公开(公告)号：WO2012152740A2

公开(公告)日：2012-11-15

申请号：PCT/EP2012/058339

申请日：2012-05-07

申请人： BAYER INTELLECTUAL PROPERTY GMBH ,  RAUSCHER, Frank ,  FELDMANN, Claus ,  KIND, Christian ,  LU, Huachang ,  KÖHLER, Karen ,  MLECZKO, Leslaw

发明人： RAUSCHER, Frank ,  FELDMANN, Claus ,  KIND, Christian ,  LU, Huachang ,  KÖHLER, Karen ,  MLECZKO, Leslaw

IPC分类号： B22F1/00 ,  B22F1/02 ,  B22F9/24 ,  H01L21/304 ,  H05K3/10 ,  H01L31/0352

CPC分类号： B22F1/0018 ,  B22F9/24 ,  B82Y30/00

摘要： Process for the synthesis of nanoparticles comprising oxidation sensitive metals, in particular copper comprising the following steps: Preparation and nucleation of citrate-capped Metal-hydroxide nanoparticles, reduction of the intermediate citrate-capped Metal-hydroxide nanoparticles to Metal 0 by reduction via NaBH 4 Cu 0 nanoparticles with narrow size distribution are obtained by NaBH 4 Li-induced reduction of CUCI 2 2H 2 O in diethylene glycol. The course of the reaction essentially involves an intermediate formation of Cu(OH) 2 nanoparticles as well as the presence of citrate to control the nucleation of almost monodisperse and non-agglomerated Cu 0 nanoparticles. The citrate-capped Cu 0 nanoparticles of the invention are surprisingly stable against air oxidation. Via simple solvent evaporation, porous Cu 0 thin-films are prepared on glass substrates that exhibit bulk-like sheet resistances of 0.23 - 0.42 Ω ϛ after vacuum sintering at 250 °C (bulk-Cu sheet under similar conditions with: 0.3 Ω ϛ ). With these features the as-prepared, citrate-capped Cu 0 nanoparticles become highly relevant to electronic devices in particular thin-film electronics, thin-film sensors and high-power batteries.

摘要翻译： 用于合成包含氧化敏感金属，特别是铜的纳米颗粒的方法包括以下步骤：柠檬酸盐封端的金属氢氧化物纳米颗粒的制备和成核，通过NaBH 4 CuO纳米颗粒还原将中间体柠檬酸盐封端的金属氢氧化物纳米颗粒还原成金属O 通过NaBH 4 Li诱导的二甘醇中CUCI 2 2H 2 O的还原获得窄尺寸分布。 反应过程基本上包括Cu（OH）2纳米颗粒的中间形成以及柠檬酸盐的存在，以控制几乎单分散和非聚集的CuO纳米颗粒的成核。 本发明的柠檬酸盐封端的CuO纳米颗粒对于空气氧化是惊人的稳定的。 通过简单的溶剂蒸发，在玻璃基板上制备多孔CuO薄膜，其表现出大体积片状电阻为0.23-0.42O？ 在250℃下真空烧结（在相似条件下为0.3O 2的块状Cu片）。 具有这些特征的是，柠檬酸盐封端的CuO纳米粒子与电子器件特别是薄膜电子学，薄膜传感器和大功率电池非常相关。

公开(公告)号：WO2012152740A3

公开(公告)日：2013-01-10

申请号：PCT/EP2012058339

申请日：2012-05-07

申请人： BAYER IP GMBH ,  RAUSCHER FRANK ,  FELDMANN CLAUS ,  KIND CHRISTIAN ,  LU HUACHANG ,  KOEHLER KAREN ,  MLECZKO LESLAW

发明人： RAUSCHER FRANK ,  FELDMANN CLAUS ,  KIND CHRISTIAN ,  LU HUACHANG ,  KOEHLER KAREN ,  MLECZKO LESLAW

IPC分类号： B22F1/00 ,  B22F1/02 ,  B22F9/24 ,  H01L21/304 ,  H01L31/0352

CPC分类号： B22F1/0018 ,  B22F9/24 ,  B82Y30/00

摘要： Process for the synthesis of nanoparticles comprising oxidation sensitive metals, in particular copper comprising the following steps: Preparation and nucleation of citrate-capped Metal-hydroxide nanoparticles, reduction of the intermediate citrate-capped Metal-hydroxide nanoparticles to Metal0 by reduction via NaBH4 Cu0 nanoparticles with narrow size distribution are obtained by NaBH4 Li-induced reduction of CUCI2 2H2O in diethylene glycol. The course of the reaction essentially involves an intermediate formation of Cu(OH)2 nanoparticles as well as the presence of citrate to control the nucleation of almost monodisperse and non-agglomerated Cu0 nanoparticles. The citrate-capped Cu0 nanoparticles of the invention are surprisingly stable against air oxidation. Via simple solvent evaporation, porous Cu0 thin-films are prepared on glass substrates that exhibit bulk-like sheet resistances of 0.23 - 0.42 O? after vacuum sintering at 250 °C (bulk-Cu sheet under similar conditions with: 0.3 O?). With these features the as-prepared, citrate-capped Cu0 nanoparticles become highly relevant to electronic devices in particular thin-film electronics, thin-film sensors and high-power batteries.

摘要翻译： 用于合成包含氧化敏感金属，特别是铜的纳米颗粒的方法包括以下步骤：柠檬酸盐封端的金属氢氧化物纳米颗粒的制备和成核，通过NaBH 4 CuO纳米颗粒还原将中间体柠檬酸盐封端的金属氢氧化物纳米颗粒还原成金属O 通过NaBH 4 Li诱导的二甘醇中CUCI 2 2H 2 O的还原获得窄尺寸分布。 反应过程基本上包括Cu（OH）2纳米颗粒的中间形成以及柠檬酸盐的存在，以控制几乎单分散和非聚集的CuO纳米颗粒的成核。 本发明的柠檬酸盐封端的CuO纳米颗粒对于空气氧化是惊人的稳定的。 通过简单的溶剂蒸发，在玻璃基板上制备多孔CuO薄膜，其表现出块状薄层电阻为0.23-0.42O？ 在250℃下真空烧结（在相似条件下为0.3O 2的块状Cu片）。 具有这些特征的是，柠檬酸盐封端的CuO纳米粒子与电子器件特别是薄膜电子学，薄膜传感器和大功率电池非常相关。