Abstract
Flexible, monolithic and superhydrophobic silica aerogels were obtained by combining methyltrimethoxysilane (MTMS), vinyltrimethoxysilane (VTMS) and tetramethylorthosilicate (TMOS) (50:30:20 mol%) in a one-step base-catalyzed co-precursor sol–gel procedure. Polybutylacrylate (PBA) and polystyrene (PS) were grafted and cross-linked in the gel aiming to enhance the mechanical performance. Fourier transform infrared spectroscopy, thermogravimetry analysis and scanning electron microscopy confirmed the presence of the polymers as a binding coating on the 3D silica network, primarily formed by firmly connected 3–5 μm secondary particles. When compared to the MTMS-based aerogels, the VTMS–MTMS–TMOS-derived aerogels, either reinforced or not, show a threefold increase of the bulk density (to ~150–160 kg m−3) and a consequent decrease in the surface area and average pore size; the thermal conductivity also increases to 60–70 mW m−1 K−1, a 50 % increase over the values of MTMS-derived aerogels. Although these tendencies are more marked in the polymer-reinforced materials, the change of the silica skeleton from MTMS to VTMS–MTMS–TMOS is responsible for the main differences. The VTMS–MTMS–TMOS underlying structure gives a fourfold increase in compressive strength relatively to the MTMS-derived aerogels, even when not reinforced. In addition, it retains a high elongation at break (40–50 %) and flexibility—modulus of 25 kPa for the PBA-reinforced aerogel, the more flexible aerogel, and modulus of 91 kPa for PS-reinforced aerogel, the stiffer and stronger material. The obtained aerogels have touch feeling that resembles that of expanded polystyrene foams, and also show negligible particle shedding, which is a valued characteristic for aerospace applications.
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References
Durães L, Ochoa M, Portugal A, Duarte N, Dias JP, Rocha N, Hernandez J (2010) Tailored silica based xerogels and aerogels for insulation in space environments. Adv Sci Technol 63:41–46
Ochoa M, Durães L, Beja AM, Portugal A (2012) Study of the suitability of silica based xerogels synthesized using ethyltrimethoxysilane and/or methyltrimethoxysilane precursors for aerospace applications. J Sol-Gel Sci Technol 61(1):151–160
Koebel M, Rigacci A, Achard P (2012) Aerogel-based thermal superinsulation: an overview. J Sol-Gel Sci Technol 63(3):315–339
Cuce E, Cuce PM, Wood CJ, Riffat SB (2014) Toward aerogel based thermal superinsulation in buildings: a comprehensive review. Renew Sustain Energy Rev 34:273–299
Gibiat V, Lefeuvre O, Woignier T, Pelous J, Phalippou J (1995) Acoustic properties and potential applications of silica aerogels. J Sol-Gel Sci Technol 186:244–255
Ward DA, Ko EI (1995) Preparing Catalytic Materials by the Sol-Gel Method. Ind Eng Chem Res 34(2):421–433
Wang D, Liu Y, Hu Z, Hong C, Pan C (2005) Michael addition polymerizations of trifunctional amines with diacrylamides. Polymer 46:3507–3514
Perdigoto MLN, Martins RC, Rocha N, Quina MJ, Gando-Ferreira L, Patrício R, Durães L (2012) Application of hydrophobic silica based aerogels and xerogels for removal of toxic organic compounds from aqueous solutions. J Colloid Interface Sci 380:134–140
Aegerter MA, Leventis N, Koebel MM (2001) Aerogels handbook. Springer, New York
Maleki H, Durães L, Portugal A (2014) An overview on silica aerogels synthesis and different mechanical reinforcing strategies. J Non-Cryst Solids 385:55–74
Active Aerogels & University of Coimbra (Inventors: Ochoa M, Durães L, Perdigoto M, Portugal A) Flexible panels of hydrophobic aerogel reinforced with fibre felts. Patent WO 2015/016739 A2
Nguyen BN, Meador MAB, Tousley ME, Shonkwiler B, McCorkle L, Scheiman DA, Palczer A (2009) Tailoring elastic properties of silica aerogels crosslinked with polystyrene. ACS Appl Mater Interfaces 1(3):621–630
Guo H, Nguyen BN, McCorkle LS, Shonkwiler B, Meador MAB (2009) Elastic low density aerogels derived from bis[3-(triethoxysilyl)propyl]disulfide, tetramethylorthosilicate and vinyltrimethoxysilane via a two-step process. J Mater Chem 19(47):9054–9062
Maleki H, Durães L, Portugal A (2015) Development of mechanically strong ambient pressure dried silica aerogels with optimized properties. J Phys Chem C 119(14):7689–7703
Durães L, Ochoa M, Rocha N, Patrício R, Duarte N, Redondo V, Portugal A (2012) Effect of the drying conditions on the microstructure of silica based xerogels and aerogels. J Nanosci Nanotechnol 12(8):6828–6834
Durães L, Maia A, Portugal A (2015) Effect of additives on the properties of silica based aerogels synthesized from methyltrimethoxysilane (MTMS). J Supercrit Fluids 106:85–92
Varino C (2012) Synthesis of silica based hybrid aerogels using vinyltrimethoxysilane precursor. MSc dissertation, University of Coimbra
Haynes WM (2015) CRC handbook of chemistry and physics, 96th edn. CRC Press, Boca Raton
Al-Oweini R, El-Rassy H (2009) Synthesis and characterization by FTIR spectroscopy of silica aerogels prepared using several Si(OR)4 and R″Si(OR′)3 precursors. J Mol Struct 919:140–145
Becker HGO, Berger W, Domschke G, Fanghänel E, Faust J, Fischer M, Gentz F, Gewald K, Gluch R, Mayer R, Müller K, Pavel D, Schmidt H, Schollberg K, Schwetlick K, Seiler E, Zeppenfeld G (1997) Organikum, 2nd edn. Calouste Gulbenkian Foundation, Lisbon
Maleki H, Durães L, Portugal A (2014) Synthesis of lightweight polymer reinforced silica aerogels with improved mechanical and thermal insulation properties for space applications. Micropor Mesopor Mater 197:116–129
Loy DA, Jamison GM, Baugher BM, Myers AS, Assink RA, Shea KJ (1996) Sol–gel synthesis of hybrid organic–inorganic materials. Hexylene- and phenylene-bridged polysiloxanes. Chem Mater 8:656–663
Maleki H, Durães L, Portugal A (2015) Synthesis of mechanically reinforced silica aerogels via surface-initiated reversible addition-fragmentation chain transfer (RAFT) polymerization. J Mater Chem A 3:1594–1600
Peterson JD, Vyazovkin S, Wight CA (2001) Kinetics of the thermal and thermo-oxidative degradation of polystyrene, polyethylene and polypropylene. Macromol Chem Phys 202:775–784
Hu Y-H, Chen C-Y, Wang C-C (2004) Thermal degradation kinetics of poly(n-butyl acrylate) initiated by lactams and thiols. Polym Degrad Stabil 84:505–514
Coelho JFJ, Silva AMFP, Popov AV, Perlec V, Abreu MV, Gonçalves PMOF, Gil MH (2006) Single electron transfer-degenerative chain transfer living radical polymerization of N-butyl acrylate catalyzed by Na2S2O4 in water media. J Polym Sci A 44:2809–2825
Acknowledgements
This work was funded by FEDER funds through the Operational Programme for Competitiveness Factors—COMPETE and National Funds, through FCT—Foundation for Science and Technology under the projects PTDC/EQU–EPR/099998/2008—GelSpace—Silica-based Aerogels for Insulation of Spatial Devices, PEst-C/EQB/UI102/2011 and PEst-C/EQB/UI102/2013. Mara Braga acknowledges FCT for the fellowship SFRH/BPD/101048/2014 and for Programa Ciência 2008. The authors also acknowledge Active Aerogels for collaborating in this work.
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Matias, T., Varino, C., de Sousa, H.C. et al. Novel flexible, hybrid aerogels with vinyl- and methyltrimethoxysilane in the underlying silica structure. J Mater Sci 51, 6781–6792 (2016). https://doi.org/10.1007/s10853-016-9965-9
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DOI: https://doi.org/10.1007/s10853-016-9965-9