CN104947046B - Multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method - Google Patents
Multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method Download PDFInfo
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Abstract
Multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method, belong to technical field of material surface treatment, and the present invention is the simple metal or multicomponent alloy material and nonmetallic materials for solving low melting point（Such as graphite）Bulky grain problem, magnetron sputtering ionization level and deposition efficiency in arc ion plating are low and high-melting-point target is using limitation, break through high-power impulse magnetron sputtering discharge instability and expand arc ion plating target and use scope.The inventive method includes：First, workpiece to be coated is placed on the sample stage in vacuum chamber, connects line related；2nd, thin film deposition：Treat that the vacuum in vacuum chamber is less than 10‑2During Pa, it is passed through working gas and adjusts air pressure, open plated film power supply, grid bias power supply and magnetron sputtering power supply output waveform are adjusted by synchronous waveform coalignment, bulky grain defect is eliminated using multi-stage magnetic field straight tube magnetic filter and ensures the efficiency of transmission of arc-plasma, technological parameter needed for setting, carries out thin film deposition.
Description
Technical field
The present invention relates to multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method, belong to material
Technical field of surface.
Background technology
Arc ion plating (aip) can obtain nearly all metal ion including carbon ion, while with high ionization
Rate, diffractive good, film-substrate cohesion are good, coating quality is good, high deposition efficiency and be taken seriously the advantages of easy equipment operation,
It is one of current physical vapour deposition (PVD) technology of preparing being used widely in the industry.It can be not only used for preparing metal and prevents
Coating is protected, the preparation of the high-temperature ceramic coatings such as nitride, carbide can also be realized by the regulation of process, while
Also there is application in function film field.Even for the irregular parts of shape, arc ion plating can also realize the fast of film
Speed deposition, or even also serve as nanometer multilayer and superlattice film preparation method（Tay B K, Zhao Z W, Chua D H C.
Review of metal oxide films deposited by filtered cathodic vacuum arc
technique [J]. Mater Sci Eng R, 2006, 52(1-3): 1-48.）.But prepared in arc ion plating thin
During film, because arc spot current density is up to 2.5 ~ 5 × 1010A/m2, cause and melted at the arc spot position of target material surface
The liquid metal melted, splash comes out in droplets in the presence of local plasma pressure, be attached to film surface or
Inlay formation " bulky grain " in the film（Macroparticles）Defect（Boxman R L, Goldsmith S.
Macroparticle contamination in cathodic arc coatings: generation, transport
and control [J]. Surf Coat Tech, 1992, 52(1): 39-50.）.Dirt just as PM2.5 to air quality
Dye is the same, is micron or the film of sub-micron relative to thickness rank, and size is in 0.1-10 microns of bulky grain defect to film
Quality and performance have serious harm.With thin-film material and thin film technique apply it is increasingly extensive, bulky grain defect is asked
The bottleneck for whether solving further to develop as arc ions electroplating method of topic, seriously constrains it in thin-film material system of new generation
Application in standby.
Originally magnetron sputtering technique uses direct current supply pattern, compared to arc ions electroplating method, does not have bulky grain defect,
The low-temperature sputter deposition of various materials can be realized, but the ionization level of its sputter material is very low, and the power density of sputtering target exists
50W/cm2, cannot get enough ion populations during thin film deposition, cause deposition efficiency very low, at the same the energy of ion institute band compared with
It is low, make Thin Film Tissue not fine and close enough., V. Kouznetsov of Linkoping,Sweden university et al. in 1999（Kouznetsov V,
Macák K, Schneider J M, Helmersson U, Petrov I. A novel pulsed magnetron
sputter technique utilizing very high target power densities [J]. Surf Coat
Tech, 1999, 122(2-3): 290-293.）Propose high-power impulse magnetron sputtering technology（HPPMS）, it utilizes higher
Pulse peak power and relatively low pulse width improve the ionization level of sputter material, while target cathode will not increase because of overheat
Plus the requirement of target cooling.Its peak power improves 100 times, about 1000 ~ 3000W/ compared to conventional DC magnetron sputtering
cm2, the density of plasma reaches 1018m-3The order of magnitude, its central region ion concentration is up to 1019m-3The order of magnitude, splashes simultaneously
The ionization level for penetrating material reaches as high as more than 90%, and without the bulky grain in current ionization level highest arc ions electroplating method
Defect.After 2008, each colleges and universities also begins to research of the expansion for high-power impulse magnetron sputtering technology at home（Li Xi
The flat high power combined pulsed magnetron sputtering plasma characteristics of and TiAlN thin film are prepared [D];Harbin Institute of Technology,
2008. Wuzhongs shake, Zhu Zongtao, Gong Chunzhi, Tian Xiubo, Yang Shiqin, the flat high-power impulse magnetron sputterings technologies of Li Xi
Development and research [J] vacuum, 2009,46 (3):18-22. and Mu Zongxin, Mu Xiaodong, Wang Chun, Jia Li, Dong
Rush dc sources coupling high power pulse non-balance magnetically controlled sputter ionization property [J] Acta Physica Sinicas, 2011,60 (1):
422-428.）, but be due to high-power impulse magnetron sputtering technology pulsed discharge it is unstable, and target current potential is relatively low, target gold
Category substantial amounts of metal ion after ionization is sucked back into target surface, fails to reach the deposition that matrix surface realizes film, causes
The efficiency of thin film deposition is substantially reduced, the paces for influenceing it to be further substituted with common magnetron sputtering and arc ion plating, follow-up
Popularization and application in terms of receive a definite limitation.
At present, it is also easy to produce greatly in the simple metal using low melting point or multicomponent alloy material to solve arc ions electroplating method
Grain defect and magnetron sputtering technique mainly have following several at present the problem of in terms of using high-melting-point target in the presence of ionization is difficult to
Kind：
The first：Bulky grain is filtered out using the method for Magnetic filter, such as Chinese patent be used for material surface modifying from
Daughter immersion ion injection device（Publication number：CN1150180, publication date：On May 21st, 1997）It is middle to use 90 ° of Magnetic filters
Bend pipe is filtered to the bulky grain of pulsed cathode arc, American scholar Anders et al. (Anders S, Anders A,
Dickinson M R, MacGill R A, Brown I G. S-shaped magnetic macroparticle filter
for cathodic arc deposition [J]. IEEE Trans Plasma Sci, 1997, 25(4): 670-
674.) and the Zhang Yujuan etc. of He'nan University (such as Zhang Yujuan, Wu Zhiguo, Zhang Weiwei filtered cathode arc plasmas prepare TiAlN thin film
Influence China YouSe Acta Metallurgica Sinica 2004,14 (8) of the middle sedimentary condition to film texture:1264-1268.) in article
Middle " S " magnetic filter that made is filtered to the bulky grain of cathode arc, also American scholar Anders et al.（Anders
A, MacGill R A. Twist filter for the removal of macroparticles from cathodic
arc plasmas [J]. Surf Coat Tech, 2000, 133-134: 96-100.）The Twist filter's of proposition
Magnetic filter, although these methods have certain effect in terms of filtering and eliminating bulky grain, the efficiency of transmission of plasma is damaged
Lose seriously, substantially reduce ion current density.Based on that can filter on the basis of bulky grain can guarantee that efficiency again, Chinese patent is true
Empty cathode arc straight filter (publication number：CN1632905, publication date：On June 29th, 2005) the middle side for proposing straight tube filtering
Method, but which in turn reduces filter effect.In a word, related researcher is by contrasting various Magnetic filter methods（Anders A.
Approaches to rid cathodic arc plasmas of macro- and nanoparticles: a review
[J] Surf Coat Tech, 1999,120-121319-330. and Takikawa H, Tanoue H. Review of
cathodic arc deposition for preparing droplet-free thin films [J]. IEEE Trans
Plasma Sci, 2007, 35(4): 992-999.）It was found that arc ion plating plasma after magnetic filter by keeping
High efficiency of transmission and elimination bulky grain is very difficult to take into account, and drastically influence application of the technology in high-quality thin-film deposition.
Second, using the method for stopping shielding, such as big is directly shielded using baffle plate before arc ion plating target source
Grain（Miernik K, Walkowicz J, Bujak J. Design and performance of the
microdroplet filtering system used in cathodic arc coating deposition [J].
Plasmas & Ions, 2000, 3(1-4): 41-51.）；Or utilize bulky grain and arc-plasma transmission speed
Difference, applies a high speed rotating unit outside arc source（Utsumi T, English J H. Study of electrode
products emitted by vacuum arcs in form of molten metal particles [J]. J Appl
Phys, 1975, 46(1): 126-131.）, by adjusting the velocity of rotation of rotating vane, realize the resistance to bulky grain defect
Gear filtering；Hole is either drilled with baffle plate, by adjusting the spacing of two layers of baffle plate so as to the transmission of arc-plasma, resistance
Gear bulky grain deposits to the dual-layered baffle plate screening arrangement of film surface（Zhao Y, Lin G, Xiao J, et al.
Synthesis of titanium nitride thin films deposited by a new shielded arc ion
plating [J]. Appl Surf Sci, 2011, 257(13): 5694-5697.）；Disappear also by regulating fender angle
Except the flap type screening arrangement of bulky grain（Zimmer O. Vacuum arc deposition by using a
Venetian blind particle filter [J]. Surf Coat Tech, 2005, 200(1-4): 440-
443.）.Stop and shield motion path by limiting bulky grain and plasma, utilize arc-plasma well diffractive
To prepare film, but this method can cause the efficiency of transmission of plasma to lose serious, receive in actual applications certain
Limitation.
3rd, using the electric field suppressing method of bias on matrix, in arc-plasma, due to the motion speed of electronics
Degree is far longer than the electron number that large particle surface is reached in the movement velocity of ion, unit interval more than number of ions, makes bulky grain
Elecrtonegativity is presented.When applying back bias voltage on matrix, electric field will produce repulsive interaction to electronegative bulky grain, and then reduce thin
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.）Replace traditional Dc bias using pulsed bias, formed
A kind of new physical gas phase deposition technology --- pulsed bias arc ion plating technology, not only greatly reduces film surface big
The number of particle, also overcomes the problems such as substrate temperature is too high, stress in thin films is larger caused by Traditional DC bias.Big couple very much in love
Woods Guoqiang of work university et al.（Process ba- sis research [D] Dalians University of Science ＆ Engineering of woods Guoqiang pulsed bias arc ion platings are big
Learn, 2008. and Huang Meidong, woods Guoqiang, Dong Chuan, Sun Chao, hear Bias On Morphologies of Films Prepared By Arc Ion Plating immediately
Influencing Mechanism [J] Acta Metallurgica Sinicas, 2003,39 (5): 510-515.）Bulky grain defect is caused to reduce for pulsed bias
Mechanism conduct in-depth analysis, pass through the adjustment to technological parameters such as pulsed bias amplitude, frequency and pulse widths, Ke Yigai
The sheaths kinetic characteristic of kind arc-plasma, reduces the bulky grain defect counts of film surface, the quality of film is improved, in reality
It is widely used in the production on border, but bulky grain defect can not be still completely eliminated.
4th, the optimization of technological parameter, by adjusting operating air pressure（Brown I G. Cathodic arc
deposition of films. Ann Rev Mater Sci, 1998, 28(1):243-269. and Chen Kangmin, Zhang Xiao
Lemon, Zheng Chenchao, Huang Yan, Guan Qingfeng, Gong Lei, Sun Chao nitrogen partial pressures are to arc ion plating CrNx organization structure of film
Influence [J] vacuum sciences and Technology, 2010,30 (6): 662-666.）Spots moving is controlled with using magnetic field（Youth
Wenchang, Xiao Jinquan, Gong Jun, Sun Chao, Huang Rongfang hear shadow of the axisymmetrical magnetic fields to arc ion plating spots moving immediately
Ring Acta Metallurgica Sinicas, 2010,46 (3):372-379. and Zhao Yanhui, Lang Wenchang, Xiao Jinquan, Gong Jun, Sun Chao electric arcs
Rotating transverse magnetic field arc source design [J] the vacuum sciences and Technology of ion plating, 2013,33 (4): 387-391.）
Etc. method, the bulky grain defect of film surface can be reduced to a certain extent, but can cause thin film preparation process parameter
Adjustable range is subject to certain restrictions.American scholar Anders is also proposed（Anders A. Growth and decay of
macroparticles: A feasible approach to clean vacuum arc plasmas. J Appl Phys,
1997, 82(8): 3679-3688）Using infrared laser come the method for assisted evaporative bulky grain, but process equipment into
This is too expensive.
6th, new method is introduced：Such as the high power combined pulsed magnetron sputtering ion implantation and deposition method of Chinese patent（It is public
The number of opening：CN101838795A, publication date：On September 22nd, 2010）The utilization high pressure and impulsive synchronization coalignment proposed is filled
Divide the advantage using high-power impulse magnetron sputtering, realize high-power impulse magnetron sputtering technology in the prominent of field ion implantation
It is broken, but be due to the limitation of high voltage power supply, the density for reaching matrix surface depositing ions can not be too high, otherwise can cause high-tension electricity
The damage in source.
The content of the invention
The invention aims to be also easy to produce bulky grain defect, Magnetic filter technology for solution conventional arc ion electroplating method to draw
Play arc-plasma efficiency of transmission low and using low melting point simple metal or multicomponent alloy material and nonmetallic materials（Such as stone
Ink）It is heavy as target bulky grain present in conventional arc ion electroplating method, conventional magnetron sputtering technology ionization level and film
The problem of efficiency is low for product, high-melting-point target is used limitation and current high-power impulse magnetron sputtering discharge instability, with eutectic
The simple metal or multicomponent alloy material and nonmetallic materials of point（Such as graphite）As the target of high-power impulse magnetron sputtering, then
The discharge instability phenomenon of hipims technology is eliminated using arc ions electroplating method, making for difficult ionization target is eliminated
With limitation and ion resorption effect to the adverse effect of thin film deposition, then pass through multi-stage magnetic field straight tube Magnetic filter method and eliminate electric arc
The bulky grain defect contained in plasma, at the same ensure arc-plasma with higher efficiency of transmission by filter,
Allow workpiece surface the situation for applying back bias voltage it is continuous, fine and close prepare high-quality thin-film, while realizing to element in film
Content addition control, reduction use the production cost of alloys target, the deposition efficiency for improving film, reduce discharge instability and big
Grain defect is to film growth and the adverse effect of performance, it is proposed that multi-stage magnetic field arc ion plating and high power pulse magnetic control splash
Penetrate composite deposition method.
The inventive method institute use device includes grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field dress
Put 4, high-power impulse magnetron sputtering power supply 5, high-power impulse magnetron sputtering target source 6, synchronous waveform coalignment 7, vacuum chamber
8th, sample stage 9, grid bias power supply kymographion 10 and high-power impulse magnetron sputtering power supply wave shape oscillograph 11；
This method comprises the following steps：
Step 1: pending workpiece is placed on the sample stage 9 in vacuum chamber 8, workpiece connects the pulse output of grid bias power supply 1
Arc power 2 is connected in end, the arc ion plating target source 3 on vacuum chamber 8, and high-power impulse magnetron sputtering target source 6 meets Gao Gong
The high power pulse output end of rate pulsed magnetron sputtering power supply 5；
Step 2: thin film deposition：Vacuum chamber 8 is vacuumized, treats that the vacuum in vacuum chamber 8 is less than 10-2During Pa, work is passed through
Make gas to 0.01Pa~10Pa, open synchronous waveform coalignment 7, the synchronous waveform exported according to grid bias power supply 1, which is triggered, to be believed
Number the high-power impulse magnetron sputtering power supply 5 is controlled to work；
Grid bias power supply 1 is opened, and it is 0~1.2kV to adjust the magnitude of voltage of the output pulse of grid bias power supply 1, pulse frequency is 0Hz
~80kHz, pulse width 1 ~ 90%；
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, regulation is needed
The technological parameter wanted, the current value that arc power 2 is exported is 10 ~ 300A, keeps arc-plasma to exist by multi-stage magnetic field device 4
Arc ion plating target source 3 is stable to be produced and carries out filtering elimination to bulky grain defect, makes arc-plasma with higher transmission
Efficiency reaches matrix surface by multi-stage magnetic field device 4, carries out the fast deposition of film；
High-power impulse magnetron sputtering power supply 5 is opened, the pre- ionization of direct current build-up of luminance is first passed through, technological parameter needed for regulation is high
The magnitude of voltage of the output pulse of Power Impulse Magnetron shielding power supply 5 is 300V~2500V, and pulse width is the μ s of 0 μ s~1000, pulse
10~1000Hz of frequency, electric current is 10~1000A；
Control the output voltage of grid bias power supply 1 and high-power impulse magnetron sputtering power supply 5 defeated by synchronous waveform coalignment 7
Go out voltage, it is the μ s of -1000 μ s~1000 to make both phase differences, it is ensured that effective attraction and ion of the matrix to metallic plasma
The regulation of energy, carries out simple metal film, the compound ceramic film of different element ratios, function film and with nanometer multilayer
Or prepared by the high-quality thin-film of gradient-structure.
Advantages of the present invention：A. using high-power impulse magnetron sputtering technology by high pressure low-frequency pulse realize target compared with
High metallic ionization level, it is not necessary to others auxiliary ionization device；B. high-power impulse magnetron sputtering technology is for eutectic
The simple metal or multicomponent alloy material of point do not produce bulky grain defect, therefore do not need filter, it is possible to achieve ionization ion
High efficiency of transmission；C. arc ion plating target source can make up the discharge instability and Gao Rong in high-power impulse magnetron sputtering target source
Point target is difficult to the limitation of ionization, it is ensured that the high density of depositing ions is persistently produced；D. multi-stage magnetic field magnetic filter can disappear
Except bulky grain defect and ensure the high efficiency of transmission of arc-plasma；E. as a result of synchronous waveform coalignment, it can make
Matrix effectively attracts the ion produced by high-power impulse magnetron sputtering target source, reduces high-power impulse magnetron sputtering technology pair
The resorption effect of produced ion, it is ensured that film deposition rate, greatly improves the energy of depositing ions；F. regulation is passed through
The technological parameter in high-power impulse magnetron sputtering target source, with reference to the technological parameter in arc ion plating target source, it is possible to achieve compound etc.
The ion ratio of various elements in gas ions, realizes the thin film deposition of different element ratios；G. the microstructure of prepared film
It can be adjusted with performance by pulsed bias parameter, high energy is realized using the amplitude, pulse width and frequency of pulsed bias
The pinning effect of ion pair film growth, improves the texture and stress state of film growth, improves film substrate bond strength；h.
Due to eliminating the simple metal or multicomponent alloy material and nonmetallic materials of low melting point（Such as graphite）In arc ion plating
Using limitation, it is possible to achieve the originally addition of these elements and being adjusted flexibly for ratio in multi-element film preparation process；I. it is made
Standby film avoids the bulky grain defect of low melting point element, and texture is finer and close, can further improve the power of film
Learn performance.
Step 3: Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating, multistage can be used individually
Magnetic field arc ion plating and the compound progress film of the compound bias of pulsed cathode arc combination Dc bias, pulsed bias or DC pulse
Deposition, to prepare simple metal film, the compound ceramic film of different element ratio, function film and with nanometer multilayer or ladder
Spend the high-quality thin-film of structure.
Brief description of the drawings
Fig. 1 is multi-stage magnetic field arc ion plating of the present invention and high-power impulse magnetron sputtering composite deposition method sketch, Fig. 2
For the timing chart of grid bias power supply, Fig. 3 synchronous waveform coalignments, Fig. 4 grid bias power supplies impulse waveform and high power pulse magnetic
Control sputtering impulse waveform integral multiple matching figure, grid bias power supply impulse waveform and high-power impulse magnetron sputtering during Fig. 5 outs of phase
Impulse waveform matching figure, grid bias power supply impulse waveform and high-power impulse magnetron sputtering impulse waveform during Fig. 6 difference pulse widths
Matching figure.
Embodiment
Embodiment one：Illustrate present embodiment, present embodiment multi-stage magnetic field electric arc with reference to Fig. 1 and Fig. 2
Ion plating and high-power impulse magnetron sputtering composite deposition method institute use device include grid bias power supply 1, arc power 2, electric arc from
Son plating target source 3, multi-stage magnetic field device 4, high-power impulse magnetron sputtering power supply 5, high-power impulse magnetron sputtering target source 6, waveform
Simultaneously match device 7, vacuum chamber 8, sample stage 9, grid bias power supply kymographion 10 and high-power impulse magnetron sputtering power supply ripple
Kymographion 11；
This method comprises the following steps：
Step 1: pending workpiece is placed on the sample stage 7 in vacuum chamber 8, workpiece connects the pulse output of grid bias power supply 1
End, the arc ion plating target source 3 on vacuum chamber 8 connects the output end of arc power 2；Magnetic controlled sputtering target source 4 connects high power arteries and veins
Rush the high power pulse output end of magnetron sputtering power supply 5；
Step 2: thin film deposition：Vacuum chamber 8 is vacuumized, treats that the vacuum in vacuum chamber 8 is less than 10-2During Pa, work is passed through
Make the pulsed bias synchronous triggering signal that gas is exported to 0.01Pa~10Pa, synchronous waveform coalignment 7 according to grid bias power supply 1
To control high-power impulse magnetron sputtering power supply 5 to work；
Grid bias power supply 1 is opened, and it is 0~1.2kV, pulse frequency to adjust the peak voltage of the output pulse of grid bias power supply 1
For 0Hz~80kHz, pulse width 5 ~ 90%；
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, regulation is needed
The technological parameter wanted, the current value that arc power 2 is exported is 10 ~ 300A, keeps arc-plasma to exist by multi-stage magnetic field device 4
Arc ion plating target source 3 is stable to be produced and carries out filtering elimination to bulky grain defect, makes arc-plasma with higher transmission
Efficiency reaches matrix surface by multi-stage magnetic field device 4, carries out the fast deposition of film；
High-power impulse magnetron sputtering power supply 5 is opened, the pre- ionization of direct current build-up of luminance is first passed through, technological parameter needed for regulation is high
The magnitude of voltage of the output pulse of Power Impulse Magnetron shielding power supply 5 is 300V~2500V, and pulse width is the μ s of 0 μ s~1000, pulse
10~1000Hz of frequency, electric current is 10~1000A；
Control the output voltage of grid bias power supply 1 and high-power impulse magnetron sputtering power supply 5 defeated by synchronous waveform coalignment 7
Go out voltage-phase, carry out thin film deposition.
Synchronous waveform coalignment 7 in present embodiment realized using two 1/2 CD4098 chips, physical circuit
Structure is shown in Figure 2, and the bias synchronous triggering signal that grid bias power supply 1 is exported is transferred to synchronous waveform coalignment 7, and waveform is same
The step output Remote triggering signal control high-power impulse magnetron sputtering of coalignment 7 power supply 5 works, synchronous waveform coalignment 7
Two power supply signal frequencies of grid bias power supply 1 and high-power impulse magnetron sputtering power supply 5 can be realized, it is possible to carry out different phases
The regulation of position.
During the pre- ionization of direct current build-up of luminance, chopped pulse starter time delay or make pulse starter easily, direct current
Current value changes according to power output, output voltage and the target area in high-power impulse magnetron sputtering target source 6, or directly gradually
Boosted output voltages value, makes the build-up of luminance of high-power impulse magnetron sputtering target source 6.
The output waveform of grid bias power supply 1 is direct current, pulse, DC pulse is compound or multiple-pulse is compound.
The output of arc power 2 direct current, pulse, DC pulse are compound or multiple-pulse is compound.
The output waveform of high-power impulse magnetron sputtering power supply 5 is direct current, pulse, DC pulse is compound or multiple-pulse is multiple
Close.
Arc ion plating target source 3 is using high-melting-point or the simple metal or multicomponent alloy material of low melting point, high power pulse magnetic
Control simple metal or multicomponent alloy material and nonmetallic materials of the sputtering target source 6 using low melting point（Especially semi-conducting material and absolutely
Edge material）, single target, multiple targets or composition target can be used, simple metal film, the compound ceramic of different element ratios is carried out
Film, function film, multi-component multi-layer, superlattices, the high-quality thin-film with nanometer multilayer or gradient-structure.
Working gas selects argon gas, or working gas to select one or more in nitrogen, acetylene, methane, silane or oxygen
Mixed gas, to prepare simple metal film, the compound ceramic film of different element ratio, function film, multi-component multi-layer, super
Lattice, the film with nanometer multilayer or gradient-structure.
The proposition of multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method, makes full use of Gao Gong
Sputtering target source carries out the generation and ionization of ion simultaneously in rate pulsed magnetron sputtering, breaks through the simple metal or multicomponent alloy of low melting point
Material and nonmetallic materials（Such as graphite）Application limitation in arc ion plating, is prevented effectively from produced by low melting material
Bulky grain problem；Control to apply back bias voltage and high-power impulse magnetron sputtering on workpiece using synchronous waveform coalignment simultaneously
Technological parameter, is conducive to improving the interval Potential Distributing of high-power impulse magnetron sputtering target source plasma, fully attracts Gao Gong
The ion that rate pulsed magnetron sputtering is produced solves high-power impulse magnetron sputtering intermediate ion resorption effect to workpiece motion s, effectively and led
Cause the problem of thin film deposition efficiency is low；High metal of the stable lasting, ionization level of generation of arc ion plating (aip) etc. is utilized simultaneously
Gas ions, make up the defect of high-power impulse magnetron sputtering technology discharge instability, are conducive to high ionization level ion in workpiece table
The chemosynthesis reaction in face, prepare the compound ceramic films of different element ratios, function film, multi-component multi-layer, superlattices and
Film or simple metal film with gradient-structure.
Embodiment two：The difference of present embodiment and embodiment one is, this method institute use device
Also include grid bias power supply kymographion 8 and high-power impulse magnetron sputtering power supply wave shape oscillograph 9, grid bias power supply waveform oscillography
Device 8 is used to show the voltage and current waveform that grid bias power supply 1 is sent, and high-power impulse magnetron sputtering power supply wave shape oscillograph 9 is used
The pulse voltage and current waveform sent in display high-power impulse magnetron sputtering power supply 5, other are identical with embodiment one.
Embodiment three：Illustrate present embodiment, the difference of present embodiment and embodiment one with reference to Fig. 3
Part is, during plated film, is controlled first to open grid bias power supply 1 by synchronous waveform coalignment 7, is then then turned on high power pulse magnetic
Shielding power supply 5 is controlled, other are identical with embodiment one.
Embodiment four：The difference of present embodiment and embodiment one is, is matched and filled by synchronous waveform
Put 7 control grid bias power supplies 1 and high-power impulse magnetron sputtering power supply 5 to open simultaneously, high-power impulse magnetron sputtering power supply 5 is exported
The cycle of pulse is the integral multiple that grid bias power supply 1 exports pulse, and other are identical with embodiment one.
As shown in figure 3, the pulse period that high-power impulse magnetron sputtering power supply 5 is exported is the pulse that grid bias power supply 1 is exported
10 times of cycle.
Embodiment five：Illustrate present embodiment, the difference of present embodiment and embodiment one with reference to Fig. 4
It is, the bias pulse waveform phase that the output high-power pulse of high-power impulse magnetron sputtering power supply 5 and grid bias power supply 1 are exported can
Adjust, in same pulse width, different phase differences allows two power supply output pulse waveforms all to overlap, partially overlap or not
Overlap, so that according to the Proper Match of two power pulses of process choice of thin film deposition, other are identical with embodiment one.
Embodiment six：Illustrate present embodiment with reference to Fig. 5 and Fig. 6, present embodiment and embodiment one are not
It is with part, the pulse width of the output high-power pulse of high-power impulse magnetron sputtering power supply 5 and the output pulse of grid bias power supply 1
Independently adjustable, different pulse widths causes the output pulse waveform of two power supplys to be covered with the former before the latter, the latter's covering
Person is completely superposed, and carries out different thin film deposition processes selections, other are identical with embodiment one.
Embodiment seven：The difference of present embodiment and embodiment one is that this method also includes：
Step 3: Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating, multistage can be used individually
Magnetic field arc ion plating and the compound bias of pulsed cathode arc combination Dc bias, pulsed bias or DC pulse carry out film and sunk
Product, to prepare simple metal film, the compound ceramic film of different element ratio, function film and with nanometer multilayer or gradient
The high-quality thin-film of structure；
First magnetron sputtering, which can be carried out, in step 2 using high-power impulse magnetron sputtering power supply 5 combines high-tension pulse
Grid bias power supply carries out ion implantation and deposition, improves the adhesion of film and matrix, then carries out step 3, obtains certain thickness
Film.
Embodiment eight：The difference of present embodiment and embodiment seven is, perform repeatedly step one to
Step 3, prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment seven
It is identical.
First magnetron sputtering combination high pressure, which can be carried out, in step 2 using high-power impulse magnetron sputtering power supply 5 carries out ion
Injection and deposition, improve the adhesion of film and matrix, then carry out step 3, step 2 and step 3 are then performed repeatedly,
So repeatedly, the multilayer films with different stress, microstructure and element ratio are prepared.
Embodiment nine：The difference of present embodiment and embodiment one is, perform repeatedly step one to
Step 3, prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment seven
It is identical.
The electric arc that 2 sets or the arc ion plating target source 3 of the above and multi-stage magnetic field device 4 can be used to coordinate in step 2
Ion plating apparatus is carried out using various simple metal elements and multicomponent alloy material as the thin film deposition of target, then carries out step 3,
Then step 2 and step 3 are performed repeatedly, so repeatedly, are prepared with different stress, microstructure and element ratio
Multilayer films.
Claims (6)
1. multi-stage magnetic field arc ion plating and high-power impulse magnetron sputtering composite deposition method, it is characterised in that this method institute
Use device is splashed including grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field device 4, high power pulse magnetic control
Radio source 5, high-power impulse magnetron sputtering target source 6, synchronous waveform coalignment 7, vacuum chamber 8, sample stage 9, grid bias power supply ripple
Kymographion 10 and high-power impulse magnetron sputtering power supply wave shape oscillograph 11；
This method comprises the following steps：
Step 1: pending substrate work-piece is placed on the sample stage 9 in vacuum chamber 8, workpiece connects the output end of grid bias power supply 1,
Arc ion plating target source 3 on vacuum chamber 8 connects the output end of arc power 2, high-power impulse magnetron sputtering target source 6 and connects height
The high power pulse output end of Power Impulse Magnetron shielding power supply 5；
Step 2: thin film deposition：Vacuum chamber 8 is vacuumized, treats that the vacuum in vacuum chamber 8 is less than 10-2During Pa, work gas is passed through
Body opens grid bias power supply 1 to 0.01Pa~10Pa, and adjusts the bias amplitude of the output of grid bias power supply 1, and pulse frequency and pulse are wide
Degree, opens grid bias power supply 1, and it is 0~1.2kV to adjust the peak voltage of the output pulse of grid bias power supply 1, and pulse frequency is 0Hz
~80kHz, pulse width 1 ~ 90%；
Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, what regulation needed
Technological parameter, the current value that arc power 2 is exported is 10 ~ 300A, and arc-plasma is kept in electric arc by multi-stage magnetic field device 4
Ion plating target source 3 is stable to be produced and carries out filtering elimination to bulky grain defect, makes arc-plasma with higher efficiency of transmission
Matrix surface is reached by multi-stage magnetic field device 4, the fast deposition of film is carried out；High-power impulse magnetron sputtering power supply 5 is opened,
First pass through direct current build-up of luminance and pre- ionization is carried out to working gas, the surface of high-power impulse magnetron sputtering target source 6 is cleaned；Open
Synchronous waveform coalignment 7, the synchronous triggering signal exported according to grid bias power supply 1, is controlled by synchronous waveform coalignment 7
The work of high-power impulse magnetron sputtering power supply 5, is configured to required technological parameter, high-power impulse magnetron sputtering power supply
The magnitudes of voltage of 5 output pulses are 300V~2500V, and pulse width is 0 μ s~1000 μ s, 10~1000Hz of pulse frequency, electric current
For 10~1000A, the phase of the control output voltage of grid bias power supply 1 and the output voltage of high-power impulse magnetron sputtering power supply 5, it is ensured that
Effective attraction and the regulation of ion energy of the matrix to metallic plasma, carry out the deposition of film and control the proof gold of low melting point
The ratio of category or multicomponent alloy material and nonmetallic materials in the film；Grid bias power supply kymographion 10 and high power pulse magnetic
Control shielding power supply kymographion 11, grid bias power supply kymographion 10 be used to showing the pulse voltage that grid bias power supply 1 is sent and
Current waveform, high-power impulse magnetron sputtering power supply wave shape oscillograph 11 is used to show that high-power impulse magnetron sputtering power supply 5 is sent out
The pulse voltage and current waveform gone out, is controlled by synchronous waveform coalignment 7 while opening the high power pulse magnetic control of grid bias power supply 1
Shielding power supply 5, the cycle of the output pulse of high-power impulse magnetron sputtering power supply 5 exports the integral multiple of pulse for grid bias power supply 1；So
After be then turned on arc power 2 and multi-stage magnetic field device 4 and carry out thin film deposition.
2. multi-stage magnetic field arc ion plating according to claim 1 and high-power impulse magnetron sputtering composite deposition method,
Characterized in that, the output pulse of high-power impulse magnetron sputtering power supply 5 is pulse, DC pulse is compound or multiple-pulse is compound,
The electric current that arc power 2 is exported is direct current, pulse or DC pulse are compound, and realizes that bulky grain lacks by multi-stage magnetic field device 4
Sunken removing and the high efficiency of transmission of arc-plasma；The output pulse of grid bias power supply 1 is pulse, DC pulse is compound or many arteries and veins
Punching is compound, and the waveform parameter of the output of high-power impulse magnetron sputtering power supply 5 is controlled by synchronous waveform coalignment 7.
3. multi-stage magnetic field arc ion plating according to claim 1 and high-power impulse magnetron sputtering composite deposition method,
Characterized in that, this method also includes：
Step 3: individually using the compound bias of Traditional DC magnetron sputtering combination Dc bias, pulsed bias or DC pulse, arteries and veins
Rush magnetron sputtering combination Dc bias, the compound bias of pulsed bias or DC pulse, conventional arc ion plating combination Dc bias,
Pulsed bias or the compound bias of DC pulse, the compound bias of pulsed cathode arc combination Dc bias, pulsed bias or DC pulse
Thin film deposition is carried out, to prepare simple metal film, the compound ceramic film of different element ratio, function film and with nanometer
The film of multilayer or gradient-structure.
4. multi-stage magnetic field arc ion plating according to claim 1 and high-power impulse magnetron sputtering composite deposition method,
Characterized in that, perform step one repeatedly to step 2, come prepare simple metal film, different element ratios compound ceramic it is thin
Film, function film and the film with nanometer multilayer or gradient-structure.
5. multi-stage magnetic field arc ion plating according to claim 1 and high-power impulse magnetron sputtering composite deposition method,
Characterized in that, simple metal or multicomponent alloy target of the target body material that uses of high-power impulse magnetron sputtering target source 6 for low melting point
Material and nonmetallic materials, arc ion plating target source 3 are difficult to the high-melting-point simple metal of ionization or polynary conjunction using magnetron sputtering technique
Golden material, also effectively avoids the proof gold using low melting point using multi-stage magnetic field device 4 using conventional arc ion plating technique
Category or multicomponent alloy target and nonmetallic materials.
6. multi-stage magnetic field arc ion plating according to claim 1 and high-power impulse magnetron sputtering composite deposition method,
Characterized in that, working gas selects argon gas, or working gas to select a kind of or many in nitrogen, acetylene, methane, silane or oxygen
Kind mixed gas, to prepare simple metal film, the compound ceramic film of different element ratio, function film and with nanometer
The film of multilayer or gradient-structure.
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