Extraction of high purity Nano-silicon from Quartz Sand by Metallothermic-reduction technique
DOI:
https://doi.org/10.31185/wjes.Vol14.Iss2.919Keywords:
Porous Silicon, Magnesiothermic Reduction, Chemical Leaching, NanoparticlesAbstract
This study presents an improved approach for extracting high-purity silicon nanoparticles using an enhanced thermal magnesium-aluminum reduction methodology. It lays the foundation for a systematic understanding and transformation of silicon, converting silica (SiO₂) particles into nanosilicon using an optimized aluminum-magnesium mixture for low-temperature silica reduction (a note of low-impact reduction) through a unique chemical treatment. The study employed a protocol of leaching with 4 N HCl followed by treatment with 2.5NNaOH. This was followed by reduction with an aluminum-magnesium mixture, and then a unique chemical treatment involving synergistic leaching and etching of the silicon nanoparticles, along with revitalization etching using a mixture of hydrofluoric and acetic acids. Using this protocol, high-purity silicon nanoparticles with interconnected porous networks were obtained after the complete removal of residual impurities (including methyl green, silicate residues, and other contaminants). Characterization techniques have confirmed the integrated nature of the structure and form of the extracted silicon. All the products were characterized using a field emission scanning electron microscope (FE-SEM), energy dispersive spectroscopy (EDS/EDX), and x-ray diffraction (XRD). The results showed that nanosilicon production had an average diameter of 49.8625 nm, 30.155, and 58.635 nm when extracted from S1, S2, and S3. Also, the XRD and FT-IR results confirm the high purity of the produced nanosilicon nanoparticles. Despite current challenges associated with producing large quantities of porous silicon nanomaterials using MTR technology, the modified thermochemical method offers a scalable, low-cost, high-throughput approach to manufacturing advanced silicon-based nanomaterials.
References
[1] Alonso Sanchez, P., Thangai, K., Oie, O. A., Gaarud, A., Rodriguez Gomez, M., Diadkin, V., Campo, J., Cova, F. H., & Blanco, M. V. (2025). Toward the Controlled Synthesis of Nanostructured Si and SiOx Anodes for Li-Ion Batteries via SiO2 Magnesiothermic Reduction Reaction. ACS Applied Energy Materials, *8*(4), 2249–2259. https://doi.org/10.1021/acsaem.4c02836
[2] Ajeel, S. A., Sukkar, K. A., & Zedin, N. K. (2021). "Evaluation of acid leaching process and calcination temperature on the silica extraction efficiency." Journal of Physics: Conf. Series, 1773, 012014. https://doi.org/10.1088/1742-6596/1773/1/012014
[3] Zuo, X., et al. (2017). "Silicon based lithium-ion battery anodes: A review." Journal of Materials Chemistry A, 5(26), 13188-13218. https://doi.org/10.1039/C7TA01398H
[4] Saeedi, M., et al. (2022). "Porous silicon as a drug carrier: Opportunities and challenges." Journal of Controlled Release, 341, 523-542. https://doi.org/10.1016/j.jconrel.2021.12.007
[5] Lin, N., et al. (2015). "Scalable synthesis of Si nanoparticles from low-cost sand." Angewandte Chemie, 127(31). https://doi.org/10.1002/ange.201503153
[6] Huang, Z., et al. (2011). "Metal-assisted chemical etching of silicon: A review." Advanced Materials, 23(2), 285-308. https://doi.org/10.1002/adma.201001784
[7] Pi, X., et al. (2016). "Silicon nanocrystals: Preparation, characterization, and applications." Journal of Nanomaterials. https://doi.org/10.1155/2016/9128504
[8] Entwistle, J., et al. (2018). "Magnesiothermic reduction of silica to cost-effective solar-grade silicon." Journal of Materials Chemistry A. https://doi.org/10.1039/C8TA00115K
[9] Zhang, R., et al. (2019). "Aluminothermic reduction of silica for the fabrication of porous silicon: A review." Materials Science in Semiconductor Processing, 93, 230-241. https://doi.org/10.1016/j.mssp.2019.01.011
[10] Wang, W., et al. (2013). "A heat-acceleration method to ignite magnesiothermic reduction for the synthesis of mesoporous Si." Chemical Communications, 49(80). https://doi.org/10.1039/C3CC45610A
[11] Liu, X., et al. (2021). "Recent advances in the metallothermic reduction of silica for lithium-ion battery anodes." Energy Storage Materials, 35, 12-32. https://doi.org/10.1016/j.ensm.2020.11.006
[12] Salonen, J., et al. (2008). "Mesoporous silicon in drug delivery applications." Journal of Pharmaceutical Sciences. https://doi.org/10.1002/jps.21054
[13] Priolo, F., et al. (2014). "Silicon nanostructures for photonics and photovoltaics." Nature Nanotechnology, 9(1). https://doi.org/10.1038/nnano.2013.271
[14] Ajeel, S. A., Sukkar, K. A., & Zedin, N. K. (2021). "Chemical Extraction Process for Producing High Purity Nanosilica from Iraqi Rice Husk." Engineering and Technology Journal, 39(01). https://doi.org/10.30684/etj.v39i1A.1696
[15] Tan, Y., Jiang, T., & Chen, G. Z. (2021). Mechanisms and Product Options of Magnesiothermic Reduction of Silica to Silicon for Lithium-Ion Battery Applications. Frontiers in Energy Research, *9*, 651386. https://doi.org/10.3389/fenrg.2021.651386
[16] Ajeel, S. A., Sukkar, K. A., & Zedin, N. K. (2020). "Extraction of High Purity Amorphous Silica from Rice Husk by Chemical Process." IOP Conf. Series: Materials Science and Engineering, 881, 012096. https://doi.org/10.1088/1757-899X/881/1/012096
[17] Entwistle, J., Rennie, A., & Patwardhan, S. (2018). A review of magnesiothermic reduction of silica to porous silicon for lithium-ion battery applications and beyond. Journal of Materials Chemistry A, *6*(38), 18344-18356. https://doi.org/10.1039/C8TA06370B
[18] Namus, R. M., Abass, M. H., Alali, M., & Zedin, N. K. (2024). "Using green corrosion inhibitor to reduce maintenance cost for carbon steel saline water storage systems." KOM – Corrosion and Material Protection Journal, 68, 43-50. https://doi.org/10.2478/kom-2024-0005
[19] Zedin, N. K., Ajeel, S. A., & Husseinc, S. S. (2025). "Cellulose nanofibers extracted from oat husk by thermochemical processes." AIP Conf. Proc., 3292, 030005. https://doi.org/10.1063/5.0264929
[20] Borisov, V. A., Kiselev, A. D., Kraidenko, R. I., & Malyutin, L. N. (2020). The production of silicon by magnesiothermic reduction of silicon dioxide. AIP Conference Proceedings, *2310*(1), 020048. https://doi.org/10.1063/5.0033077
[21] Zedin, N. K., Salman, R. A., & Jaber, A. A. (2022). "Extraction of Cellulose Nanoparticles via Modified Thermochemical Processes from Agricultural Wastes." IJASEIT, 12(2). https://doi.org/10.18517/ijaseit.12.2.15652
[22] Salman, R. A., & Zedin, N. K. (2021). "Effect Multiple Addition (TiO2 and Fly Ash) on Wear Behavior and Hardness of 2024 Al Alloy." Materials Science Forum, 1039, 201-208. https://doi.org/10.4028/www.scientific.net/MSF.1039.201
[23] Zedin, N. K., Ajeel, S. A., & Sukkar, K. A. (2020). "Nanosilicon Powder Extraction as a Sustainable Source (From Iraqi Rice husks) by Hydrothermal Process." AIP Conf. Proc., 2213, 020155. https://doi.org/10.1063/5.0000147
[24] Lai, Y., Thompson, J. R., & Dasog, M. (2018). Metallothermic Reduction of Silica Nanoparticles to Porous Silicon for Drug Delivery Using New and Existing Reductants. Chemistry – A European Journal, *24*(31), 7913-7920. https://doi.org/10.1002/chem.201705818
[25] Ajeel, S. A., Sukkar, K. A., & Zedin, N. K. (2021). "New magnesio-thermal reduction technique to produce high-purity crystalline nano-silicon via semi-batch reactor." Materials Today: Proceedings, 42, 1966-1972. https://doi.org/10.1016/j.matpr.2020.12.243
[26] Salman, R. A., Ajeel, S. A., & Zedin, N. K. (2020). "Influence of Sulphate and Chlorides Acidic Media on Mechanical and Corrosion Behavior." IOP Conf. Series: Materials Science and Engineering, 671, 012153. https://doi.org/10.1088/1757-899X/671/1/012153
[27] Haouli, S., Boudebane, S., Slipper, I. J., Lemboub, S., Gebara, P., & Mezrag, S. (2018). Combustion synthesis of silicon by magnesiothermic reduction. Phosphorus, Sulfur, and Silicon and the Related Elements, *193*(4), 280-287. https://doi.org/10.1080/10426507.2017.1416615
[28] Al-Razzaq, A. W. A., Ajeel, S. A., & Zedin, N. K. (2025). "Optimization with a Novel Hybrid Approach for Alumina Extraction from the Cement Industry Tailing." AIP Conf. Proc., 3303, 060022. https://doi.org/10.1063/5.0264561
[29] Favors, Z., Wang, W., Bay, H. H., Mutlu, Z., Ahmed, K., Liu, C., Ozkan, M., & Ozkan, C. S. (2014). Scalable Synthesis of Nano-Silicon from Beach Sand for Long Cycle Life Li-ion Batteries. Scientific Reports, *4*(1), 5623. https://doi.org/10.1038/srep05623
[30] Cai, M., Zhao, Z., Qu, J., Ma, Q., Qu, X., Guo, L., Xie, H., Wang, D., & Yin, H. (2021). Zincothermic reduction of silica to silicon: make the impossible possible. Journal of Materials Chemistry A, *9*(34), 18630-18638. https://doi.org/10.1039/D1TA06073B
[31] Darghouth, A., Aouida, S., & Bessais, B. (2021). High Purity Porous Silicon Powder Synthesis by Magnesiothermic Reduction of Tunisian Silica Sand. Silicon, *13*(3), 667-676. https://doi.org/10.1007/s12633-020-00433-1
[32] Ash-Shidiq, M. G., Pramono, A., & Fauzi, F. (2023). Comparative study of carbon sources and briquetting in the carbothermic reduction of silica for silicon production. E3S Web of Conferences, *429*, 02006. https://doi.org/10.1051/e3sconf/202342902006
Downloads
Published
Issue
Section
License
Copyright (c) 2026 Ruaa A. Salman, Asaad H. Lafta
This work is licensed under a Creative Commons Attribution 4.0 International License.
