WO2007052512A1 - 光による水分解触媒及びその製造方法。 - Google Patents

光による水分解触媒及びその製造方法。 Download PDF

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WO2007052512A1
WO2007052512A1 PCT/JP2006/321254 JP2006321254W WO2007052512A1 WO 2007052512 A1 WO2007052512 A1 WO 2007052512A1 JP 2006321254 W JP2006321254 W JP 2006321254W WO 2007052512 A1 WO2007052512 A1 WO 2007052512A1
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water
gallium nitride
type gallium
oxide
catalyst
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PCT/JP2006/321254
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English (en)
French (fr)
Japanese (ja)
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Yasunobu Inoue
Nobuo Saito
Hiroshi Nishiyama
Naoki Arai
Kazunari Domen
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National University Corporation Nagaoka University Of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/825—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with gallium, indium or thallium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/0203—Preparation of oxygen from inorganic compounds
    • C01B13/0207—Water
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
    • C01B3/042—Decomposition of water
    • 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

  • a water splitting catalyst by light and a method for producing the same are identical to A water splitting catalyst by light and a method for producing the same.
  • the present invention relates to a catalyst for water splitting utilizing light energy using p-type gallium nitrides.
  • a solid catalyst is irradiated with light to reduce the reactant with electrons generated in the conduction band, and a reaction with holes generated in the valence band.
  • Techniques for oxidizing products to obtain products are known.
  • Non-Patent Literature l Catal. Lett., 58 (1999), 153-155
  • Non-Patent Document 2 J. AM. CHEM. SOC. (2005), 127, 4150-4151
  • Non-Patent Document 3 J. AM. CHEM. SOC. (2005), 127, 8286-8287
  • Patent Document 1 Japanese Patent Laid-Open No. 2005-131531
  • Patent Document 2 Japanese Patent Laid-Open No. 2003-24764
  • Non-patent document 1 discloses a catalyst that decomposes water into hydrogen and oxygen, and in particular, an alkali or alkalinity metal oxide containing tantalum has a high catalyst for complete decomposition of water. It is described to show activity.
  • Patent Document 1 and Non-Patent Document 2 describe the hydrolytic catalytic action of nitrides and oxynitrides containing germanium elements having a d 1G electronic state.
  • Non-Patent Document 3 describes the use of a solid solution of gallium nitride and zinc oxide in the design of a visible light active water splitting catalyst. This document discloses that this solid solution of gallium nitride and zinc oxide functions as a catalyst for complete water decomposition, but gallium nitride alone has no water decomposition activity.
  • Patent Document 2 describes a gas generation method by light irradiation of a nitride semiconductor. It is disclosed that the source of this is a nitride surface or a bonded metal surface.
  • gallium nitride functions as a catalyst for generating hydrogen and oxygen from water.
  • this catalyst generates a large amount of nitrogen rather than a stoichiometric hydrogen and oxygen generator. This phenomenon is caused by the decomposition of gallium nitride. Therefore, it is difficult to obtain hydrogen from water stably for a long period of time with the technique described in this patent document.
  • an object of the present invention is to provide a catalyst for complete decomposition of water that can stably decompose water into hydrogen and oxygen by light irradiation for a long period of time and a method for producing the same.
  • the present inventors have discovered that the above problem can be solved by supporting a co-catalyst such as ruthenium oxide on p-type gallium nitride added with different metal atoms, and completed the present invention. .
  • the present invention employs the following configurations 1 to 14.
  • the average particle size of p-type gallium nitride added with metal atoms with selected zinc, magnesium, and beryllium strength is ⁇ !
  • a compound selected from zinc nitrate, magnesium nitrate and beryllium nitrate and gallium nitrate are dissolved in water, and the product obtained by adding ammonia water is calcined in air at 600-800 ° C.
  • the p-type gallium nitride obtained by firing the precursor in an ammonia stream is immersed in water or an organic solvent solution containing the promoter precursor and then fired in air.
  • the method for producing a water-splitting catalyst by light according to any one of 1 to 6, wherein: 12.
  • the water according to 11 or 12, wherein the p-type gallium indium nitride obtained by firing for 24 hours is immersed in water or an organic solvent solution containing a promoter precursor and then fired in air.
  • the present invention by using a water splitting catalyst supporting the promoter having the above-described configuration, water can be decomposed into hydrogen and oxygen with high efficiency by light irradiation stably for a long period of time. It became.
  • the present invention opens the way for producing clean energy sources without using any fossil fuels.
  • the present invention provides a catalyst applicable to the photodecomposition reaction and the photosynthesis reaction of environmental pollutants contained in oil, exhaust gas, etc., and has extremely high practical value.
  • FIG. 1 is a diagram showing the water splitting activity of the ruthenium oxide-supported zinc-added gallium nitride obtained in Example 1.
  • FIG. 2 is a view showing the water decomposing activity of the ruthenium oxide-supported magnesium-added gallium nitride obtained in Example 2.
  • FIG. 3 is a view showing the water decomposing activity of the ruthenium oxide-supported magnesium-added gallium nitride obtained in Example 3.
  • FIG. 4 is a view showing the water splitting activity of the ruthenium oxide-supported beryllium-added gallium nitride obtained in Example 4.
  • FIG. 5 is a diagram showing the water splitting activity of gallium nitride obtained in each example of the present invention.
  • FIG. 6 is a diagram showing an X-ray diffraction pattern of gallium nitride obtained in each example of the present invention.
  • FIG. 7 is a diagram showing an ultraviolet-visible diffuse reflection spectrum of gallium nitride obtained in each example of the present invention.
  • FIG. 8 is a diagram showing an emission spectrum of gallium nitride obtained in each example of the present invention.
  • FIG. 9 is a graph showing the hydrolytic activity of the ruthenium oxide-supported zinc-doped gallium indium nitride obtained in Example 5.
  • ruthenium oxide, nickel oxide, cobalt oxide, iron oxide, chromium oxide, iridium oxide, iridium oxide are added to p-type gallium nitride to which metal atoms having selected zinc, magnesium, and beryllium power are added.
  • P-type gallium nitride doped with metal atoms with selected zinc, magnesium, and beryllium forces is commonly used in the semiconductor field as light-emitting diodes and laser diodes.
  • the use of the p-type gallium nitride as a catalyst for complete water decomposition by light has not been known so far.
  • the above-mentioned p-type gallium nitride containing different atoms is selected from ruthenium oxide, acid nickel, cobalt oxide, iron oxide, acid chromium, acid rhodium, and iridium oxide force.
  • the above-mentioned p-type gallium nitride containing different atoms means that a metal atom selected from zinc, magnesium, and beryllium is added to gallium by a standard method.
  • 0001-7 was ⁇ Ka ⁇ so that mole 0/0 approximately, the chemical formula: in Ga N (However, 0 ⁇ x ⁇ 1) denote the p-type gallium nitride and the p-type gallium indium nitride represented by .
  • Such P-type gallium nitride has, for example, an average particle size of ⁇ ! It can be used as a powdery product of about ⁇ 10 / zm.
  • the p-type gallium nitride containing a hetero atom is preferably loaded with a promoter.
  • a promoter Selected from ruthenium oxide, acid nickel oxide, cobalt oxide, iron oxide, acid chromium chromium, acid sodium rhodium, iridium oxide so that the strength is about 0.1 to LO weight% based on 3 ⁇ 4 type gallium nitride
  • the promoter is ruthenium oxide.
  • the sample thus mixed is used as a precursor.
  • the product obtained by dropping ammonia water into an aqueous solution in which a compound selected from zinc nitrate, magnesium nitrate, and beryllium nitrate and gallium nitrate are dissolved in water is heated at a temperature of 600 to 800 ° C in air.
  • a calcined sample can also be used as a precursor.
  • a precursor sample is introduced into the center of a nitriding apparatus having a rotation mechanism, for example, a quartz furnace core tube having a length of 50 cm and an inner diameter of 2 to 3 cm. Then, both ends of the precursor are fixed with quartz wool, and nitrogen gas is sufficiently circulated from the high purity nitrogen cylinder (purity 99.99% or more) to the quartz core. By using a rotary kiln furnace equipped with a rotating mechanism, homogeneous nitrides can be produced.
  • ammonia gas is circulated in an amount of 50 to 1000 mLZ from an ammonia cylinder (purity 99.8% or more) to the quartz core. At this time, the flow rate of ammonia is controlled by a mass flow controller.
  • the quartz furnace tube is rotated at a speed of 0.5 to 1 revolution per minute, and the vicinity of the sample is heated to a temperature of 700 to 1100 ° C by a horizontal tube furnace.
  • the characteristics of the obtained gallium nitride are measured by an X-ray diffraction pattern, an ultraviolet-visible diffuse reflection spectrum, and an emission spectrum.
  • a mixture obtained by adding 1 to 50 mol% indium sulfide to the p-type gallium nitride thus obtained is heated at a temperature of 500 to 900 ° C under an ammonia stream.
  • P-type gallium indium nitride can be produced by firing for 5 to 24 hours.
  • the obtained p-type gallium nitride or p-type gallium indium nitride is immersed in, for example, a solution in which triruthenium dodecacarbonyl serving as a promoter precursor is dissolved in tetrahydrofuran. Next, it is refluxed at room temperature to 100 ° C for 1 to 5 hours, and further in air at 200 to 500 ° C. By calcination for 1 to 10 hours, a target water decomposition catalyst by light is obtained.
  • nickel nitrate, cobalt chloride, iron chloride, chromium nitrate, rhodium chloride, iridium chloride, etc. can be used, and these precursors should be about 1 to about LO weight%.
  • P-type gallium nitrides may be immersed in a solution dissolved in water or an organic solvent.
  • Powdered gallium sulfide was introduced into the center of a nitriding device consisting of a quartz furnace core tube with a rotation mechanism and a length of 50 cm and an inner diameter of 2 to 3 cm.
  • nitrogen gas was sufficiently circulated from the high purity nitrogen cylinder (purity 99.99% or more) to the quartz core.
  • ammonia gas was introduced into the quartz core from an ammonia cylinder (purity: 99.8% or more), and nitriding was performed by baking at 1000 ° C for 15 hours in an ammonia stream of 500 mLZ. Thereby, additive-free gallium nitride was obtained.
  • Figures 6, 7, and 8 show the X-ray diffraction pattern, ultraviolet-visible diffuse reflection spectrum, and emission spectrum of gallium nitride without the addition of different metal atoms, respectively. From these figures, it can be seen that high-quality gallium nitride having an emission center at a high crystallinity of 373 nm is generated.
  • Powdery gallium sulphate and zinc sulphate zinc with a molar ratio of 200% zinc to gallium
  • the mixture was baked at 1000 ° C for 8 hours in an ammonia stream of 500 mLZ for nitriding.
  • Most of the zinc components were volatilized during firing, and gallium nitride with zinc added at a concentration of several to several tens of ppm was obtained.
  • Figures 6, 7, and 8 show the XRD pattern, ultraviolet-visible diffuse reflectance spectrum, and emission spectrum of p-type gallium nitride doped with zinc.
  • Zinc-doped gallium nitride has almost the same degree of crystallinity as gallium nitride without addition, but the absorption wavelength has shifted slightly to a longer wavelength, and the emission center has shifted to a longer wavelength of 440 nm. In this way, gallium nitride with an emission spectrum specific to p-type was produced.
  • This p-type gallium nitride was loaded with ruthenium oxide in the same manner as in Reference Example 1 and irradiated with light in the same manner as in Reference Example 1. The results are shown in Fig. 1. As can be seen in Figure 1, hydrogen 208 ⁇ molZ time, oxygen 88 ⁇ molZ time, and nitrogen 4 ⁇ molZ time were observed, and it was found to have high photocatalytic activity for water splitting reaction.
  • Example 1 For comparison, the zinc-added p-type gallium nitride obtained in Example 1 was irradiated with light in the same manner as in Reference Example 1 without supporting ruthenium oxide as a promoter. As a result, the production activity was 2 ⁇ molZ for hydrogen, 0 ⁇ molZ for oxygen, and 0 ⁇ molZ for nitrogen, and almost no activity for water splitting reaction was observed.
  • Powdery gallium sulphate and magnesium sulphate are mixed so that the molar ratio of magnesium element to gallium is 3%, and in the same manner as in Reference Example 1, in an ammonia stream of 500 mLZ at 1000 ° C. Nitrided by firing for 15 hours.
  • the obtained precursor was calcined at 1000 ° C. for 15 hours in an ammonia stream of 50 to: LOOOmLZ to obtain magnesium-added p-type gallium nitride.
  • Figures 6, 7, and 8 show the XRD pattern, UV-visible diffusion spectrum, and emission spectrum of gallium nitride with magnesium loading.
  • a p-type gallium nitride similar to the zinc-doped gallium nitride of Example 1 was obtained.
  • Example 2 For comparison, the magnesium-added p-type gallium nitride obtained in Example 2 was irradiated with light in the same manner as in Reference Example 1 without supporting ruthenium oxide as a promoter. As a result, the generation activity was 5 ⁇ molZ for hydrogen, 0 ⁇ molZ for oxygen, and 0 ⁇ molZ for nitrogen, and almost no activity for water splitting was observed.
  • the product obtained by dissolving gallium nitrate and magnesium nitrate in water at the same molar ratio as in Example 2 and dropwise adding ammonia water was baked in air at a temperature of 600 to 800 ° C. for 1 to 60 minutes.
  • the obtained precursor was calcined for 15 hours at 1000 ° C. in an ammonia stream of 50 to: LOOOmL Z in the same manner as in Reference Example 1 to obtain the same p-type as the magnesium-added gallium nitride of Example 2.
  • Gallium nitride was obtained.
  • This p-type gallium nitride was loaded with ruthenium oxide in the same manner as in Reference Example 1 and irradiated with light in the same manner as in Reference Example 1.
  • the results are shown in Fig. 3.
  • Fig. 3 As can be seen in Fig. 3, the generation activity of hydrogen at 341 ⁇ molZ time, oxygen at 173 ⁇ molZ time, and nitrogen at 0 ⁇ molZ time was observed, and it was found to have high photocatalytic activity for water complete decomposition reaction .
  • Example 3 For comparison, the magnesium-added p-type gallium nitride obtained in Example 3 was irradiated with light in the same manner as in Reference Example 1 without supporting ruthenium oxide as a promoter. As a result, the production activity was 4 ⁇ molZ for hydrogen, 0 ⁇ molZ for oxygen, and 0 ⁇ molZ for nitrogen, and almost no activity was observed for water splitting.
  • Powdery gallium sulphate and beryllium oxide are mixed so that the molar ratio of beryllium to gallium is 3%, and in the same manner as in Reference Example 1, in an ammonia stream of 500 mLZ at 1 000 ° C. Nitrided by firing for 15 hours.
  • Figures 6, 7, and 8 show the XRD pattern, UV-visible diffuse reflection spectrum, and emission spectrum of beryllium-doped gallium nitride. P-type gallium nitride similar to the zinc-added gallium nitride of Example 1 was obtained.
  • Example 4 For comparison, the beryllium-added p-type gallium nitride obtained in Example 4 was irradiated with light in the same manner as in Reference Example 1 without supporting ruthenium oxide as a promoter. The result was a production activity of 2 ⁇ molZ time for hydrogen, 0 ⁇ molZ time for oxygen, and 0 ⁇ molZ time for nitrogen, and almost no activity for water splitting reaction was observed.
  • Example 1 The zinc-added P-type gallium nitride obtained in Example 1 was mixed with indium sulfide at a molar ratio of 30% with respect to gallium, and 10% at 630 ° C in an ammonia stream of 500 mLZ in the same manner as in Reference Example 1. Nitrided by firing for a period of time. The obtained p-type gallium indium nitride was loaded with ruthenium oxide in the same manner as in Reference Example 1 above.
  • This ruthenium oxide-supported zinc-doped gallium indium nitride (0.8 g) was suspended in distilled water (lOOOOmL) and irradiated with light through a cylindrical Pyrex (registered trademark) jacket using a 200 W mercury xenon lamp as a light source. A cut filter capable of blocking light up to 420 nm was introduced between the light source and the suspension to irradiate the light. The results are shown in Fig. 9.
  • Example 2 For comparison, the indium obtained in Example 1 was added! /,!, And ruthenium oxide-supported zinc-added gallium nitride was used, and light was irradiated in the same manner as described above. As a result, when light was irradiated without using a force filter, activity of generating hydrogen 82 / z molZ time, oxygen molZ time, and nitrogen 0 molZ time was observed. On the other hand, when a cut filter was introduced to block light up to 420 nm, production activity of 2 ⁇ molZ time for hydrogen, 1 ⁇ molZ time for oxygen, and 0 molZtime for nitrogen was observed. (See Figure 9)
  • Indium gallium nitride Compared to zinc-doped gallium nitride supported on ruthenium oxide, zinc-supported ruthenium oxide Indium gallium nitride has higher catalytic activity when irradiated with light having a wavelength of 420 nm or more. Therefore, it has been found that adding indium absorbs light of longer wavelengths.
  • Example 5 the zinc-added p-type gallium indium nitride obtained in Example 5 was irradiated with light in the same manner as in Reference Example 1 without supporting ruthenium oxide as a promoter.
  • the production activity was 0 ⁇ molZ time for hydrogen, 0 ⁇ molZ time for oxygen, and 0 ⁇ molZ time for nitrogen, and no activity for water splitting reaction was observed.
  • the water-based water splitting catalyst of the present invention opens the way for producing a clean energy source without using any fossil fuel or the like. Further, the catalyst obtained by the present invention is not limited to the decomposition of water, but also the decomposition of organic substances such as ethanol and oil, the photodecomposition reaction of environmental pollutants contained in exhaust gas, and various photosynthesis reactions. It can be applied to a wide range of fields.

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PCT/JP2006/321254 2005-11-04 2006-10-25 光による水分解触媒及びその製造方法。 WO2007052512A1 (ja)

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