CN105349951A - Method for preparing zinc alloy oxide target through plasma spraying process - Google Patents
Method for preparing zinc alloy oxide target through plasma spraying process Download PDFInfo
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- CN105349951A CN105349951A CN201510737723.4A CN201510737723A CN105349951A CN 105349951 A CN105349951 A CN 105349951A CN 201510737723 A CN201510737723 A CN 201510737723A CN 105349951 A CN105349951 A CN 105349951A
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- spraying
- bushing pipe
- zinc
- zinc alloy
- target material
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
Abstract
Provided is a method for preparing a zinc alloy oxide target through a plasma spraying process. A zinc alloy oxide target material is subjected to full mixing and spray granulation, a liner pipe with an inner stainless steel tube made of an aluminum zinc oxide rotating target is additionally selected, and then the zinc alloy oxide target material is sprayed to the surface of the liner pipe through electric arcs to form a bonding layer; and the liner pipe with the formed bonding layer is mounted on plasma transmission equipment, thermal spraying equipment is started, and after the thickness reaches a set value, and no crack or pore exists, the zinc alloy oxide target is prepared further through surface machining and treatment. The preparation cost of the zinc alloy oxide target is reduced, and the production efficiency of the target is improved. The length is not limited, the large-area film coating need can be directly met, and the use rate is high.
Description
Technical field
The present invention relates to the C23C sputtering method coating technology in IPC classification, belong to and be applied to glass coating, photovoltaic and flat-panel monitor, photoelectric field new and high technology material, especially adopt plasma spray coating process to prepare the method for zinc alloy oxide target material.
Background technology
20th century flat panel display appearance, the mankind have been brought into information society, and from then on human society there occurs qualitative leap.And the core parts of flat pannel display are exactly thin film transistor TFT (ThinFilmTransistor), a kind of on the glass substrate by FET device that thin-film technique makes.Conductor oxidate is made TFT as active layer to be used in flat pannel display, and can not only obtain high mobility, device performance is superior, and manufacturing process is simple, can obtain under low temperature, shows huge application prospect.
In recent years, along with the fast development of sputter coating technology, new preparation of target materials technology constantly occurs, target quality and performance also achieves and significantly improves.The Application and Development of rotating cathode target makes the utilization ratio of target bring up to 80% from 30% of traditional rectangular planar target, and substantial saving in coating cost, from then on rotary target material is widely applied in plated film industry.
Target is the starting material of vacuum plating, and the purity of target, density directly affect composition and the over-all properties of film system.Therefore, for ensureing that sputtered film has the homogeneity of lower resistivity, the high transparency and film thickness, the target used is the homogeneity that composition or crystalline orientation all must have, high-density and low resistivity.So preparing in zinc alloy oxide target material process, should ensure that zinc alloy oxide composite powder purity is not less than 99.95%, strict kind and the quantity controlling impurity.The consistence of excellent homogeneity and bulk article quality just can be had like this in target length of life sputtered film.
Transparent conductive oxide film is the focus of photoelectric field always, wherein tin indium oxide (ITO) film is current investigation and application transparent conductive oxide (Transparentcondactiveoxide the most widely, TCO) film, the photoelectric characteristic good because of it and be widely used in various photoelectric device, but because the prices of raw and semifnished materials are expensive, indium resource scarcity and to environment, thus limit its development and application.
Zinc alloy is based on zinc, add other elementary composition alloys.The alloying element often added has the Low Temperature Zn alloys such as aluminium, copper, magnesium, cadmium, lead, titanium.Zinc alloy fusing point is low, good fluidity, easy melting welding, and soldering and plastic working are corrosion-resistant in an atmosphere, and maimed material is convenient to reclaim and remelting; But creep strength is low, easily there is natural aging and cause dimensional change.Prepared by scorification, die casting or press working are become a useful person.Cast zinc alloy and deformation zinc alloy can be divided into by manufacturing process.The main adding elements of zinc alloy has aluminium, copper and magnesium etc. and zinc alloy can be divided into deformation and cast zinc alloy two class by complete processing. and cast zinc alloy mobility and erosion resistance better, are applicable to die casting instrument, auto parts shell etc.
Zinc oxide aluminum (AZO) film not only has the photoelectric characteristic compared favourably with ITO, and there is aboundresources, material non-toxic, the advantage such as chemical stability is good, with low cost and wear-resistant in hydrogen plasma, therefore zinc oxide aluminum film is regarded as the optimal candidate material of alternative ito thin film, has then started research boom at home and abroad.
The preparation method of AZO transparent conductive film is various, and the best approach of generally acknowledging is magnetron sputtering, this method technical maturity, film resiativity is low, transmissivity is high and surface topography is good, film growth temperature near room temperature, good with substrate attachment, can Large-Area-Uniform masking and masking cost is low.
Be generally used for ZnO, In of preparation TFT
2o
3, SnO
2be easy to be formed polycrystalline state Deng film, there is very important a large amount of crystal boundary and oxygen defect, and it is poor to form device rear stability, volt-ampere characteristic is changed significantly in time, and these all hinder it and further develop.Zinc-tin oxide (ZnSnO) film generally presents non-crystalline state, but also ensures higher electronic mobility.In recent years, adopt zinc-tin oxide amorphous alloy oxide semiconductor to do raceway groove in the world and develop high performance thin film transistor and become study hotspot, be considered to a very promising material.
Adopt amorphous ZnSnO alloy firm as active layer to make TFT, device all has good electric property, and device mobility can reach 9.1cm
2/ (V.s), on-off ratio also reaches 10
4above.By subsequent annealing process, the performance of device is obtained for obvious improvement.
From the viewpoint of technology of preparing, target tissue and sputtering performance, it is utilize electric arc target material to be heated to melting or semi-melting state that metallic target is prepared in spraying, be atomized by high-speed gas, form little molten drop, and accelerating jetting is to bushing pipe or backing surface, quick cooled and solidified becomes the process of metallic coating target; Nonmetal and ceramic target normally utilizes the method for heating plasma powdered material to spray and makes.
Traditional method preparing zinc alloy oxide target material has: hot isostatic pressing method, sintering process, extrusion process and teeming practice four kinds.Four kinds of methods respectively have relative merits, but all can not meet the demand of large-area coating film practical application well, prepare length close to 4 meters, the high purity hollow circuit cylinder target of diameter of phi 150 ~ 190mm remains difficulty.Specifically, adopt hot isostatic pressing method cannot produce large-size target, existing record display, adopts the target length of this legal system to fail more than 2m; Adopt sintering process only can single target within production length 500mm; Also there is many limiting factors in extrusion process and teeming practice, as being applied to nonmetal target manufacture.So under prior art conditions, can only be fastened on to reach length requirement on bushing pipe by more piece, this method has increased considerably cost, and can not meet large-area coating film, and especially building glass plated film is to the requirement of target.
Comparatively close prior art is less, published patent documentation does not have good reference value yet, such as: Chinese patent application 201110256260.1 prepares cylindrical large-area coating film target and method with plasma spraying, preparation method comprises 4 steps, and namely spraying powder is produced, matrix prepares, key coat sprays, plasma spraying is shaping; By single metal and non-metallic material, or various metals or non-metallic material form the monomer target with thickness on bushing pipe by thermospray, and Technological adaptability is strong, meets various material and the requirement of length dimension target simultaneously.
Summary of the invention
The object of this invention is to provide a kind of method adopting plasma spray coating process to prepare zinc alloy oxide target material, overcome the weak point of existing metal rotation target production technique, a kind of plasma spray coating process is provided to prepare zinc alloy oxide target material, make the cylinder target length that obtains unrestricted, can directly meet large-area coating film demand, there is higher rate of utilization, realize the good control of target manufacturing cost simultaneously.
Object of the present invention will be realized by following technical measures: preparation method comprises following steps:
1) spraying powder is produced: take the zinc alloy oxide target material material that purity is not less than 99.95wt%, and fully sieve after grinding, grit number is 200 ~ 450 orders, obtains spraying powder through mist projection granulating;
2) matrix prepares: the internal lining pipe being zinc alloy oxide compound rotary target material with stainless steel tube or titanium pipe, surface treatment is carried out to bushing pipe, comprise and remove liner surface dirt and zone of oxidation, sandblasting is carried out to liner surface, by the liner surface roughness (Ra) after sandblasting roughening treatment 1.5 ~ 2.5;
3) key coat spraying: to step 2) in bushing pipe after surface treatment form one deck key coat by electric arc spraying mode in liner surface, key coat comprises at least one in Ni, Cr, Al, Ti;
4) plasma spraying is shaping: by step 1) in obtained zinc alloy oxide compound spraying powder load plasma spraying powder feeder, by step 3) in formed key coat after bushing pipe be arranged on plasma transmission apparatus, bushing pipe rotates with own central axis, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, in spraying process, keeps bushing pipe wall and thermospray spray gun spacing distance, control the translational speed of spray gun, guarantee coating is smooth, setting coating thickness, obtained target.
Especially, be the AZO target material material of 99.99% by purity, wherein alumina content is 2%, through fully mixing, crosses 250 mesh sieves, then by mist projection granulating, makes material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3855mm is zinc oxide aluminum rotary target material, after removing surface smut and zone of oxidation, sandblasting is carried out to liner surface, then form the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacer is kept to off normal 200mm, obtained zinc oxide aluminum spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-aluminium of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 8mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained AZO target material.
Especially, be the zinc-tin oxide target material of 99.95% by purity, stannic oxide content is 5%, through fully mixing, crosses 300 mesh sieves, then by mist projection granulating, makes material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3850mm is zinc-tin oxide rotary target material, after removing surface smut and zone of oxidation, sandblasting is carried out to liner surface, then form the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacer is kept to off normal 200mm, obtained zinc-tin oxide spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-tin of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 9mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained zinc-tin oxide target.
Advantage of the present invention and effect: adopt plasma spray coating process to prepare zinc alloy oxide target material, reduce zinc alloy oxide target material preparation cost, improve target production efficiency; Length is unrestricted, can directly meet large-area coating film demand, have higher rate of utilization.
Embodiment
The principle of the invention is, by zinc alloy oxide target material material, through fully mixing, and mist projection granulating, alternative gets the internal lining pipe that interior stainless steel tube is zinc oxide aluminum rotary target material, then forms key coat by electric arc spraying in liner surface; Being arranged on plasma transmission apparatus by forming the bushing pipe after key coat, starting thermal spraying apparatus, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained zinc alloy oxide target material.
In the present invention, preparation method comprises following steps:
1) spraying powder is produced: take the zinc alloy oxide target material material that purity is not less than 99.95wt%, and fully sieve after grinding, grit number is 200 ~ 450 orders, obtains spraying powder through mist projection granulating, makes powder have good mobility;
2) matrix prepares: the internal lining pipe being zinc alloy oxide compound rotary target material with stainless steel tube or titanium pipe, surface treatment is carried out to bushing pipe, comprise and remove liner surface dirt and zone of oxidation, sandblasting is carried out to liner surface, by the liner surface roughness (Ra) after sandblasting roughening treatment 1.5 ~ 2.5, liner surface after roughening treatment has larger contact area, to increase the contact strength between follow-up coating and bushing pipe wall;
3) key coat spraying: to step 2) in bushing pipe after surface treatment form one deck key coat by electric arc spraying mode in liner surface, key coat comprises one or more in Ni, Cr, Al, Ti;
4) plasma spraying is shaping: zinc alloy oxide compound spraying powder obtained in step one is loaded plasma spraying powder feeder, by step 3) in formed key coat after bushing pipe be arranged on plasma transmission apparatus, bushing pipe rotates with own central axis, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, in spraying process, keeps bushing pipe wall and thermospray spray gun spacing distance, control the translational speed of spray gun, guarantee coating is smooth, setting coating thickness, obtained target.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1: be the AZO target material material of 99.99% by purity, wherein alumina content is 2%, through fully mixing, crosses 250 mesh sieves, then by mist projection granulating, makes material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3855mm is zinc oxide aluminum rotary target material, after removing surface smut and zone of oxidation, sandblasting is carried out to liner surface, then form the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacer is kept to off normal 200mm, obtained zinc oxide aluminum spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-aluminium of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 8mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained AZO target material.
Embodiment 2: be the zinc-tin oxide target material of 99.95% by purity, stannic oxide content is 5%, through fully mixing, crosses 300 mesh sieves, then by mist projection granulating, makes material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3850mm is zinc-tin oxide rotary target material, after removing surface smut and zone of oxidation, sandblasting is carried out to liner surface, then form the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacer is kept to off normal 200mm, obtained zinc-tin oxide spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-tin of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 9mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained zinc-tin oxide target.
Claims (3)
1. adopt plasma spray coating process to prepare the method for zinc alloy oxide target material, it is characterized in that, preparation method comprises following steps:
1) spraying powder is produced: take the zinc alloy oxide target material material that purity is not less than 99.95wt%, and fully sieve after grinding, grit number is 200 ~ 450 orders, obtains spraying powder through mist projection granulating;
2) matrix prepares: the internal lining pipe being zinc alloy oxide compound rotary target material with stainless steel tube or titanium pipe, surface treatment is carried out to bushing pipe, comprise and remove liner surface dirt and zone of oxidation, sandblasting is carried out to liner surface, by the liner surface roughness (Ra) after sandblasting roughening treatment 1.5 ~ 2.5;
3) key coat spraying: to step 2) in bushing pipe after surface treatment form one deck key coat by electric arc spraying mode in liner surface, key coat comprises at least one in Ni, Cr, Al, Ti;
4) plasma spraying is shaping: by step 1) in obtained zinc alloy oxide compound spraying powder load plasma spraying powder feeder, by step 3) in formed key coat after bushing pipe be arranged on plasma transmission apparatus, bushing pipe rotates with own central axis, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, in spraying process, keeps bushing pipe wall and thermospray spray gun spacing distance, control the translational speed of spray gun, guarantee coating is smooth, setting coating thickness, obtained target.
2. the method adopting plasma spray coating process to prepare zinc alloy oxide target material as claimed in claim 1, it is characterized in that, it is the AZO target material material of 99.99% by purity, wherein alumina content is 2%, through fully mixing, cross 250 mesh sieves, then by mist projection granulating, make material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3855mm is zinc oxide aluminum rotary target material, sandblasting is carried out to liner surface, after removing surface smut and zone of oxidation, forms the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface again, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacing distance is kept to be 200mm, obtained zinc oxide aluminum spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-aluminium of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 8mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained AZO target material.
3. the method adopting plasma spray coating process to prepare zinc alloy oxide target material as claimed in claim 1, it is characterized in that, it is the zinc-tin oxide target material of 99.95% by purity, stannic oxide content is 5%, through fully mixing, cross 300 mesh sieves, then by mist projection granulating, make material powder have good mobility, choose internal diameter 125mm, external diameter 133mm, internal lining pipe that the stainless steel tube of length 3850mm is zinc-tin oxide rotary target material, sandblasting is carried out to liner surface, after removing surface smut and zone of oxidation, forms the thick key coat of one deck 0.2mm by electric arc spraying mode in liner surface again, be arranged on plasma transmission apparatus by forming the bushing pipe after key coat, start transmission mechanism, bushing pipe rotates with own central axis, arranging bushing pipe rotating speed is 100r/min, thermal spraying gun is unidirectional or move back and forth along liner conduit length direction, arranging spray gun translational speed is 0.8m/min, spraying area length 3820mm, in spraying process, bushing pipe wall and thermospray spray gun spacer is kept to off normal 200mm, obtained zinc-tin oxide spraying powder is loaded plasma spraying powder feeder, start thermal spraying apparatus, consume the timely supplemental zinc-tin of situation according to powder to dust, guarantee coating is smooth, setting coating thickness is 9mm, treat that thickness arrives set(ting)value and flawless and pore, further through surface working process i.e. obtained zinc-tin oxide target.
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| CN201510737723.4A CN105349951A (en) | 2015-11-03 | 2015-11-03 | Method for preparing zinc alloy oxide target through plasma spraying process |
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| CN201510737723.4A CN105349951A (en) | 2015-11-03 | 2015-11-03 | Method for preparing zinc alloy oxide target through plasma spraying process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280877A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and AZO target of AZO target |
| CN109881162A (en) * | 2018-11-29 | 2019-06-14 | 芮瑛 | A kind of sputtering target material preparation process based on plasma spraying technology |
| CN112746260A (en) * | 2020-12-30 | 2021-05-04 | 湖南柯盛新材料有限公司 | Process for manufacturing rotary target material by cold spraying and production equipment thereof |
| CN114182222A (en) * | 2021-11-03 | 2022-03-15 | 梭莱镀膜工业(江阴)有限公司 | Preparation process of conductive metal oxide target |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286717A (en) * | 2011-09-01 | 2011-12-21 | 基迈克材料科技（苏州）有限公司 | Cylindrical large-area film coating target prepared through plasma spray coating and method |
-
2015
- 2015-11-03 CN CN201510737723.4A patent/CN105349951A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286717A (en) * | 2011-09-01 | 2011-12-21 | 基迈克材料科技（苏州）有限公司 | Cylindrical large-area film coating target prepared through plasma spray coating and method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280877A (en) * | 2018-11-13 | 2019-01-29 | 江苏迪丞光电材料有限公司 | The preparation method and AZO target of AZO target |
| CN109881162A (en) * | 2018-11-29 | 2019-06-14 | 芮瑛 | A kind of sputtering target material preparation process based on plasma spraying technology |
| CN112746260A (en) * | 2020-12-30 | 2021-05-04 | 湖南柯盛新材料有限公司 | Process for manufacturing rotary target material by cold spraying and production equipment thereof |
| CN112746260B (en) * | 2020-12-30 | 2023-02-28 | 湖南柯盛新材料有限公司 | Process for manufacturing rotary target material by cold spraying and production equipment thereof |
| CN114182222A (en) * | 2021-11-03 | 2022-03-15 | 梭莱镀膜工业(江阴)有限公司 | Preparation process of conductive metal oxide target |
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Application publication date: 20160224 |