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Dried hybrid imogolite nanotubes as solids with a changeable surface area: an insight into textural properties based on the correlation between nitrogen gas adsorption, immersion calorimetry into water, and small angle X-ray scattering
Physical Chemistry Chemical Physics ( IF 2.9 ) Pub Date : 2024-09-04 , DOI: 10.1039/d4cp02396j Ali Dhaini 1 , Amine Geneste 1 , Fadwa Alfadel Raad 2 , Pierre Picot 2 , Gaelle Martin-Gassin 1 , Benedicte Prelot 1 , Pierre-Marie Gassin 1 , Philippe Trens 1 , Antoine Thill 2 , Jerzy Zajac 1
Physical Chemistry Chemical Physics ( IF 2.9 ) Pub Date : 2024-09-04 , DOI: 10.1039/d4cp02396j Ali Dhaini 1 , Amine Geneste 1 , Fadwa Alfadel Raad 2 , Pierre Picot 2 , Gaelle Martin-Gassin 1 , Benedicte Prelot 1 , Pierre-Marie Gassin 1 , Philippe Trens 1 , Antoine Thill 2 , Jerzy Zajac 1
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Powdered samples of three imogolite materials with an inner surface covered with Si–CH3 groups (hybrid IMO-CH3) were prepared by ambient drying at 323 K, freeze drying, and spray drying. Reliable estimates of the intra-tube (SA), inter-tube (SB), and inter-bundle (SC) specific surface areas of these samples were inferred from a model-guided correlation between the results of measurements by small angle X-ray scattering (SAXS), nitrogen gas adsorption, and immersion calorimetry into water. Since the SAXS studies indicated no significant deformations of IMO-CH3 nanotubes upon drying, further studies by gaseous N2 adsorption at 77 K indicated the intra-tube and inter-bundle specific surface areas as being only accessible to this adsorbate. The outer curved surfaces of IMO nanotubes, including the inter-tube surface areas, were evaluated based on the calorimetric measurements of the enthalpy of immersion into water, using the enthalpy of immersion per unit surface area for a modelled curved surface of gibbsite as the conversion factor. Given the uncertainty in the determination of surface areas, the IMO-CH3 samples were found to possess the limiting values of specific surface areas ranging between 1150 and 1480 m2 g−1. In contrast to the two other materials, ambient-dried IMO-CH3 was characterized by the highest value of SC parameter due to the much smaller bundles formed by the constituent imogolite nanotubes. The accessibility of these surface areas, together with the hydrophobic and hydrophilic surface domains, was demonstrated to depend on the nature of the surrounding medium and the size of the adsorbing species.
中文翻译：
具有可变表面积的干燥杂化伊毛缟石纳米管：基于氮气吸附、水中浸入量热法和小角度 X 射线散射之间的相关性深入了解织构特性
通过323 K环境干燥、冷冻干燥和喷雾干燥制备了内表面覆盖有Si-CH 3基团的三种伊缟石材料的粉末样品（杂化IMO-CH 3 ）。这些样品的管内 ( SA )、管间 (SB) 和管束间 (SC )比表面积的可靠估计是根据模型引导的小角度测量结果之间的相关性推断出来的X 射线散射 (SAXS)、氮气吸附和水中浸入量热法。由于SAXS研究表明IMO-CH 3纳米管在干燥时没有显着变形，因此在77 K下进行的气态N 2吸附的进一步研究表明管内和束间比表面积仅可由该吸附物接触。 IMO纳米管的外曲面，包括管间表面积，是根据浸入水中的热函的量热测量来评估的，使用三水铝石曲面模型的每单位表面积的浸入函作为转换因素。鉴于表面积测定的不确定性，发现IMO-CH 3样品具有范围在1150至1480 m 2 g -1之间的比表面积极限值。 与其他两种材料相比，常温干燥的IMO-CH 3的特点是SC参数最高，因为伊毛缟石纳米管形成的束要小得多。这些表面区域的可及性以及疏水性和亲水性表面域被证明取决于周围介质的性质和吸附物质的大小。
更新日期：2024-09-04
中文翻译：
具有可变表面积的干燥杂化伊毛缟石纳米管：基于氮气吸附、水中浸入量热法和小角度 X 射线散射之间的相关性深入了解织构特性
通过323 K环境干燥、冷冻干燥和喷雾干燥制备了内表面覆盖有Si-CH 3基团的三种伊缟石材料的粉末样品（杂化IMO-CH 3 ）。这些样品的管内 ( SA )、管间 (SB) 和管束间 (SC )比表面积的可靠估计是根据模型引导的小角度测量结果之间的相关性推断出来的X 射线散射 (SAXS)、氮气吸附和水中浸入量热法。由于SAXS研究表明IMO-CH 3纳米管在干燥时没有显着变形，因此在77 K下进行的气态N 2吸附的进一步研究表明管内和束间比表面积仅可由该吸附物接触。 IMO纳米管的外曲面，包括管间表面积，是根据浸入水中的热函的量热测量来评估的，使用三水铝石曲面模型的每单位表面积的浸入函作为转换因素。鉴于表面积测定的不确定性，发现IMO-CH 3样品具有范围在1150至1480 m 2 g -1之间的比表面积极限值。 与其他两种材料相比，常温干燥的IMO-CH 3的特点是SC参数最高，因为伊毛缟石纳米管形成的束要小得多。这些表面区域的可及性以及疏水性和亲水性表面域被证明取决于周围介质的性质和吸附物质的大小。
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