Monodisperse mesoporous zirconium titanium oxide microspheres with varying compositions (Zr content from 0 to 100%), high surface areas (up to 413 m 2/g) and well-interconnected mesopores are synthesized via a combined sol-gel self-assembly and solvothermal process. Surface areas, pore diameters, crystallinity and mesostructures of the products are controlled by changing the composition of the microspheres. The resulting mesoporous microspheres are tested as adsorbents to remove Cr (VI) anions from solution and the binary oxides show very high adsorption capacities (>25.40 mg/g, that is 0.49 mmol/g) in contrast to previously reported oxides (4.25 mg/g for TiO 2, 4.47 mg/g for α-Fe 2O 3, 5.8 mg/g for CeO 2). The maximum adsorption capacities of the mesoporous microspheres of varying compositions correlate with the amount of surface hydroxyl groups on the materials. A maximum adsorption capacity of 29.46 mg/g (0.57 mmol/g) is achieved on the microspheres containing 30% Zr due to abundant active hydroxyl groups for heavy metal ion adsorption. Owing to their integrated features (including variable compositions, high specific surface area, tunable pore size and monodisperse grain size) as well as specific acid-base surface properties, such mesoporous zirconium titanium oxide microspheres are also expected to have potential either as catalysts or catalyst supports for industrial applications.

Facile Synthesis of Monodisperse Mesoporous Zirconium Titanium Oxide Microspheres with Varying Compositions and High Surface Areas for Heavy Metal Ion Sequestration

The solid state thermal, one pot, efficient chemical reaction between Zn and S or Se elements in a closed reactor at 650 °C/60 min under their autogenic pressure in an inert atmosphere yielded luminescent ZnS and ZnSe semiconducting nanopowders (NPs). Scanning and Transmission electron microscopy measurements confirmed the size and shape of the as formed ZnS and ZnSe NPs. The wide size distributions of ZnS and ZnSe NPs are confirmed by UV−vis and TEM measurements. The crystalline wurtzite phase of ZnS and face centered cubic phase of ZnSe NPs is revealed from XRD and HR-TEM measurements. The obtained Raman scattering bands also supports the formation of pure ZnS and ZnSe phases. At room temperature, a strong visible green emission centered at ∼525 nm is measured for ZnS, while ZnSe NPs showed a broad red emission band extending from 550 to 760 nm. The putative reaction mechanism is based on the low melting and boiling points of reactants (Zn, S and Se) under their autogenic pressure in an inert atmosphere.

Facile synthesis of photoluminescent ZnS and ZnSe nanopowders.

This review compiles various nanostructures fabricated by a distinct "dry autoclaving" approach, where the chemical reactions are carried out without solvents; above the dissociation temperature of the chemical precursor(s) at elevated temperature in a closed reactor. The diversity to fabricate carbides (SiC, Mo(2) C, WC), oxides (VOx-C, ZnO, Eu(2) O(3) , Fe(3) O(4) , MoO(2) ), hexaborides (LaB(6) , CeB(6) , NdB(6) , SmB(6) , EuB(6) , GdB(6) ), nitrides (TiN, NbN, TaN), phosphides (PtP(2) , WP), sulfides (ZnS, FeS/C, SnS/C, WS(2) , WS(2) /C), and selenides (Zn(1-x) Mn(x) Se/C, Cd(1-x) Mn(x) Se/C), with various shapes and sizes is accounted with plausible applications. This unique single-step, solvent-free synthetic process opens up a new route in the growing nanomaterials science; owing to its considerable advantages on the existing approaches.

Dry Autoclaving for the Nanofabrication of Sulfides, Selenides, Borides, Phosphides, Nitrides, Carbides, and Oxides

Polycrystalline zirconium titanate, ZrTiO4, has been prepared via sol–gel chemistry and its properties both as a semiconducting oxide and as a photoactive system have been investigated by experimental and computational techniques. The oxide exhibits a structure analogous to those of the main TiO2 polymorphs with a slightly higher band gap of 3.65 eV. Theoretical results explain this small difference in terms of composition of the lower part of the conduction band, which is based on Ti 3d orbitals. Interestingly zirconium titanate is much less reducible than TiO2 upon annealing under a vacuum in the range between room temperature and 673 K. Over this temperature the system releases O2, forming oxygen vacancies and trapping excess electrons on tetravalent Ti ions as firmly indicated by both electron paramagnetic resonance (EPR) and computational results. Irradiating the solid with UV photons a charge separation is observed by EPR and the photogenerated carriers easily reach the surface where they react with...

Fifty–Fifty Zr–Ti Solid Solution with a TiO2-Type Structure: Electronic Structure and Photochemical Properties of Zirconium Titanate ZrTiO4

The rapid, solvent-less, straightforward reactions under autogenic pressure at elevated temperature (RAPET) approach is explored for the fabrication of core−shell nanomaterials Carbon-encapsulated ZnS and ZnSe nanoparticles are synthesized by a one-step thermal decomposition of diethyl zinc in the presence of either S or Se powders in a closed reactor at 700 °C for 30 min under their autogenic pressure in an inert atmosphere The Raman spectroscopy measurements provide the structural evidence for the formation of pure ZnS or ZnSe particles and ensure the nature of the coated carbon The X-ray diffraction measurements confirm the hexagonal phase of ZnS and the face-centered cubic crystal structure of ZnSe The high-resolution transmission electron microscopy technique distinguishes core and shell morphologies Interestingly, core−shell nanostructures of ZnS and ZnSe coated with carbon show a single electron spin resonance signal, whereas the bare ZnS and ZnSe nanoparticles demonstrate several signals The

Encapsulating ZnS and ZnSe Nanocrystals in the Carbon Shell: A RAPET Approach

The thermal decomposition of a ZrTi2[(OC2H4)2NH]3(OC3H7)6 precursor by the RAPET (reaction under autogenic pressure at elevated temperature) method provided the formation of crystalline zirconium titanate nanoparticles. These as-prepared nanoparticles are embedded in a carbon shell, which can be removed completely by calcination at 500 °C under air for 3 h, resulting in pure white crystalline nanoparticles. At a reaction temperature of 700 °C, the nanoparticles are mainly ZrTi2O6 (srilankite), whereas at 800 °C, the product is predominately Zr5Ti7O24. The structural, morphological, compositional, magnetic, and AC electrical properties are measured for the as-prepared ZrTi2O6 embedded in carbon (ZTEC), as well as the crystalline ZrTi2O6 nanoparticles (ZTN) obtained after sintering. The reaction mechanism is based on the decomposition products containing pyrrol and pyrazine. The presence of these compounds provides an understanding of the decomposition of the diethanolamine ligands and the formation of the nanoparticles in general.

Synthesis of Nanocrystalline Zirconium Titanate and its Dielectric Properties

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Synthesis of Nanocrystalline Zirconium Titanate and its Dielectric Properties