Abstract
Polyimide cross-linked silica aerogels with different weight percentages of polyimide were prepared through sol–gel technology and supercritical CO2 fluid drying technology. Tetraethoxysilane (TEOS) was used as a silica source precursor, 3-aminopropyltriethoxysilane (APTES) end-capped polyimide was used as a cross-linking agent, derived from 3, 3′, 4, 4′-biphenyltetracarboxylic dianhydride (BPDA) and 4, 4′-oxydianiline (ODA). The acid produced during the imidization process catalyzed the hydrolysis reaction without additional catalyst. After condensation reaction catalyzed by ammonium hydroxide solution, the polyimide cross-linked silica gels were obtained and then dried in supercritical CO2. The polyimide cross-linked silica aerogels have low density (0.132~0.187 g/cm3), high specific surface area (623–741 m2/g), low thermal conductivity (0.0306~0.0347 W/m K at room temperature), relatively high compressive strength (1.03~3.82 MPa) and high thermal decomposition temperature (360 °C). This research provided a simple and efficient method that used the polyimide as a strengthening phase to improve the mechanical properties of TEOS-based silica aerogels.
Similar content being viewed by others
References
Hrubesh LW (1998) Aerogel applications. J Non-Cryst Solids 225:335–342
Morris CA, Anderson ML, Stroud RM, Merzbacher CI, Rolison DR (1999) Silica sol as a nanoglue: flexible synthesis of composite aerogels. Science 284:622–624
Pierre AC, Pajonk GM (2002) Chemistry of aerogels and their applications. Chem Rev 102:4243–4266
Koebel M, Rigacci A, Achard P (2012) Aerogel-based thermal superinsulation: an overview. J Sol-Gel Sci Technol 63:315–339
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
Aegerter MA, Leventis N, Koebel MM (2011) Aerogels handbook. Springer-Verlag, New York, NY
Karout A, Buisson P, Perrard A, Pierre AC (2005) Shaping and mechanical reinforcement of silica aerogel biocatalysts with ceramic fiber felts. J Sol-Gel Sci Technol 36:163–171
Yang J, Li S, Luo Y, Wang F (2011) Compressive properties and fracture behavior of ceramic fiber-reinforced carbon aerogel under quasi-static and dynamic loading. Carbon 49:1542–1549
Gao QF, Feng J, Zhang CR, Feng JZ, Wu W, Jiang YG (2009) Mechanical properties of ceramic fiber-reinforced silica aerogel insulation composites. J Chin Ceram Soc 37:1–5
Yuan B, Ding S, Wang D, Wang G, Li H (2012) Heat insulation properties of silica aerogel/glass fiber composites fabricated by press forming. Mater Lett 75:204–206
Liao YD, Wu HJ, Ding YF (2012) Engineering thermal and mechanical properties of flexible fiber-reinforced aerogel composites. J Sol-Gel Sci Technol 63:445–456
Meador MAB, Vivod SL, Mccorkle L, Quade D, Sullivan RM, Ghosn LD, Clark N, Capadona LA (2008) Reinforcing polymer cross-linked aerogels with carbon nanofibers. J Mater Chem 18:1843–1852
Zhang G, Dass A, Rawashdeh AMM, Thomas J, Counsil JA, Leventis CS, Fabrizio EF, Ilhan F, Vassilaras P, Scheiman DA, Mccorkel L, Palczer A, Johnston CJ, Meador MA, Leventis N (2004) Isocyanate-cross-linked silica aerogel monoliths: preparation and characterization. J Non-Cryst Solids 350:152–164
Capadona LA, Meador MAB, Alunni A, Fabrizio E, Vassilaras P, Leventis N (2006) Flexible, low-density polymer cross-linked silica aerogels. Polymer 47:5754–5761
Sabri F, Marchetta J, Smith KM (2013) Thermal conductivity studies of a polyurea cross-linked silica aerogel-RTV 655 compound for cryogenic propellant tank applications in space. Acta Astronaut 91:173–179
Yang H, Kong X, Zhang Y, Wu C, Cao E (2011) Mechanical properties of polymer-modified silica aerogels dried under ambient pressure. J Non-Cryst Solids 357:3447–3453
Meador MAB, Fabrizio EF, Ilhan F, Dass A, Zhang G, Vassilaras P, Johnston JC, Leventis N (2005) Cross-linking amine-modified silica aerogels with epoxies: mechanically strong lightweight porous materials. Chem Mater 17:1085–1098
Meador MAB, Scherzer CM, Vivod SL, Quade D, Nguyen BN (2010) Epoxy reinforced aerogels made using a streamlined process. ACS Appl Mater Interfaces 2:2162–2168
Ge D, Yang L, Li Y, Zhao JP (2009) Hydrophobic and thermal insulation properties of silica aerogel/epoxy composite. J Non-Cryst Solids 355:2610–2615
Ahmad Z, Al-Sagheer F (2015) Novel epoxy-silica nano-composites using epoxy-modified silica hyper-branched structure. Progress Org Coat 80:65–70
Shao Z, Wu G, Cheng X, Zhao Y (2012) Rapid synthesis of amine cross-linked epoxy and methyl co-modified silica aerogels by ambient pressure drying. J Non-Cryst Solids 358:2612–2615
Randall JP, Meador MAB, Jana SC (2013) Polymer reinforced silica aerogels: effects of dimethyldiethoxysilane and bis (trimethoxysilylpropyl) amine as silane precursors. J Mater Chem A 1:6642–6652
Mirshafiei-Langari SA, Haddadi-Asl V, Roghani-Mamaqani H, Sobani M, Khezri K (2013) Synthesis of hybrid free and nanoporous silica aerogel-anchored polystyrene chains via in situ atom transfer radical polymerization. Polym Compos 34:1648–1654
Mirshafiei-Langari SA, Roghani-Mamaqani H, Sobani M, Sobani M, Khezri K (2013) In situ atom transfer radical polymerization of styrene in the presence of nanoporous silica aerogel: kinetic study and investigation of thermal properties. J Polym Res 20:163
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
Mulik S, Sotiriou-Leventis C, Churu G, Lu H, Leventis N (2008) Cross-linking 3D assemblies of nanoparticles into mechanically strong aerogels by surface-initiated free-radical polymerization. Chem Mater 20:5035–5046
Maleki H, Durães L, Portugal A (2014) Synthesis of lightweight polymer-reinforced silica aerogels with improved mechanical and thermal insulation properties for space applications. Microporous Mesoporous Mater 197:116–129
White LS, Bertino MF, Saeed S, Saoud K (2015) Influence of silica derivatizer and monomer functionality and concentration on the mechanical properties of rapid synthesis cross-linked aerogels. Microporous Mesoporous Mater 217:244–252
White LS, Bertino MF, Kitchen G, Young J, Newton C, Al-soubaihi R, Saeed S, Saoud K (2015) Shortened aerogel fabrication times using an ethanol–water azeotrope as a gelation and drying solvent. J Mater Chem A 3(2):762–772
Matsuura T, Yamada N, Nishi S, Hasuda Y (1993) Polyimides derived from 2,2′-bis (trifluoromethyl)-4, 4′-diaminobiphenyl. III: properties control for polymer blends and copolymerization of fluorinated polyimides. Macromolecules 26:419–423
Guo J, Nguyen BN, Li L, Meador MAB, Scheiman DA, Cakmak M (2013) Clay reinforced polyimide/silica hybrid aerogel. J Mater Chem A 1(24):7211–7221
Yan P, Zhou B, Du A (2014) Synthesis of polyimide cross-linked silica aerogels with good acoustic performance. RSC Adv 4:58252–58259
Rao AP, Pajonk GM, Rao AV (2005) Effect of preparation conditions on the physical and hydrophobic properties of two step processed ambient pressure dried silica aerogels. J Mater Sci 40:3481–3489
Acknowledgements
This work was supported by the National Natural Science Foundation of China (Grant No. 51702364) and Independent Project of Naval University of Engineering, China (Grant No. 425517K152).
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no conflict of interest.
Rights and permissions
About this article
Cite this article
Fei, Z., Yang, Z., Chen, G. et al. Preparation of tetraethoxysilane-based silica aerogels with polyimide cross-linking from 3, 3′, 4, 4′-biphenyltetracarboxylic dianhydride and 4, 4′-oxydianiline. J Sol-Gel Sci Technol 85, 506–513 (2018). https://doi.org/10.1007/s10971-017-4566-x
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10971-017-4566-x