WO2022254617A1 - Appareil de réaction d'oxydoréduction - Google Patents

Appareil de réaction d'oxydoréduction Download PDF

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Publication number
WO2022254617A1
WO2022254617A1 PCT/JP2021/021034 JP2021021034W WO2022254617A1 WO 2022254617 A1 WO2022254617 A1 WO 2022254617A1 JP 2021021034 W JP2021021034 W JP 2021021034W WO 2022254617 A1 WO2022254617 A1 WO 2022254617A1
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semiconductor photoelectrode
light
photovoltaic element
oxidation
semiconductor
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PCT/JP2021/021034
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English (en)
Japanese (ja)
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裕也 渦巻
紗弓 里
晃洋 鴻野
武志 小松
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日本電信電話株式会社
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Priority to PCT/JP2021/021034 priority Critical patent/WO2022254617A1/fr
Priority to JP2023525247A priority patent/JPWO2022254617A1/ja
Publication of WO2022254617A1 publication Critical patent/WO2022254617A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C25B11/067—Inorganic compound e.g. ITO, silica or titania
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • 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
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the present invention relates to an oxidation-reduction reactor.
  • oxidation-reduction reaction devices are known that allow oxidation-reduction reactions to proceed in an aqueous solution to cause water decomposition reactions.
  • a conventional oxidation-reduction reaction device is generally configured by combining a semiconductor photoelectrode and a photovoltaic device.
  • the decomposition reaction of water by the semiconductor photoelectrode consists of the oxidation reaction of water and the reduction reaction of protons.
  • the photocatalyst material constituting the semiconductor photoelectrode is irradiated with light, holes (h + ) and electrons (e ⁇ ) are generated and separated in the photocatalyst material.
  • the holes move to the surface of the semiconductor photoelectrode and contribute to the water oxidation reaction as shown in equation (1).
  • the electrons move to the reduction electrode inserted in the same aqueous solution as the semiconductor photoelectrode via the conducting wire, and contribute to the reduction reaction of protons (H + ) as shown in Equation (2).
  • the photovoltaic element is placed on the back side of the light-receiving surface of the semiconductor photoelectrode, and is connected to the conducting wire that connects the semiconductor photoelectrode and the reduction electrode.
  • a photovoltaic element receives light transmitted through a semiconductor photoelectrode to generate holes and electrons, which are supplied to a semiconductor photoelectrode and a reduction electrode, respectively.
  • the photovoltaic element generates electricity from the received light, raises the pressure between the semiconductor photoelectrode and the reduction electrode, increases the electromotive force of the oxidation-reduction reaction system, and improves the efficiency of the oxidation-reduction reaction.
  • the present invention has been made in view of the above circumstances, and an object of the present invention is to provide a technology capable of suppressing deterioration of a semiconductor photoelectrode and driving an oxidation-reduction reaction using light energy for a long time. be.
  • An oxidation-reduction reaction apparatus includes a semiconductor photoelectrode that causes an oxidation reaction with an aqueous solution by light, and a reduction electrode that causes a reduction reaction with an aqueous solution or gas by means of electrons transferred from the semiconductor photoelectrode through a lead wire. and a photovoltaic element arranged on the back side of the light receiving surface of the semiconductor photoelectrode, connected to the conducting wire, and generating electricity by light transmitted through the semiconductor photoelectrode, and between the semiconductor photoelectrode and the photovoltaic element. and a cut filter that cuts out a predetermined wavelength range of light that reaches the photovoltaic element after passing through the semiconductor photoelectrode, or weakens the intensity of the light.
  • the present invention it is possible to provide a technology that suppresses the deterioration of the semiconductor photoelectrode and can drive the oxidation-reduction reaction using light energy for a long time.
  • FIG. 1 is a diagram showing the configuration of an oxidation-reduction reaction system.
  • a cut filter is provided on the optical path between the semiconductor photoelectrode and the photovoltaic element to remove a predetermined wavelength range of the light transmitted through the semiconductor photoelectrode or reduce the intensity of the light.
  • the photocurrent generated from the photovoltaic element is controlled to be the same as the photocurrent generated from the semiconductor photoelectrode.
  • the cut filter maximizes the efficiency of the water decomposition reaction by combining the semiconductor photoelectrode and the photovoltaic element, and makes the number of holes generated in the photovoltaic element approximately equal to the number of electrons generated in the semiconductor photoelectrode. to control.
  • the heat generation and deterioration of the semiconductor photoelectrode can be suppressed, the water decomposition reaction by oxidation-reduction using light energy can be driven for a long time, and the life of the oxidation-reduction reaction device can be extended.
  • the water decomposition reaction is an example of the target reaction.
  • the present invention can be applied to reactions other than the water decomposition reaction, that is, target products other than hydrogen. That is, the present invention can be applied to any oxidation-reduction reaction apparatus that advances an oxidation-reduction reaction.
  • FIG. 1 is a diagram showing the configuration of an oxidation-reduction reaction system according to this embodiment.
  • the oxidation-reduction reaction system includes an oxidation-reduction reaction device 1 and a light source 2.
  • the light source 2 is, for example, a xenon lamp, a mercury lamp, a halogen lamp, a pseudo-sunlight source, sunlight, or a light source combining these.
  • the oxidation-reduction reaction device 1 includes a tank 11, an aqueous solution 12, a semiconductor photoelectrode 13, a reduction electrode 14, a photovoltaic element 15, a cut filter 16, and a lead wire 17.
  • the aqueous solution 12 is, for example, an aqueous sodium hydroxide solution, an aqueous potassium hydroxide solution, an aqueous sodium chloride solution, an aqueous potassium chloride solution, and hydrochloric acid.
  • the semiconductor photoelectrode 13 is, for example, gallium nitride or a nitride semiconductor. Metal oxides, such as titanium oxide, tungsten oxide, and gallium oxide, and compound semiconductors, such as cadmium sulfide, having a photocatalytic function may also be used.
  • the semiconductor photoelectrode 13 is inserted into the aqueous solution 12 in the bath 11 and connected to the reduction electrode 14 in the same aqueous solution 12 through the photovoltaic element 15 and the lead wire 17 .
  • the semiconductor photoelectrode 13 generates and separates holes and electrons in the photocatalyst material when the photocatalyst material constituting itself is irradiated with light from the light source 2 .
  • the holes move to the surface of the semiconductor photoelectrode 13 and proceed with the oxidation reaction of water on the surface. Therefore, the semiconductor photoelectrode 13 functions as an oxidation electrode. On the other hand, electrons move to the reduction electrode 14 via the photovoltaic element 15 and the conducting wire 17 .
  • the reduction electrode 14 is a metal or metal compound, such as nickel, iron, gold, platinum, silver, copper, indium, or titanium.
  • the shape of the reduction electrode 14 is, for example, a wire, a plate, a wire mesh, or an electrode substrate in which metal particles are applied on a conductive substrate. Electrons transferred from the semiconductor photoelectrode 13 via the photovoltaic element 15 and the conducting wire 17 cause the reduction reaction of protons to proceed on the surface of the reduction electrode 14 . This produces the desired product, hydrogen.
  • the photovoltaic element 15 is, for example, a silicon-based element, a copper indium gallium selenide-based element, a III-V group-based element, a cadmium telluride-based element, a dye-sensitized element, or an organic semiconductor-based element.
  • the photovoltaic element 15 is arranged on the back side of the light receiving surface of the semiconductor photoelectrode 13 and further on the back side of the cut filter 16 and connected to the conducting wire 17 .
  • the photovoltaic element 15 receives light transmitted through the semiconductor photoelectrode 13 and the cut filter 16 to generate holes and electrons, which are supplied to the semiconductor photoelectrode 13 and the reduction electrode 14, respectively.
  • the photovoltaic element 15 generates electricity with the received light, raises the pressure between the semiconductor photoelectrode 13 and the reduction electrode 14, increases the electromotive force of the oxidation-reduction reaction system, and improves the efficiency of the oxidation-reduction reaction.
  • the cut filter 16 is, for example, a removal filter that removes a predetermined wavelength band, or a neutral density filter that uniformly attenuates the light intensity. A commercially available filter may be used.
  • the cut filter 16 is arranged on the optical path between the semiconductor photoelectrode 13 and the photovoltaic element 15, and cuts out a predetermined wavelength range of the light that reaches the photovoltaic element 15 after passing through the semiconductor photoelectrode 13, or cuts off the light. reduce strength.
  • the cut filter 16 is such that the current value (the number of holes generated in the photovoltaic element) generated in the photovoltaic element 15 by the light transmitted through the semiconductor photoelectrode 13 and itself is equal to the current generated in the semiconductor photoelectrode 13 by the light from the light source 2 .
  • a predetermined wavelength range of the light that passes through the semiconductor photoelectrode 13 and reaches the photovoltaic element 15 is removed or the intensity of the light is weakened so that it becomes the same as the value (the number of electrons generated in the semiconductor photoelectrode).
  • the redox reactor 1 is also applicable to target products other than hydrogen.
  • the type of metal for example, Ni, Fe, Au, Pt, Ag, Cu, In, Ti, Co, Ru
  • each of the semiconductor photoelectrode 13 and the reduction electrode 14 is changed.
  • the reduction reaction of carbon dioxide produces a carbon compound
  • the reduction reaction of nitrogen Ammonia can also be produced by
  • n-GaN semiconductor thin film was epitaxially grown on a GaN substrate by metal organic chemical vapor deposition (MOCVD).
  • MOCVD metal organic chemical vapor deposition
  • the film thickness of n-GaN was set to 2 ⁇ m.
  • Carrier density was 3 ⁇ 10 18 cm ⁇ 3 .
  • InGaN with a composition ratio of indium (In) of 5% was grown.
  • the film thickness of InGaN was set to 100 nm, which is sufficient for light absorption.
  • Ni with a film thickness of about 1 nm was vacuum-deposited on the surface of InGaN.
  • NiO was formed by heat-treating this semiconductor thin film in air at 300° C. for 1 hour. Observing the cross section of NiO with a transmission electron microscope (TEM), the film thickness was 2 nm. Measurements of the optical transmittance of NiO revealed that it absorbs light of about 400 nm or less in sunlight.
  • TEM transmission electron microscope
  • the photovoltaic element 15 can absorb light up to about 1100 nm out of light of about 400 nm or more transmitted through the semiconductor photoelectrode 13 , and the current generated by itself is larger than the current generated by the semiconductor photoelectrode 13 .
  • the short-circuit current of the single photovoltaic element 15 was about 10 mA.
  • the respective electromotive forces were 0.6 V for the photovoltaic element 15 and 1.2 V for the semiconductor photoelectrode 13 .
  • a cut filter 16 for cutting light in the wavelength range of 960 nm or less was installed on the optical path between the photovoltaic element 15 and the semiconductor photoelectrode 13.
  • a long wavelength cut filter such as SIX960 may be used.
  • the cut filter 16 the photocurrent value generated from the photovoltaic element 15 is reduced from the previously measured photocurrent value between the semiconductor photoelectrode 13 and the reduction electrode 14 (1.0 mA (when 0.6 V is applied)). equated with
  • Nitrogen gas was flowed into the vessel 11 at 10 ml/min, the light-receiving area of the semiconductor photoelectrode 13 was set to 1 cm 2 , and the aqueous solution 12 was stirred at the center position of the vessel bottom at a rotational speed of 250 rpm using a stirrer and stirrer.
  • the light source 2 was fixed so as to face the NiO formation surface of the semiconductor photoelectrode 13 produced by the above procedure.
  • a high pressure xenon lamp of 300 W was used as the light source 2 to uniformly irradiate the semiconductor photoelectrode 13 and the photovoltaic element 15 with light. 10 hours, 50 hours, 100 hours, 200 hours and 300 hours after the light irradiation, the gas in the tank 11 was sampled and the reaction product was analyzed by gas chromatography. As a result, it was confirmed that oxygen and hydrogen were produced.
  • Example 2 [Production of semiconductor photoelectrode] A semiconductor thin film of n-GaN was epitaxially grown on a GaN substrate by the MOCVD method. The film thickness of n-GaN was set to 2 ⁇ m. Carrier density was 3 ⁇ 10 18 cm ⁇ 3 . Thereafter, a Ta 3 N 5 thin film was formed by sputtering metal tantalum or tantalum oxide and nitriding the film. The film thickness of Ta 3 N 5 was set to 500 nm, which is sufficient for light absorption. Ni with a film thickness of about 1 nm was vacuum-deposited on the surface of Ta 3 N 5 . NiO was formed by heat-treating this semiconductor thin film in air at 300° C. for 1 hour. Observing the cross section of NiO with a TEM, the film thickness was 2 nm. Measurements of the optical transmittance of NiO showed that it absorbs light below about 600 nm in sunlight.
  • the photovoltaic element 15 can absorb light up to about 1100 nm out of light of about 600 nm or more transmitted through the semiconductor photoelectrode 13 , and the current generated by itself is larger than the current generated by the semiconductor photoelectrode 13 .
  • the short-circuit current of the single photovoltaic element 15 was about 10 mA.
  • the respective electromotive forces were 0.6 V for the photovoltaic element 15 and 0.8 V for the semiconductor photoelectrode 13 .
  • Two photovoltaic elements 15 were connected in series between the semiconductor photoelectrode 13 and the reduction electrode 14 .
  • a cut filter 16 for cutting light in the wavelength range of 840 nm or less was installed on the optical path between the photovoltaic element 15 and the semiconductor photoelectrode 13.
  • a long wavelength cut filter such as SIX840 may be used.
  • Example 1 for comparison In Comparative Example 1, the photovoltaic element 15 and the cut filter 16 were not used. After that, the procedure was the same as in Example 1.
  • Example 3 for comparison
  • the cut filter 16 was used to reduce the photocurrent value generated from the photovoltaic element 15 from the previously measured photocurrent value (1.0 mA) between the semiconductor photoelectrode 13 and the reduction electrode 14. was controlled to 0.5mA so that After that, the procedure was the same as in Example 1.
  • Example 4 for comparison In Comparative Example 4, the photovoltaic element 15 and the cut filter 16 were not used. After that, the procedure was the same as in Example 2.
  • Example 6 for comparison In Comparative Example 6, the cut filter 16 was used to reduce the photocurrent value generated from the photovoltaic element 15 from the previously measured photocurrent value (2.0 mA) between the semiconductor photoelectrode 13 and the reduction electrode 14. was controlled to 1.0 mA so that After that, the procedure was the same as in Example 2.
  • Table 1 shows the amount of oxygen/hydrogen gas generated with respect to the light irradiation time in the examples and comparative examples.
  • the amount of each gas produced is shown normalized by the surface area of the semiconductor photoelectrode 13 . In every example, it was found that oxygen and hydrogen were generated during light irradiation.
  • Example 1 when comparing Example 1 with Comparative Examples 1 and 3, the amount of gas generated in Comparative Example 3 is different from that in Example 1, although the photovoltaic element 15 is combined in the same manner as in Example 1. It was different and comparable to Comparative Example 1. This is because the amount of current generated from the photovoltaic element 15 is reduced by the cut filter 16 compared to the amount of current generated from the semiconductor photoelectrode 13. Therefore, in Comparative Example 3, the efficiency of the oxidation-reduction reaction is improved by the photovoltaic element 15. was not expressed.
  • Example 1 when comparing Example 1 and Comparative Example 2, there was no difference in the amount of gas generated 10 hours after light irradiation.
  • Comparative Example 2 the amount of hydrogen produced gradually decreased after 10 hours, and after 100 hours, almost deactivated. Oxygen production was almost deactivated after 100 hours.
  • Comparative Example 2 the production ratio of hydrogen and oxygen after 50 hours and 100 hours of light irradiation was not 2:1. It is considered that this is because, on the surface of the semiconductor photoelectrode 13, not the oxidation reaction of water but the degradation reaction of the semiconductor is proceeding simultaneously.
  • Example 2 when comparing Example 2 with Comparative Examples 4 and 5, it was found that the combination of the photovoltaic element 15 significantly improved the amount of gas generated.
  • a semiconductor such as Ta 3 N 5 that has a narrow bandgap and does not straddle the water oxidation reaction level and the hydrogen generation level is used for the semiconductor photoelectrode 13 , the desired reaction does not occur unless the photovoltaic element 15 is combined to boost the voltage.
  • Example 2 when comparing Example 2 and Comparative Example 6, the amount of gas generated up to 200 hours later in Comparative Example 6 was the same as in Example 2, although the photovoltaic element 15 was combined. It was about 1/2 of 2. This is because the amount of current generated from the photovoltaic element 15 is reduced by the cut filter 16 as compared with that generated from the photoelectrode, so that in comparative example 6, the effect of improving the efficiency of the oxidation-reduction reaction by the photovoltaic element 15 is exhibited. presumably not.
  • Example 2 when comparing Example 2 and Comparative Example 5, there was no difference in the amount of gas generated 10 hours after light irradiation.
  • Example 2 although the same properties could be maintained even after 200 hours, in Comparative Example 5, the activity was almost lost after 100 hours.
  • the production ratio of hydrogen and oxygen after 50 hours of light irradiation in Comparative Example 5 was not 2:1. It is considered that this is because, on the surface of the semiconductor photoelectrode 13, not the oxidation reaction of water but the degradation reaction of the semiconductor is proceeding simultaneously.
  • the cut filter 16 As described above, by combining the cut filter 16 with the combination of the semiconductor photoelectrode 13 and the photovoltaic element 15, the amount of hydrogen and oxygen generated by the water decomposition reaction (light energy conversion efficiency) can be extended.
  • the photocurrent generated from the photovoltaic element 15 can be controlled to be the same as the photocurrent generated from the semiconductor photoelectrode 13 .
  • the heat generation and deterioration of the semiconductor photoelectrode 13 can be suppressed, the water decomposition reaction by oxidation-reduction using light energy can be driven for a long time, and the life of the oxidation-reduction reaction device can be extended.
  • redox reaction device 11 tank 12: aqueous solution 13: semiconductor photoelectrode 14: reduction electrode 15: photovoltaic element 16: cut filter 17: conducting wire 2: light source

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Abstract

Un appareil de réaction d'oxydoréduction (1) comprend : une photoélectrode à semi-conducteur (13) qui entraîne la progression d'une réaction oxydative avec une solution aqueuse au moyen d'une lumière ; une électrode de réduction (14) qui entraîne la progression d'une réaction réductrice avec un gaz ou une solution aqueuse au moyen d'électrons qui ont été transférés à partir de la photoélectrode semi-conductrice par l'intermédiaire d'un fil conducteur ; un élément photovoltaïque (15) qui est situé sur le côté arrière de la surface de réception de lumière de la photoélectrode à semi-conducteur, qui est connectée au fil de connexion, et qui génère de l'électricité au moyen de la lumière qui a traversé la photoélectrode à semi-conducteur ; et un filtre de coupure (16) qui est situé sur un trajet optique entre la photoélectrode à semi-conducteur et l'élément photovoltaïque, et qui élimine une bande de longueur d'onde prédéterminée de la lumière qui a traversé la photoélectrode à semi-conducteur et atteint l'élément photovoltaïque ou réduit l'intensité de ladite lumière.
PCT/JP2021/021034 2021-06-02 2021-06-02 Appareil de réaction d'oxydoréduction WO2022254617A1 (fr)

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PCT/JP2021/021034 WO2022254617A1 (fr) 2021-06-02 2021-06-02 Appareil de réaction d'oxydoréduction
JP2023525247A JPWO2022254617A1 (fr) 2021-06-02 2021-06-02

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10290017A (ja) * 1997-04-14 1998-10-27 Mitsubishi Heavy Ind Ltd 光触媒
JP2003504799A (ja) * 1999-07-05 2003-02-04 エコル ポリテクニク フェデラル ドゥ ローザンヌ （エペエフエル） 可視光による水開裂用のタンデム電池
JP2007525593A (ja) * 2003-06-27 2007-09-06 ゼネラル・モーターズ・コーポレーション 光電気化学装置及び電極
JP2019059996A (ja) * 2017-09-27 2019-04-18 株式会社豊田中央研究所 人工光合成セル

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10290017A (ja) * 1997-04-14 1998-10-27 Mitsubishi Heavy Ind Ltd 光触媒
JP2003504799A (ja) * 1999-07-05 2003-02-04 エコル ポリテクニク フェデラル ドゥ ローザンヌ （エペエフエル） 可視光による水開裂用のタンデム電池
JP2007525593A (ja) * 2003-06-27 2007-09-06 ゼネラル・モーターズ・コーポレーション 光電気化学装置及び電極
JP2019059996A (ja) * 2017-09-27 2019-04-18 株式会社豊田中央研究所 人工光合成セル

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