Thermoporometry as a new tool in analyzing mesoporous MCM-41 materials

Kloetstra, K. R.; Zandbergen, H.W.; Koten, Mark A.; Bekkum, H. van

doi:10.1007/bf00817054

Cited by 29 publications

(18 citation statements)

References 23 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…One of the first reports of application DSC to study the porosity of MCM-41 molecular sieves with various pore diameters was presented by Kloetstra et al [18]. Using water as the confined liquid, the authors obtained the results that stayed in a very good agreement with the nitrogen physisorption data.…”

Section: Introductionmentioning

confidence: 78%

Pore size distribution of micelle-templated silicas studied by thermoporosimetry using water and n-heptane

Majda

Makowski

Mańko

2012

J Therm Anal Calorim

View full text Add to dashboard Cite

Thermoporosimetry, i.e., DSC measurements of melting point depression of water and heptane confined in mesopores, has been used for determination the pore size distribution of several mesoporous silicas synthesized with the use of micelle templates. Porosity of these materials was additionally characterized by low-temperature nitrogen adsorption and quasi-equilibrated thermodesorption of nonane. The pore size distributions obtained using the water thermoporosimetry were similar to those determined using the other methods, but the pore size values found for the narrow pore materials were underestimated by ca 1 nm. Too large pore sizes obtained for the wide pore silica from heptane thermoporosimetry were attributed to nonlinear dependence of the melting point depression on the reciprocal of the pore size.

show abstract

Section: Introductionmentioning

confidence: 78%

Pore size distribution of micelle-templated silicas studied by thermoporosimetry using water and n-heptane

Majda

Makowski

Mańko

2012

J Therm Anal Calorim

View full text Add to dashboard Cite

show abstract

“…Thus, the thermoporometer records the energy evolved by the solidification of the condensate when the temperature is decreased. An important advantage of this technique is that information is obtained about the internal size of the pores and not of their entrances [12]. Furthermore, thermoporometry particularly applied for the characterization of porous materials allows the materials to be investigated in the medium in which they are normally used.…”

Section: General Principles Of Therrnoporornetrymentioning

confidence: 99%

Thermoporometry

Stcker¹

2002

Handbook of Porous Solids

View full text Add to dashboard Cite

The texture of porous materials with pore diameters larger than about 2 nm can be characterized by a calorimetric investigation of the liquid-solid state transition of a capillary condensate saturating these materials. The method, called thermoporometry, is based on the thermodynamic conditions of the liquid-solid transformation of the capillary condensate inside the porous material [l, 21. Thermoporometry is mainly used for the determination of pore-size distribution. Upon solidification and melting of a condensate that totally saturates the porous material, the phase change takes place inside the pores and no material transport occurs. This is not the case in most adsorption experiments. The resulting freezing-point depression of the confined probe molecules and the thermal energy released or absorbed are measured as a hnction of the temperature [3]. The thermal analysis of these transformations for condensates such as water or benzene leads to the pore-size distribution through the "solidification curve". The pore shape is related to the hysteresis phenomenon observed between the solidification and melting curves, allowing a shape factor to be calculated. Thermoporometry has the following advantages:(1) it gives the actual size of the cavities instead of indicating the size of the (2) it can be performed on nonrigid materials, and (3) it can be used for the study of materials in the medium in which they are opening, applied.Thermoporometry can be used also for studying materials in which the pore diameters are in the range of approximately 2-30 nm (i.e., in the mesopore range).

show abstract

“…TPM, although still not well recognized and developed, has been known since the works of Thomson [8,9] who demonstrated that a fluid confined in the pores of a solid material experiences an important shift of its liquid to solid transition temperature (DT). It has been observed that this shift is related to the size of the pores, in which the liquid is trapped [10], according to the Gibbs-Thomson equation. A liquid to solid phase transition requires formation of crystallization nuclei.…”

Section: Introductionmentioning

confidence: 96%

“…[10,21,22]. Also, several liquid compounds have been used to probe porous properties, for example benzene [14], acetonitrile [23], carbon tetrachloride [24] or acetone [25], however water and n-alkanes seem to be the most important and promising.…”

Section: Introductionmentioning

confidence: 98%