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Growth and Characterization of Bisthiourea Nickel Bromide—New Semiorganic Nonlinear Optical Crystal 新型半有机非线性光学晶体双硫脲-溴化镍的生长与表征
Pub Date : 2013-04-30 DOI: 10.4236/JCPT.2013.32008
R. Sundararajan, M. Senthilkumar, C. Ramachandraraja
A new semiorganic nonlinear optical crystal of bisthiourea nickel bromide (BTNB) was grown successfully by slow evaporation technique using water as solvent. The lattice parameters of the grown crystal have been determined by X-ray diffraction studies. Vibrational spectrum is recorded to determine symmetries of molecular vibrations. Optical absorbance spectrum recorded revealed that this crystal has good transparency in the visible region. The second harmonic generation test of BTNB confirmed the nonlinear nature of the crystal. The BTNB crystal was analyzed by a differential thermal analysis and thermogravimetric analysis (DTA-TGA) to obtain its thermal stability. Vickers microhardness test done on the crystal shows that the crystal has greater physical strength.
以水为溶剂,采用慢蒸发法制备了新型双硫脲-溴化镍半有机非线性光学晶体。通过x射线衍射研究确定了生长晶体的晶格参数。记录振动谱以确定分子振动的对称性。光学吸收光谱记录表明,该晶体在可见光区具有良好的透明度。BTNB的二次谐波产生试验证实了晶体的非线性性质。采用差热分析和热重分析(DTA-TGA)对BTNB晶体进行了热稳定性分析。对该晶体进行维氏显微硬度测试,表明该晶体具有较高的物理强度。
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引用次数: 3
Optical Methods in Orientation of High-Purity Germanium Crystal 高纯锗晶体取向的光学方法
Pub Date : 2013-04-30 DOI: 10.4236/JCPT.2013.32009
Guojian Wang, Yongchen Sun, Y. Guan, D. Mei, Gang Yang, A. A. Chiller, Bruce Gray
Two optical methods, namely crystal facet reflection and etching pits reflection, were used to orient and high-purity germanium crystals. The X-ray diffraction patterns of three slices that were cut from the oriented and crystals were measured by X-ray diffraction. The experimental errors of crystal facet reflection method and etching pits reflection method are in the range of 0.05° - 0.12°. The crystal facet reflection method and etching pits reflection method are extremely simple and cheap and their accuracies are acceptable for characterizing high purity detector-grade germanium crystals.
采用晶体面反射和蚀刻凹坑反射两种光学方法对高纯度锗晶体进行定向。用x射线衍射仪测量了从取向和晶体上切下的三个薄片的x射线衍射图。晶体面反射法和蚀刻坑反射法的实验误差在0.05°~ 0.12°之间。晶体面反射法和蚀刻坑反射法是一种非常简单和廉价的方法,它们的精度对于表征高纯度探测级锗晶体是可以接受的。
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引用次数: 9
Dielectric and Optical Characterization of Boron Doped Ammonium Dihydrogen Phosphate 掺硼磷酸二氢铵的介电和光学特性
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31002
Delci Zion, Shyamala Devarajan, T. Arunachalam
Single crystals of pure and boron doped ammonium dihydrogen phosphate were grown from aqueous solution by slow solvent evaporation process. ICP studies were done to confirm the presence of the dopant boron in the parent crystal. The values of the lattice parameters were determined by single crystal X-ray diffraction. The pure and doped ADP crystals were found to have tetragonal structure. Complete optical characterizations of the crystals were done using the FTIR, UV-Vis and NLO studies. The presences of the various functional groups in the crystals were identified by FTIR spectrum. The band gap energies of the pure and doped crystals have been calculated at their cut off frequencies using the UV-Vis spectrum. The second harmonic generation efficiency of the crystals was determined. The electric properties of the grown crystal have been analyzed by studying the variation of dielectric constant and dielectric loss with frequency.
采用缓慢溶剂蒸发法制备了纯磷酸二氢铵和掺硼磷酸二氢铵单晶。ICP研究证实了掺杂硼在母晶中的存在。通过单晶x射线衍射测定了晶格参数的取值。发现纯ADP和掺杂ADP晶体具有四方结构。使用FTIR, UV-Vis和NLO研究完成了晶体的完整光学表征。用FTIR光谱鉴定了晶体中各种官能团的存在。利用紫外-可见光谱计算了纯晶体和掺杂晶体在其截止频率处的带隙能。测定了晶体的二次谐波产生效率。通过研究晶体介电常数和介电损耗随频率的变化,分析了晶体的电性能。
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引用次数: 15
Crystallization and Characterization of a New Fluorescent Molecule Based on Schiff Base 一种新型希夫碱荧光分子的结晶与表征
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31004
Dehua Zhang, Xiaoyan Zhang
In this analysis, the single crystal of schiff base has been synthesized and the purity of material has been increased by repeated recrystallization process. Single crystal was grown by adopting the method growing in a slow evaporation solution using ethanol as solvent at room temperature. A new fluorescent molecule based on Schiff base has been synthesised and its binding properties investigated by fluorescence spectroscopy to show that it can selectively bind Cu2+ with fluorescence quenching.
在此分析中,合成了席夫碱单晶,并通过反复的再结晶工艺提高了材料的纯度。在室温下,以乙醇为溶剂,在缓慢蒸发溶液中生长单晶。合成了一种新的基于希夫碱的荧光分子,并通过荧光光谱研究了其结合特性,表明它可以选择性地结合Cu2+并具有荧光猝灭作用。
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引用次数: 4
ACCEPT-NMR: A New Tool for the Analysis of Crystal Contacts and Their Links to NMR Chemical Shift Perturbations ACCEPT-NMR:一种分析晶体接触及其与核磁共振化学位移摄动的联系的新工具
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31003
I. Sergeyev, A. McDermott
We have developed an open-source cross-platform software toolkit entitled ACCEPT-NMR (Automated Crystal Contact Extrapolation/Prediction Toolkit for NMR) as a helpful tool to automate many of the complex tasks required to find and visualize crystal contacts in structures of biomolecules and biomolecular assemblies. This toolkit provides many powerful features geared toward NMR spectroscopy and related disciplines, such as isotopic labeling, advanced visualization options, and reporting tools. Using this software, we have undertaken a survey of available chemical shift data in the literature and deposited in the BMRB, and show that the mere presence of one or more crystal contacts to a residue confers an approximately 65% likelihood of significant chemical shift perturbations (relative to solution NMR chemical shifts). The presence of each additional crystal contact subsequently increases this probability, resulting in predictive accuracies in excess of 80% in many cases. Conversely, the presence of a significant experimental chemical shift perturbation indicates a >60% likelihood of finding one or more crystal contacts to a particular residue. Pinpointing sites likely to experience large CSPs is critical to mapping solution NMR chemical shifts onto solid-state NMR data as a basis for preliminary assignments, and can thus simplify the assignment process for complex biomolecules. Mapping observed CSPs onto the molecular structure, on the other hand, can indicate the presence of crystal interfaces where no crystal structure is available. Finally, by detecting sites critical to intermolecular interfaces, ACCEPT-NMR can help guide experimental approaches (e.g. isotopic labeling schemes) to detect and probe specific inter-subunit interactions.
我们开发了一个开源的跨平台软件工具包,名为ACCEPT-NMR(自动晶体接触外推/预测工具包,用于核磁共振),作为一个有用的工具,可以自动执行许多复杂的任务,以发现和可视化生物分子和生物分子组装结构中的晶体接触。该工具包提供了许多强大的功能,面向核磁共振光谱和相关学科,如同位素标记,高级可视化选项和报告工具。使用该软件,我们对文献中可用的化学位移数据进行了调查,并将其保存在BMRB中,结果表明,仅仅存在一个或多个晶体接触到残留物,就会产生大约65%的显著化学位移扰动的可能性(相对于溶液核磁共振化学位移)。每个额外的晶体接触的存在随后增加了这种可能性,导致在许多情况下预测精度超过80%。相反,如果存在显著的实验化学位移扰动,则表明有60%的可能性找到一个或多个与特定残留物的晶体接触。精确定位可能经历大型csp的位点对于将溶液核磁共振化学转移映射到固态核磁共振数据上作为初步分配的基础至关重要,因此可以简化复杂生物分子的分配过程。另一方面,将观察到的csp映射到分子结构上,可以表明在没有晶体结构的地方存在晶体界面。最后,通过检测分子间界面的关键位点,ACCEPT-NMR可以帮助指导实验方法(例如同位素标记方案)检测和探测特定的亚基间相互作用。
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引用次数: 1
The Oleic Acid Composition Effect on the Carboxymethyl Cellulose Based Biopolymer Electrolyte 油酸组成对羧甲基纤维素基生物聚合物电解质的影响
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31001
M. Chai, D. Zion, S. Devarajan, I. Sergeyev, D. H. Zhang, R. Rastogi, S. K. Srivastava, A. Fouzri, M. A. Boukadhaba, A. H. Tauré, N. Sakly, I. Sergeyev, Ann E. McDermott
Biopolymer electrolyte based on carboxymethyl cellulose has been prepared by doping with different concentration of oleic acid via solution casting technique. Fourier Transform Infrared spectroscopy was used to study the complexation between the salt and polymer. New peak was observed at 1710, 2850, 2920 cm-1. X-ray diffraction study reveals the amorphous nature of the biopolymer electrolyte. Impedance study shows the highest ionic conductivity, σ, was found to be 2.11 × 10-5 S·cm-1 at room temperature (303 K) for sample containing 20 wt.% of oleic acid and the biopolymer electrolyte obeys Arrhenius behaviour.
采用溶液浇铸技术,在羧甲基纤维素上掺杂不同浓度的油酸,制备了生物聚合物电解质。利用傅里叶变换红外光谱对盐与聚合物的络合作用进行了研究。在1710、2850、2920 cm-1处出现新峰。x射线衍射研究揭示了生物聚合物电解质的无定形性质。阻抗研究表明,在室温(303 K)下,当油酸含量为20%时,生物聚合物电解质的最高离子电导率σ为2.11 × 10-5 S·cm-1,符合阿伦尼乌斯行为。
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引用次数: 111
Synthesis, Spectral Characterization and Ligation of N-(2-(Phenylseleno)ethyl)phthalimide N-(2-(苯硒基)乙基)邻苯亚胺的合成、光谱表征及连接
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31005
R. Rastogi, S. Srivastava, Shikha Asolia, R. Butcher
PhSe-Na+ generated in situ by reduction of PhSeSePh, with sodium borohydride on reaction with N-(2-bromoethyl) phthalimide in N2 atmosphere results in the formation of N-[2-(phenylseleno)ethyl]phthalimide (L1). The title compound has been characterized by elemental analysis, FT-IR, 1H and 13C NMR techniques. The crystal structure of L1 has been solved by direct methods and refined by full-matrix least squares. The ligand L1 crystallize in the monoclinic space group. Selenium forms two Se-C linkages, one is due to Se-Calkyl and the other one to Se-Caryl. Further, the ligation reaction of L1 with complex 1 is also explored whose identities are characterized by spectroscopic techniques.
用硼氢化钠还原PhSeSePh原位生成PhSe-Na+,与N-(2-溴乙基)邻苯亚胺在N2气氛下反应生成N-[2-(苯硒基)乙基]邻苯亚胺(L1)。通过元素分析、FT-IR、1H和13C NMR等技术对该化合物进行了表征。用直接法求解了L1的晶体结构,并用全矩阵最小二乘法对其进行了细化。配体L1在单斜空间群中结晶。硒形成两个Se-C键,一个是Se-Calkyl键,另一个是Se-Caryl键。此外,还探讨了L1与配合物1的连接反应,并利用光谱技术对其身份进行了表征。
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引用次数: 4
Structural, Morphological, Optical and Electrical Properties of Zn(1−x)CdxO Solid Solution Grown on a- and r-Plane Sapphire Substrate by MOCV MOCV法生长Zn(1−x)CdxO固溶体的结构、形态、光学和电学性质
Pub Date : 2013-01-28 DOI: 10.4236/JCPT.2013.31006
A. Fouzri, M. A. Boukadhaba, A. H. Tauré, N. Sakly, A. Bchetnia, V. Sallet
Zn(1-x)CdxO films have been grown on (a-plane) and (r-plane) sapphire substrate by metal organic chemical vapor deposition. A maximum cadmium incorporation of 8.5% and 11.2% has been respectively determined for films deposited on a- and r-plane sapphire. The optical transmission spectra and energy band-gap equation established by Makino et al. were used to estimate the cadmium mole fraction of the solid solutions. Structural, morphological and optical properties of these films were examined using high resolution X-ray diffraction (HRXRD), atomic force microscopy (AFM) and room and low temperature photoluminescence (Pl) as Cd incorporation and employed substrate. X-ray diffraction study revealed that all films had wurtzite phase but solid solution grown on a-plane sapphire are polycrystalline with a preferred orientation along the [0001] direction and a-plane film are epitaxially grown on r-plane sapphire. AFM image show significant differences between morphologies depending on orientation sapphire substrate but no significant differences on surface roughness have been found. The near band-edge photoluminescence emission shifts gradually to lower energies as Cd is incorporated and reaches 2.916 eV for the highest Cd content (11.2%) at low temperature (20 K). The room temperature hall mobility decreases with the Cd incorporation but it is larger for Zn(1-x)CdxO grown on r-plane sapphire.
采用金属有机化学气相沉积方法在(a面)和(r面)蓝宝石衬底上生长了Zn(1-x)CdxO薄膜。测定了沉积在-面和r面蓝宝石薄膜上的镉的最大掺入量分别为8.5%和11.2%。利用Makino等人建立的光透射光谱和能带方程估算固溶体中镉的摩尔分数。采用高分辨率x射线衍射仪(HRXRD)、原子力显微镜(AFM)和室温和低温光致发光仪(Pl)作为掺杂和衬底,研究了这些薄膜的结构、形态和光学性能。x射线衍射研究表明,所有薄膜均为纤锌矿相,但在a面蓝宝石上生长的固溶体是沿[0001]方向优先取向的多晶,而在r面蓝宝石上生长的是外延生长的a面薄膜。AFM图像显示不同取向蓝宝石衬底的形貌有显著差异,但表面粗糙度无显著差异。随着Cd的掺入,近带边光致发光发射能量逐渐降低,在低温(20 K)下,Cd含量最高(11.2%)达到2.916 eV。室温霍尔迁移率随着掺入而降低,但在r面蓝宝石上生长的Zn(1-x)CdxO的霍尔迁移率较大。
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引用次数: 6
Rietveld Refinement of Nanocrystalline LiFeO 2 Synthesized by Sol-Gel Method and Its Structural and Magnetic Properties 溶胶-凝胶法制备纳米晶life2o2的Rietveld细化及其结构和磁性能
Pub Date : 2012-10-17 DOI: 10.4236/JCPT.2012.24022
K. Kumar, A. Sangeetha, A. Raghavender, Ž. Skoko, G. Kumar
Nanocrystalline lithium iron oxide LiFeO2 was synthesized using sol-gel method. Rietveld analysis was performed to confirm the different phases associated in the formation of LiFeO2. Quantitative Rietveld refinement revealed that sample contains: 39.9 wt% of cubic α – LiFeO2 phase, 58.5 wt% of monoclinic β - LiFeO2 and tetragonal 1.7 wt%. of γ - LiFeO2. The nanocrystalline nature of the prepared samples was confirmed by SEM analysis. The magnetic properties of LiFeO2 showed ferromagnetic property at room temperature.
采用溶胶-凝胶法制备了纳米晶氧化铁锂LiFeO2。Rietveld分析证实了不同相与LiFeO2的形成有关。定量Rietveld细化表明,样品中含有:立方相α - LiFeO2 39.9%,单斜相β - LiFeO2 58.5%,四方相1.7 wt%。γ - LiFeO2通过扫描电镜分析证实了所制备样品的纳米晶性质。LiFeO2的磁性能在室温下表现为铁磁性。
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引用次数: 4
Growth of Gallium Oxide Nanowires by Pulsed Laser Deposition 脉冲激光沉积法生长氧化镓纳米线
Pub Date : 2012-10-17 DOI: 10.4236/JCPT.2012.24017
H. Yamahara, M. Seki, H. Tabata
We report on the synthesis of gallium oxide nanowires by pulsed laser deposition using a gold catalyst. In the vapor-liquid-solid process, gold thickness was the crucial parameter for deciding the morphology of nanowires. In the case of 1 nm thick gold, homogeneous nanowire growth was confirmed at temperatures of 700°C to 850°C. Transmission electron microscopy and selected area electron diffraction measurements showed that the nanowires were polycrystalline. In the cathode luminescence spectra, UV, blue, green and red emission peaks were observed, as reported in previous studies. As growth temperature was increased, the relative intensities of blue, green, and red emissions decreased. Thermal annealing treatments were effective in decreasing the blue, green and red emission peaks, suggesting that these emission peaks were associated with oxygen vacancies.
报道了以金为催化剂,脉冲激光沉积法制备氧化镓纳米线的方法。在气-液-固工艺中,金的厚度是决定纳米线形貌的关键参数。在1 nm厚的金的情况下,在700°C到850°C的温度下,证实了均匀的纳米线生长。透射电镜和选择区域电子衍射测试表明,纳米线是多晶的。在阴极发光光谱中,观察到紫外、蓝、绿、红等发射峰,与前人的研究一致。随着生长温度的升高,蓝、绿、红排放的相对强度降低。热退火处理可以有效地降低蓝色、绿色和红色发射峰,表明这些发射峰与氧空位有关。
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引用次数: 12
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