WO2015109684A1 - Procédés pour préparer une cible d'oxyde conducteur au graphène composite et leur film conducteur transparent - Google Patents

Procédés pour préparer une cible d'oxyde conducteur au graphène composite et leur film conducteur transparent Download PDF

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Publication number
WO2015109684A1
WO2015109684A1 PCT/CN2014/076825 CN2014076825W WO2015109684A1 WO 2015109684 A1 WO2015109684 A1 WO 2015109684A1 CN 2014076825 W CN2014076825 W CN 2014076825W WO 2015109684 A1 WO2015109684 A1 WO 2015109684A1
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graphene
conductive oxide
conductive film
transparent conductive
graphene composite
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PCT/CN2014/076825
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English (en)
Chinese (zh)
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陈斐
杨爽
吴俊彦
沈强
加乐为
沙龙朱莉
张联盟
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武汉理工大学
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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
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth

Definitions

  • the invention relates to the technical field of photoelectric material preparation, in particular to an electric field activated sintering of a graphene composite conductive oxide target and a magnetron sputtering deposition method of the transparent conductive film.
  • conductive oxide ceramic is a sputtering target widely used for preparing a transparent conductive film, and the transparent conductive film prepared by the same has a large forbidden band width, excellent electrical and optical characteristics, and thus can be widely applied to solar cells, Piezoelectric devices, liquid crystal displays, reflection heat mirrors and other fields.
  • conductive oxide ceramic materials include indium trioxide (In 2 O 3 ), tin dioxide (SnO 2 ), zinc oxide (ZnO) and doping systems thereof, and mass production of various oxide ceramics and transparent conductive films thereof. Improving its optical and electrical properties is of great significance to the development of the electronic information industry.
  • the preparation of transparent conductive films by sputtering is the most studied, most mature, and most widely used method for preparing thin films.
  • the conductive oxide target required for sputter deposition plays an important role in the quality of the transparent conductive film.
  • the quality of the ceramic target such as purity, density, resistivity, etc., will directly affect the performance of the transparent conductive film.
  • Graphene has excellent electrical, mechanical and optical properties and is often used as an enhancement phase to improve the electrical, mechanical and optical properties of materials.
  • Graphene has an electron mobility of more than 15,000 V•s at room temperature and a resistivity of about 10 - 6 ⁇ •cm. It is the material with the lowest resistivity in the world. When it is added as a reinforcing phase to the ceramic matrix, the conductivity of the ceramic material is large. The range is increased.
  • A. Centeno et al. incorporated a graphene with a mass ratio of 0.22% in an alumina matrix by spark plasma sintering to modify the non-conductive ceramic alumina into a conductive ceramic with a resistivity of 8 ⁇ •cm, which broadened its Application area.
  • the silicon nitride ceramic has a resistivity of 1 to 10 ⁇ •cm.
  • MS Jang et al. by incorporating a small amount of graphene into the silicon nitride powder, obtains a conductive silicon nitride ceramic having a low electrical conductivity of at least 2.5. ⁇ 10 -2 ⁇ •cm, greatly improving its electrical conductivity. Therefore, graphene has a wide range of applications for improving the performance of oxide ceramics, and it has a good application prospect by using graphene composite conductive oxide ceramics with excellent performance as sputtering targets for preparing high light transmittance and high conductivity films.
  • the graphene composite conductive oxide powder is sintered at a high temperature to obtain a graphene composite conductive oxide target, which greatly improves the conductivity of the target while ensuring high purity and high density of the target.
  • Preparation of transparent conductive film by magnetron sputtering deposition using graphene composite conductive oxide target the process is simple, the equipment requirements are low, and mass production is easy, and the prepared transparent conductive film and oxide prepared by pure oxide target are prepared. Compared with the film, the conductivity is improved and the high visible light transmittance is maintained.
  • the technical problem to be solved by the present invention is to provide a method for preparing a highly conductive, highly dense graphene composite conductive oxide target, and to prepare a highly transparent, highly conductive oxide film by magnetron sputtering deposition.
  • the addition of trace amounts of graphene to the oxide powder for electric field activation sintering greatly improves the electrical conductivity of the oxide target under high-density conditions, thereby preparing an oxide film having excellent electrical conductivity and good light transmittance.
  • the graphene composite conductive oxide target and the transparent conductive film provided by the invention are prepared by adding trace and high-purity graphene to the conductive oxide to prepare a highly dense and highly conductive graphene composite conductive oxide target. And using a target for magnetron sputtering deposition method to prepare a transparent conductive film with excellent electrical conductivity and good light transmittance, the method comprises the following steps:
  • the graphene and the conductive oxide powder are (0.05 to 2%) by mass ratio: (98 to 99.5%) dispersed and mixed in a solvent, and dried to obtain a uniformly dispersed graphene composite conductive oxide powder;
  • the ground graphene composite conductive oxide powder is placed in a graphite mold, and then subjected to electric field activation sintering, and the sintered ceramic block is the graphene composite conductive oxide target;
  • the sputtering power was adjusted to 10 to 40 W, and the sputtering time was 10 to 60 minutes to obtain a transparent conductive film.
  • the conductive oxide powder may be indium tin oxide, antimony tin oxide or zinc aluminum oxide powder.
  • the technical parameters of the graphene may be: purity ⁇ 99%, thickness 0.5-1.0 nm, and resistivity ⁇ 2 ⁇ •cm.
  • the solvent may be anhydrous ethanol, deionized water or acetone.
  • the dispersing agent used may be dimethylformamide.
  • the graphene composite oxide powder can be composited by the following method:
  • the graphene and the conductive oxide powder are respectively ultrasonically dispersed in a solvent for 2 hours, and the dispersing agent dimethylformamide is added during the dispersion of the graphene to obtain a uniformly dispersed graphene and a conductive oxide solution;
  • the electric field activation sintering process may be: sintering temperature is 900-1500 ° C, pressure is 0-100 MPa, and the temperature is kept for 0-30 minutes.
  • the sintering environment may be a vacuum or a protective atmosphere
  • the protective atmosphere may be a non-oxidizing atmosphere including hydrogen, an ammonia reducing atmosphere, and a nitrogen, argon or helium inert atmosphere.
  • the graphene composite conductive oxide powder is prepared by physical method, which avoids the disadvantages of introducing impurities in the chemical process.
  • the solvent and dispersant used are all volatile organic solvents, which can be completely removed by drying, which ensures the high quality of the prepared ceramics. purity.
  • the electric field activated sintering is used to prepare the conductive oxide target, the heating rate is fast, the sintering time is short, the process is simple, the energy consumption is low, and the utility model can be applied to industrial scale production, and the temperature is 200-300 ° C lower than the conventional sintering temperature.
  • the conductive oxide target prepared by electric field activation sintering has uniform grain size, high density and obvious conductivity, and its density is as high as 98.6%, and the resistivity is as low as 1.6 ⁇ 10 -4 ⁇ •cm.
  • the transparent conductive film prepared by using the graphene composite conductive oxide target has good uniformity, the average visible light transmittance is higher than 85%, and the minimum resistivity is 7.4 ⁇ 10 -5 ⁇ •cm, which is beneficial to popularize large-scale applications.
  • Example 1 is a Raman spectrum of a graphene-composited zinc oxide aluminum ceramic prepared in Example 1.
  • Example 2 is a Raman spectrum diagram of a graphene composite tin antimony oxide ceramic prepared in Example 2.
  • FIG. 3 is a graph showing the resistivity, carrier mobility, and carrier concentration of graphene-composited zinc oxide aluminum ceramics prepared in Examples 4, 6, and 7.
  • Example 4 is a microstructure diagram of a zinc oxide aluminum ceramic prepared in Example 3.
  • Fig. 5 is a sectional view showing the microstructure of an indium tin oxide film prepared in Example 11.
  • Fig. 6 is a view showing the surface topography of the zinc oxide aluminum thin film prepared in Example 12.
  • Zinc oxide aluminum powder and graphene were used as raw materials, and 2 mg of graphene and 4 g of zinc aluminum oxide powder were weighed according to mass fraction of 0.05% and 99.95%, respectively.
  • the graphene and zinc aluminum oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the zinc aluminum oxide dispersion solution were mixed and stirred for 30 minutes. After 1 hour, the mixture was stirred at 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity zinc oxide aluminum ceramic of the present invention having a density of 96.1% and a specific resistance of 4.2 ⁇ 10 -4 ⁇ •cm.
  • tin oxide bismuth powder and graphene as raw materials, 80% of graphene and 4 g of tin oxide were weighed according to mass fraction of 2% and 98%, respectively.
  • the graphene and tin oxide strontium powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the tin oxide cerium dispersion solution were mixed and stirred for 30 minutes. After 1 hour, the mixture was stirred at 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity tin oxide ceramic target of the invention, which has a density of 96.8% and a resistivity of 7.2 ⁇ 10 -4 ⁇ •cm.
  • Zinc oxide aluminum powder and graphene were used as raw materials, and 40% of graphene and 4 g of zinc oxide aluminum were weighed according to mass fraction of 1% and 99%, respectively.
  • the graphene and zinc aluminum oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the zinc aluminum oxide dispersion solution were mixed and stirred for 30 minutes. After 1 hour, the mixture was stirred at 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity zinc oxide aluminum ceramic target of the invention, which has a density of 97.8% and a resistivity of 2.2 ⁇ 10 -4 ⁇ •cm.
  • Zinc oxide aluminum powder and graphene were used as raw materials, and 4% of graphene and 4 g of zinc oxide aluminum were weighed according to mass fraction of 0.1% and 99.9%, respectively.
  • the graphene and zinc aluminum oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the zinc aluminum oxide dispersion solution were mixed and stirred for 30 minutes. After 1 hour, the mixture was stirred at 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity zinc oxide aluminum ceramic target of the invention, which has a density of 96.9% and a resistivity of 3.2 ⁇ 10 -4 ⁇ •cm.
  • indium tin oxide powder and graphene as raw materials, 20 mg of graphene and 4 g of zinc aluminum oxide were weighed according to the mass fraction of 0.5% and 99.5%, respectively.
  • the graphene and indium tin oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the indium tin oxide dispersion solution were mixed and stirred for 30 minutes. After 1 hour, the mixture was stirred at 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a highly dense, highly conductive indium tin oxide ceramic target of the invention, which has a density of 98.4% and a resistivity of 1.6 ⁇ 10 -4 ⁇ •cm.
  • Zinc oxide aluminum powder and graphene were used as raw materials, and 4% of graphene and 4 g of zinc oxide aluminum were weighed according to mass fraction of 0.1% and 99.9%, respectively.
  • the graphene and zinc aluminum oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the zinc oxide dispersion solution were mixed and stirred for 30 minutes, and the ultrasonic 1 After an hour, the mixture was stirred at a constant temperature of 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity zinc oxide aluminum ceramic target of the invention, which has a density of 98.6% and a resistivity of 3.0 ⁇ 10 -4 ⁇ •cm.
  • Zinc oxide aluminum powder and graphene were used as raw materials, and 4% of graphene and 4 g of zinc oxide aluminum were weighed according to mass fraction of 0.1% and 99.9%, respectively.
  • the graphene and zinc aluminum oxide powders were ultrasonically dispersed in an ethanol solvent for 2 hours, and a dispersing agent dimethylformamide was added during the graphene dispersion process, and the graphene and the zinc oxide dispersion solution were mixed and stirred for 30 minutes, and the ultrasonic 1 After an hour, the mixture was stirred at a constant temperature of 100 ° C for 4 hours, placed in a dry box, and dried at 100 ° C for 6 hours.
  • the obtained product is a high-density, high-conductivity zinc oxide aluminum ceramic target of the invention, which has a density of 97.6% and a resistivity of 2.8 ⁇ 10 -4 ⁇ •cm.
  • Example 8 Preparation of zinc oxide aluminum transparent conductive film
  • the zinc oxide aluminum ceramic target prepared in Example 1 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 100 ° C, and the sputtering chamber was filled with oxygen and argon gas, and the flow ratio of oxygen to argon was 1:3, and the pressure in the chamber was adjusted to 2 Pa.
  • the sputtering power was adjusted to 20 W, and the sputtering time was 30 minutes to obtain a zinc oxide aluminum transparent conductive film having a specific resistance of 2.4 ⁇ 10 -4 ⁇ cm and a visible light transmittance of 86%.
  • Example 9 Preparation of zinc oxide aluminum transparent conductive film
  • the zinc oxide aluminum ceramic target prepared in Example 1 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 300 ° C, and the sputtering chamber was filled with oxygen and argon gas.
  • the flow ratio of oxygen to argon was 1:3, and the pressure in the chamber was adjusted to 4 Pa.
  • the sputtering power was adjusted to 30 W and the sputtering time was 60 minutes to obtain a zinc oxide aluminum transparent conductive film having a specific resistance of 2.8 ⁇ 10 -4 ⁇ cm and a visible light transmittance of 85%.
  • Example 10 Preparation of tin oxide antimony transparent conductive film
  • the tin oxide ceramic target prepared in Example 2 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 100 ° C, and the sputtering chamber was filled with oxygen and argon gas, the oxygen to argon flow ratio was 1:3, and the intracavity pressure was 8 Pa.
  • the sputtering power was adjusted to 10 W and the sputtering time was 30 minutes to obtain a tin oxide transparent conductive film having a specific resistance of 3.1 ⁇ 10 -4 ⁇ cm and a visible light transmittance of 87%.
  • Example 11 Preparation of indium tin oxide transparent conductive film
  • the indium tin oxide ceramic target prepared in Example 5 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 400 ° C, and the sputtering chamber was filled with oxygen and argon gas, and the flow ratio of oxygen to argon was 1:3, and the pressure in the chamber was adjusted to 4 Pa.
  • the sputtering power was adjusted to 40 W, and the sputtering time was 10 minutes to obtain an indium tin oxide transparent conductive film having a specific resistance of 7.4 ⁇ 10 -5 ⁇ cm and a visible light transmittance of 87%.
  • Example 12 Preparation of zinc oxide aluminum transparent conductive film
  • the zinc oxide aluminum ceramic target prepared in Example 6 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 300 ° C, and oxygen and argon were charged into the sputtering chamber.
  • the flow ratio of oxygen to argon was 1:3, and the pressure in the chamber was adjusted to 1 Pa.
  • the sputtering power was adjusted to 20 W and the sputtering time was 30 minutes to obtain a zinc oxide aluminum transparent conductive film having a specific resistance of 3.5 ⁇ 10 -4 ⁇ cm and a visible light transmittance of 85%.
  • Example 13 Preparation of zinc oxide aluminum transparent conductive film
  • the zinc oxide aluminum ceramic target prepared in Example 6 and the cleaned quartz glass substrate were placed in a sputtering chamber of a magnetron sputtering apparatus, pumped to a high vacuum of 10 -5 Pa, and pre-sputtered for 5 minutes.
  • the substrate was heated to 200 ° C, and oxygen and argon were charged into the sputtering chamber.
  • the flow ratio of oxygen to argon was 1:3, and the pressure in the chamber was adjusted to 8 Pa.
  • the sputtering power was adjusted to 30 W and the sputtering time was 30 minutes to obtain a zinc oxide aluminum transparent conductive film having a specific resistance of 3.0 ⁇ 10 -4 ⁇ cm and a visible light transmittance of 85%.
  • the conductive oxide ceramic samples obtained in Example 1 and Example 2 were subjected to Raman spectroscopy to determine the phase composition thereof, and Fig. 1 and Fig. 2 were obtained.
  • the obtained compound is ZnO and graphene; the Raman characteristic peak in Fig. 2 is SnO 2 and graphene.
  • Example 6 The resistivity, mobility, and carrier concentration of the conductive oxide ceramic samples prepared in Example 4, Example 6, and Example 7 were measured, and FIG. 3 was obtained.
  • the conductive oxide ceramic sample obtained in Example 3 was subjected to scanning electron microscopy to obtain a microstructure 4 thereof. It can be seen from Fig. 4 that the microstructure of the target after sintering is dense, no obvious pores, and the layered graphene is still dispersed in the oxide ceramic.
  • the morphology of the films prepared in Example 11 and Example 12 was analyzed to obtain Fig. 5 and Fig. 6. It can be seen from the figure that the film thickness is about 400 nm, the grain growth is uniform, and the surface is flat.

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Abstract

L'invention porte sur un procédé pour préparer une cible d'oxyde conducteur au graphène composite et sur son film conducteur transparent, lequel procédé met en œuvre de façon spécifique : l'utilisation d'un graphène de haute pureté et d'une poudre d'oxyde conducteur comme matières premières, la teneur en masse du graphène étant de 0,05 % à 2 % ; le mélange uniforme de ces derniers par un procédé en phase liquide, une agitation et un traitement aux ultrasons dans un solvant, respectivement, puis un mélange et un séchage afin d'obtenir une poudre d'oxyde conducteur au graphène composite ; le fait de soumettre la poudre à un frittage activé par un champ électrique pour obtenir la cible d'oxyde conducteur au graphène composite de densité élevée et de conductivité élevée, la température de frittage étant de 900° C à 1400° C, la pression étant de 0 à 100 MPa et le temps de maintien en température étant de 0 à 30 min ; puis la réalisation d'une déposition par pulvérisation cathodique par magnétron à l'aide de la cible de façon à préparer le film conducteur transparent. Les avantages de la présente invention sont que la cible a une pureté élevée, une densité élevée et une conductivité électrique significativement améliorée ; le film conducteur transparent préparé à partir de la cible a une conductivité électrique améliorée, il peut maintenir un facteur de transmission de la lumière visible relativement élevé, et il peut être largement appliqué dans le domaine de la fabrication d'électrodes transparentes.
PCT/CN2014/076825 2014-01-22 2014-05-06 Procédés pour préparer une cible d'oxyde conducteur au graphène composite et leur film conducteur transparent WO2015109684A1 (fr)

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CN201410028577.3A CN103741094A (zh) 2014-01-22 2014-01-22 石墨烯复合导电氧化物靶材及其透明导电薄膜的制备方法

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CN107068247A (zh) * 2017-04-20 2017-08-18 成都川烯科技有限公司 一种复合导电薄膜及其制备方法以及触控传感器及其制备方法
CN107298583B (zh) * 2017-07-03 2020-02-14 中科院微电子研究所昆山分所 一种二氧化锡复合涂层及其制备方法
CN112349667A (zh) * 2019-08-09 2021-02-09 昆山微电子技术研究院 一种石墨烯/铜复合金属互连线的制备方法
CN114437393A (zh) * 2020-11-06 2022-05-06 湖南七点钟文化科技有限公司 锌基大电阻薄膜镀膜液、其制备方法与锌基大电阻薄膜的制备方法

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