WO2012147219A1 - Pellicule conductrice transparente et procédé de formation associé - Google Patents

Pellicule conductrice transparente et procédé de formation associé Download PDF

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Publication number
WO2012147219A1
WO2012147219A1 PCT/JP2011/069550 JP2011069550W WO2012147219A1 WO 2012147219 A1 WO2012147219 A1 WO 2012147219A1 JP 2011069550 W JP2011069550 W JP 2011069550W WO 2012147219 A1 WO2012147219 A1 WO 2012147219A1
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Prior art keywords
transparent conductive
conductive film
film
forming
transparent
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PCT/JP2011/069550
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English (en)
Japanese (ja)
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高橋　大輔
裕士 今田
真佑 前田
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シャープ株式会社
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Publication of WO2012147219A1 publication Critical patent/WO2012147219A1/fr

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    • 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

Definitions

  • the present invention relates to a transparent conductive film and a film forming method thereof, and more specifically to a transparent conductive film provided on a transparent substrate of a thin film solar cell and a film forming method thereof.
  • a thin film solar cell is manufactured by forming a transparent conductive film on a transparent substrate and further forming a photoelectric conversion layer or the like thereon.
  • the thin-film solar cell has a demerit that the power generation cost is several times higher than other power sources and the production cost is high. In order to eliminate these disadvantages, it is necessary to increase the photoelectric conversion efficiency and simplify the manufacturing method.
  • Patent Document 1 discloses a method for easily producing the transparent conductive film using a spray pyrolysis method. According to the method of Patent Document 1, a transparent conductive film can be produced without forming an underlayer or a buffer layer on a glass substrate. For this reason, it is not necessary to form the film in two stages, and the film forming method can be simplified.
  • the sheet resistance of the transparent conductive film is 10 ⁇ / ⁇ or less, the light transmittance is 80% or more, and the haze ratio is 7 to 15%. It is extremely difficult to adjust these three characteristics. For example, if the film thickness of the transparent conductive film is increased, the sheet resistance can be lowered, but the light transmittance is also lowered.
  • tin oxide As a material satisfying these characteristics, the use of tin oxide, zinc oxide, indium oxide or the like for the transparent conductive film has been studied.
  • tin oxide is widely used for a transparent conductive film of a thin film solar cell because it is a low-cost and chemically stable material.
  • Patent Document 2 a film forming raw material solution blended so as to obtain desired characteristics is adjusted to a high temperature, and then fluorine-doped tin oxide (FTO) is formed by a spray pyrolysis method.
  • FTO fluorine-doped tin oxide
  • Patent Document 2 since a transparent conductive film is formed by a moving spray mechanism, a transparent conductive film having high crystallinity can be formed in a large area regardless of crystal orientation.
  • Patent Document 2 discloses forming a transparent conductive film regardless of the crystal orientation, but generally there is a correlation between the crystal orientation and the surface shape of the transparent conductive film.
  • Non-patent Document 1 K.Murakami et al.Thin Solid Films 515 (2007) 8632-8636 (Non-patent Document 1), when crystal grains with uniform crystal orientation are combined and enlarged, haze is caused by the effect of surface irregularities. Has been reported to be higher.
  • JP 7-330336 A International Publication No. 2008/117605
  • the transparent conductive film disclosed in Patent Document 2 described above is not sufficient in light transmittance, haze ratio, and sheet resistance, and further improvement in performance is required.
  • the crystallinity of the transparent conductive film is good and the light transmittance is high by bonding the crystal grains at a high substrate temperature. And since the size of the crystal grain of a transparent conductive film becomes large, a haze rate can also be raised.
  • the transparent conductive film formed by the film forming method of Patent Document 2 satisfies desired characteristics in that the light transmittance and haze ratio are high.
  • fluorine evaporates due to the high temperature when forming the transparent conductive film.
  • the carrier density in the transparent conductive film decreases and the sheet resistance increases.
  • the present invention has been made in view of the above situation, and the object of the present invention is to provide a transparent conductive film having a high haze ratio and light transmittance and a low sheet resistance, and the transparent An object is to provide a method for easily forming a conductive film.
  • the method for forming a transparent conductive film of the present invention comprises a step of heating a transparent substrate to 510 ° C. or more, and spraying droplets of a film forming raw material solution onto the transparent substrate, thereby forming a transparent conductive film on the transparent substrate.
  • the step of depositing the transparent conductive film is characterized by depositing the transparent conductive film at a deposition rate of 12 nm / sec or more.
  • the film forming raw material solution preferably contains a tin and fluorine compound.
  • the present invention relates to a transparent conductive film formed by the above film forming method, and in the X-ray diffraction pattern of the transparent conductive film, the diffraction peak intensity of the (301) plane is any crystal plane other than the (301) plane. It is characterized by being larger than the diffraction peak intensity.
  • the average particle diameter of the crystal grains calculated from the half-value width of the diffraction peak intensity on the (301) plane is the diffraction peak intensity on any crystal plane other than the (301) plane. It is preferable that the average particle diameter of the crystal grains calculated from the half width is larger.
  • the transparent conductive film can be formed by a simple process by having the above-described configuration.
  • the transparent conductive film formed by the film forming method described above exhibits excellent performance such as high light transmittance and haze ratio and low sheet resistance.
  • FIG. 1 is a schematic cross-sectional view of a film forming apparatus using the method for forming a transparent conductive film of the present invention.
  • the transparent conductive film forming method of the present invention is typically formed using the film forming apparatus shown in FIG.
  • the film forming apparatus in FIG. 1 includes a film forming raw material solution 1 containing a film forming material, a liquid feed pump 2 for transporting the film forming raw material solution 1, and droplet generation for replacing the film forming raw material solution 1 with liquid droplets 5.
  • a part 6, a transparent substrate 7 for forming a transparent conductive film on the surface, and a heating part 8 for heating the transparent substrate 7 are included.
  • the carrier gas 3 is introduced into the nozzle head 4, and the droplet 5 is sprayed onto the transparent substrate 7 by the carrier gas.
  • the transparent substrate 7 is heated by heating the transparent substrate 7 to 510 ° C. or more, and the droplet 5 of the film forming raw material solution 1 is sprayed on the transparent substrate 7.
  • the step of forming the transparent conductive film is characterized in that the transparent conductive film is formed at a film formation rate of 12 nm / sec or more. By forming a film at such a high film formation rate, a transparent conductive film having a high light transmittance and a high haze ratio and a low sheet resistance can be formed. Below, each said step is demonstrated.
  • the film forming method of the present invention includes a step of heating the transparent substrate 7 to 510 ° C. or higher.
  • the transparent substrate 7 By heating the transparent substrate 7 to such a temperature, the crystallinity of the transparent conductive film is improved during or after film formation even if fluorine is taken into the transparent conductive film during film formation. Therefore, the light transmittance can be improved.
  • the transparent substrate 7 is preferably heated to 510 ° C. or higher, more preferably 530 ° C. or higher.
  • the temperature of the transparent substrate 7 is lower than 510 ° C.
  • the crystallinity of the transparent conductive film is lowered due to the temperature lowered by the sprayed film forming raw material solution, which is not preferable.
  • the upper limit of the heating temperature of the transparent substrate 7 is preferably a temperature lower than 700 ° C.
  • the heating temperature of the transparent substrate exceeds 700 ° C., it is not preferable because droplets made of the film forming raw material solution do not easily reach the surface of the substrate and the film forming rate is lowered.
  • the transparent substrate 7 is disposed on the upper surface of the heating unit 8. In the following, the transparent substrate 7 and the heating unit 8 will be described.
  • any material can be used as the transparent substrate 7 as long as it is a transparent material in the absorption region of the photoelectric conversion layer.
  • a glass substrate, a resin material substrate, or the like can be used.
  • a material exhibiting transparency at the wavelength of the absorption region of the photoelectric conversion layer is preferable, and alkali-free glass is preferably used as such a material.
  • the heating unit 8 is provided to heat the transparent substrate to 510 ° C. or higher.
  • the heating unit 8 can be used without particular limitation as long as it can heat the transparent substrate 7 to a predetermined temperature.
  • Such a heating unit 8 includes a method of heating by direct conduction heat transfer using a hot plate, a method of heating by convection heat transfer using a furnace in which the inside is heated, and a method of heating by radiation heat transfer irradiating an infrared lamp or the like. Any of these heating methods can be used.
  • a transparent substrate is heated by direct conduction heat transfer using a hot plate.
  • a transparent conductive film is formed on the transparent substrate 7 by spraying droplets of the film forming raw material solution 1 on the transparent substrate 7.
  • the transparent conductive film is formed at a film formation rate of 12 nm / sec or more.
  • the upper limit of the film forming rate of the transparent substrate 7 is preferably 30 nm / sec or less, and more preferably 20 nm / sec or less. If a transparent conductive film is formed at a film formation rate exceeding 20 nm / sec, there is a problem that the film quality such as crystal orientation deteriorates due to a decrease in the substrate temperature or the like, which is not preferable.
  • any method can be used as long as the film forming raw material solution 1 is formed into droplets 5 having an average particle diameter of 0.1 ⁇ m to several tens ⁇ m.
  • a spray method, an ultrasonic method, or the like can be used.
  • FIG. 1 shows a spray-type droplet generator 6 that applies a high-pressure gas to the film-forming raw material solution 1 to form fine droplets from a fine slit nozzle.
  • the spray method is preferably a two-fluid spray method in which two fluids, a liquid and a carrier gas, are mixed and a droplet is ejected from the tip of the spray nozzle.
  • the film forming raw material solution becomes droplets through the droplet generation unit immediately before the transparent substrate. For this reason, the film-forming raw material solution is conveyed to the tip of the spray nozzle.
  • the droplet is formed by a high-pressure carrier gas, the droplet and the carrier gas are sprayed onto the transparent substrate.
  • a carrier gas may be used in order to provide directivity in the droplet transport direction.
  • compressed air, N 2 , H 2 , water vapor, O 2 , or a mixture of one or more of these can be used.
  • the spray nozzle is made of, for example, a metal and a resin material.
  • droplets are generated from the transparent substrate 7 by applying ultrasonic waves to the film forming raw material solution 1 from the droplet generator 6 attached to the solution bottle. Since the droplet itself has no kinetic energy, the droplet is transported by a carrier gas.
  • the carrier gas the same gas as that used in the above-described spray method can be used.
  • the ultrasonic vibrator can spray droplets having a relatively uniform average particle diameter, there is an advantage that the droplets hardly aggregate.
  • the liquid feed pump 2 preferably has a function of adjusting the supply amount as well as supplying the film forming raw material solution 1 to the nozzle head 4.
  • the transparent conductive film scans either one or both of the transparent substrate 7 and the droplet generator 6, so that the entire surface of the transparent substrate 7 is scanned.
  • the film is formed.
  • the transparent conductive film may be formed by one droplet generator 6 or may be formed by two or more droplet generators 6.
  • two or more droplet generation units are arranged on the entire upper surface of the transparent substrate and droplets are sprayed, it is not always necessary to scan either the transparent substrate 7 or the droplet generation unit 6.
  • the film-forming raw material solution 1 used in the present invention is obtained by dissolving a film-forming material composed of an organic metal or a metal halide compound of an inorganic material such as zinc, tin, indium, cadmium, or strontium in one or more kinds of solvents. Is.
  • the film forming raw material solution 1 generally dissolves the organometallic or metal halide compound at a concentration of 0.1 to 3 mol / L, but is not limited to this concentration.
  • said film-forming raw material solution 1 it is preferable to contain the compound of tin and a fluorine, and it is more preferable to use the thing containing the organometallic compound containing tin and containing the compound of fluorine as a dopant agent.
  • the fluorine compound contained in the film forming raw material solution include hydrogen fluoride and ammonium fluoride.
  • examples of tin contained in the film forming raw material solution include tin tetrachloride, tin dichloride, dibutyltin diacetate, and tetrabutyltin.
  • water, an organic solvent, or a mixture thereof can be used as the solvent used for the film forming raw material solution.
  • the organic solvent here include methanol, ethanol, acetone, isopropyl alcohol, and the like, but are not limited thereto.
  • the film forming raw material solution may further contain an additive in addition to the solvent and the film forming material.
  • additives include a dopant agent, a surfactant, a pH adjuster, and the like, but it is preferable to use a mixture of two or more of these additives.
  • examples of the dopant agent include materials containing Mg, Ga, Al, Te, Ag, Ge, Cu, Sr, B, Sb, F, As, and the like, and examples of the surfactant include lower organic compounds.
  • examples of the pH adjuster include nitric acid, acetic acid, sulfuric acid, hydrofluoric acid, hydrogen peroxide, butyric acid, hydrochloric acid, and ammonia.
  • the film thickness of the transparent conductive film formed by the above film forming method is in the range of 600 nm to 1200 nm in order to satisfy the specifications of sheet resistance, haze ratio, and transmittance.
  • the diffraction peak intensity on the (301) plane is larger than the diffraction peak intensity on any crystal plane other than the (301) plane.
  • the large peak from the (301) plane suggests that even crystal grains that have sufficiently incorporated fluorine have high crystallinity, and the transparent conductive film that satisfies the specifications of low resistance, light transmittance, and haze ratio It becomes.
  • the average particle diameter of the crystal grains calculated from the half-value width of the diffraction peak intensity of the (301) plane is the diffraction peak of any crystal plane other than the (301) plane. It is preferably larger than the average particle diameter of the crystal grains calculated from the half width of the strength. This suggests that crystal grains sufficiently incorporating fluorine are growing dominantly, and means that the transparent conductive film satisfies the specifications of light transmittance and haze ratio with lower resistance. .
  • Example 1 In this example, first, as the film forming raw material solution 1, the concentration of tin chloride pentahydrate is 0.9 mol / L and the concentration of ammonium fluoride is 0.9 mol / L with respect to 200 mL of water. Dissolved in. Furthermore, 20 mL of 35% hydrochloric acid was mixed as a pH adjuster. On the other hand, a hot plate was used as the heating unit 8, and a transparent substrate 7 made of a glass substrate was set on the hot plate. Then, the temperature of the hot plate was set to 590 ° C., and the transparent substrate 7 was heated until the surface temperature of the transparent substrate 7 reached 513 ° C. The surface temperature of the transparent substrate 7 was measured with a K thermocouple.
  • the film-forming raw material solution 1 was sent to the nozzle head 4 by the liquid feed pump 2, and droplets were generated by a spray method in which the film-forming raw material solution 1 was compressed with high-pressure gas into droplets.
  • a compressed air spray having a flow rate of 200 L / min was flowed in the ejection direction.
  • the conveyance stage was conveyed at the speed
  • a transparent conductive film made of SnO 2 is formed on the glass substrate by spraying droplets of the film forming raw material solution on the glass substrate at a flow rate of 12 mL / min for 75 seconds from the nozzle head 4 toward the transparent substrate 7. Filmed. At this time, the time during which the transparent conductive film was formed on the glass substrate was 60 seconds.
  • Example 2 comparative example 2
  • Example 2 and Example 2 were performed in the same manner as in Example 1 except that the film formation rate was changed by changing the supply rate of the film formation raw material solution.
  • the transparent conductive film of Comparative Example 2 was formed.
  • Example 3 Comparative Example 1
  • Example 3 Comparative Example 1
  • the film formation raw material solution supply rate and the film formation rate were changed, and the film formation stage was kept stationary to form a film for 60 seconds.
  • the transparent conductive films of Example 3 and Comparative Example 1 were formed by the same method as in Example 1.
  • Example 4 With respect to Example 3, as shown in Table 1 below, film formation was performed for 60 seconds by changing the substrate temperature, the film formation raw material solution supply rate, and the film formation rate. Except for these differences, the transparent conductive film of Example 4 was formed by the same method as in Example 3.
  • Comparative Example 3 As shown in Table 1 below, the transparent conductive film of Comparative Example 3 was formed by the same method as Example 1 except that the temperature of the transparent substrate during film formation was changed as shown in Table 1 below. did.
  • Comparative Example 4 Compared to Example 3, as shown in Table 1 below, the transparent conductive film of Comparative Example 4 was formed by the same method as Example 3 except that the temperature of the transparent substrate during film formation was changed. did.
  • the haze ratio (%) and the transmittance (%) of the transparent conductive film prepared in each example and each comparative example were measured with a spectral haze meter (product name: TC-1800H (manufactured by Tokyo Denshoku Co., Ltd.)). .
  • the measurement results are shown in Table 1 below.
  • FIG. 2 is an X-ray diffraction profile when the crystal structure analysis of the transparent conductive film of each example and comparative example is performed. Based on the X-ray diffraction profile shown in FIG. 2, the position of each peak (2 ⁇ B ), the intensity and the full width at half maximum (FWHM), and the crystal grain size t were calculated. The results are shown in Table 2.
  • the crystal grain size t means the crystal size in the film thickness direction, and was calculated based on the following Scherrer equation (1).
  • the (301) plane is the preferential orientation plane.
  • the transparent conductive film of the comparative example has a (200) plane as a preferential orientation plane.
  • the transparent conductive film of each example has a maximum crystal grain size of (301) -oriented crystals, while in Comparative Example 1 ( 200) A plane-oriented crystal has the largest crystal grain size in the film.
  • the transparent conductive films of Examples 1 to 3 have the properties of high haze and transmittance and low sheet resistance.
  • the transparent conductive film of Comparative Example 1 has the properties of high transmittance but low haze ratio and high sheet resistance.
  • a transparent conductive film having a high haze ratio and transmittance and a low sheet resistance can be formed by forming a transparent conductive film at a deposition rate of 12 nm / s or more. became.
  • the reason for this is thought to be that the re-evaporation of fluorine is suppressed by forming the film at a high film formation rate, and the transparent conductive film oriented in the (301) plane is preferentially formed.
  • the transparent conductive film formed by the film forming method of the present invention forms a transparent conductive film having a high light transmittance and a high haze ratio and a low sheet resistance without forming a buffer layer and an underlayer. be able to. For this reason, the transparent conductive film of this invention can be used conveniently as a transparent electrode for thin film solar cells, especially a thin film silicon solar cell.

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  • Computer Hardware Design (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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Abstract

La présente invention concerne un procédé simple de formation d'une pellicule conductrice transparente, ladite pellicule conductrice transparente ayant des caractéristiques excellentes, à savoir une transmissivité de la lumière élevée, une intensité de brouillard élevée, et une faible résistance de couche. Ce procédé de formation d'une pellicule conductrice transparente est caractérisé en ce qu'il comprend une étape de chauffage d'un substrat transparent (7) à 510 °C ou plus, et une étape de formation d'une pellicule conductrice transparente sur le substrat transparent (7) par pulvérisation de gouttelettes liquides (5) de la solution de matière première filmogène (1) sur le substrat transparent (7), et en ce que dans l'étape de formation de la pellicule conductrice transparente, la pellicule conductrice transparente est formée à une vitesse filmogène de 12 nm/sec ou plus.
PCT/JP2011/069550 2011-04-25 2011-08-30 Pellicule conductrice transparente et procédé de formation associé WO2012147219A1 (fr)

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JP2011097068A JP5073843B1 (ja) 2011-04-25 2011-04-25 透明導電膜の成膜方法

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
JP2020080275A (ja) * 2018-11-14 2020-05-28 トヨタ自動車株式会社 燃料電池用セパレータの製造方法

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JP7280751B2 (ja) * 2019-06-05 2023-05-24 東芝三菱電機産業システム株式会社 成膜方法

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Publication number Priority date Publication date Assignee Title
JPS5945926A (ja) * 1982-09-08 1984-03-15 Nippon Sheet Glass Co Ltd 基体に酸化錫膜を形成する方法
JP2000044238A (ja) * 1998-07-22 2000-02-15 Matsushita Battery Industrial Co Ltd 二酸化錫膜の製造方法および太陽電池
JP2002146536A (ja) * 2000-11-08 2002-05-22 Japan Science & Technology Corp 酸化スズ薄膜の低温形成方法
JP2007290958A (ja) * 2006-03-31 2007-11-08 Dainippon Printing Co Ltd 金属酸化物膜の製造方法

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Publication number Priority date Publication date Assignee Title
JPS5945926A (ja) * 1982-09-08 1984-03-15 Nippon Sheet Glass Co Ltd 基体に酸化錫膜を形成する方法
JP2000044238A (ja) * 1998-07-22 2000-02-15 Matsushita Battery Industrial Co Ltd 二酸化錫膜の製造方法および太陽電池
JP2002146536A (ja) * 2000-11-08 2002-05-22 Japan Science & Technology Corp 酸化スズ薄膜の低温形成方法
JP2007290958A (ja) * 2006-03-31 2007-11-08 Dainippon Printing Co Ltd 金属酸化物膜の製造方法

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2020080275A (ja) * 2018-11-14 2020-05-28 トヨタ自動車株式会社 燃料電池用セパレータの製造方法
JP7031564B2 (ja) 2018-11-14 2022-03-08 トヨタ自動車株式会社 燃料電池用セパレータの製造方法

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