The crystal structures and physical properties of the solid solution compound Ba5Y8-xMn4O21-1.5x (x=0, 1)

New oxometallides with the formula Ba5Y8 xMn4O21 1.5x(x = 0,1) are prepared through an atmospherecontrolled solid-state reaction.Two single-phase samples with Ba/Y/Mn atomic ratios 5/8/4(Y8) and 5/7/4(Y7) are obtained.The crystal structures and the physical properties of the compounds are investigated by X-ray powder diffraction,magnetization,conductivity,and dielectricity measurements.The Ba5Y8 xMn4O21 1.5x compound is demonstrated to be a Y-deficient solid solution.The solid solution compound Ba5Y8 xMn4O21 1.5x crystallizes into tetragonal symmetry with the space group I4/m.Detailed structure analysis by Rietveld refinement of the X-ray powder diffraction data reveals that the Y vacancies occur preferentially at the Y(2) site.Thermal magnetization measurements indicate the presence of antiferromagnetic interaction between Mn ions in the compounds,and temperature-dependent resistivity measurements show that insulator-semiconductor transitions occur around 175 K and 170 K for the Y8 and Y7 samples,respectively.Strong frequency dependences of the dielectric constant are observed above ～175 K for the two compounds.     

The crystal structures and physical properties of the solid solution compound Ba₅Y_8-xMn₄O_21-1.5x（x = 0,1）

New oxometallides with the formula Ba5Y8 xMn4O21 1.5x(x = 0,1) are prepared through an atmospherecontrolled solid-state reaction.Two single-phase samples with Ba/Y/Mn atomic ratios 5/8/4(Y8) and 5/7/4(Y7) are obtained.The crystal structures and the physical properties of the compounds are investigated by X-ray powder diffraction,magnetization,conductivity,and dielectricity measurements.The Ba5Y8 xMn4O21 1.5x compound is demonstrated to be a Y-deficient solid solution.The solid solution compound Ba5Y8 xMn4O21 1.5x crystallizes into tetragonal symmetry with the space group I4/m.Detailed structure analysis by Rietveld refinement of the X-ray powder diffraction data reveals that the Y vacancies occur preferentially at the Y(2) site.Thermal magnetization measurements indicate the presence of antiferromagnetic interaction between Mn ions in the compounds,and temperature-dependent resistivity measurements show that insulator-semiconductor transitions occur around 175 K and 170 K for the Y8 and Y7 samples,respectively.Strong frequency dependences of the dielectric constant are observed above ～175 K for the two compounds.     

Superconductivity in LiTi2O4 Prepared by Hybrid Microwave Method

The well-known superconducting oxide LiTi2 04 has a structural phase transition from spinel to ramsdellite around 900℃. We have successfully obtained the superconducting spinel phase and the non-superconducting ramsdellitephase of LiTi2O4 using a hybrid microwave method. The samples are characterized by x-ray powder diffraction, scanning electron microscopy, and measurements of resistivity and magnetic susceptibility. The results show thatthe low-temperature spinel phase is a superconductor with Tc=13K, while the high-temperature ramsdellite phase is a semiconductor. By comparison between the crystal structures of the spinel and the ramsdellite phases, it is suggested that the geometrical frustration plays an important role in the superconductivity of the spinel LiTi2O4.     

High-pressure Raman study of MgV2O6 synthesized at high pressure and high temperature

A new structural phase of MgV2O6 was obtained by a high-pressure,high-temperature(HPHT) synthesis method.The new phase was investigated by the Rietveld analysis of X-ray powder diffraction data,showing space group Pbcn(No.60) symmetry and a = 13.6113(6) (1 = 0.1 nm),b = 5.5809(1) ,c = 4.8566(3) ,V = 368.93(2) 3(Z = 4).High pressure behavior was studied by Raman spectroscopy at room temperature.Under 22.5 GPa,there was no sign of a structural phase transition in the spectra,demonstrating stability of the HPHT phase up to the highest pressure.     

Anti-HepG-2 Cell Properties of Rare Earth Tungstosilicic Polyoxometalates Containing 5-Fluorouracil

Two novel rare earth tungstosilicic polyoxometalate containing 5-fluorouracil,K26(C4H4FN2O2)8Pr(SiW11O39)4·10H2O(FPSW) and K26(C4H4FN2O2)8Sm(SiW11O39)4·9H2O(FSSW),were synthesized and their structure were characterized by using elemental analysis,FTIR spectra,X-ray powder diffraction and TG.The antitumor activity tests of the compounds FPSW and FSSW were carried out by the methyl thiazolyl tetrazolium method in hepatocellular carcinoma cell HepG-2.The results showed that FPSW and FSSW could inhibit the HepG-2 cells in vitro significantly.The EC50 of FPSW and FSSW is 1.94×10-5 and 1.32×10-5 mol·L-1 respectively.The therapeutic index of FPSW and FSSW is 0.76 and 1.58 respectively.     

R-site cation randomness effect in the A-site ordered Y0.5La0.5BaMn2O6 compound

The R/Ba-ordered and R-site mixed compound Y0.5La0.5BaMn2O6 is synthesized, in which (Y, La) and Ba are regularly arranged, while Y and La randomly occupy the R-site. Y0.5La0.5BaMn2O6 has a tetragonal unit cell with a space group of P4/mmm. A structural transition between tetragonal and orthorhombic is observed at about 325 K by X-ray powder diffraction (XRD). Thermal magnetic measurement shows the occurrence of an antiferromagnetic transition at the temperature TN～190 K. Anomalies in magnetization, resistivity and lattice parameters observed around 340 K indicate a charge/orbital order transition accompanying the structural phase transition. The R-site randomness effect is discussed to interpret the different properties of Y0.5La0.5BaMn2O6 between NdBaMn2O6 and SmBaMn2O6.     

Temperature dependences of optical properties,chemical composition,structure,and laser damage in Ta2O5 films

Ta2O5 films are prepared by e-beam evaporation with varied deposition temperatures,annealing temperatures,and annealing times.The effects of temperature on the optical properties,chemical composition,structure,and laserinduced damage threshold(LIDT) are systematically investigated.The results show that the increase of deposition temperature decreases the film transmittance slightly,yet annealing below 923 K is beneficial for the transmittance.The XRD analysis reveals that the film is in the amorphous phase when annealed below 873 K and in thehexagonal phase when annealed at 1073 K.While an interesting near-crystalline phase is found when annealed at 923 K.The LIDT increases with the deposition temperature increasing,whereas it increases firstly and then decreases as the annealing temperature increases.In addition,the increase of the annealing time from 4 h to 12 h is favourable to improving the LIDT,which is mainly due to the improvement of the O/Ta ratio.The highest LIDT film is obtained when annealed at 923 K,owing to the lowest density of defect.     

Subsolidus phase relation in the Bi_2O_3–Fe_2O_3–La_2O_3 system

Bismuth-containing semiconductor material is a hot topic in photocatalysts because of its effective absorption under the visible light.In this paper,we expect to explore a new bismuth-based photocatalyst by studying the subsolidus phase relations of the Bi2O3–Fe2O3–La2O3system.The X-ray diffraction data shows that in this ternary system the ternary compound does not exist,while seven binary compounds(including one solid solution series Bi1 xLaxO1.5with 0.167≤x≤0.339)are obtained and eight compatibility triangles are determined.     

Subsolidus phase relation in the Bi2O3-Fe203-La2O3 system

Bismuth-containing semiconductor material is a hot topic in photocatalysts because of its effective absorption under the visible light. In this paper, we expect to explore a new bismuth-based photocatalyst by studying the subsolidus phase relations of the Bi2O3-Fe2O3-La2O3 system. The X-ray diffraction data shows that in this ternary system the ternary compound does not exist, while seven binary compounds （including one solid solution series Bi1-xLaxO1.5 with 0.167 〈 x 〈 0.339） are obtained and eight compatibility triangles are determined.     

Phase Transition and EOS of Cinnabar （α-HgS） at High Pressure and High Temperature

Phase relations and equation of state （EOS） of natural cinnabar （α-HgS） are investigated by high-pressure and high-temperature synchrotron x-ray powder diffraction. The unambiguous cinnabar-rocksalt structure phase boundaries are determined to be PI （GPa）=15.54- 0.014T（℃） and Pupper（GPa）= 23.84- 0.014T（℃） at 300-623K. With K1 fixed at 4, we obtain K0 = 37（4） GPa, （aK/aT）p= -0.025（2） GPaK-1, and α0 = 3.79（20） × 10-5 K-1 for the cinnabar phase of α-HgS. The （aK/aT）p and α0 of cinnabar phase are obtained for the first time. A nearly isotropic compression of cinnabar phase is observed by linear regressions.     

Conductivity and water uptake of Sr4(Sr2Nb2)O11·nH2O and Sr4(Sr2Ta2)O11·nH2O

The hydrated oxygen deficient complex perovskite-related materials Sr₄(Sr₂Nb₂)O₁₁·nH₂O and Sr₄(Sr₂Ta₂)O₁₁·nH₂O were studied at high water vapour pressures over a large temperature range by electrical conductivity measurements, thermogravimetry (TG), and X-ray powder diffraction (XRPD). In humid atmospheres both materials are known to exhibit protonic conductivity below dehydration temperatures, with peak-shaped maxima at about 500 °C. In this work we show that the peaks expand to plateaus of high conductivity from 500 to 700 °C at a water vapour pressure of 1 atm. However, in situ synchrotron XRPD of Sr₄(Sr₂Nb₂)O₁₁·nH₂O as a function of temperature shows that these observations are in fact coincident with melting and dehydration of a secondary phase Sr(OH)₂. The stability of Sr₄(Sr₂Nb₂)O₁₁·nH₂O and Sr₄(Sr₂Ta₂)O₁₁·nH₂O in humid atmospheres is thus insufficient, causing decomposition into perovskites with lower Sr content and SrO/Sr(OH)₂ secondary phases. This, in turn, rationalizes the observation of peaks and plateaus in the conductivity of these materials.     

Al2O3-Y2O3-ZrO2三相复合陶瓷的介电谱研究

采用传统的固相反应法,在1400–1500 ℃下烧结,制备得到Al₂O₃-Y₂O₃-ZrO₂三相复合陶瓷.样品的结构、形貌和电性能分别用X射线衍射(XRD)、扫描电子显微镜(SEM)及介电谱表征.XRD表明此三相复合体系无其他杂相,加入Y₂O₃及ZrO₂后使得Al₂O₃成瓷温度降低;SEM表明此体系晶粒直径为200–500 nm,并且样品随烧结温度的升高而变得更加致密,晶界更加清晰;介电损耗谱中出现峰值弛豫现象,根据Cole-Cole复阻抗谱得出其为非德拜弛豫. 关键词： 2O₃-Y₂O₃-ZrO₂三相陶瓷')" href="#">Al₂O₃-Y₂O₃-ZrO₂三相陶瓷 介电弛豫 阻抗谱 热导率     

Structural properties of Al2O3 dielectrics grown on TiN metal substrates by atomic layer deposition

We investigated on the structural properties of Al₂O₃ dielectrics grown on TiN metal substrates using an atomic layer deposition technique with tri-methyl-aluminum and either O₃ or H₂O as the precursor and oxidant, respectively. The structural and morphological features of these films were examined by atomic force microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy measurements. We find that Al₂O₃ dielectric films with the O₃ oxidant exhibit a rough morphology, a thick TiO₂ film, and a small amount of contaminants such as carbon and hydrogen. The reason for the rapid diffusion of oxygen atoms into the TiN lattice leads to the formation of TiO₂ layer on the TiN substrate. This is due to the higher oxidation potential of the O₃ compared to the H₂O.     

Deposition and characterization of binary Al2O3/SiO2 coating layers on the surfaces of rutile TiO2 and the pigmentary properties

Binary Al₂O₃/SiO₂-coated rutile TiO₂ composites were prepared by a liquid-phase deposition method starting from Na₂SiO₃·9H₂O and NaAlO₂. The chemical structure and morphology of binary Al₂O₃/SiO₂ coating layers were investigated by Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, TG-DSC, Zeta potential, powder X-ray diffraction, and transmission electron microscopy techniques. Binary Al₂O₃/SiO₂ coating layers both in amorphous phase were formed at TiO₂ surfaces. The silica coating layers were anchored at TiO₂ surfaces via Si-O-Ti bonds and the alumina coating layers were probably anchored at the SiO₂-coated TiO₂ surfaces via Al-O-Si bonds. The formation of continuous and dense binary Al₂O₃/SiO₂ coating layers depended on the pH value of reaction solution and the alumina loading. The binary Al₂O₃/SiO₂-coated TiO₂ composites had a high dispersibility in water. The whiteness and brightness of the binary Al₂O₃/SiO₂-coated TiO₂ composites were higher than those of the naked rutile TiO₂ and the SiO₂-coated TiO₂ samples. The relative light scattering index was found to depend on the composition of coating layers.     

Effect of Li2O and CoO-doping of CuO/Fe2O3 system on its surface and catalytic properties

Physicochemical, surface and catalytic properties of pure and doped CuO/Fe₂O₃ system were investigated using X-ray diffraction (XRD), energy dispersive X-ray analysis (EDX), nitrogen adsorption at −196 °C and CO-oxidation by O₂ at 80-220 °C using a static method. The dopants were Li₂O (2.5 mol%) and CoO (2.5 and 5 mol%). The results revealed that the increase in precalcination temperature from 400 to 600 °C and Li₂O-doping of CuO/Fe₂O₃ system enhanced CuFe₂O₄ formation. However, heating both pure and doped solids at 600 °C did not lead to complete conversion of reacting oxides into CuFe₂O₄. The promotion effect of Li₂O dopant was attributed to dissolution of some of dopant ions in the lattices of CuO and Fe₂O₃ with subsequent increase in the mobility of reacting cations. CoO-doping led also to the formation of mixed ferrite Co_xCu_1−xFe₂O₄. The doping process of the system investigated decreased to a large extent the crystallite size of unreacted portion of Fe₂O₃ in mixed solids calcined at 600 °C. This process led to a significant increase in the S_BET of the treated solids. Doping CuO/Fe₂O₃ system with either Li₂O or CoO, followed by calcination at 400 and 600 °C decreased its catalytic activity in CO-oxidation by O₂. However, the activation energy of the catalyzed reaction was not much affected by doping.     

Bi2Ti2O7/Si薄膜的制备及C-V特性研究

采用化学溶液分解法(CSD)在Si衬底上制备了Bi₂Ti₂O₇薄膜.X射线双晶衍射和原子力显微镜检测表明,所制备的薄膜主要为Bi₂Ti₂O₇相的多晶材料.同时还研究了AuBi₂Ti₂O₇/n-Si(100)结构的电容电压(C-V)特性,结果表明,在Bi₂Ti₂O关键词： C-V特性 2Ti₂O₇薄膜')" href="#">Bi₂Ti₂O₇薄膜 电荷迁移     

Controlled synthesis of BaWO4 hierarchical nanostructures by exploiting oriented attachment in the solution of H2O and C2H5OH

Shape-controlled synthesis of BaWO₄ hierarchical nanostructures has been successfully achieved by exploiting oriented attachment in a mixture of water and ethanol. A controlled change in the volume ratio of C₂H₅OH and H₂O or the concentration of initial reagents has resulted in the synthesis of products of various morphologies, such as shuttle-like, ellipsoid-like, and flower-like ones. The obtained products are characterized by field emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray powder diffraction, and Fourier transform infrared spectroscopy. The altered nucleation and growth rates of primary particles that assembled to the final hierarchical nanostructures through oriented attachment are the main cause of the evolution of their morphologies. The room-temperature photoluminescent intensities of the products strongly depend on their morphology.     

Optical characteristics of amorphous V2O5 thin films colored by an excimer laser

The V₂O₅ films were prepared by an RF sputtering method, and the amorphous films were colored by an UV excimer laser. The crystallinity of the as-grown V₂O₅ film was degenerated greatly by laser irradiation, as determined by X-ray diffraction (XRD) and Raman studies. The transmission and complex refractive index spectra of the V₂O₅ film were affected by variations in the microstructure, including the surface morphology, crystalline structure, and substoichiometry with an oxygen deficiency. Considerable emissions due to oxygen vacancies and band transition of photoluminescence (PL) peaks were observed, and the peaks were significantly changed after laser irradiation. The variations in the optical properties in both films may be attributed to oxygen deficiency induced by laser irradiation.     

Emission analysis of Pr and Tm: Ca2Gd2W3O14 phosphors

5 mol% of Pr³⁺ and Tm³⁺ ions activated calcium gadolinium tungstate (Ca₂Gd₂W₃O₁₄₎ phosphors were synthesized by traditional solid state reaction method. Crystalline phase structure was identified from the X-ray diffraction (XRD) profiles. From the scanning electron microscopy (SEM) images, we have observed the agglomeration of the particles, and average grain size is around 40-300 nm. Using the energy dispersive X-ray analysis (EDAX) and Fourier transform infrared (FTIR) spectra, identified the elements and functional groups present in the prepared phosphors. The emission spectrum of Pr³⁺: Ca₂Gd₂W₃O₁₄ powder phosphors have shown an intense red emission at 615 nm with the excitation wavelength λ_exci=450 nm and thus these red color emitting powder phosphors are used as one of the components in the preparation of WLEDs. The excitation spectrum of Tm³⁺: Ca₂Gd₂W₃O₁₄ powder phosphor has shown a ligand to metal charge transfer (W-O) band (LMCT) within the WO₄²⁻ group. Emission spectrum of Tm³⁺: Ca₂Gd₂W₃O₁₄ phosphors have shown blue emissions at 453 nm (¹D₂→³F₄).     

A new self-activated yellow-emitting phosphor Zn2V2O7 for white LED

A new self-activated yellow-emitting Zn₂V₂O₇ phosphor was synthesized by high temperature solid-state reaction. X-ray powder diffraction (XRD) analysis confirmed the sample with monoclinic formation of Zn₂V₂O₇. The excitation and emission spectra indicated the phosphor can be efficiently excited by near ultraviolet (NUV) light in 220–400 nm range and exhibit a bright broad yellow emission with the highest emission intensity at 531 nm. The broad emission band from 400 to 650 nm can be attributed to the charge transfer transition in the VO₄ tetrahedra, which suggests that the phosphor is a promising yellow phosphor applied for white light-emitting diodes (WLED).