Directly ambient pressure dried robust bridged silsesquioxane and methylsiloxane aerogels: effects of precursors and solvents

Robust low-cost silica based aerogels can be obtained by choosing appropriate silane precursors and chemical conditions. In this paper, we synthesized two kinds of bridged siloxane precursors, bridged silsesquioxane (BSQ) from (3-aminopropyl)-triethoxysilane (APTES) and m-phthalaldehyde (MPA), and bridged methylsiloxane (BMSQ) from (3-aminopropyl)-diethoxymethylsilane (APDEMS) and m-phthalaldehyde (MPA) to prepare robust aerogels. Methanol and ethanol were used individually as solvents in the experiment and all the products were dried directly at ambient pressure without any solvent exchange process. All the products show low densities (about 0.15 g cm−3) and large porosities (larger than 80%). The influence of the precursor and solvent was investigated. The BSQ aerogels have larger specific surface areas, smaller pore sizes and more stable mechanical performances. Aerogels prepared using methanol as the solvent gel faster and have larger pore sizes. The solvent has greater impacts on the BSQ aerogels, the BSQ aerogels prepared using ethanol as the solvent can withstand 60% deformation in repeated compression tests, exhibiting good mechanical performance.

[1]  Hyung‐Ho Park,et al.  Facile synthesis of hydrophobic, thermally stable, and insulative organically modified silica aerogels using co-precursor method , 2018 .

[2]  Luísa Durães,et al.  Effect of different types of surfactants on the microstructure of methyltrimethoxysilane-derived silica aerogels: A combined experimental and computational approach. , 2018, Journal of colloid and interface science.

[3]  Hongyi Gao,et al.  Vacuum-Dried Synthesis of Low-Density Hydrophobic Monolithic Bridged Silsesquioxane Aerogels for Oil/Water Separation: Effects of Acid Catalyst and Its Excellent Flexibility , 2018 .

[4]  K. Nakanishi,et al.  Transparent, Superflexible Doubly Cross-Linked Polyvinylpolymethylsiloxane Aerogel Superinsulators via Ambient Pressure Drying. , 2018, ACS nano.

[5]  Hyung‐Ho Park,et al.  Ambient pressure dried tetrapropoxysilane-based silica aerogels with high specific surface area , 2018 .

[6]  Hyung‐Ho Park,et al.  Role of oxalic acid in structural formation of sodium silicate-based silica aerogel by ambient pressure drying , 2018, Journal of Sol-Gel Science and Technology.

[7]  Hyung‐Ho Park,et al.  Flexible and Transparent Silica Aerogels: An Overview , 2017 .

[8]  Yulu Zhang,et al.  Robust urethane-bridged silica aerogels available for water-carved aerosculptures , 2017 .

[9]  K. Nakanishi,et al.  Transparent Ethylene-Bridged Polymethylsiloxane Aerogels and Xerogels with Improved Bending Flexibility. , 2016, Langmuir : the ACS journal of surfaces and colloids.

[10]  D. Tang,et al.  Robust and superhydrophobic thiourethane bridged polysilsesquioxane aerogels as potential thermal insulation materials , 2016 .

[11]  K. Nakanishi,et al.  Low-density, transparent aerogels and xerogels based on hexylene-bridged polysilsesquioxane with bendability , 2016, Journal of Sol-Gel Science and Technology.

[12]  Huaihe Song,et al.  Highly flexible silica aerogels derived from methyltriethoxysilane and polydimethylsiloxane , 2015 .

[13]  C. Su,et al.  Highly porous aerogels based on imine chemistry: syntheses and sorption properties , 2015 .

[14]  Yanfeng Gao,et al.  Low-density, hydrophobic, highly flexible ambient-pressure-dried monolithic bridged silsesquioxane aerogels , 2015 .

[15]  Jian Xu,et al.  Robust superhydrophobic bridged silsesquioxane aerogels with tunable performances and their applications. , 2015, ACS applied materials & interfaces.

[16]  Kentaro Abe,et al.  Polymethylsilsesquioxane-cellulose nanofiber biocomposite aerogels with high thermal insulation, bendability, and superhydrophobicity. , 2014, ACS applied materials & interfaces.

[17]  H. Maleki,et al.  An overview on silica aerogels synthesis and different mechanical reinforcing strategies , 2014 .

[18]  J. Wu,et al.  Vacuum‐Dried Robust Bridged Silsesquioxane Aerogels , 2013, Advanced materials.

[19]  S. Jana,et al.  Reinforcement of silica aerogels using silane-end-capped polyurethanes. , 2013, Langmuir : the ACS journal of surfaces and colloids.

[20]  Y. Yamauchi,et al.  Preparation of Colloidal Mesoporous Silica Nanoparticles with Different Diameters and Their Unique Degradation Behavior in Static Aqueous Systems , 2012 .

[21]  M. A. Meador,et al.  Elastic behavior of methyltrimethoxysilane based aerogels reinforced with tri-isocyanate. , 2010, ACS applied materials & interfaces.

[22]  K. Sinkó Influence of Chemical Conditions on the Nanoporous Structure of Silicate Aerogels , 2010, Materials.

[23]  Tian Sang,et al.  Preparation of spherical silica particles by Stöber process with high concentration of tetra-ethyl-orthosilicate. , 2010, Journal of colloid and interface science.

[24]  A. V. Rao,et al.  Effect of protic solvents on the physical properties of the ambient pressure dried hydrophobic silica aerogels using sodium silicate precursor , 2008 .

[25]  Shih‐Yuan Lu,et al.  Transparent, hydrophobic composite aerogels with high mechanical strength and low high-temperature thermal conductivities. , 2008, The journal of physical chemistry. B.

[26]  D. Zhao,et al.  A facile aqueous route to synthesize highly ordered mesoporous polymers and carbon frameworks with Ia3d bicontinuous cubic structure. , 2005, Journal of the American Chemical Society.

[27]  J. Chwastowski,et al.  Aerogel Cherenkov detectors for the luminosity measurement at HERA , 2003 .

[28]  G. Stucky,et al.  Manipulation of pore size distributions in silica and ormosil gels dried under ambient pressure conditions , 2002 .

[29]  M. Einarsrud,et al.  Effect of precursors, methylation agents and solvents on the physicochemical properties of silica aerogels prepared by atmospheric pressure drying method , 2001 .

[30]  W. C. Ackerman,et al.  Use of surface treated aerogels derived from various silica precursors in translucent insulation panels , 2001 .

[31]  U. Schubert,et al.  Aerogels-Airy Materials: Chemistry, Structure, and Properties. , 1998, Angewandte Chemie.

[32]  J. Pirard,et al.  Mercury Porosimetry Applied to Low Density Xerogels; Relation between Structure and Mechanical Properties , 1998 .

[33]  G. M. Jamison,et al.  Sol-gel synthesis of hybrid organic-inorganic materials. Hexylene- and phenylene-bridged polysiloxanes , 1996 .

[34]  S. Blacher,et al.  Interpretation of mercury porosimetry applied to aerogels , 1995 .

[35]  J. Sjöblom,et al.  Preparation of silica particles utilizing the sol-gel and the emulsion-gel processes , 1995 .

[36]  G. Pajonk,et al.  Effect of solvents and catalysts on monolithicity and physical properties of silica aerogels , 1994, Journal of Materials Science.

[37]  Larry L. Hench,et al.  The sol-gel process , 1990 .

[38]  E. Gulari,et al.  Dynamics of Growth of Silica Particles from Ammonia-Catalyzed Hydrolysis of Tetra-ethyl-orthosilicate , 1988 .

[39]  J. Mackenzie,et al.  Sol-gel processing of silica: I. The role of the starting compounds , 1986 .

[40]  W. Stöber,et al.  Controlled growth of monodisperse silica spheres in the micron size range , 1968 .

[41]  E. W. Washburn Note on a Method of Determining the Distribution of Pore Sizes in a Porous Material. , 1921, Proceedings of the National Academy of Sciences of the United States of America.