Abstract
The biocompatibility of calcined silica aerogel (900 °C) synthesized from rice husk ash via sol–gel ambient-pressure drying technique was studied. The silica aerogel was characterized by Fourier transform infrared spectroscopy, X-ray diffraction and field emission-scanning electron microscopy. The structure of silica aerogel remains intact but is deficient in silanol groups after calcination. The bioactivity of the silica aerogel was tested by immersion in simulated body fluid for 7 days with various mass concentrations (0.08–0.8 wt%). The results from Fourier transform infrared, X-ray diffraction, field emission-scanning electron microscopy and phosphorous analyses confirm that the silica aerogel could facilitate the nucleation of apatite. The silica aerogel was simultaneously resorbed and the broken Si–O–Si bonds were replaced with new apatite bonds. The optimal mass concentration was 0.16 wt%. At a higher mass concentration (0.8 wt%), silica aerogel tends to form polymeric interactions with tris-hydroxymethyl-aminomethane, a chemical compound in simulated body fluid. In the in vitro cell viability assay of the calcined silica aerogel against human dermal fibroblast cells, the cell viability increased with the increase of silica aerogel mass concentration. This early evidence shows that the calcined silica aerogel synthesized from rice husk ash via the sol–gel ambient-pressure drying technique can be considered as a potential alternative material for tissue engineering applications.
Graphical Abstract

This is a preview of subscription content,
to check access.







References
Ciriminna R, Fidalgo A, Pandarus V, Béland F, Ilharco LM, Pagliaro M (2013) The sol–gel route to advanced silica-based materials and recent applications. Chem Rev 113(8):6592–6620
Huang Y, Niu JL (2015) Application of super-insulating translucent silica aerogel glazing system on commercial building envelope of humid subtropical climates—impact on space cooling load. Energy 83:316–325
Mabrouk M, Selim MM, Beherei H, El-Gohary MI (2012) Effect of incorporation of nano bioactive silica into commercial glass ionomer cement (GIC). J Genet Eng Biotechnol 10(1):113–119
Seleem MN, Munusamy P, Ranjan A, Alqublan H, Pickrell G, Sriranganathan N (2009) Silica-antibiotic hybrid nanoparticles for targeting intracellular pathogens. Antimicrob Agents Chemother 53(10):4270–4274
Wang X, Ben Ahmed N, Alvarez GS, Tuttolomondo MV, Hélary C, Desimone MF, Coradin T (2015) Sol–gel encapsulation of biomolecules and cells for medicinal applications. Curr Top Med Chem 15(3):223–244
Yousefi Amiri T, Moghaddas J (2015) Cogeled copper–silica aerogel as a catalyst in hydrogen production from methanol steam reforming. Int J Hydrog Energy 40(3):1472–1480
Yang K-N, Zhang C-Q, Wang W, Wang PC, Zhou J-P, Liang X-J (2014) pH-responsive mesoporous silica nanoparticles employed in controlled drug delivery systems for cancer treatment. Cancer Biol Med 11(1):34–43
Godec A, Maver U, Bele M, Planinšek O, Srčič S, Gaberšček M, Jamnik J (2007) Vitrification from solution in restricted space: formation and stabilization of amorphous nifedipine in a nanoporous silica xerogel carrier. Int J Pharm 343(1–2):131–140
Baek SM, Singh R, Khanal D, Patel KD, Lee E-J, Leong KW, Chrzanowski W, Kim H-W (2015), Smart multifunctional drug delivery towards anticancer therapy harmonized in mesoporous nanoparticles. Nanoscale 7:14191–14216.
Walia S, Acharya A (2015) Silica micro/nanospheres for theranostics: from bimodal MRI and fluorescent imaging probes to cancer therapy. Beilstein J Nanotechnol 6(1):546–558
Henstock JR, Canham LT, Anderson SI (2015) Silicon: the evolution of its use in biomaterials. Acta Biomater 11(1):17–26
Soleimani Dorcheh A, Abbasi MH (2008) Silica aerogel: synthesis, properties and characterization. J Mater Process Technol 199(1):10–26
Gurav JL, Jung I-K, Park H-H, Kang ES, Nadargi DY (2010) Silica aerogel: synthesis and applications. J Nanomater 2010:1–11
Venkateswara Rao A, Bhagat SD (2004) Synthesis and physical properties of TEOS-based silica aerogels prepared by two step (acid-base) sol–gel process. Solid State Sci 6(9):945–952
Toledo-Fernández JA, Mendoza-Serna R, Morales V, De La Rosa-Fox N, Piñero M, Santos A, Esquivias L (2008) Bioactivity of wollastonite/aerogels composites obtained from a TEOS-MTES matrix. J Mater Sci Mater Med 19(5):2207–2213
Carlson G, Lewis D, McKinley K, Richardson J, Tillotson T (1995) Aerogel commercialization: technology, markets and costs. J Non Cryst Solids 186:372–379
He S, Huang D, Bi H, Li Z, Yang H, Cheng X (2015) Synthesis and characterization of silica aerogels dried under ambient pressure bed on water glass. J Non Cryst Solids 410:58–64
Cai H, Sharma S, Liu W, Mu W, Liu W, Zhang X, Deng Y (2014) Aerogel microspheres from natural cellulose nanofibrils and their application as cell culture scaffold. Biomacromolecules 15:2540–2547
Mallepally RR, Marin MA, Surampudi V, Subia B, Rao RR, Kundu SC, McHugh MA (2015) Silk fibroin aerogels: potential scaffolds for tissue engineering applications. Biomed Mater 10(3):35002
Ding B, Cai J, Huang J, Zhang L, Chen Y, Shi X, Du Y, Kuga S (2012) Facile preparation of robust and biocompatible chitin aerogels. J Mater Chem 22(12):5801
Lu T, Li Q, Chen W, Yu H (2014) Composite aerogels based on dialdehyde nanocellulose and collagen for potential applications as wound dressing and tissue engineering scaffold. Compos Sci Technol 94:132–138
Salinas AJ, Maria VR, José ATF, Roberto MS, Piñero M, Esquivias L, Julio RC, José MGC (2009) Nanostructure and bioactivity of hybrid aerogels. Chem Mater 21(1):41–47
Martins M, Barros AA, Quraishi S, Gurikov P, Raman SP, Smirnova I, Duarte ARC, Reis RL (2015) Preparation of macroporous alginate-based aerogels for biomedical applications. J Supercrit Fluids 106:152–159
Stergar J, Maver U (2016) Review of aerogel-based materials in biomedical applications. J Sol Gel Sci Technol 77(3):738–752
Schneider M, Stracke F, Hansen S, Schaefer UF (2009) Nanoparticles and their interactions with the dermal barrier. Dermatoendocrinol 1(4):197–206
Alshatwi AA, Athinarayanan J, Periasamy VS (2015) Biocompatibility assessment of rice husk-derived biogenic silica nanoparticles for biomedical applications. Mater Sci Eng C 47:8–16
Hamdan H, Muhid MNM, Endud S, Listiorini E, Ramli Z (1997) 29Si MAS NMR, XRD and FESEM studies of rice husk silica for the synthesis of zeolites. J Non Cryst Solids 211(1–2):126–131
Kokubo T, Takadama H (2006) How useful is SBF in predicting in vivo bone bioactivity? Biomaterials 27(15):2907–2915
Van Kooten TG, Klein CL, Otto M (1998) Current trends in biocompatibility testing. Proc Inst Mech Eng 212:75–84
Aminian A, Solati-Hashjin M, Samadikuchaksaraei A, Bakhshi F, Gorjipour F, Farzadi A, Moztarzadeh F, Schmücker M (2011) Synthesis of silicon-substituted hydroxyapatite by a hydrothermal method with two different phosphorous sources. Ceram Int 37(4):1219–1229
Blagosklonny MV, El-Deiry WS (1996) In vitro evaluation of A P53-expressing adenovirus as an anti-cancer drug. Int J Cancer 67(3):386–392
Avelar-Freitas BA, Almeida VG, Pinto MCX, Mourão FAG, Massensini AR, Martins-Filho OA, Rocha-Vieira E, Brito-Melo GEA (2014) Trypan blue exclusion assay by flow cytometry. Braz J Med Biol Res 47(4):307–315
Altman S, Randers L, Rao G (1999) Comparison of trypan blue dye exclusion and fluorometric assays for mammalian cell viability determinations. Biotechnol Prog 9:671–674
Xian W, (2009) A laboratory course in biomaterials. CRC Press. Boca Raton, Florida, US. pp. 99–128
Boinski F, Khouchaf L, Tuilier MH (2010) Study of the mechanisms involved in reactive Silica. Mater Chem Phys 122(1):311–315
Athinarayanan J, Periasamy VS, Alhazmi M, Alatiah KA, Alshatwi AA (2014) Synthesis of biogenic silica nanoparticles from rice husks for biomedical applications. Ceram Int 41(1):275–281
Nayak JP, Bera J (2009) Preparation of silica aerogel by ambient pressure drying process using rice husk Ash as raw material. Trans Indian Ceram Soc 68(2):1–4
Bhagat SD, Kim YH, Ahn YS, Yeo JG (2006) Textural properties of ambient pressure dried water-glass based silica aerogel beads: one day synthesis. Microporous Mesoporous Mater 96(1–3):237–244
Sani S, Mohd Muhid MN, Hamdan H (2011) Design, synthesis and activity study of tyrosinase encapsulated silica aerogel (TESA) biosensor for phenol removal in aqueous solution. J Sol Gel Sci Technol 59(1):7–18
de Oliveira AAR, de Souza DA, Dias LLS, de Carvalho SM, Mansur HS, de Magalhães Pereira M (2013) Synthesis, characterization and cytocompatibility of spherical bioactive glass nanoparticles for potential hard tissue engineering applications. Biomed Mater 8(2):25011
Shi F, Wang L, Liu J (2006) Synthesis and characterization of silica aerogels by a novel fast ambient pressure drying process. Mater Lett 60(29–30):3718–3722
Zhang Y, Hu L, Yu D, Gao C (2010) Influence of silica particle internalization on adhesion and migration of human dermal fibroblasts. Biomaterials 31(32):8465–8474
Reséndiz-Hernández PJ, Cortés-Hernández DA, Méndez Nonell J, Escobedo-Bocardo JC (2014) Bioactive and biocompatible silica/pseudowollastonite aerogels. Adv Sci Technol 96:21–26
Hayakawa S, Kanaya T, Tsuru K, Shirosaki Y, Osaka A, Fujii E, Kawabata K, Gasqueres G, Bonhomme C, Babonneau F, Jäger C, Kleebe H (2013) Heterogeneous structure and in vitro degradation behavior of wet-chemically derived nanocrystalline silicon-containing hydroxyapatite particles. Acta Biomater 9(1):4856–4867
Rehman I, Bonfield W (1997) Characterization of hydroxyapatite and carbonated apatite by photo acoustic FTIR spectroscopy. J Mater Sci Mater Med 8(1):1–4
Guo X, Xiao P (2006) Effects of solvents on properties of nanocrystalline hydroxyapatite produced from hydrothermal process. J Eur Ceram Soc 26:3383–3391
Fontinha IR, Salta MM, Zheludkevich ML, Ferreira MGS (2013) EIS study of amine cured epoxy-silica-zirconia sol–gel coatings for corrosion protection of the aluminium alloy EN AW 6063. Port Electrochim Acta 31(6):307–319
Zhang G, Dass A, Rawashdeh AMM, Thomas J, Counsil JA, Sotiriou-Leventis C, Fabrizio EF, Ilhan F, Vassilaras P, Scheiman DA, McCorkle L, Palczer A, Johnston JC, Meador MA, Leventis N (2004) Isocyanate-crosslinked silica aerogel monoliths: preparation and characterization. J Non Cryst Solids 350:152–164
Ulker Z, Erkey C (2014) An emerging platform for drug delivery: aerogel based systems. J Control Release 177(1):51–63
Wang Z, Wang D, Qian Z, Guo J, Dong H, Zhao N, Xu J (2015) Robust superhydrophobic bridged silsesquioxane aerogels with tunable performances and their applications. ACS Appl Mater Interfaces 7(3):2016–2024
Naghizadeh F, Abdul Kadir MR, Doostmohammadi A, Roozbahani F, Iqbal N, Taheri MM, Naveen SV, Kamarul T (2015) Rice husk derived bioactive glass-ceramic as a functional bioceramic: synthesis, characterization and biological testing. J Non Cryst Solids 427:54–61
Lu X, Leng Y (2005) Theoretical analysis of calcium phosphate precipitation in simulated body fluid. Biomaterials 26(10):1097–1108
Li P, Ohtsuki C, Kokubo T, Nakanishi K, Soga N, de Groot K (1994) The role of hydrated silica, titania, and alumina in inducing apatite on implants. J Biomed Mater Res 28(1):7–15. Jan
Li T, Wang T (2008) Preparation of silica aerogel from rice hull ash by drying at atmospheric pressure. Mater Chem Phys 112(2):398–401
Andersson ÖH, Karlsson KH (1991) On the bioactivity of silicate glass. J Non Cryst Solids 129(1–3):145–151
Pierre AC, Pajonk M (2002) Chemistry of aerogels and their applications. Chem Rev 102:4243–4265
Pei X, Zhai W, Zheng W (2015) Preparation of poly (aryl ether ketone ketone)–silica composite aerogel for thermal insulation application. J Sol Gel Sci Technol 76(1):98–109
Mad Jin R, Sultana N, Baba S, Hamdan S, Ismail AF (2015), Porous PCL/chitosan and nHA/PCL/chitosan scaffolds for tissue engineering applications: fabrication and evaluation. J Nanomater. Article ID 357372:1–8
Mohd Daud N, Sing NB, Yusop AH, Abdul Majid FA, Hermawan H (2014) Degradation and in vitro cell–material interaction studies on hydroxyapatite-coated biodegradable porous iron for hard tissue scaffolds. J Orthop Transl 2(4):177–184
Maury S, Buisson P, Perrard A, Pierre AC (2004) Influence of the sol–gel chemistry on the activity of a lipase encapsulated in a silica aerogel. J Mol Catal B 29(1–6):133–148
Fruijtier-Pölloth C (2012) The toxicological mode of action and the safety of synthetic amorphous silica-A nanostructured material. Toxicology 294(2–3):61–79
Acknowledgments
The authors would like to thank the Ministry of Education, Malaysia and Universiti Teknologi Malaysia (UTM) for financially supporting this research work under the Fundamental Research Grant Scheme (FRGS, Vot No: 4F514).
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no competing interests.
Rights and permissions
About this article
Cite this article
Sani, N.S., Malek, N.A.N.N., Jemon, K. et al. Effect of mass concentration on bioactivity and cell viability of calcined silica aerogel synthesized from rice husk ash as silica source. J Sol-Gel Sci Technol 82, 120–132 (2017). https://doi.org/10.1007/s10971-016-4266-y
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10971-016-4266-y