The influence of drying and calcination on surface chemistry, pore structure and mechanical properties of hierarchically organized porous silica monoliths
Publikationen: Beitrag in Fachzeitschrift › Artikel › Forschung › (peer-reviewed)
Standard
in: Microporous and Mesoporous Materials, Jahrgang 288.2019, Nr. 1 November, 109578, 01.11.2019.
Publikationen: Beitrag in Fachzeitschrift › Artikel › Forschung › (peer-reviewed)
Harvard
APA
Vancouver
Author
Bibtex - Download
}
RIS (suitable for import to EndNote) - Download
TY - JOUR
T1 - The influence of drying and calcination on surface chemistry, pore structure and mechanical properties of hierarchically organized porous silica monoliths
AU - Putz, Florian
AU - Waag, Anna
AU - Balzer, Christian
AU - Braxmeier, Stephan
AU - Elsaesser, Michael S.
AU - Ludescher, Lukas
AU - Paris, Oskar
AU - Malfait, W. J.
AU - Reichenauer, Gudrun
AU - Hüsing, Nicola
PY - 2019/11/1
Y1 - 2019/11/1
N2 - Hierarchically organized, porous materials exhibit unique combinations of physical and chemical properties depending on their pore sizes, pore structure and surface chemistry. Extraction and drying methods as well as post synthetic thermal treatments influence the characteristics of the resulting porous network and thus the achievable properties. Here we present a comprehensive investigation of the effects of drying conditions and post synthesis treatments on surface chemistry, pore structure and resulting mechanical properties of hierarchically structured silica monoliths comprising pores on three hierarchy levels (micro-, meso- and macropores). Samples were either dried supercritically (SCD) with carbon dioxide or at ambient pressure (APD) after surface silylation. In addition, the impact of a post synthetic heat treatment at two different temperatures (300 °C and 500 °C) is investigated. The focus of the study is on chemical and structural changes in/at the (meso-)pore walls, including the presence of micropores and the influence of organic components on the macroscopic properties. We discuss the implications of these modifications on mechanical properties, such as their deformation behavior during fluid adsorption related to their respective bulk and skeletal Young's moduli. Scanning electron microscopy, nitrogen adsorption/desorption measurements, simultaneous thermal analysis, solid-state NMR spectroscopy, small-angle X-ray scattering, sound velocity measurements and nitrogen adsorption/desorption with in-situ dilatometry were performed on each sample. This set of data illustrates the significant impact of different fabrication steps such as drying or calcination on material properties.
AB - Hierarchically organized, porous materials exhibit unique combinations of physical and chemical properties depending on their pore sizes, pore structure and surface chemistry. Extraction and drying methods as well as post synthetic thermal treatments influence the characteristics of the resulting porous network and thus the achievable properties. Here we present a comprehensive investigation of the effects of drying conditions and post synthesis treatments on surface chemistry, pore structure and resulting mechanical properties of hierarchically structured silica monoliths comprising pores on three hierarchy levels (micro-, meso- and macropores). Samples were either dried supercritically (SCD) with carbon dioxide or at ambient pressure (APD) after surface silylation. In addition, the impact of a post synthetic heat treatment at two different temperatures (300 °C and 500 °C) is investigated. The focus of the study is on chemical and structural changes in/at the (meso-)pore walls, including the presence of micropores and the influence of organic components on the macroscopic properties. We discuss the implications of these modifications on mechanical properties, such as their deformation behavior during fluid adsorption related to their respective bulk and skeletal Young's moduli. Scanning electron microscopy, nitrogen adsorption/desorption measurements, simultaneous thermal analysis, solid-state NMR spectroscopy, small-angle X-ray scattering, sound velocity measurements and nitrogen adsorption/desorption with in-situ dilatometry were performed on each sample. This set of data illustrates the significant impact of different fabrication steps such as drying or calcination on material properties.
KW - hierarchical porosity
KW - hybrids
KW - in-situ dilatometry
KW - mechanical properties
KW - post synthesis treatments
U2 - 10.1016/j.micromeso.2019.109578
DO - 10.1016/j.micromeso.2019.109578
M3 - Article
AN - SCOPUS:85066610591
VL - 288.2019
JO - Microporous and Mesoporous Materials
JF - Microporous and Mesoporous Materials
SN - 1387-1811
IS - 1 November
M1 - 109578
ER -