CN106756824B - The multi-stage magnetic field arc ions electroplating method of liner positive bias stairstepping pipe - Google Patents
The multi-stage magnetic field arc ions electroplating method of liner positive bias stairstepping pipe Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Plasma Technology (AREA)
Abstract
The multi-stage magnetic field arc ions electroplating method of liner positive bias stairstepping pipe, 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 stairstepping pipe 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
Technical field
The present invention relates to the multi-stage magnetic field arc ions electroplating methods of liner positive bias stairstepping pipe, belong to material surface processing
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 scholar's (cathodic arc plasma sources and its film of Zhang Tao, Hou Junda, Liu Zhiguo, Zhang Yicong Magnetic filter
Prepare [J] China Surface Engineering, 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), on the bend pipe of 90 degree of bend pipe magnetic filters
Apply positive bias to improve the efficiency of transmission of plasma.
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.
Gas ions the problems such as transmission efficiency is low, in conjunction with the shielding of the mechanical stop of multi-stage magnetic field filter method and stairstepping pipe own form and
The compound action that positively biased piezoelectric field attracts, while guaranteeing that arc-plasma passes through stairstepping pipe and more with higher efficiency of transmission
Grade magnetic filtering device, allows that workpiece surface is continuous the case where applying back bias voltage, fine and close prepares high-quality thin-film, while reality
Now constituent content addition in film is controlled, the production cost for using alloys target is reduced, the deposition efficiency of raising film, reduces greatly
Grain defect is grown to film and the adverse effect of performance, proposes the multi-stage magnetic field arc ions of liner positive bias stairstepping pipe
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
4, multi-stage magnetic field power supply 5, liner positive bias stairstepping pipe device 6, positively biased voltage source 7, sample stage 8, grid bias power supply waveform is set to show
Wave device 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 stairstepping pipe dress
It sets and insulate between 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, electricity
Arc ion plating target source 3 is mounted on vacuum chamber 10, connects the cathode output end of arc power 2, and 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, positive and negative anodes connection can be determined according to output magnetic direction, liner positive bias rank
Trapezoidal pipe 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 is kept to liner positive bias stairstepping pipe device 6, adjusts output voltage,
Attract liner positive bias stairstepping pipe device 6 to bulky grain, depositing ions are repelled, reduces plasma in pipe
Loss in interior transmission process improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias stairstepping pipe
Device 6 can cooperate structure, the ladder of 2 grades of stairstepping pipes of the design of multi-stage magnetic field device 4,3 grades of stairstepping pipes or 4 grades of stairstepping pipes
Degree difference and inlet and outlet are laid out, and are connected and fixed between every grade of stairstepping pipe by bolt and nut, are polluted convenient for dismantling assembling and cleaning
Object;Activity insulation connection, liner positive bias stairstepping pipe between liner positive bias stairstepping pipe device 6 and multi-stage magnetic field device 4
Fast quick-detach installation may be implemented between device 6 and multi-stage magnetic field device 4, liner positive bias stairstepping pipe device 6 can regard table
Face pollution level dismantles cleaning and installation in time, avoids the inside pipe wall pollution and hardly possible of multi-stage magnetic field device 4 under linerless board status
In cleaning the problem of, the length of liner positive bias stairstepping pipe device 6HIt is identical with the length of multi-stage magnetic field device 4, liner positively biased
Press the internal diameter of 6 right side entrance of stairstepping pipe deviceD IntoGreater than the outer diameter in arc ion plating target source 3, liner positive bias stairstepping pipe
The outer diameter on 6 right side of device is less than the internal diameter of multi-stage magnetic field device 4, interior at 6 left side outlet of liner positive bias stairstepping pipe device
DiameterD OutIt is selected according to different targets and technological parameter, is changed by the internal diameter in entrance and exit, be may be implemented to big
The mechanical stop of particle shields;It is 304 stainless that nonmagnetic, resistance to cleaning may be selected in the material of liner positive bias stairstepping pipe device 6
Steel material can need the thickness of the stainless steel plate using the production of current producer, according to reality according to stairstepping length of tube and rigidity
Design parameter processing;The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is DC voltage, during the deposition process can be with
Continual and steady attraction is generated to bulky grain defect, is greatly reduced bulky grain by multi-stage magnetic field device 4 and is reached film surface
Probability.
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 stairstepping pipe device can carry out bulky grain by applying positive bias
Effectively attract, depositing ions are repelled, reduces loss of the plasma in pipe in transmission process, further increase electric arc
The efficiency of transmission of plasma and the deposition velocity of film;B. multi-stage magnetic field filter device can guarantee electric arc by the magnetic line of force
The high efficiency of transmission of plasma changes the motion path of bulky grain defect to eliminate the bulky grain defect in arc-plasma;
C. liner positive bias stairstepping pipe device can realize mechanical stop screen effect by own form, limit bulky grain defect
Motion path eliminate the bulky grain defect in arc-plasma;D. it is adjusted by pulsed bias parameter, including width
Value, pulse width and frequency are realized to the adjusting of arc-plasma energy and are eliminated to remaining bulky grain defect;e.
The microstructure and properties of prepared film can be adjusted by pulsed bias parameter, utilize the amplitude of pulsed bias, arteries and veins
It rushes width and frequency realizes the pinning effect that energetic ion grows film, improve the texture and stress shape of film growth
State improves bond strength;F. prepared film avoids bulky grain defect, and film crystal tissue is finer and close, can be into one
Step improves 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 stairstepping pipe device of multi-stage magnetic field arc ion plating of the present invention;Fig. 2 is
5 kinds of typical structure schematic diagrams of liner positive bias stairstepping pipe device.
Specific embodiment
Specific embodiment 1: illustrating present embodiment, present embodiment liner positive bias ladder below with reference to Fig. 1 and 2
The multi-stage magnetic field arc ions electroplating method institute use device of shape pipe 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 stairstepping pipe 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 stairstepping pipe dress
It sets and insulate between 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, electricity
Arc ion plating target source 3 is mounted on vacuum chamber 10, connects the cathode output end of arc power 2, and 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, positive and negative anodes connection can be determined according to output magnetic direction, liner positive bias rank
Trapezoidal pipe 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 stairstepping pipe device 6 keeps direct current positive bias, is adjusted output voltage, is made
Liner positive bias stairstepping pipe device 6 attracts bulky grain, repels to depositing ions, reduces plasma in pipe
Loss in transmission process improves the efficiency of transmission of plasma and the deposition velocity of film;Liner positive bias stairstepping pipe dress
Set 6 structure, the gradients that multi-stage magnetic field device 4 can be cooperated to design 2 grades of stairstepping pipes, 3 grades of stairstepping pipes or 4 grades of stairstepping pipes
Difference and inlet and outlet are laid out, and are connected and fixed between every grade of stairstepping pipe by bolt and nut, convenient for dismantling assembling and cleaning pollutant;
Activity insulation connection, liner positive bias stairstepping pipe device between liner positive bias stairstepping pipe device 6 and multi-stage magnetic field device 4
Fast quick-detach installation may be implemented between 6 and multi-stage magnetic field device 4, liner positive bias stairstepping pipe device 6 can be with apparent surface dirt
Dye degree dismantles cleaning and installation in time, avoids asking for the inside pipe wall pollution cleaning of multi-stage magnetic field device 4 under linerless board status
Topic;The internal diameter of 6 right side entrance of liner positive bias stairstepping pipe deviceD IntoGreater than the outer diameter in arc ion plating target source 3, liner is just
The outer diameter on 6 right side of bias stairstepping pipe device is less than the internal diameter of multi-stage magnetic field device 4, and liner positive bias stairstepping pipe device 6 is left
Internal diameter at side outletD OutIt is selected according to different targets and technological parameter, is become by entrance and the internal diameter ratio in exit
Change, the mechanical stop shielding to bulky grain may be implemented;The material of liner positive bias stairstepping pipe device 6 may be selected it is nonmagnetic,
304 stainless steel materials of resistance to cleaning can need the stainless steel plate using the production of current producer according to stairstepping length of tube and rigidity
Thickness, according to actual design parameter process;The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is DC voltage,
Continual and steady attraction can be generated to bulky grain defect during the deposition process, greatly reduces bulky grain and passes through multi-stage magnetic field device
4 probability.
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 stairstepping pipe, can be in stairstepping pipe device
Bulky grain is attracted using the positive bias of application, effectively avoids bulky grain problem caused by low melting material;It is right simultaneously
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;The internal diameter that liner positive bias stairstepping pipe device passes through exitD OutIt adjusts, may be implemented to bulky grain
The mechanical stop of defect shields, and reduces the probability that bulky grain reaches deposited samples surface by exit;Liner positive bias ladder
Fast quick-detach installation may be implemented in shape pipe device, avoids the inside pipe wall pollution cleaning of multi-stage magnetic field device under linerless board status
Problem;By adjusting back bias voltage parameter applied on workpiece, be conducive to the section Potential Distributing for improving plasma between target base,
Sufficiently attract compound plasma to workpiece motion s, realizes the fast deposition of film;Arc ion plating (aip) is also utilized simultaneously
It generates and stablizes metallic plasma lasting, that ionization level is high, it is anti-in the chemical synthesis of workpiece surface to be conducive to high ionization level ion
It answers, prepares the compound ceramic films of different element ratios, function film, multi-component multi-layer, superlattices and with gradient-structure
Film or pure metal 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
The multi-stage magnetic field arc ions electroplating method for the liner positive bias stairstepping pipe for pressing stairstepping pipe device 6 combined is carried out with various proof gold
Belong to element and multicomponent alloy material is the film deposition of target, then carries out step 3, then execute step 2 and step repeatedly
Three, repeatedly, prepare the multilayer films with different stress, microstructure and element ratio.
Claims (2)
1. the multi-stage magnetic field arc ions electroplating method of liner positive bias stairstepping pipe, which is characterized in that this method institute use device
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 stairstepping pipe device (6), positively biased voltage source (7), sample stage (8), grid bias power supply kymographion (9) and vacuum
Room (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 stairstepping pipe dress
It sets and insulate between (6) and vacuum chamber (10) and multi-stage magnetic field device (4), workpiece and sample stage (8) connect the cathode of grid bias power supply (1)
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 dress
The magnetic fields at different levels for setting (4) connect each output end of multi-stage magnetic field power supply (5), positive and negative anodes connection can according to output magnetic direction into
Row determines that liner positive bias stairstepping pipe 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 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;
Grid bias power supply kymographion (9) is used to show the pulse voltage and current waveform that grid bias power supply (1) issues, by adjusting
The output waveform of grid bias power supply (1), effectively attracts plated film ion, and the deposition and control deposition targets for carrying out film exist
Ratio in film realizes the adjusting of plasma energy;
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)
It closes target and adjusts the technological parameter needed, the current value of arc power (2) output is 10 ~ 300A, and arc power (2) exports direct current, simple venation
Punching, DC pulse is compound or multiple-pulse is compound, adjusts multi-stage magnetic field device (4) by multi-stage magnetic field power supply (5), keeps electric arc etc.
Gas ions arc ion plating target source (3) stablize generate and elimination is filtered to bulky grain defect, make arc-plasma with
Higher efficiency of transmission 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) avoid the temperature in the course of work from increasing problem by water-cooling pattern;
It opens positively biased voltage source (7), direct current positive bias is kept to liner positive bias stairstepping pipe device (6), adjusts output voltage,
Attract liner positive bias stairstepping pipe 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 stairstepping
Activity insulation connection between pipe device (6) and multi-stage magnetic field device (4), liner positive bias stairstepping pipe device (6) and multistage magnetic
Fast quick-detach installation may be implemented between field device (4), liner positive bias stairstepping pipe device (6) can be with apparent surface pollution level
Disassembly cleaning in time and installation avoid the inside pipe wall pollution of multi-stage magnetic field device (4) under linerless board status and are difficult to clear up
Problem;The length of liner positive bias stairstepping pipe device (6)HIt is identical with the length of multi-stage magnetic field device (4), liner positive bias rank
The internal diameter of entrance on the right side of trapezoidal pipe device (6)D IntoGreater than the outer diameter in arc ion plating target source (3), liner positive bias stairstepping pipe
Outer diameter on the right side of device (6) is less than the internal diameter of multi-stage magnetic field device (4), liner positive bias stairstepping pipe device (6) left side outlet
The internal diameter at placeD OutIt is selected, is changed by the internal diameter in entrance and exit, Ke Yishi according to different targets and technological parameter
Now the mechanical stop of bulky grain is shielded;Liner positive bias stairstepping pipe device (6) can cooperate multi-stage magnetic field device (4) to design
2 grades of stairstepping pipes, the structure of 3 grades of stairstepping pipes or 4 grades of stairstepping pipes, gradient difference and inlet and outlet layout, every grade of stairstepping pipe
Between be connected and fixed by bolt and nut, convenient for dismantling assembling and cleaning pollutant;Liner positive bias stairstepping pipe device (6)
304 stainless steel materials of nonmagnetic, resistance to cleaning may be selected in material, and it is suitable to need to select according to stairstepping length of tube and rigidity
Thickness is processed according to actual design parameter;The voltage parameter of positively biased voltage source (7) is 0 ~+200V, is DC voltage,
Continual and steady attraction can be generated to bulky grain defect during the deposition process, greatly reduces bulky grain and passes through multi-stage magnetic field device
(4) probability of film surface is reached;
Liner positive bias stairstepping pipe device (6) by apply positive bias bulky grain can effectively be attracted, to deposit from
Son is repelled, and loss of the plasma in pipe in transmission process is reduced, and further increases the transmission effect of arc-plasma
The deposition velocity of rate and film;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;Liner positive bias stairstepping pipe dress
Mechanical stop screen effect can be realized by own form by setting (6), limit the motion path of bulky grain defect to eliminate electric arc
Bulky grain defect in plasma;It is adjusted by pulsed bias parameter, including amplitude, pulse width and frequency realization pair
The adjusting of arc-plasma energy and remaining bulky grain defect is eliminated;The microstructure and properties of prepared film
It can be adjusted by pulsed bias parameter, realize energetic ion pair using the amplitude, pulse width and frequency of pulsed bias
The pinning effect of film growth, improves the texture and stress state of film growth, improves bond strength;Prepared film
Bulky grain defect is avoided, 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;
Bulky grain is attracted using the positive bias of application in stairstepping pipe device, is effectively avoided produced by low melting material
Bulky grain problem;Depositing ions are repelled simultaneously, reduce loss of the plasma in pipe in transmission process, improve etc.
The efficiency of transmission of gas ions and the deposition velocity of film;The internal diameter that liner positive bias stairstepping pipe device (6) passes through exitD Out
It adjusts, the mechanical stop shielding to bulky grain defect may be implemented, reduce bulky grain by exit and reach deposited samples surface
Probability;Fast quick-detach installation may be implemented in liner positive bias stairstepping pipe device, avoids multi-stage magnetic field under linerless board status
The inside pipe wall of device (4) pollutes the problem of cleaning;By adjusting back bias voltage parameter applied on workpiece, be conducive to improve target base it
Between plasma section Potential Distributing, sufficiently attract compound plasma to workpiece motion s, realize the fast deposition of film;Together
When also utilize the generation of arc ion plating (aip) stablize continue, the high metallic plasma of ionization level, be conducive to high ionization level from
Son prepares the compound ceramic film of different element ratios, function film, polynary more in the chemosynthesis reaction of workpiece surface
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 stairstepping pipe according to claim 1, feature exist
In working gas selects argon gas or working gas to select mixing one or more in nitrogen, acetylene, methane, silane or oxygen
Gas, this method can singly cover or 2 sets or more of arc ion plating target source (3), multi-stage magnetic field device (4) and liner positive bias
The multi-stage magnetic field arc ions electroplating method of the liner positive bias stairstepping pipe of stairstepping pipe device (6) combination is carried out with various proof gold
Belong to element and multicomponent alloy material is the film deposition of target, then executes step 2 and step 3 repeatedly, repeatedly, preparation
Multilayer films with different stress, microstructure and element ratio.
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CN109989012A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of vacuum deposition method that combination field is compound with liner ladder pipe and perforated baffle |
CN109989017A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | The arc ion plating of combination field and liner bias ladder pipe composite filter |
CN109989040A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of combination field and liner conical pipe and the compound vacuum deposition method of ladder pipe |
CN109989029A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | The arc ion plating of combination field and liner bias conical pipe and ladder pipe combined filtration |
CN109989018A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of combination field and the compound vacuum coating method of liner bias ladder pipe |
CN109989028A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | The arc ion plating of multi-stage magnetic field and liner bias conical pipe and ladder pipe combined filtration |
CN109989013A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of combination field and the compound vacuum deposition method of liner bias ladder 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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