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WO1992018990A1 - Procede pour la fabrication de films conducteurs transparents - Google Patents

Procede pour la fabrication de films conducteurs transparents Download PDF

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Publication number
WO1992018990A1
WO1992018990A1 PCT/JP1992/000455 JP9200455W WO9218990A1 WO 1992018990 A1 WO1992018990 A1 WO 1992018990A1 JP 9200455 W JP9200455 W JP 9200455W WO 9218990 A1 WO9218990 A1 WO 9218990A1
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WO
WIPO (PCT)
Prior art keywords
transparent conductive
conductive film
gas
film
sputtering
Prior art date
Application number
PCT/JP1992/000455
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English (en)
Japanese (ja)
Inventor
Tokio Nakada
Original Assignee
Tokio Nakada
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tokio Nakada filed Critical Tokio Nakada
Priority to JP50807692A priority Critical patent/JP3325268B2/ja
Publication of WO1992018990A1 publication Critical patent/WO1992018990A1/fr

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Classifications

    • 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
    • C23C14/087—Oxides of copper or solid solutions thereof
    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • C23C14/0057—Reactive sputtering using reactive gases other than O2, H2O, N2, NH3 or CH4

Definitions

  • the present invention relates to a method for manufacturing a transparent conductive film having a surface texture structure, and more particularly to a method for manufacturing a transparent conductive film suitable for a configuration of a photoelectric conversion device by sputtering.
  • a transparent conductive film conventionally, S n 0 2 system, (eg, I n 2 O 3: S n O 2 (1 0 wt%), ITO) I n 2 0 3 system and the like are known .
  • S n 0 2 system eg, I n 2 O 3: S n O 2 (1 0 wt%), ITO
  • the film surface is also incident due to the light confinement effect. It is important to have a surface texture structure that allows effective use of light and to have high transmittance in the near-infrared region. Also, it is desired that the resistive resistance be as low as possible ( ⁇ 10 ⁇ / port).
  • a transparent conductive film having a surface texture structure is conventionally known by a chemical vapor deposition (CVD) method.
  • the S n 0 2 is resistant problem of poor to hydrogen plasma.
  • ZnO has good resistance to hydrogen plasma. Therefore, the Amorufu ⁇ scan S i film, when forming on S n 0 2 by the plasma CVD method is considered to be Koti ring of Z n O film on S n 0 2.
  • a sputtering method as a method for producing a transparent conductive film that does not use a toxic gas as a main raw material.
  • a transparent conductive film having a surface texture structure has not been obtained by the sputtering method.
  • the transparent conductive ZnO: B film obtained by the MOCVD method described above has a problem that the change with time is large. For example, This film is 200 in air. If left for 10 hours in the state of C, the resistance value changes to about twice the initial value. In the case of solar batteries, environmental resistance is a major issue, and this is also an issue to be solved.
  • An object of the present invention is to provide a method for manufacturing a transparent conductive film capable of forming a transparent conductive film having a surface texture structure by a sputtering method.
  • a method for producing a transparent conductive film on a substrate by sputtering at least a part of the composition of a target film is used as a component.
  • a method for producing a transparent conductive film is provided, wherein the target is sputtered in a gas atmosphere containing OH to form a transparent conductive film.
  • the target transparent conductive film is, for example, Zn0,
  • Zn0 X (X is one of Al, Si, B, F, and CI)
  • OH in the gas atmosphere containing OH is generated by decomposing a compound having an OH group.
  • the compound having an OH group for example, at least one of water and alcohol can be used. These can be used alone or as a mixture with an inert gas such as Ar.
  • a compound gas containing an unblendable substance to be doped can be mixed into the sputtering gas.
  • a target for forming a film of the target substance described above a target composed of the same substance as the target substance can be used.
  • reactive sputtering is performed by introducing metals such as n, Sn, and InSn, which are mixed or not mixed with unbleached substances, and introducing oxygen in addition to other gases. You can also do
  • the present invention uses an oxide-based target having at least the composition of a target film as a component, and performs sputtering in a gas atmosphere containing OH to form an oxide on a substrate.
  • a system transparent conductive film may be formed.
  • a method of manufacturing an oxide-based transparent conductive film on a substrate by sputtering wherein the oxide-based transparent conductive film has at least a target film composition as a component.
  • a method for producing a transparent conductive film is provided, wherein sputtering is performed using a target and a gas containing B 2 H ⁇ .
  • the gas containing B 2 Hs for example, a gas obtained by diluting B 2 Hs with Ar is used.
  • the target for example, ZnO is used. It is.
  • a texture structure is formed on the surface of the film. This generation mechanism is not always clear, but can be considered as follows.
  • OH in the atmosphere is generated by decomposing compounds having OH groups.
  • compounds having OH groups For example, water and alcohol.
  • ⁇ H in the atmosphere for example, and H which is generated by decomposing a gas containing hydrogen such as B 2 H e, is made fresh from 0 Metropolitan separated from the oxide-based target.
  • the film is formed by sputtering, not only is toxic gas not used as a raw material, but also it is easy to form a large-area transparent conductive film.
  • a transparent conductive film having a surface texture structure can be formed by sputtering.
  • FIG. 1 is a cross-sectional view showing one embodiment of a DC magnetron sputtering apparatus preferably used for producing a transparent conductive film of the present invention.
  • FIG. 3 is a graph showing the wavelength dependence of the total transmittance T d, turbidity M and diffuse reflectance R of the sample of Example 2.
  • FIG. 4 is a graph showing the wavelength dependence of the total transmittance Td, turbidity M, and diffuse reflectance R of the sample of Example 3 (3-a, 3-b, 3-c).
  • FIG. 5 is a graph showing the wavelength dependence of the total transmittance T d, turbidity, and diffuse reflectance R of the sample of Example 4.
  • Figure 6 is a graph showing the substrate temperature dependence of resistivity, mobility, and carrier concentration for the sample of Example 3 (3-a, 3-b, 3-c).
  • FIG. 7A is a photograph showing the observation result of the sample of Comparative Example 4 by SEM
  • FIG. 7B is a photograph showing the observation result of the sample surface of Example 5 by SEM.
  • FIG. 8 shows the results for the samples of Examples 5 to 7 and Comparative Examples 4 and 5.
  • FIG. 9 is a graph showing the dependence of resistivity, mobility, and carrier concentration on the doping amount of B 2 H 6 for each of the samples of Examples 5 to 7 and Comparative Example 4.
  • FIG. 10A is a photograph showing the observation result of the sample of Comparative Example 6 by SEM
  • FIG. 10B is a photograph showing the observation result of the sample surface of Example 9 by SEM.
  • FIG. 11 is a graph showing the dependence of resistivity, mobility, and carrier concentration on the doping amount of B 2 H 6 for each of the samples of Examples 8 to 13 and Comparative Example 6.
  • the DC magnetron sputtering device shown in FIG. 1 has a vacuum chamber 1 that is evacuated by an exhaust system 2 having an exhaust device (not shown), and a gas chamber for introducing gas into the vacuum chamber 1.
  • the system includes a gas introduction system 3, a target electrode 4, a substrate electrode 5, and a power supply device (not shown).
  • the gas introduction system 3 is connected to an Ar gas supply source (not shown) to regulate the introduction amount of Ar gas and a flow control valve 31 for controlling the introduction amount of the mixture of the impurity doping gas and the texture structure forming gas. It is provided with a flow control valve 32 for adjusting the flow rate, a flow control valve 33 for adjusting the introduction amount of the mixed gas, and a gas inlet 34 to which the gas introduction system 3 is connected.
  • the target gas May be introduced in advance. For example, as shown in the examples below, B 2 previously diluted with Ar
  • Target electrode 4 is connected to target 40 and this target
  • the substrate electrode 5 includes a plate 51 on which the substrate 50 is placed, a plate holder 52 for holding the plate 51, and a heater 53 for heating the substrate 50.
  • the substrate glass, quartz or the like is used.
  • the distance between the substrate 50 and the target 40 is 35 ⁇ in Examples 1 to 4 and Comparative Examples 1 and 2. Further, in Example 5 and later, and in Comparative Example 4 and later, 5 Omm is set.
  • a disk having a diameter of 10 cm is used as the target 40.
  • Is a substance, Z n O (9 9 9 wt.) Or Z n O: sintered body of A 1 (2 wt% A 1 2 0 3) is used.
  • a mixed gas of A r and beta 2 Eta epsilon is Ru is used.
  • Sputtering was carried out under the same conditions as in Example 1 except that the sputtering gas was Ar, and a ZnO thin film having a thickness of 1.5 m was formed on a glass substrate.
  • Td-T / Td T is the transmittance at normal incidence
  • R the measurement results of the wavelength dependence of the diffuse reflectance R are shown.
  • FIG. 2 (shown by a solid line in this figure) sample was deposited by introducing Eta 2 0 is compared with the sample of Comparative Example was sputtered using A r 1 (indicated by a broken line in this figure)
  • a r 1 indicated by a broken line in this figure
  • the sputtering gas was changed to boric acid solution under the conditions of a sputtering gas pressure (operating gas pressure) of 5 X 10 _3 Torr and a substrate temperature of 400.
  • H 3 B 0 3 + H 2 0) solution gas and Ar are mixed in a one-to-one ratio and sputtered for 1 hour to form a film having a thickness of about 1.5 ⁇ m on a glass substrate.
  • a ZII0: B thin film was formed.
  • a sputtering gas, a solution gas and Alpha iota »and mixed gas in a one-to-one borate methyl alcohol (H 3 B 0 3 + CH a OH), the substrate temperature, room temperature (Example 3 - a) , At 300 ° C. (Example 3—b) and at 400 ° C. (Example 3—c), the sputtering was performed under the same conditions as in Example 2 above, A Zn0 ⁇ B thin film was formed with a thickness of 1.5 m.
  • the sputtering gas, solution gas boric acid + H 2 0 + CH 3 OH and A Sputtering was performed under the same conditions as in Example 2 except that r and were mixed in a one-to-one ratio, and a ZnO: B thin film was formed on a glass substrate to a thickness of about 1.5 jam. Was formed.
  • FIG. 3 to 5 show the wavelength dependence of the total transmittance T d, turbidity M and diffuse reflectance R for each of the samples of Examples 2 to 4.
  • FIG. 6 shows the substrate temperature dependence of resistivity, mobility, and carrier concentration for the sample of Example 3.
  • the turbidity indicating the degree of white turbidity was highest when a mixed solution of boric acid water and alcohol was used, and reached 70% or more at 600 nm.
  • the turbidity increased with the substrate temperature.
  • the transmittance in the near-infrared region decreases with decreasing substrate temperature, suggesting that the lower the temperature, the higher the boron concentration doped in the film.
  • Tag gas pressure (operating gas pressure) 2 X 10 Torr, substrate temperature 2000, sputtering gas used to dilute ⁇ 2 ⁇ 6 with Ar ⁇ 2 ⁇ ⁇ concentration 1 Sputtering was performed for 1 hour using a gas of 0.0 vol% to form a Zn0: B thin film with a thickness of about 2 ⁇ on a glass substrate.
  • the sputtering gas, B 2 except that the H e was B 2 H e concentration 0. 8 vol% gas obtained by diluting with A r is performed Supadzuta the same conditions as in Example 5, a glass substrate A ZnO: B thin film having a thickness of about 2 m was formed thereon.
  • the sputtering gas, in addition to the beta 2 Eta epsilon was beta 2 Eta epsilon concentration 0 ⁇ 5 vol% of gas obtained by diluting with A r is performed sputtering under the same conditions as those in Example 5, a glass substrate A Zn0: B thin film was formed on the upper surface with a thickness of about 2 m.
  • Sputtering was performed for 1 hour using Ar 100% gas as the sputter gas under the conditions of 10 Torr and a substrate temperature of 200.
  • Ar 100% gas as the sputter gas under the conditions of 10 Torr and a substrate temperature of 200.
  • a ZnO Al thin film was formed on a glass substrate with a thickness of about 2 tm.
  • Fig. 7 (A) shows a photograph of the observation result of the sample of Comparative Example 4
  • Fig. 7 (B) shows a photograph of the observation result of the sample of Example 5.
  • the surface has a pyramid-shaped irregularity peculiar to the texture structure.
  • FIG. 8 shows the wavelength dependence of the total transmittance T d for the samples of Examples 5 to 7 and Comparative Examples 4 and 5.
  • FIG. 9 shows the dependence of resistivity, mobility, and carrier concentration on the doping amount of ⁇ 2 ⁇ 6 for each of the samples of Examples 5 to 7 and Comparative Example 4.
  • the B 2 H 6 -doped sample (b, c, d) in the near infrared region was smaller than the ZnO: A1 thin film of Comparative Example 5 in the near-infrared region.
  • the transmittance is ⁇ ⁇ . Comparing d and e in the figure, ZnO: B (d) has a high mobility and a low carrier concentration even at almost the same resistivity. For this reason, ZnO: B (d) can reduce free electron absorption and correspondingly increase the transmittance.
  • each sample thin film B satisfies substantially the condition.
  • the sample thin film of ZnO: B of Example 5 has a remarkable texture structure, can expect an effect of confining incident light, and is preferable as a transparent conductive film.
  • a spa Ttagasu pressure (the working gas pressure) 2 X 1 0- Torr, as a spatter gas, beta 2 Eta epsilon at A r using diluted B 2 H s concentration 1 obtained.
  • 0 vol% of a gas in each of the following substrate temperature, perform the 1 hour spatter, Z n a thickness of approximately 2 m on a glass substrate ⁇ : B thin film was formed.
  • New paper Sputtering was carried out under the same conditions as in Example 8 except that the substrate temperature was set to 100 ° C (sputtered without heating) to form a Zn film with a thickness of about 2 m on the glass substrate.
  • FIG. 10 (B) shows a photograph of the observation result of the sample of Example 9.
  • the figure has a surface structure exhibiting pyramid-shaped irregularities peculiar to the texture structure.
  • the surface structure was almost the same for each sample from 200 ° C to 400 ° C.
  • it can have sample Nitsu of Comparative Example 6, not using B 2 H e, as compared to that shown in FIG. 7 (A), slight but although irregularities of the surface were observed.
  • FIG. 10 (A) shows a photograph of the observation result of Comparative Example 6.
  • Example 8-1 3 Oyopi Comparative Example 6 shows the resistivity, mobility, the doping amount dependency of B 2 H e of calibration Li A concentration. As shown in the figure, a material having a low resistivity is obtained in a wide temperature range from 150 ° to 300 °. In addition, even if the substrate temperature is low, low resistivity is obtained. Then, as described above, 200. In the range of C to 400 ° C, the surface structure exhibits pyramid-shaped irregularities peculiar to the texture structure. Is obtained.
  • H 2 0 or alcohol or by using these mixed solution gas as the sputtering gas, rather by efficiency, texturing of the film can be realized. Further, as shown in Examples 2 to 4, by doping with boron, a low-resistance film having a high total transmittance could be obtained.
  • a film having a low resistivity and a texture structure can be formed at a relatively low temperature in a film forming process.
  • a film can be formed.
  • the initial sheet resistance value 4 ⁇ changed to 4.4 ⁇ . Therefore, the change was reduced by about 10%.
  • the transparent conductive film produced by the present invention has a low resistivity, a high transmittance, and is textured, so that it can be used as a window material for a solar cell or an optical sensor. By using this, improvement of photoelectric conversion efficiency is expected. In addition, since the device has good environmental resistance, it is possible to reduce the time-dependent change of a device used outdoors such as a solar cell, and to prolong its life.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing Of Electric Cables (AREA)
  • Physical Vapour Deposition (AREA)
  • Non-Insulated Conductors (AREA)

Abstract

L'invention se rapporte à un procédé qui sert à former un film conducteur transparent, dont la surface présente une structure à texture, par une technique de dépôt par pulvérisation. A cet effet, on utilise une cible (40) à base d'un oxyde, qui possède comme constituant au moins la composition du film désiré, et on pulvérise la cible dans une atmosphère gazeuse contenant OH, afin de former un film conducteur transparent sur la base (50).
PCT/JP1992/000455 1991-04-10 1992-04-10 Procede pour la fabrication de films conducteurs transparents WO1992018990A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP50807692A JP3325268B2 (ja) 1991-04-10 1992-04-10 透明導電膜の製造方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP7784291 1991-04-10
JP3/77842 1991-04-10

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WO1992018990A1 true WO1992018990A1 (fr) 1992-10-29

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012504306A (ja) * 2008-09-30 2012-02-16 エルジー・ケム・リミテッド 透明導電膜及びそれを備えた透明電極
JP2012506486A (ja) * 2008-10-21 2012-03-15 アプライド マテリアルズ インコーポレイテッド 透明導電性亜鉛酸化物ディスプレイフィルム及びその製造方法
JP2012160661A (ja) * 2011-02-02 2012-08-23 Ulvac Japan Ltd 透明導電膜付き基板、太陽電池及びそれらの製造方法
JP2012158823A (ja) * 2011-02-02 2012-08-23 Ulvac Japan Ltd 成膜方法
JP2013517381A (ja) * 2010-01-19 2013-05-16 フラウンホーファー−ゲゼルシャフト ツル フェルデルング デル アンゲヴァンテン フォルシュング エー ファウ 透明で伝導性の金属合金酸化物を有する基板を真空被覆する方法並びに金属合金酸化物でできた透明で伝導性の層

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63181462A (ja) * 1987-01-23 1988-07-26 Hitachi Ltd 受光素子およびこの受光素子を使用する一次元イメ−ジセンサ
JPH0238568A (ja) * 1988-07-28 1990-02-07 Toshiba Corp 薄膜形成装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63181462A (ja) * 1987-01-23 1988-07-26 Hitachi Ltd 受光素子およびこの受光素子を使用する一次元イメ−ジセンサ
JPH0238568A (ja) * 1988-07-28 1990-02-07 Toshiba Corp 薄膜形成装置

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012504306A (ja) * 2008-09-30 2012-02-16 エルジー・ケム・リミテッド 透明導電膜及びそれを備えた透明電極
JP2012506486A (ja) * 2008-10-21 2012-03-15 アプライド マテリアルズ インコーポレイテッド 透明導電性亜鉛酸化物ディスプレイフィルム及びその製造方法
JP2013517381A (ja) * 2010-01-19 2013-05-16 フラウンホーファー−ゲゼルシャフト ツル フェルデルング デル アンゲヴァンテン フォルシュング エー ファウ 透明で伝導性の金属合金酸化物を有する基板を真空被覆する方法並びに金属合金酸化物でできた透明で伝導性の層
JP2012160661A (ja) * 2011-02-02 2012-08-23 Ulvac Japan Ltd 透明導電膜付き基板、太陽電池及びそれらの製造方法
JP2012158823A (ja) * 2011-02-02 2012-08-23 Ulvac Japan Ltd 成膜方法

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