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Uniform pore structure silica aerogel powders prepared by pore repair method

  • Original Paper: Nano-structured materials (particles, fibers, colloids, composites, etc.)
  • Published:
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Abstract

Nowadays, the rapid preparation of silica aerogel powders by ambient pressure drying (APD) method has been widely studied. However, the internal pore structures of the aerogel powders prepared by the conventional rapid aging method (CM) are difficult to be controlled due to the increase in the particle agglomeration and the macropores structure. In this research, a rapid way was introduced to control the microstructure of the silica aerogel powders through pore repairing (PR) method in the aging process. The bulk gel and gel particles were double aged to enhance the skeleton structure of gel particles. The new silica nanoparticles were formed, and filled in the macropores of gel particles by adhesion or deposition in the networks of gel particles during the late ageing process, the pore structure in the gel particles were uniform within just 2 h of aging. Under optimal ageing conditions, silica aerogel powders with low density (0.089 g/cm3), low thermal conductivity (0.0243 W/m K) and high specific surface (882 m2/g) was obtained through the pore repairing method. Pore repairing method in the aging process has certain research significance to control the pore structure of aerogel powders.

Graphical Abstract

Graphical abstract shows the schematic illustration of the silica aerogel powders preparation process by pore repairing method. In the pore repairing method, the block gel was formed by mixing silica sol and ethanol solution under basic condition. After a short period of preliminary aging in the aging liquid prepared by mixing with ethanol and tetraethoxysilane, the silica network structure with certain strength was formed in the block gel. Then, the preliminary aged block gel was mechanically crushed into a number of gel particles, and the gel particles were put into the aging liquid to further age. The new generated silica nanoparticles in the aging liquid can fill the macropore of gel particles by deposition on the networks of silica aggregates or form new Si–O–Si cross-linking structures via condensation between hydroxyl groups or hydrogen bonding interaction to obtain the repaired gel particles.

Highlights

  • The study of controlling the pore size distribution of silica aerogel powder was discussed for the first time.

  • The pore repairing method endows the silica aerogel powder with uniform pore structure.

  • The pore structure in the gel particles were uniform within just 2 h of aging.

  • The thermal conductivities experiences were decreased from 0.0301 W/m·k to 0.0243 W/m·k, which is attributed to the macropore reduced.

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References

  1. Antonietti M, Fechler N, Fellinger T-P (2013) Carbon aerogels and monoliths: control of porosity and nanoarchitecture via sol–gel routes. Chem Mater 26:196–210

    Article  Google Scholar 

  2. Pisal AA, Rao AV (2016) Comparative studies on the physical properties of TEOS, TMOS and Na2SiO3 based silica aerogels by ambient pressure drying method. J Porous Mater 23:1547–1556

    Article  CAS  Google Scholar 

  3. Sarawade PB, Kim J-K, Hilonga A, Kim HT (2010) Production of low-density sodium silicate-based hydrophobic silica aerogel beads by a novel fast gelation process and ambient pressure drying process. Solid State Sci 12:911–918

    Article  CAS  Google Scholar 

  4. Yun S, Luo H, Gao Y (2014) Superhydrophobic silica aerogel microspheres from methyltrimethoxysilane: rapid synthesis via ambient pressure drying and excellent absorption properties. RSC Adv 4:4535–4542

    Article  CAS  Google Scholar 

  5. Afşin Kariper İ (2020) Effect of acids on thermal insulation of solid powder silica aerogels. Ceram Int 46:8669–8674

    Article  Google Scholar 

  6. Schultz J, Jensen K, Kristiansen F (2005) Super insulating aerogel glazing. Sol Energy Mater Sol Cells 89:275–285

    Article  CAS  Google Scholar 

  7. 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

    Article  CAS  Google Scholar 

  8. Katti A, Shimpi N, Roy S, Lu H, Fabrizio EF, Dass A, Capadona LA, Leventis N (2006) Chemical, physical, and mechanical characterization of isocyanate cross-linked amine-modified silica aerogels. Chem Mater 18:285–296

    Article  CAS  Google Scholar 

  9. Capadona LA, Meador MAB, Alunni A, Fabrizio EF, Vassilaras P, Leventis N (2006) Flexible, low-density polymer crosslinked silica aerogels. Polymer 47:5754–5761

    Article  CAS  Google Scholar 

  10. Zu G, Kanamori K, Wang X, Nakanishi K, Shen J (2020) Superelastic triple-network polyorganosiloxane-based aerogels as transparent thermal superinsulators and efficient separators. Chem Mater 32:1595–1604

    Article  CAS  Google Scholar 

  11. Huang Y, He S, Feng M, Dai H, Pan Y, Cheng X (2019) Organic solvent-saving preparation of water glass based aerogel granules under ambient pressure drying. J Non Cryst Solids 521:119507

  12. Bhagat SD, Kim Y-H, Moon M-J, Ahn Y-S, Yeo J-G (2007) A cost-effective and fast synthesis of nanoporous SiO2 aerogel powders using water-glass via ambient pressure drying route. Solid State Sci 9:628–635

    Article  CAS  Google Scholar 

  13. Iswar S, Snellings GMBF, Zhao S, Erni R, Bahk YK, Wang J, Lattuada M, Koebel MM, Malfait WJ (2018) Reinforced and superinsulating silica aerogel through in situ cross-linking with silane terminated prepolymers. Acta Mater 147:322–328

    Article  CAS  Google Scholar 

  14. Stojanovic A, Zhao S, Angelica E, Malfait WJ, Koebel MM (2019) Three routes to superinsulating silica aerogel powder. J Sol Gel Sci Technol 90:57–66

    Article  CAS  Google Scholar 

  15. Iswar S, Malfait WJ, Balog S, Winnefeld F, Lattuada M, Koebel MM (2017) Effect of aging on silica aerogel properties. Microporous Mesoporous Mater 241:293–302

    Article  CAS  Google Scholar 

  16. Zhao S, Stojanovic A, Angelica E, Emery O, Rentsch D, Pauer R, Koebel MM, Malfait WJ (2020) Phase transfer agents facilitate the production of superinsulating silica aerogel powders by simultaneous hydrophobization and solvent- and ion-exchange. Chem Eng J 381:122421

  17. Bhagat SD, Rao AV (2006) Surface chemical modification of TEOS based silica aerogels synthesized by two step (acid–base) sol–gel process. Appl Surf Sci 252:4289–4297

    Article  CAS  Google Scholar 

  18. Hilonga A, Kim J-K, Sarawade PB, Quang DV, Shao GN, Elineema G, Kim HT (2012) Two-step rapid synthesis of mesoporous silica for green tire. Korean J Chem Eng 29:1643–1646

    Article  CAS  Google Scholar 

  19. Shewale PM, Venkateswara Rao A, Parvathy Rao A, Bhagat SD (2009) Synthesis of transparent silica aerogels with low density and better hydrophobicity by controlled sol–gel route and subsequent atmospheric pressure drying. J Sol Gel Sci Technol 49:285–292

    Article  CAS  Google Scholar 

  20. Lesov I, Tcholakova S, Kovadjieva M, Saison T, Lamblet M, Denkov N (2017) Role of Pickering stabilization and bulk gelation for the preparation and properties of solid silica foams. J Colloid Interface Sci 504:48–57

    Article  CAS  Google Scholar 

  21. Estella J, Echeverría JC, Laguna M, Garrido JJ (2007) Effects of aging and drying conditions on the structural and textural properties of silica gels. Microporous Mesoporous Mater 102:274–282

    Article  CAS  Google Scholar 

  22. Woignier T, Phalippou J (1988) Mechanical strength of silica aerogels. J Non Cryst Solids 100:404–408

    Article  CAS  Google Scholar 

  23. Sarawade PB, Kim J-K, Hilonga A, Kim HT (2010) Influence of aging conditions on textural properties of water-glass-based silica aerogels prepared at ambient pressure. Korean J Chem Eng 27:1301–1309

    Article  CAS  Google Scholar 

  24. Xia T, Yang H, Li J, Sun C, Lei C, Hu Z, Zhang Y (2019) Tailoring structure and properties of silica aerogels by varying the content of the Tetramethoxysilane added in batches. Microporous Mesoporous Mater 280:20–25

    Article  CAS  Google Scholar 

  25. Lei C, Li J, Sun C, Yang H, Xia T, Hu Z, Zhang Y (2018) Transparent, elastic and crack-free polymethylsilsesquioxane aerogels prepared by controllable shrinkage of the hydrogels in the aging process. Microporous Mesoporous Mater 267:107–114

    Article  CAS  Google Scholar 

  26. Xia T, Yang H, Li J, Sun C, Lei C, Hu Z, Zhang Y (2019) Synthesis and physicochemical characterization of silica aerogels by rapid seed growth method. Ceram Int 45:7071–7076

    Article  CAS  Google Scholar 

  27. Schwertfeger F, Frank D, Schmidt M (1998) Hydrophobic waterglass based aerogels without solvent exchange or supercritical drying. J Non Cryst Solids 225:24–29

    Article  CAS  Google Scholar 

  28. Saeed S, Al Soubaihi RM, White LS, Bertino MF, Saoud KM (2016) Rapid fabrication of cross-linked silica aerogel by laser induced gelation. Microporous Mesoporous Mater 221:245–252

    Article  CAS  Google Scholar 

  29. Wang J, Zhang Y, Wei Y, Zhang X (2015) Fast and one-pot synthesis of silica aerogels via a quasi-solvent-exchange-free ambient pressure drying process. Microporous Mesoporous Mater 218:192–198

    Article  CAS  Google Scholar 

  30. Pan Y, He S, Cheng X, Li Z, Li C, Huang Y, Gong L (2017) A fast synthesis of silica aerogel powders-based on water glass via ambient drying. J Sol Gel Sci Technol 82:594–601

    Article  CAS  Google Scholar 

  31. Huber L, Zhao S, Malfait WJ, Vares S, Koebel MM (2017) Fast and minimal-solvent production of superinsulating silica aerogel granulate. Angew Chem Int Ed Engl 56:4753–4756

    Article  CAS  Google Scholar 

  32. Tillotson TM, Hrubesh LW (1992) Transparent ultralow-density silica aerogels prepared by a two-step sol-gel process. J Non Cryst Solids 145:44–50

    Article  CAS  Google Scholar 

  33. Liu R, Wang J, Du Y, Liao J, Zhang X (2019) Phase-separation induced synthesis of superhydrophobic silica aerogel powders and granules. J Solid State Chem 279:120971

  34. Cho H, Jin KS, Lee J, Lee KH (2018) Estimation of degree of polymerization of poly-acrylonitrile-grafted carbon nanotubes using Guinier plot of small angle x-ray scattering. Nanotechnology 29:9

    Article  Google Scholar 

  35. Lei C, Hu Z, Zhang Y, Yang H, Li J, Hu S (2018) Tailoring structural and physical properties of polymethylsilsesquioxane aerogels by adjusting NH3·H2O concentration. Microporous Mesoporous Mater 258:236–243

    Article  CAS  Google Scholar 

  36. Lei Y, Chen X, Hu Z, Song H, Cao B (2017) A general strategy for improving the thermal insulation performance of aerogels by multiple impregnation. Scr Mater 139:5–8

    Article  CAS  Google Scholar 

  37. Lamy-Mendes A, Girao AV, Silva RF, Duraes L (2019) Polysilsesquioxane-based silica aerogel monoliths with embedded CNTs. Microporous Mesoporous Mater 288:12

    Article  Google Scholar 

  38. Bangi UKH, Jung I-K, Park C-S, Baek S, Park H-H (2013) Optically transparent silica aerogels based on sodium silicate by a two step sol–gel process and ambient pressure drying. Solid State Sci 18:50–57

    Article  CAS  Google Scholar 

  39. Feng J, Feng J, Zhang C (2011) Shrinkage and pore structure in preparation of carbon aerogels. J Sol Gel Sci Technol 59:371–380

    Article  CAS  Google Scholar 

  40. Balzer C, Wildhage T, Braxmeier S, Reichenauer G, Olivier JP (2011) Deformation of porous carbons upon adsorption. Langmuir 27:2553–2560

    Article  CAS  Google Scholar 

  41. 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

    Article  CAS  Google Scholar 

  42. Rosenberg OS, Deindl S, Sung R-J, Nairn AC, Kuriyan J (2005) Structure of the autoinhibited kinase domain of CaMKII and SAXS analysis of the holoenzyme. Cell 123:849–860

    Article  CAS  Google Scholar 

  43. Duda DM, Borg LA, Scott DC, Hunt HW, Hammel M, Schulman BA (2008) Structural insights into NEDD8 activation of Cullin-RING ligases: conformational control of conjugation. Cell 134:995–1006

    Article  CAS  Google Scholar 

  44. Borgia A, Zheng WW, Buholzer K, Borgia MB, Schuler A, Hofmann H, Soranno A, Nettels D, Gast K, Grishaev A, Best RB, Schuler B (2016) Consistent view of polypeptide chain expansion in chemical denaturants from multiple experimental methods. J Am Chem Soc 138:11714–11726

    Article  CAS  Google Scholar 

  45. Xian-lang Q, Min Y, Hong L, Jia-wen X, Mu-su R, Jin-liang S (2022) Optimized preparation of thermal insulation hydrophobic SiO2 aerogel based on orthogonal design method. J Porous Mater 29:1027–1037

    Article  Google Scholar 

  46. Zhao C, Li Y, Ye W, Shen X, Yuan X, Ma C, Cao Y (2021) Performance regulation of silica aerogel powder synthesized by a two-step sol-gel process with a fast ambient pressure drying route. J Non Cryst Solids 567:120923

  47. Rudaz C, Courson R, Bonnet L, Calas-Etienne S, Sallee H, Budtova T (2014) Aeropectin: fully biomass-based mechanically strong and thermal superinsulating aerogel. Biomacromolecules 15:2188–2195

    Article  CAS  Google Scholar 

  48. Wu S, Du A, Xiang Y, Liu M, Li T, Shen J, Zhang Z, Li C, Zhou B (2016) Silica-aerogel-powders “jammed” polyimide aerogels with excellent hydrophobicity and conversion to ultra-light polyimide aerogel. RSC Adv 6:58268–58278

    Article  CAS  Google Scholar 

  49. Rettelbach T, Säuberlich J, Korder S, Fricke J (1995) Thermal conductivity of silica aerogel powders at temperatures from 10 to 275 K. J Non Cryst Solids 186:278–284

    Article  CAS  Google Scholar 

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Acknowledgements

Thanks to Shanghai Synchrotron Radiation Facility for its supporting.

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Authors and Affiliations

  1. Engineering Research Center for Eco-Dyeing and Finishing of Textiles, Zhejiang Sci-Tech University, Hangzhou, 310018, Zhejiang, China

    Chao Li, Shanli Wang, Licong Xu & Minghua Wu

  2. Key Laboratory of Advanced Textile Materials and Manufacturing Technology, Ministry of Education, College of Textile Science and Engineering, Zhejiang Sci-Tech University, Hangzhou, 310018, Zhejiang, China

    Chao Li, Shanli Wang, Hao Zhang, Licong Xu & Minghua Wu

  3. Zhejiang Kaide Chemical Co. Ltd, Hangzhou, 310018, Zhejiang, China

    Yumei He

  4. Zhejiang Provincial Engineering Research Center for Green and Low-carbon Dyeing & Finishing, Zhejiang Sci-Tech University, Hangzhou, 310018, Zhejiang, China

    Minghua Wu

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  1. Chao Li
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  3. Shanli Wang
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  4. Hao Zhang
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Contributions

CL: performing the experiments, data curation, formal analysis, writing—original draft, writing—review and editing. YH: data curation, formal analysis, investigation. SW: data curation, formal analysis, investigation. HZ: data curation, formal analysis, investigation. LX: data curation, formal analysis, investigation. MW: formal analysis, writing—original draft, writing—review and editing.

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Correspondence to Minghua Wu.

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Li, C., He, Y., Wang, S. et al. Uniform pore structure silica aerogel powders prepared by pore repair method. J Sol-Gel Sci Technol 106, 715–725 (2023). https://doi.org/10.1007/s10971-023-06088-9

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