Preparation and Characterization of Ni-Al and Co-Al Layered Double Hydroxide by Reduction-Oxidation Method

Authors

  • Pallavi G. Department of Studies and Research in Chemistry University College of Science, Tumkur University, Tumkakuru 572103, India
  • Vidyashree B. K. Department of Studies and Research in Chemistry University College of Science, Tumkur University, Tumkakuru 572103, India
  • Ramesh T. N. Department of Studies and Research in Chemistry University College of Science, Tumkur University, Tumkakuru 572103, India

DOI:

https://doi.org/10.33736/jaspe.13337.2026

Keywords:

Cobalt-aluminium based layered double hydroxide,, nickel-aluminium based layered double hydroxide, layered compound, band gap,, morphology

Abstract

Layered double hydroxides have been extensively used as electrode materials, adsorbents and precursors for catalysts. In this work, a simple preparative method was adopted, and its influence on the crystallinity and band gap values was investigated. Cobalt-aluminium and nickel-aluminium based layered double hydroxides (0.75:0.25/0.667:0.333) were prepared using the reduction-oxidation method. Ni2+/Co2+ cations were reduced to metallic cobalt/nickel using sodium borohydride in the presence of trivalent aluminium ions and sodium carbonate solution at 28- 30 °C to prepare layered double hydroxides (LDHs). The resulting compounds were characterized using powder X-ray diffraction, infrared spectra, scanning electron microscopy and UV-visible diffuse reflectance spectra. The interplanar spacings around 7.6 Å for Co-Al LDHs (0.75/667:0.333) and Ni-Al LDHs (0.75:0.25/0.667:0.333) were observed from the powder X-ray diffraction patterns. Infrared spectral data confirm the presence of water molecules and carbonate ions in the interplanar region. Co-Al (0.75:0.25/0.667:0.333) LDH and Ni-Al (0.75:0.25/0.667:0.333) LDHs exhibit band gaps in the range of 2 to 5.4 eV, indicating that the compounds exhibit semiconducting to insulating behaviour. Scanning electron microscopic data shows irregular morphologies with particle sizes in the micrometer range for both Co-Al (0.75:0.25/0.667:0.333) LDH and Ni-Al (0.75:0.25/0.667:0.333) LDH samples, respectively.

References

He, J., Wei, M., Li, B., Kang, Y., Evans, D. G., & Duan, X. (2006). Preparation of layered double hydroxides. In: Duan, X., Evans, D. G. (eds) Layered Double Hydroxides. Structure and Bonding, Vol 119, 89-119, Springer, Berlin, Heidelberg. https://doi.org/10.1007/b100426

Mishra, G., Dash, B., & Pandey, S. (2017). Layered double hydroxides: A brief review from fundamentals to application as evolving biomaterials. Applied Clay Science, 153, 172–186. https://doi.org/10.1016/j.clay.2017.12.021

Altalhi, A. A., Mohamed, E. A., & Negm, N. A. (2024). Recent advances in layered double hydroxide (LDH)-based materials: fabrication, modification strategies, characterization, promising environmental catalytic applications, and prospective aspects. Energy Advances, 3(9), 2136–2151. https://doi.org/10.1039/d4ya00272e

Mohapi, M., Sefadi, J. S., Mochane, M. J., Magagula, S. I., & Lebelo, K. (2020). Effect of LDHs and other clays on polymer composite in adsorptive removal of contaminants: A review. Crystals, 10(11), 957. https://doi.org/10.3390/cryst10110957

Hadnadjev-Kostic, M., Vulic, T., Karanovic, D., Tomic, A., & Cvetkovic, D. (2025). Layered double hydroxide-based materials for wastewater treatment: Recent progress in multifunctional environmental applications. Processes, 13(12), 3757. https://doi.org/10.3390/pr13123757

Kumari, S., Sharma, V., Sharma, V., Soni, S., Sharma, A., Thakur, A., Kumar, S., Dhama, K., Sharma, A. K., & Bhatia, S. K. (2023). Layered double hydroxides and their tailored hybrids/composites: Progressive trends for delivery of natural/synthetic-drug/cosmetic biomolecules. Environmental Research, 238(Pt 2), 117171. https://doi.org/10.1016/j.envres.2023.117171

Vuksanović, M. M., Egelja, A., Barudžija, T., Tomić, N., Petrović, M., Marinković, A., Radojević, V., & Heinemann, R. J. (2021). Inorganically modified particles FeAl-LDH@SiO2 as reinforcement in poly (methyl) methacrylate matrix composite. Royal Society Open Science, 8(9), 210835. https://doi.org/10.1098/rsos.210835

Yu, S., Choi, G., & Choy, J.-H. (2023). Multifunctional layered double hydroxides for drug delivery and imaging. Nanomaterials, 13(6), 1102. https://doi.org/10.3390/nano13061102

Zhang, Y., Xu, H., & Lu, S. (2021). Preparation and application of layered double hydroxide nanosheets. RSC Advances, 11(39), 24254–24281. https://doi.org/10.1039/d1ra03289e

Rashed, S. H., Abd-Elhamid, A., Abdalkarim, S. Y. H., El-Sayed, R. H., El-Bardan, A. A., Soliman, H. M., & Nayl, A. (2022). Preparation and characterization of layered-double hydroxides decorated on graphene oxide for dye removal from aqueous solution. Journal of Materials Research and Technology, 17, 2782–2795. https://doi.org/10.1016/j.jmrt.2022.02.040

Raheem, S. A., & Mohammed, A. A. (2024). Synthesis, characterization, and applications of layered double hydroxides nanocomposites for the adsorption of organic and inorganic contaminants from an aqueous solution: An overview. Results in Surfaces and Interfaces, 18, 100386. https://doi.org/10.1016/j.rsurfi.2024.100386

Liu, Q., Fan, G., Zhang, S., Liu, Y., & Li, F. (2012). Synthesis of uniform Ni–Al layered double hydroxide via a novel reduction–oxidation route. Materials Letters, 82, 4–6. https://doi.org/10.1016/j.matlet.2012.05.039

Zhao, Y., Li, F., Zhang, R., Evans, D. G., & Duan, X. (2002). Preparation of layered double-hydroxide nanomaterials with a uniform crystallite size using a new method involving separate nucleation and aging steps. Chemistry of Materials, 14(10), 4286–4291. https://doi.org/10.1021/cm020370h

Klydziute, G., Gliaudyte, L., Sokol, D., Vasiliauskiene, D., Yang, T. C., & Kareiva, A. (2024). Layered double hydroxides: Sol-gel synthesis, characterization and application. Research Square. https://doi.org/10.21203/rs.3.rs-5346865/v1

Jin, L., Sun, Y., Zhou, X., Wen, J., Wang, F., Ning, X., Wen, Y., Wu, D., & Peng, L. (2022). One-Step synthesis of layered double hydroxides by a Solvent-Free method. ACS Sustainable Chemistry & Engineering, 10(39), 12955–12961. https://doi.org/10.1021/acssuschemeng.2c04436

Gao, Z., Sasaki, K., & Qiu, X. (2018). Structural memory effect of Mg–Al and Zn–Al layered double hydroxides in the presence of different natural humic acids: Process and mechanism. Langmuir, 34(19), 5386–5395. https://doi.org/10.1021/acs.langmuir.8b00059

Singha Roy, A., Kesavan Pillai, S., & Ray, S. S. (2022). Layered double hydroxides for sustainable agriculture and environment: An overview. ACS omega, 7(24), 20428–20440. https://doi.org/10.1021/acsomega.2c01405

Kameliya, J., Verma, A., Dutta, P., Arora, C., Vyas, S., & Varma, R. S. (2023). Layered double hydroxide materials: A review on their preparation, characterization, and applications. Inorganics, 11(3), 121. https://doi.org/10.3390/inorganics11030121

Bhojaraj, & Rajamathi, M. (2023). Anion Exchange Reactions of 3R2-MgAl-Carbonate-LDH: Comparison with the 3R1 analogue and formation of 3R2 polytype of MgAl-LDH with other interlayer anions. ACS Omega, 8(11), 10185–10190. https://doi.org/10.1021/acsomega.2c07515

Richardson, M. C., & Braterman, P. S. (2007). Infrared spectra of oriented and nonoriented layered double hydroxides in the range from 4000 to 250 cm-1, with evidence for regular short-range order in a synthetic magnesium−aluminum LDH with Mg:Al = 2:1 but Not with Mg:Al = 3:1. The Journal of Physical Chemistry C, 111(11), 4209–4215. https://doi.org/10.1021/jp064744w

Zamaraite, I., Vieira, D. E. L., Vieira, L. G., Ribeiro, J. L., Vieira, J. M., Salak, A. N., & Banys, J. (2021). Dielectric and infrared spectroscopy characterization of Co–AL layered double hydroxides. Physica Status Solidi (A), 218(15). https://doi.org/10.1002/pssa.202100106

Zhou, J., Ma, P., Li, C., Li, S., Li, C., Wu, F., & Dou, Y. (2026). Research Progress on Layered Double Hydroxides and Their Derivatives toward Solar-to-Chemical Energy Conversion. ACS Applied Materials & Interfaces, 18(15), 21424–21443. https://doi.org/10.1021/acsami.6c00782

Kaur, H., Singh, S., & Pal, B. (2021). A brief review on modified layered double hydroxides for H2 production through photoinduced H2O splitting. Environmental Nanotechnology Monitoring & Management, 16, 100451. https://doi.org/10.1016/j.enmm.2021.100451

Santos, M. F., Moraes, P. I. R., Tavares, S. R., Martins, A., Capaz, R. B., Wypych, F., & Leitão, A. A. (2025). Analysis of the energy and nature of bandgap in layered double hydroxides Mg-Al-X and Zn-Al-X (X= Cl−, OH−, CO32−, or NO3−). Applied Clay Science, 279, 108061. https://doi.org/10.1016/j.clay.2025.108061

Saeed, M., Zafar, M., Razzaq, A., Khan, S. A., Khan, Z., & Kim, W. Y. (2022). Visible-light-active Zn–Fe layered double hydroxide (LDH) for the photocatalytic conversion of rice husk extract to value-added products. Applied Sciences, 12(5), 2313. https://doi.org/10.3390/app12052313

Bobde, P., Patel, R. K., Panchal, D., Sharma, A., Sharma, A. K., Dhodapkar, R. S., & Pal, S. (2021). Utilization of layered double hydroxides (LDHs) and their derivatives as photocatalysts for degradation of organic pollutants. Environmental Science and Pollution Research, 28(42), 59551–59569. https://doi.org/10.1007/s11356-021-16296-x

Mohapatra, L., & Parida, K. (2011). Zn–Cr layered double hydroxide: Visible light responsive photocatalyst for photocatalytic degradation of organic pollutants. Separation and Purification Technology, 91, 73–80. https://doi.org/10.1016/j.seppur.2011.10.028

Downloads

Published

2026-10-30

How to Cite

G., P., B. K., V., & Ramesh T. N. (2026). Preparation and Characterization of Ni-Al and Co-Al Layered Double Hydroxide by Reduction-Oxidation Method. Journal of Applied Science &Amp; Process Engineering, 13(2), 202–216. https://doi.org/10.33736/jaspe.13337.2026