Sonochemical syntheses of a nanoparticles cadmium(II) supramolecule as a precursor for the synthesis of cadmium(II) oxide nanoparticles

Nanoparticles of a three-dimensional supramolecular Cd(II) compound, [Cd(L)(2)(H(2)O)(2)] (1), (L(-)=1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 in both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared with each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied. Calcination of the single crystals and nano-sized compound 1 at 650°C under air atmosphere yields CdO nanoparticles.     

Sonochemical syntheses of a nano-sized copper(II) supramolecule as a precursor for the synthesis of copper(II) oxide nanoparticles

Nanoparticles of a three-dimensional supramolecular, [Cu(L)₂(H₂O)₂] (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied. Calcination of the nano-sized compound 1 at 600 °C under air atmosphere yields CuO nanoparticles.     

Sonochemical synthesis of a novel nano-rod two-dimensional zinc(II) coordination polymer; preparation of zinc(II) oxide nanoparticles by direct thermolyses

A novel mixed-ligand zinc(II) coordination polymer, {[Zn(μ-4,4'-bipy)(μ-3-bpdh)(H(2)O)(2)](ClO(4))(2)·(4,4'-bipy)(0.5)}(n) (1); 3-bpdh=2,5-bis(3-pyridyl)-3,4-diaza-2,4-hexadiene and 4,4'-bipy=4,4'-bipyridine, has been synthesized and characterized by IR, (1)HNMR and (13)CNMR spectroscopy. The single crystal X-ray data of compound 1 shows that this coordination polymer grows in two dimensions by two different bridging ligands, 4,4'-bipy and 3-bpdh. Also, nano-scale of compound 1 has been synthesized by sonochemical method and characterized by IR, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Thermal stability of compound 1 in single crystalline and nano-scale form was carried out by thermal gravimetric (TG) and differential thermal analysis (DTA). The ZnO nanoparticles were obtained by calcination of compound 1 at 500°C under air atmosphere and by thermolyses in oleic acid at 200°C. The zinc(II) oxide nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM).     

Sonochemical synthesis and characterization of new one-dimensional manganese(II) coordination polymer nanostructures

A new Mn(II) coordination polymer, [Mn (L₁)₂(NCS)₂]_n (1) [L₁ = 3,4-bis(4-pyridyl)-5-(2-pyridyl)-1,2,4-triazole] was synthesized by the reaction of ligand L₁ and mixtures of manganese(II) acetate and potassium thiocyanate using the heat gradient method. Compound 1 has been characterized by IR spectroscopy, elemental analyses and X-ray crystallography. The crystal structure of compound 1 was determined by single-crystal X-ray diffraction and shows a new interesting one-dimensional coordination polymer. Nanostructures of compound 1 have been synthesized by sonochemical method. The products were characterized by X-ray powder diffraction, scanning electron microscopy (SEM), and IR spectroscopy. The thermal stability of nano particles of compound 1 was studied by thermal gravimetric and differential thermal analyses.     

Sonochemical syntheses of binuclear lead(II)-azido supramolecule with ligand 3,4,7,8-tetramethyl-1,10-phenanthroline as precursor for preparation of lead(II) oxide nanoparticles

The new neutral binuclear lead(II) azido coordination compound, [Pb₂(tmph)₂(μ-N₃)₂(CH₃COO)₂] (1) [tmph = 3,4,7,8-tetramethyl-1,10-phenanthroline], has been synthesized by a sonochemical method. Single crystal X-ray structure shows that the overall structure of 1 is binuclear unit. Complex 1 has a bridging azido pathway, end-to-end bridging azides between a pair of lead(II) centers. This is further extended into a one-dimensional (1D) and three-dimensional (3D) supramolecular structure by Pb⋯C and π–π weak directional intermolecular interactions. The coordination number of lead(II) ions is seven, PbN₄O₃, with two N-donor atoms from tmph ligands and three O-donors from acetate anions and two N-donors from two azide anions. It has a “stereo-chemically active” electron lone pair, and the coordination sphere is hemidirected. The PbO nanoparticles were obtained by thermolysis of 1 at 180 °C with oleic acid as a surfactant. The morphology and size of the prepared PbO samples were further observed using scanning electron microscopy (SEM).     

Sonochemical synthesis and characterization of nano-sized lead(II) 3D coordination polymer: Precursor for the synthesis of lead(II) oxybromide nanoparticles

Nanoparticles of a three-dimensional coordination polymer, [Pb(L)(μ₂-Br)(H₂O)]_n (1), (L^? = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by an ultrasonic method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal (DTA) analyses and compared each other. Concentration of initial reagents effects and the role of power ultrasound irradiation on size and morphology of nano-structured compound 1, have been studied. Calcination of the compound 1 at 500 °C under air atmosphere yields Pb₃O₂Br₂ nanoparticles.     

Sonochemical synthesis and characterization of three nano zinc(II) coordination polymers; Precursors for preparation of zinc(II) oxide nanoparticles

Nanostructures of three Zinc(II) coordination polymers, [Zn(NNO)₂(H₂O)₄]_n (1), [Zn(PNNO)₂(H₂O)₂]_n (2) and [Zn(H₂O)₆]·(INNO)₂ (3) {NNO: Nicotinic acid N-oxide, PNNO: Picolinic acid N-oxide and INNO: Isonicotinic acid N-oxide}, have been synthesized by a sonochemical process and reaction of ligands with Zn(CH₃COO)₂. The Zinc(II) oxide nano-particles have been synthesized from thermolysis of [Zn(NNO)₂(H₂O)₄]_n (1), [Zn(PNNO)₂(H₂O)₂]_n (2) and [Zn(H₂O)₆]·(INNO)₂ (3) at two different methods (with surfactant and without surfactant) and two temperatures (200 and 600 °C). The ZnO nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Comparison of the SEM images of ZnO nano-particles at two different methods and temperatures shows that higher temperature results in an increasing of agglomeration and thus small and spherical ZnO particles with good separation were produced by thermolysis of compounds at 200 °C and by use of surfactant.     

Sonochemical synthesis and structural characterization of a new nanostructured Co(II) supramolecular coordination polymer with Lewis base sites as a new catalyst for Knoevenagel condensation

A new Co(II) mixed-ligand coordination supramolecular polymer with composition [Co₂(ppda)(4-bpdh)₂(NO₃)₂]_n (1) (where, ppda = p-phenylenediacrylic acid, 4-bpdh = 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene) was synthesized using solvothermal, mechanochemical and sonochemical methods. Compound 1 and the new nanostructure have been characterized by single-crystal X-ray, infrared spectroscopy (IR), powder X-ray diffraction (PXRD) analysis and scanning electron microscopy (SEM). The thermal stability of compound 1 was also studied by thermal gravimetric analysis (TGA). The surface area of these compounds was determined by BET. The single-crystal X-ray data shows a new interesting two-dimensional coordination polymer (CP). In addition, the effect of various sonication concentrations of initial reagents, power of ultrasound irradiation and also the time on the size and morphology of nano-structured coordination polymer 1 were evaluated. Moreover, it has been demonstrated that the nanostructure of the CP1 can be used as a catalyst in Knoevenagel condensation reaction.     

Sonochemical syntheses of a new fibrous-like nano-scale manganese(II) coordination supramolecular compound; precursor for the fabrication of octahedral-like Mn3O4 nano-structure

Nanoparticles of a new three-dimensional Mn(II) coordination supramolecular compound, [Mn(L)₂(H₂O)₂] (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy and elemental analyses. Structural determination of compound 1 reveals the Mn(II) ion is six coordinated, bonded to two nitrogen atoms, two oxygen atoms from the L⁻ ligand and two water molecules. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied and shows that low concentrations of initial reagents decreased particles size and also leaded to fibrous-like nanostructures morphology. Mn₃O₄ nano-structure with an octahedral-like morphology were simply synthesized by solid-state transformation of compound 1 at 650 °C.     

Sonochemical syntheses and characterization of nano-sized lead(II) coordination polymer with ligand 1H-1,2,4-triazole-3-carboxylate

Nanoparticles of a two-dimensional coordination polymer, {[Pb(L)(μ_1,1-NCS)(H₂O)]}_n (1), (L⁻ = 1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal (DTA) analyses and compared each other. Concentration of initial reagents effects and the role of power ultrasound irradiation on size and morphology of nano-structured compound 1, have been studied. Calcination of the single crystals and nano-sized compound 1 at 400 °C under air atmosphere yields mixture of PbS and Pb₂(SO₄)O nanoparticles. Results show that the size and morphology of the PbS and Pb₂(SO₄)O nanoparticles are dependent upon the particles size of compound 1. A decrease in the particles size of compound 1 leads to a decrease in the particles size of the PbS and Pb₂(SO₄)O.     

Sonochemical synthesis of two new nano structure zinc(II) 1,10-phenanthroline coordination supramolecular compounds: New precursors to produce nano-sized zinc(II) oxide

Nanoparticles of two zinc(II) coordination supramolecule compounds (CSCs), [Zn(L)Cl2] (1) and [Zn(L)Br2] (2) L = 1,10-phen = 1,10-phenanthroline ligand, have been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared (FTIR) spectroscopy and elemental analyses. The single crystal X-ray data of compounds 1 and 2 imply that the Zn⁺² ions are four coordinated. Topological analysis shows that the compound 1 and 2 are new topology for net: 1,3M4-1. Nanoparticles of zinc(II) oxide have been prepared by calcination of two different zinc(II) CPs at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD) and IR spectroscopy.     

Sonochemical synthesis of a new nano-sized barium coordination polymer and its application as a heterogeneous catalyst towards sono-synthesis of biodiesel

A new nano-sized barium coordination polymer, {(bipyH)[Ba₂(pydc)₂(Hpydc)(H₂O)₂]}_n·nH₂O (1), (bipy = 4,4′-bipyridine and H₂pydc = pyridine-2,6-dicarboxylic acid), has been sonochemically synthesized and fully characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), FT-IR spectroscopy, thermogravimetric analysis (TGA) and elemental analyses. Compound 1 was structurally characterized by single crystal X-ray diffraction and it was shown that this compound consists of 1D anionic coordination polymers and bipyH⁺ cationic species that construct a three-dimensional supramolecular architecture via non-covalent interactions i.e. ion-pairing and hydrogen bonding. The role of compound 1 as a heterogeneous catalyst in the production of biodiesel was also investigated. A full conversion of soybean oil to biodiesel was accomplished in an exceptionally short timeframe through an ultrasonic-assisted transesterification process in the presence of compound 1.     

Synthesis of a new Hg(II) coordination polymer: Ultrasonic-assisted synthesis and mechanical preparation of nanostructure

A new mercury(II) coordination polymer, [Hg(4-bpmo)I₂]_n (1), (4-bpmo = N,N′-bis(pyridin-4-ylmethyl)oxalamide), was synthesized, by branched tube method, and structurally characterized by single-crystal X-ray diffraction. Compound 1 is a polymer with a distorted tetrahedral HgN₂I₂ coordination environment. The thermal stability of 1 was studied by thermal gravimetric (TG) and differential thermal (DTA) analyses. Also 1 was prepared by a sonochemical process at ambient temperature. Reaction time and concentration of initial reagents effects on the size and morphology were studied. Nanoparticles of 1, was synthesized easily by a mechanical method (neat grinding). The resulting structures were characterized by scanning electron microscopy (SEM), IR spectroscopy and X-ray powder diffraction (XRD).     

Sonochemical synthesis of two new nano lead(II) coordination polymers: Evaluation of structural transformation via mechanochemical approach

Two new lead(II) mixed-ligand coordination polymers, [Pb(PNO)(SCN)]_n (1) and [Pb(PNO)(N₃)]_n (2), (HPNO = picolinic acid N-oxide) were synthesized by a sonochemical method and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analysis. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction. The thermal behavior of 1 and 2 were studied by thermal gravimetric analysis. Structural transformations of compounds 1 and 2 were evaluated through anion-replacement processes by mechanochemical method. Moreover, the effect of sonication conditions including time, concentrations of initial reagents and power of irradiation were evaluated on size and morphology of compounds 1 and 2.     

Sonochemical synthesis of a new nano-structures bismuth(III) supramolecular compound: New precursor for the preparation of bismuth(III) oxide nano-rods and bismuth(III) iodide nano-wires

A new nanostructured Bi(III) supramolecular compound, {[Bi₂(4,4′-Hbipy)_1.678(4,4′-Hbipy)_0.322(μ-I)₂I_5.678] (4,4′-bipy)} (1), 4,4′-bipy = 4,4′-bipyridine} was synthesized by a sonochemical method. The nano-structure of 1 was investigated using scanning electron microscopy, powder X-ray powder diffraction (XRD), IR spectroscopy and elemental analysis, and the crystal structure of compound 1 was determined by single-crystal X-ray diffraction. The thermal stability of bulk compound 1 and of nano sized particles was studied by thermal gravimetric (TG) and differential thermal analyses (DTA). Bi₂O₃ and BiI₃ nano-structures were obtained by calcinations of nano-structures of compound 1 at 400 °C under air and nitrogen atmospheres, respectively.     

Sonochemical synthesis of TiO(2 nanoparticles on graphene for use as photocatalyst

Using ultrasonication we succeed in a controlled incorporation of TiO(2) nanoparticles on the graphene layers homogeneously in a few hours. The average size of the TiO(2) nanoparticles was controlled at around 4-5 nm on the sheets without using any surfactant, which is attributed to the pyrolysis and condensation of the dissolved TiCl(4) into TiO(2) by ultrasonic waves. The photocatalytic activity of the resultant graphene-TiO(2) composites containing 25 wt.% TiO(2) is better than that of commercial pure TiO(2). This is partly due to the extremely small size of the TiO(2) nanoparticles and partly due to the graphene-TiO(2) composite structure consisting of homogeneous dispersion of crystalline TiO(2) nanoparticles on the graphene sheets. As the graphene in the composites has a very good contact with the TiO(2) nanoparticles it enhances the photo-electron conversion of TiO(2) by reducing the recombination of photo-generated electron-hole pairs.     

Sonochemical preparation of pure t-LaVO4 nanoparticles with the aid of tris(acetylacetonato)lanthanum hydrate as a novel precursor

Herein a simple and fast method is introduced for the synthesis of lanthanum orthovanadate (LaVO₄) nanoparticles under ultrasound irradiation. The effect of tris(acetylacetonato)lanthanum hydrate ([La(acac)₃·3H₂O]) and La(OAc)₃ as two different precursors on the morphology and phase purity of LaVO₄ was investigated. To optimum the particle size of the products, sonication time and the kind of surfactants have been changed. The as-synthesized products were characterized by XRD, FT-IR, SEM, TEM, and EDS. Based on the obtained results, it was found that the size and shape of the sonochemically formed LaVO₄ nanoparticles were dramatically dependent on the sonication time, type of surfactant and lanthanum precursor. According to the XRD results, it was observed that pure tetragonal phase lanthanum orthovanadate (t-LaVO₄) could be obtained only by using [La(acac)₃·3H₂O] as precursor under ultrasound irradiation for 30 min. On the other hand, monoclinic phase lanthanum orthovanadate (m-LaVO₄) with poor crystallinity has been produced by vigorous stirring at room temperature without sonication.     

Synthesis and characterization of a new nano lead(II) 0-D coordination supramolecular compound: A precursor to produce pure phase nano-sized lead(II) oxide

Nano-structure of a new 0D Pb(II) coordination supramolecular compound, [Pb₄(8-Quin)₆](ClO₄)₂(1), L = 8-HQuin = 8-hydroxyquinolin ligand has been synthesized by use of a sonochemical process and characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and elemental analyses. The structure of compound 1 was determined by single-crystal X-ray diffraction. The single crystal X-ray data of compound 1 implies that the Pb⁺² ions are five coordinated. Each lead atom is coordinated to nitrogen and oxygen atoms of 8-hydroxyquinolin ligand. Topological analysis shows that the compound 1 is 1,2,3,4,4M12-1net. Nanoparticles of lead(II) oxide have been prepared by calcination of lead(II) coordination polymer at 500 °C that were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRPD) and IR spectroscopy.     

Sonochemical synthesis of nanoscale mixed-ligands lead(II) coordination polymers as precursors for preparation of Pb2(SO4)O and PbO nanoparticles; thermal,structural and X-ray powder diffraction studies

Nano-structures of two new Pb(II) two-dimensional coordination polymers, [Pb(μ-4-pyc)(μ-NCS)(μ-H₂O)]_n (1) and [Pb(μ-4-pyc)(μ-N₃)(μ-H₂O)]_n (2), 4-Hpyc = 4-pyridinecarboxylic acid were synthesized by a sonochemical method. The new nano-structures were characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. Compounds 1 and 2 were structurally characterized by single crystal X-ray diffraction and consist of two-dimensional polymeric units. The thermal stability of compounds 1 and 2 were studied by thermal gravimetric and differential thermal analyses and compared. Pb₂(SO₄)O and PbO nanoparticles were obtained by calcination of the nano-structures of compounds 1 and 2 at 600 °C, respectively.