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).     

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.     

Self-catalytic branch growth of SnO2 nanowire junctions

Multiple branched SnO₂ nanowire junctions have been synthesized by thermal evaporation of SnO powder. Their nanostructures were studied by transmission electron microscopy and field emission scanning electron microcopy. It was observed that Sn nanoparticles generated from decomposition of the SnO powder acted as self-catalysts to control the SnO₂ nanojunction growth. Orthorhombic SnO₂ was found as a dominate phase in nanojunction growth instead of rutile structure. The branches and stems of nanojunctions were found to be an epitaxial growth by electron diffraction analysis and high-resolution electron microscopy observation. The growth directions of the branched SnO₂ nanojunctions were along the orthorhombic [1 1 0] and . A self-catalytic vapor–liquid–solid growth mechanism is proposed to describe the growth process of the branched SnO₂ nanowire junctions.     

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).     

Growth and properties of Pb[(Zn1/3Nb2/3)0.91Ti0.09]O3 single crystals directly from melt

Pb[(Zn_1/3Nb_2/3)_0.91Ti_0.09]O₃ (PZNT91/9) single crystals were grown by a modified Bridgman method directly from melt using an allomeric Pb[(Mg_1/3Nb_2/3)_0.69Ti_0.31]O₃ (PMNT69/31) single crystal as a seed. X-ray diffraction (XRD) measurement confirmed that the as-grown PZNT91/9 single crystals are of pure perovskite structure. Electrical properties and thermal stabilization of PZNT91/9 crystals grown directly from melt exhibit different characters from those of PZNT91/9 crystals grown from flux, although segregation and the variation of chemical composition are not seriously confirmed by X-ray fluorescence analysis (XPS). The [0 0 1]-oriented PZNT91/9 crystals cut from the middle part of the as-grown crystal boules exhibit broad dielectric-response peaks at around 105 °C, accompanied by apparent frequency dispersion. The values of piezoelectric constant d₃₃, remnant polarization P_r, and induced strain are about 1800–2200 pC/N, 38.8 μC/cm², and 0.3%, respectively, indicating that the quality of PZNT crystals grown directly from melt can be comparable to those of PZNT91/9 single crystals grown from flux. However, further work deserves attention to improve the dielectric properties of PZNT crystals grown directly from melt. Such unusual characterizations of dielectric properties of PZNT crystals grown directly from melt are considered as correlating with defects, microinhomogeneities, and polar regions.     

High-resolution electron microscopy of microstructure of SrTiO3/BaZrO3 bilayer thin films on MgO substrates

SrTiO₃/BaZrO₃ heterofilms as buffer layers are deposited on (0 0 1) MgO substrates by an RF-sputtering technique. The atomic structure and the defect configuration at the interfaces are investigated by means of aberration-corrected high-resolution transmission electron microscopy. At the BaZrO₃/MgO interface, two types of interfacial structures, MgO/ZrO₂-type and MgO/BaO-type, are observed. Antiphase boundaries and dislocations are found at the BaZrO₃/MgO interface. The formation of these lattice defects is discussed in terms of film growth and structural imperfections of the substrate surface. At the SrTiO₃/BaZrO₃ interface, a high density of misfit dislocations is observed with different configurations. The formation of these dislocations contributes both to the relaxation of the large misfit strain and to stopping of the further propagation of lattice defects which are formed in the BaZrO₃ layer into the SrTiO₃ layer.     

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.     

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.     

High-velocity banding structure in the laser-resolidified hypoperitectic Ti47Al53 alloy

Stability analysis of a growing solid/liquid interface is the fundamental concept of modern solidification theory. Here, serial laser rapid solidification experiments were performed on a hypoperitectic Ti₄₇Al₅₃ alloy to explore the dendritic growth behavior near the limit of high-velocity absolute stability. SEM and TEM techniques were carried out to investigate the microstructure and identify the phase composition. By adopting an improved sampling method of TEM, the growth morphology evolution of the laser-resolidified layer was observed directly and high-velocity banding structure was firstly detected in Ti–Al peritectic alloys. The high-velocity banding structures are parallel to the solid/liquid interface (normal to the growth direction) and made of the oscillation structures grown alternatively in modes of cell and plane morphologies. In light bands with cellular growth mode, all dislocation assembles are parallel to the growth direction and forms the cell boundaries, while all dislocation distributes randomly in dark bands. The determined growth velocity range for the appearance of high-velocity banding structures is about 0.51.1 m s⁻¹ according to the rapid solidification experiments, and the origin of the banding agrees well with the prediction of the CGZK phenomenological model (Acta Metal. Mater. 40 (1992) 983).     

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.     

Microstructure and ferroelectric properties of BaTiO3 films on LaNiO3 buffer layers by rf sputtering

We have fabricated LaNiO₃ and BaTiO₃ films using the rf sputtering method. The LaNiO₃ were deposited on Si substrates, demonstrating a (1 0 0) highly oriented structure and nanocrystalline characteristic with a grain size of 30 nm. The BaTiO₃ thin films were deposited on the LaNiO₃ buffer layers, and have exhibited a (1 0 0) texture with a thickness of 400 nm. A smooth interface is obtained between the LaNiO₃ bottom electrode and the BaTiO₃ film from cross-section observations by scanning electron microscopy. The bi-layer films show a dense and column microstructure with a grain size of 60 nm. Ferroelectric characterizations have been obtained for the BaTiO₃ films. The remnant polarization and coercive field are 2.1 μC/cm² and 45 kV/cm, respectively. The leak current measurements have shown a good insulating property.     

Facile synthesis of submicron BaTiO3 crystallites by a liquid–solid reaction method

Uniform, submicron BaTiO₃ crystallites in tetragonal structure were synthesized by a novel low-temperature liquid–solid reaction method mainly via two simple steps: firstly, BaO₂·H₂O₂ submicron particles of about 130–450 nm were precipitated from the reaction of BaCl₂ and H₂O₂ in a slightly alkaline (pH 8) aqueous solution under the ambient condition; secondly, tetragonal phase BaTiO₃ submicrocrystals with the size in the range of 180 to 400 nm could be produced by subjecting the as-prepared BaO₂·H₂O₂ and commercial TiO₂ submicron particles to thermal treatment in air at 700 °C for 10 h. The as-obtained products were characterized by X-ray powder diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy and inductively coupled plasma-atomic emission spectroscopy, and scanning electron microscopy.     

Growth and spectroscopic properties of Er single doped and Er–Yb co-doped YAl3(BO3)4 crystals

Er³⁺-doped and Er³⁺–Yb³⁺ co-doped yttrium aluminum borate (YAB) single crystals have been grown by the top-seeded solution growth method using a new flux system, namely NaF–MoO₃–B₂O₃. The Er³⁺ concentrations were 1.3 mol% for both single doped and co-doped crystals and the Yb³⁺ concentration in the Er³⁺–Yb³⁺ co-doped crystal was 20.0 mol% in the raw materials. The distribution coefficients of Er³⁺ single doped and Er³⁺–Yb³⁺ co-doped crystals were measured. The polarized absorption and fluorescence spectra of Er³⁺–Yb³⁺ co-doped crystal were recorded and compared with those of Er³⁺ single doped crystal. The results demonstrate that Er³⁺–Yb³⁺ co-doped YAB crystal is a potential candidate for 1.55 μm laser materials.     

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.     

A simple method to synthesize single-crystalline β-wollastonite nanowires

The single-crystalline β-wollastonite (β-CaSiO₃) nanowires were prepared via a simple hydrothermal method, in the absence of any template or surfactant using cheap and simple inorganic salts as raw materials. Xonotlite [Ca₆(Si₆O₁₇)(OH)₂] nanowires were first obtained after hydrothermal treatment at a lower temperature of 200 °C for 24 h, and after being calcinated at 800 °C for 2 h, xonotlite nanowires completely transformed into β-wollastonite nanowires and the wire-like structure was preserved. The synthesized β-wollastonite nanowires had a diameter of 10–30 nm, and a length up to tens of micrometers, and the single-crystalline monoclinic parawollastonite structured β-wollastonite was identified by XRD with the space group of P2₁/a and cell constants of a=15.42 Å, b=7.325 Å, c=7.069 Å and β=95.38°. A possible growth mechanism of β-wollastonite nanowires was also proposed. The advantages of this method for the nanowire synthesis lie in the high yield, low temperature and mild reaction conditions, which will allow large-scale production at low cost.     

Growth and spectral properties of Nd-doped Sr3Y(BO3)3 crystal

A new crystal of Nd³⁺:Sr₃Y(BO₃)₃ with dimension up to 25×35 mm² was grown by Czochralski method. Absorption and emission spectra of Nd³⁺: Sr₃Y(BO₃)₃ were investigated . The absorption band at 807 nm has a FWHM of 18 nm. The absorption and emission cross sections are 2.17×10⁻²⁰ cm² at 807 nm and 1.88×10⁻¹⁹ cm² at 1060 nm, respectively. The luminescence lifetime τ_f is 73 μs at room temperature     

Effect of NH3 on the growth characterization of TiN films at low temperature

Titanium nitride (TiN) films were obtained by the atmospheric pressure chemical vapor deposition method of the TiCl₄–N₂–H₂ system with various flow rates of NH₃ at 600°C. The growth characteristics, morphology and microstructure of the TiN films deposited were analyzed by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Without NH₃ addition, no TiN was deposited at 600°C as shown in the X-ray diffraction curve. However, by adding NH₃ into the TiCl₄–N₂–H₂ system, the crystalline TiN was obtained. The growth rate of TiN films increased with the increase of the NH₃ flow rate. The lattice constant of TiN films decreased with the increase of the NH₃ flow rate. At a low NH₃ flow rate, the TiN (2 2 0) with the highest texture coefficient was found. At a high NH₃ flow rate, the texture coefficient of TiN (2 0 0) increased with the increase of the NH₃ flow rate. In morphology observation, thicker plate-like TiN was obtained when the NH₃ flow rate was increased. When the flow rate of NH₃ was 15 sccm, Moiré fringes were observed in the TiN film as determined by TEM analysis. The intrinsic strain was found in the TiN film as deposited with 60 sccm NH₃.     

Influence of cooling rate on the liquid-phase epitaxial growth of Zn3P2

We report the liquid-phase epitaxial growth of Zn₃P₂ on InP (1 0 0) substrates by conventional horizontal sliding boat system using 100% In solvent. Different cooling rates of 0.2–1.0 °C/min have been adopted and the influence of supercooling on the properties of the grown epilayers is analyzed. The crystal structure and quality of the grown epilayers have been studied by X-ray diffraction and high-resolution X-ray rocking measurements, which revealed a good lattice matching between the epilayers and the substrate. The supercooling-induced morphologies and composition of the epilayers were studied by scanning electron microscopy and energy dispersive X-ray analysis. The growth rate has been calculated and found that there exists a linear dependence between the growth rate and the cooling rate. Hall measurements showed that the grown layers are unintentionally doped p-type with a carrier mobility as high as 450 cm²/V s and a carrier concentration of 2.81×10¹⁸ cm⁻³ for the layers grown from 6 °C supercooled melt from the cooling rate of 0.4 °C/min.     

Large-size β-Ga2O3 single crystals and wafers

Large-size single crystals of β-Ga₂O₃ with 1 inc in diameter have been grown by the floating zone technique. The stable growth conditions have been determined by the examination of the crystal structure. Wafers have been cut and fine polished in the (1 0 0), (0 1 0) and (0 0 1) planes. These were highly transparent in the visible and near UV, as well as electrically conductive, indicating the potential use of β-Ga₂O₃ as a substrate for optoelectic devices operating in the visible/near UV and with vertical current flow.     

Crystal growth of Ce: PrF3 by micro-pulling-down method

Micro-pulling-down (μ-PD) growth apparatus was modified for fluoride crystals. PrF₃ was grown with various concentrations of Ce³⁺ from 0–100%. The crystals were transparent and colorless (CeF₃) or greenish and 3 mm in diameter and 15–50 mm in length. Neither visible inclusions nor cracks were observed. Radioluminescence spectra and decay kinetics were measured for the sample set at room temperature. In comparison to the Czochralski or Bridgman method, the μ-PD method allows to produce single crystalline material in a faster thus more economic way. Once it is established for the fluoride crystals, it is an efficient tool for exploring the field of new functional fluorides.