Synthesis and Study of Sr[HSiUO6]2·2H2O and Ba[HSiUO6]2·2H2O

Uranosilicates of the general formula M^{I I}[HSiUO₆]₂·2H₂O (M^{I I} = Sr, Ba) were prepared by hydrothermal synthesis. Previously unknown intermediate crystal hydrates were separated and studied by X-ray diffraction (XRD), IR spectroscopy, and thermal analysis. Polymorphic transitions -Sr[HSiUO₆]₂ -Sr[HSiUO₆]₂ and -Ba[HSiUO₆]₂ -Ba[HSiUO₆]₂ were revealed at 700 and 780°C, respectively.     

Photocatalytic Properties of the MgHPO4·3H2O and MgKPO4·6H2O Phosphates

Inorganic Materials - Magnesium double phosphates, MgHPO4·3H2O and MgKPO4·6H2O, isostructural with the minerals newberyite and struvite-K have been synthesized in powder form via...     

Phase diagram of the Na2CO3 · 10H2O-Na2S2O3 · 5H2O system

Using thermal analysis, we have constructed the phase diagram of the crystalline hydrate system Na₂CO₃ · 10H₂O-Na₂S₂O₃ · 5H₂O, which has been shown to have eutectic phase relationships. The eutectic composition is 27 wt % Na₂CO₃ · 10H₂O + 73 wt % Na₂S₂O₃ · 5H₂O, and the eutectic temperature is T _e = ?0.92°C. We have determined the enthalpy of fusion of the alloys in this system and evaluated the activities of their components both at the liquidus temperatures and in metastable regions. The composition dependences of the above thermodynamic characteristics are shown to correlate with each other and to have extreme values at the eutectic composition. The results obtained lead us to recommend the eutectic mixture of the crystalline hydrates in this system as a heat storage material.     

Synthesis and study of hydrated uranium(VI) oxides, UO3·nH2O

A procedure was developed for preparing synthetic schoepite [(UO₂)₈O₂(OH)₁₂](H₂O)₁₂ (UO₃·2.25H₂O). The dehydration and thermal decomposition of this compound were studied by X-ray diffraction, IR spectroscopy, and differential scanning calorimetry. The relationship between schoepite and other hydrated forms of uranium(VI) oxide was found.     

Synthesis and structure of actinide(VII) compounds Rb3NpO4(OH)2·3H2O and Rb3PuO4(OH)2·3H2O

Actinide(VII) salts Rb₃[NpO₄(OH)₂]·3H₂O (I) and Rb₃[PuO₄(OH)₂]·3H₂O (II) were prepared as single crystals and examined by X-ray diffraction. The compounds are isostructural and crystallize in the monoclinic system, space group C2/c, Z = 4; unit cell parameters: a = 12.1544(3), b = 10.9942(2), c = 7.789(2) ?, ?? = 91.0930(11)° for I and a = 12.1254(3), b = 10.9506(2), c = 7.7699(2) ?, ?? = 90.8253(12)° for II. The main structural elements of I and II are centrosymmetrical anions [AnO₄(OH)₂]^3? forming together with water molecules, owing to strong hydrogen bonding, chains oriented along [101]. In [AnO₄(OH)₂]^3? anions, the central An(VII) atom has a tetragonal-bipyramidal oxygen surrounding. The An-O(OH) interatomic distances decrease in going from I to II owing to actinide contraction by a factor of ??2 more strongly than the An-O bond lengths in the equatorial planes of the bipyramids. The previously studied structure of Cs₃[NpO₄(OH)₂]·3H₂O (III) was refined.     

Synthesis of H2Ti2O3·H2O nanotubes and their effects on the flame retardancy of bamboo fiber/high-density polyethylene composites

H₂Ti₂O₃·H₂O nanotubes (TNTs) were prepared through hydrothermal synthesis and dispersed in bamboo fiber/HDPE (BH) composites to improve the flame retardancy of the composites. TEM observation showed that TiO₂ particles were transformed into TNTs through hydrothermal treatment at 120 °C for 12 h in 8 M NaOH solution. Then, a cone calorimeter and a limiting oxygen index chamber were used to evaluate the effects of the TNTs on the flame retardancy of the BH composites. Results demonstrated that TNTs definitely improved the flame retardancy of BH composites by absorbing decomposition products from combustion due to its large specific area and tubular structure. Additionally, the TNTs reduced the free volume in the microzone, strengthened the molecular chain rigidity, and then contributed to the thermostability and flame retardancy of the BH composites.     

Synthesis and characterization of Cu2O·TeO2 and CuI·Cu2O·TeO2 glasses

Cu₂O·TeO₂ and CuI·Cu₂O·TeO₂ glasses were synthesized and characterized by complex impedance measurement, Raman spectroscopy, X-ray photoelectron spectroscopy, and atomic force microscopy techniques. Samples of the binary and the ternary systems are found to have both Cu⁺ and Cu²⁺ with their relative concentration being composition dependent. Bonds like -O-Cu²⁺-O-, leading to the formation of bridging oxygen are found to form in the binary system. Structural units like (Te₃O₈ ^4–)_n are also found to form when Cu₂O content is high in the binary system. Phase separation is observed in the ternary system. The glass structure and hence the ionic conduction behavior are found to depend upon chemical composition. When CuI content exceeds 60 mol%, the crystalline phase of -Cul gets stabilized at room temperature, thus causing the enhancement in conductivity.     

Synthesis and characterization of Mu-11: a porous sodium trisilicate Na2Si3O7·H2O with 10-membered ring openings

The title compound (named Mu-11) is a new type of sodium trisilicate which was synthesized by using the quasi non-aqueous route in the presence of ethylene glycol as solvent. This material was characterized by XRD, SEM, ²⁹Si solid-state MAS NMR spectroscopy, elemental and thermal analyses. The structure was determined by single-crystal X-ray diffraction. The symmetry is monoclinic, space group P2₁/c, a=7.3087(8)Å, b=12.7246(13)Å, c=9.0913(11)Å, β=119.01(1)° and V=739.39(10) ų. The structure consists of corrugated sheets built from four-, six- and eight-membered ring units. The connection of such sheets leads to a three-dimensional framework with a monodimensional channel system delimited by a 10-ring aperture. After heating to 300°C another novel phase crystallizes, which is stable up to 600°C.     

Novel self-assembled decavanadate clusters forming 1D molecular chains and 2D molecular arrays: [HMTA-H···H2O][HMTA-CH2OH][H3V10O28{Na(H2O)4}]·4H2O and [Na2(H2O)10] [H3V10O28 {Na(H2O)2}]·3H2O

Two novel materials, [HMTA-H··H₂O] [HMTA-CH₂OH] [H₃V₁₀O₂₈[Na(H₂O)₄}]·4H₂O, 1 and [Na₂(H₂O)₁₀][H₃V₁₀O₂₈[Na(H₂O)₂}]·3H₂O, 2 containing decavanadate clusters interconnected through hydrated sodium cations forming 1D molecular chains and 2D molecular arrays have been self-assembled from acidified, aqueous vanadate solution in the presence of organic bases, hexamethylenetetramine and 1,3,5-triazine respectively.     

X-ray powder diffraction and IR study of NaMg(H2O)2[BP2O8]·H2O and NH4Mg(H2O)2[BP2O8]·H2O

NaMg(H₂O)₂[BP₂O₈]·H₂O was prepared by hydrothermal synthesis and was characterized by X-ray powder difraction and IR method. The title compound was synthesized from MgCl₂·6H₂O, NaBO₃·4H₂O, and (NH₄)₂HPO₄ with variable molar ratios using hydrothermal method by heating at 165 °C for 3 days. The X-ray powder diffraction data was indexed in hexagonal system, the unit cell parameters were found to be as a = 9.428, c = 15.82 Å, Z = 4 and the space group is P6₁22. It is isostructural with M^lM^ll(H₂O)[BP₂O₈] type compounds where M^l = Na, K; M^ll = Mg, Mn, Fe, Co, Ni and Zn. In addition NH₄Mg(H₂O)₂[BP₂O₈]·H₂O was also synthesized the first time in this research. Its unit cell parameters and hkl values were in good agreement with the sodium magnesium compound. The unit cell parameters are a = 9.529, c = 15.736 Å. The indexed X-ray powder diffraction data of both compounds which were not reported in the literature is presented in this work. The IR data of NaMg(H₂O)₂[BP₂O₈]·H₂O is also reported.     

Synthesis and characterization of a new organic sulphate, [2,3-(CH3)2C6H3NH3]HSO4·H2O

Crystals of a new hybrid compound C₈H₁₂N⁺, HSO₄^?·H₂O were synthesized in aqueous solution and characterized by X-ray diffraction and IR absorption spectroscopy. This compound crystallizes in the orthorhombic non-centrosymmetrical space group P2₁2₁2₁ and an unit cell with a = 5.74(2) Å, b = 9.17(2) Å, c = 21.34(4) Å, V = 1124(6) Å³, and Z = 4. Its crystal structure is a packing of alternated inorganic and organic layers parallel to (a,b) planes. The different components are connected by a bi-dimensional network of strong OH…O and NH…O hydrogen bonds. Then, in order to detect phase transitions and watch changes in the conductivity behaviour, investigations by DTA–TG and differential scanning calorimetry (DSC) and electrical conductivity measurements were carried out.     

Synthesis and structure of Cs3[UO2(CH3COO)3]2(NCS)·H2O

The compound Cs₃[UO₂(CH₃COO)₃]₂(NCS)·H₂O (I) was synthesized and studied by IR spectroscopy and single crystal X-ray diffraction. Compound I crystallizes in the monoclinic system with the following unit cell parameters: a = 7.8286(9), b = 19.892(2), c = 20.050(2) Å, β = 94.527(2)°, space group P2₁/c, Z = 4, R = 0.0387. The uranium-containing structural units in crystals of I are mononuclear complexes [UO₂(CH₃COO)₃]^? belonging to crystal-chemical group AB ₃ ⁰¹ (A = UO ₂ ²⁺ , B⁰¹ = CH₃COO^?) of uranyl complexes.     

Complexes with substituted 2,5-dihydroxy-p-benzoquinones: The inclusion compounds [Y(H2O)3]2 (C6Cl2O4)3·6.6H2O and [Y(H2O)3]2 (C6Br2O4)3·6H2O

Single crystal of [Y(H₂O)₃]₂ (C₆Br₂O₄)₃·6H₂O and [Y(H₂O)₃]₂ (C₆Cl₂O₄)₃·6.6H₂O were grown in aqueous silicagel. The compounds are in principle isostructural. In Y chloranilate one additional water site is occupied as verified by X-ray single crystal structure analysis. Y³⁺ is nine-coordinated by three water molecules and six oxygen atoms of the bischelating (C₆X₂O₄)²⁻ ions (XCl, Br). The coordination polyhedron is an only slightly distorted tri-capped trigonal prism. The connection of Y³⁺ with the dianions leads to infinite, corrugated layers. The layer stacking yields cage-like cavities in which water molecules are accomodated. Hydrogen bonds interlink adjacent layers. Further hydrogen bonds involve the entrapped water molecules. DSC measurements indicated a complicated dehydration process which caused right at the start destruction of the single crystals.     

X-ray Diffraction Study of Y2W3O12· 3H2O

Under ordinary conditions, yttrium tungstate exists in the form of the trihydrate Y₂W₃O₁₂· 3H₂O and has a monoclinic structure (sp. gr. P2/m; a= 14.308 Å, b= 4.354 Å, c= 12.430 Å, = 119.78°). The dehydration Y₂W₃O₁₂· 3H₂O Y₂W₃O₁₂occurs at 142°C.     

Effect of Bi2O3 on structural and optical properties of Li2O·PbO·Bi2O3·B2O3 glasses

Journal of Materials Science: Materials in Electronics - The quaternary glass system has a composition of 30Li2O·20PbO·xBi2O3·(50-x)B2O3 (where x?=?0, 10, 20, 30, and...     

Fabrication and properties of SiC fibre-reinforced Li2O·Al2O3·6SiO2 glass-ceramic composites

Ta₂O₅, Nb₂O₅ and TiO₂ were used separately as additives to a Li₂O·Al₂O₃·6SiO₂ glass-ceramic composition, to act as nucleating dopants and to aid the formation of an interfacial carbide layer (TaC and NbC) between the fibre and matrix in SiC fibre uniaxially reinforced glass-ceramic composites, The composites exhibited high modulus of rupture (>800 MPa) and fracture toughness (K _IC > 15 MPam^1/2). The interfacial amorphous carbon rich layer and carbide layer were responsible for lowered interfacial shear strength but permitted high composite fracture toughness. The composite with the TiO₂ additive in the matrix showed a lower flexural strength (<500MPa) and a smaller K _IC (-11 MPam^1/2) which resulted from the high interfacial shear strength between the SiC fibre and the matrix due to the formation of the interfacial TiC layer.     

Synthesis, Physicochemical Properties, and Electrode Behavior of Ni2[Ni(OH)6W6O18 ] · 8H2O

Nickel(II) hexatungstonickelate(II) was synthesized and characterized by elemental analysis, x-ray diffraction, thermal analysis, IR spectroscopy, and ¹H nuclear magnetic resonance. The results demonstrate that constitutional water is present in the form of OH groups, which can be removed by heating to 230–370°C. The chemical formula of the compound is Ni₂[Ni(OH)₆W₆O₁₈] · 8H₂O. Nickel(II) hexatungstonickelate(II), a poorly soluble compound, was tested as an electrode for Ni(II) determination in solution. Its electrode properties and selectivity for other ions suggest that it is a promising material for such applications. At pH 5, the ion-selective electrode we fabricated has a Nernstian response to Ni(II) (10^–5 to 10^–1 mol/l) which is close to that predicted theoretically.