Effect of γ‐irradiation on spectral properties of undoped Y2SiO5 crystals

The absorption spectra of undoped Y₂SiO₅ crystals were studied before and after γ‐irradiation. After γ‐irradiation, the additional absorption peaks at 260‐270 and 320nm were observed in as‐grown and H₂‐annealed Y₂SiO₅ crystal, but it did not occur in air‐annealed Y₂SiO₅ crystal. These absorption peaks were attributed to F color centers and O^– hole centers, respectively. Owing to more oxygen vacancies and color centers in H₂‐annealed Y₂SiO₅ crystal than that in as‐grown Y₂SiO₅ crystal after γ‐irradiation, the additional absorption peaks were more intense in the former than that in the latter. With the irradiation dose increasing from 20 to 220kGy, the intensity of additional absorption peaks increased. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Growth and optical damage properties of In:Zn:LiNbO3 waveguide substrate

In:Zn:LiNbO₃ crystals doped with different indium concentrations were grown by Czochralski technique. The optical damage threshold value and ultraviolet‐visible absorption spectra of the In:Zn:LiNbO₃ crystals were measured. The In:Zn:LiNbO₃ crystals were made into optical waveguide substrates using hexanedioic acid as proton exchange agent. The optical damage resistant ability of those optical waveguide substrates was investigated by the m‐line method. The optical damage threshold values of In(2mol.%):Zn(3mol.%):LiNbO₃ crystal and optical waveguide substrate are two orders of magnitude higher than those of pure LiNbO₃. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth of zirconium‐doped KTiOPO4 crystals in the K2O‐P2O5‐TiO2‐ZrF4 system

Zirconium‐doped KTiOPO₄ (KTP) crystals were grown using a high temperature flux method in the K₂O‐P₂O₅‐TiO₂‐ZrF₄ system. The dopant content in the single crystals with general composition KTi_1‐xZr_xOPO₄ (where x = 0 – 0.026) strongly depends on zirconium concentration in the homogeneous melts. AES‐ICP method and X‐ray fluorescence analysis were used to determine the composition of the obtained crystals. Phase analyses of the products were performed using the powder XRD. The structures of KTiOPO₄ containing different quantities of Zr were refined on the basis of single crystal XRD data. Applying ZrF₄ precursor for zirconium injection into the flux allowed growing the zirconium‐doped KTP crystals at 930–750°C. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Defect structure and light‐induced scattering of Zr‐doped near‐stoichiometric Mn:Fe:LiNbO3 crystals grown by TSSG method

Near‐stoichiometric Mn:Fe:LiNbO₃ crystals doped with various concentration of ZrO₂ were grown by top seed solution growth (TSSG) method in the air atmosphere. The Zr concentration in the crystal was determined by inductively coupled plasma optical emission spectrometer. The defect structures were analyzed by means of ultraviolet‐visible and infrared transmittance spectra. The appearance of vibration peak at 3466 cm^‐1 in infrared spectra manifested that Li/Nb ratio in crystals approached to stoichiometric proportion. The fundamental absorption edge represented continuous red‐shift which was discrepancy with congruent doped LiNbO₃ crystals showed that doping ions possessed different location mechanism. The light‐induced scattering of the doped stoichiometric LiNbO₃crystals were quantitatively scaled via incident exposure energy. The results demonstrated that Zr(2 mol%):Mn:Fe:LiNbO₃ crystal had the weakest light‐induced scattering and the mechanism related to their defect structures was discussed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characterization of KDP crystal grown from solution with low pH value

Solubility curves of KDP (KH₂PO₄) in solutions with different pH values were measured. It was found that the solubility of KDP crystal increased with the reduction pH value of solution. Transparent KDP crystal was grown from solution with 1.5 pH by point seed. Chemical etching experiments revealed that pyramid sector of the crystal displayed more growth defects. Growth defects, such as growth striation and inclusion, were analyzed by white‐beam synchrotron radiation X‐ray topography. The reasons for the formation of these growth defects were discussed. Transmittance spectra test of both prismatic sector and pyramidal sector was performed. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Increased optical damage resistance of Zr:LiNbO3 crystals

Zr: LiNbO₃ crystals has been grown. The crystal composition and phase are analyzed by X‐ray diffration. The optical damage resistance ability of Zr: LiNbO₃ crystals is studied by the Sénarmont compensation method and the transmitted beam pattern distortion method. The saturated value of the birefringence change of 6 mol% Zr: LiNbO₃ crystal is 1.01×10^‐4, which is seven times smaller than that of congruent pure LiNbO₃ crystal. The results of UV‐Visible and IR absorption spectra of Zr: LiNbO₃ crystals powerfully confirm that the optical damage resistance threshold concentration of the Zr⁴⁺ ions doped in LiNbO₃ crystals is about 6 mol% in the melt. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural and mechanical properties of KН2PО4 single crystals with embedded nanoparticles and organic molecules

Single crystals of KDP crystals with embedded Urea molecules and TiO₂ nanoparticles have been grown from aqueous solution by the temperature lowering method. The effect of the organic molecules and nanoparticles on the structural and mechanical properties has been studied. It has been observed that addition of Urea molecules improves laser induced damage threshold and mechanical strength of the crystal, while TiO₂ nanoparticles have the opposite effect. The structure and composition of KDP:Urea crystal are studied by three‐crystal X‐ray diffraction analysis, which reveals the existence of a correlation between the increase of the microhardness value and the change of the crystal lattice parameter. The surface features of KDP:TiO₂ crystals are analyzed by scanning electron microscopy that reveals the presence of quasi‐equidistant growth bands caused by capture of the nanoparticles. It is shown that the rise of TiO₂ nanoparticles concentration up to 10⁻⁴ wt.% and higher resulted in 3‐fold reduction of the laser damage threshold of KDP:TiO₂ relative to pure KDP in [001] and [100] crystallographic directions. It is found that microhardness and fracture toughness decrease at the nanoparticles concentration of 10⁻³ wt.% due to crack formation at crystal lattice discontinuities. The grown crystals also have been subjected to dielectric studies.     

Solution growth and morphology of CH3NH3PbBr3 single crystals in different solvents

In this work, large‐sized CH₃NH₃PbBr₃ single crystals were successful grown using solution evaporation method with hydrohalic acid and N, N‐Dimethylformamide (DMF) as solvent respectively. The lattice parameters of cubic CH₃NH₃PbBr₃ were estimated using XRD method. The solubility of CH₃NH₃PbBr₃ in hydrobromic acid was determined at the temperature range between 20 °C–90 °C. A special micro‐solution crystallizer was designed to in‐situ study the morphology of CH₃NH₃PbBr₃ crystal. The largest crystal face was indexed by the XRD patterns and it would be {110} for CH₃NH₃PbBr₃ grown from HBr solution and {100} from DMF solution. The results show that solvent would affect the morphology and crystal habit greatly during crystal growth from solution.     

Structure and Photo‐Damage Resistance of Li‐Rich LiNbO3 Crystals Co‐Doped with Zn2+/Er3+

The pure congruent LiNbO₃, Er:LiNbO₃ and Zn,Er co‐doped Li‐rich LiNbO₃ crystals were grown by Czochralski method. The X‐ray diffraction method and ultraviolet‐visible absorption spectra of the crystals were used to analyze the structure of the crystals. The photo‐damage ability resistance of the crystals was measured. The Zn,Er co‐doped Li‐rich LiNbO₃ crystals show a decrease in lattice constant values, a shift in absorption edge of ultraviolet‐visible absorption spectra towards shorter wavelength, and three orders of magnitude increase in photo‐damage resistance compared to congruent LiNbO₃ crystal. The intrinsic and extrinsic defects are discussed to explain the enhance of the photo‐damage ability resistance     

Studies on the structural,thermal and optical behaviour of solution grown organic NLO material: 8‐hydroxyquinoline

Single crystal of 8‐hydroxyquinoline (8HQ) having chemical formula C₉H₇NO, an organic nonlinear optical (NLO) material has been successfully grown by slow evaporation solution growth technique at room temperature. The crystal system has been confirmed from the powder X‐ray diffraction (PXRD) analysis. The crystalline perfection was evaluated by high resolution X‐ray diffractometry (HRXRD). From this analysis we found that the quality of the crystal is quite good. However, a very low angle (tilt angle 14 arc sec) boundary was observed which might be due to entrapping of solvent molecules in the crystal during growth. Its optical behavior has been examined by UV‐Vis. analysis, which shows the absence of absorbance between the wavelengths ranging from 400 to 1200 nm. From the thermal analysis it was observed that the material exhibits single sharp weight loss starting at 113°C without any degradation. The laser damage threshold was measured at single shot mode and the SHG behavior has been tested using Nd:YAG laser as a source. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

KDP single crystal growth via three‐dimensional motion growth method

A novel system for rapid crystal growth, namely three‐dimensional motion growth method (“3D MGM”) was proposed. Using this system, a potassium dihydrogen phosphate (KDP) seed was grown to a single crystal with a final size of 50×55×85 mm³. The KDP crystal was characterized by Raman spectroscopy, UV‐vis‐NIR spectroscopy, extinction ratio, laser damage threshold, and etching studies. Raman spectrum shows KDP crystal grown by “3D MGM” maintains good crystallinity as that grown by rotating‐crystal method (“RCM”). The “3D MGM” grown KDP crystal has much better transmittance, higher extinction ratio, higher damage threshold and less dislocation density, compared to “RCM” grown crystal.     

Influence of La3+ ions on growth and NLO properties of KDP single crystals

Single crystals of pure and Lanthanum added KDP crystals were grown from aqueous solution. The influence of La³⁺ ions in KDP crystals is studied. Isolated centers are formed by La³⁺ ions in KDP structure along (100) plane. La³⁺ ions incorporated into superficial crystal growth layer and slightly affect the growth process as they generate weak lattice stresses. The creation of these weak lattice stress is confirmed by Vickers's micro hardness test. The HRXRD analysis showed reduced structural defects in the La added KDP in the (100) plane than pure KDP. The incorporation of La in the crystal was confirmed by EDAX analysis. The Kurtz's powder SHG efficiency was found to be 1.5 times that of pure KDP. The UV‐Vis transmission spectra of La added KDP showed excellent transmittance from 1100 nm to 340 nm and did not show any change in lower cutoff wavelength with respect to pure KDP. Laser damage threshold value has been determined using Q‐switched Nd:YAG laser operating at 1064 nm and with 65 ns pulses in single shot mode. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization and characterization of nonlinear optical l‐histidinium dihydrogen orthophosphate orthophosporic acid single crystal

L‐histidinium dihydrogen orthophosphate orthophosporic acid (abbreviated as LHP) with molecular formula C₆H₁₀N₃O₂⁺·H₂PO₄^‐·H₃PO₄ was successfully grown by slow evaporation technique from aqueous solution. The crystal was characterized by X‐ray diffractometry (XRD), UV‐Vis‐NIR, TGA, DTA, microhardness and solubility studies. The dielectric constant and dielectric loss of the crystal were studied as function of frequency. Photoconductivity studies were also carried out on the sample. The SHG efficiency of the crystal is studied using the Kurtz and Perry technique. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

原料的均匀性对CsB3O5晶体光学性质的影响

本文是针对紫外非线性光学晶体CsB3O5的原料处理对晶体光学质量的影响的研究报道.利用液相法合成出高度分散的原料,生长出高光学质量的CBO单晶.消除了晶体内部的光散射颗粒,并测量了该晶体的透过光谱、光学均匀性和抗激光损伤阈值.     

Synthesis,growth and characterization of l‐alaninium oxalate ‐ a novel organic NLO crystal

Nonlinear optical material of L‐alaninium oxalate (LAO) has been synthesized and single crystals are grown by slow evaporation technique. The solubility data of LAO is determined in water. Single crystal X‐ray diffraction study showed that LAO belongs to orthorhombic system with a non‐centrosymmetric space‐group P2₁2₁2₁. The functional groups have been identified from FT‐IR spectrum. The UV‐Vis‐NIR spectrum of LAO shows less optical absorption in the entire visible region. The second harmonic generation (SHG) in the material was estimated using Nd:YAG laser. The mechanical properties of the grown crystals are studied using Vickers microhardness tester. The AC and DC conductivity, and dielectric studies are also carried out and reported for the first time. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of La3Ga5.5Ta0.5O14 crystal

La₃Ga_5.5Ta_0.5O₁₄ (LGT) crystal was grown by using the Czochralski method. The as‐grown crystal is transparent, free from inclusions and with no cracks. Specific heat, thermal expansion, dielectric constants, transmission spectrum and optical damage threshold of LGT have been measured, and the results show general properties of LGT are similar to that of La₃Ga₅SiO₁₄ (LGS) crystal. The experiment to research the Q‐switch properties of LGT has been performed and the results show LGT possesses smaller electrooptic coefficients than that of LGS and may not be an ideal material used as a Q‐switch. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of high quality anthracene crystals by a simple solution technique

In recent years considerable effort has gone into the preparation and characterisation of high purity anthracene crystals, since anthracene is used as a model organic molecular crystal in studies of solid‐state properties. Studies of organic molecular crystals and their applications in optics and electronics have been increasing attractive interest. Several attempts have been made to grow single crystals of anthracene. This is the first attempt to grow high quality anthracene crystals by solution technique adopting slow evaporation method in different solvents like CS₂ and CCl₄. The harvested crystals were subjected to various characterization studies. The results of characterisation studies support the purity of solution grown anthracene crystals. The solubility of anthracene in various solvents like CS₂ and CCI₄ was determined. The crystals of anthracene were grown by systematic method of slow evaporation technique in various solvents. Different morphology is noted with varying solvents. The crystal was subjected to XRD studies, FTIR studies and thermal studies. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Optical and mechanical properties of a new second order nonlinear optical crystal urea l‐threonine

A new second order non‐linear optical organic crystal Urea L‐threonine has been grown by aqueous solution slow cooling technique. The grown crystal is non hygroscopic and transparent in the visible region. The solubility of the grown crystal was found. The crystal structure and perfection were determined using powder XRD and High resolution XRD. The molecular structure was confirmed by ¹H‐NMR spectrum. Thermal properties of the crystal have been studied using thermogravimetric (TG) and differential thermal analysis (DTA). The dielectric response of the crystal with varying frequencies at different temperatures was studied. UV‐Visible spectrum was recorded to study the optical transparency of the grown crystals. The second order non linear optical property was examined by Kurtz powder technique and found that the second order susceptibilities is 1.2 KDP at wavelength 1064 nm. The mechanical behaviour was studied by Vickers Microhardness test. The results are discussed in detail. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Nucleation kinetics and growth aspects of organic nonlinear optical L‐arginine trifluoroacetate single crystals

Experimental determination of solubility, metastable zonewidth and induction period for an organic nonlinear optical (NLO) L‐arginine trifluoroacetate (LATF) crystal is reported. The interfacial tension for different supersaturation conditions has been estimated for the LATF solution at 45°C. Bulk crystal of dimensions 57x5x3 mm³ has been grown by temperature lowering technique using optimized growth parameters. Powder X‐ray diffraction and FTIR studies confirm the crystalline nature and the functional groups of the grown crystals respectively. Linear optical property of the grown crystal has been studied by UV‐Vis spectrum. Thermal analyses have revealed that the compound is thermally stable upto 212°C. Kurtz powder SHG test confirm the nonlinear optical properties of the as‐grown LATF crystal. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Solubility and crystallization of BaHPO4 crystals

A study of growth of barium hydrogen phosphate (BaHPO₄) crystal from solution is reported. The raw materials of barium hydrogen phosphate were successfully synthesized through chemical reaction in water. The solubility in HCl and H₃PO₄ solution were studied. It increased when acid concentration and temperature become higher, and the fitted curve of solubility is nearly a line. The acid concentration affects crystalline morphology of BaHPO₄ crystal. The crystallization is well when the acid solution ranges from 0.5 to 0.8M. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim