Sn3O4 single crystal nanobelts grown by carbothermal reduction process

This article reports on the growth of single crystal Sn₃O₄ nanobelts and SnO by a carbothermal reduction process in two different regions of a furnace tube. Even though intermediate tin oxide compounds (Sn₃O₄) have been observed experimentally, the study of structures based on them is a challenging task. Characterization data allowed us to propose that Sn₃O₄ nanobelts grew by vapor–solid mechanism while SnO grew by self-catalyst vapor–liquid–solid mechanism. Electrical measurements of a single Sn₃O₄ nanobelt were performed at different temperatures, revealing undoped semiconductor characteristics.     

Synthesis of Y2O3:Eu phosphors by bicontinuous cubic phase process

A novel approach for preparation of red-emitting europium-doped yttrium oxide phosphor (Y₂O₃:Eu) by using the bicontinuous cubic phase (BCP) process was reported in this paper. The BCP system was composed of anionic surfactant sodium bis(2-ethylhexyl)sulfosuccinate (AOT) and aqueous yttrium nitrate/europium nitrate solution. Energy dispersive spectrometer analysis revealed the homogeneous precipitation occurred in the BCP structure. Thermogravimetric analysis measurements indicated the precursor powder was europium-doped yttrium hydroxide, Y_1−xEu_x(OH)₃. Scanning electron microscopy micrographs showed the precursor powder had a primary size about 30 nm and narrow size distribution. After heat treatment in furnace above 700 °C for 4 h, high crystallinity Y₂O₃:Eu phosphors was obtained. However, the primary size of particles grew to 50–200 nm and the dense agglomerates with a size below 1 μm were formed. X-ray diffraction patterns indicated the crystal structure of precursor powders and Y₂O₃:Eu phosphors were amorphous and body-centered cubic structure, respectively. The photoluminescence analysis showed that the obtained Y₂O₃:Eu phosphor had a strong red emitting at 612 nm and the quenching started at a Eu concentration of 10 mol%. This study indicated that the BCP process could be used to prepare the highly efficient oxide-based phosphors.     

Synthesis and characteristics of Na-doped Bi4Ti3O12 thin films on Si substrate

Bi_3.25Na_2.25Ti₃O₁₂ thin films were prepared on p-Si(1 1 1) substrate by a metalorganic solution decomposition (MOSD) method. The structural characteristic and crystallization of the films were examined by X-ray diffraction. The current–voltage characteristic shows ohmic conductivity in the lower voltage range and space-charge-limited conductivity in the higher voltage range. The dielectric constant is 53 at a frequency of 100 kHz at room temperature and the dissipation factor exists at a minimal value of 0.02 at a frequency of 200 kHz. The retention time estimated by measuring capacitance is about 10⁶ s. Nonhysteretic C–V curves at various frequencies were also collected.     

Catalytic growth of In2O3 nanobelts by vapor transport

Indium oxide (In₂O₃) nanobelts have been fabricated by thermal evaporation of metallic indium powders with the assistance of Au catalysts. The as-synthesized nanobelts are single-crystalline In₂O₃ with cubic structure, and usually tens of nanometers in thickness, tens to hundreds of nanometers in width, and several hundreds of micrometers in length. The room temperature photoluminescence spectrum of In₂O₃ nanobelts features a broad emission band at 620 nm, which could be attributed to oxygen deficiencies in the as-synthesized belts. The formation of In₂O₃ nanobelts follows a catalyst-assistant vapor—liquid–-solid growth mechanism, which enables the controlled growth of individual belts on predetermined sites.     

Flux growth of PbMg1/3Ta2/3O3 single crystals

Single crystals of PbMg_1/3Ta_2/3O₃ (PMT) were grown by the flux method. The PbO–Pb₃O₄–B₂O₃ system was used as a solvent. Transparent and light yellow PMT single crystals of rectangular shape and dimensions up to 10×6×4 mm³ were obtained. For the applied growth conditions only, the crystals of the perovskite structure were grown. X-ray diffraction tests showed that at room temperature PMT exhibits cubic symmetry with lattice parameter a=4.042(1) Å. Dielectric studies pointed to relaxor properties of PMT. The characteristic broad and frequency-dependent maximum of dielectric permittivity was observed at 179.7 K (1 kHz).     

Thermal-induced phase transition and assembly of hexagonal metastable In2O3 nanocrystals: A new approach to In2O3 functional materials

This paper reports on the thermal-induced performance of hexagonal metastable In₂O₃ nanocrystals involving in phase transition and assembly, with particular emphasis on the assembly for the preparation of functional materials. For In₂O₃ nanocrystals, the metastable phase was found to be thermally unstable and transform to cubic phase when temperature was higher than 600 °C, accompanied by assembly as well as evolution of optical properties, but the two polymorphs coexisted at the temperature ranging from 600 to 900 °C, during which the content of product phase and crystal size gradually increased upon increasing temperature. The assembly of In₂O₃ nanocrystals can be developed to fabricate In₂O₃ functional materials, such as various ceramic materials, or even desired nano- or micro-structures, by using metastable In₂O₃ nanocrystals as precursors or building blocks. The electrical resistivity of In₂O₃ conductive film fabricated by a hot-pressing route was as low as 3.72×10⁻³ Ω cm, close to that of In₂O₃ single crystal, which is important for In₂O₃ that is always used as conductive materials. The findings should be of importance for both the wide applications of In₂O₃ in optical and electronic devices and theoretical investigations on crystal structures.     

Solvothermal synthesis of K2V3O8 nanorods

A solvothermal route has been developed to synthesize K₂V₃O₈ nanorods via the reduction of V₂O₅ using ethanol as the reducing agent as well as the solvent at 200°C. X-ray diffraction and selected area electron diffraction analysis revealed that the as-synthesized products are of tetragonal structure K₂V₃O₈. Transmission electron spectroscopy image showed that the obtained K₂V₃O₈ comprises rod-like nanocrystallites. The formation mechanism of K₂V₃O₈ was studied.     

Epitaxial growth of the CoFe2O4 film on SrTiO3 and its characterization

Cobalt ferrite (CoFe₂O₄) thin film is epitaxially grown on (0 0 1) SrTiO₃ (STO) by laser molecular beam epitaxy (LMBE). The growth modes of CoFe₂O₄ (CFO) film are found to be sensitive to laser repetition, the transitions from layer-by-layer mode to Stranski–Krastanov (SK) mode and then to island mode occur at the laser repetition of 3 and 5 Hz at 700 °C, respectively. The X-ray diffraction (XRD) results show that the CFO film on (0 0 1) SrTiO₃ is compressively strained by the underlying substrate and exhibits high crystallinity with a full-width at half-maximum of 0.86°. Microstructural studies indicate that the as-deposited CFO film is c-oriented island structure with rough surface morphology and the magnetic measurements reveal that the compressive strained CoFe₂O₄ film exhibits an enhanced out-of-plane magnetization (190 emu/cm³) with a large coercivity (3.8 kOe).     

Anisotropic vapor phase growth of Ga2O3 crystalline nanobelts

Ga₂O₃ nanobelts were synthesized by gas reaction at high temperature in the presence of oxygen in ammonia. X-ray diffraction and chemical microanalysis revealed that the nanostructures were Ga₂O₃ with the monoclinic structure. Electron microscopy study indicated the nanobelts were single crystalline with broad (0 1 0) crystallographic planes. The nanostructures grew anisotropically with the growth direction of . Statistical analysis of the anisotropic morphology of the nanobelts and electron microscopy investigation of the nanobelt tips indicated that both vapor–solid and vapor–liquid–solid mechanisms controlled the growth process. The anisotropic nature of crystallographic morphology is explained in terms of surface energy.     

The growth and spectroscopic characteristics of Ca3Y2(BO3)4:Er laser crystal

The Ca₃Y₂(BO₃)₄:Er³⁺ crystal with a size up to 20 mm×30 mm was grown by the Czochralski method. The absorption spectrum was measured and its absorption peaks were assigned to the corresponding transitions between the Er³⁺ energy levels. A broad emission spectrum from 1429.4 to 1662.8 nm was exhibited from 530 nm wavelength pumping. This crystal is promising as a tunable infrared laser crystal.     

Densities of Li2O–B2O3 melts

The densities have been systematically measured in xLi₂O–(1−x)B₂O₃ melts of different compositions with Li₂O content varying from x=0 to 0.68 from their respective melting points up to about 1450 K with a modified Archimedean method. The density decreased with increasing temperature for all the melts measured in this work. When x<0.15, the plot of temperature versus density could be well fitted by a quadratic polynomial function, and when x0.15, density decreased linearly with increasing temperature. At a fixed temperature, the density of the melts increased rapidly with Li₂O content, went through a maximum at about x=0.333 (Li₂O–2B₂O₃), and then decreased slowly as Li₂O content was further increased. In addition, the volume expansion coefficient (β) was calculated based on the densities measured in this work, and it was found that a maximum value appeared in the dependence of β on the molar ratio of Li₂O at about x=0.333.     

Phase relations around langasite (La3Ga5SiO14) in the system La2O3–Ga2O3–SiO2 in air

Phase relations around langasite (LGS, La₃Ga₅SiO₁₄) were studied on the basis of phase assemblage observed during calcination and crystallization process of samples of various compositions in the ternary system La₂O₃–Ga₂O₃–SiO₂. A ternary compound of apatite structure, La₁₄Ga_xSi_9–xO_39–x/2 was found for the first time. Crystallization of this compound was observed in the cooling process of molten samples of stoichiometric LGS as well as LGS single crystal, demonstrating that LGS is an incongruent-melting compound. A phase diagram was established primarily based on the crystallization sequence in the cooling process.     

Growth and properties of Nd:Lu3Ga5O12 laser crystal by floating-zone method

Neodymium (Nd) doped lutetium gallium garnet (Nd:Lu₃Ga₅O₁₂, Nd:LuGG) single crystal was successfully grown by the optical floating-zone method for the first time to our knowledge. Its absorption and luminescence spectra at room temperature were measured. By using the J–O theory, the spectral parameters of Nd:LuGG were calculated, which indicated that Nd:LuGG should possess comparable and even better laser properties than Nd:YAG. The maximum output power of 855 mW at 1062 nm was achieved with slope efficiency of 23.4% under a pump power of 5.2 W, and optical conversion efficiency of 16.4%. All the results show that Nd:LuGG is a potential laser material.     

Thermal and laser properties of Yb:YAl3(BO3)4 crystal

Large optical-quality Yb:YAl₃(BO₃)₄(Yb:YAB) crystals have been grown by the flux method. The thermal properties of Yb:YAB crystal were measured for the first time. The thermal properties of Yb:YAB crystal with different Yb³⁺ ion concentrations are also reported. The results show that the ytterbium concentration influences the properties of Yb:YAB crystal. The specific heat decreases with the increase of Yb³⁺ ion concentrations in the experiment range. Apparently, the thermal expansion coefficient increases along the c-direction with the increase of Yb³⁺ ion concentrations, while it changes slightly along the a-direction. The output laser in 1120–1140 nm ranges has been demonstrated pumped by InGaAs laser. The slope efficiency is 3.8%. The self-frequency-doubling output power of 1 mW is achieved.     

Ambient-condition growth of superconducting YBa2Cu4O8 single crystals using KOH flux

YBa₂Cu₄O₈ is a stoichiometric oxide superconductor of T_c80 K. Unlike YBa₂Cu₃O_7−δ, this compound is free from oxygen vacancy or twin formation and does not have any microscopic disorder in the crystal. Doping with Ca raises its T_c to 90 K. The compound is a promising superconductor for technological application. Up to now, single crystals have not been grown without using specialized apparatus with extremely high oxygen pressure up to 3000 bar and at over 1100 °C due to the limited range of reaction kinetics of the compound. This fact has delayed the progress in the study of its physical properties and potential applications. We present here a simple growth method using KOH as flux that acts effectively for obtaining high-quality single crystals in air/oxygen at the temperature as low as 550 °C. As-grown crystals can readily be separated from the flux and exhibit a perfect orthorhombic morphology with sizes up to 0.7×0.4×0.2 mm³. Our results are reproducible and suggest that the crystals can be grown using a conventional flux method under ambient condition.     

Thermogravimetric analysis and microstructural observations on the formation of GaN from the reaction between Ga2O3 and NH3

Thermogravimetric analysis (TGA) and microstructural observations were carried to investigate the nitridation mechanism of β-Ga₂O₃ powder to GaN under an NH₃/Ar atmosphere. Non-isothermal TGA showed that nitridation of β-Ga₂O₃ starts at ∼650 °C, followed by decomposition of GaN at ∼1100 °C. Isothermal TGA showed that nitridation follows linear kinetics in the temperature range 800–1000 °C. At an early stage of nitridation, small GaN particles (∼5 nm) are deposited on the β-Ga₂O₃ crystal surface and they increase with time. We proposed a mechanism for the nitridation of Ga₂O₃ by NH₃ whereby nitridation of β-Ga₂O₃ proceeds via the intermediate vapor species Ga₂O(g).     

Growth and characterization of nanostructured Al2O3/YAG/ZrO2 hypereutectics with large surfaces under laser rapid solidification

The preparation of large bulk oxide eutectics with homogeneous and dense structure in nano-scale by melt growth method is a difficult challenge. Fully dense, homogeneous and crack-free ternary nanostructured Al₂O₃/YAG/ZrO₂ hypereutectic plate with large surface is successfully obtained by laser remelting. The hypereutectic in selected composition presents an ultra-fine eutectic-like microstructure consisting of alternating interpenetrating Al₂O₃, YAG and ZrO₂ lamellae with mean interphase spacing of about 150 nm, which is much smaller than the ternary eutectic composition grown at the same growth conditions. With the increase of laser scanning rate, the lamellar spacing is rapidly decreased. The minimum value obtained is 50 nm. The analysis indicates that the strong faceted growth behavior and cooperative branching of the component phases related with high entropies of fusion and large kinetic undercooling during laser rapid solidification are the primary formation reasons for the irregular eutectic growth morphology. Furthermore, the unique cellular microstructure with complex structure is also observed at high growth rate, and their formation mechanism and effect of the composition on the microstructure are discussed.     

Synthesis of crystalline TiO2 nanostructure arrays by direct microwave irradiation on a metal substrate

We report a method for synthesizing TiO₂ nanostructures by applying microwave irradiation (1200 W, 2.45 GHz, single-mode) to a Ti substrate under an atmosphere comprising of O₂ and Ar. After 1200 W microwave irradiation, one-dimensional (1D) nanostructure arrays were synthesized on the surface of the substrate. The average dimensions of the 1D structures were 200 nm in length and 30 nm in diameter. The structures were single crystalline. The EDX elemental maps of the areas examined using HAADF-STEM demonstrated that Ti and O were distributed homogeneously throughout the nanostructure. Quantitative analysis of the mean atomic ratios in the nanostructures disclosed a Ti:O ratio of 0.331:0.669. XPS analysis demonstrated that the predominant oxidation state of Ti in the samples was +4. On the basis of these results, we propose a possible mechanism for the formation of the TiO₂ nanostructures via microwave irradiation.     

Synthesis, thermal and magnetic properties of new metal iodate: (LiFe1/3)(IO3)2

This paper reports the detail synthesis of a new kind of metal iodate, anhydrous (LiFe_1/3)(IO₃)₂, from aqueous solutions. The synthesized compound shows spinal morphology and is chemical stable up to 400°C. The iodate shows paramagnetic behavior from room temperature down to 4.2 K. At room temperature, the new compound has a hexagonal structure with the lattice parameters a=5.4632(2) Å, c=5.0895(6) Å, Z=1, space group of P6₃.     

Raman scattering study of crystalline and melting states of BaO·2B2O3

Melting and crystallization scenarios of barium tetraborate BaB₄O₇ (BaO·2B₂O₃) are studied in situ by Raman spectroscopy. It is shown that the scenario depends on the temperature–time history of melt. Crystallization conditions of the beta modification of barium tetraborate (β-BaB₄O₇) from a stoichiometric glass structure BaO·2B₂O₃ were investigated.