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首页> 外文期刊>Crystal growth & design >Kinetics study on the sol-gel reactions in supercritical CO2 by using in situ ATR-FTIR spectrometry
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Kinetics study on the sol-gel reactions in supercritical CO2 by using in situ ATR-FTIR spectrometry

机译：原位ATR-FTIR光谱法研究超临界CO2中溶胶-凝胶反应的动力学

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Direct sol-gel processing in supercritical CO2 (ScCO2) has been of significant interest for synthesizing oxide nanomaterials, and the reactions of metal alkoxides with organic acids have been extensively used for preparing metal complex crystals; however, a kinetics analysis of these reactions has not been reported. In this research, in situ ATR-FTIR spectra were collected during the sol-gel synthesis of Si, Ti, and Zr oxides in scCO(2). Because of overlapping of the IR peaks, it was difficult to directly correlate the optical absorbance with the analyte concentrations. To solve this problem, we used a chemometrics method, simple-to-use interactive self-modeling mixture analysis (SIMPLISMA), to calculate the concentration profiles. The precursor conversions and the intermediate concentration profiles under different synthesis conditions were obtained. The different kinetics profiles of Ti and Zr complexes in the sol-gel reactions were related to the activity of the metal complexes, and the competition of the various condensation reactions.
机译：在超临界CO2（ScCO2）中直接进行溶胶-凝胶处理对于合成氧化物纳米材料具有重大意义，并且金属醇盐与有机酸的反应已广泛用于制备金属络合物晶体。然而，尚未报道这些反应的动力学分析。在这项研究中，在scCO（2）中的Si，Ti和Zr氧化物的溶胶-凝胶合成过程中收集了原位ATR-FTIR光谱。由于IR峰重叠，因此很难将光吸收率与分析物浓度直接相关。为了解决此问题，我们使用化学计量学方法，易于使用的交互式自建模混合物分析（SIMPLISMA）来计算浓度曲线。获得了不同合成条件下的前体转化率和中间浓度分布。 Ti和Zr配合物在溶胶-凝胶反应中的不同动力学特征与金属配合物的活性以及各种缩合反应的竞争有关。

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