CN105088150A - Multilevel magnetic field arc ion plating method with adjustable transmission directions - Google Patents
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- 238000007733 ion plating Methods 0.000 title claims abstract description 35
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- 239000002184 metal Substances 0.000 claims abstract description 23
- 239000010409 thin film Substances 0.000 claims abstract description 17
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- 239000007789 gas Substances 0.000 claims abstract description 12
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- 238000000427 thin-film deposition Methods 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 150000002500 ions Chemical class 0.000 claims description 24
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- 238000009713 electroplating Methods 0.000 claims description 18
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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
- 238000010891 electric arc Methods 0.000 claims description 4
- 230000008030 elimination Effects 0.000 claims description 4
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
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- 239000002245 particle Substances 0.000 abstract description 5
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Abstract
The invention relates to a multilevel magnetic field arc ion plating method with adjustable transmission directions and belongs to the technical field of the material surface treatment. According to the multilevel magnetic field arc ion plating method with the adjustable transmission directions, the large particle problem occurring in the arc ion plating process of pure metal with low-melting-point or multi-component alloy materials and non-metallic materials (such as graphite) is solved; the using limitation of target materials with the low-melting-point is broken; the usable range of arc ion plating target materials and the field of thin film preparation are expanded. The multilevel magnetic field arc ion plating method comprises the steps that 1 a workpiece to be coated with a film is placed on a sample stage in a vacuum chamber and related power sources are connected; and 2 thin film deposition is conducted, when the vacuum degree in the vacuum chamber is less than 10-2 Pa, working gases are pumped in and the air pressure is adjusted, a film plating power source, namely, a grid bias power source is started, a multilevel magnetic field straight pipe magnetic filtration device removes the defect of large particles and guarantees the transmission efficiency of arc plasma, and then the magnetic field device with the adjustable transmission directions is used for guaranteeing the arc plasma to reach substrate surfaces of optional positions in the vacuum chamber and sets up needed technological parameters to make the thin film to deposit.
Description
Technical field
The present invention relates to the multi-stage magnetic field arc ions electroplating method that transmission direction is adjustable, 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 (TayBK, ZhaoZW, ChuaDHC.Reviewofmetaloxidefilmsdepositedbyfilteredcathod icvacuumarctechnique [J] .MaterSciEngR, 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 (BoxmanRL in the film, GoldsmithS.Macroparticlecontaminationincathodicarccoatin gs:generation, transportandcontrol [J] .SurfCoatTech, 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.
At present, in order to solve the problem that arc ions electroplating method is using the pure metal of low melting point or multicomponent alloy material easily to produce macrobead defect, the main way of Magnetic filter that adopts filters out macrobead at present, 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 (AndersS, AndersA, DickinsonMR, MacGillRA, BrownIG.S-shapedmagneticmacroparticlefilterforcathodicar cdeposition [J] .IEEETransPlasmaSci, 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 filters, also have the people (AndersA such as American scholar Anders, MacGillRA.Twistfilterfortheremovalofmacroparticlesfromca thodicarcplasmas [J] .SurfCoatTech, 2000, the Magnetic filter of Twistfilter 133-134:96-100.) proposed, 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.The people such as the Dai Hua of Shanghai Communications University propose a kind of adjustable flexure type magnetic filter (DaiH; ShenY; LiL; LiX; CaiX; ChuPK.Aflexiblecurvilinearelectromagneticfilterfordirect currentcathodicarcsource [J] .RevSciInstrum, 2007,78 (9): 095103-095106. and Dai Hua. in vacuum cathode arc ion plating layer, macroscopic particles removes technical study [D]; Shanghai Communications University's Ph D dissertation, 2009.), by the curvature of adjusted filter bend, can average out between macroscopic particles removal effect and plated film efficiency.The people such as the Lossy of Hua Sheng research laboratory of the U.S. in 1992 adopt and apply bent magnetic field at plasma exit place, change the direction (LossyR of plasma body, PappasDL, RoyRA, CuomoJJ, SuraVM.Filteredarcdepositionofamorphousdiamond [J] .ApplPhysLett, 1992,61 (2): 171-173.), linear pattern filtration unit outlet one end have one can by the magnetic field of plasma beam along initial axis runout 20 °, realize being separated of macrobead and plasma body, eliminate the disadvantageous effect of macrobead to film.Scholar is also had to propose magnetic island formula linear pattern magnetic filter (KleimanA, MarquezA, BoxmanRL.Performanceofamagneticislandmacroparticlefilter inatitaniumvacuumarc [J] .PlasmaSourcesSciTechnol, 2008, 17 (1): 015008. and BoltH, KochF, RodetJL, KarpovD, MenzelS.Al2O3coatingsdepositedbyfilteredvacuumarc-charac terizationofhightemperatureproperties [J] .SurfCoatTech, 1999, 116-119:956-962.), by a magnetic field additional in the middle of linear pattern magnetic field, change the transmission direction of plasma body, stop that macrobead exports from linear pattern strainer simultaneously.In a word, relevant researchist is by the various Magnetic filter method of contrast (AndersA.Approachestoridcathodicarcplasmasofmacro-andnano particles:areview [J] .SurfCoatTech, 1999, 120-121319-330. and TakikawaH, TanoueH.Reviewofcathodicarcdepositionforpreparingdroplet-freethinfilms [J] .IEEETransPlasmaSci, 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.
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, the macrobead defect contained in arc plasma is eliminated by multi-stage magnetic field straight tube Magnetic filter method, ensure arc plasma with higher transmission efficiency by straight tube filtration unit simultaneously, recycling transmission direction adjustable magnetic field device makes the substrate work-piece of optional position in the plated film space situation that surface is applying negative bias can be continuous, fine and close prepares high-quality thin-film, realize adding constituent content in film controlling, 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 the multi-stage magnetic field arc ions electroplating method that transmission direction is adjustable.
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, multi-stage magnetic field power supply 5, the adjustable magnetic field device of transmission direction 6, the adjustable magnetic field power supply 7 of transmission direction, vacuum chamber 8, sample table 9;
The method comprises the following steps:
Step one, be placed in pending substrate work-piece in vacuum chamber 8 sample table 9 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 8, multi-stage magnetic field device 4 connects multi-stage magnetic field power supply 5, and the adjustable magnetic field device of transmission direction 6 connects the adjustable magnetic field power supply 7 of transmission direction;
Step 2, thin film deposition: vacuumized by vacuum chamber 8, treat that the vacuum tightness in vacuum chamber 8 is less than 10
-2during Pa, pass into working gas to 0.01Pa ~ 10Pa;
Open grid bias power supply 1, 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%; By the bias voltage amplitude regulating grid bias power supply 1 to export, pulse-repetition and pulse width, control the effective attraction of substrate work-piece to metallic plasma and the adjustment of ion energy, carry out the deposition of film and control the pure metal of low melting point or multicomponent alloy material and non-metallic material (such as graphite) ratio in the film, realizing pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film preparation of nanometer multilayer or gradient-structure;
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, open multi-stage magnetic field power supply 5 and regulate multi-stage magnetic field device 4, keep arc plasma in the stable generation in arc ion plating target source 3 and filtration elimination is carried out to macrobead defect, make arc plasma with higher transmission efficiency by multi-stage magnetic field device 4, the adjustable magnetic field power supply of recycling transmission direction 7 regulates the adjustable magnetic field device 6 of transmission direction, ensure that arc plasma arrives the substrate work-piece surface of optional position in vacuum chamber, carry out the fast deposition of film.
Advantage of the present invention: a. multi-stage magnetic field magnetic filter can eliminate macrobead defect and ensure ionization level close to 100% the high efficiency of transmission of arc plasma; B. multi-stage magnetic field device is in conjunction with the processing parameter in arc ion plating target source, can realize utilizing many cover deposition apparatuss to regulate the ion ratio of various element in the compound plasma produced, and realizes the fast deposition of the multi-component multi-layer film of different element ratio; C. the adjustable magnetic field device of transmission direction can regulate arc plasma transmission direction in a vacuum chamber, realizes the fast deposition of substrate work-piece surface film in optional position in vacuum chamber; D. magnetic field can be utilized to control effectively to the ablation of electric arc on target surface, eliminate " steamed bun target " phenomenon because ablation inequality produces, realize the efficiency utilization of even ablation and target; E. 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 film substrate bond strength; F. owing to eliminating the pure metal of low melting point or multicomponent alloy material and non-metallic material (such as graphite) application limitations in arc ion plating, the interpolation of these elements and the flexible adjustment of different element ratio in original multi-element film preparation process can be realized; G. 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, conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filtration unit and the adjustable magnetic field device of transmission direction 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.
Accompanying drawing explanation
Fig. 1 is the adjustable multi-stage magnetic field arc ions electroplating method sketch of transmission direction of the present invention, 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, the adjustable multi-stage magnetic field arc ions electroplating method institute using appts of present embodiment transmission direction comprises 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, the adjustable magnetic field device of transmission direction 6, the adjustable magnetic field power supply 7 of transmission direction, vacuum chamber 8, sample table 9;
The method comprises the following steps:
Step one, be placed in pending substrate work-piece in vacuum chamber 8 sample table 9 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 8, multi-stage magnetic field device 4 connects multi-stage magnetic field power supply 5, and the adjustable magnetic field device of transmission direction 6 connects the adjustable magnetic field power supply 7 of transmission direction;
Step 2, thin film deposition: vacuumized by vacuum chamber 8, treat that the vacuum tightness in vacuum chamber 8 is less than 10
-2during Pa, pass into working gas to 0.01Pa ~ 10Pa;
Open grid bias power supply 1, 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%; By the bias voltage amplitude regulating grid bias power supply 1 to export, pulse-repetition and pulse width, control the effective attraction of substrate work-piece to metallic plasma and the adjustment of ion energy, carry out the deposition of film and control the pure metal of low melting point or multicomponent alloy material and non-metallic material (such as graphite) ratio in the film, realizing pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film preparation of nanometer multilayer or gradient-structure;
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, open multi-stage magnetic field power supply 5 and regulate multi-stage magnetic field device 4, keep arc plasma in the stable generation in arc ion plating target source 3 and filtration elimination is carried out to macrobead defect, make arc plasma with higher transmission efficiency by multi-stage magnetic field device 4, the adjustable magnetic field power supply of recycling transmission direction 7 regulates the adjustable magnetic field device 6 of transmission direction, ensure that arc plasma arrives the substrate work-piece surface of optional position in vacuum chamber, carry out the fast deposition of film.
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, 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 the multi-stage magnetic field arc ions electroplating method that transmission direction is adjustable, for the further genralrlization application of arc ion plating creates favourable condition, lasting, that ionization level is high metallic plasma is stablized in the generation that can make full use of arc ion plating (aip), remove macrobead defect by multi-stage magnetic field device and realize the high efficiency of transmission of arc plasma, compensate for linear pattern Magnetic filter method in the transmit direction can not the defect of flexible simultaneously, is conducive to the chemosynthesis reaction film forming of high ionization level plasma body workpiece surface at an arbitrary position; Simultaneously in conjunction with biasing electric field, the energy of arc plasma is regulated, 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, conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filtration unit and the adjustable magnetic field device of transmission direction 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.
Embodiment three: 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 one.
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 one.
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, multi-stage magnetic field device 4 and adjustment transmission direction adjustable magnetic field device 6 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 film of different stress, microtexture, element ratio and multi-component multi-layer structure.
Claims (8)
1. the multi-stage magnetic field arc ions electroplating method that transmission direction is adjustable, 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, multi-stage magnetic field power supply 5, the adjustable magnetic field device of transmission direction 6, the adjustable magnetic field power supply 7 of transmission direction, vacuum chamber 8, sample table 9;
The method comprises the following steps:
Step one, be placed in pending substrate work-piece in vacuum chamber 8 sample table 9 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 8, multi-stage magnetic field device 4 connects multi-stage magnetic field power supply 5, and the adjustable magnetic field device of transmission direction 6 connects the adjustable magnetic field power supply 7 of transmission direction;
Step 2, thin film deposition: vacuumized by vacuum chamber 8, treat that the vacuum tightness in vacuum chamber 8 is less than 10
-2during Pa, pass into working gas to 0.01Pa ~ 10Pa;
Open grid bias power supply 1, 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%; By the bias voltage amplitude regulating grid bias power supply 1 to export, pulse-repetition and pulse width, control the effective attraction of substrate work-piece to metallic plasma and the adjustment of ion energy, carry out the deposition of film and control the pure metal of low melting point or multicomponent alloy material and non-metallic material (such as graphite) ratio in the film, realizing pure metal film, the compound ceramic film of different element ratio, function film and there is the high-quality thin-film preparation of nanometer multilayer or gradient-structure;
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, open multi-stage magnetic field power supply 5 and regulate multi-stage magnetic field device 4, keep arc plasma in the stable generation in arc ion plating target source 3 and filtration elimination is carried out to macrobead defect, make arc plasma with higher transmission efficiency by multi-stage magnetic field device 4, the adjustable magnetic field power supply of recycling transmission direction 7 regulates the adjustable magnetic field device 6 of transmission direction, ensure that arc plasma arrives the substrate work-piece surface of optional position in vacuum chamber, carry out the fast deposition of film.
2. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, it is characterized in that, the electric current that arc power 2 exports is direct current, pulse or DC pulse compound, and realizes the high efficiency of transmission of macrobead removal of defect and arc plasma by multi-stage magnetic field device 4 and the adjustable magnetic field device 6 of transmission direction.
3. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, it is characterized in that, grid bias power supply 1 can be adjusted respectively by the dutycycle of pulse-repetition, pulsed bias amplitude and pulsed bias, controls arc plasma energy peak intensity and density that the unit time arrives substrate work-piece surface.
4. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, is characterized in that, it is monopulse, DC pulse compound or multipulse compound that grid bias power supply 1 exports pulse.
5. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, it is characterized in that, the method also comprises:
Step 3, conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filtration unit and the adjustable magnetic field device of transmission direction 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.
6. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, 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.
7. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, it is characterized in that, effectively can utilize multi-stage magnetic field device 4 and the adjustable magnetic field device 6 of transmission direction, the target body material that arc ion plating target source 3 adopts can be the pure metal of low melting point or multicomponent alloy target and non-metallic material (such as graphite), breach conventional arc ion plating target source 3 and adopt the pure metal of low melting point or the restriction of multicomponent alloy material and non-metallic material (such as graphite), realize the flexible of thin film composition and microtexture.
8. the multi-stage magnetic field arc ions electroplating method that transmission direction according to claim 1 is adjustable, 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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Effective date of registration: 20190730 Address after: 450015 Henan Province, Zhengzhou District, No. 27 University Road, No. 2 Patentee after: Zhengzhou Institute of Aeronautical Industry Management Address before: 27 University District Road 450015 Henan city of Zhengzhou province No. 2 Zhengzhou Institute of family hospital No. 26 building 4 unit 2 floor of the south door Patentee before: Wei Yongqiang |