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首页> 外文期刊>Crystal growth & design >In Situ In-House Powder X-ray Diffraction Study of Zero-Valent Copper Formation in Supercritical Methanol
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In Situ In-House Powder X-ray Diffraction Study of Zero-Valent Copper Formation in Supercritical Methanol

机译：原位内部粉末X射线衍射研究超临界甲醇零价铜形成

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Nano-/microcrystalline copper is widely used in catalysts, and it has potential for being used as conductive additive to ink for inkjet printed electronics. Copper is attractive, because it has excellent electrical conductivity and low cost compared to noble metals. The nucleation and phase transitions from the precursor to the final micrometer sized Cu in supercritical methanol have been studied for the first time using in-house in situ powder X-ray diffraction (PXRD). Temperatures have a significant impact on the reduction process of Cu2+; at a low synthesis temperature (250 degrees C), it was observed how the Cu2+ precursor initially formed copper hydroxy nitrate (Cu-2(OH)(3)NO3) and transformed to copper(II)oxide (CuO), i.e., no reduction took place. At 300 degrees C, multiple phase transformation could be observed from initial copper hydroxy nitrate to zerovalent copper; the in situ investigations reveal the following phase transitions; Cu-2(II)(OH)(3)NO3 -> (CuO)-O-II + (Cu2O)-O-I -> Cu-0. Increasing the synthesis temperature causes the pure Cu-0 to form much faster; at 350 degrees C, it takes 8.7 min to produce phase pure Cu-0, while at 450 degrees C, the formation takes similar to 0.7 min. Increasing the initial concentration of Cu2+ in the precursor causes formation of larger Cu-0 crystallites in the final product. Finally, the in situ observations were used as guidance for making Cu-0 using a supercritical flow setup.
机译：纳米/微晶铜广泛用于催化剂，它具有用作喷墨印刷电子的墨水的导电添加剂。铜具有吸引力，因为与贵金属相比，它具有优异的导电性和低成本。使用内部原位粉末X射线衍射（PXRD）首次使用在超临界甲醇中的前体与最终微米尺寸Cu的成核和相转变。温度对Cu2 +的还原过程产生显着影响;在低合成温度（250℃）时，观察到Cu 2 +前体最初形成氢羟基硝酸铜（Cu-2（OH）（3）NO 3）并转化为铜（II）氧化物（CUO），即，不减少发生了。在300℃下，可以从初始铜羟基硝酸盐中观察到多相变换到Zeropalent铜;原位调查揭示了以下阶段过渡; Cu-2（ii）（OH）（3）NO 3 - >（CUO）-O-II +（CU2O）-O-I-> Cu-0。增加合成温度使纯Cu-0形成更快;在350℃下，生产相纯Cu-0需要8.7分钟，而在450℃下，形成类似于0.7分钟。增加前体中Cu2 +的初始浓度导致在最终产物中形成较大的Cu-0微晶。最后，使用了使用超临界流量设定的制造CU-0的引导。

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