CN103031524B - Method for realizing metallization of back of indium tin oxide (ITO) target material by ion deposition - Google Patents
Method for realizing metallization of back of indium tin oxide (ITO) target material by ion deposition Download PDFInfo
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Abstract
The invention relates to a method for realizing metallization of the back of an indium tin oxide (ITO) target material by ion deposition. The method comprises the following steps: preparing indium into an indium target; after ultrasonically cleaning and drying the ITO target material, mounting and fixing the ITO target material on a workpiece rest of a multi-arc ion plating machine; after cleaning under biasing, starting the multi-arc ion plating function and depositing one layer of metal indium film on the surface of the ITO, wherein in the plating process, the temperature is 100 to 150 DEG C, the voltage is 20 to 80 V, the current is 0.1 to 0.6 A, the time is 5 to 15 minutes and the argon pressure intensity is 0.3 to 1 Pa; and cooling, taking out and cleaning the target material to obtain the ITO target material with the surface subjected to uniform metallization. The method is simple; the back of the ITO target material can be metalized through multi-arc ion deposition and then production of components can be realized by braze welding; the metalized layer has a high binding force and a high speed; and pollution is avoided, other metal impurities are not introduced, and recovery of the target material is promoted.
Description
Technical field
The present invention relates to a kind of making method that is applied in the ITO target material assembly of preparing transparent conductive film, particularly a kind of ion deposition is realized the method for ITO target back face metalization.
Background technology
Be widely used transparent conductive oxide (TCO) thin-film material in fields such as plane demonstration, solar cells, wherein ITO is use range TCO material the most widely, and in ito thin film preparation process, the working order of ITO target has important impact to the performance of film.
In ITO target coating process, ITO target good with heat conductivility and the formation target material assembly that is connected of the backboard with certain physical strength, metal backing is mainly target in magnetron sputtering provides enough physical strengths to support, a large amount of heat energy that target can be produced in sputter procedure again take away to prevent that with water coolant target excessive temperature from raising in time, need target to connect with metal backing processing for this reason.On coating wire, the general red copper that uses is as metal backing material.
ITO target will stand the continuous bombardment of high-energy argon ion in film coating sputtering process, also will in high vacuum, have enough linking intensities with copper backboard simultaneously.The heat that copper backboard produces sputter by strong water coolant is taken away in time, causes target cracking otherwise heat can make target temperature sharply rise, and even comes off and causes industrial accident from backboard, so target must have the good quality that connects with backboard.
Because ITO target is stupalith, fusing point, more than 2000 degree, can only adopt method for welding and can not adopt fusion welding method so backboard connects with target big area; Adopt of the welding of ITO target and metallic copper backboard at present welded as the welding process of solder using indium metal or indium alloy more.ITO target is the high temperature ceramic material that consists of tin indium oxide, very poor with the interface wetting property of indium metal scolder and other indium alloy scolders, need to, by the whole bag of tricks at least excessively layer (this process is known as the back face metalization of target) of layer of metal of target back side preplating, could meet soldering requirement.
The method of target back face metalization has: the disclosed pressure welding connection of CN101279401A, the disclosed electron beam welding connection of CN1880000A and CN1015595515B, the disclosed target material surface sintering silver of CN1475465A slurry method, the electrolysis process that CN101705501A adopts, conventional gas evaporation, magnetically controlled sputter method that high Long Qiao proposes at " the practical sealing technology of ceramic-metal ".
Pressure braze method is applicable to the welding of metal targets and backboard, but be not suitable for using for the ITO ceramic target of fragility, electrons leaves welding still belongs to melt welding method, be only applicable to the welding of metal targets and backboard, and the fusing point of ITO target and backboard differs greatly, be not used in electro-beam welding method.The back side is brushed silver slurry and not only can be affected in the performance of the lower ITO target of higher sintering temperature (600 ~ 800 DEG C) at sintering method, and the auxiliary agent such as silver, copper containing in silver slurry can introduce other a large amount of metal ions in the time that target reclaims, increase target cost recovery.Electrolysis process not only produces a large amount of pollutions, and metal layer exists empty unsound phenomenon, affects soldering effect below.Metallized method is prepared in conventional evaporation, the sputter adopting needs the equipment that expense is higher, and because coating speed is low, efficiency ratio is lower, and main is that metal level and target bonding force are not high, affects soldering effect.Therefore current various ITO target back side metallization technology is not all ideal.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of ion deposition and realizes the method for ITO target back face metalization, by multi-arc ion coating method at ITO target material surface deposition one deck even compact, indium metal film that bonding force is strong, thereby realize the object at ITO back face metalization.
In order to realize the object solving the problems of the technologies described above, the present invention has adopted following technical scheme:
The present invention is a kind of method that ion deposition is realized ITO target back face metalization, comprises use multi-Arc Ion Plating, adopts Mud-arc ion-plating, and detailed process is:
The 99.99% indium metal heat fused that is 4N by purity, is cast in ganoid graphite jig, is made into indium metal target, and surface is fixed on target pedestal after cleaning with acetone;
ITO target, after oxalic acid, acetone and pure water ultrasonic cleaning are dried, is fixed on multi-Arc Ion Plating, ITO target to be processed is placed on the vacuum chamber work rest of multi-Arc Ion Plating; First forvacuum to 5 × 10
-4pa, is heated to after temperature, is filled with argon gas and prepares plated film after certain pressure;
First after the 200V negative voltage bias voltage of 5 ~ 10min cleans, start multi-Arc Ion Plating, at ITO surface deposition layer of metal indium film;
When vacuum chamber greenhouse cooling to 60 DEG C takes out and clean target material surface below, can obtain the even ITO target of metalized of surface.This target can be processed the production for ITO target material assembly by soldering.
Concrete, as follows at the coating process parameter area of ITO surface deposition layer of metal indium film, temperature is 100 ~ 150 DEG C of scopes, voltage is 20 ~ 80V, current control is in 0.1 ~ 0.6A scope, and the time, it was 0.3 ~ 1Pa scope that ar pressure is controlled in 5 ~ 15min scope.The too low meeting of temperature causes metal level and substrate caking power to reduce, the too high meeting of temperature causes layer on surface of metal to occur larger particles, the too low meeting of electric current causes Efficiency Decreasing, the too high meeting of electric current causes metal level inhomogeneous, overlong time can cause metal layer thickness blocked up, reduce the service efficiency of indium metal, the too high or too low meeting of ar pressure causes the inhomogeneous of metal level or can not produce the arc light that test needs.
By adopting technique scheme, the present invention compares other and has following beneficial effect about ITO target method for metallising: (1) compares magnetically controlled sputter method, and target utilization is up to more than 90%, far above the less than 40% of magnetically controlled sputter method; ITO target metallization velocity ratio is very fast, and the time can shorten more than 1/3; The bonding force of metal level and matrix is higher, weigh 90% atom is ionized in deposition process, in the situation that not significantly improving substrate temperature, can significantly improve like this bonding force of metal level and matrix, not only higher than magnetically controlled sputter method also far above the method such as evaporation, plating; (2) indium metal is low melting point metal, and physical method is realized deposition and easily produced oxidative phenomena, and the present invention, in the situation that not introducing impurity and not producing pollution, realizes non-oxidation low temperature depositing, thus the making high quality target material assembly ensureing; (3) assembly temperature rise is smaller, and in 200 DEG C, workpiece deformation amount is very little, negligible, effectively improves assembly good article rate.(4) compare conventional multi-arc ion plating film, by Optimizing Process Parameters, improved quality of coating, the big particle quantity of coating significantly reduces, and square millimeter amounts of particles is controlled at 2 × 10
3below, less than 30% of conventional multi sphere plating.
The inventive method is simple, just can realize ITO target back face metalization by multi-arc ion deposition, then just can soldering realizes the production of assembly; There is high, the fireballing feature of metal layer bonding force, and do not produce pollution, do not introduce other metallic impurity be conducive to target reclaim.
Embodiment
Below in conjunction with embodiment, this patent is further explained.But the protection domain of this patent is not limited to concrete embodiment.
Embodiment 1
The indium metal of 4N is heated to 190 degree fusings, is cast to and in graphite jig, is made into indium metal target and is contained on TSU-600 multi-Arc Ion Plating.ITO target first cleans 10 minutes with 10% oxalic acid, and then acetone cleans 5 minutes, then puts into pure water ultrasonic cleaning 20min, after dry, be fixed in the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started multi-arc ion plating film function, in T(temperature)=120 DEG C, P
arplated film 7 minutes under the processing parameter of=0.7Pa, V=30V, I=0.3A, after cooling, in coating equipment, take out, clean target material surface 10 minutes with ethanol, to remove surperficial pollutent, expose silvery white metal level, so just can, at the good thickness of ITO target material surface deposition one deck bonding force greatly about the indium metal layer of 10 microns of left and right, meet the requirement of next step soldering making target material assembly.
Embodiment 2
The indium metal of 4N is heated to 180 degree fusings, is cast to and in graphite jig, is made into indium metal target and is contained on TSU-600 multi-Arc Ion Plating.ITO target first cleans 10 minutes with 10% oxalic acid, and then cleans 5 minutes with acetone, then puts into pure water ultrasonic cleaning 20min, after dry, be fixed in the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started multi-arc ion plating film function, in T(temperature)=150 DEG C, P
arplated film 5 minutes under the processing parameter of=0.9Pa, V=50V, I=0.4A, after cooling, in coating equipment, take out, clean target material surface 10 minutes with ethanol, to remove surperficial pollutent, expose silvery white metal level, so just can, at the good thickness of ITO target material surface deposition one deck bonding force greatly about the indium metal layer of 15 microns of left and right, meet the requirement of next step soldering making target material assembly.
Embodiment 3
The indium metal of 4N is heated to 180 degree fusings, is cast to and in graphite jig, is made into indium metal target and is contained on TSU-600 multi-Arc Ion Plating.ITO target first cleans 10 minutes with 10% oxalic acid, and then cleans 5 minutes with acetone, then puts into pure water ultrasonic cleaning 20min, after dry, be fixed in the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started multi-arc ion plating film function, in T(temperature)=150 DEG C, P
arplated film 10 minutes under the processing parameter of=0.7Pa, V=59V, I=0.5A, after cooling, in coating equipment, take out, clean target material surface 10 minutes with ethanol, to remove surperficial pollutent, expose silvery white metal level, so just can, at the good thickness of ITO target material surface deposition one deck bonding force greatly about the indium metal layer of 25 microns of left and right, meet the requirement of next step soldering making target material assembly.
Embodiment 4
The indium metal of 4N is heated to 180 degree fusings, is cast to and in graphite jig, is made into indium metal target and is contained on TSU-600 coating equipment.ITO target first cleans 10 minutes with 10% oxalic acid, and then cleans 5 minutes with acetone, then puts into pure water ultrasonic cleaning 20min, after dry, be fixed in the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started multi-arc ion plating film function, in T(temperature)=150 DEG C, P
arplated film 10 minutes under the processing parameter of=0.7Pa, V=72V, I=0.6A, after cooling, in coating equipment, take out, clean target material surface 10 minutes with ethanol, to remove surperficial pollutent, expose silvery white metal level, so just can, at the good thickness of ITO target material surface deposition one deck bonding force greatly about the indium metal layer of 30 microns of left and right, meet the requirement of next step soldering making target material assembly.
Comparative example 1
The indium metal of 4N is heated to 180 degree fusings, is cast to and in graphite jig, is made into indium metal target and is contained on TSU-600 coating equipment.ITO target first cleans 10 minutes with 10% oxalic acid, and then acetone cleans 5 minutes, put into again pure water ultrasonic cleaning 20min, after being fixed in the coating equipment movements and postures of actors after dry, start multi-arc ion plating film function, under higher coating temperature and under higher current/voltage, carry out plated film, technique is as follows: T(temperature)=200 DEG C, P
arplated film 10 minutes under the processing parameter of=1Pa, V=100V, I=6A, after cooling, in coating equipment, take out, clean target material surface 10 minutes with ethanol, to remove surperficial pollutent, expose silvery white metal level, so just can be in ITO target material surface deposition a layer thickness greatly about the indium metal layer of 150 microns of left and right, more coarse by observing metal plating, pellet density is 8 × 10
3individual, can not meet the requirement of next step soldering making target material assembly.
Claims (1)
1. ion deposition is realized a method for ITO target back face metalization, comprises use multi-Arc Ion Plating, adopts Mud-arc ion-plating, it is characterized in that detailed process is:
The 99.99% indium metal heat fused that is 4N by purity, is cast in ganoid graphite jig, is made into indium metal target, and surface is fixed on target pedestal after cleaning with acetone;
ITO target, after oxalic acid, acetone and pure water ultrasonic cleaning are dried, is fixed on multi-Arc Ion Plating, ITO target to be processed is placed on the vacuum chamber work rest of multi-Arc Ion Plating; First forvacuum to 5 × 10
-4pa, is heated to after 100 ~ 150 DEG C of temperature, is filled with argon gas and prepares plated film after certain pressure;
First after the 200V negative voltage bias voltage of 5 ~ 10min cleans, start multi-Arc Ion Plating, at ITO surface deposition layer of metal indium film;
When vacuum chamber greenhouse cooling to 60 DEG C takes out and clean target material surface below, can obtain the even ITO target of metalized of surface;
Coating process parameter area is as follows: temperature is 100 ~ 150 DEG C, and voltage is 20 ~ 80V, electric current 0.1 ~ 0.6A, and time 5 ~ 15min, ar pressure is 0.3 ~ 1Pa.
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| CN106893980B (en) * | 2017-03-28 | 2019-06-14 | 常州市爱华真空设备有限公司 | Low-temperature vacuum coating method |
| CN112359331B (en) * | 2020-10-23 | 2022-11-29 | 北京安泰六九新材料科技有限公司 | Planar binding target and binding method thereof |
| CN115094378B (en) * | 2022-06-13 | 2023-11-03 | 桂林电子科技大学 | Multilayer composite ITO film |
| CN115074666B (en) * | 2022-06-13 | 2023-11-03 | 桂林电子科技大学 | Preparation method of multilayer composite ITO film |
| CN114836726A (en) * | 2022-06-29 | 2022-08-02 | 亚芯半导体材料(江苏)有限公司 | Method for realizing metallization of back of ITO target by cold spraying |
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