JP5155393B2 - 球形の酸化第一銅凝集体粒子組成物及びその製造方法 - Google Patents
球形の酸化第一銅凝集体粒子組成物及びその製造方法 Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims description 155
- 239000000203 mixture Substances 0.000 title claims description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 25
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title 1
- 229940112669 cuprous oxide Drugs 0.000 title 1
- 239000010949 copper Substances 0.000 claims description 157
- 239000011882 ultra-fine particle Substances 0.000 claims description 27
- 239000003638 chemical reducing agent Substances 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 20
- 239000004094 surface-active agent Substances 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 19
- -1 copper carboxyl compound Chemical class 0.000 claims description 16
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 150000001879 copper Chemical class 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 238000004220 aggregation Methods 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 125000000524 functional group Chemical group 0.000 claims description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 4
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 3
- 229930091371 Fructose Natural products 0.000 claims description 3
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims description 3
- 239000005715 Fructose Substances 0.000 claims description 3
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 2
- 239000005750 Copper hydroxide Substances 0.000 claims description 2
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 claims 1
- 239000001384 succinic acid Substances 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 230000000704 physical effect Effects 0.000 description 9
- 238000006722 reduction reaction Methods 0.000 description 9
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910001431 copper ion Inorganic materials 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000000879 optical micrograph Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 239000012691 Cu precursor Substances 0.000 description 1
- IILUTRCPUABLDZ-UHFFFAOYSA-N acetyl acetate;copper Chemical compound [Cu].CC(=O)OC(C)=O IILUTRCPUABLDZ-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- UGWKCNDTYUOTQZ-UHFFFAOYSA-N copper;sulfuric acid Chemical compound [Cu].OS(O)(=O)=O UGWKCNDTYUOTQZ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000059 patterning Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Description
[化学式1]
(R1−COO)2Cu
化学式1において、R1は炭素数が1ないし18のアルキル基である。
R1−COOH
化学式2において、R1は炭素数が1ないし18のアルキル基である。
(R1−COO)2Cu
化学式1において、R1は炭素数が1ないし18のアルキル基である。
R1−COOH
化学式2において、R1は炭素数が1ないし18のアルキル基である。
(CH3COO)2Cu・H2O 50mg及びポリアクリルアミド200mgを蒸留水4.5mlに溶解して第1溶液を用意し、アスコルビン酸22mgを蒸留水0.5mlに溶解して第2溶液を用意した。室温、常圧、及び空気中で、用意した2つの溶液を混合して10分間静置した。2000rpmで3分間遠心分離した後、上層の上澄み液を捨てて残った沈殿物を水20mlに再分散した後、遠心分離過程をさらに一回行ってCu2O粒子を得た。
ポリアクリルアミドを添加しないことを除き、実施例1と同様の方法でCu2O粒子を製造した。図8のSEM写真を参照すれば、大きい凝集体が一部形成されているものの、比較的均一な大きさのCu2O凝集体粒子である球体から形成されていることが分かる。平均大きさは777.2nm、標準偏差は300.6(39%)と計算された。
特許文献1の実施例1に記載された方法と同様に、下記のようにしてCu2O粒子を製造した。
Claims (15)
- 平均粒径が1ないし100nmであって粒径の標準偏差が0ないし10%である複数のCu2O超微粒子が相互凝集して形成された球形のCu2O凝集体粒子から構成され、
前記球形のCu2O凝集体粒子の平均粒径が0.1ないし10μmであって粒径の標準偏差が0ないし40%である球形のCu2O凝集体粒子組成物。 - 前記球形のCu2O凝集体粒子の表面が界面活性剤で被覆されていることを特徴とする請求項1に記載の球形のCu2O凝集体粒子組成物。
- 前記界面活性剤は、−OH、−COOH、−SH及び−NHからなる群より選択されたいずれか1つの官能基またはこれらのうち2種以上の官能基を持つ低分子、ポリアクリルアミド、ポリビニルピロリドン及びポリビニルアルコールからなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項2に記載の球形のCu2O凝集体粒子組成物。
- 前記界面活性剤はポリアクリルアミドであり、前記球形のCu2O凝集体粒子の粒径の標準偏差が0ないし20%であることを特徴とする請求項3に記載の球形のCu2O凝集体粒子組成物。
- (ステップ1)下記化学式1で表される銅カルボキシル化合物または下記化学式2で表されるカルボキシル基含有化合物と銅塩とを溶媒に溶解させてCu2O前駆体溶液を用意する段階;
[化学式1]
(R1−COO)2Cu
化学式1において、R1は炭素数が1ないし18のアルキル基である。
[化学式2]
R1−COOH
化学式2において、R1は炭素数が1ないし18のアルキル基である。
(ステップ2)前記Cu2O前駆体溶液に標準還元電位が−0.2ないし−0.05Vである弱還元剤を投入して、平均粒径が1ないし100nmであって粒径の標準偏差が0ないし10%である複数のCu2O超微粒子が相互凝集して形成され、その平均粒径が0.1ないし10μmであって粒径の標準偏差が0ないし40%である球形のCu2O凝集体粒子を形成する段階;
(ステップ3)ステップ2の結果物から前記球形のCu2O凝集体粒子を分離する段階を含む球形のCu2O凝集体粒子組成物の製造方法。 - 前記銅カルボキシル化合物は(CH3COO)2Cuであり、前記カルボキシル基含有化合物はCH3COOHであることを特徴とする請求項5に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記銅塩は、硝酸銅、ハロゲン化銅、水酸化銅、硫酸銅からなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項5に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記溶媒は、水、C1−C6の低級アルコール、ジメチルホルムアミド、ジメチルスルホキシド、テトラヒドロフラン及びアセト二トリルからなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項5に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記溶媒は水を含むことを特徴とする請求項8に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記弱還元剤は、アスコルビン酸、ジオール化合物、クエン酸、フルクトース、アミン化合物、α−ヒドロキシケトン化合物、コハク酸及びマルトースからなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項5に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記弱還元剤はアスコルビン酸であることを特徴とする請求項10に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記Cu2O前駆体溶液に界面活性剤をさらに添加することを特徴とする請求項5に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記界面活性剤は、−OH、−COOH、−SH、及び−NHからなる群より選択されたいずれか1つの官能基またはこれらのうち2種以上の官能基を持つ低分子、ポリアクリルアミド、ポリビニルピロリドン及びポリビニルアルコールからなる群より選択されたいずれか1つまたはこれらのうち2種以上の混合物であることを特徴とする請求項12に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記界面活性剤はポリアクリルアミドであり、前記球形のCu2O凝集体粒子の粒径の標準偏差が0ないし20%であることを特徴とする請求項13に記載の球形のCu2O凝集体粒子組成物の製造方法。
- 前記ステップ2は5ないし40℃で行われることを特徴とする請求項5に記載のCu2O凝集体粒子の製造方法。
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