CN103031524A - 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 preparation 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 the most widely TCO material of use range, and the working order of ITO target has important impact to the performance of film in the ito thin film preparation process.
In ITO target coating process, the ITO target formation target material assembly that is connected with heat conductivility backboard good and that have certain physical strength, metal backing is mainly target in magnetron sputtering provide enough physical strengths to support, a large amount of heat energy that target can be produced in sputter procedure again simultaneously in time take away to prevent that with water coolant the target excessive temperature from raising, and need target is connected processing with metal backing for this reason.The normal operation red copper is as the metal backing material on the coating wire.
The ITO target will stand the continuous bombardment of high-energy argon ion in the film coating sputtering process, also will have enough linking intensities with the copper backboard in high vacuum simultaneously.The copper backboard is then in time taken away the heat that sputter produces by strong water coolant, causes the target cracking otherwise heat can make the target temperature sharply rise, even comes off from backboard and to cause industrial accident, so target must have the good quality that connects with backboard.
Because the ITO target is stupalith, fusing point is more than 2000 degree, so backboard connects with the target big area and can only adopt method for welding and can not adopt fusion welding method; Adopt of the at present welding of ITO target and metallic copper backboard welded as the welding process of solder with indium metal or indium alloy more.The 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 the target back side preplating excessive layer (this process is known as the back face metalization of target) of layer of metal at least, could satisfy the 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 ".
The pressure braze method is fit to the welding of metal targets and backboard, but the ITO ceramic target for fragility is not suitable for using, 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, and is not used in electro-beam welding method.The back side is brushed the silver slurry and not only can be affected in the performance of the lower ITO target of higher sintering temperature (600 ~ 800 ℃) at sintering method, and the auxiliary agents such as the silver that contains in the silver slurry, copper can introduce other a large amount of metal ions when target reclaims, and have increased the target cost recovery.Electrolysis process not only produces a large amount of pollutions, and there is empty unsound phenomenon in metal layer, affects back soldering effect.Conventional evaporation, the sputter of adopting prepares metallized method needs the higher equipment of expense, and because coating speed is low, and efficiency ratio is lower, main is that metal level and target bonding force are not high, affects the soldering effect.Therefore present various ITO target back side metallization technologies all are not ideal.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of ion deposition is realized ITO target back face metalization, by the 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 purpose at the ITO back face metalization.
For the purpose that realizes solving the problems of the technologies described above, the present invention has adopted following technical scheme:
The present invention is the method that a kind of ion deposition is realized ITO target back face metalization, comprises the use multi-Arc Ion Plating, adopts Mud-arc ion-plating, and detailed process is:
Be the 99.99% indium metal heat fused of 4N with purity, be cast in the ganoid graphite jig, be made into the indium metal target, the surface is fixed on the target pedestal after cleaning with acetone;
The ITO target is fixed on the multi-Arc Ion Plating after drying through oxalic acid, acetone and pure water ultrasonic cleaning, ITO target to be processed is placed on the vacuum chamber work rest of multi-Arc Ion Plating; Elder generation's forvacuum to 5 * 10
-4Pa, be heated to temperature after, be filled with argon gas and behind certain pressure, prepare plated film;
At first after the 200V negative voltage bias voltage cleaning through 5 ~ 10min, start multi-Arc Ion Plating, at ITO surface deposition layer of metal indium film;
Below vacuum chamber greenhouse cooling to 60 ℃, take out and clean target material surface, can obtain the even ITO target of metalized of surface.This target can be processed the production that is used for the 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 ℃ 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 larger particles to occur, 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 excessively low arc light that can cause the inhomogeneous of metal level or can not produce the test needs of ar pressure.
By adopting technique scheme, the present invention compares other relevant ITO target method for metallising and has following beneficial effect: (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 do not significantly improve the bonding force that substrate temperature can significantly improve metal level and matrix, not only be higher than magnetically controlled sputter method also far above methods such as evaporation, plating like this; (2) indium metal is low melting point metal, and physical method realizes that deposition easily produces oxidative phenomena, and the present invention does not produce pollution in the situation that do not introduce impurity, realizes the non-oxidation low temperature depositing, thus the making high quality target material assembly that guarantees; (3) the assembly temperature rise is smaller, and in 200 ℃, the workpiece deformation amount is very little, can ignore Effective Raise 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 the 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; Have high, the fireballing characteristics of metal layer bonding force, and do not produce pollution, do not introduce other metallic impurity and be conducive to target and 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 is made into the indium metal target in the graphite jig and is contained on the TSU-600 multi-Arc Ion Plating.The ITO target cleaned 10 minutes with 10% oxalic acid first, and then acetone cleaned 5 minutes, put into pure water ultrasonic cleaning 20min again, be fixed on after the drying on the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started the multi-arc ion plating film function, in the T(temperature)=120 ℃, P
ArPlated film is 7 minutes under the processing parameter of=0.7Pa, V=30V, I=0.3A, in coating equipment, take out after the cooling, cleaned target material surface 10 minutes with ethanol, to remove the pollutent on surface, expose silvery white metal level, so just can deposit the greatly indium metal layer about about 10 microns of the good thickness of one deck bonding force at the ITO target material surface, satisfy the requirement that target material assembly is made in next step soldering.
Embodiment 2
The indium metal of 4N is heated to 180 degree fusings, is cast to and is made into the indium metal target in the graphite jig and is contained on the TSU-600 multi-Arc Ion Plating.The ITO target cleaned 10 minutes with 10% oxalic acid first, and then cleaned 5 minutes with acetone, put into pure water ultrasonic cleaning 20min again, be fixed on after the drying on the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started the multi-arc ion plating film function, in the T(temperature)=150 ℃, P
ArPlated film is 5 minutes under the processing parameter of=0.9Pa, V=50V, I=0.4A, in coating equipment, take out after the cooling, cleaned target material surface 10 minutes with ethanol, to remove the pollutent on surface, expose silvery white metal level, so just can deposit the greatly indium metal layer about about 15 microns of the good thickness of one deck bonding force at the ITO target material surface, satisfy the requirement that target material assembly is made in next step soldering.
Embodiment 3
The indium metal of 4N is heated to 180 degree fusings, is cast to and is made into the indium metal target in the graphite jig and is contained on the TSU-600 multi-Arc Ion Plating.The ITO target cleaned 10 minutes with 10% oxalic acid first, and then cleaned 5 minutes with acetone, put into pure water ultrasonic cleaning 20min again, be fixed on after the drying on the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started the multi-arc ion plating film function, in the T(temperature)=150 ℃, P
ArPlated film is 10 minutes under the processing parameter of=0.7Pa, V=59V, I=0.5A, in coating equipment, take out after the cooling, cleaned target material surface 10 minutes with ethanol, to remove the pollutent on surface, expose silvery white metal level, so just can deposit the greatly indium metal layer about about 25 microns of the good thickness of one deck bonding force at the ITO target material surface, satisfy the requirement that target material assembly is made in next step soldering.
Embodiment 4
The indium metal of 4N is heated to 180 degree fusings, is cast to and is made into the indium metal target in the graphite jig and is contained on the TSU-600 coating equipment.The ITO target cleaned 10 minutes with 10% oxalic acid first, and then cleaned 5 minutes with acetone, put into pure water ultrasonic cleaning 20min again, be fixed on after the drying on the coating equipment movements and postures of actors, bias voltage cleaned after 10 minutes, started the multi-arc ion plating film function, in the T(temperature)=150 ℃, P
ArPlated film is 10 minutes under the processing parameter of=0.7Pa, V=72V, I=0.6A, in coating equipment, take out after the cooling, cleaned target material surface 10 minutes with ethanol, to remove the pollutent on surface, expose silvery white metal level, so just can deposit the greatly indium metal layer about about 30 microns of the good thickness of one deck bonding force at the ITO target material surface, satisfy the requirement that target material assembly is made in next step soldering.
Comparative Examples 1
The indium metal of 4N is heated to 180 degree fusings, is cast to and is made into the indium metal target in the graphite jig and is contained on the TSU-600 coating equipment.The ITO target cleaned 10 minutes with 10% oxalic acid first, and then acetone cleaned 5 minutes, put into again pure water ultrasonic cleaning 20min, after being fixed on the coating equipment movements and postures of actors after the drying, start the multi-arc ion plating film function, the T(temperature)=200 ℃, P carrying out plated film under the higher coating temperature and under the higher current/voltage, technique is as follows:
ArPlated film is 10 minutes under the processing parameter of=1Pa, V=100V, I=6A, in coating equipment, take out after the cooling, cleaned target material surface 10 minutes with ethanol, to remove the pollutent on surface, expose silvery white metal level, so just can deposit the greatly indium metal layer about about 150 microns of a layer thickness at the ITO target material surface, more coarse by observing metal plating, pellet density is 8 * 10
3Individual, can not satisfy the requirement that target material assembly is made in next step soldering.
Claims (2)
1. the method for an ion deposition realization ITO target back face metalization comprises the use multi-Arc Ion Plating, adopts Mud-arc ion-plating, it is characterized in that detailed process is:
Be the 99.99% indium metal heat fused of 4N with purity, be cast in the ganoid graphite jig, be made into the indium metal target, the surface is fixed on the target pedestal after cleaning with acetone;
The ITO target is fixed on the multi-Arc Ion Plating after drying through oxalic acid, acetone and pure water ultrasonic cleaning, ITO target to be processed is placed on the vacuum chamber work rest of multi-Arc Ion Plating; Elder generation's forvacuum to 5 * 10
-4Pa, be heated to temperature after, be filled with argon gas and behind certain pressure, prepare plated film;
At first after the 200V negative voltage bias voltage cleaning through 5 ~ 10min, start multi-Arc Ion Plating, at ITO surface deposition layer of metal indium film;
Below vacuum chamber greenhouse cooling to 60 ℃, take out and clean target material surface, can obtain the even ITO target of metalized of surface.
2. described ion deposition is realized the method for ITO target back face metalization according to claim 1, it is characterized in that: the coating process parameter area at ITO surface deposition layer of metal indium film is as follows, temperature is 100 ~ 150 ℃, voltage is 20 ~ 80V, electric current 0.1 ~ 0.6A, time 5 ~ 15min, ar pressure are 0.3 ~ 1Pa.
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| CN106893980A (en) * | 2017-03-28 | 2017-06-27 | 泉州市中知信息科技有限公司 | Low-temperature vacuum coating method |
| CN112359331A (en) * | 2020-10-23 | 2021-02-12 | 北京安泰六九新材料科技有限公司 | Planar binding target and binding method thereof |
| 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 |
| CN115074666A (en) * | 2022-06-13 | 2022-09-20 | 桂林电子科技大学 | Preparation method of multilayer composite ITO film |
| CN115094378A (en) * | 2022-06-13 | 2022-09-23 | 桂林电子科技大学 | Multilayer composite ITO film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115094378A (en) * | 2022-06-13 | 2022-09-23 | 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 |
| CN115094378B (en) * | 2022-06-13 | 2023-11-03 | 桂林电子科技大学 | 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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