, to heavy Product ion is repelled, and loss of the plasma in pipe in transmission process is reduced, and improves the efficiency of transmission of plasma and thin The deposition velocity of film;Activity insulation between liner positive bias ladder pipe and perforated baffle hybrid device 6 and multi-stage magnetic field device 4 It is assembled together, liner positive bias ladder pipe and perforated baffle hybrid device 6 can be dismantled in time clearly with apparent surface pollution level Reason and installation avoid the inside pipe wall pollution of multi-stage magnetic field device 4 under linerless board status and are difficult to the problem of clearing up;Liner positively biased Press the ladder length of tube of ladder pipe and perforated baffle hybrid device 6HIdentical with the length of multi-stage magnetic field device 4, ladder pipe is right Internal diameter at side-entranceD IntoGreater than the outer diameter in arc ion plating target source 3, the outer diameter on right side is less than the internal diameter of multi-stage magnetic field device 4, Internal diameter at ladder pipe left side outletD OutIt is selected according to different targets and technological parameter, by entrance and exit The mechanical stop shielding to bulky grain may be implemented in diameter variation;The structure of ladder pipe can cooperate multi-stage magnetic field device 4 to design 2 The structure of grade ladder pipe, 3 grades of ladder pipes or 4 grades and the above ladder pipe, gradient difference and inlet and outlet are laid out, between every grade of ladder pipe It is connected and fixed by bolt and nut, convenient for dismantling assembling and cleaning pollutant;Liner positive bias ladder pipe and perforated baffle are compound Perforated baffle spacing in type device 6 is matched with the outlet of the length of magnetic field at different levels of multi-stage magnetic field device 4 and ladder pipe at different levels, Ladder pipe and perforated baffle by together with rivet assembly connection, perforated baffle can cooperate ladder pipe design baffle size, Baffle spacing and structure combination, baffle is bolted and carries out position using nut and fixes, convenient for dismantling assembling and cleaning Pollutant, the structure combination of pore size, type and baffle at different levels in perforated baffle according to different targets and technological parameter into Row selection;Nothing may be selected in the material of ladder pipe and perforated baffle in liner positive bias ladder pipe and perforated baffle hybrid device 6 304 stainless steel materials of magnetic, resistance to cleaning, ladder pipe need to select suitable thickness, perforated baffle root according to length and rigidity According to the topology layout of the size in aperture, type and baffle at different levels, processed according to actual design parameter;Positively biased voltage source 7 Voltage parameter is 0 ~+200V, is DC voltage, can generate continual and steady suction to bulky grain defect during the deposition process Draw, greatly reduces the probability that bulky grain reaches film surface by multi-stage magnetic 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 ladder pipe and perforated baffle hybrid device can by applying positive bias Effectively to be attracted bulky grain, depositing ions are repelled, reduce loss of the plasma in pipe in transmission process, Further increase the efficiency of transmission of arc-plasma and the deposition velocity of film;B. multi-stage magnetic field filter device can pass through The magnetic line of force guarantees the high efficiency of transmission of arc-plasma, changes the motion path of bulky grain defect to eliminate in arc-plasma Bulky grain defect;C. liner positive bias ladder pipe and perforated baffle hybrid device can pass through own form and structure group It closes and realizes mechanical stop screen effect, limit the motion path of bulky grain defect and lacked to eliminate the bulky grain in arc-plasma It falls into;D. it is adjusted by pulsed bias parameter, including amplitude, pulse width and frequency are realized to arc-plasma energy Adjusting and remaining bulky grain defect is eliminated;E. the microstructure and properties of prepared film can pass through pulse Bias parameters are adjusted, and realize the nail that energetic ion grows film using the amplitude, pulse width and frequency of pulsed bias Effect is pricked, the texture and stress state of film growth are improved, improves bond strength;F. prepared film avoids greatly 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 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 liner ladder pipe of multi-stage magnetic field arc ion plating of the present invention and a kind of dress of perforated baffle hybrid device With schematic diagram;Fig. 2 is the structure and dismantling schematic diagram of a kind of liner positive bias ladder pipe and perforated baffle hybrid device;Fig. 3 is 5 kinds Typical ladder pipe and composite structure schematic diagram;Fig. 4 is a kind of perforated baffle structure and 4 kinds of exemplary porous baffle schematic diagrams.
Specific embodiment
Specific embodiment 1: illustrating present embodiment, present embodiment liner below with reference to Fig. 1, Fig. 2, Fig. 3 and Fig. 4 Ladder pipe and the compound multi-stage magnetic field arc ions electroplating method institute use device of perforated baffle include 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 ladder pipe and perforated baffle are compound Type 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 ladder pipe and more It insulate between hole baffle hybrid device 6 and vacuum chamber 10 and multi-stage magnetic field device 4, workpiece and sample stage 8 connect grid bias power supply 1 Cathode 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 device 4 magnetic fields at different levels connect each output end of multi-stage magnetic field power supply 5, and positive and negative anodes connection can carry out true according to output magnetic direction Calmly, liner positive bias ladder pipe and perforated baffle hybrid device 6 connect the cathode output end of positively biased voltage source 7, open external water SAPMAC method 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 ladder pipe and perforated baffle hybrid device 6 keep direct current positive bias, Adjust output voltage, attract liner positive bias ladder pipe and perforated baffle hybrid device 6 to bulky grain, to deposition from Son is repelled, loss of the plasma in pipe in transmission process is reduced, and improves the efficiency of transmission and film of plasma Deposition velocity;Activity insulation assembly between liner positive bias ladder pipe and perforated baffle hybrid device 6 and multi-stage magnetic field device 4 Together, liner positive bias ladder pipe and perforated baffle hybrid device 6 can be dismantled in time with apparent surface pollution level cleaning and Installation avoids the inside pipe wall pollution of multi-stage magnetic field device 4 under linerless board status and is difficult to the problem of clearing up;Liner positive bias rank The ladder length of tube of ladder pipe and perforated baffle hybrid device 6HIt is identical with the length of multi-stage magnetic field device 4, on the right side of ladder pipe into Internal diameter at mouthfulD IntoGreater than the outer diameter in arc ion plating target source 3, the outer diameter on right side is less than the internal diameter of multi-stage magnetic field device 4, ladder Internal diameter at pipe left side outletD OutIt is selected according to different targets and technological parameter, is become by the internal diameter in entrance and exit Change, the mechanical stop shielding to bulky grain may be implemented;The structure of ladder pipe can cooperate multi-stage magnetic field device 4 to design 2 grades of ranks The structure of ladder pipe, 3 grades of ladder pipes or 4 grades and the above ladder pipe, gradient difference and inlet and outlet are laid out, and are passed through between every grade of ladder pipe Bolt and nut is connected and fixed, convenient for dismantling assembling and cleaning pollutant;Liner positive bias ladder pipe and the compound dress of perforated baffle The perforated baffle spacing set in 6 is matched with the outlet of the length of magnetic field at different levels of multi-stage magnetic field device 4 and ladder pipe at different levels, ladder For pipe together with perforated baffle is by rivet assembly connection, perforated baffle can cooperate the size of ladder pipe design baffle, baffle Spacing and structure combination, baffle is bolted and carries out position using nut and fixes, convenient for dismantling assembling and cleaning pollution The structure combination of object, pore size, type and baffle at different levels in perforated baffle is selected according to different targets and technological parameter It selects;In liner positive bias ladder pipe and perforated baffle hybrid device 6 material of ladder pipe and perforated baffle may be selected it is nonmagnetic, 304 stainless steel materials of resistance to cleaning, ladder pipe need to select suitable thickness according to length and rigidity, and perforated baffle is according to aperture Size, type and baffle at different levels topology layout, according to actual design parameter process;The voltage of positively biased voltage source 7 is joined Number is 0 ~+200V, is DC voltage, can generate continual and steady attraction to bulky grain defect during the deposition process, significantly Reduce the probability that bulky grain passes through multi-stage magnetic field 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 liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle, can be in ladder pipe Bulky grain is attracted with the positive bias in perforated baffle hybrid device using application, effectively low melting material is avoided to be produced Raw bulky grain problem;Depositing ions are repelled simultaneously, reduction plasma is in hybrid device in transmission process Loss, improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias ladder pipe and perforated baffle are compound Device passes through the knot between stairstepping pipe gradient difference and structure combination, the pore size of perforated baffle, Change of types and baffle at different levels Structure combination and the structure combination of hybrid device, may be implemented the mechanical stop shielding to bulky grain defect, it is logical to reduce bulky grain Cross the probability that hybrid device reaches deposited samples surface;Liner positive bias ladder pipe and perforated baffle hybrid device can be real Now fast quick-detach installation, the inside pipe wall for avoiding multi-stage magnetic field device under linerless board status pollute the problem of clearing up;By adjusting Applied back bias voltage parameter on workpiece is conducive to the section Potential Distributing for improving plasma between target base, sufficiently attracts compound Plasma realizes the fast deposition of film to workpiece motion s;While also being stablized using the generation of arc ion plating (aip) and being continued, The high metallic plasma of ionization level is conducive to high ionization level ion in the chemosynthesis reaction of workpiece surface, prepares different members The compound ceramic film of plain ratio, function film, multi-component multi-layer, superlattices and film with gradient-structure or pure metal are thin Film.
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 Press ladder pipe and the combined compound multi-stage magnetic field electric arc of liner ladder pipe and perforated baffle of perforated baffle hybrid device 6 from Sub- electroplating method deposit using various pure metal elements and multicomponent alloy material as the film of target, then carries out step 3, so Execute step 2 and step 3 repeatedly afterwards, repeatedly, preparing has the more of different stress, microstructure and element ratio Layer structural membrane.

Claims (2)

1. liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle, which is characterized in that this 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), liner positive bias ladder pipe and perforated baffle hybrid device (6), positively biased voltage source (7), sample stage (8), bias Power supply wave shape 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 ladder pipe and more It insulate between hole baffle hybrid device (6) and vacuum chamber (10) and multi-stage magnetic field device (4), workpiece and sample stage (8) connect partially The cathode output end of voltage source (1), arc ion plating target source (3) are mounted on vacuum chamber (10), and the cathode for connecing arc power (2) is defeated Outlet, the magnetic fields at different levels of multi-stage magnetic field device (4) connect each output end of multi-stage magnetic field power supply (5), and positive and negative anodes connection can be according to It is determined according to output magnetic direction, liner positive bias ladder pipe and perforated baffle hybrid device (6) connect positively biased voltage source (7) Cathode output end, open 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 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;
Open arc power (2), the surface in arc ion plating target source (3) is cleaned by the spots moving of electric arc, electric arc from Single target, multiple targets or multiple can be used using high-melting-point or the pure metal or multicomponent alloy material of low melting point in son plating target source (3) Target is closed, the technological parameter of needs is adjusted, the current value of arc power (2) output is 10 ~ 300A, exports direct current, pulse, direct current arteries and veins It is compound to rush compound or multiple-pulse;Multi-stage magnetic field device (4) are adjusted by multi-stage magnetic field power supply (5), arc-plasma is kept to exist Arc ion plating target source (3), which is stablized, to be generated and is filtered elimination to bulky grain defect, makes arc-plasma with higher biography Defeated efficiency reaches matrix surface 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) avoids the temperature in the course of work from increasing problem by water-cooling pattern;
It opens positively biased voltage source (7), direct current positively biased is kept to liner positive bias ladder pipe and perforated baffle hybrid device (6) Pressure adjusts output voltage, attracts liner positive bias ladder pipe and perforated baffle hybrid device (6) to bulky grain, right Depositing ions are repelled, and loss of the plasma in pipe in transmission process is reduced, improve plasma efficiency of transmission and The deposition velocity of film;It is living between liner positive bias ladder pipe and perforated baffle hybrid device (6) and multi-stage magnetic field device (4) Dynamic insulation is assembled together, liner positive bias ladder pipe and perforated baffle hybrid device (6) can with apparent surface pollution level and When disassembly cleaning and installation, avoid the inside pipe wall pollution of multi-stage magnetic field device (4) under linerless board status and be difficult to clear up ask Topic;The ladder length of tube of liner positive bias ladder pipe and perforated baffle hybrid device (6)HWith the length of multi-stage magnetic field device (4) Spend identical, the internal diameter of entrance on the right side of ladder pipeD IntoGreater than the outer diameter in arc ion plating target source (3), the outer diameter on right side is less than multistage The internal diameter of magnetic field device (4), the internal diameter at ladder pipe left side outletD OutIt is selected, is passed through according to different targets and technological parameter The mechanical stop shielding to bulky grain may be implemented in the variation of the internal diameter in entrance and exit;The structure of ladder pipe can cooperate Multi-stage magnetic field device (4) designs structure, gradient difference and the disengaging of 2 grades of ladder pipes, 3 grades of ladder pipes or 4 grades and the above ladder pipe Mouth is laid out, and is connected and fixed between every grade of ladder pipe by bolt and nut, convenient for dismantling assembling and clears up pollutant;Liner positive bias The length of magnetic field at different levels of perforated baffle spacing and multi-stage magnetic field device (4) in ladder pipe and perforated baffle hybrid device (6) Outlet with ladder pipes at different levels matches, and by together with rivet assembly connection, perforated baffle can be with for ladder pipe and perforated baffle Cooperate the size, baffle spacing and structure combination of ladder pipe design baffle, baffle is bolted and carries out position using nut Fixation is set, convenient for dismantling assembling and cleaning pollutant, the structure of pore size, type and baffle at different levels in perforated baffle is combined It is selected according to different targets and technological parameter;Ladder in liner positive bias ladder pipe and perforated baffle hybrid device (6) 304 stainless steel materials of nonmagnetic, resistance to cleaning may be selected in the material of pipe and perforated baffle, and ladder pipe is according to length and rigidity needs Suitable thickness is selected, perforated baffle is joined according to the topology layout of the size in aperture, type and baffle at different levels according to actual design Number processing;The voltage parameter of positively biased voltage source (7) is 0 ~+200V, is DC voltage, during the deposition process can be to big Grain defect generates continual and steady attraction, greatly reduces the machine that bulky grain reaches film surface by multi-stage magnetic field device (4) Rate;
Institute's use device further include grid bias power supply kymographion (9) be used for show grid bias power supply (1) issue pulse voltage and Current waveform effectively attracts plated film ion by adjusting the output waveform of grid bias power supply (1), carries out the heavy of film The ratio of product and control deposition targets in the film, realizes the adjusting of plasma energy;
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 high-quality thin-film with nanometer multilayer or gradient-structure of ratio;
Step 1 is executed repeatedly to step 2, using 2 sets or cover the system to prepare pure metal film, difference element ratio more Compound ceramic film, function film and the high-quality thin-film with nanometer multilayer or gradient-structure;
Liner positive bias ladder pipe and perforated baffle hybrid device (6) can carry out effectively bulky grain by applying positive bias Attract, depositing ions repelled, reduce loss of the plasma in pipe in transmission process, further increase electric arc etc. from The efficiency of transmission of daughter and the deposition velocity of film;(6 can pass through for liner positive bias ladder pipe and perforated baffle hybrid device Own form and structure combination realize mechanical stop screen effect, limit bulky grain defect motion path come eliminate electric arc etc. from Bulky grain defect in daughter;Multi-stage magnetic field filter device can guarantee the high efficiency of transmission of arc-plasma by the magnetic line of force, Change the motion path of bulky grain defect to eliminate the bulky grain defect in arc-plasma;It is carried out by pulsed bias parameter Adjustment is realized including amplitude, pulse width and frequency to the adjusting of arc-plasma energy and to remaining bulky grain defect It is eliminated;The microstructure and properties of prepared film can be adjusted by pulsed bias parameter, utilize pulsed bias Amplitude, pulse width and frequency realize the pinning effect that energetic ion grow film, improve the texture that film is grown And stress state, improve bond strength;Prepared film avoids bulky grain defect, and film crystal tissue is finer and close, can To further increase the mechanical property of film;
Liner ladder pipe and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle can be in ladder pipe and perforated baffles Bulky grain is attracted using the positive bias of application in hybrid device, effectively avoids bulky grain caused by low melting material Problem;Depositing ions are repelled simultaneously, reduce loss of the plasma in hybrid device in transmission process, improve etc. The efficiency of transmission of gas ions and the deposition velocity of film;Liner positive bias ladder pipe and perforated baffle hybrid device (6) pass through Between stairstepping pipe gradient difference and structure combination, the pore size of perforated baffle, Change of types and baffle at different levels structure combination and The structure of hybrid device combines, and the mechanical stop shielding to bulky grain defect may be implemented, reduction bulky grain passes through compound The probability on device arrival deposited samples surface;Liner positive bias ladder pipe and perforated baffle hybrid device (6) may be implemented fastly Quick-detach installation, the inside pipe wall for avoiding multi-stage magnetic field device (4) under linerless board status pollute the problem of clearing up;By adjusting work Applied back bias voltage parameter on part is conducive to the section Potential Distributing for improving plasma between target base, sufficiently attracts compound etc. Gas ions realize the fast deposition of film to workpiece motion s;Simultaneously also using arc ion plating (aip) generation stablize continue, from The high metallic plasma of rate is conducive to high ionization level ion in the chemosynthesis reaction of workpiece surface, prepares different elements The compound ceramic film of ratio, function film, multi-component multi-layer, superlattices and film with gradient-structure or pure metal are thin Film.
2. liner ladder pipe according to claim 1 and the compound multi-stage magnetic field arc ions electroplating method of perforated baffle, It is characterized in that, working gas selects argon gas or working gas to select one kind or more in nitrogen, acetylene, methane, silane or oxygen The mixed gas of kind, using single set or 2 sets or more of arc ion plating target source (3), multi-stage magnetic field device (4) and liner positively biased Press the liner ladder pipe of ladder pipe and perforated baffle hybrid device (6) combination and the multi-stage magnetic field electric arc that perforated baffle is compound Ion electroplating method deposit using various pure metal elements and multicomponent alloy material as the film of target, then executes step repeatedly Two and step 3, repeatedly, prepare the multilayer films with different stress, microstructure and element ratio.
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CN109989004A (en) * 2017-12-30 2019-07-09 魏永强 The arc ion plating of combination field and ladder pipe and perforated baffle composite filter
CN109989011A (en) * 2017-12-30 2019-07-09 魏永强 A kind of combination field and liner special pipe and the compound vacuum deposition method of perforated baffle
CN109989038A (en) * 2017-12-30 2019-07-09 魏永强 A kind of vacuum coating method that combination field is compound with liner ladder pipe and perforated baffle
CN108385057B (en) * 2018-01-26 2020-07-31 清华大学 Stepped collimator structure for direct-writing vacuum evaporation system
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
CN111778484B (en) * 2020-06-08 2022-07-15 季华实验室 Reducing magnetic filtering plasma leading-out device and vacuum ion beam coating equipment

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CN105925940A (en) * 2016-06-12 2016-09-07 魏永强 Multi-stage magnetic field arc ion plating method for lining positive bias straight pipe

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CN105925940A (en) * 2016-06-12 2016-09-07 魏永强 Multi-stage magnetic field arc ion plating method for lining positive bias straight pipe

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