JP6173951B2 - 層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 - Google Patents
層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 Download PDFInfo
- Publication number
- JP6173951B2 JP6173951B2 JP2014048253A JP2014048253A JP6173951B2 JP 6173951 B2 JP6173951 B2 JP 6173951B2 JP 2014048253 A JP2014048253 A JP 2014048253A JP 2014048253 A JP2014048253 A JP 2014048253A JP 6173951 B2 JP6173951 B2 JP 6173951B2
- Authority
- JP
- Japan
- Prior art keywords
- layered
- iridium
- iridium oxide
- iridate
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002135 nanosheet Substances 0.000 title claims description 63
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 title claims description 59
- 229910000457 iridium oxide Inorganic materials 0.000 title claims description 58
- 239000002253 acid Substances 0.000 title claims description 31
- 229910052741 iridium Inorganic materials 0.000 title claims description 31
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims 3
- 239000000243 solution Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229910052700 potassium Inorganic materials 0.000 claims description 11
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 10
- 239000011591 potassium Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 239000003929 acidic solution Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000009830 intercalation Methods 0.000 claims description 2
- 230000002687 intercalation Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- 239000010410 layer Substances 0.000 description 11
- 239000000758 substrate Substances 0.000 description 9
- 239000008188 pellet Substances 0.000 description 8
- 238000005868 electrolysis reaction Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 6
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 6
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 5
- 150000001339 alkali metal compounds Chemical class 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 238000010304 firing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 150000003973 alkyl amines Chemical class 0.000 description 2
- 125000005210 alkyl ammonium group Chemical group 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000557 Nafion® Polymers 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- GTKRFUAGOKINCA-UHFFFAOYSA-M chlorosilver;silver Chemical compound [Ag].[Ag]Cl GTKRFUAGOKINCA-UHFFFAOYSA-M 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 238000002524 electron diffraction data Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0063—Granulating
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0215—Coating
- B01J37/0217—Pretreatment of the substrate before coating
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/002—Compounds containing, besides ruthenium, rhodium, palladium, osmium, iridium, or platinum, two or more other elements, with the exception of oxygen or hydrogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
- C01G55/004—Oxides; Hydroxides
-
- 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
-
- 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
- C25B1/13—Ozone
-
- 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
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
-
- 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
-
- 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
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Description
本発明に係る層状イリジウム酸塩は、MxIrOy・nH2O(Mは1価の金属、xは0.1〜0.5、yは1.5〜2.5、nは0.5〜1.5)が層状に重なり合っている。Mは、アルカリ金属であることが好ましく、例えば、Li、Na、K、Rb、Cs等を挙げることができる。また、x、yは、酸化イリジウムとアルカリ金属化合物の配合量で調製することができる。
本発明に係る酸化イリジウムナノシートは、3nm以下の厚さの酸化イリジウム単結晶シートである。この酸化イリジウムナノシートは、先ず、上記で得られた層状イリジウム酸に、アルキルアンモニウム又はアルキルアミンを反応させて、アルキルアンモニウム−層状イリジウム酸層間化合物とし、その後、そのアルキルアンモニウム−層状イリジウム酸層間化合物を水等の溶媒と混合して、酸化イリジウムナノシート分散溶液(濃紺色の分散溶液)を得る。得られた酸化イリジウムナノシート分散溶液を用いて、相互吸着法で酸化イリジウムナノシートを得ることができる。なお、アルキルアンモニウム又はアルキルアミンとしては、各種のものを用いることができるが、例えばテトラブチルアンモニウム等を好ましく用いることができる。
層状のイリジウム酸カリウム及び層状イリジウム酸を作製した。先ず、窒素置換したグローブボックス内で、酸化イリジウム(IrO2)を粉砕した後に炭酸カリウム(K2CO3)と混ぜ、30分間混合した。混合比(IrO2:K2CO3)は1:2とした。グローブボックスから出した混合物を、1.5tonで10分間のプレスを行ってペレットを成形した。次いで、成形したペレットをアルゴン雰囲気中にて750℃、1時間の焼成(第1回目の焼成)を行った。再びグローブボックス内に入れ、粉砕混合を行った後、1.5tonで10分間のプレスを行ってペレットを再び成形した。次いで、成形したペレットをアルゴン雰囲気中にて780℃、1時間の焼成(第2回目の焼成)を行った。焼成後のものは、光沢を持つ黒色を呈した。次いで、超音波を印加しながら中性になるまで水洗浄した。こうして、濃紺色がなくなった層状イリジウム酸カリウムを得た。その層状イリジウム酸カリウムを、1MHCl溶液に入れ、3日間放置して層状イリジウム酸を得た。上澄み液は褐色であった。
層状イリジウム酸から酸化イリジウムナノシートを作製した。実施例1で得た層状イリジウム酸を用い、10%テトラブチルアンモニウムヒドロキシド(TBAOH)溶液を、Ir:TBAOH=1:5で加えた。このとき、得られる酸化イリジウムナノシートの濃度が0.5g/Lになるように調製した。その後、25℃、160rpm、7日間振とうした。こうして、0.5g/L酸化イリジウムナノシート分散溶液を得た。この酸化イリジウムナノシート分散溶液は濃紺色であった。
実施例2で得た酸化イリジウムナノシート分散溶液を用いて酸化イリジウムナノシートを得た。ナノシートは、交互吸着積層法(Layer by Layer; LbL)により成膜した。先ず、酸化イリジウムナノシートを被覆するためのSi基板を準備し、10質量%PVA水溶液に10分間浸漬して洗浄し、超純水で洗浄した後、Si基板を0.3g/L酸化イリジウムナノシート分散溶液中に20分間浸漬した。Si基板を引き上げて超純水で洗浄し、再び10質量%PVA水溶液に戻して洗浄、浸漬を繰り返した。こうして、酸化イリジウムナノシートを被覆したSi基板を得た。
予め0.05μmのアルミナ粉末を用いてバフ研磨した直径5mmのグラッシーカーボン(東海カーボン株式会社)上に、実施例2で得た0.3g/L酸化イリジウムナノシート分散溶液20μLを滴下し、60℃30分乾燥させた。その上に、5質量%のナフィオン(Nafion、デュポン社の登録商標)溶液20μLを滴下し、60℃30分乾燥させた。こうして評価用電極を作製した。
電解液を1MLi2SO4に変えた他は、実施例4と同様にして比静電容量評価と安定性評価を行った。0.05V〜1.5V(vs.RHE)の電位範囲で、電気分解を伴うガス発生がなく、電極(酸化イリジウムナノシート)の溶解もなかった。
Claims (5)
- MxIrOy・nH2O(Mは1価の金属、xは0.1〜0.5、yは1.5〜2.5、nは0.5〜1.5)が層状に重なり合っていることを特徴とする層状イリジウム酸塩。
- 前記Mがカリウムであり、回折角2θ=13.0°、26.0°に回折ピークがある、請求項1に記載の層状イリジウム酸塩。
- HxIrOy・nH2O(xは0.1〜0.5、yは1.5〜2.5、nは0〜1)が層状に重なり合っていることを特徴とする層状イリジウム酸。
- 回折角2θ=12.3°、24.6°に回折ピークがある、請求項3に記載の層状イリジウム酸。
- 3nm以下の厚さの酸化イリジウム単結晶シートである酸化イリジウムナノシートの製造方法であって、
MxIrOy・nH2O(Mは1価の金属、xは0.1〜0.5、yは1.5〜2.5、nは0.5〜1.5)が層状に重なり合っている層状イリジウム酸塩を酸性溶液中で処理してHxIrOy・nH2O(xは0.1〜0.5、yは1.5〜2.5、nは0〜1)が層状に重なり合っている層状イリジウム酸とし、
次いで、前記層状イリジウム酸をアルキルアンモニウム−層状イリジウム酸層間化合物とし、溶媒と混合して、酸化イリジウムナノシート分散溶液を得て、
前記酸化イリジウムナノシート分散溶液から相互吸着法で得る3nm以下の厚さの酸化イリジウム単結晶シートを得る、ことを特徴とする酸化イリジウムナノシートの製造方法。
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2014048253A JP6173951B2 (ja) | 2014-03-11 | 2014-03-11 | 層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 |
PCT/JP2015/056972 WO2015137322A1 (ja) | 2014-03-11 | 2015-03-10 | 層状イリジウム酸塩、層状イリジウム酸及び酸化イリジウムナノシート |
US15/261,331 US9689080B2 (en) | 2014-03-11 | 2016-09-09 | Layered alkali iridate, layered iridic acid, and iridium oxide nanosheet |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2014048253A JP6173951B2 (ja) | 2014-03-11 | 2014-03-11 | 層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2017075604A Division JP6356301B2 (ja) | 2017-04-05 | 2017-04-05 | 酸化イリジウムナノシート、その酸化イリジウムナノシートを含む分散溶液及びその分散溶液の製造方法 |
Publications (2)
Publication Number | Publication Date |
---|---|
JP2015171966A JP2015171966A (ja) | 2015-10-01 |
JP6173951B2 true JP6173951B2 (ja) | 2017-08-02 |
Family
ID=54071766
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2014048253A Active JP6173951B2 (ja) | 2014-03-11 | 2014-03-11 | 層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 |
Country Status (3)
Country | Link |
---|---|
US (1) | US9689080B2 (ja) |
JP (1) | JP6173951B2 (ja) |
WO (1) | WO2015137322A1 (ja) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2023079246A (ja) * | 2021-11-28 | 2023-06-08 | 国立大学法人信州大学 | 酸化イリジウムナノシートを助触媒として含む電極触媒 |
JP2023080494A (ja) * | 2021-11-30 | 2023-06-09 | 国立大学法人信州大学 | イリジウム固溶マンガン酸化物 |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA2127749A1 (en) * | 1993-07-09 | 1995-01-10 | Takashi Itoh | Catalyst for purifying exhaust gas and method for purifying exhaust gas |
CA2144366A1 (en) * | 1995-03-09 | 1996-09-11 | Takashi Itoh | Method of purifying exhaust gas from internal combustion engine |
US7976989B2 (en) * | 2003-10-29 | 2011-07-12 | Umicore Ag & Co. Kg | Precious metal oxide catalyst for water electrolysis |
US7255745B2 (en) | 2004-10-21 | 2007-08-14 | Sharp Laboratories Of America, Inc. | Iridium oxide nanowires and method for forming same |
US7494840B2 (en) | 2004-10-21 | 2009-02-24 | Sharp Laboratories Of America, Inc. | Optical device with IrOx nanostructure electrode neural interface |
US7438759B2 (en) | 2004-10-21 | 2008-10-21 | Sharp Laboratories Of America, Inc. | Ambient environment nanowire sensor |
US7098144B2 (en) | 2004-10-21 | 2006-08-29 | Sharp Laboratories Of America, Inc. | Iridium oxide nanotubes and method for forming same |
US20080277746A1 (en) | 2004-10-21 | 2008-11-13 | Sharp Laboratories Of America, Inc. | Nanowire sensor with self-aligned electrode support |
US7022621B1 (en) | 2004-10-21 | 2006-04-04 | Sharp Laboratories Of America, Inc. | Iridium oxide nanostructure patterning |
JP4934799B2 (ja) | 2005-02-15 | 2012-05-16 | 国立大学法人 宮崎大学 | スポンジ状白金ナノシートをカーボンに担持せしめてなる白金−カーボン複合体とその製造方法 |
JP2008029838A (ja) * | 2006-07-31 | 2008-02-14 | Sharp Corp | IrOXナノ構造体電極のニューラル・インターフェースを有する光学装置 |
JP4779118B2 (ja) | 2006-09-04 | 2011-09-28 | 国立大学法人九州大学 | 貴金属ナノシートの製造方法 |
JP5582464B2 (ja) | 2009-06-08 | 2014-09-03 | 国立大学法人信州大学 | 金属ナノシートの製造方法、および金属ナノシート |
JP5792567B2 (ja) * | 2011-09-09 | 2015-10-14 | 国立大学法人信州大学 | 酸素還元能を有する電極触媒 |
-
2014
- 2014-03-11 JP JP2014048253A patent/JP6173951B2/ja active Active
-
2015
- 2015-03-10 WO PCT/JP2015/056972 patent/WO2015137322A1/ja active Application Filing
-
2016
- 2016-09-09 US US15/261,331 patent/US9689080B2/en active Active
Also Published As
Publication number | Publication date |
---|---|
WO2015137322A1 (ja) | 2015-09-17 |
US9689080B2 (en) | 2017-06-27 |
US20160376715A1 (en) | 2016-12-29 |
JP2015171966A (ja) | 2015-10-01 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Li et al. | Bottom-up MOF-intermediated synthesis of 3D hierarchical flower-like cobalt-based homobimetallic phophide composed of ultrathin nanosheets for highly efficient oxygen evolution reaction | |
Li et al. | Facile synthesis of porous Pt–Pd nanospheres supported on reduced graphene oxide nanosheets for enhanced methanol electrooxidation | |
Konkena et al. | MoSSe@ reduced graphene oxide nanocomposite heterostructures as efficient and stable electrocatalysts for the hydrogen evolution reaction | |
Srivastava et al. | Preparation and characterization of self-assembled layer by layer NiCo2O4–reduced graphene oxide nanocomposite with improved electrocatalytic properties | |
Zhang et al. | Anodic Transformation of a Core‐Shell Prussian Blue Analogue to a Bifunctional Electrocatalyst for Water Splitting | |
Deng et al. | Assembling Co9S8 nanoflakes on Co3O4 nanowires as advanced core/shell electrocatalysts for oxygen evolution reaction | |
Rovetta et al. | Cobalt hydroxide nanoflakes and their application as supercapacitors and oxygen evolution catalysts | |
Chang et al. | Hydrothermal synthesis of hydrous crystalline RuO2 nanoparticles for supercapacitors | |
Ishihara et al. | Titanium-niobium oxides mixed with Ti4O7 as precious-metal-and carbon-free cathodes for polymer electrolyte fuel cells | |
Lindstrom et al. | Facile synthesis of an efficient Ni–Fe–Co based oxygen evolution reaction electrocatalyst | |
Soares et al. | High Surface area LaNiO 3 electrodes for oxygen electrocatalysis in alkaline media | |
Li et al. | Electrodeposited ternary iron-cobalt-nickel catalyst on nickel foam for efficient water electrolysis at high current density | |
Lee et al. | Nanostructuring of metal surfaces by corrosion for efficient water splitting | |
Park et al. | Pseudocapacitive behavior of carbon nanoparticles modified by phosphomolybdic acid | |
Zhou et al. | A facile approach to tailor electrocatalytic properties of MnO2 through tuning phase transition, surface morphology and band structure | |
Bai et al. | Electrodeposition of cobalt nickel hydroxide composite as a high-efficiency catalyst for hydrogen evolution reactions | |
Atta et al. | Conducting polymer-mixed oxide composite electrocatalyst for enhanced urea oxidation | |
Fan et al. | Synthesis of small-sized freestanding Co3O4 nanosheets with improved activity for H2O2 sensing and oxygen evolution | |
Zhou et al. | Highly active surface structure in nanosized spinel cobalt-based oxides for electrocatalytic water splitting | |
Sun et al. | Bifunctional OER/NRR catalysts based on a thin-layered Co3O4–x/GO sandwich structure | |
Alharbi et al. | Hydrothermal synthesis of Er2O3–NiO material for oxidation of water in alkaline media | |
JP6173951B2 (ja) | 層状イリジウム酸塩及び層状イリジウム酸並びに酸化イリジウムナノシートの製造方法 | |
Kumar et al. | Unraveling the Effect of A-Site Sr-Doping in Double Perovskites Ca2–x Sr x ScRuO6 (x= 0 and 1): Structural Interpretation and Mechanistic Investigations of Trifunctional Electrocatalytic Effects | |
Yang et al. | Porous TiO2/Co9S8 core-branch nanosheet arrays with high electrocatalytic activity for a hydrogen evolution reaction | |
Rahmanian et al. | Graphene oxide-assisted electrochemical growth of Ni (OH) 2 nanoflowers on nickel foam as electrode material for high-performance supercapacitors |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20160608 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20161115 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20170112 |
|
A131 | Notification of reasons for refusal |
Free format text: JAPANESE INTERMEDIATE CODE: A131 Effective date: 20170207 |
|
A521 | Request for written amendment filed |
Free format text: JAPANESE INTERMEDIATE CODE: A523 Effective date: 20170405 |
|
TRDD | Decision of grant or rejection written | ||
A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20170620 |
|
A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20170705 |
|
R150 | Certificate of patent or registration of utility model |
Ref document number: 6173951 Country of ref document: JP Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |