JP6297095B2 - 金属酸化物メソ結晶及びその製造方法 - Google Patents
金属酸化物メソ結晶及びその製造方法 Download PDFInfo
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- JP6297095B2 JP6297095B2 JP2016102699A JP2016102699A JP6297095B2 JP 6297095 B2 JP6297095 B2 JP 6297095B2 JP 2016102699 A JP2016102699 A JP 2016102699A JP 2016102699 A JP2016102699 A JP 2016102699A JP 6297095 B2 JP6297095 B2 JP 6297095B2
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- metal oxide
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- metal
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- 229910044991 metal oxide Inorganic materials 0.000 title claims description 110
- 150000004706 metal oxides Chemical class 0.000 title claims description 110
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- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical group [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims description 21
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- 229910052725 zinc Inorganic materials 0.000 claims description 10
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- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 description 5
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- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
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- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
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- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
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- PSBDWGZCVUAZQS-UHFFFAOYSA-N (dimethylsulfonio)acetate Chemical compound C[S+](C)CC([O-])=O PSBDWGZCVUAZQS-UHFFFAOYSA-N 0.000 description 1
- GKQHIYSTBXDYNQ-UHFFFAOYSA-M 1-dodecylpyridin-1-ium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+]1=CC=CC=C1 GKQHIYSTBXDYNQ-UHFFFAOYSA-M 0.000 description 1
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- XPALGXXLALUMLE-UHFFFAOYSA-N 2-(dimethylamino)tetradecanoic acid Chemical compound CCCCCCCCCCCCC(N(C)C)C(O)=O XPALGXXLALUMLE-UHFFFAOYSA-N 0.000 description 1
- UNWFFCPRJXMCNV-UHFFFAOYSA-N 3-[dodecanoyl(methyl)amino]propanoic acid Chemical compound CCCCCCCCCCCC(=O)N(C)CCC(O)=O UNWFFCPRJXMCNV-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- 229910020366 ClO 4 Inorganic materials 0.000 description 1
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000012692 Fe precursor Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- SJIHVGHAFMPBSY-UHFFFAOYSA-N O=[Ni].O=[Cu] Chemical compound O=[Ni].O=[Cu] SJIHVGHAFMPBSY-UHFFFAOYSA-N 0.000 description 1
- ZXFQDPHJZVBMJZ-UHFFFAOYSA-N OCC[N+]1(CC([O-])=O)CCN=C1 Chemical compound OCC[N+]1(CC([O-])=O)CCN=C1 ZXFQDPHJZVBMJZ-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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- KHSLHYAUZSPBIU-UHFFFAOYSA-M benzododecinium bromide Chemical compound [Br-].CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 KHSLHYAUZSPBIU-UHFFFAOYSA-M 0.000 description 1
- CADWTSSKOVRVJC-UHFFFAOYSA-N benzyl(dimethyl)azanium;chloride Chemical compound [Cl-].C[NH+](C)CC1=CC=CC=C1 CADWTSSKOVRVJC-UHFFFAOYSA-N 0.000 description 1
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- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
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- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 1
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- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- REZZEXDLIUJMMS-UHFFFAOYSA-M dimethyldioctadecylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC REZZEXDLIUJMMS-UHFFFAOYSA-M 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- YVIGPQSYEAOLAD-UHFFFAOYSA-L disodium;dodecyl phosphate Chemical compound [Na+].[Na+].CCCCCCCCCCCCOP([O-])([O-])=O YVIGPQSYEAOLAD-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000004664 distearyldimethylammonium chloride (DHTDMAC) Substances 0.000 description 1
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 1
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
- SYELZBGXAIXKHU-UHFFFAOYSA-N dodecyldimethylamine N-oxide Chemical compound CCCCCCCCCCCC[N+](C)(C)[O-] SYELZBGXAIXKHU-UHFFFAOYSA-N 0.000 description 1
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 229940070765 laurate Drugs 0.000 description 1
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
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- IWIUXJGIDSGWDN-UQKRIMTDSA-M sodium;(2s)-2-(dodecanoylamino)pentanedioate;hydron Chemical compound [Na+].CCCCCCCCCCCC(=O)N[C@H](C([O-])=O)CCC(O)=O IWIUXJGIDSGWDN-UQKRIMTDSA-M 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
Images
Classifications
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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
- 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
- B01J23/80—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 zinc, cadmium or mercury
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
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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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/066—Zirconium or hafnium; Oxides or hydroxides thereof
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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Description
項1.金属酸化物メソ結晶の製造方法であって、
1種又は2種以上の金属酸化物前駆体、アンモニア塩、界面活性剤、及び水を含む前駆体水溶液を、300〜600℃の条件下に焼成する工程
を備える、製造方法。
項2.前記金属酸化物前駆体が、金属硝酸塩及び/又は金属フッ化物塩である、項1に記載の製造方法。
項3.前記アンモニア塩がNH4NO3である、項1又は2に記載の製造方法。
項4.前記界面活性剤が、陰イオン系界面活性剤、陽イオン系界面活性剤、両性界面活性剤及び非イオン性界面活性剤よりなる群から選ばれる少なくとも1種である、項1〜3のいずれかに記載の製造方法。
項5.前記前駆体水溶液は、
金属酸化物前駆体と界面活性剤との含有比率が1〜1000:1(モル比)であり、
アンモニア塩と界面活性剤の含有比率が1〜1000:1(モル比)である、
項1〜4のいずれかに記載の製造方法。
項6.項1〜5のいずれかに記載の製造方法により得られる金属酸化物メソ結晶。
項7.比表面積が0.5m2/g以上であり、平均幅が0.01〜1000μmである、遷移金属(ただしチタンを除く)の酸化物からなるメソ結晶。
項8.平均幅が400〜1000nmであり、比表面積が10m2/g以上である、酸化チタンメソ結晶。
項9.2種以上の金属を含むメソ結晶。
項10.比表面積が0.5m2/g以上である、項9に記載のメソ結晶。
項11.2種類以上の金属酸化物からなる、項9又は10に記載のメソ結晶。
項12.前記金属酸化物が、2種以上の遷移金属酸化物からなる、項11に記載のメソ結晶。
項13.合金の酸化物からなる、項9又は10に記載のメソ結晶。
項14.機能性材料の表面に、項6〜13のいずれかに記載のメソ結晶からなる層が形成された複合材料。
本発明の金属酸化物メソ結晶は、1種又は2種以上の金属酸化物前駆体、アンモニア塩、界面活性剤、及び水を含む前駆体水溶液を、300〜600℃の条件下に焼成する工程を備える方法により、製造することができる。これにより、酸化チタンメソ結晶だけでなく、様々な金属酸化物メソ結晶を製造することができる。
HO(CH2CH2O)a(CH2CH(CH3)O)b(CH2CH2O)cH
[式中、a〜cは同じか又は異なり、aは10〜140、bは10〜90、cは10〜140である。]
で示される化合物が好ましい。
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
が特に好ましい。
本発明の遷移金属(ただしチタンを除く)の酸化物からなるメソ結晶(以下、「メソ結晶A」とも言う)は、特に制限されないが、例えば、上記の製造方法により得られる。つまり、上記の製造方法において、金属酸化物前駆体として、チタン酸化物以外の金属酸化物の前駆体を用いることにより得られる。
本発明の酸化チタンメソ結晶(以下、「メソ結晶B」とも言う)は、特に制限されないが、例えば、上記の製造方法により得られる。つまり、上記の製造方法において、金属酸化物前駆体として、酸化チタン前駆体を用いることにより得られる。
本発明の2種以上の金属を含むメソ結晶(以下、「メソ結晶C」とも言う)は、特に制限されないが、例えば、上記の製造方法により得られる。つまり、上記の製造方法において、金属酸化物前駆体として、2種以上の金属酸化物の前駆体を用いる(例えば、金属酸化物Aの前駆体と金属酸化物Bの前駆体を使用)ことにより得られる。これにより、2種以上の金属酸化物ナノ粒子からなるメソ結晶を得ることもできるし、合金酸化物ナノ粒子からなるメソ結晶を得ることもできる。
本発明の金属酸化物メソ結晶は、上記のように、比表面積が大きいとともに、金属酸化物ナノ結晶を規則的に配列したものであり、且つ、サイズも大きく凝集を抑制できることから、光触媒活性が高く、導電性も高いものである。また、従来は得られなかった、2種以上の金属を含むメソ結晶も得ることができ、光触媒能をさらに向上させることも可能である。また、本発明によれば、非常に簡便な方法で上記メソ結晶を製造することができるため、大量生産性にも優れる。そのため、環境浄化光触媒、水素発生光触媒、色素増感太陽電池、リチウムイオンバッテリー等、種々様々な用途に適用することが可能である。
<酸化チタン>
実施例1:500℃焼成(Meso-TiO 2 -500)
まず、TiF4、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、TiF4:NH4NO3:P123:H2O=93:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例1の酸化チタンメソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
焼成温度を350℃とすること以外は実施例1と同様に、実施例2の酸化チタンメソ結晶を作製した。
焼成温度を300℃とすること以外は実施例1と同様に、実施例3の酸化チタンメソ結晶を作製した。
焼成温度を250℃とすること以外は実施例1と同様に、比較例1の酸化チタン結晶を含む混合物を作製した。
焼成温度を200℃とすること以外は実施例1と同様に、比較例2の酸化チタン結晶を含む混合物を作製した。
焼成温度を150℃とすること以外は実施例1と同様に、比較例3の酸化チタン結晶を含む混合物を作製した。
実施例4:500℃焼成(Meso-ZnO-500)
まず、Zn(NO3)2、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、Zn(NO3)2:NH4NO3:P123:H2O=126:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例4の酸化亜鉛メソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
焼成温度を350℃とすること以外は実施例4と同様に、実施例5の酸化亜鉛メソ結晶を作製した。
焼成温度を300℃とすること以外は実施例4と同様に、実施例6の酸化亜鉛メソ結晶を作製した。
焼成温度を250℃とすること以外は実施例4と同様に、比較例4の酸化亜鉛結晶を含む混合物を作製した。
実施例7:500℃焼成(Meso-NiO-500)
まず、Ni(NO3)2、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、Ni(NO3)2:NH4NO3:P123:H2O=55:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例7の酸化ニッケルメソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
焼成温度を350℃とすること以外は実施例7と同様に、実施例8の酸化ニッケルメソ結晶を作製した。
焼成温度を300℃とすること以外は実施例7と同様に、比較例5の酸化ニッケル結晶を含む混合物を作製した。
焼成温度を250℃とすること以外は実施例7と同様に、比較例6の酸化ニッケル結晶を含む混合物を作製した。
実施例9:500℃焼成(Meso-CuO-500)
まず、Cu(NO3)2、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、Cu(NO3)2:NH4NO3:P123:H2O=29:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例9の酸化銅メソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
焼成温度を350℃とすること以外は実施例9と同様に、実施例10の酸化銅メソ結晶を作製した。
焼成温度を300℃とすること以外は実施例9と同様に、実施例11の酸化銅メソ結晶を作製した。
焼成温度を250℃とすること以外は実施例9と同様に、比較例7の酸化銅結晶を含む混合物を作製した。
焼成温度を200℃とすること以外は実施例9と同様に、比較例7の酸化銅結晶を含む混合物を作製した。
焼成温度を150℃とすること以外は実施例9と同様に、比較例7の酸化銅結晶を含む混合物を作製した。
実施例12:酸化亜鉛ナノ粒子及び酸化銅ナノ粒子からなるメソ結晶(Meso-ZnO/CuO-500)
まず、Zn(NO3)2、Cu(NO3)2、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、Zn(NO3)2:Cu(NO3)2:NH4NO3:P123:H2O=39:20:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例12の酸化亜鉛/酸化銅複合型メソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
まず、Zn(NO3)2、Ni(NO3)2、NH4NO3、界面活性剤であるP123:
HO(CH2CH2O)20(CH2CH(CH3)O)70(CH2CH2O)20H
を含む前駆体水溶液(組成はモル比で、Zn(NO3)2:Ni(NO3)2:NH4NO3:P123:H2O=25:44:453:1:32000)からなる液層を、シリコン基板に形成した。具体的には、前駆体水溶液を基板上に滴下した。液層の厚みは、1mm程度となるようにした。シリコン基板上に形成した液層を、空気雰囲気下500℃で2時間焼成することで、シリコン基板上に実施例13の亜鉛ニッケル合金の酸化物ナノ粒子からなる複合型メソ結晶を形成した。なお、前駆体水溶液に使用した原料はいずれも市販品を使用した。
試験例1:比表面積
実施例1、4、7、9、12及び13の各メソ結晶の比表面積をBET法により測定した。結果を表1に示す。
実施例1、4、7、9、12及び13のメソ結晶の細孔径をBJH法により測定した。結果を表1に示す。
実施例1、4、7、9、12及び13のメソ結晶の特性を粉末X線回折(XRD)により測定した。また、実施例1、4、7、9、12及び13のメソ結晶について、X線回折ピークから、シェラーの式を用いて、各結晶を構成する金属酸化物ナノ結晶の粒子径を評価した。結果を表1及び図4に示す。なお、図4において、aは酸化チタン(実施例1〜3及び比較例1〜3)、bは酸化亜鉛(実施例4〜6及び比較例4)、cは酸化ニッケル(実施例7〜8及び比較例5〜6)、dは酸化銅(実施例9〜11及び比較例7〜9)、eは酸化亜鉛/酸化銅複合型メソ結晶(実施例12)、fは亜鉛ニッケル合金の酸化物ナノ粒子からなる複合型メソ結晶(実施例13)の結果である。
実施例1、4、7、9、12及び13のメソ結晶の特性を走査型電子顕微鏡(SEM)及び透過型電子顕微鏡(TEM)により観察した。結果を図5〜7に示す。
光生成した電子と正孔の再結合により、はっきりとしたフォトルミネッセンスが得られる。金属酸化物のフォトルミネッセンス特性を評価するため、単一粒子蛍光分光を行った。蛍光分光は、高い空間分解能で表面反応を観測することができる強力な手法である。
p−クロロフェノールの光触媒酸化を測定した。
実施例12の複合型メソ結晶について、その構造を分析するため、高角散乱環状暗視野走査透過顕微鏡測定(HAADF−STEM)及びエネルギー分散型X線分光測定(EDX)を行った。
実施例4、9及び12で得たメソ結晶の電子スピン共鳴スペクトル(EPRスペクトル)を、真空中77Kで測定した。結果を図13に示す。
超界面電荷移動ダイナミクスを明らかにするために、実施例4、9及び12で得たメソ結晶について、フェムト秒スケールの時間分解拡散反射分光測定を行った。結果を図14に示す。
Claims (9)
- 金属酸化物のナノ結晶又はナノ粒子が規則的に配列した構造体からなり、前記ナノ結晶又はナノ粒子の粒子径が5〜60nmであり、前記構造体が電子顕微鏡観察において均一格子縞が観測され、前記構造体の比表面積が0.5m2/g以上であり、前記金属酸化物が酸化ニッケルである、金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶の平均幅が、0.01〜1000μmである、請求項1に記載の金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶の平均細孔径が、2〜60nmである、請求項1又は2に記載の金属酸化物メソ結晶。
- 直径100〜300nmの略球状の結晶である、請求項1〜3のいずれか1項に記載の金属酸化物メソ結晶。
- 2種以上の金属を含む金属酸化物メソ結晶であって、前記金属酸化物メソ結晶の比表面積が0.5m2以上であり、かつ前記金属が、チタン、亜鉛、ニッケル、銅、鉄、コバルト、ジルコニア、セリウムから選ばれる2種以上であり、平均細孔径が20〜60nmである、金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶が、前記金属の金属酸化物ナノ結晶が規則的に配列しているものである、請求項5に記載の金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶が、前記金属の合金酸化物ナノ結晶が規則的に配列しているものである、請求項5に記載の金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶を構成する金属酸化物ナノ結晶又は合金酸化物ナノ結晶の平均粒子径が、5〜60nmである、請求項6又は7に記載の金属酸化物メソ結晶。
- 前記金属酸化物メソ結晶が、電子顕微鏡観察において均一格子縞が観測される、請求項6〜8のいずれか1項に記載の金属酸化物メソ結晶。
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |