Abstract
This study aims to improve thermal insulation by incorporating silica aerogel into PVDF-HFP nanofiber membranes. The nanofiber membranes were created using needleless electrospinning, with careful optimization of voltage and polymer concentration. Silica aerogel was synthesized via the sol–gel ambient drying method. To integrate silica aerogel particles into PVDF-HFP nanofiber two approaches were used. First, ex-situ, involving the mixing of silica aerogel particles with the PVDF-HFP polymeric solution in predetermined proportions prior to electrospinning, and in-situ, which entailed synthesizing silica aerogel within pre-fabricated PVDF-HFP nanofiber membranes. Multiple analytical tools SEM, EDX, BET, FTIR, and TGA–DSC, were used to assess the composition, microstructure, pore-size, and thermal behavior of PVDF-HFP nanofiber embedded with silica aerogel. It was evident that the in-situ method proved to be more effective in reducing the thermal conductivity, more breathable, and water repellent making it a preferred choice for extreme cold-weather protection.
Graphical abstract
Similar content being viewed by others
Data availability
Readers can access the data upon request (prashantjinde@gmail.com).
References
K.E. Parmenter, F. Milstein, Mechanical properties of silica aerogels. J. Non Cryst. Solids 223, 179–189 (1998). https://doi.org/10.1016/S0022-3093(97)00430-4
Z. Mazrouei-Sebdani, M. Naeimirad, S. Peterek, H. Begum, S. Galmarini, F. Pursche, E. Baskin, S. Zhao, T. Gries, W.J. Malfait, Multiple assembly strategies for silica aerogel-fiber combinations—a review. Mater. Des. (2022). https://doi.org/10.1016/j.matdes.2022.111228
O. Palacio, W.J. Malfait, S. Michel, M. Barbezat, Z. Mazrouei-Sebdani, Vibration and structure-borne sound isolation properties of silica aerogels. Constr. Build. Mater. (2023). https://doi.org/10.1016/j.conbuildmat.2023.132568
R. Hasanzadeh, T. Azdast, P.C. Lee, C.B. Park, A review of the state-of-the-art on thermal insulation performance of polymeric foams. Therm. Sci. Eng. Prog. (2023). https://doi.org/10.1016/j.tsep.2023.101808
S. Ahmad, S. Ahmad, J.N. Sheikh, Silica centered aerogels as advanced functional material and their applications: a review. J. Non Cryst. Solids (2023). https://doi.org/10.1016/j.jnoncrysol.2023.122322
J.C.H. Wong, H. Kaymak, S. Brunner, M.M. Koebel, Mechanical properties of monolithic silica aerogels made from polyethoxydisiloxanes. Microporous Mesoporous Mater. 183, 23–29 (2014). https://doi.org/10.1016/J.MICROMESO.2013.08.029
L.W. Hrubesh, Aerogel applications. J. Non Cryst. Solids 225, 335–342 (1998). https://doi.org/10.1016/S0022-3093(98)00135-5
F. Akhter, S.A. Soomro, V.J. Inglezakis, Silica aerogels; a review of synthesis, applications and fabrication of hybrid composites. J. Porous Mater. 28, 1387–1400 (2021). https://doi.org/10.1007/S10934-021-01091-3/METRICS
A. Soleimani Dorcheh, M.H. Abbasi, Silica aerogel; synthesis, properties and characterization. J. Mater. Process. Technol. 199, 10 (2008). https://doi.org/10.1016/j.jmatprotec.2007.10.060
H. Choi, V.G. Parale, K.Y. Lee, H.Y. Nah, Z. Driss, D. Driss, A. Bouabidi, S. Euchy, H.H. Park, Polypropylene/silica aerogel composite incorporating a conformal coating of methyltrimethoxysilane-based aerogel. J. Nanosci. Nanotechnol. 19, 1376–1381 (2018). https://doi.org/10.1166/JNN.2019.16257
N. Nazeran, J. Moghaddas, Synthesis and characterization of silica aerogel reinforced rigid polyurethane foam for thermal insulation application. J. Non Cryst. Solids 461, 1–11 (2017). https://doi.org/10.1016/J.JNONCRYSOL.2017.01.037
Z.A. Abdul Halim, M.A. Mat Yajid, M.H. Idris, H. Hamdan, Effects of silica aerogel particle sizes on the thermal–mechanical properties of silica aerogel—unsaturated polyester composites. Plast Rubber Compos 46, 184–192 (2017). https://doi.org/10.1080/14658011.2017.1306913
G. Guzel Kaya, H. Deveci, Synergistic effects of silica aerogels/xerogels on properties of polymer composites: a review. J. Ind. Eng. Chem. 89, 13–27 (2020). https://doi.org/10.1016/J.JIEC.2020.05.019
R. Szczepaniak, A. Komorek, P. Przybyłek, A. Krzyżak, M. Roskowicz, J. Godzimirski, E. Pinkiewicz, W. Jaszczak, E. Kosicka, Research into mechanical properties of an ablative composite on a polymer matrix base with aerogel particles. Compos. Struct. (2022). https://doi.org/10.1016/j.compstruct.2021.114855
M. Kucharek, W. MacRae, L. Yang, Investigation of the effects of silica aerogel particles on thermal and mechanical properties of epoxy composites. Compos. Part A Appl. Sci. Manuf. 139, 106108 (2020). https://doi.org/10.1016/J.COMPOSITESA.2020.106108
S. Ramesh, H.S. Kim, Y.J. Lee, G.W. Hong, J.H. Kim, Nanostructured silica/gold-cellulose-bonded amino-POSS hybrid composite via sol-gel process and its properties. Nanoscale Res. Lett. (2017). https://doi.org/10.1186/s11671-017-2122-9
J.H. Moon, J.S. Seo, Y. Xu, S. Yang, Direct fabrication of 3D silica-like microstructures from epoxy-functionalized polyhedral oligomeric silsesquioxane (POSS). J. Mater. Chem. (2009). https://doi.org/10.1039/b901226e
G. Hayase, K. Kanamori, K. Nakanishi, T. Hanada, Synthesis of new flexible aerogels from di- and trifunctional organosilanes. MRS Proc. (2011). https://doi.org/10.1557/opl.2011.216
S. Sert Çok, N. Gizli, Microstructural properties and heat transfer characteristics of in-situ modified silica aerogels prepared with different organosilanes. Int. J. Heat Mass Transf. (2022). https://doi.org/10.1016/j.ijheatmasstransfer.2022.122618
D.B. Anthony, S.N. Nguyen, H. Qian, S. Xu, C.M.D. Shaw, E.S. Greenhalgh, A. Bismarck, M.S.P. Shaffer, Silica aerogel infused hierarchical glass fiber polymer composites. Compos. Commun. 39, 101531 (2023). https://doi.org/10.1016/j.coco.2023.101531
J. Liu, Z.W. He, G. Bai, W.Y. Zhu, X. Li, H.X. Xie, H. Wang, M.J. Chang, J. Yang, Y.Q. Wang, Z.M. Luo, Fabrication of novel water glass-based monolithic aerogels with fibrous skeleton under alkaline for oil sorption and thermal evaporation. J. Non Cryst. Solids (2023). https://doi.org/10.1016/j.jnoncrysol.2023.122349
X. Yang, Y. Sun, D. Shi, J. Liu, Experimental investigation on mechanical properties of a fiber-reinforced silica aerogel composite. Mater. Sci. Eng. A 528, 4830–4836 (2011). https://doi.org/10.1016/J.MSEA.2011.03.013
S. Sedighi, A. Khoddami, H. Izadan, M.A. Alsharif, M. Naeimirad, The influence of silica aerogels on physical, mechanical, and morphological properties of melt-spun POY and DTY polyester yarns. Polym. Test. 112, 107628 (2022). https://doi.org/10.1016/J.POLYMERTESTING.2022.107628
S. Meng, J. Zhang, W. Chen, X. Wang, M. Zhu, Construction of continuous hollow silica aerogel fibers with hierarchical pores and excellent adsorption performance. Microporous Mesoporous Mater. 273, 294–296 (2019). https://doi.org/10.1016/J.MICROMESO.2018.07.021
H. Li, L. Song, C. Sun, R. Li, Y. Fu, H. Zhang, A. Yang, H. Liu, Thermal insulation of silica aerogel/PMMA composites with amino-capped polydivinylsiloxane phase interfaces. IEEE J. Sel. Top. Quantum Electron. 25, 1107–1114 (2018). https://doi.org/10.1515/SECM-2017-0248/MACHINEREADABLECITATION/RIS
Z. Sheng, Z. Liu, Y. Hou, H. Jiang, Y. Li, G. Li, X. Zhang, The rising aerogel fibers: status, challenges, and opportunities. Adv. Sci. 10, 2205762 (2023). https://doi.org/10.1002/ADVS.202205762
U. Berardi, S. Zaidi, Characterization of commercial aerogel-enhanced blankets obtained with supercritical drying and of a new ambient pressure drying blanket. Energy Build 198, 542–552 (2019). https://doi.org/10.1016/J.ENBUILD.2019.06.027
Y. Huang, S. He, G. Chen, H. Dai, B. Yuan, X. Chen, X. Yang, Fast preparation of glass fiber/silica aerogel blanket in ethanol & water solvent system. J. Non Cryst. Solids 505, 286–291 (2019). https://doi.org/10.1016/J.JNONCRYSOL.2018.11.003
P. Jinde, R. Naik, A. Rakshit, Characterization and synthesis of polyester and viscose nonwovens fabrics embedded with nanoporous amorphous silica. J. Text. Inst. 110, 972–979 (2019). https://doi.org/10.1080/00405000.2018.1534305
F. He, W.J. Yu, M.H. Fang, X.D. He, M.W. Li, An overview on silica aerogels synthesized by siloxane co-precursors. J. Inorg. Mater. 30, 1243 (2015). https://doi.org/10.15541/JIM20150223
R. Al-Oweini, H. El-Rassy, 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 (2009). https://doi.org/10.1016/J.MOLSTRUC.2008.08.025
M.A.R. Bhuiyan, L. Wang, R.A. Shanks, Z.A. Ara, T. Saha, Electrospun polyacrylonitrile–silica aerogel coating on viscose nonwoven fabric for versatile protection and thermal comfort. Cellulose 27, 10501–10517 (2020). https://doi.org/10.1007/s10570-020-03489-9
H. Zheng, H. Shan, Y. Bai, X. Wang, L. Liu, J. Yu, B. Ding, Assembly of silica aerogels within silica nanofibers: towards a super-insulating flexible hybrid aerogel membrane. RSC Adv. 5, 91813–91820 (2015). https://doi.org/10.1039/c5ra18137b
N.M. Mahmoodi, Z. Mokhtari-Shourijeh, S. Langari, A. Naeimi, B. Hayati, M. Jalili, K. Seifpanahi-Shabani, Silica aerogel/polyacrylonitrile/polyvinylidene fluoride nanofiber and its ability for treatment of colored wastewater. J. Mol. Struct. (2021). https://doi.org/10.1016/j.molstruc.2020.129418
H. Wu, Y. Chen, Q. Chen, Y. Ding, X. Zhou, H. Gao, Synthesis of flexible aerogel composites reinforced with electrospun nanofibers and microparticles for thermal insulation. J. Nanomater. (2013). https://doi.org/10.1155/2013/375093
R. Arat, H. Baskan, G. Ozcan, P. Altay, Hydrophobic silica-aerogel integrated polyacrylonitrile nanofibers. J. Ind. Text. 51, 4740S-4756S (2022). https://doi.org/10.1177/1528083720939670
Y.G. Kim, H.S. Kim, S.M. Jo, S.Y. Kim, B.J. Yang, J. Cho, S. Lee, J.E. Cha, Thermally insulating, fire-retardant, smokeless and flexible polyvinylidene fluoride nanofibers filled with silica aerogels. Chem. Eng. J. 351, 473–481 (2018). https://doi.org/10.1016/j.cej.2018.06.102
K.P. Matabola, R.M. Moutloali, The influence of electrospinning parameters on the morphology and diameter of poly(vinyledene fluoride) nanofibers—effect of sodium chloride. J. Mater. Sci. 48, 5475–5482 (2013). https://doi.org/10.1007/S10853-013-7341-6/METRICS
V. Jacobs, R.D. Anandjiwala, M. Maaza, The influence of electrospinning parameters on the structural morphology and diameter of electrospun nanofibers. J. Appl. Polym. Sci. 115, 3130–3136 (2010). https://doi.org/10.1002/APP.31396
I. Partheniadis, I. Nikolakakis, I. Laidmäe, J. Heinämäki, A mini-review: needleless electrospinning of nanofibers for pharmaceutical and biomedical applications. Processes 8, 673 (2020). https://doi.org/10.3390/PR8060673
A. Venkateswara Rao, S.D. Bhagat, Synthesis and physical properties of TEOS-based silica aerogels prepared by two step (acid–base) sol–gel process. Solid State Sci. 6, 945–952 (2004). https://doi.org/10.1016/J.SOLIDSTATESCIENCES.2004.04.010
A.M. Al-Dhahebi, M.S.M. Saheed, M. Mustapha, Effects of solution concentration on the synthesis of polyvinylidene fluoride (PVDF) electrospun nanofibers. Mater Today Proc 80, 2119–2124 (2023). https://doi.org/10.1016/J.MATPR.2021.06.128
T.M.W.J. Bandara, A.M.J.S. Weerasinghe, M.A.K.L. Dissanayake, G.K.R. Senadeera, M. Furlani, I. Albinsson, B.E. Mellander, Characterization of poly (vinylidene fluoride-co-hexafluoropropylene) (PVdF-HFP) nanofiber membrane based quasi solid electrolytes and their application in a dye sensitized solar cell. Electrochim. Acta 266, 276–283 (2018). https://doi.org/10.1016/J.ELECTACTA.2018.02.025
S.V.K. Shalu, R.K. Singh, Development of ion conducting polymer gel electrolyte membranes based on polymer PVdF-HFP, BMIMTFSI ionic liquid and the Li-salt with improved electrical, thermal and structural properties. J Mater Chem C Mater 3, 7305–7318 (2015). https://doi.org/10.1039/C5TC00940E
D. Saikia, Y.W. Chen-Yang, Y.T. Chen, Y.K. Li, S.I. Lin, Investigation of ionic conductivity of composite gel polymer electrolyte membranes based on P(VDF-HFP), LiClO4 and silica aerogel for lithium ion battery. Desalination 234, 24–32 (2008). https://doi.org/10.1016/J.DESAL.2007.09.066
P.M. Shewale, A.V. Rao, A.P. Rao, Effect of different trimethyl silylating agents on the hydrophobic and physical properties of silica aerogels. Appl. Surf. Sci. 254, 6902–6907 (2008). https://doi.org/10.1016/j.apsusc.2008.04.109
S.A. Mahadik, F. Pedraza, V.G. Parale, H.H. Park, Organically modified silica aerogel with different functional silylating agents and effect on their physico-chemical properties. J. Non Cryst. Solids 453, 164–171 (2016). https://doi.org/10.1016/j.jnoncrysol.2016.08.035
Y. Xia, J. Li, H. Wang, Z. Ye, X. Zhou, H. Huang, Y. Gan, C. Liang, J. Zhang, W. Zhang, Synthesis and electrochemical performance of poly(vinylidene fluoride)/SiO2 hybrid membrane for lithium-ion batteries. J. Solid State Electrochem. 23, 519–527 (2018). https://doi.org/10.1007/S10008-018-4161-2
H.Y. Nah, V.G. Parale, K.Y. Lee, H. Choi, T. Kim, C.H. Lim, J.Y. Seo, Y.S. Ku, J.W. Park, H.H. Park, Silylation of sodium silicate-based silica aerogel using trimethylethoxysilane as alternative surface modification agent. J. Solgel Sci. Technol. 87, 319–330 (2018). https://doi.org/10.1007/S10971-018-4729-4/METRICS
Z. Li, X. Cheng, S. He, X. Shi, L. Gong, H. Zhang, Aramid fibers reinforced silica aerogel composites with low thermal conductivity and improved mechanical performance. Compos. Part A Appl. Sci. Manuf. 84, 316–325 (2016). https://doi.org/10.1016/J.COMPOSITESA.2016.02.014
Y.J. Kim, C.H. Ahn, M.B. Lee, M.S. Choi, Characteristics of electrospun PVDF/SiO2 composite nanofiber membranes as polymer electrolyte. Mater. Chem. Phys. 127, 137–142 (2011). https://doi.org/10.1016/J.MATCHEMPHYS.2011.01.046
Á. Lakatos, A. Trnik, Thermal characterization of fibrous aerogel blanket. MATEC Web of Conf. 282, 01001 (2019). https://doi.org/10.1051/MATECCONF/201928201001
A. Lakatos, A. Csik, A. Trnik, I. Budai, Effects of the heat treatment in the properties of fibrous aerogel thermal insulation. Energies 12, 2001 (2019). https://doi.org/10.3390/EN12102001
F.K. Ko, Y. Wan, Introduction to nanofiber materials (Cambridge University Press, Cambridge, 2014). https://doi.org/10.1017/CBO9781139021333
F. Yang, X. Zhao, T. Xue, S. Yuan, Y. Huang, W. Fan, T. Liu, Superhydrophobic polyvinylidene fluoride/polyimide nanofiber composite aerogels for thermal insulation under extremely humid and hot environment. Sci. China Mater. 64, 1267–1277 (2021). https://doi.org/10.1007/S40843-020-1518-4/METRICS
Á. Lakatos, A. Csík, I. Csarnovics, Experimental verification of thermal properties of the aerogel blanket. Case Stud. Therm. Eng. 25, 100966 (2021). https://doi.org/10.1016/J.CSITE.2021.100966
M. Venkataraman, R. Mishra, D. Jasikova, T.M. Kotresh, J. Militky, Thermodynamics of aerogel-treated nonwoven fabrics at subzero temperatures. J. Ind. Text. 45, 387–404 (2015). https://doi.org/10.1177/1528083714534711
Y. Liu, H. Wu, Y. Zhang, J. Yang, F. He, Structure characteristics and hygrothermal performance of silica aerogel composites for building thermal insulation in humid areas. Energy Build (2020). https://doi.org/10.1016/j.enbuild.2020.110452
Z. Mazrouei-Sebdani, L. Javazmi, A. Khoddami, F. Shams-Ghahfarokhi, T. Low, Fabrication of a silica aerogel and examination of its hydrophobic properties via contact angle and 3M water repellency tests. IOP Conf. Ser. Mater. Sci. Eng. (2017). https://doi.org/10.1088/1757-899X/204/1/012014
H. Cai, Y. Jiang, J. Feng, S. Zhang, F. Peng, Y. Xiao, L. Li, J. Feng, Preparation of silica aerogels with high temperature resistance and low thermal conductivity by monodispersed silica sol. Mater. Des. 191, 108640 (2020). https://doi.org/10.1016/J.MATDES.2020.108640
J. Liu, P. Buahom, C. Lu, H. Yu, C.B. Park, Microscopic revelation of the solid–gas coupling and Knudsen effect on the thermal conductivity of silica aerogel with inter-connected pores. Sci. Rep. 12, 1–14 (2022). https://doi.org/10.1038/s41598-022-24133-5
Acknowledgments
We thank The Bombay Textile Research Association (BTRA, Mumbai) for support in synthesizing and characterizing nanofibers, utilizing the Nanospider facility and SEM analysis. We also extend our appreciation to DST-FIST Analytical Instrumentation Laboratory, Jaysingpur College Jaysingpur, Sophisticated Analytical Instrument Facilities (DST- CFC) Shivaji University, Kolhapur for providing characterization facilities BET, ATR-FTIR, TGA-DSC.
Author information
Authors and Affiliations
Contributions
The list of authors for this paper and their respective contributions is as follows: PDJ (Corresponding Author)—Conceptualization, Methodology, Formal Analysis, Data Curation, Investigation, Writing—Original Draft. Prof. (Dr.) MYG (co-author)—Validation, Resources, Supervision. We (the corresponding author and co-author) confirm that, to our knowledge, all the claims, statements, and conclusions are true and are our jointly held opinions. We confirm that the manuscript has been approved by all named authors and that there are no other persons who satisfied the criteria for authorship but are not listed.
Corresponding author
Ethics declarations
Competing interests
We wish to confirm that we have no known competing financial interests or personal relationships that could have appeared to influence the work. No funding was received for this work.
Ethical approval
Not applicable.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Supplementary Information
Below is the link to the electronic supplementary material.
Rights and permissions
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.
About this article
Cite this article
Jinde, P.D., Gudiyawar, M.Y. Synthesis, characterization, and thermal behavior of silica aerogel-embedded PVDF-HFP nanofibers. Journal of Materials Research 39, 1396–1410 (2024). https://doi.org/10.1557/s43578-024-01317-5
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1557/s43578-024-01317-5