Köck Eva-Maria, Kogler Michaela, Pramsoler Reinhold, Klötzer Bernhard, Penner Simon
Institute of Physical Chemistry, University of Innsbruck, Innrain 80-82, A-6020 Innsbruck, Austria.
Rev Sci Instrum. 2014 Aug;85(8):084102. doi: 10.1063/1.4891630.
The construction of a newly designed high-temperature, high-pressure FT-IR reaction cell for ultra-dry in situ and operando operation is reported. The reaction cell itself as well as the sample holder is fully made of quartz glass, with no hot metal or ceramic parts in the vicinity of the high-temperature zone. Special emphasis was put on chemically absolute water-free and inert experimental conditions, which includes reaction cell and gas-feeding lines. Operation and spectroscopy up to 1273 K is possible, as well as pressures up to ambient conditions. The reaction cell exhibits a very easy and variable construction and can be adjusted to any available FT-IR spectrometer. Its particular strength lies in its possibility to access and study samples under very demanding experimental conditions. This includes studies at very high temperatures, e.g., for solid-oxide fuel cell research or studies where the water content of the reaction mixtures must be exactly adjusted. The latter includes all adsorption studies on oxide surfaces, where the hydroxylation degree is of paramount importance. The capability of the reaction cell will be demonstrated for two selected examples where information and in due course a correlation to other methods can only be achieved using the presented setup.
报道了一种新设计的用于超干燥原位和操作条件下操作的高温、高压傅里叶变换红外(FT-IR)反应池的构建。反应池本身以及样品架完全由石英玻璃制成,在高温区附近没有热金属或陶瓷部件。特别强调了化学上绝对无水和惰性的实验条件,这包括反应池和气体输送管路。可以在高达1273 K的温度以及高达环境条件的压力下进行操作和光谱分析。该反应池具有非常简单且可变的结构,并且可以适配任何现有的傅里叶变换红外光谱仪。其独特优势在于能够在非常苛刻的实验条件下对样品进行检测和研究。这包括在非常高的温度下进行研究,例如用于固体氧化物燃料电池研究,或者在反应混合物的含水量必须精确调节的研究中。后者包括所有关于氧化物表面的吸附研究,其中羟基化程度至关重要。将通过两个选定的示例展示反应池的能力,在这些示例中,只有使用所展示的装置才能获得信息并在适当的时候与其他方法建立关联。