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Adapting the concepts of nonaqueous sol–gel chemistry to metals: synthesis and formation mechanism of palladium and palladium–copper nanoparticles in benzyl alcohol
Journal of Sol-Gel Science and Technology ( IF 2.5 ) Pub Date : 2020-06-11 , DOI: 10.1007/s10971-020-05278-z
Malwina Staniuk , Felix Rechberger , Elena Tervoort , Markus Niederberger

Abstract

Benzyl alcohol is a versatile reaction medium for the synthesis of different types of nanoparticles. Its ability to act as an oxygen source gave access to metal oxide nanoparticles, while its reducing properties can be harnessed for the preparation of metals. Here we report the synthesis of Pd and PdCu nanoparticles in benzyl alcohol supplemented by a detailed mechanistic study for both systems. To elucidate the chemical formation mechanism of the Pd nanoparticles, we performed in situ attenuated total reflection ultraviolet–visible (ATR-UV–vis) and Fourier transform infrared spectroscopy (ATR-FTIR), providing information on the organic as well as on the inorganic side of the reaction. Potential gaseous products were analyzed by in situ gas chromatography (GC) and mass spectrometry (MS). We observed the formation of benzaldehyde, toluene, and dibenzyl ether as the three main organic products. The formation of the PdCu alloy nanoparticles was studied by ex situ powder X-ray diffraction (PXRD). A time-resolved study of the synthesis at 100 °C indicated that initially three types of particles formed, composed of an alloy with high Pd content, an alloy with high content of copper, and palladium particles, and only later in the reaction course they transformed into an alloy with a Pd-to-Cu ratio close to 1.



中文翻译:

使非水溶胶-凝胶化学概念适用于金属:苯甲醇中钯和钯铜纳米颗粒的合成和形成机理

摘要

苄醇是用于合成不同类型纳米粒子的通用反应介质。其充当氧气源的能力使人们能够接触到金属氧化物纳米颗粒,同时可以利用其还原性来制备金属。在这里,我们报告了在苯甲醇中合成Pd和PdCu纳米粒子的过程,并辅以针对这两个系统的详细机理研究。为了阐明Pd纳米粒子的化学形成机理,我们进行了原位衰减全反射紫外可见(ATR-UV-vis)和傅立叶变换红外光谱(ATR-FTIR),提供了有关有机以及无机方面的信息反应的一面。通过原位气相色谱(GC)和质谱(MS)分析潜在的气态产物。我们观察到苯甲醛,甲苯,和二苄基醚作为三种主要有机产物。通过异位粉末X射线衍射(PXRD)研究了PdCu合金纳米颗粒的形成。一项在100°C下进行的时间分辨研究表明,最初形成了三种类型的颗粒,它们由高Pd含量的合金,高铜含量的合金和钯颗粒组成,并且仅在反应过程的后期才形成。转变为钯铜比接近1的合金

更新日期:2020-08-16
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