JP5189289B2 - ペロブスカイト型複合酸化物の製造方法 - Google Patents
ペロブスカイト型複合酸化物の製造方法 Download PDFInfo
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- JP5189289B2 JP5189289B2 JP2006528423A JP2006528423A JP5189289B2 JP 5189289 B2 JP5189289 B2 JP 5189289B2 JP 2006528423 A JP2006528423 A JP 2006528423A JP 2006528423 A JP2006528423 A JP 2006528423A JP 5189289 B2 JP5189289 B2 JP 5189289B2
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- nitrate
- complex oxide
- perovskite complex
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- precursor powder
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- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000000843 powder Substances 0.000 claims description 25
- 229910002651 NO3 Inorganic materials 0.000 claims description 18
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 18
- 239000002243 precursor Substances 0.000 claims description 18
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 16
- 238000010304 firing Methods 0.000 claims description 9
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 8
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 8
- RFVVBBUVWAIIBT-UHFFFAOYSA-N beryllium nitrate Chemical compound [Be+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O RFVVBBUVWAIIBT-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000620 organic polymer Polymers 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 description 17
- 150000001875 compounds Chemical class 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- 239000004372 Polyvinyl alcohol Substances 0.000 description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000011575 calcium Substances 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 229910052748 manganese Inorganic materials 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000003826 uniaxial pressing Methods 0.000 description 4
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 229910002909 Bi-Te Inorganic materials 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000005679 Peltier effect Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 229910052747 lanthanoid Chemical group 0.000 description 2
- 150000002602 lanthanoids Chemical group 0.000 description 2
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920000609 methyl cellulose Polymers 0.000 description 2
- 239000001923 methylcellulose Substances 0.000 description 2
- 235000010981 methylcellulose Nutrition 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- 229920003169 water-soluble polymer Polymers 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical group [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- BFLBVMIBEQIANV-UHFFFAOYSA-N O.O.O.O.[Y] Chemical compound O.O.O.O.[Y] BFLBVMIBEQIANV-UHFFFAOYSA-N 0.000 description 1
- 230000005678 Seebeck effect Effects 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910008310 Si—Ge Inorganic materials 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- XWFVFZQEDMDSET-UHFFFAOYSA-N gadolinium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XWFVFZQEDMDSET-UHFFFAOYSA-N 0.000 description 1
- MWFSXYMZCVAQCC-UHFFFAOYSA-N gadolinium(iii) nitrate Chemical compound [Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O MWFSXYMZCVAQCC-UHFFFAOYSA-N 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 229940093474 manganese carbonate Drugs 0.000 description 1
- 239000011656 manganese carbonate Substances 0.000 description 1
- 235000006748 manganese carbonate Nutrition 0.000 description 1
- YMKHJSXMVZVZNU-UHFFFAOYSA-N manganese(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YMKHJSXMVZVZNU-UHFFFAOYSA-N 0.000 description 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 1
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- XRKAJAPEZSHSLG-UHFFFAOYSA-N yttrium(3+);trinitrate;tetrahydrate Chemical compound O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XRKAJAPEZSHSLG-UHFFFAOYSA-N 0.000 description 1
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- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1264—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing rare earth, e.g. La1-xCaxMnO3, LaMnO3
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Description
Michitaka Ohtaki et.al., Journal of Solid State Chemistry 120, 105−111(1995)
(2) 前記アルカリ土類金属元素を含有する硝酸塩は、硝酸ベリリウム、硝酸マグネシウム、硝酸マグネシウム六水和物、硝酸カルシウム及び硝酸カルシウム四水和物からなる群から選択される少なくとも1種の硝酸塩である(1)に記載のペロブスカイト型複合酸化物の製造方法。
0.0975molの硝酸カルシウムと、0.1molの硝酸マンガンおよび0.0025molの硝酸イットリウムを純水100mlに溶解し、更に20質量%のポリビニルアルコール(PVA)水溶液を20g添加して攪拌混合した。得られた水溶液を180℃の乾燥機で加熱乾燥し、黒褐色の前駆体粉末を得た。その後、この粉末を解砕した後、1t/cm2の圧力で1軸プレスにより成形した。これを大気中1100℃で5時間焼成を行い、棒状の焼結体セルを得た。焼結体密度は3.11g/cm3であり、理論密度の68%程度であった。
0.099molの硝酸カルシウムと、0.1molの硝酸マンガンおよび0.001molの硝酸イットリウムを純水100mlに溶解し、更に20質量%PVA水溶液を20g添加し攪拌混合した。得られた水溶液を180℃の乾燥機で加熱乾燥し、黒褐色の前駆体粉末を得た。その後、この粉末を解砕した後、1t/cm2の圧力で1軸プレスにより成形した。大気中1100℃で5時間焼成を行い、棒状の焼結体を得た。焼結体密度は3.20g/cm3であり、理論密度の70%程度であった。
0.095molの硝酸カルシウムと、0.1molの硝酸マンガンおよび0.005molの硝酸イットリウムを純水100mLに溶解し、更に20質量%PVA水溶液を20g添加し攪拌混合した。得られた水溶液を180℃の乾燥機で加熱乾燥し、黒褐色の前駆体粉末を得た。その後、この粉末を解砕した後、1t/cm2の圧力で1軸プレスにより成形した。大気中1100℃で5時間焼成を行い、棒状の焼結体を得た。焼結体密度は3.05g/cm3であり、理論密度の66%程度であった。
0.0975molの硝酸カルシウムと、0.1molの硝酸マンガンおよび0.0025molの硝酸ランタンを純水100mlに溶解し、更に20質量%PVA水溶液を20g添加し攪拌混合した。得られた水溶液を180℃の乾燥機で加熱乾燥し、黒褐色の前駆体粉末を得た。その後、この粉末を解砕した後、1t/cm2の圧力で1軸プレスにより成形した。大気中1100℃で5時間焼成を行い、棒状の焼結体を得た。焼結体密度は3.16/cm3であり、理論密度の69%程度であった。
0.0975molの炭酸カルシウムと、0.1molの炭酸マンガンおよび0.00125molの酸化イットリウムを秤量し、自動乳鉢で1時間攪拌混合した後、1000℃で10時間、大気中で仮焼を行った。得られた仮焼紛は解砕後、1t/cm2の圧力で1軸プレスにより成形した。これを1100℃で5時間、大気中で焼成し棒状の焼結体を得た。焼結体密度は3.84g/cm3であり、理論密度の84%程度であった。
Claims (2)
- ペロブスカイト型複合酸化物の製造方法であって、
希土類元素を含有する硝酸塩と、アルカリ土類金属元素を含有する硝酸塩と、マンガンを含有する硝酸塩と、有機高分子と、を溶媒に溶解する工程と、
この溶液を攪拌混合する工程と、
加熱乾燥により前駆体粉末を得る工程と、
この前駆体粉末を大気中で焼成する工程と、を備え、
前記加熱乾燥により前駆体粉末を得る工程は、150〜200℃で行われ、
前記前駆体粉末を大気中で焼成する工程は、1000〜1200℃で行われるペロブスカイト型複合酸化物の製造方法。 - 前記アルカリ土類金属元素を含有する硝酸塩は、硝酸ベリリウム、硝酸マグネシウム、硝酸マグネシウム六水和物、硝酸カルシウム及び硝酸カルシウム四水和物からなる群から選択される少なくとも1種の硝酸塩である請求項1に記載のペロブスカイト型複合酸化物の製造方法。
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FR2942624B1 (fr) * | 2009-03-02 | 2011-03-18 | Rhodia Operations | Composition comprenant une perovskite a base de lanthane sur un support en alumine ou en oxyhydroxyde d'aluminium, procede de preparation et utilisation en catalyse |
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US9425396B2 (en) | 2013-11-26 | 2016-08-23 | Hunt Energy Enterprises L.L.C. | Perovskite material layer processing |
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US9305715B2 (en) * | 2014-08-01 | 2016-04-05 | Hunt Energy Enterprises Llc | Method of formulating perovskite solar cell materials |
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