New synthesis of mullite. Structural evolution study by 17O, 27Al and 29Si MAS NMR spectroscopy

Mullite has been prepared from a new combination of precursors. An aluminum alkoxide, aluminium isopropoxide, and silicon tetrachloride, are hydrolysed in tetrahydrofuran solution by ¹⁷O enriched water. The resulting powder is chemically homogeneous, crystallizing into mullite at 980°C. The structural evolution has been studied by DTA, TGA, XRD and ¹⁷O, ²⁷Al and ²⁹Si MAS NMR spectroscopy.     

From Al4B2O9 nanowires to BN-coated Al18B4O33 nanowires

A novel route was proposed to completely coat aluminum borate nanowires by in situ providing the precursor for BN coating. Uniformly BN-coated Al18B4O33 nanowires could be obtained by the reaction of Al4B2O9 nanowires with ammonia at high temperature. The high-temperature unstable Al4B2O9 nanowires were converted into Al18B4O33 nanowires, simultaneously evaporated boron oxide. The reaction between the in situ generated vapors and ammonia ensures that the BN layers are attached tightly on the surface of the as-formed Al18B4O33 nanowires.     

Preparation and Characterization of Al8.31Si1.91Mg3.78O20/Al4.8Si1.2O9.6/Mg2.0Al4.02Si4.98O18 Multiphase Material

A two-step sintering method was used to prepare Al8.31Si1.91Mg3.78O20 (corundum solid solution)/Al4.8Si1.2O9.6 (mullite solid solution)/Mg2.0Al4.02Si4.98O18 (cordierite solid solution) multiphase material, for the purposes of making these three crystal structures have point defects which could help the particles diffuse and transfer at high temperature, accelerate the sintering efficiently and enhance the material strength as well as the bulk density. The impacts of different formulas on the structure and properties of the multiphase material were investigated. With XRD and SEM analyses, for each sample, the crystal structure and microstructure were characterized, the crystalline phase content and cell parameters were determined with Rietveld Quantification software, and the properties were tested. The comparative optimal formula determined was calcinated chamotte of 80wt% and calcinated sludge of 20wt%; and its corresponding bending strength and retention rate of bending strength after a thermal shock were 29.74 MPa and 80.15%, respectively.     

Fluoride-assisted trifluoromethylation of aromatic thiones with (trifluoromethyl)trimethylsilane

In the presence of a stoichiometric amount of Bu₄NF·3H₂O, (trifluoromethyl)trimethylsilane reacts with aromatic thiones in both thiophilic and carbophilic ways to deliver, in medium yield, a mixture of (trifluoromethylthio)diarylmethane and 1,1-diaryl-2,2,2-trifluoroethanethiol, the former product being the major one.     

Die Kristallstruckturen von TiSi,Ti(Al,Si)2 und Mo(Al,Si)2

Zusammenfassung Es werden die Kristallstrukturen der Silicidphasen: TiSi, TiAl_0,3–0,6Si_1,7–1,4 und MoAl_1,3Si_0,7 ermittelt. TiSi ist mit der FeB-Struktur isotyp, wie bereits früher festgestellt wurde. Die Gitterparameter sind:a=6,53₁,b=3,63₁ undc=4,98₇ kX. E. Die Struktur TiAl_0,3–0,6Si_1,7–1,4 kann zum ZrSi₂-Typ gerechnet werden, ist aber pseudotetragonal:a=c=3,58₃–3,61₁ undb=13,49 kX. E. Neben Mo(Si,Al)₂ mit C 40-Typ besteht noch eine weitere Al-reichere, ternäre Kristallart MoAl_1,3Si_0,7 mit TiSi₂-Typ. Die Gitterparameter errechnen sich zu:a=8,23₉,b=4,78₃ undc=8,75₈ kX. E.     

Unidirectional Pt silicide nanowires grown on vicinal Si(100)

We investigated the structure and electronic properties of unidirectional Pt(2)Si nanowires (NWs) grown on a Si(100)-2 degrees off surface. We found that Pt(2)Si NWs were formed along the step edges of the Si(100)-2 degrees off surface with c(4x6) reconstructions that occurred on the terraces of Si(100) using scanning tunneling microscopy and the structure of formed NWs was found to be Pt(2)Si by core-level photoemission spectroscopy. Moreover, we confirmed that the electronic band structures of the NWs along the NW direction are different from those perpendicular to the NWs and the surface state induced by the Pt(2)Si NWs was observed with a small density of state using the angle-resolved photoemission spectra.     

Formation of well-aligned ZnGa(2)O(4) nanowires from Ga(2)O(3)/ZnO core-shell nanowires via a Ga(2)O(3)/ZnGa(2)O(4) epitaxial relationship

Formation of well-aligned and single-crystalline ZnGa(2)O(4) nanowires on sapphire (0001) substrates has been achieved via annealing of the Ga(2)O(3)/ZnO core-shell nanowires. Ga(2)O(3)/ZnO core-shell nanowires were prepared using a two-step method. The thickness of the original ZnO shell and the thermal budget of the annealing process play crucial roles for preparing single-crystalline ZnGa(2)O(4) nanowires. Structural analyses of the annealed nanowires reveal the existence of an epitaxial relationship between ZnGa(2)O(4) and Ga(2)O(3) phases during the solid-state reaction. A strong CL emission band centered at 360 nm and a small tail at 680 nm are obtained at room temperature from the single-crystalline ZnGa(2)O(4) nanowires.     

Microstructures of Alkoxide-Derived Barium Osumilite (BaMg2Al6Si9O30) Glass Ceramics

The crystallisation sequence of stoichiometric barium osumilite prepared by partial-alkoxide (PAR) and all-alkoxide routes (AAR) and the microstructure of the fully crystallised glass ceramic were examined. Comparing the crystallisation behaviours of the gel-glasses obtained revealed that the first phase to crystallise was mullite in PAR but hexacelsian in AAR. Barium osumilite crystals grew randomly and more homogeneously in PAR while in AAR larger barium osumilite crystals grew in clusters. Cordierite formed as a secondary phase in both routes and it crystallised on and between the osumilite lamellae. Mullite and hexacelsian also persisted up to the stage when full crystallisation and taken place.     

Cubic aluminum silicides RE8Ru12Al49Si9(Al(x)Si12-x) (RE = Pr, Sm) from liquid aluminum. Empty (Si,Al)12 cuboctahedral clusters and assignment of the Al/Si distribution with neutron diffraction.

Two new quaternary aluminum silicides, RE8Ru12Al49Si9(Al(x)Si12-x) (x approximately 4; RE = Pr, Sm), have been synthesized from Sm (or Sm2O3), Pr, Ru, and Si in molten aluminum between 800 and 1000 degrees C in sealed fused silica tubes. Both compounds form black shiny crystals that are stable in air and NaOH. The Nd analog is also stable. The compounds crystallize in a new structural type. The structure, determined by single-crystal X-ray diffraction, is cubic, space group Pm3m with Z = 1, and has lattice parameters of a = 11.510(1) A for Sm8Ru12Al49Si9(Al(x)Si12-x) and a = 11.553(2) A for Pr8Ru12Al49Si9(Al(x)Si12-x) (x approximately 4). The structure consists of octahedral units of AlSi6, at the cell center, Si2Ru4Al8 clusters, at each face center, SiAl8 cubes, at the middle of the cell edges, and unique (Al,Si)12 cuboctohedral clusters, at the cell corners. These different structural units are connected to each other either by shared atoms, Al-Al bonds, or Al-Ru bonds. The rare earth metal atoms fill the space between various structural units. The Al/Si distribution was verified by single-crystal neutron diffraction studies conducted on Pr8Ru12Al49Si9(Al(x)Si12-x). Sm8Ru12Al49Si9(Al(x)Si12-x) and Pr8Ru12Al49Si9(Al(x)Si12-x) show ferromagnetic ordering at Tc approximately 10 and approximately 20 K, respectively. A charge of 3+ can be assigned to the rare earth atoms while the Ru atoms are diamagnetic.     

Preparation of Si/O/C nanotubes using Ge nanowires as template

The silicon oxycarbide Si/O/C nanotubes were prepared by two-step procedure. First, a nanostructure deposit mainly composed of nanocables with germanium core was synthetized by low pressure chemical vapor deposition (LPCVD) using hexamethyldigermane Ge₂Me₆ and 1,1,3,3-tetramethyldisilazane (Me₂SiH)₂NH as the volatile precursors. Second, LPCVD was followed by annealing at 850 °C in vacuum to evaporate germanium core. As a result Si/O/C nanotubes were formed. Various techniques such as Raman spectroscopy, TEM, SEM/EDX, XPS and HRTEM were used to study the physical and chemical properties.     

IR study of dickite-formamide intercalate, Al2Si2O5(OH)4-H2NCOH

Direct intercalation of formamide (FAM) in dickite occurs spontaneously when samples are treated by ultrason. The X-ray diffraction patterns show that this intercalation increases the d001 spacing from 7.19 to 10.77 A. It is concluded from infrared studies that hydrogen bonds are formed between C=O groups of formamide and inner surface hydroxyls of dickite, indicated by the shift of the hydroxyl bands from 3708, 3654 cm(-1) and 3622 for natural dickite to 3575, 3520, 3450 and 3612 cm(-1) for FAM-intercalated dickite.     

A synthesis of high-efficiency Pd-Cu-Cl(x)/Al(2)O(3) catalyst for low temperature CO oxidation

Pd-Cu-Cl(x)/Al(2)O(3) catalysts were prepared by a NH(3) coordination-impregnation method and exhibited an excellent activity for low-temperature CO oxidation and 100% CO conversion was obtained at -30 °C for 400 ppm CO and 1000 ppm H(2)O/air.     

Selective growth of ag nanowires on Si(111) surfaces by electroless deposition

Electroless deposition of Ag on atomically flat H-terminated Si(111) surfaces in aqueous alkaline solutions containing Ag ions produced two different sizes of Ag nanowires along atomic step edges: (1) a narrow nanowire of 10 nm in width and 0.5 nm in height and (2) a wide nanowire of 35 nm in width and 11 nm in height. The narrow and wide nanowires were formed by immersion in the solutions containing less than 1 ppb and 8 ppm dissolved-oxygen concentrations, respectively. This result indicates that the dissolved oxygen initiates the formation of Ag nucleation sites and that the fabrication method has a possibility of controlling the size of Ag nanowires.     

Phase range of the type-I clathrate Sr8Al(x)Si(46-x) and crystal structure of Sr8Al10Si36

Samples of the type-I clathrate Sr(8)Al(x)Si(46-x) have been prepared by direct reaction of the elements. The type-I clathrate structure (cubic space group Pm3n) which has an Al-Si framework with Sr(2+) guest atoms forms with a narrow composition range of 9.54(6) ≤ x ≤ 10.30(8). Single crystals with composition A(8)Al(10)Si(36) (A = Sr, Ba) have been synthesized. Differential scanning calorimetry (DSC) measurements provide evidence for a peritectic reaction and melting point at ～1268 and ～1421 K for Sr(8)Al(10)Si(36) and Ba(8)Al(10)Si(36), respectively. Comparison of the structures reveals a strong correlation between the 24k-24k framework sites distances and the size of the guest cation. Electronic structure calculation and bonding analysis were carried out for the ordered models with the compositions A(8)Al(6)Si(40) (6c site occupied completely by Al) and A(8)Al(16)Si(30) (16i site occupied completely with Al). Analysis of the distribution of the electron localizability indicator (ELI) confirms that the Si-Si bonds are covalent, the Al-Si bonds are polar covalent, and the guest and the framework bonds are ionic in nature. The Sr(8)Al(6)Si(40) phase has a very small band gap that is closed upon additional Al, as observed in Sr(8)Al(16)Si(30). An explanation for the absence of a semiconducting "Sr(8)Al(16)Si(30)" phase is suggested in light of these findings.     

Facile synthesis of the tridecameric Al13 nanocluster Al13(mu3-OH)6(mu2-OH)18(H2O)24(NO3)15

Treatment of aluminum nitrate with an organic nitroso-containing compound yields the "flat", tridecameric nanocluster Al 13(mu 3-OH) 6(mu 2-OH) 18(H 2O) 24(NO 3) 15 ( Al 13 ) in good yield on a preparative scale under ambient conditions. Synthetic procedures yielding two different single-crystal forms of the Al 13 cation with two varying counterion compositions are described.