WO2010038954A2 - 투명 도전막 및 이를 구비한 투명 전극 - Google Patents
투명 도전막 및 이를 구비한 투명 전극 Download PDFInfo
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- WO2010038954A2 WO2010038954A2 PCT/KR2009/005482 KR2009005482W WO2010038954A2 WO 2010038954 A2 WO2010038954 A2 WO 2010038954A2 KR 2009005482 W KR2009005482 W KR 2009005482W WO 2010038954 A2 WO2010038954 A2 WO 2010038954A2
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- conductive film
- zinc oxide
- dopant
- transparent conductive
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 86
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000011787 zinc oxide Substances 0.000 claims abstract description 42
- 238000004544 sputter deposition Methods 0.000 claims abstract description 24
- 239000002019 doping agent Substances 0.000 claims description 42
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 claims description 29
- 229910052733 gallium Inorganic materials 0.000 claims description 27
- 238000004519 manufacturing process Methods 0.000 claims description 27
- 229910052782 aluminium Inorganic materials 0.000 claims description 26
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- 239000007789 gas Substances 0.000 claims description 19
- 239000000758 substrate Substances 0.000 claims description 17
- 229910052796 boron Inorganic materials 0.000 claims description 13
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229910052795 boron group element Inorganic materials 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 4
- 150000003624 transition metals Chemical class 0.000 claims description 4
- 230000008685 targeting Effects 0.000 claims 1
- 238000001039 wet etching Methods 0.000 abstract description 6
- 239000010408 film Substances 0.000 description 81
- 230000000052 comparative effect Effects 0.000 description 22
- 238000001878 scanning electron micrograph Methods 0.000 description 11
- 239000010409 thin film Substances 0.000 description 11
- 238000000151 deposition Methods 0.000 description 9
- 230000008021 deposition Effects 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 3
- 229910006404 SnO 2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
- H01L31/022483—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers composed of zinc oxide [ZnO]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0236—Special surface textures
- H01L31/02366—Special surface textures of the substrate or of a layer on the substrate, e.g. textured ITO/glass substrate or superstrate, textured polymer layer on glass substrate
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02554—Oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
Definitions
- the present invention relates to a zinc oxide-based transparent conductive film having irregularities formed on its surface, a method of manufacturing the same, and a transparent electrode for a solar cell using the same.
- the front electrode of the thin film solar cell forms irregularities on its surface in order to increase light conversion efficiency.
- FTO F doped SnO 2
- ZnO ZnO
- FTO fluoride-onitride-onitride
- HF and SnCl 4 are used as the reactor gas, and are prepared by an atmospheric pressure CVD method, which has to be very thick (usually ⁇ 1 ⁇ m or more) and the deposition process is performed at a high temperature of 600 ° C. or higher.
- FTO is very vulnerable to the H atmosphere, that is, there is a problem that is reduced by the H plasma generated in PECVD, which is an active layer (eg, amorphous Si) manufacturing process of a thin-film silicon solar cell has a problem that the transmittance is reduced.
- a thick zinc oxide transparent conductive film is deposited through a sputter, and the surface is formed by wet etching.
- a two-step manufacturing method has been developed. However, in this method, a wet etching process is required after the deposition of a thick film, and thus, the process is cumbersome and increases in time.
- the problem to be solved by the present invention is to use a zinc oxide (ZnO) -based transparent electrode and to form the surface irregularities to increase the light conversion efficiency, wherein the surface irregularities are not subjected to wet etching process
- ZnO zinc oxide
- the present invention is to provide a transparent electrode having the transparent conductive film and a solar cell including the same.
- this invention is a zinc oxide type transparent conductive film in which the unevenness
- a zinc oxide-based transparent conductive film including a protrusion having an obtuse angle of 90 ° or more formed by a ridge line around a vertex.
- the X-ray diffraction image of the conductive film having irregularities has only a peak of the (002) plane.
- the protrusions of the concave-convex portion may have a diagonal length of 200 to 600 nm and a height of 30 to 250 nm, but the present invention is not limited thereto.
- the conductive film may have an element selected from the group consisting of a Group 13 element and a transition metal having an oxidation number of +3 as a dopant.
- the conductive film may have at least one selected from the group consisting of aluminum, gallium, boron or silicon as a dopant.
- the content of the dopant in the conductive film may be 4% by weight or less, preferably 3% by weight or less. More specifically, in the case of using gallium alone as the dopant, the content of gallium in the conductive film is 3% by weight.
- the content of aluminum may be 1% by weight or less, and when boron is used alone as the dopant, the content of boron in the conductive film may be 1% by weight or less.
- the content of aluminum in the conductive film may be 0.5 wt% or less, and the content of gallium may be 1.0 wt% or less.
- the present invention targets a zinc oxide having a dopant content of 0 to 4% by weight, the pressure of 1 to 30 mTorr and 100 to 500 °C in the presence of a mixed gas of argon and hydrogen gas It provides a method for producing a zinc oxide transparent conductive film, characterized in that carried out by a sputtering method of temperature conditions.
- the content of the hydrogen gas may be 1 to 30% by volume in the total gas, but is not limited thereto.
- H 2 O may be further added during the sputtering process.
- the zinc oxide-based transparent conductive film of the present invention is formed on a transparent substrate and can be utilized as a transparent electrode.
- the transparent electrode according to the present invention is very useful for the front electrode of a solar cell.
- FIG. 1 is a SEM image of the surface of a zinc oxide transparent conductive film prepared in Example 1.
- FIG. 2 is an enlarged photograph of a SEM image of the surface of the zinc oxide transparent conductive film prepared in Example 1.
- FIG. 2 is an enlarged photograph of a SEM image of the surface of the zinc oxide transparent conductive film prepared in Example 1.
- FIG. 3 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Comparative Example 1.
- FIG. 4 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Comparative Example 2.
- FIG. 4 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Comparative Example 2.
- FIG. 5 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Comparative Example 3.
- FIG. 5 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Comparative Example 3.
- FIG. 6 is an XRD graph of the zinc oxide transparent conductive film prepared in Example 1.
- FIG. 7 is a SEM image of the surface of the zinc oxide transparent conductive film prepared in Example 2.
- FIG. 8 is a SEM image of the surface of a zinc oxide transparent conductive film prepared in Comparative Example 6.
- FIG. 9 is an AFM photograph of a zinc oxide transparent conductive film prepared in Example 2.
- FIG. 1 A SEM photograph of one embodiment of a zinc oxide-based transparent conductive film having irregularities on its surface according to the present invention is shown in FIG. 1.
- the configuration described in the embodiments and drawings described below are only the most preferred embodiment of the present invention and do not represent all of the technical idea of the present invention, which can be replaced at the time of the present application It should be understood that there may be various equivalents and variations.
- the transparent conductive film of the present invention has irregularities formed by protrusions having a relatively gentle inclination.
- protrusions of the surface irregularities according to the present invention there are substantially two forms (A, B).
- the first shape of the protruding portion 10 is a shape in which the ridge portion 11 where the face meets the arc in the protruding direction of the protruding portion 10.
- the "arc" includes not only a perfect arc as part of a circle, but also a case of a substantially curved line rather than a straight line.
- the second shape of the protrusion 10 is a horn shape in which the protrusion 10 has a vertex, the vertex is formed by two or more ridges meet, the angle ( ⁇ ) formed by the two ridges (11, 12) of the ridges It is an obtuse angle of more than 90 °.
- "obtuse angle” means an angle having a size of 90 degrees or more and less than 180 degrees.
- two forms in most means that at least 40%, preferably at least 50%, more preferably at least 70% of the surface uneven protrusions have the two forms.
- the upper limit thereof is not particularly limited. For example, it may be 90%, preferably 99%, but is not limited thereto.
- the size of the protrusions of the unevenness according to the present invention may vary depending on the specific sputtering conditions in the manufacturing process, for example, the diagonal length of the bottom surface may be 200 to 600 nm, the height may be 30 to 250 nm. . Excellent light scattering effect can be obtained in the above range.
- the unevenness may have a value of R a (surface roughness) of 15 nm or more.
- FIG. 3 An X-ray diffraction image of the conductive film having surface irregularities according to the exemplary embodiment of the present invention is illustrated in FIG. 3.
- the X-ray diffraction image has only a peak of the (002) plane, and accordingly, the surface unevenness of the conductive film of the present invention has a certain directivity.
- the zinc oxide transparent conductive film of the present invention may further include an element selected from the group consisting of a Group 13 element and a transition metal having an oxidation number of +3 as a dopant to enhance conductivity.
- the dopant may have at least one selected from the group consisting of aluminum, gallium, boron, and silicon, but is not limited thereto.
- the content of the dopant in the conductive film of the present invention may be 4% by weight or less, preferably 3% by weight or less. If the content exceeds 4% by weight, surface irregularities may not be formed and the resistivity of the conductive film may be increased. .
- the lower limit of the dopant content is not particularly limited because the conductivity only needs to be increased, but it may be 0.1 wt% as a preferable example in which an additional dopant addition effect can be expected.
- the content of gallium in the conductive film may be less than 3% by weight.
- the content of aluminum in the conductive film may be 1% by weight or less.
- the content of boron in the conductive film may be 1 wt% or less.
- the content of aluminum in the conductive film is 0.5 wt% or less.
- the content of gallium may be 1.0 wt% or less.
- the conductive film of the present invention may preferably have a thickness of 100 to 500 nm, but since the thickness can be adjusted according to a specific use, the thickness is not particularly limited. If the thickness is less than 100 nm, the electrical conductivity is lowered and the size of the surface irregularities is smaller, and if it is more than 500 nm, the transparency of the conductive film may be lowered.
- the conductive film of the present invention may have various haze values according to surface irregularities formed under various conditions. For example, it can have a haze value of 5% or more.
- the conductive film of this invention it is preferable to have suitable electroconductivity, For example, it is preferable to have a specific resistance of 5 * 10 ⁇ -2> Pacm or less.
- a zinc oxide having a dopant content of 0 to 4% by weight is targeted, and a pressure of 1 to 30 mTorr and 100 to 500 ° C in the presence of a mixed gas of argon and hydrogen gas. It is characterized in that it is carried out by the sputtering method of the temperature conditions.
- the method for producing a transparent conductive film of the present invention uses zinc oxide rather than FTO (F doped SnO 2 ), which is vulnerable to a hydrogen atmosphere.
- the conventional method of manufacturing a zinc oxide transparent conductive film was a wet etching process after the deposition process was essential, the method of manufacturing a zinc oxide transparent conductive film of the present invention by adjusting the various conditions of the sputtering process surface unevenness without additional wet process It is a method which can manufacture the formed zinc oxide type transparent conductive film.
- the zinc oxide that is the target of sputtering may further contain a dopant, and the specific content thereof is as described above.
- a mixed gas of argon (Ar) and hydrogen (H 2 ) is used as the atmosphere gas.
- the hydrogen gas is preferably 1 to 30% by volume based on the total gas. If the content is less than 1% by volume, surface irregularities are not properly formed, and if it exceeds 30% by volume, the light transmittance of the formed thin film may be reduced.
- H 2 O may be further added during the sputtering process according to the present invention.
- H 2 O may be introduced into the chamber through a separate injection device (eg leak valve), it is preferred that the injected H 2 O is 20% by volume or less based on the total gas.
- the pressure is preferably 1 to 30 mTorr. If the pressure is less than 1 mTorr, the plasma is not stably formed, and thus film deposition is difficult. If the pressure is more than 30 mTorr, the size of the irregularities formed is significantly reduced.
- the temperature is preferably carried out at 100 to 500 ° C, preferably at 100 to 400 ° C, more preferably around 200 ° C. If the said temperature is less than 100 degreeC, the magnitude
- the sputtering method applicable in the present invention is not particularly limited as long as it is a method commonly used in the art, and for example, RF or DC sputtering may be used.
- a zinc oxide-based transparent conductive film formed by sputtering is deposited on an appropriate substrate, and when the substrate is a transparent substrate, a transparent electrode can be formed.
- the substrate capable of forming the transparent electrode by depositing the zinc oxide-based transparent conductive film of the present invention is not limited as long as it is a transparent substrate.
- the substrate may be a glass substrate, a plastic substrate, an oxide deposited substrate, or the like.
- the transparent electrode according to the present invention can be usefully used as a front electrode of a thin film solar cell.
- Example 1 Ga doped ZnO / Glass with (Ar + H 2 ) Transparent conductive film manufacturing
- a zinc oxide-based transparent conductive film was deposited on the glass substrate at a thickness of about 200 ° C. and a pressure of about 3 mTorr using an RF magnetron sputter and a Ga-doped zinc oxide target of 2.72 wt%.
- the working gas was a gas mixed with Ar and H 2 , the ratio was H 2 / (Ar + H 2 ) to 7 vol%.
- Comparative Example 1 Ga doped ZnO / Glass with Ar transparent conductive film manufacturing
- a zinc oxide transparent conductive film was prepared in the same manner as in Example 1, except that only Ar gas was used as the working gas.
- Comparative Example 2 Ga doped ZnO / Glass with (Ar + H 2 ) Transparent conductive film manufacturing
- a zinc oxide transparent conductive film was manufactured in the same manner as in Example 1, except that the doping content of Ga was 5.5 wt%.
- Comparative Example 3 Ga doped ZnO / Glass with (Ar + H 2 ) Transparent conductive film manufacturing
- a zinc oxide transparent conductive film was prepared in the same manner as in Example 1 except that the deposition temperature of the thin film was RT ( ⁇ 23 ° C.).
- Example 1 The haze of the zinc oxide transparent conductive films prepared in Example 1 and Comparative Examples 1 to 3 was measured and described in Table 1, and surface SEM photographs of each conductive film were measured to show FIGS. 1 (Example 1) and 3. To FIG. 5 (Comparative Examples 1 to 3, respectively).
- Example 1 Specimen Type Atmosphere gas Deposition temperature (°C) Thickness (nm) Haze (%)
- Example 1 GZO (2.72 wt%) / Glass Ar + H 2 200 To 450 36.30 Comparative Example 1 GZO (2.72 wt%) / Glass Ar 200 To 550 0.16 Comparative Example 2 GZO (5.5 wt%) / Glass Ar + H 2 200 To 440 0.13 Comparative Example 3 GZO (2.5 wt%) / Glass Ar + H 2 RT To 400 0.21
- Example 1 is a SEM image of the surface of the transparent conductive film prepared in Example 1, it can be seen that the irregularities are effectively formed on the surface according to FIG. Light scattering occurs due to the irregularities, and as a result, the haze value is very large (36.3%).
- FIG. 3 is a SEM image of the surface of the transparent conductive film prepared in Comparative Example 1.
- Comparative Example 1 only Ar was used without mixing hydrogen gas as a working gas. As a result, surface irregularities were not observed. This confirms that the incorporation of hydrogen gas has a decisive influence on the formation of surface irregularities.
- FIG. 4 is a SEM image of the surface of the transparent conductive film prepared in Comparative Example 2.
- FIG. Also, unlike FIG. 1, large irregularities were not observed on the surface, and as a result, the haze value was very small (0.13%).
- Comparative Example 2 In the case of the specimen, the specimen was deposited with the dopant content outside the scope of the present invention, and as a result, no surface irregularities were observed.
- Figure 5 is a SEM image of the surface of the transparent conductive film prepared in Comparative Example 3, it can be seen that also uneven surface is not formed sufficiently unlike in Example 1. From this, the dependence of the surface asperity shape with the deposition temperature was confirmed. That is, it can be seen that the specimen should be deposited in the temperature range of the present invention in order to form the appropriate surface irregularities.
- Sputtering deposition was performed in the same manner as in Example 1 except that the Ga content was changed as shown in Table 2 below.
- the surface irregularities of the deposited conductive film were evaluated according to the change of the content, and when haze was 5% or more, "O" and "X" were evaluated.
- sputtering deposition was performed in the same manner as in Example 1 except for using a zinc oxide target having an Al content.
- Sputtering deposition was carried out in the same manner as in Example 1, except that aluminum and gallium were simultaneously used as dopants, and zinc oxide targets in which the Al and Ga contents were changed as shown in Table 4 were used.
- X-ray diffraction analysis was performed on the unevenly formed transparent conductive film prepared according to Example 1, and the graph is shown in FIG.
- the zinc oxide-based transparent conductive film having the surface irregularities according to the present invention can be seen that only the peak of the (002) plane appears.
- Example 2 (Ga + B) doped ZnO / Glass with (Ar + H 2 + H 2 O) Transparent conductive film manufacturing
- a zinc oxide transparent conductive film was deposited on a glass substrate using an RF magnetron sputter and a zinc oxide target doped with Ga and B 2.5 wt% and 0.2 wt%, respectively, at a temperature of about 200 ° C. and a pressure of about 3 mTorr. .
- a sputtering gas As a sputtering gas, a mixture of Ar and H 2 was used, and a ratio of H 2 / (Ar + H 2 ) was 7 vol%.
- the device was configured to allow H 2 O to flow into the chamber through a leak valve that can inject water into the middle of the gas line, and the thickness of the thin film was controlled between 150 and 200 nm.
- Comparative Example 4 Ga doped ZnO / Glass with (Ar + H 2 O) Transparent conductive film manufacturing
- Example 2 In the same manner as in Example 2, a zinc oxide transparent conductive film was produced.
- the surface shape and roughness of the zinc oxide transparent conductive films prepared in Example 2 and Comparative Example 4 were analyzed by SEM and AFM, and the results are shown in Table 5 and FIGS. 7 to 9.
- the measured part was measured in the center (center, denoted by c in Table 5 below) and the edge (edge, denoted by e in Table 5 below).
- Example 2 of the present invention is a sufficient unevenness to form an effective roughness degree
- Comparative Example 4 can be confirmed that it is not.
- Example 2 of the present invention irregularities were formed on the surface (FIG. 7), but in Comparative Example 4, it was confirmed that the irregularities were not substantially formed on the surface (FIG. 8). Referring to Figure 9, Example 2 of the present invention can be confirmed that the irregularities formed uniformly over the entire surface.
- a zinc oxide transparent conductive film having surface irregularities can be manufactured by a sputtering process without a separate process such as wet etching, thereby simplifying the process and manufacturing time, and the overall thin film. It is possible to form irregularities of uniform size and uniform shape, and to manufacture a transparent conductive film having a small thickness and small specific resistance.
- the zinc oxide-based transparent conductive film according to the present invention can be used as electrodes of various devices such as thin film solar cells.
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- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Non-Insulated Conductors (AREA)
- Physical Vapour Deposition (AREA)
- Manufacturing Of Electric Cables (AREA)
- Photovoltaic Devices (AREA)
- Laminated Bodies (AREA)
Abstract
Description
시편 종류 | 분위기 가스 | 증착온도(℃) | 두께(nm) | Haze(%) | |
실시예 1 | GZO(2.72 wt%)/Glass | Ar + H2 | 200 | ~450 | 36.30 |
비교예 1 | GZO(2.72 wt%)/Glass | Ar | 200 | ~550 | 0.16 |
비교예 2 | GZO(5.5 wt%)/Glass | Ar + H2 | 200 | ~440 | 0.13 |
비교예 3 | GZO(2.5 wt%)/Glass | Ar + H2 | RT | ~400 | 0.21 |
Ga 함량(wt%) | 0.0 | 0.5 | 1.8 | 2.5 | 2.7 | 3.0 | 4.5 | 5.5 |
요철 형성 여부 | O | O | O | O | O | X | X | X |
Al 함량(wt%) | 1.00 | 1.25 | 1.50 | 2.00 |
요철 형성 여부 | O | X | X | X |
Al 함량(wt%) | 0.50 | 0.80 | 0.50 | 0.80 | 1.00 |
Ga 함량(wt%) | 0.75 | 0.50 | 1.00 | 1.00 | 1.50 |
요철 형성 여부 | O | O | O | X | X |
구분 | 스퍼터링 조건 | 표면 요철 여부 | 거칠기(Ra(nm)기준) |
실시예 2 | Ga(2.5wt%) doping + B(0.2wt%) doping + Ar + H2 + H2O | 있음 | c ~ e = 21 |
비교예 4 | Ga(2.5wt%) doping + Ar + H2O | 없음 | c ~ e = 3 |
Claims (23)
- 표면에 요철이 형성된 산화아연계 투명 도전막으로서,상기 요철은, 돌출부의 능선부가 돌출부의 돌출 방향으로 호를 이루거나, 돌출부의 말단이 꼭지점을 갖는 경우에는 꼭지점을 중심으로 두 능선부가 이루는 각이 90°이상의 둔각인 돌출부를 포함하는 산화 아연계 투명 도전막.
- 제1항에 있어서,상기 요철을 갖는 도전막의 X선 회절 상은 (002)면의 피크만을 갖는 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제1항에 있어서,상기 요철의 돌출부는 밑면의 대각선 길이가 200 내지 600 nm이고, 높이가 30 내지 250 nm인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제1항에 있어서,상기 도전막은 13족 원소 및 +3의 산화수를 갖는 전이금속으로 구성된 군에서 선택된 원소를 도펀트로 갖는 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제1항에 있어서,상기 도전막은 알루미늄, 갈륨, 붕소 또는 실리콘으로 이루어진 군에서 선택되는 적어도 하나를 도펀트로 갖는 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제5항에 있어서,상기 도전막 내에 도펀트의 함량은 4중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제5항에 있어서,도펀트로 갈륨을 단독으로 사용하는 경우에는 도전막 내에 갈륨의 함량은 3중량% 미만인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제5항에 있어서,도펀트로 알루미늄을 단독으로 사용하는 경우에는 도전막 내에 알루미늄의 함량은 1중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제5항에 있어서,도펀트로 붕소를 단독으로 사용하는 경우에는 도전막 내에 붕소의 함량은 1중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제5항에 있어서,도펀트로 갈륨과 알루미늄을 사용하는 경우에는 도전막 내에 알루미늄의 함량은 0.5 중량% 이하이며, 갈륨의 함량은 1.0 중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 제1항에 있어서,상기 도전막은 두께가 100 내지 500 nm인 것을 특징으로 하는 산화 아연계 투명 도전막.
- 도펀트의 함량이 0 내지 4중량%인 산화 아연을 타켓으로 하여, 아르곤과 수소 가스의 혼합가스 존재 하에 1 내지 30 mTorr의 압력 및 100 내지 500 ℃의 온도 조건의 스퍼터링 방식으로 수행되는 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제12항에 있어서,상기 도펀트는 13족 원소 및 +3의 산화수를 갖는 전이금속으로 구성된 군에서 선택된 원소인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제12항에 있어서,상기 도펀트는 알루미늄, 갈륨, 붕소 또는 실리콘으로 이루어진 군에서 선택되는 적어도 하나인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제14항에 있어서,도펀트로 갈륨을 단독으로 사용하는 경우에는 도전막 내에 갈륨의 함량은 3중량% 미만인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제14항에 있어서,도펀트로 알루미늄을 단독으로 사용하는 경우에는 도전막 내에 알루미늄의 함량은 1중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제14항에 있어서,도펀트로 붕소를 단독으로 사용하는 경우에는 도전막 내에 붕소의 함량은 1중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제14항에 있어서,도펀트로 갈륨과 알루미늄을 사용하는 경우에는 도전막 내에 알루미늄의 함량은 0.5 중량% 이하이며, 갈륨의 함량은 1.0 중량% 이하인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제12항에 있어서,스퍼터링 공정 시 H2O를 더 투입하는 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 제12항에 있어서,상기 수소 가스의 함량은 전체 가스에 대하여 1 내지 30 부피%인 것을 특징으로 하는 산화 아연계 투명 도전막의 제조방법.
- 기판; 및상기 기판 상에 형성된 제1항 내지 제11항 중 어느 한 항의 투명 도전막;을 구비하는 산화 아연계 투명 전극.
- 제21항에 있어서,상기 기판은 유리 기판, 플라스틱 기판 또는 산화물 증착 기판으로서, 투명성을 갖는 것을 특징으로 하는 산화 아연계 투명 전극.
- 제22항의 투명 전극을 구비한 태양전지.
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EP09817964.1A EP2333818B1 (en) | 2008-09-30 | 2009-09-25 | Transparent conductive film, and transparent electrode comprising same |
US13/121,577 US20110174361A1 (en) | 2008-09-30 | 2009-09-25 | Transparent conductive layer and transparent electrode comprising the same |
CN2009801380876A CN102165559B (zh) | 2008-09-30 | 2009-09-25 | 透明导电层和包括该透明导电层的透明电极 |
JP2011528939A JP5581527B2 (ja) | 2008-09-30 | 2009-09-25 | 透明導電膜、その製造方法、透明電極及び太陽電池 |
US14/480,392 US9966495B2 (en) | 2008-09-30 | 2014-09-08 | Transparent conductive layer and transparent electrode comprising the same |
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US14/480,392 Division US9966495B2 (en) | 2008-09-30 | 2014-09-08 | Transparent conductive layer and transparent electrode comprising the same |
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JP (1) | JP5581527B2 (ko) |
KR (1) | KR101201099B1 (ko) |
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2009
- 2009-09-25 KR KR20090090854A patent/KR101201099B1/ko active IP Right Grant
- 2009-09-25 EP EP09817964.1A patent/EP2333818B1/en active Active
- 2009-09-25 JP JP2011528939A patent/JP5581527B2/ja active Active
- 2009-09-25 CN CN2009801380876A patent/CN102165559B/zh active Active
- 2009-09-25 US US13/121,577 patent/US20110174361A1/en not_active Abandoned
- 2009-09-25 WO PCT/KR2009/005482 patent/WO2010038954A2/ko active Application Filing
- 2009-09-28 TW TW098132729A patent/TWI494452B/zh active
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2014
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US20120270013A1 (en) * | 2011-04-22 | 2012-10-25 | Samsung Corning Precision Materials Co., Ltd. | ZnO-BASED TRANSPARENT CONDUCTIVE THIN FILM FOR PHOTOVOLTAIC CELL AND MANUFACTURING METHOD THEREOF |
CN103258866A (zh) * | 2012-02-21 | 2013-08-21 | 三星康宁精密素材株式会社 | 导电膜基板、具有该基板的光伏电池及制造该基板的方法 |
Also Published As
Publication number | Publication date |
---|---|
JP2012504306A (ja) | 2012-02-16 |
EP2333818A4 (en) | 2015-06-17 |
CN102165559A (zh) | 2011-08-24 |
CN102165559B (zh) | 2013-09-04 |
US20110174361A1 (en) | 2011-07-21 |
US20140374242A1 (en) | 2014-12-25 |
TW201028487A (en) | 2010-08-01 |
KR101201099B1 (ko) | 2012-11-13 |
US9966495B2 (en) | 2018-05-08 |
TWI494452B (zh) | 2015-08-01 |
JP5581527B2 (ja) | 2014-09-03 |
KR20100036957A (ko) | 2010-04-08 |
WO2010038954A3 (ko) | 2010-07-22 |
EP2333818A2 (en) | 2011-06-15 |
EP2333818B1 (en) | 2019-12-25 |
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