CN106756823B - Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube - Google Patents
Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube Download PDFInfo
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- CN106756823B CN106756823B CN201710053016.2A CN201710053016A CN106756823B CN 106756823 B CN106756823 B CN 106756823B CN 201710053016 A CN201710053016 A CN 201710053016A CN 106756823 B CN106756823 B CN 106756823B
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- 239000002131 composite material Substances 0.000 claims abstract description 55
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- 230000000694 effects Effects 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007733 ion plating Methods 0.000 claims description 30
- 230000008021 deposition Effects 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 13
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- 239000000956 alloy Substances 0.000 claims description 7
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- 238000001755 magnetron sputter deposition Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
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- 238000009434 installation Methods 0.000 claims description 5
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
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Classifications
-
- 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 & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, belong to technical field of material surface treatment, the present invention is 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 conical pipe and straight tube set composite 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 compound multi-stage magnetic field arc ions electroplating methods of liner positive bias conical pipe and straight tube, 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 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.
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 conical pipe own form and just
The compound action that biasing electric field attracts, while guaranteeing that arc-plasma passes through conical pipe and multistage magnetic with higher efficiency of transmission
Filter device, allows that workpiece surface is continuous the case where applying back bias voltage, fine and close prepares high-quality thin-film, while realization pair
Constituent content addition control, reduction use the production cost of alloys target, the deposition efficiency for improving film, reduce bulky grain in film
Defect is grown to film and the adverse effect of performance, proposes liner positive bias conical pipe and the compound multi-stage magnetic field electric arc of straight tube
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 conical pipe and straight tube set composite 6, positively biased voltage source 7, sample stage 8, bias plasma
Source waveform oscillograph 9 and vacuum chamber 10；
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 conical pipe and straight
It insulate between pipe set composite 6 and vacuum chamber 10 and multi-stage magnetic field device 4, the cathode that workpiece and sample stage 8 connect grid bias power supply 1 is defeated
Outlet, 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 it is each
Grade magnetic field connects each output end of multi-stage magnetic field power supply 5, and positive and negative anodes connection can be determined according to output magnetic direction, liner
Positive bias conical pipe and straight tube set composite 6 connect the cathode output end of positively biased voltage source 7, 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 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 are kept to liner positive bias conical pipe and straight tube set composite 6
Output voltage attracts liner positive bias conical pipe and straight tube set composite 6 to bulky grain, arranges depositing ions
Reprimand reduces loss of the plasma in pipe in transmission process, improves the efficiency of transmission of plasma and the deposition velocity of film；
Liner positive bias conical pipe and straight tube set composite 6 can cooperate multi-stage magnetic field device 4 to design various structures and inlet and outlet layout,
It is connected and fixed between each pipe by bolt and nut, convenient for dismantling assembling and cleaning pollutant；Liner positive bias conical pipe and straight tube
Activity insulation connection between set composite 6 and multi-stage magnetic field device 4, liner positive bias conical pipe and straight tube set composite 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
Be difficult to the problem of clearing up, the length of liner positive bias conical pipe and straight tube set composite 6HWith the length of multi-stage magnetic field device 4
It is identical, the internal diameter of 6 right side entrance of liner positive bias conical pipe and straight tube set compositeD IntoIt is outer greater than arc ion plating target source 3
The outer diameter of diameter, 6 right side of liner positive bias conical pipe and straight tube set composite is less than the internal diameter of multi-stage magnetic field device 4, liner positively biased
Press the internal diameter at conical pipe and 6 left side outlet of straight tube set compositeD OutIt is selected, is passed through according to different targets and technological parameter
The variation of the internal diameter in entrance and exit and the structure combination of set composite, may be implemented the mechanical stop shielding to bulky grain,
304 stainless steel materials of nonmagnetic, resistance to cleaning may be selected in the material of liner positive bias conical pipe and straight tube set composite 6, can root
It needs to select suitable thickness according to the length and rigidity of conical pipe and straight tube set composite, is according to the processing of actual design parameter
It can；The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is DC voltage, can produce during the deposition process to bulky grain defect
Raw continual and steady attraction 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 conical pipe and straight tube set composite can be to big by applying positive bias
Particle is effectively attracted, and is repelled to depositing ions, reduces loss of the plasma in pipe in transmission process, further
Improve 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
Guarantee the high efficiency of transmission of arc-plasma, changes the motion path of bulky grain defect to eliminate big in arc-plasma
Grain defect；C. liner positive bias conical pipe and straight tube set composite can realize mechanical stop screen effect by own form,
The motion path of bulky grain defect is limited to eliminate the bulky grain defect in arc-plasma；D. pass through pulsed bias parameter
It is adjusted, realizes including amplitude, pulse width and frequency to the adjusting of arc-plasma energy and to remaining bulky grain
Defect is eliminated；E. the microstructure and properties of prepared film can be adjusted by pulsed bias parameter, utilize arteries and veins
The amplitude, pulse width and frequency for rushing bias realize the pinning effect that energetic ion grows film, improve the crystalline substance of film growth
Body tissue and stress state improve bond strength；F. prepared film avoids bulky grain defect, and film crystal tissue is more
Add densification, 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 positive bias conical pipe of multi-stage magnetic field arc ion plating of the present invention and a kind of dress of straight tube set composite
With schematic diagram；Fig. 2 is 4 kinds of typical structure schematic diagrams of liner positive bias conical pipe and straight tube set composite.
Specific embodiment
Specific embodiment 1: illustrating present embodiment, present embodiment liner positive bias taper below with reference to Fig. 1 and 2
Pipe and the compound multi-stage magnetic field arc ions electroplating method institute use device of straight tube include grid bias power supply 1, arc power 2, arc ions
Plate target source 3, multi-stage magnetic field device 4, multi-stage magnetic field power supply 5, liner positive bias conical pipe and straight tube set composite 6, positively biased piezoelectricity
Source 7, sample stage 8, grid bias power supply kymographion 9 and vacuum chamber 10；
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 conical pipe and straight
It insulate between pipe set composite 6 and vacuum chamber 10 and multi-stage magnetic field device 4, the cathode that workpiece and sample stage 8 connect grid bias power supply 1 is defeated
Outlet, 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 it is each
Grade magnetic field connects each output end of multi-stage magnetic field power supply 5, and positive and negative anodes connection can be determined according to output magnetic direction, liner
Positive bias conical pipe and straight tube set composite 6 connect the cathode output end of positively biased voltage source 7, 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 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 conical pipe and straight tube set composite 6 keep direct current positive bias, is adjusted defeated
Voltage out attracts liner positive bias conical pipe and straight tube set composite 6 to bulky grain, repels to depositing ions,
Loss of the plasma in pipe in transmission process is reduced, the efficiency of transmission of plasma and the deposition velocity of film are improved；It is interior
Lining positive bias conical pipe and straight tube set composite 6 can cooperate multi-stage magnetic field device 4 to design various structures and inlet and outlet layout, respectively
It is connected and fixed between pipe by bolt and nut, convenient for dismantling assembling and cleaning pollutant；Liner positive bias conical pipe and straight tube are multiple
It attaches together and sets 6 the installation of fast quick-detach may be implemented, avoid the inside pipe wall pollution cleaning of multi-stage magnetic field device 4 under linerless board status
Problem, the internal diameter of 6 right side entrance of liner positive bias conical pipe and straight tube set compositeD IntoIt is outer greater than arc ion plating target source 3
The outer diameter of diameter, 6 right side of liner positive bias conical pipe and straight tube set composite is less than the internal diameter of multi-stage magnetic field device 4, liner positively biased
Press the internal diameter at conical pipe and 6 left side outlet of straight tube set compositeD OutIt is selected, is passed through according to different targets and technological parameter
Entrance and the variation of the internal diameter ratio in exit and the structure combination of set composite, may be implemented the mechanical stop screen to bulky grain
It covers, 304 stainless steel materials of nonmagnetic, resistance to cleaning may be selected in the material of liner positive bias conical pipe and straight tube set composite 6, can
It needs to select suitable thickness according to the length and rigidity of conical pipe and straight tube set composite, is according to the processing of actual design parameter
It can；The voltage parameter of positively biased voltage source 7 is 0 ~+200V, is DC voltage, can produce during the deposition process to bulky grain defect
Raw continual and steady attraction greatly reduces 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 positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, can be in conical pipe
Bulky grain is attracted with the positive bias in straight tube set composite using application, is effectively avoided big caused by low melting material
Particle issues；Depositing ions are repelled simultaneously, loss of the plasma in pipe in transmission process is reduced, improves plasma
The efficiency of transmission of body and the deposition velocity of film；Liner positive bias conical pipe and straight tube set composite are combined and are exported by structure
The internal diameter at placeD OutIt adjusts, the mechanical stop shielding to bulky grain defect may be implemented, reduce bulky grain and reached by exit and sunk
The probability of product sample surfaces；Fast quick-detach installation may be implemented in liner positive bias conical pipe and straight tube set composite, avoids nothing
The inside pipe wall of multi-stage magnetic field device pollutes the problem of cleaning under liner plate state；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.
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 conical pipe and the combined compound multi-stage magnetic field arc ion plating side of liner positive bias conical pipe and straight tube of straight tube set composite 6
Method deposit using various pure metal elements and multicomponent alloy material as the film of target, then carries out step 3, then repeatedly
Step 2 and step 3 are executed, repeatedly, prepares the multilayered structure with different stress, microstructure and element ratio
Film.
Claims (2)
1. liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube, 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 conical pipe and straight tube set composite (6), positively biased voltage source (7), sample stage (8), grid bias power supply wave
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 conical pipe and straight
It insulate between pipe set composite (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),
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 output
Magnetic direction is determined, and liner positive bias conical pipe and straight tube set composite (6) connect the positive of positively biased voltage source (7) and export
External water-cooling circulating system is opened at end；
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%；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, compound ceramic film, function film, multi-component multi-layer, superlattices, the tool of pure metal film, different element ratios are carried out
There is the film of nanometer multilayer or gradient-structure；The technological parameter needed is adjusted, 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；
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；
It opens positively biased voltage source (7), direct current positive bias, adjustment is kept to liner positive bias conical pipe and straight tube set composite (6)
Output voltage attracts liner positive bias conical pipe and straight tube set composite (6) to bulky grain, arranges depositing ions
Reprimand reduces loss of the plasma in pipe in transmission process, improves the efficiency of transmission of plasma and the deposition velocity of film；
Liner positive bias conical pipe and straight tube set composite (6) can cooperate multi-stage magnetic field device (4) design various structures and inlet and outlet
It is laid out, is connected and fixed between each pipe by bolt and nut, convenient for dismantling assembling and cleaning pollutant；Liner positive bias conical pipe and
Activity insulation connection, liner positive bias conical pipe and the compound dress of straight tube between straight tube set composite (6) and multi-stage magnetic field device (4)
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 pollutes and is difficult to the problem of clearing up, the length of liner positive bias conical pipe and straight tube set composite (6)HAnd multi-stage magnetic field
The length of device (4) is identical, the internal diameter of entrance on the right side of liner positive bias conical pipe and straight tube set composite (6)D IntoGreater than electric arc
Outer diameter on the right side of the outer diameter in ion plating target source (3), liner positive bias conical pipe and straight tube set composite (6) is filled less than multi-stage magnetic field
Set the internal diameter of (4), the internal diameter at liner positive bias conical pipe and straight tube set composite (6) left side outletD OutAccording to different targets and
Technological parameter is selected, and is combined, be may be implemented pair by the structure of the variation of the internal diameter in entrance and exit and set composite
The mechanical stop of bulky grain shields, and the material of liner positive bias conical pipe and straight tube set composite (6) may be selected nonmagnetic, resistance to clear
304 stainless steel materials of reason, can need to select suitable thickness, press according to the length and rigidity of conical pipe and straight tube set composite
According to the facts border design parameter is processed；The voltage parameter of positively biased voltage source (7) is 0 ~+200V, is DC voltage, was depositing
Continual and steady attraction can be generated in journey to bulky grain defect, greatly reduces bulky grain and is reached by multi-stage magnetic field device (4)
The probability of film surface；
Liner positive bias conical pipe and straight tube set composite (6) can effectively attract bulky grain by applying positive bias,
Depositing ions are repelled, loss of the plasma in pipe in transmission process is reduced, further increases arc-plasma
Efficiency of transmission and film deposition velocity；Multi-stage magnetic field filter device can guarantee the height of arc-plasma by the magnetic line of force
Effect transmission changes the motion path of bulky grain defect to eliminate the bulky grain defect in arc-plasma；Liner positive bias cone
Shape pipe and straight tube set composite (6) can realize mechanical stop screen effect by own form, limit the fortune of bulky grain defect
The bulky grain defect in arc-plasma is eliminated in dynamic path；It is adjusted by pulsed bias parameter, including amplitude, pulse
Width and frequency are realized to the adjusting of arc-plasma energy and are eliminated to remaining bulky grain defect；Prepared film
Microstructure and properties can be adjusted by pulsed bias parameter, utilize the amplitude, pulse width and frequency of pulsed bias
Rate realizes the pinning effect that energetic ion grows film, improves the texture and stress state of film growth, improves and combines
Intensity；Prepared film avoids bulky grain defect, and film crystal tissue is finer and close, can be further improved the power of film
Learn performance；
This method further include: Step 3: can in conjunction with using Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc from
Son plating and pulsed cathode arc and Dc bias, pulsed bias or the compound bias of DC pulse carry out film deposition, to prepare proof gold
Belong to compound ceramic film, function film and the film with nanometer multilayer or gradient-structure of film, different element ratios；
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 film with nanometer multilayer or gradient-structure；
Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube can be compound in conical pipe and straight tube
Bulky grain is attracted using the positive bias of application in device, effectively avoids bulky grain problem caused by low melting material；
Depositing ions are repelled simultaneously, loss of the plasma in pipe in transmission process is reduced, improves the transmission of plasma
The deposition velocity of efficiency and film；Liner positive bias conical pipe and straight tube set composite (6) pass through structure combination and exit
Internal diameterD OutIt adjusts, the mechanical stop shielding to bulky grain defect may be implemented, reduce bulky grain by exit and reach deposition sample
The probability on product surface；Fast quick-detach installation may be implemented in liner positive bias conical pipe and straight tube set composite (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. liner positive bias conical pipe according to claim 1 and the compound multi-stage magnetic field arc ions electroplating method of straight tube,
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 positive bias conical pipe of conical pipe and straight tube set composite (6) combination and the multi-stage magnetic field arc ion plating that straight tube is compound
Method deposit using various pure metal elements and multicomponent alloy material as the film of target, then carries out step 3, then instead
Step 2 and step 3 are executed again, repeatedly, prepare the multilayer knot with different stress, microstructure and element ratio
Structure film.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710053016.2A CN106756823B (en) | 2017-01-22 | 2017-01-22 | Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube |
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| CN201710053016.2A CN106756823B (en) | 2017-01-22 | 2017-01-22 | Liner positive bias conical pipe and the compound multi-stage magnetic field arc ions electroplating method of straight tube |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109989016A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of combination field, compound tube and the compound vacuum coating method of perforated baffle |
| 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 |
| 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 |
| CN109989039A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of combination field, compound tube and the compound vacuum deposition method of perforated baffle |
| CN109989023A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | A kind of vacuum coating method that combination field is compound with liner bias conical pipe and straight tube |
| CN109989026A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | The arc ion plating of multi-stage magnetic field and liner compound tube and perforated baffle combined filtration |
| CN109989008A (en) * | 2017-12-30 | 2019-07-09 | 魏永强 | The arc ion plating of combination field and liner compound tube and perforated baffle combined filtration |
| 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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Effective date of registration: 20200624 Address after: 450015 Henan Province, Zhengzhou District, No. 27 University Road, No. 2 Patentee after: ZHENGZHOU INSTITUTE OF AERONAUTICAL INDUSTRY MANAGEMENT Address before: 450015, building 4, unit 2, building 26, Zheng Hang family hospital, 2 Middle School Road, 27 District, Henan, Zhengzhou Patentee before: Wei Yongqiang |
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