Visible light responsive 2 : 1 Ni/Ti layered double hydroxide (LDH) was synthesized by a single step hydrothermal route using commercially available Ni(NO3)2·6H2O, TiCl4 and urea. The material exhibited significant absorption in the visible range with a very narrow band gap (2.68 eV). This could be attributed to structural defects as confirmed by diffuse reflectance spectroscopy (DRS), photoluminescence (PL), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) measurements. FT-IR, TGA, DTA, DSC, HR-TEM and SEM-EDX measurements yielded information about structural aspects, thermal stability and surface morphology. Surface and pore characteristics of the material were obtained from the BET isotherm for N2 adsorption at 77 K. Zeta potential measurements were used to characterize the electrical properties of the surface while XPS revealed changes in surface states and oxygen deficiencies. The material was found to be an excellent photocatalyst for the degradation of aqueous methylene blue in visible light. The photocatalytic properties of the material were explained on the basis of the narrow band gap, the high surface area and the presence of surface defects. The photocatalytic activity improved in alkaline media [pH 11.0, catalyst load 15 mg in 200 ml dye solution, dye concentration 1 × 10−6 M (= 0.3198 mg L−1)] due to the electrostatic attractions between the dye cations and the negative charges on the Ni/Ti LDH surface. The catalytic activity was found to be higher than the common commercial catalysts like ZnO, ZnS, NiO, TiO2 and Degussa P25. The catalytic activity was retained even after five methylene blue degradation cycles, demonstrating that the LDH could be an important addition to the field of wastewater treatment.

2 : 1 Co/Ti layered double hydroxide (LDH) was synthesized hydrothermally using commercially available Co(NO3)2·6H2O and TiCl4, on a urea template. The high surface area material (~180 m2 g−1) had a narrow band gap (2.67 eV) and shallow and deep trap defect sites. The layered nanomaterial exhibited remarkable semiconductor properties and demonstrated excellent visible light decolourisation efficiency for the anionic dye Congo Red in aqueous medium. The photocatalytic efficiency of the LDH was better than common commercial materials in use such as ZnO, ZnS, NiO, CoO, TiO2 and Degussa P25. The presence of different surface states of defect sites in the LDH was confirmed by PL, EIS and XPS measurements. XRD, DRS, FT-IR, AFM, TEM, SEM/EDX and TG/DTG analyses yielded information about the structural, morphological properties and thermal stability of the LDH. BET N2 adsorption-desorption measurements at 77 K gave surface area and porosity data for the LDH. The surface charge characteristics of the LDH were evaluated with ξ-potential measurements over a wide pH-range in aqueous medium. The photocatalytic behaviour towards decolourisation of the dye was evaluated depending on the reaction variables of pH, LDH amount, initial dye concentration and effects of quenchers, and variation of molar ratios of Co/Ti LDH. The pseudo-first order model satisfactorily described the degradation kinetics of the anionic dye. The photocatalytic mechanistic pathways of the LDH were explained on the basis of an electron-hole (e--h+) hopping conduction model and also photosensitization of the dye. The maximum catalytic efficiency was observed with 15.0 mg of LDH at pH 4 for the anionic Congo Red dye at a concentration 1 × 10−5 M. The LDH was stable even after the fifth catalytic cycle, indicating its remarkable efficiency in potential decolourisation treatments. The dye degradation products were analysed with GC-MS and a reaction mechanism was proposed for the breakdown of the dye to simple and less toxic components.

Optically responsive, luminescent Ni/Co/Ti layered double hydroxide (LDH), synthesized by a single step hydrothermal route, exhibits highly efficient photodegradation of cationic and anionic dyes, Rhodamine B (∼99.8%) and Acid Red G (∼99.6%) respectively, better than that of commercial catalysts like NiO, CoO and TiO2.The LDH has been characterized by using XRD, XPS, PL, TRES, EIS, TEM, SEM-EDX, AFM, UV-visible DRS, N2-sorption desorption, ξ-potential, FT-IR and TG techniques. The characterized results indicate that the LDH possesses hexagonal morphology, a high surface area, a narrow band gap, defect states and oxygen vacancies within its layered framework. The degradations follow the e−–h+ hopping pattern and dye-photosensitized mechanistic pathways. The active species generated during photocatalysis have been evaluated using ESR, terephthalic acid fluorescence probe and indirect radical–hole trapping experiments. The colourless end products were investigated by GC-MS and reaction mechanisms have been established for the degradation of the dyes to less toxic and more eco-friendly molecules than their parent analogues. Dye mineralization studies (performed using a TOC analyser) and closure of carbon mass balance experiments quantified the amount of carbon entering and leaving the reaction systems. Reaction mechanisms have been proposed on the basis of the asymmetric cleavage of the dyes. The LDH demonstrated its remarkable efficiency in the field of waste water treatment.