CN1281057A - Equipment and process for preparing film by pulse aided filter and arc deposition - Google Patents
Equipment and process for preparing film by pulse aided filter and arc deposition Download PDFInfo
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- CN1281057A CN1281057A CN 99121640 CN99121640A CN1281057A CN 1281057 A CN1281057 A CN 1281057A CN 99121640 CN99121640 CN 99121640 CN 99121640 A CN99121640 A CN 99121640A CN 1281057 A CN1281057 A CN 1281057A
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Abstract
A multi-arc ionic film-plating equipment has a vacuum chamber with built-in reaction gas feeding mechanism and evaporation source target. A vacuumizing system is communicated to said vacuum chamber and vacuum cavity is grounded to play the role of anode. The cathode of DC power supply is connected to evaporation source target. A support on bottom of vacuum chamber has a heating element under it connected with heating power supply. Another power supply is connected to magnetic-field winding under the arc evaporation source. The DC power supply for magnetic field and pulse power supply are connected with a switch at each individual end, and connected to DC power source of evaporation source target and grounded with vacuum cavity at another individual end, while one terminal of the switch is electrically connected with the workpiece.
Description
The invention belongs to and relate to surface diposition, relate in particular to the apparatus and method of multi-arc ion plating film.
The multi-arc ion plating film technology comes from USSR (Union of Soviet Socialist Republics), and the relevant patent of multinomial arc ion plating membrane technique has been authorized by the seventies U.S..Its ultimate principle is: be anode with the vacuum chamber, be installed on the vacuum-chamber wall as negative electrode with desire plating material, use with the equipotential striking pin of anode and draw back with surperficial instantaneous the contact, the starting arc discharge.Cause formed electric arc in certain vacuum degree scope, can form the arc spot of controlling oneself, do random motion on the target surface.The diameter of this electric arc arc spot is about 0.1-100 μ m, the about 100m/S of movement velocity, and current density is about 10
2-10
8A/cm
2Of living in some temperature of arc spot can reach 8000-10000K; make target directly from solid-state vaporization and ionization, launch electronics, ion, atom and fused target particulate (claiming macrobead or drop again), these particles under the effect of negative bias at workpiece surface formation of deposits film.If charge into reactant gases in the vacuum chamber, but deposited compound film then.
The principal feature of multi-arc ion coating membrane technique is: the one, and target material vaporator rate height, thereby can obtain bigger film deposition rate; The 2nd, the ionization level height of target material can reach 60%-95% usually, is beneficial to and feeds gas reaction and form compound film; The 3rd, the energy height of emitted particle at tens electron-volts, can reach the hundreds of electron-volt under the negative bias effect, greatly improved the homogeneity and the sticking power of film.Simultaneously because handiness, the terseness of structure, particularly non-environmental-pollution that target is laid make it decorate field acquisition application such as plating at wear resistant tools coating, anti-corrosion part and material.
The existence of " yet drop " has seriously hindered the multi-arc ion coating membrane technique to field expanded application widely." drop " is the macrobead of following electronics and ion to come out from emission of cathode jointly, and its quantity is more, and size is bigger, might not influence its performance to the partial coating instrument among depositing to film.Yet for optical thin film, microelectronics film and growing high precision cutting tools, mould, a macrobead yardstick has often just exceeded the requirement of its accuracy error; To high-grade decoration, oarse-grained existence directly influences its surface smoothness; To corrosion-resistant finishes, often there is hole in the film at macrobead place, and corrosive medium infiltrates from hole, and directly etched the matrix causes that film comes off, and can not demonstrate fully the good anti-corrosion of film own.It is excessive that " macrobead " problem also makes target consume, and utilization ratio descends, and cost improves.Thereby the existence of " macrobead " becomes the bottleneck problem of restriction multi-arc ion plating film technical development.
In order to solve " macrobead " problem of multi-arc ion coating membrane technique, eliminate " macrobead " influence to film performance, the researchist has proposed the method for many solutions and improvement.People such as S.Ramalingam (S.Ramalingam, et al., Controlled vacuum arc material deposition, method and apparatus, United States Patent, No.4,673,477,1987) designed a kind of cathode assembly of controlled arc, principal character is to adopt motor-operated eccentric permanent magnet rotation at the target back, makes arc spot on the target surface according to the route of design, evenly, motion in an orderly manner.People such as I.I.Aksenov (I.I.Aksenov, V.A.Belous, etal., Apparatus to rid the plasma of a vacuum arc of macroparticles, Instrum.Exp.Tech., Vol.21,1978,1416) the arc line type filtration unit has been proposed, basic characteristics are before the particle that target material is launched enters vacuum chamber, by an arc line type magnetic field passage, stop " macrobead " to enter vacuum chamber by the camber passage on the one hand, charged particle and " macrobead " by rotation is although collision reaches the quantity that this method of purpose that smashes can lower " macrobead " effectively on the other hand, and the serious reduction of the complicacy of device structure and sedimentation rate makes it be difficult to promote the use of in actual applications.B.F.Coll, D.M.Sanders, Design of vacuum arc-based sources, Surf.Coat.Tech., Vol.81,1996,42-51) waiting the people to design a kind of linear pattern magnetic field principal feature is filtration unit will influence the arc spot in the magnetic field that cathode surface forms motion, and arc spot division refinement is made its acceleration, thereby has shortened the arc spot a locational residence time, reduce the current density of each arc spot, reduced the emission of " macrobead ".Magnetic field makes the charged particle rotation increase collision opportunity simultaneously, and " macrobead " smashed, and " macrobead " size and quantity can both reduce.But still having part " macrobead " to pass magnetic field deposits on the substrate.
The objective of the invention is to eliminate " macrobead " problem in the multi-arc ion coating technology, reduce the consumption of target, reduce cost; In order to improve coating quality, thereby provide a kind of deposited film of preparing itself to have good corrosion resistance, pulse aided filter arc deposited membrane unit and method that surface smoothness is good.
The object of the present invention is achieved like this:
Pulse aided filter arc deposited membrane unit provided by the invention comprises: the mechanism that arc evaporation source target, feeding reactant gases are used, power supply, support, heating unit, heating unit power supply, vacuum system, wherein in the vacuum chamber that can hold workpiece, be equipped with and feed the mechanism that reactant gases is used, be connected with vacuum system with vacuum chamber by valve tube, the arc evaporation source target of at least one desire plating material is installed on the vacuum chamber locular wall, and vacuum chamber locular wall ground connection is anode; The negative electrode of direct supply is connected with the evaporation source target, and anode is connected ground connection with the vacuum chamber locular wall; One support with revolution and rotation is arranged in vacuum chamber bottom, place work piece on the support, the oriented workpiece of vacuum chamber provides the mechanism of heating, heating arrangements is electrically connected with vacuum chamber heating power supply outward, it is characterized in that: also comprise a magnetic field power supply and at least one magneticfield coil of arc evaporation source target positioned beneath in vacuum chamber; Magnetic field power supply is electrically connected with magneticfield coil, and a direct current power supply and a pulse power, direct supply and the pulse power end separately are connected a switch, switch one end is electrically connected with workpiece, and direct supply is connected ground connection with the direct supply that the evaporation source target is connected with the vacuum chamber locular wall with the pulse power the other end.
Wherein settle the magneticfield coil before the arc evaporation source target can be with soft magnetic core, also clearance; It is direct current, interchange or pulsed current that magnetic field power supply offers magneticfield coil, but and superposition, the riding position of magneticfield coil guarantees that vacuum chamber has the maximum useful space; The magnetic field power supply group comprises the pulse power and direct supply, and direct supply provides volts DS to magneticfield coil, and the pulse power provides pulsed voltage to magneticfield coil, both can provide pulsed voltage or volts DS separately, but superposition pulsed voltage and volts DS again.
Wherein workpiece bias has by a direct current power supply and a pulse power provides, and the two all links to each other with switch, both can provide pulsed bias separately, can provide direct-current biasing separately again, but also superposition pulsed bias and direct-current biasing.
Use pulse aided filter arc deposited membrane unit provided by the invention carries out the method for arc deposited film, carries out according to the following step:
The vacuum system that forepump and diffusion pump are formed makes vacuum chamber reach certain vacuum tightness, in vacuum chamber, feed rare gas element and reactant gases by gas control system, utilize outer heating system to make workpiece be heated to certain temperature, by the direct supply and the pulse power workpiece is applied bias voltage, the magneticfield coil that is opposite to the arc cathode front end is granted suitable electric current with direct supply, open the arc cathode power supply, electric arc ignites, the cathode arc spot is launched metal ion, atom and atomic group, by the magnetic field channel space, under the acting in conjunction of magnetic field and negative bias, atomic group and atom further decompose ionization, to the workpiece surface motion, metal ion and reaction gas chemical combination form compound film at workpiece surface.When not feeding reaction gas, then form metallic film.
The final vacuum of institute's use vacuum chamber is not less than 1 * 10 in the method
-3Pa feeds rare gas element (as argon gas) and reactant gases, and reactant gases can be nitrogen, acetylene gas, methane gas, diborane and oxygen and other required reactant gases, and its gaseous tension changes in the 0.1-10Pa scope; The workpiece Heating temperature can be ℃ continuous adjustable in room temperature to 500; Dc bias power voltage is adjustable continuously at 0-2000V, and pulsed bias power supply voltage is adjustable at 0-1200V, and dutycycle is continuous variable in the 0-100% scope; The magneticfield coil electric current changes in the 0-50A scope; The material of arc cathode can be the simple substance or the alloy of various metals such as titanium, chromium, zirconium, nickel, niobium, tungsten, molybdenum, tantalum vanadium, copper, aluminium and hafnium, various targets can be in vacuum chamber single or mixed-arrangement, direct supply provides the electric current of arc cathode adjustable at 0-200A.
In the vacuum chamber of multi-arc ion coating target cathode front end or outside, add linear pattern magnetic field in the device of the present invention, magnetic field is twined and is produced by enameled wire, and a soft magnetic core that has the clearance can be installed by portion in coil, to optimize and to strengthen magnetic field.This device produces a strong and long and narrow bottle-neck type magnetic field in plasma channel, add a pulse power simultaneously between two negative electrodes and vacuum-chamber wall anode.Reduce emission, passage filtration and collide the purpose that the comprehensive action that smashes reaches elimination " macrobead ".
Because the linear pattern magneticfield coil influences the motion of arc spot in the effect of the magnetic field parallel component of cathode surface generation, it is quickened, shortened the residence time of arc spot, also can make the division of arc spot simultaneously, reduce the current density of each arc spot.Thereby reduce the emission of " macrobead ".
The linear pattern magneticfield coil focuses at the bottle-neck type magnetic field article on plasma body that hub of a spool produces, can reflect bigger electronics and the ion of those transmit directions and target surface angle, electronics that these reflections reflux and ion and " macrobead " bump, on the one hand " macrobead " divided because of collision, on the other hand because the energy exchange of collision, the temperature of " macrobead " is increased greatly, make " macrobead " further carburation by evaporation awing.
Pulsed bias that substrate adds produces three effects to electronics and ion between cathode arc and bottle-neck type magnetic field: the one, and booster action; The 2nd, increase the number of charged particles that refluxes; The 3rd, make charged particle produce the intensive oscillation action.Thereby probability of collision is increased greatly, greatly reduced " macrobead " that deposit to substrate.Even there be " macrobead " to pass bottle-neck type magnetic field, the interaction energy of pulsed bias further is crashed to pieces it.
The quantity of minimizing " macrobead " has been played in the comprehensive action of above-mentioned three aspects, reduces the size of " macrobead " simultaneously, finally smashes " macrobead ", makes the film that deposits on the substrate eliminate " macrobead " fully.Another significant advantage of the present invention is owing to improved the movement velocity of arc spot, has reduced the residence time of arc spot in a certain position, and the current density of arc spot is descended, and the consumption of target material surface is homogenizing more.Although overall emission quantity does not reduce, reduced the emission of " macrobead ", increased the effective rate of utilization of target, and then made the production cycle shorten cost decreases.
Advantage of the present invention: pulse aided filter arc deposited membrane unit provided by the invention carries out the arc deposited film and has overcome in the past " macrobead " problem in the deposit film method, reduces the consumption of target widely, has reduced cost; The workpiece surface film smooth finish of using apparatus and method preparation of the present invention significantly improves, and surface roughness Ra is reduced to 0.0271 μ m from 0.785.And the corrosion resistance nature of workpiece is improved, in 20% hydrochloric acid, only be 1/5th of traditional multi sphere plating TiN film through corrosion speed with the TiN film behind the present invention.
The present invention is described in detail below in conjunction with drawings and Examples:
Fig. 1 is an apparatus structure synoptic diagram of the present invention
Fig. 2 is to use device of the present invention to deposit the thick TiN film surface appearance figure of 1 μ m
Fig. 3 is the surface topography map of the traditional multi-arc ion coating TiN film of contrast
Embodiment 1
Make a pulse aided filter arc deposited membrane unit by Fig. 1
Different positions in the vacuum chamber that can hold workpiece is equipped with and feeds reactant gases structure 12, and vacuum chamber ground connection is anode; The arc evaporation source target 1 of at least one desire plating material is installed on the vacuum-chamber wall; The negative electrode of direct supply 3 is connected with evaporation source target 1, and anode is connected ground connection with vacuum chamber; In the scope of arc evaporation source target 1 preceding adjustable distance, settle at least one magneticfield coil 2, band soft magnetic core magneticfield coil 2, power supply 4 is electrically connected with magneticfield coil 2, and power supply 4 is power cabinets, and a direct supply and the pulse power are installed, provide volts DS to magneticfield coil, or pulsed voltage, or the two superposition, laying of magneticfield coil guarantees that vacuum chamber has the maximum useful space; Below vacuum chamber, have one to have the revolution and the support 13 of rotation, workpiece 9 be placed on have revolve round the sun and the support 13 of rotation on; 13 ends of support, are equipped with one and provide the heating unit 8 of heating to workpiece, and heating unit 8 is electrically connected with heating unit power supply 10; Direct supply 5 provides direct-current biasing to workpiece 9, and power supply 6 provides pulsed bias to workpiece 9, and the two can use separately, but also superposition uses.Vacuum system 11 is by pipeline and vacuum chamber, and common reactant gases feeds mechanism and control section 12 sealings are installed on the vacuum-chamber wall.
Embodiment 2
The device of using the embodiment of the invention 1 carries out the method for TiN film; At first workpiece is deoiled and ultrasonic cleaning; The workpiece that the cleans up vacuum chamber of packing into, and utilize 11 pairs of vacuum chambers of vacuum system to vacuumize makes the vacuum chamber vacuum tightness 10 that reaches capacity
-3Pa utilizes outer heating power supply 10 to heat by the workpiece 9 on 8 pairs of substrates of heating unit, when temperature reaches temperature required, charges into argon gas to 0.1Pa by gas control system 12, at M
2Add pulsed bias 200V on the rapid steel substrate 9, dutycycle 60%, carry out ion bombardment, inflated with nitrogen makes vacuum chamber pressure 0.8Pa then, powers up for magneticfield coil 2 by magneticfield coil power supply 4 and flows to 50A, apply voltage by 3 pairs of titanium target evaporations of power supply source, and starting arc, make arc stream about 60A, under this mode of deposition, deposit the thick TiN film surface appearance of 1 μ m as shown in Figure 2.Contrast surface topography Fig. 3 of traditional multi-arc ion coating TiN film, install the existence that sedimentary TiN film has been eliminated " macrobead " basically at this as can be seen, comprehensive advantage of the present invention will be widened multi-arc ion coating Application of membrane field, have huge industrial significance and use value.
Claims (10)
1, a kind of pulse aided filter arc deposited membrane unit, comprise the arc evaporation source target, feed mechanism, power supply, support, heating unit, heating unit power supply, vacuum system that reactant gases is used, wherein in the vacuum chamber that can hold workpiece, be equipped with and feed the mechanism that reactant gases is used, be connected with vacuum system with vacuum chamber by vacuum pipe, the arc evaporation source target of desire plating material is installed on the vacuum chamber locular wall, and vacuum chamber ground connection is anode; The negative electrode of direct supply is connected with the evaporation source target, and anode is connected ground connection with vacuum chamber; One support with revolution and rotation is arranged in vacuum chamber bottom, place work piece on the support, the oriented workpiece of vacuum chamber provides the mechanism of heating, heating arrangements is electrically connected with vacuum chamber heating power supply outward, it is characterized in that: also comprise magnetic field power supply and at least one magneticfield coil of arc evaporation source target positioned beneath in vacuum chamber; Magnetic field power supply is electrically connected with magneticfield coil, and a magnetic field direct supply and a pulse power, magnetic field direct supply and pulse ac power supply an end separately are connected a switch, switch one end is electrically connected with workpiece, the magnetic field direct supply is electrically connected with the direct supply that the pulse ac power supply the other end is connected with the evaporation source target, is connected ground connection with vacuum chamber again.
2, by the described pulse aided filter arc deposited of claim 1 membrane unit, it is characterized in that: said magneticfield coil comprises: the magneticfield coil of band soft magnetic core, the magneticfield coil of clearance.
3, by the described pulse aided filter arc deposited of claim 1 membrane unit, it is characterized in that: said magnetic field power supply group comprises the direct supply and the pulse power.
4,, it is characterized in that by the described pulse aided filter arc deposited of claim 1 membrane unit: said evaporation source target be one or by the kind of requirement arc deposited film the number of target is set.
5, by the described pulse aided filter arc deposited of claim 1 membrane unit, it is characterized in that: said magneticfield coil is one or more.
6, a kind of method of using the described pulse aided filter arc deposited of claim 1 membrane unit to carry out the arc deposited film is characterized in that: carry out according to following order: the vacuum system that forepump and diffusion pump are formed makes vacuum chamber reach capacity vacuum tightness 1 * 10
-3Pa-* 10
-3Behind the Pa, feed rare gas element and reaction gas by gas control system in vacuum chamber, its gaseous tension changes in the 0.1-10Pa scope; Utilize outer heating system heated parts ℃ continuous adjustable then in room temperature to 700, by the direct supply and the pulse power workpiece is applied bias voltage, the magneticfield coil that is opposite to the arc cathode front end imposes on suitable electric current with direct supply, by power supply the evaporation source target is applied voltage 60A; Open the arc cathode power supply, the electric arc that ignites, electric arc flow at 50-70A; Metal ion and reactant gases chemical combination form compound film at workpiece surface, then form metallic film when not feeding reaction gas.
7, by the described pulse aided filter arc deposited of claim 6 film process, it is characterized in that: said feeding rare gas element comprises: argon gas, nitrogen.
8, by the described pulse aided filter arc deposited of claim 6 film process, it is characterized in that: said reactant gases comprises nitrogen, acetylene gas, methane gas, diborane and oxygen and other required reactant gases, and its gaseous tension changes in the 0.1-10Pa scope.
9, by the described pulse aided filter arc deposited of claim 6 film process, it is characterized in that: said magneticfield coil dc bias power voltage is adjustable continuously at 0-1000V, pulsed bias power supply voltage is adjustable at 0-1000V, and dutycycle is continuous variable in the 0-100% scope; The magneticfield coil electric current changes in the 0-50A scope;
10, by the described pulse aided filter arc deposited of claim 6 film process, it is characterized in that: said evaporation source target material comprises the simple substance or the alloy of titanium, chromium, zirconium, nickel, niobium, tungsten, molybdenum, tantalum vanadium, copper, aluminium and hafnium, metal, various targets are can be in vacuum chamber single-or mixed-arrangement, direct supply provides the electric current of arc cathode adjustable at 0-200A.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB991216407A CN1136332C (en) | 1999-10-11 | 1999-10-11 | Equipment and process for preparing film by pulse aided filter and arc deposition |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB991216407A CN1136332C (en) | 1999-10-11 | 1999-10-11 | Equipment and process for preparing film by pulse aided filter and arc deposition |
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| CN1281057A true CN1281057A (en) | 2001-01-24 |
| CN1136332C CN1136332C (en) | 2004-01-28 |
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| CN1312317C (en) * | 2004-12-10 | 2007-04-25 | 北京丹鹏表面技术研究中心 | Vacuum ionic film coater with gas ionic source arrangement |
| CN100460555C (en) * | 2006-01-20 | 2009-02-11 | 大连理工大学 | Equipment and method for low temperature depositing high-quality decorative film by electric arc ion plating |
| CN1904133B (en) * | 2005-07-29 | 2010-05-12 | 株式会社爱发科 | Sputtering device and sputtering method |
| CN101838789A (en) * | 2004-01-21 | 2010-09-22 | 纳峰科技私人有限公司 | Pressure in the plated film that reduces to generate by physical vapor deposition |
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| CN104046942A (en) * | 2013-03-12 | 2014-09-17 | 中国兵器工业第五九研究所 | Metal tantalum coating preparation method |
| CN105200378A (en) * | 2015-10-27 | 2015-12-30 | 中国科学院兰州化学物理研究所 | Gate-assisted columnar arc ion plating apparatus |
| CN105385994A (en) * | 2015-11-27 | 2016-03-09 | 广州巴达精密刀具有限公司 | Film coating system and method for improving coating adhesion of cutting tool |
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- 1999-10-11 CN CNB991216407A patent/CN1136332C/en not_active Expired - Fee Related
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| CN101838789A (en) * | 2004-01-21 | 2010-09-22 | 纳峰科技私人有限公司 | Pressure in the plated film that reduces to generate by physical vapor deposition |
| CN101838789B (en) * | 2004-01-21 | 2012-11-14 | 纳峰真空镀膜（上海）有限公司 | Method of reducing stress in coatings produced by physical vapour deposition |
| CN1312317C (en) * | 2004-12-10 | 2007-04-25 | 北京丹鹏表面技术研究中心 | Vacuum ionic film coater with gas ionic source arrangement |
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| CN100460555C (en) * | 2006-01-20 | 2009-02-11 | 大连理工大学 | Equipment and method for low temperature depositing high-quality decorative film by electric arc ion plating |
| CN102199753A (en) * | 2010-03-24 | 2011-09-28 | 沈阳科友真空技术有限公司 | Magnetron-enhanced aluminum ion vapor deposition process and apparatus |
| CN102199761A (en) * | 2011-05-10 | 2011-09-28 | 绿种子能源科技股份有限公司 | Thin film deposition apparatus |
| CN104046942A (en) * | 2013-03-12 | 2014-09-17 | 中国兵器工业第五九研究所 | Metal tantalum coating preparation method |
| CN104046942B (en) * | 2013-03-12 | 2016-09-14 | 中国兵器工业第五九研究所 | A kind of preparation method of metal tantalum coating |
| CN103290367A (en) * | 2013-05-29 | 2013-09-11 | 哈尔滨工业大学 | Preparation method of film bulk acoustic resonator lower electrode |
| CN103290367B (en) * | 2013-05-29 | 2015-02-11 | 哈尔滨工业大学 | Preparation method of film bulk acoustic resonator lower electrode |
| CN105200378A (en) * | 2015-10-27 | 2015-12-30 | 中国科学院兰州化学物理研究所 | Gate-assisted columnar arc ion plating apparatus |
| CN105385994A (en) * | 2015-11-27 | 2016-03-09 | 广州巴达精密刀具有限公司 | Film coating system and method for improving coating adhesion of cutting tool |
| CN105385994B (en) * | 2015-11-27 | 2018-08-03 | 广州巴达精密刀具有限公司 | A kind of method of coating system and the adhesion of coating film for improving cutting tool |
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| CN111005065A (en) * | 2020-01-07 | 2020-04-14 | 北京科技大学 | Plasma arc deposition device and method for diamond film |
| CN111893439A (en) * | 2020-08-11 | 2020-11-06 | 苏州众智泽智能科技有限公司 | Method for preparing personal ornaments with titanium nitride hard coating |
| CN116145089A (en) * | 2023-03-21 | 2023-05-23 | 纳狮新材料有限公司杭州分公司 | Arc evaporation device |
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