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TiO2 powder has been prepared by simple and low cost sol–gel procedure. The structural and morphological properties of prepared TiO2 powder were studied using X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The XRD pattern clearly shows (1 1 1) maximum intensive plane of TiO2 material with other less intensive peaks, in absence of any other impurities. The dye degradation properties of TiO2 powder were characterized using UV–Visible absorption spectroscopic technique. The photocatalytic dye degradation properties for methylene blue (MB) dye were studied. The photocatalytic dye degradation results show fast degradation of methylene blue (MB) dye in presence of TiO2 powder in solution. Above results show TiO2 material is useful for photocatalytic dye degradation application.

A simple, efficient and economically viable method for the Heck reaction has been accomplished in the absence of phosphine ligand. The Heck reaction was performed using nanostructured Ni-Co/ZnO material as a heterogeneous catalyst in a DMF/H2O solvent system and in the presence of K2CO3, at 120 °C. The Ni-Co/ZnO nanostructures were prepared by the facile reduction-impregnation method. The structural and morphological properties of Ni-Co/ZnO nanostructure were investigated using various physico-chemical characterization techniques. Structural studies displayed the formation of hexagonal (wurtzite) ZnO. Electron microscopy imaging showed the presence of agglomerated clusters of Ni-Co nanoparticles over the surfaces of elliptical, flower bud-like and irregularly shaped sub-micron sized particle bundles of ZnO. The elemental composition analysis (EDX) confirmed the loading of Ni and Co nanoparticles over the nanocrystalline ZnO. The surface chemical state analysis of Ni-Co/ZnO material validated that Ni nanostructure exists in Ni2+ and Ni3+ species, whereas, Co nanostructure exists in Co2+ and Co3+ species. UV–Vis diffuse reflectance spectroscopy displays red shift in the light absorption edge of Ni-Co/ZnO catalyst compared to pure ZnO. The as-prepared Ni-Co bimetallic supported ZnO nanostructure showed better catalytic activity and stability for the Heck reactions under phosphine ligand-free conditions. Ni-Co/ZnO catalyzed Heck reactions afforded the corresponding cross-coupled products with moderate to good yields (up to 92%). Ni-Co/ZnO catalyst could be reused for five successive runs without significant loss of catalytic activity.

Herein, we report nitrogen-doped TiO2 (N-TiO2) solid-acid nanocatalysts with heterogeneous structure employed for the solvent-free synthesis of α-aminophosphonates through Kabachnik–Fields reaction. N-TiO2 were synthesized by direct amination using triethylamine as a source of nitrogen at low temperature and optimized by varying the volume ratios of TiCl4, methanol, water, and triethylamine, under identical conditions. An X-ray diffraction (XRD) study showed the formation of a rutile phase and the crystalline size is 10 nm. The nanostructural features of N-TiO2 were examined by HR-TEM analysis, which showed they had rod-like morphology with a diameter of ∼7 to 10 nm. Diffuse reflectance spectra show the extended absorbance in the visible region with a narrowing in the band gap of 2.85 eV, and the high resolution XPS spectrum of the N 1s region confirmed successful doping of N in the TiO2 lattice. More significantly, we found that as-synthesized N-TiO2 showed significantly higher catalytic activity than commercially available TiO2 for the synthesis of a novel series of α-amino phosphonates via Kabachnik–Fields reaction under microwave irradiation conditions. The improved catalytic activity is due to the presence of strong and Bronsted acid sites on a porous nanorod surface. This work signifies N-TiO2 is an efficient stable catalyst for the synthesis of α-aminophosphonate derivatives.

We have explored nanocrystalline ZnO and Cu-ZnO catalyst for the preparation of 3-styrylchromones with trans selectivity derived from 3-formylchromones. Synthesis of ZnO and Cu-ZnO nano flakes (NFs) was carried by precipitation technique. The analytical techniques such as UV-Visible spectroscopy, X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET), field emission scanning electron microscopy (FESEM) and energy-dispersive analysis X-ray spectroscopy (EDAX) were used to characterize the catalysts. The XRD pattern showed highly pure wurtzite ZnO and Cu-ZnO. The FESEM images showed nano flakes such as sunflower seed morphology in the range width of 9–34 nm and length 90–180 nm. Doping of copper in ZnO was employed to study the selectivity of Knoevenagel and Knoevenagel-Doebner reactions. Knoevenagel condensation was catalyzed efficiently by pure ZnO nano flakes, whereas the Cu-ZnO nano flakes facilitate the Knoevenagel-Doebner reaction. Present synthetic protocols are novel, very clean and high yielding for synthesis of 3-styrylchromones. Almost same yield was observed to the recycled catalyst up to four runs. Keywords: Heterogeneous catalysis, ZnO nano flakes, Knoevenagel condensation, Knoevenagel-Doebner reaction, 3-Styrylchromone

For synthesis of flavoring agent E-ethyl cinnamate in an economic way using Wittig reaction, MnO2 doped MgO nanocomposites were prepared by alkali leached hydrothermal method. The resultant nanocomposites were characterized by XRD, UV-DRS, FT-IR, FESEM, EDAX, XPS and Hammett indicator method. This surface modified MnO2 doped MgO can be used as green solid base for Wittig reaction between benzaldehyde and phosponium salt for synthesis of E-ethyl cinnamate under solvent free approach. Nanocomposite of MgO with MnO2 in combination with green mechanochemical approach seems to be more economic in comparison to pure nanosized MgO under conventional solvent stirring. Both efforts are complementary for promoting surface basic activity of MgO for high-yield synthesis of E-ethyl cinnamate using Wittig reaction. The product ethyl cinnamate has been characterized by HR-MS, IR, 1H NMR.

One-pot green synthesis of propargylamines using ZnCl2 loaded TiO2 nanomaterial under solvent-free conditions has been effectively accomplished. The aromatic aldehydes, amines, and phenylacetylene were reacted at 100 °C in the presence of the resultant catalyst to form propargylamines. The nanocrystalline TiO2 was initially synthesized by a sol–gel method from titanium(IV) isopropoxide (TTIP) and further subjected to ZnCl2 loading by a wet impregnation method. X-ray diffraction (XRD) patterns revealed the formation of crystalline anatase phase TiO2. Field emission scanning electron microscopy (FESEM) showed the formation of agglomerated spheroid shaped particles having a size in the range of 25–45 nm. Transmission electron microscopy (TEM) validates cubical faceted and nanospheroid-like morphological features with clear faceted edges for the pure TiO2 sample. Surface loading of ZnCl2 on spheroid TiO2 nanoparticles is evident in the case of the ZnCl2 loaded TiO2 sample. X-ray photoelectron spectroscopy (XPS) confirmed the presence of Ti4+ and Zn2+ species in the ZnCl2 loaded TiO2 catalyst. Energy-dispersive X-ray (EDS) spectroscopy also confirmed the existence of Ti, O, Zn and Cl elements in the nanostructured catalyst. 15% ZnCl2 loaded TiO2 afforded the highest 97% yield for 3-(1-morpholino-3-phenylprop-2-ynyl)phenol, 2-(1-morpholino-3-phenylprop-2-ynyl)phenol and 4-(1,3-diphenylprop-2-ynyl)morpholine under solvent-free and aerobic conditions. The proposed nanostructure-based heterogeneous catalytic reaction protocol is sustainable, environment-friendly and offers economic viability in terms of recyclability of the catalyst.

The syntheses of Cu, Fe and Mn doped nanocrystalline MgO was carried out using alkali leached hydrothermal technique. The synergistic effect of transition metals (Cu, Fe and Mn) doping, particle size and nano-scale morphology on surface basicity enhancement was established in one pot Wittig reaction. The doped and undoped nanocrystalline MgO catalysts are characterized by XRD, UV-DRS, FT-IR, FESEM, EDS and XPS techniques. XRD study revealed formation of pure cubic phase of undoped and up to 1 wt% Cu, Fe and Mn doped MgO. The FESEM photographs of transition metal doped MgO indicated the formation of prismatic hexagonal nano plates and nanosheets with thickness in the range 20–70 nm. The catalytic activity of synthesized catalysts was investigated in one pot Wittig reaction of benzaldehyde, triphenylphosphine and ethyl bromoacetate at room temperature in DMF solvent. The Mn doped nanocrystalline MgO catalyst shows 98% yield under optimized reaction conditions. Enhancement of surface basicity due to doping of Mn in MgO was ascertained by UV-DRS and XPS study. The characterization of Wittig product ethyl cinnamate was carried out using HR-MS, 1H NMR, 13C NMR. The 1H NMR evaluates 95:5% E/Z ratio of ethyl cinnmate. Reported methodology is eco-friendly and easy to scale up.

TiO2 thin films have been effectively fused onto F:SnO2 (FTO) substrates via the electrodeposition method. The influence of deposition temperature on the synthesis of F:SnO2 substrates and relative information of as-deposited and annealed TiO2 thin films have been studied. Novel TiO2 microspheres are detected on F:SnO2 substrates at an optimized electrodeposition potential. Raman bands approve the creation of single-anatase-phase TiO2. The optimized deposition surroundings show a decrease in the band gap of F:SnO2 substrates and TiO2 thin films. The determined photoelectrochemical properties of annealed TiO2 thin films indicate a fill factor of 51% and power conversion efficiency of 0.15% for application in solar cells.

Flower-like nanostructures of molybdenum disulphide (MoS2) have been effectively synthesised by the hydrothermal method and further doped with nitrogen using varying concentrations of urea. The formed hierarchical nanostructures are characterised by spectroscopy as well as electrochemical techniques. The structural analysis confirms the formation of a hexagonal MoS2 crystal structure. The existence of MoO2/MoO3/MoS2 composites is also observed after heating MoS2 with a lower urea concentration. Surface morphological analysis of all the prepared compositions shows the appearance of flower-like nanostructures formed by the stacking of 20–80 nanosheets to create individual flower petals. Nitrogen doping shows enhancement in the specific capacitance of MoS2 due to an increase in the electronic conductivity. Furthermore, the specific capacitance is enhanced due to the formation of an MoO2/MoO3/MoS2 composite. The highest specific capacitance calculated from the charge–discharge curve for nitrogen-doped MoS2 prepared using 1 : 1 (MoS2 : urea) weight ratio is observed at around 129 (F g−1) at 2 (A g−1) specific current. The nitrogen-doped MoS2 demonstrates almost four-fold enhancement in specific capacitance than pristine nano-shaped MoS2.

A set of hierarchical Cd x Zn1−x O nanoflakes (x = 0, 0.01 and 0.03) was prepared by the co-precipitation method using methanol as solvent. The prepared samples were characterized by UV–visible, X-ray diffraction, field emission scanning electron microscopy and energy-dispersive X-ray analysis techniques. The slight red shift in the Cd-doped ZnO confirms the doping of Cd2+ ions into ZnO lattices. The average crystallite size of Cd-doped ZnO nanoflakes was found to be in the range of 10–28 nm. The catalytic activity of Cd-ZnO nanoflakes in conjunction with microwave irradiation was investigated for reactions between o-phenylenediamine with aldehydes. It was found that the presence of Cd content in ZnO promotes rapid and selective synthesis of 2-substituted benzimidazoles under solvent-free conditions. The improvement of the catalytic activity by Cd doping is discussed in the light of the Brunauer–Emmet–Teller method. The catalyst could be reused up to five cycles without any significant loss of catalytic activity.

Pd loaded ZnO nanoparticles have been explored as an efficient catalyst for Suzuki-Miyaura cross-coupling reactions under ambient and ligand-free conditions. For this purpose, the low temperature synthesis of ZnO nanoparticle was accomplished by the solution based approach using stoichiometric amount of zinc acetate and urea. The Pd/ZnO nanocrystalline catalyst was prepared by loading 3% PdCl2 on ZnO nanoparticles by simple wet impregnation technique. This catalyst efficiently performed Suzuki-Miyaura reactions with various ring substituted aryl bromides and boronic acids. The resultant Pd/ZnO nanocrystalline material conferred 97% yield under optimized reaction conditions. The nanostructured Pd loaded ZnO catalyst was characterized by XRD, FESEM, EDS, FETEM, STEM-BF-DF, XPS and BET techniques. XRD pattern of Pd/ZnO sample hints the presence of Pd as minor phase loaded on ZnO nanocrystalline material, while overall XPS analysis discloses effective loading of Pd (0) on ZnO surface. FESEM/TEM–EDS also revealed reasonable Pd loading on ZnO nanoparticles. The FETEM examination of unloaded ZnO and Pd loaded ZnO disclosed particle size in the range 25–40 nm. The nanocrystalline Pd/ZnO catalyst was reused without significant loss of catalytic activity. The present methodology is cost effective, environmentally friendly, easy to scale up and can become an alternative to homogeneous catalysis.

TiO2/Cu2O heterojunction solar cells have been successfully synthesized by an electrochemical route. The structural, morphological and optical properties of TiO2/Cu2O heterojunction solar cells were studied using x-ray diffraction, scanning electron microscopy and UV–vis spectroscopic techniques. The change in morphology is observed due to the effect of the annealing atmosphere on TiO2/Cu2O heterojunction. The surface morphological study shows truncated triangular and nanostar-like Cu2O material using air and nitrogen annealing. The oxidation state of TiO2 and Cu2O materials was studied by x-ray photoelectron spectroscopy. The J–V characteristics curve shows maximum 0.31% photoconversion efficiency of nitrogen-annealed TiO2/Cu2O heterojunction solar cells.