FABRICATION OF TERNARY SILICA-CALCIUM-MAGNESIUM AEROGELS: EFFECT OF FEEDING RATE AND MOLAR RATIO ON PROPERTIES

Year 2023, Volume: 11 Issue: 4, 905 - 915, 01.12.2023

Burcu Karakuzu İkizler , Pınar Terzioğlu , Tülay Merve Temel Soylu , Sevil Yücel

https://doi.org/10.36306/konjes.1260218

Abstract

The silica-calcium-magnesium ternary aerogels were prepared by a solvent exchange method and a subsequent ambient pressure drying process. The effect of process parameters such as feeding rate (9-70 mL.min-1) and molar ratio (Si/(Ca:Mg) = 1:1 - 3:1) on the material characteristics including density, elemental content, surface area, pore size, pore volume, and morphology of powders were investigated. Aerogels were characterized by Fourier transform infrared spectroscopy (FTIR), inductively coupled plasma optical emission spectroscopy (ICP-OES), scanning electron microscopy (SEM), Brunauer–Emmett–Teller (BET), Barrett–Joiner–Halenda (BJH) and tapping density analysis. It was found that the molar ratio of Si/(Ca:Mg) could remarkably affect the surface area and density of aerogels, while the feeding rate had slight effect. The resultant aerogels exhibited high specific surface areas. The results showed that the aerogel has a Si/(Ca:3Mg) molar composition obtained with 9 mL.min-1 had the highest surface area (524 m2.g−1). The increase of Ca to Mg molar ratio caused a decrease in the surface area and density of samples. The resultant aerogels are promising candidates as adsorbents to remove various contaminants.

Keywords

Ambient pressure drying, Co-doped silica, Pore structure, Structural evolution, Ternary aerogel

Supporting Institution

TÜBİTAK 1005

Project Number

115M469

Thanks

This work was supported by the TUBITAK (The Scientific and Technological Research Council of Turkey) a 1005 project (Project No: 115M469).

References

• T. Zhou, X. Cheng, Y. Pan, C. Li, L. Gong, and H. Zhang, “Mechanical performance and thermal stability of glass fiber reinforced silica aerogel composites based on co-precursor method by freeze drying,” Applied Surface Science, vol. 437, pp. 321–328, 2018.
• F. Pan, B. Zhang, Y. Ding, L. Wang, F. Xie, W. Cai, S. Liu, and J. Zhou, “New composite aerogel-like adsorbents for thiophene based on π-complexation,” Separation and Purification Technology, 192, pp. 46–54, 2018.
• T. M. Temel, B. K. İkizler, P. Terzioğlu, S. Yücel, and Y. B. Elalmış, “The effect of process variables on the properties of nanoporous silica aerogels: an approach to prepare silica aerogels from biosilica,” Journal of Sol-Gel Science and Technology, vol. 84, no. 1, pp. 51–59, Jul. 2017.
• J. L. Mohanan and S. L. Brock, “Influence of Synthetic and Processing Parameters on the Surface Area, Speciation, and Particle Formation in Copper Oxide/Silica Aerogel Composites,” Chemistry of Materials, vol. 15, no. 13, pp. 2567–2576, May 2003.
• C. Zhao, Y. Li, W. Ye, X. Shen, X. Yuan, C. Ma, and Y. Cao, “Performance regulation of silica aerogel powder synthesized by a two-step Sol-gel process with a fast ambient pressure drying route,” Journal of Non-Crystalline Solids, vol. 567, pp.120923, Sep 2021.
• X. Wu, G. Shao, S. Cui, L. Wang, and X. Shen, “Synthesis of a novel Al2O3–SiO2 composite aerogel with high specific surface area at elevated temperatures using inexpensive inorganic salt of aluminum,” Ceramics International, vol. 42, no. 1, Part A, pp. 874–882, Jan. 2016.
• X. Hou, R. Zhang, and D. Fang, “Novel whisker-reinforced Al2O3–SiO2 aerogel composites with ultra-low thermal conductivity,” Ceramics International, vol. 43, no. 12, pp. 9547–9551, Aug. 2017.
• J. Yao, X. Gao, Y. Wu, X. Zhao, and X. Li, “High-temperature resistant ambient pressure-dried aluminum doped silica aerogel from inorganic silicon and aluminum sources.” Ceramics International, vol. 48, pp.15006-15016, Jun. 2022.
• S. Zhang, Z. Zhang, J. Pei, R. Li, J. Zhang, J. Cai, and J. Cui, “A novel TiO2-SiO2 aerogel nanocomposite absorbent: preparation, characterization and photocatalytic degradation effects on automobile exhaust,” Materials Research Express, vol. 5, no. 2, p. 025036, Feb. 2018.
• W. Zou, H. Bian, J. Guo, J. Xu and B. Guo, “Preparation of Titania–Silica Composite Aerogel at Atmospheric Pressure and Its Catalytic Performance in the Synthesis of Poly (Butylene Succinate)” Materials, vol 16, pp. 3296, Apr. 2023.
• G. Zu, J. Shen, L. Zou, W. Zou, D. Guan, Y. Wu, and Y. Zhang, “Highly thermally stable zirconia/silica composite aerogels prepared by supercritical deposition,” Microporous and Mesoporous Materials, vol. 238, pp. 90–96, Jan. 2017.
• Y. Han, Y. Wu, H. Zhang, S. Huang, S. Wu, and Z. Liang, “A three-dimensional network modifier (dimethyldiethoxysilane) makes ZrO2-SiO2 aerogel with excellent thermal insulation performance and high-temperature stability.” Colloids and Surfaces A: Physicochemical and Engineering Aspects, vol. 671, pp. 131716, Aug. 2023.
• L. M. Hair, P. R. Coronado, and J. G. Reynolds, “Mixed-metal oxide aerogels for oxidation of volatile organic compounds,” Journal of Non-Crystalline Solids, vol. 270, no. 1–3, pp. 115–122, May 2000.
• B. Karakuzu Ikizler, E. Yapıcı, S. Yucel, and E. Ermiş, “Production and Characterization of Calcium Silica Aerogel Powder as a Food Additive,” ACS omega, vol. 8, no.12, pp.11479-11491, March 2023.
• X. Wu, W. Li, G. Shao, X. Shen, S. Cui, J. Zhou, Y. Wei, and X. Chen, “Investigation on textural and structural evolution of the novel crack-free equimolar Al2O3-SiO2-TiO2 ternary aerogel during thermal treatment,” Ceramics International, vol. 43, no. 5, pp. 4188–4196, Apr. 2017.
• X. Li, G. Qin, Y. Wang, and W. Wei, “Preparation and characterization of equimolar SiO2–Al2O3–TiO2 ternary aerogel beads,” Journal of Porous Materials, vol. 21, no. 5, pp. 611–621, Apr. 2014.
• V. G. Parale, W. Han, H.N.R. Jung, K.Y. Lee, and H.H. Park, “Ambient pressure dried tetrapropoxysilane-based silica aerogels with high specific surface area,” Solid State Sciences, vol. 75, pp. 63–70, Jan. 2018.
• B. Karakuzu, T. M. Temel, S. Yücel, P. Terzi̇oğlu, and Y. Elalmiş, “Effect of Acid Type and Gelation pH on The Structural Properties of Silica Aerogels Prepared by Use of Rice Hull,” Sigma Journal of Engineering and Natural Sciences, vol. 34, no. 2, pp. 175–182, Jun. 2016.
• P. Terzioğlu, and S. Yucel, “Synthesis of Magnesium Silicate from Wheat Husk Ash,” Bioresources vol. 7, pp. 5435-5447, 2012.
• J.H. Lee, S.Y. Choi, C.E. Kim, and G.D. Kim, “The effects of initial sol parameters on the microstructure and optical transparency of TiO2–SiO2 binary aerogels,” Journal of Materials Science, vol. 32, no. 13, pp. 3577–3585, 1997.
• J. Chen, B. Zhang, G. Miao, and J. Men, “New SiO2–NiO Aerogel Sorbents for Desulfurization by π-Complexation: Influence of Molar Ratio of Si/Ni,” Industrial & Engineering Chemistry Research, vol. 55, no. 17, pp. 5036–5042, Apr. 2016.
• G. S. Pappas, P. Liatsi, I. A. Kartsonakis, I. Danilidis, and G. Kordas, “Synthesis and characterization of new SiO2–CaO hollow nanospheres by sol–gel method: Bioactivity of the new system,” Journal of Non-Crystalline Solids, vol. 354, no. 2, pp. 755–760, Jan. 2008.
• R. Akkari, A. Ghorbel, N. Essayem, and F. Figueras, “Synthesis and characterization of mesoporous silica-supported nano-crystalline sulfated zirconia catalysts prepared by a sol–gel process: Effect of the S/Zr molar ratio,” Applied Catalysis A: General, vol. 328, no. 1, pp. 43–51, Aug. 2007.
• F. He, L. Zhou, X. Zhang, W. Li, L. Yang, H. Zhao, and X. He, “Synthesis and anisotropic properties of alumina-silica aerogels constructed by silica sols infiltrated into unidirectional frozen alumina templates,” Ceramics International, vol. 45, no. 9, pp. 11963–11970, Jun. 2019.
• L. F. Posada, M. K. Carroll, A. M. Anderson, and B. A. Bruno, “Inclusion of Ceria in Alumina- and Silica-Based Aerogels for Catalytic Applications,” The Journal of Supercritical Fluids, vol. 152, p. 104536, Oct. 2019.
• H. Hu, N. Chen, W. Wei, H. Li, Z. Jiang, Y. Xu, and J. Xie, “The effect of solvent parameters on properties of iron-based silica binary aerogels as adsorbents,” Journal of Colloid and Interface Science, vol. 549, pp. 189–200, Aug. 2019.
• Z.G. Wu, Y.X. Zhao, and D.S. Liu, “The synthesis and characterization of mesoporous silica–zirconia aerogels,” Microporous and Mesoporous Materials, vol. 68, no. 1–3, pp. 127–132, Mar. 2004.