CN104975263A - Multi-stage magnetic field arc ion plating and radio-frequency magnetron sputtering composite deposition method - Google Patents
Multi-stage magnetic field arc ion plating and radio-frequency magnetron sputtering composite deposition method Download PDFInfo
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Abstract
The invention provides a multi-stage magnetic field arc ion plating and radio-frequency magnetron sputtering composite deposition method and belongs to the technical field of material surface processing. The method aims to solve the problem that low-melting-point pure metal or multicomponent alloy materials and non-metal materials, such as graphite are large in particle in traditional arc ion plating, breaking through the limitations that semiconductor materials and insulating materials can not be used, the ionization rate and thin film deposition efficiency of traditional magnetron sputtering are low and high- melting-point targets are difficult to ionize, and eliminating the limitations of an original method in the aspect of use of the targets. The composite deposition method includes the steps that 1, a workpiece to be plated is placed on a sample table in a vacuum room, and a relative power source is powered on; 2, a thin film is deposited, wherein when the vacuum degree in the vacuum room is smaller than 10-4Pa, work gas is introduced, gas pressure is adjusted, a plating power source is powered on, and energy of a composite plasma is adjusted through a grid bias power supply. By means of a multi-stage magnetic field straight tube magnetic filter device, the defect of large particles is overcome, transmission efficiency of arc plasmas is guaranteed, and required process parameters are set for thin film deposition.
Description
Technical field
The present invention relates to multi-stage magnetic field arc ion plating and rf magnetron sputtering composite deposition method, belong to technical field of material surface treatment.
Background technology
Arc ion plating (aip) can obtain the nearly all metal ion comprising carbon ion, simultaneously with high ionization level, diffractive good, the advantage such as film-substrate cohesion is good, coating quality is good, sedimentation effect is high and operation of equipment is easy and coming into one's own, it is one of physical vapor deposition technology of preparing of being used widely in the industry at present.It not only may be used for preparing metal protection coating, by the adjustment of processing method, can also realize the preparation of the high-temperature ceramic coating such as nitride, carbide, also has application in function film field simultaneously.Even if for the component that shape is irregular, arc ion plating also can realize the fast deposition of film, even also 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 prepare in the process of film at arc ion plating, because arc spot current density is up to 2.5 ~ 5 × 10
10a/m
2the arc spot position of target material surface is caused to occur the liquid metal of melting, under the effect of local plasma pressure with the form splash of drop out, be attached to film surface or inlay and form " macrobead " (Macroparticles) defect (Boxman R L in the film, Goldsmith S. Macroparticle contamination in cathodic arc coatings:generation, transport and control [J]. Surf Coat Tech, 1992,52 (1): 39-50.).Just as PM2.5 is to the pollution of Air quality, be the film of micron or submicron relative to thickness rank, size has serious harm at the quality and performance of macrobead defect to film of 0.1-10 micron.Increasingly extensive along with thin-film material and thin film technique application, whether the solution of macrobead defect problem becomes the bottleneck that arc ions electroplating method further develops, and seriously constrains its application in thin-film material preparation of new generation.
Originally magnetron sputtering technique adopts direct current supply pattern, compared to arc ions electroplating method, does not have macrobead defect, and can realize the low-temperature sputter deposition of various material, but the ionization level of its sputter material is very low, the power density of sputtering target is at 50W/cm
2, can not get enough ion populations during thin film deposition, cause sedimentation effect very low, simultaneously ion with energy lower, make Thin Film Tissue fine and close not.1999, people (the Kouznetsov V such as the V. Kouznetsov of Linkoping,Sweden university, Mac á k 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.) high-power impulse magnetron sputtering technology (HPPMS) is proposed, it utilizes higher pulse peak power and lower pulse width to improve the ionization level of sputter material, target cathode can not increase the requirement of target cooling because of overheated simultaneously.Its peak power improves 100 times compared to conventional DC magnetron sputtering, is about 1000 ~ 3000W/cm
2, the density of plasma body reaches 10
18m
-3the order of magnitude, its central region ion density can reach 10
19m
-3the order of magnitude, the ionization level of sputter material reaches as high as more than 90% simultaneously, and does not contain the macrobead defect in the highest arc ions electroplating method of current ionization level.After 2008, at home each colleges and universities also start launch for high-power impulse magnetron sputtering technology research (Li Xiping. high power combined pulsed magnetron sputtering plasma characteristics and TiAlN thin film preparation [D], Harbin Institute of Technology, 2008. Wuzhong shakes, Zhu Zongtao, Gong Chunzhi, Tian Xiubo, Yang Shiqin, Li Xiping. the development and research [J] of high-power impulse magnetron sputtering technology. vacuum, 2009, 46 (3): 18-22. and Mu Zongxin, Mu Xiaodong, Wang Chun, Jia Li, Dong Chuan. direct supply coupling high power pulse non-balance magnetically controlled sputter ionization property [J]. Acta Physica Sinica, 2011, 60 (1): 422-428.), but because the impulsive discharge of high-power impulse magnetron sputtering technology is unstable, and target current potential is lower, the metal ion a large amount of after ionization of target metal is sucked back into target surface, fail to arrive the deposition that matrix surface realizes film, the efficiency of thin film deposition is caused greatly to reduce, affect the paces that it replaces common magnetron sputtering and arc ion plating further, a definite limitation is received in follow-up applying.
At present, using the pure metal of low melting point or multicomponent alloy material easily to produce macrobead defect and magnetron sputtering technique is using the problem existing in high-melting-point target and be difficult to ionization to solve arc ions electroplating method, mainly containing several as follows at present:
The first: adopt the way of Magnetic filter to filter out macrobead, as Chinese patent is used for the plasma immersion and ion implantation device (publication number: CN1150180 of material surface modifying, publication date: on May 21st, 1997) in adopt the macrobead of 90 ° of magnetic filter paired pulses cathode arcs to filter, the people such as American scholar Anders (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 (Zhang Yujuan such as the Zhang Yujuan of He'nan University, Wu Zhiguo, Zhang Weiwei etc. filtered cathode arc plasma to prepare in TiAlN thin film mode of deposition to the impact of film texture. China YouSe Acta Metallurgica Sinica. 2004, 14 (8): 1264-1268.) macrobead having made " S " magnetic filter anticathode arc in article filters, also have people (the Anders A such as American scholar Anders, MacGill R A. Twist filter for the removal of macroparticles from cathodic arc plasmas [J]. Surf Coat Tech, 2000, 133-134:96-100.) Magnetic filter of Twist filter that proposes, although these methods have certain effect in filtration and elimination macrobead, but the loss of the transmission efficiency of plasma body is serious, ion current density is reduced greatly.Again can on the basis of guaranteed efficiency based on macrobead can be filtered, Chinese patent vacuum cathode arc straight tube filter (publication number: CN1632905, publication date: on June 29th, 2005) the middle method proposing straight tube and filter, but which in turn reduces filter effect.In a word, relevant researchist by the various Magnetic filter method of contrast (Anders A. Approaches to rid cathodic arc plasmas of macro-and nanoparticles:a review [J]. Surf Coat Tech, 1999, 120-121319-330. with 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 that arc ion plating plasma body is very difficult to take into account by keeping high transmission efficiency after magnetic filter and eliminating macrobead, drastically influence the application of this technology in high-quality thin-film deposition.
Second, adopt the method stopping shielding, before arc ion plating target source, such as directly adopt baffle plate to shield macrobead (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 the difference of macrobead and arc plasma transmission speed, a high speed rotating unit (Utsumi T is applied outside arc source, 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 paddle, realize filtering the stop of macrobead defect; Or hole is drilled with on baffle plate, by adjusting the spacing of two-layer baffle plate so that the transmission of arc plasma, stop that macrobead deposits to dual-layered baffle plate shielding unit (the Zhao Y of film surface, 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.); Also have by regulating fender angle eliminate oarse-grained flap type shielding unit (Zimmer O. Vacuum arc deposition by using a Venetian blind particle filter [J]. Surf Coat Tech, 2005,200 (1-4): 440-443.).Stop that shielding is by restriction macrobead and the movement path of plasma body, utilize good diffractive of arc plasma to prepare film, but the method can cause the transmission efficiency loss of plasma body serious, receives certain restriction in actual applications.
3rd, matrix adopts the electric field suppressing method of bias voltage, and in arc plasma, the movement velocity due to electronics is far longer than the movement velocity of ion, and the electronic number arriving large particle surface in the unit time is greater than number of ions, makes macrobead present electronegativity.When matrix applying negative bias, electric field will produce repulsive interaction to electronegative macrobead, and then reduce the generation of film surface macrobead defect.The people such as German scholar Olbrich (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.) adopt pulsed bias to replace traditional direct current (DC) bias, define a kind of new physical gas phase deposition technology---pulsed bias arc ion plating technology, not only greatly reduce the oarse-grained number of film surface, also overcome the substrate temperature that Traditional DC bias voltage causes too high, the problems such as stress in thin films is larger.The people such as the woods Guoqiang of Dalian University of Technology (woods Guoqiang. Process ba-sis research [D] of pulsed bias arc ion plating. Dalian University of Technology, 2008. and Huang Meidong, woods Guoqiang, Dong Chuan, Sun Chao, hear immediately. the Influencing Mechanism [J] of Bias On Morphologies of Films Prepared By Arc Ion Plating. Acta Metallurgica Sinica, 2003, 39 (5): 510-515.) mechanism causing macrobead defect to reduce for pulsed bias conducts in-depth analysis, by paired pulses bias voltage amplitude, the adjustment of the processing parameter such as frequency and pulse width, the sheaths motion characteristics of arc plasma can be improved, reduce the macrobead defect counts of film surface, improve the quality of film, be widely used in the production of reality, but still can not eliminate macrobead defect completely.
4th, the optimization of processing parameter, by adjustment operating air pressure (Brown I G. Cathodic arc deposition of films. Ann Rev Mater Sci, 1998, 28 (1): 243-269. and Chen Kangmin, open lemon dawn, Zheng Chenchao, Huang Yan, Guan Qingfeng, Gong Lei, Sun Chao. nitrogen partial pressure is on the impact [J] of arc ion plating CrNx organization structure of film. vacuum science and technology journal, 2010, 30 (6): 662-666.) and utilize Magnetic control spots moving (Lang Wenchang, Xiao Jinquan, Gong Jun, Sun Chao, Huang Rongfang, to hear immediately. axisymmetrical magnetic field is on the impact of arc ion plating spots moving. Acta Metallurgica Sinica, 2010, 46 (3): 372-379. and Zhao Yanhui, Lang Wenchang, Xiao Jinquan, Gong Jun, Sun Chao. rotating transverse magnetic field arc source design [J] of arc ion plating. vacuum science and technology journal, 2013, 33 (4): 387-391.) method such as, the macrobead defect of film surface can be reduced to a certain extent, but the regulation range of thin film preparation process parameter can be caused to be subject to certain restrictions.American scholar Anders also proposes (Anders A. Growth and decay of macroparticles:A feasible approach to clean vacuum arc plasmas. J Appl Phys, 1997,82 (8): 3679-3688) adopt infrared laser to carry out the oarse-grained method of assisted evaporative, but the cost of processing unit is too expensive.
6th, novel method is introduced: pulsed magnetron sputtering ion implantation and deposition method (publication number: CN101838795A as high power combined in Chinese patent, publication date: on September 22nd, 2010) utilize high pressure and the pulse synchronization matching set that propose make full use of the advantage of high-power impulse magnetron sputtering, realize the breakthrough of high-power impulse magnetron sputtering technology at field ion implantation, but due to the restriction of high-voltage power supply, the density arriving matrix surface depositing ions can not be too high, otherwise can cause the damage of high-voltage power supply.
In a word, in order to expand existing arc ion plating and magnetron sputtering two kinds of methods in target use limitation separately, make full use of current rf magnetron sputtering and do not require that the target as electrode is conduction, namely utilize rf magnetron sputtering can any material of sputtering sedimentation, comprise semi-conductor and insulating material (Kelly, P. J., J. Hisek, Y. Zhou, R. D. Pilkington, R. D. Arnell. Advanced Coatings Through Pulsed Magnetron Sputtering. Surface Engineering, 2004, 20 (3): 157-162), arc ions is plated in the advantage of high-melting-point and the use of difficult ionization target aspect simultaneously, in conjunction with multi-stage magnetic field straight tube Magnetic filter, macrobead is eliminated and the guarantee of Plasma Transport efficiency, realize preparing various material, the film of component proportions and structure.
Summary of the invention
The present invention seeks to easily produce macrobead defect for solving conventional arc ion electroplating method, Magnetic filter technology causes the macrobead that arc plasma transmission efficiency is low and adopt the pure metal of low melting point or multicomponent alloy material and non-metallic material (such as graphite) to exist in conventional arc ion electroplating method as target, conventional magnetron sputtering technology ionization level and thin film deposition efficiency low, the limitation that high-melting-point target uses, using the pure metal of low melting point or multicomponent alloy material and non-metallic material (especially semiconductor material and insulating material) as the target of rf magnetron sputtering, recycling arc ions electroplating method can produce continually and steadily, the plasma body of high ionization level, eliminated the macrobead defect contained in arc plasma by multi-stage magnetic field straight tube Magnetic filter method simultaneously, ensure that arc plasma passes through filtration unit with higher transmission efficiency simultaneously, make workpiece surface apply the situation of negative bias can be continuous, fine and close prepares high-quality thin-film, realize adding constituent content in film controlling simultaneously, reduce the production cost using alloys target, improve the sedimentation effect of film, reduce discharge instability and the macrobead defect disadvantageous effect to film growth and performance, propose multi-stage magnetic field arc ion plating and rf magnetron sputtering composite deposition method.
The inventive method institute using appts comprises grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field device 4, rf magnetron sputtering power supply 5, rf magnetron sputtering target source 6, vacuum chamber 7, sample table 8 and grid bias power supply kymographion 9;
The method comprises the following steps:
Step one, be placed in pending workpiece in vacuum chamber 7 sample table 8 on, workpiece connects the pulse output end of grid bias power supply 1, arc power 2 is connected in the arc ion plating target source 3 be arranged on vacuum chamber 7, and rf magnetron sputtering target source 6 connects the high power pulse output terminal of rf magnetron sputtering power supply 5;
Step 2, thin film deposition: vacuumized by vacuum chamber 7, treat that the vacuum tightness in vacuum chamber 7 is less than 10
-4during Pa, pass into working gas to 0.01Pa ~ 10Pa, open grid bias power supply kymographion 9, the waveform parameter that grid bias power supply 1 exports is adjusted in time;
Open grid bias power supply 1, and the magnitude of voltage regulating grid bias power supply 1 to export pulse is 0 ~ 1.2kV, pulse-repetition is 0Hz ~ 80kHz, pulse width 1 ~ 90%;
Open arc power 2, cleaned by the surface of spots moving to arc ion plating target source 3 of electric arc, regulate the processing parameter needed, the current value that arc power 2 exports is 10 ~ 300A, keep arc plasma in the stable generation in arc ion plating target source 3 by multi-stage magnetic field device 4 and filtration elimination is carried out to macrobead defect, make arc plasma arrive matrix surface with higher transmission efficiency by multi-stage magnetic field device 4, carry out the fast deposition of film;
Open rf magnetron sputtering power supply 5, carry out filament pre-heating, after adjusting output rating and reflective power, make rf magnetron sputtering target source 6 build-up of luminance, surface, film by RF magnetron sputtering target source 6 is cleaned, and the radio frequency of rf magnetron sputtering power supply 5 is 5 ~ 30MHz, adopt general 13.56MHz, by the operating power that adjustment rf magnetron sputtering power supply 5 exports, operating voltage and working current, produce stable radio-frequency plasma;
According to the needs of film preparation, the processing parameter that adjustment is relevant carries out pure metal film, the compound ceramic film of different element ratio, function film and has the high-quality thin-film preparation of nanometer multilayer or gradient-structure.
Advantage of the present invention: a. adopts radiofrequency magnetron sputtering technology not produce macrobead defect for the pure metal of low melting point or multicomponent alloy material, does not therefore need filtration unit, can realize the high efficiency of transmission of ionization ion; B. arc ion plating target source can make up rf magnetron sputtering is difficult to ionization restriction to high-melting-point target, ensures that the high-density of depositing ions continues to produce; C. multi-stage magnetic field magnetic filter can be eliminated macrobead defect and ensure the high efficiency of transmission of arc plasma; D. owing to have employed pulsed bias Waveform output device, the ion that matrix can be made effectively to attract rf magnetron sputtering target source produce, ensure that film deposition rate, the energy of depositing ions is improved greatly; E. by regulating the processing parameter in rf magnetron sputtering target source, in conjunction with the processing parameter in arc ion plating target source, the ion ratio of various element in compound plasma can be realized, realizing the thin film deposition of different element ratio; F. the microstructure and properties of prepared film can be adjusted by pulsed bias parameter, the amplitude of pulsed bias, pulse width and frequency is utilized to realize the pinning effect of energetic ion to film growth, improve crystalline structure and the stressed condition of film growth, improve bonding strength; G. because rf magnetron sputtering eliminates the pure metal of low melting point or multicomponent alloy material and non-metallic material (especially semiconductor material and the insulating material) application limitations in arc ion plating, the interpolation of these elements in original multi-element film preparation process and the film of ratio adjustment can be realized; H. prepared film avoids the macrobead defect of low melting point element, and crystalline structure is finer and close, can improve the mechanical property of film further.
Step 3, Traditional DC magnetron sputtering, pulsed magnetron sputtering, conventional arc ion plating, multi-stage magnetic field arc ion plating and pulsed cathode arc can be adopted separately to carry out thin film deposition in conjunction with direct current (DC) bias, pulsed bias or DC pulse compound bias voltage compound, prepare pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Accompanying drawing explanation
Fig. 1 is multi-stage magnetic field arc ion plating of the present invention and rf magnetron sputtering composite deposition method sketch, and Fig. 2 is the timing chart of grid bias power supply.
Embodiment
Embodiment one: present embodiment is described below in conjunction with Fig. 1 and Fig. 2, present embodiment multi-stage magnetic field arc ion plating and rf magnetron sputtering composite deposition method institute using appts comprise grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field device 4, rf magnetron sputtering power supply 5, rf magnetron sputtering target source 6, vacuum chamber 7, sample table 8 and grid bias power supply kymographion 9;
The method comprises the following steps:
Step one, be placed in pending workpiece in vacuum chamber 7 sample table 7 on, workpiece connects the pulse output end of grid bias power supply 1, and the arc ion plating target source 3 be arranged on vacuum chamber 7 connects the output terminal of arc power 2; Rf magnetron sputtering target source 6 connects the output terminal of rf magnetron sputtering power supply 5;
Step 2, thin film deposition: vacuumized by vacuum chamber 7, treat that the vacuum tightness in vacuum chamber 7 is less than 10
-4during Pa, pass into working gas to 0.01Pa ~ 10Pa;
Open grid bias power supply 1, and the peak voltage regulating grid bias power supply 1 to export pulse is 0 ~ 1.2kV, pulse-repetition is 0Hz ~ 80kHz, pulse width 5 ~ 90%;
Open arc power 2, cleaned by the surface of spots moving to arc ion plating target source 3 of electric arc, regulate the processing parameter needed, the current value that arc power 2 exports is 10 ~ 300A, keep arc plasma in the stable generation in arc ion plating target source 3 by multi-stage magnetic field device 4 and filtration elimination is carried out to macrobead defect, make arc plasma arrive matrix surface with higher transmission efficiency by multi-stage magnetic field device 4, carry out the fast deposition of film;
Open rf magnetron sputtering power supply 5, carry out filament pre-heating, after adjusting output rating and reflective power, make rf magnetron sputtering target source 6 build-up of luminance, surface, film by RF magnetron sputtering target source 6 is cleaned, and the radio frequency of rf magnetron sputtering power supply 5 is 5 ~ 30MHz, adopt general 13.56MHz, by the operating power that adjustment rf magnetron sputtering power supply 5 exports, operating voltage and working current, produce stable radio-frequency plasma;
Grid bias power supply 1 output waveform is direct current, monopulse, DC pulse compound or multipulse compound.
Arc power 2 exports direct current, monopulse, DC pulse compound or multipulse compound.
Arc ion plating target source 3 adopts pure metal or the multicomponent alloy material of high-melting-point or low melting point, rf magnetron sputtering target source 6 adopts the pure metal of low melting point or multicomponent alloy material and non-metallic material (especially semiconductor material and insulating material), single target, multiple target or composition target can be used, carry out pure metal film, the compound ceramic film of different element ratio, function film, multi-component multi-layer, superlattice, there is the high-quality thin-film of nanometer multilayer or gradient-structure.
Working gas selects argon gas, or working gas to select in nitrogen, acetylene, methane, silane or oxygen one or more mixed gas, prepare pure metal film, the compound ceramic film of different element ratio, function film, multi-component multi-layer, superlattice, there is the film of nanometer multilayer or gradient-structure.
The proposition of multi-stage magnetic field arc ion plating and rf magnetron sputtering composite deposition method, make full use of the popularity of rf magnetron sputtering to sputtering target select materials, achieve the pure metal of low melting point or multicomponent alloy material and non-metallic material (especially semiconductor material and the insulating material) application in arc ion plating, effectively avoid the macrobead problem that low melting material produces, breach again non-metallic material (especially semiconductor material and the insulating material) application limitations in arc ion plating; Utilize Waveform output device to adjust in time on workpiece simultaneously apply negative bias parameter, be conducive to improving the interval Potential Distributing of plasma body between target base, fully attract compound plasma to workpiece motion s, realize the fast deposition of film; Also utilize the generation of arc ion plating (aip) to stablize lasting, that ionization level is high metallic plasma simultaneously, decrease high-melting-point, restriction that the metallic substance of difficult ionization uses in magnetron sputtering, be conducive to the chemosynthesis reaction of high ionization level ion at workpiece surface, prepare the compound ceramic film of different element ratio, function film, multi-component multi-layer, superlattice and there is film or the pure metal film of gradient-structure.
Embodiment two: the difference of present embodiment and embodiment one is, the method also comprises:
Step 3, Traditional DC magnetron sputtering, pulsed magnetron sputtering, high-power impulse magnetron sputtering, conventional arc ion plating, multi-stage magnetic field arc ion plating and pulsed cathode arc can be adopted separately to carry out thin film deposition in conjunction with direct current (DC) bias, pulsed bias or DC pulse compound bias voltage, prepare pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure;
Rf magnetron sputtering power supply 5 first can be used in step 2 to carry out magnetron sputtering and to carry out ion implantation and deposition in conjunction with high-tension pulsed bias power supply, improve the bonding force of film and matrix, then carry out step 3, obtain certain thickness film.
Embodiment three: the difference of present embodiment and embodiment two is, repeatedly perform step one to step 3, preparation has the multilayer films of different stress, microtexture and element ratio, and other are identical with embodiment two.
Rf magnetron sputtering power supply 5 first can be used in step 2 to carry out magnetron sputtering and to carry out ion implantation and deposition in conjunction with high pressure, improve the bonding force of film and matrix, then step 3 is carried out, then repeatedly step 2 and step 3 is performed, so repeatedly, preparation has the multilayer films of different stress, microtexture and element ratio.
Embodiment four: the difference of present embodiment and embodiment one is, repeatedly perform step one to step 3, preparation has the multilayer films of different stress, microtexture and element ratio, and other are identical with embodiment two.
The thin film deposition that it is target that the arc ion plating apparatus that 2 covers or above arc ion plating target source 3 and multi-stage magnetic field device 4 can be used in step 2 to coordinate carries out with various pure metal element and multicomponent alloy material, then step 3 is carried out, then repeatedly step 2 and step 3 is performed, so repeatedly, preparation has the multilayer films of different stress, microtexture and element ratio.
Claims (7)
1. multi-stage magnetic field arc ion plating and rf magnetron sputtering composite deposition method, it is characterized in that, the method institute using appts comprises grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field device 4, rf magnetron sputtering power supply 5, rf magnetron sputtering target source 6, vacuum chamber 7, sample table 8 and grid bias power supply kymographion 9;
The method comprises the following steps:
Step one, be placed in pending substrate work-piece in vacuum chamber 7 sample table 8 on, workpiece connects the output terminal of grid bias power supply 1, the high power pulse output terminal that the arc ion plating target source 3 be arranged on vacuum chamber 7 connects the output terminal of arc power 2, rf magnetron sputtering target source 6 connects rf magnetron sputtering power supply 5;
Step 2, thin film deposition: vacuumized by vacuum chamber 7, treat that the vacuum tightness in vacuum chamber 7 is less than 10
-4during Pa, pass into working gas to 0.01Pa ~ 10Pa, open grid bias power supply 1 and grid bias power supply kymographion 9, and the bias voltage amplitude regulating grid bias power supply 1 to export, pulse-repetition and pulse width, the peak voltage that grid bias power supply 1 exports pulse is 0 ~ 1.2kV, and pulse-repetition is 0Hz ~ 80kHz, pulse width 1 ~ 90%;
Open arc power 2, cleaned by the surface of spots moving to arc ion plating target source 3 of electric arc, regulate the processing parameter needed, the current value that arc power 2 exports is 10 ~ 300A, keep arc plasma in the stable generation in arc ion plating target source 3 by multi-stage magnetic field device 4 and filtration elimination is carried out to macrobead defect, make arc plasma arrive matrix surface with higher transmission efficiency by multi-stage magnetic field device 4, carry out the fast deposition of film;
Open rf magnetron sputtering power supply 5, carry out filament pre-heating, after adjusting output rating and reflective power, make rf magnetron sputtering target source 6 build-up of luminance, surface, film by RF magnetron sputtering target source 6 is cleaned, and the radio frequency of rf magnetron sputtering power supply 5 is 5 ~ 30MHz, adopt general 13.56MHz, by the operating power that adjustment rf magnetron sputtering power supply 5 exports, operating voltage and working current, produce stable radio-frequency plasma.
2. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, it is characterized in that, the method institute using appts also comprises grid bias power supply kymographion 9 for the pulsed voltage that shows grid bias power supply 1 and send and current waveform, by adjusting the output waveform of grid bias power supply 1, plated film ion is effectively attracted, carry out the deposition of film and control low melting point and non-metallic material (especially semiconductor material and insulating material) ratio in the film, realizing the adjustment of plasma energy.
3. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, is characterized in that, it is monopulse, DC pulse compound or multipulse compound that grid bias power supply 1 exports pulse.
4. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, it is characterized in that, the method also comprises:
Step 3, Traditional DC magnetron sputtering, pulsed magnetron sputtering, high-power impulse magnetron sputtering, conventional arc ion plating and pulsed cathode arc can be adopted separately to carry out thin film deposition in conjunction with direct current (DC) bias, pulsed bias or DC pulse compound bias voltage, prepare pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
5. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, it is characterized in that, repeatedly perform step one to step 2, prepare pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
6. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, it is characterized in that, the target body material that rf magnetron sputtering target source 6 adopts can be pure metal or the multicomponent alloy target of low melting point, and arc ion plating target source 3 can not adopt non-metal semiconductor materials and insulating material, and arc ion plating target source 3 can for high-melting-point pure metal or the multicomponent alloy material adopting magnetron sputtering technique to be difficult to ionization, also can effectively utilize multi-stage magnetic field device 4 and adopt conventional arc ion plating technique avoid use low melting point pure metal or multicomponent alloy target.
7. multi-stage magnetic field arc ion plating according to claim 1 and rf magnetron sputtering composite deposition method, it is characterized in that, working gas selects argon gas, or working gas to select in nitrogen, acetylene, methane, silane or oxygen one or more mixed gas, prepare pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film of nanometer multilayer or gradient-structure.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734501A (en) * | 2016-05-06 | 2016-07-06 | 魏永强 | Method for multi-level magnetic field arc ion plating and twin-target medium-frequency magnetron sputtering composite deposition |
| CN107841711A (en) * | 2017-11-03 | 2018-03-27 | 西安工业大学 | A kind of method for reducing optical window tetrahedral amorphous carbon film residual stress |
| 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 |
| CN113198804A (en) * | 2021-04-30 | 2021-08-03 | 辽宁科技大学 | Method and apparatus for cleaning inner wall of slender pipeline by inert gas ionization |
| CN114032513A (en) * | 2021-12-14 | 2022-02-11 | 湘潭大学 | Method for preparing welding wire coating based on magnetic filtration cathode vacuum arc method |
| CN115354283A (en) * | 2022-09-30 | 2022-11-18 | 广东鼎泰高科技术股份有限公司 | Target material pretreatment device |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105734501A (en) * | 2016-05-06 | 2016-07-06 | 魏永强 | Method for multi-level magnetic field arc ion plating and twin-target medium-frequency magnetron sputtering composite deposition |
| CN107841711A (en) * | 2017-11-03 | 2018-03-27 | 西安工业大学 | A kind of method for reducing optical window tetrahedral amorphous carbon film residual stress |
| CN107841711B (en) * | 2017-11-03 | 2019-05-03 | 西安工业大学 | A method of reducing optical window tetrahedral amorphous carbon film residual stress |
| 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 |
| CN113198804A (en) * | 2021-04-30 | 2021-08-03 | 辽宁科技大学 | Method and apparatus for cleaning inner wall of slender pipeline by inert gas ionization |
| CN114032513A (en) * | 2021-12-14 | 2022-02-11 | 湘潭大学 | Method for preparing welding wire coating based on magnetic filtration cathode vacuum arc method |
| CN115354283A (en) * | 2022-09-30 | 2022-11-18 | 广东鼎泰高科技术股份有限公司 | Target material pretreatment device |
| CN115354283B (en) * | 2022-09-30 | 2023-08-29 | 广东鼎泰高科技术股份有限公司 | Target pretreatment device |
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