Characterization of porous samples containing mesopores larger than 10 nm in size is often difficult due to limitations of standard methods. In the present work thermoporometry (TPM) was introduced to address these challenges. Various probe liquids (water, n-heptane, cyclohexane and o-xylene) were previously applied for TPM characterization of mesoporous silicon containing pores of 20–50 nm. The results, obtained with the use of calibration equations, confirmed the necessity of new probe liquid more suitable for characterization of such samples. Octamethylcyclotetrasiloxane was found to be the most appropriate choice. Mesoporous silicon samples were used as model materials in order to establish an empirical equation between the pore sizes, derived from mercury porometry, and the solid-liquid transition temperature depressions derived from differential scanning calorimetry for the octamethylcyclotetrasiloxane confined inside the pores and in bulk phase. The new calibration equations obtained within this work can be successfully used for characterization of the samples with large mesopores.

由于标准方法的局限性，通常难以表征包含中孔尺寸大于10 nm的多孔样品。在当前的工作中，引入了热孔法（TPM）来应对这些挑战。先前已使用各种探针液体（水，正庚烷，环己烷和邻二甲苯）对含20–50 nm孔的中孔硅进行TPM表征。通过使用校准方程式获得的结果证实了使用新的探针液体更适合表征此类样品的必要性。发现八甲基环四硅氧烷是最合适的选择。使用中孔硅样品作为模型材料，以建立由汞孔度法得出的孔径之间的经验方程，以及差示扫描量热法测定的八甲基环四硅氧烷的固-液相转变温度降低，该八甲基环四硅氧烷被限制在孔内和本体相中。在这项工作中获得的新的校准方程式可以成功地用于表征具有大中孔的样品。