Growth,defects,and properties of GdCa4O（BO3）3 and Nd：GdCa4O（BO3）3 crystals

Pure and neodymium-doped gadolinium calcium oxoborate crystals of high quality were grown by the Czochralski method.The orientation of crystal was precisely determined,and the samples for measurements were prepared.Through synchrotron x-ray topography and high-resolution x-ray diffractometry,the twin structure was discovered.Some properties such as the figure of merit value,and dielectric,piezoelectric,and elastic constants were meausured along with a discussion of the anisotropy of the laser properties.

Image shifts resulting from the misorientation of two individuals in GdCa4O（BO3）3 crystal

Large GdCa4O(BO3)3 crystal has been grown by the Czochralski method.The quality of GdCa4(BO3)3 crystal was assessed by white-beam synchrotron radiation topography.It has been found that there is a sub-grain boundary in the GdCa4O(BO3)3 crystal.The boundary divides the large GdCa4O(BO3)3 crystal into two individuals.Due to the misorientation between the two individuals,the image shifts can be observed in the synchrotron topopraphs.Based on the misorientation determined by high resolution X-ray diffractometer,the image shifts were calculated for several reflections.The calculations are in agreement with the measurements from the topogrphs very Well.In addition,the formation mechanism of sub-grain boundary is discussed.2001 Elsevier science B.V.All rights reserved.

GdCa4O（BO3）3晶体中由小角晶界导致的同步辐射形貌像漂移的观察和计算

采用Czochralski法，我们成功地生长了大尺寸GdCa4O(BO3)3单晶。在对晶体的完整性进行检测的过程中发现：晶体中存在亚晶界，该晶界贯穿整个大单晶。由于亚晶界两边的单体存在取向差，在同步辐射形貌像中可观察到像漂移。根据高分辨X射线衍射所确定的取向差，我们计算了对应几个典型衍射的形貌像漂移，计算结果与从形貌像中测量的结果符合得很好。

Characterization of Growth Defects in Nd:YCa4O(BO3)3 Crystals by Transmission Synchrotron Topography

The growth detects in Nd:YCa4O(BO3)3(Nd:YCOB) crystals were investigated by transmission synchrotron topography.It was found that growth striations were the primary defects in Nd:YCOB crystals.Grown-in dislocations.mosaic blocks and inclusions were also obsered in the crystals.The effect of temperature field on the formation of growth defects in the crystals was discussed.

GdAl3（BO3）4和Nd离子掺杂的倍频与自变频激光晶体研究

采用熔盐顶部籽晶法从K 2 Mo 3 O 10-B 2 O 3助熔剂中生长出尺寸为20 mm的优质GdAl 3(BO 3)4(简称GAB)和Nd^3+激活的自变频激光晶体。确定了GAB晶体的透光波长范围、折射率和倍频系数随波长的变化,结果表明其在整个透光范围内均可实现相位匹配。测定了Nd^3+∶GAB晶体在室温下的偏振吸收、荧光光谱和荧光寿命,进行了光谱计算,测试了晶体的自变频激光性能,实现了紫外-可见光-红外-中红外多波段激光输出。

Growth and Characteristic of YbAl_3(BO_3)_4 Crystal

YbAl3(BO3)4 crystal of good optical quality was grown by the flux method. The structure of YbAl3(BO3)4 crystal was determined by single-crystal X-ray diffraction. The experiment shows that YbAl3(BO3)4 belongs to the double bo-rates with a trigonal structure. The space group is R32 and its unit cell constants were measured to be a = 0.92965 nm, c=0.72129 nm, V = 0.53673 nm3, Z=3. The transmittance spectra were measured. The cut-off of YbAl3(BO3)4 crystal is 216 nm, and there are two absorption peaks located at 940 and 975 nm from 190 nm to 2600 nm. The thermal properties of YbAl3(BO3)4 crystal were studied for the first time. The average thermal expansion coefficients were determined to be 2×10-6/℃, 9.5×10-6/℃along a- and c- direction. The specific heat of YbAl3(BO3)4 crystal was measured to be 0.6695 J·(g·℃) -1 at room temperature . All results indicate that the YbAl3(BO3)4 crystal is an excellent stoichioimet-ric laser material.

Growth and Spectroscopic Properties of Nd^(3+):Sr_3Gd_2(BO_3)_4 Crystal

This paper reports the growth, X-ray diffraction and spectroscopy of Nd3＋：Sr3Gd2（BO3）4 crystal. A Nd3＋：Sr3Gd2（BO3）4 crystal with dimensions of φ20 × 45 mm3 has been grown by the Czochralski method. Nd3＋：Sr3Gd2（BO3）4 crystal belongs to the orthorhombic system, space group Pnma （D2h） with a = 0.7401, b = 1.604 and c = 0.8755 nm. The absorption and emission spectra of Nd3＋：Sr3Gd2（BO3）4 were investigated. The absorption cross section oa is 3.11 × 10^-20cm2 at 808 nm. The absorption transition at 808 nm has an FWHM of 14 nm. The luminescence lifetime τf is 51.7 μs. The emission cross section oc at 1064 nm wavelength is 1.09 × 10^-19 cm2.

Synthesis, Crystal Structure and Fungicidal Activity of (Z)-3,3-Dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one O-2-Chlorobenzyl Oxime Nitrate

The title compound has been synthesized by the reaction of 3,3-dimethyl-1-（1H-1,2,4-triazol-1-yl）butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65～68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481（8）, b = 9.3351（5）, c = 13.1911（7） , β = 98.9450（10）°, Z = 4, V = 1769.67（17） 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F（000） = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections （I 2σ（I））. X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.

Preparation of microsized single-crystalline Co_3O_4 by high-temperature hydrolysis

Microsized single-crystalline Co3O4 has been synthesized by high-temperature hydrolysis of CoCD2H20 at 600℃. The samples were characterized by powder X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. The results reveal that the as-prepared powders are microsized single-crystalline CO3O4 with cubic spinel structure. An increase in the high-temperature hydrolysis time results in the evolution of particle shapes from cube to quasi-sphere, and then to octahedron. The effect of NaCl additive on the surface morphologies of Co3O4 particles was experimentally investigated. The results indicate that the NaCl additive acts as an inert disperse phase in the high-temperature hydrolysis, and prevents the aggregation of Co3O4 particles effectively.

Growth and Crystal Structure of YbAl_3(BO_3)_4

The compound YbAl3(BO3)4 belongs to huntite, space group R32 with cell parameters: a = 9.251(2), c = 7.189(3) ? Z = 3, Dc = 4.574 g/cm3, F(000) = 675.0, V = 532.84 3, ?= 13.63 mm-1, (MoK? = 0.71073 ? Mr = 489.22, (YbAl3B4O12), the final R = 0.0286 and wR = 0.0710. The Yb3+ ion occupies the trigonal prismatic site and the Al3+ ion occupies the octahedral site. There are two sets of (BO3)3- planar triangles. The Yb3+ ions are connected by means of YbOAl[B(2)]Yb with the distance 5.854 ?

Growth and Characteristics of Nd^(3+):GdAl_3(BO_3)_4 Crystal

Nd3+:GdAl3(BO3)4 (NGAB) crystal with the size of 30 mm was grown from the solvent system of K2O-Gd2O3-MoO3-B2O3 by combining accelerated seed rotation technology with medium seeded solution growth (MSSG) method, and its crystal structure has been determined by X-ray powder diffraction. It crystallizes in the trigonal system, space group R32 with a = 9.2734(2), c = 7.2438(1) ? V = 538 ?, Z = 3 and Dc = 4.379 g/cm3. The absorption and emission spectra of NGAB in the function of s and polarizations at room temperature have been measured. UV generation tuneable in 378～382 nm, green (531 nm) generation and blue generation tuneable in 436～443 nm as well as red (669 nm) generation by self-frequency changing were obtained with the output of 105, 119.5, 445 and 19 mJ/pulse, respectively, when the crystal was pumped by a dye laser.

Growth and Structure of Sr_3Yb_2(BO_3)_4 Crystal

A Sr3Yb2（BO3）4 single crystal was obtained by the Czochralski method. The structure of Sr3Yb2 （BO3）4 crystal was determined by single-crystal X-ray diffraction. The compound crystallizes in orthorhombic, space group Pnma with a=7.3750（8）, b=15.9265（14）, c=8.6776（9）, V=1019.25（18）3 , Mr=844.18, Z=4, Dc=5.501 g/cm3 , λ（MoKa）=0.71073, μ= 33.835 mm-1 , F（000）=1480, the final R=0.0339 and wR=0.0907 for 1090 observed reflections with I〉2σ（I）. The structure features a three-dimensional framework composed of isolated BO3 planar triangles bridged by YbO8 and SrO8 polyhedra. The Sr2＋ and Yb3＋ occupy statistically three independent sites with a Cm and two C1 local symmetries.

CRYSTAL STRUCTURE OF DI(α-HYDROXYISOBUTYRATE)DIAQUO NEODYMIUM NITRATE Nd(C_4H_7O_3)_2NO_32H_2O

The crystal structure of di-hydroxyisobutyrate)diaquo neodymium nitrate Nd(C_4H_7O_3)_2NO_32H_2O was determined by X-ray diffraction analysis. It belongs to monoclinic,space group C2/C,with cell dimensionsa=8.996(1), b=8.601(1),c=21.111(3),β=92.38°,V=1632.O,Z=4,D_c=1.83g/cm^3.Crystal structure has been refined by full-matrix least-square techniques giving a final R value of 0.036.The neodymium atom is coordinated to eight oxygen atoms.The nitrate group in complex is not bonded to neodymium,each two neodymium atoms are linked by bridging carboxyl group forming a chain polymeric molecule.

Synthesis and CrystalStructure of Dicesiumtrans-Dicarbonatotetraaquom agnesium ,Cs_2[Mg(CO_3)_2(H_2O)_4]

The title compound, Cs 2[Mg(CO 3) 2(H 2O) 4], was synthesized by the dropwise addition of an aqueous solution of Mg(NO 3) 2 to a stirred aqueous Cs 2CO 3/CsHCO 3 solution. A colorless needle shaped crystal was formed by slow evaporation. The crystal structure was established on the basis of the single crystal X ray diffraction data. Cs 2[Mg(CO 3) 2(H 2O) 4] crystallized in the orthorhombic space group Pbca (No. 61) with a =0.658 4(1) nm, b =1.257 9(1) nm, c =1.301 3(1) nm, \{ V =1.077 8 nm 3, Z =4, D x=2.971 g·cm -3 , μ =69.20 cm -1 , F (000)=888, T =298 K, final R =0.029 and R w=0.024 for 1 037 observed reflections. The crystal consists of Cs + cations and the complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions with each Mg atom coordinated by the six oxygens of two carbonate groups and four water molecules [ d (Mg_O)=0.203 6(4), 0.207 4(4), 0.213 4(4) nm]. The complex trans [Mg(CO 3) 2(H 2O) 4] 2- anions are arranged in a strongly compressed bcc pattern. A 3D network was formed through the intermolecular hydrogen bonds. The Cs + cations are located in cavities, each being surrounded by nine oxygens of five complex anions with d (Cs_O)=0.306 1-0.348 8 nm. The CO 2- 3 group reveals a lowering of D 3h symmetry due to site and coordination effects, but not any observable deviation from co planarity [ d (C_O)=0.127 2(6), 0.127 5(7) , 0.130 5(6) nm and O_C_O=119.6(5)°, 120.1(5)°, 120.4(5)°].

Synthesis,Characterization and Crystal Structure of 3-o-Fluorophenyl-6-(4-decarboxydehydroabietyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole

Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole（6a,C28H31FN4S） was structurally determined by single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a=6.0153（14）,b=12.2577（19）,c=34.055（3）A,V=2511.0（7）A^3,Z=4,Mr=474.63,Dc=1.255Mg/m^3,λ=0.71073 A,μ（MoKα）=0.160 mm^-1,F（000）=1008,the final R=0.0555 and wR=0.1248 for 3094 observed reflections with I〉2σ（I）.There are six rings in the crystal structure of the title compound.The dihedral angle between 1,2,4-triazole and 1,3,4-thiadiaole rings is 1.4o,and that between 1,2,4-triazole and benzene ring D 25.5o.

Synthesis and Characterization of CaPd₃O₄Crystals

A new method for the crystal growth of alkaline-earth palladate CaPd3O4 was developed. The crystals were synthesized on a voltage-applied electrode in a molten chloride solvent. The maximum length of the crystal was about 1.5 mm. The X-ray diffraction data were refined well by assuming a cubic structure of the space group Pm n, and the lattice constant a was 5.7471 (10) ?. The temperature dependence of the resistivity showed semiconductor-like characteristics with a very small activation energy Ea of 0.45 meV at low temperatures, and the resistivity at 300 K was 0.1 cm. The temperature dependence of the molar magnetic susceptibility showed the Curie-Weiss paramagnetic behavior with a small molar Curie constant Cmol of 5.0(1) × 10-3 emu K/(mol Oe), indicating the existence of localized spin moments.

Na_(2)O对锂铝硅微晶玻璃析晶及性能的影响

采用熔融法制备了不同Na_(2)O含量的透明锂铝硅微晶玻璃,通过DSC、XRD、FESEM等测试方法研究了不同Na_(2)O含量对玻璃析晶及性能的影响。结果表明:Na_(2)O的引入能显著降低玻璃的转变温度和析晶温度,抑制LiAlSi_(4)O_(10)晶相的析出。但Na_(2)O的引入促使微晶玻璃中析出Li_(2)Si_(2)O_(5)新相,并且随着Na_(2)O引入量的增加,Li_(2)Si_(2)O_(5)转变为主晶相。由于晶体尺寸均为纳米级,主晶相的转变对透过率影响较小,微晶玻璃的可见光透过率均高于85%。主晶相的转变有效增强了微晶玻璃的机械性能,其弯曲强度由300 MPa提升至331 MPa。Na_(2)O的引入有效增强了Na-K交换,Na_(2)O含量为4%(质量分数)的Li 2O-Al_(2)O_(3)-SiO_(2)微晶玻璃在410℃的KNO_(3)熔盐中交换6 h后,维氏硬度由7.108 GPa提升至7.403 GPa,弯曲强度由331 MPa提升至470 MPa。

Yb∶YAl_3(BO_3)_4 晶体形貌与生长速度的关系

观察测量了不同生长速度 (相应于不同降温速度 )自发成核生长的Yb∶YAl3(BO3) 4 晶体形貌。粒度较大 ( >2mm)的晶体不管降温速度快慢形态都很简单 ,只发育六方柱 { 112 0 }和菱面体 { 10 11} ;粒度较小 ( <2mm)的晶体形态随降温速度增快而变复杂 ,发育一些罕见的高指数晶面。说明在生长速度较快的条件下 ,在晶体生长早期 ,一些高能面发育 ,在晶体生长后期已尖灭了 ,晶体生长的大部分时间是在低能面 { 112 0 }和 { 10 11}上进行的。对比了不同生长条件下晶面的粗糙度 ,随着降温速度的增快 ,六方柱面 { 112 0 }和菱面体面 { 10 11}由光滑变粗糙 ,顶面 { 0 0 0 1}永远是粗糙的。从晶体结构上定性地探讨了 3种晶面的杰克逊因子α及生长机理。

H_3BO_3添加量对SrAl_2O_4:Eu^(2+),Dy^(3+)蓄光性能的影响

采用共沉淀法制备SrAl2O4∶Eu2+,Dy3+蓄光材料,研究了H3BO3添加量对SrAl2O4:Eu2+,Dy3+蓄光性能的影响.XRD和光学性能测试结果表明,硼酸添加量为5wt%的样品结晶完全,其初始亮度达到5000mcd/m2,余辉时间大于8h,随着硼酸添加量增加,样品结晶程度降低、发光强度逐渐下降、余辉衰减速度加快.因此添加适量硼酸可以改善SrAl2O4:Eu2+,Dy3+的结晶性能和发光性能,过量添加硼酸将导致样品严重结块,SrAl2O4相减少、发光性能大大降低.

H_3BO_3对微波等离子体法合成SrAl_2O_4∶Eu^(2+),Dy^(3+)的影响

采用微波等离子体法合成SrAl2O4∶Eu2+,Dy3+长余辉发光材料,探讨了H3BO3的加入对材料的光谱性能、余辉性能、相组成结构、微观形貌的影响。结果表明,适量的添加助溶剂H3BO3,有利于增强材料的发光强度,延长余辉时间,但过量的添加反而会导致发光性能下降。本试验确定硼酸的最佳添加量为10%。综合检测分析结果推断,硼酸加入后在高温下大部分形成液相,并通过液相传质促进晶体生长,提高基质的结晶程度,同时促进稀土离子Eu2+,Dy3+进入晶格并使其分布更均匀;而少部分则会进入晶格发生B取代Al,引起晶体场畸变,从而提高了材料的发光强度和长余辉特性。