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.     

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     

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.     

Growth and spectral properties of Nd:LaVO4 crystal

This paper reports the growth and spectral properties of 3.5 at% Nd³⁺:LaVO₄ crystal with diameter of 20×15 mm² which has been grown by the Czochralski method. The spectral parameters were calculated based on Judd–Ofelt theory. The intensity parameters Ω_λ are: Ω₂=2.102×10⁻²⁰ cm², Ω₄=3.871×10⁻²⁰ cm², Ω₆=3.235×10⁻²⁰ cm². The radiative lifetime τ_r is 209 μs and calculated fluorescence branch ratios are: β₁(0.88μm)=45.2, β₂(1.06μm)=46.7, β₃(1.34μm)=8.1. The measured fluorescence lifetime τ_f is 137 μm and the quantum efficiency η is 65.6%. The absorption band at 808 nm wavelength has an FWHM of 20 nm. The absorption and emission cross sections are 3×10⁻²⁰ and 6.13×10⁻²⁰ cm², respectively.     

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.     

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.     

Growth of NaBi(WO4)2 crystal by modified-Bridgman method

NaBi(WO₄)₂ (NBW) crystals have been grown for the first time by modified-Bridgman method. Influences of some factors on the crystal growth process are discussed. X-ray powder diffraction experiments show that the unit cell parameters of NBW crystal are a=b=0.5284 nm, c=1.1517 nm, and V=0.3215 nm³. The differential thermal analysis shows that the NBW crystal melts at 923°C.     

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.     

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 BPO4 crystals

Single crystals of BPO₄ with sizes up to 15×10×12 mm³ were grown by top-seeded solution growth method using Li₂O–Li₄P₂O₇ as fluxes. The components volatilized from the melt were characterized by the method of X-ray powder diffraction. The defects of grown crystals have also been investigated. The measured ultraviolet cutoff edge of BPO₄ was about 130 nm. Its density was 2.82 g/cm³ determined using drainage method.     

Growth of laser single-crystals Er:YVO4 by floating zone method

High optical quality Er³⁺:YVO₄ laser crystals have been grown by using the floating zone method (FZ). The spectroscopic properties and 3 μm lasing of Er³⁺:YVO₄ were investigated. It is found that the Er³⁺ concentration has a negative effect on the emission of the transition ⁴I_13/2→⁴I_15/2(1.55 μm ), and a positive effect on that of the ⁴I_11/2→⁴I_13/2 transition (2.68 μm). With direct upper-state pumping and a plane-concave cavity a self-terminating laser was achieved at the wavelength of 2.724 μm in the 30 at% Er³⁺ doped sample.     

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.     

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).     

Hydrothermal synthesis of MoS2 nanowires

The MoS₂ nanowires with diameters of 4 nm and lengths of 50 nm were synthesized by a hydrothermal method using 0.36 g MoO₃ and 1.8 g Na₂S as precursors in 0.4 mol/l HCl solution at 260°C. The products are characterized by XRD, XPS, TEM, HTEM and BET. Results show that the as-prepared MoS₂ nanowires consist of 1–10 sulfide layers with BET surface areas of 107 m²/g. The possible reaction route and the formation mechanism of the MoS₂ nanowires are discussed. The effects of exterior conditions such as pH value, temperature, concentration of precursors and additives on the particle size and morphology of MoS₂ crystallites were investigated.     

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.     

Improved growth of PbI2 single crystals

The phase equilibrium and the crystallization process of lead iodide (PbI₂) melt have been primarily investigated according to the lead–iodine phase diagram. It is found that the iodine evaporation and the segregated lead deposition are the two important factors that affect the PbI₂ crystal quality. The new method of Pulling U-type quartz growth ampoule has been made to impede the decomposition of PbI₂ and the vaporization and condensation of iodine. An orange and translucent PbI₂ single crystal of large size was obtained by the improved growth method, i.e. U-type ampoule pulling. Resistivity of the as-grown crystal is up to 4×10¹¹ Ω cm, and IR transmission is up to 45% in the region from 7800 to 450 cm⁻¹. Therefore, the improved growth method is a promising convenient new method for the growth of high quality PbI₂ crystals.     

Growth and characterization of a new nonlinear optical material: Potassium p-nitrophenolate dihydrate (NO2–C6H4–OK·2H2O) with new bonding properties

Single crystals of potassium p-nitrophenolate dihydrate (NPK·2H₂O) have been grown successfully using the isothermal solvent evaporation technique. It is a new semiorganic nonlinear optical crystal, possessing a d_eff of about 1.5 times that of lithium niobate and in which the K⁺ ions are bonded to the nitro group instead of bonding with the phenolic O⁻. Large single crystals of dimension upto 20×6×4 mm³ are harvested within a period of 60 days. The grown crystals are subjected to single crystal X-ray, FTIR and DRS-UV visible spectral, thermal and microhardness analyses. Single crystal X-ray analysis confirms the molecular formula and the structure of the crystal. FTIR spectral studies verify the functional groups present in the crystal. The DRS-UV visible spectrum proved the optical transparency of the crystal in the entire visible and near infrared region. Thermal studies reveal that the crystals are stable upto 180 °C. Microhardness measurements on the cleaved plane (1 1 0) explain the strength and slip direction in the crystal. The SHG efficiency of the crystal is examined by performing the Kurtz powder test using Nd:YAG laser.     

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).     

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.     

Growth of large dimension BaWO4 crystal by the Czochralski method

In this paper, polycrystalline materials of BaWO₄ were synthesized by solid-state phase method, and a single crystal of BaWO₄ was successfully grown along a and c-axis direction by using the Czochralski method. Up to 20×22×80 mm³ BaWO₄ crystal was obtained, and X-ray powder diffraction results show that the as-grown BaWO₄ crystal belongs to the scheelite structure. The effective segregation coefficients of Ba and W of the BaWO₄ crystal were measured by the X-ray fluorescence method, and the effective segregation coefficients of Ba and W were near 1. The rocking curve from (2 0 0) diffraction plane of as-grown BaWO₄ single crystal was measured on the High-resolution X-ray diffractometer D5005, and the full-width at half-maximum value was found to be 26.64′′ The density and hardness of the BaWO₄ crystal was measured, the measured density was in agreement with the calculated result, and the Mohs hardness was about 4.