助熔剂提拉法生长化学计量比LiNbO3晶体

利用助熔剂提拉法,分别从掺入11mol;K2O的同成份LiNbO3熔体中和从掺入19mol;*!K2O的化学配比LiNbO3熔体中生长出高质量近化学计量比LiNbO3单晶.对这两种从不同配比熔体中生长的晶体进行光谱分析表明,与同成份比LiNbO3相比较,其紫外吸收边出现明显蓝移,OH红外吸收峰的位置和线宽也都有显著的变化.室温极化反转测试显示,两种晶体的矫顽场分别为4.4kV/mm和0.8kV/mm.根据所得测量结果,估计两种晶体中Li2O的含量分别为49.6mol;和49.9mol;.其中从掺19mol; K2O化学配比LiNbO3熔体中生长出的LiNbO3单晶的Li2O含量已非常接近50mol;的化学配比.进一步优化生长工艺,获得成份均匀、大尺寸化学计量比晶体的工作正在进行中.     

提拉法生长大尺寸γ-LiAlO2单晶的研究

由于与GaN晶格失配小(约1.4%),γ-LiAlO2单晶有望成为一种很有希望的CaN外延衬底材料.本文使用提拉法生长出了尺寸达φ45×50mm3的γ-LiAlO2单晶.对该晶体毛坯的各个有代表性的位置作了X射线粉末衍射(XRPD)分析,结果表明仅仅在晶体毛坯的底部生成了一种缺锂相(LiAl5O8).γ-LiAlO2晶体化学稳定性差,在室温时轻微水解.当在空气中于1100℃退火70h,γ-LiAlO2晶体挥发出锂组分,在表面产生缺锂相(LiAl5O8).值得注意的是,在γ-LiAlO2晶体的红外光谱区不存在氢氧根吸收带.     

近化学计量比铌酸锂晶体的研究进展

本文总结了近化学计量比铌酸锂晶体的不同生长方法及它们各自的特色,分析了锂铌摩尔比对晶体性能的影响及Li含量的各种表征方法.通过比较看出,采用K2O助熔剂生长近化学计量比铌酸锂晶体是一种较为实用的途径.基于此,我们采用K2O助熔剂提拉法和助熔剂-坩埚下降法生长了近化学计量比铌酸锂晶体,所得晶体的最大尺寸分别达到45mm×60mm和25mm×40mm.     

Ba2TiSi2O8晶体的生长及包裹物缺陷分析

采用提拉法生长了Ba2TiSi2O8 (BST)晶体,并采用SEM和EDS等手段对晶体内部包裹物缺陷进行了分析.发现多晶原料中的Na,K,C1杂质元素的存在是导致晶体内部产生包裹物缺陷的主要诱因,采用低的生长速率和较快的晶体转速有利于获得高质量BTS单晶.另外,本论文还对晶体的硬度和透过光谱进行了测试与分析.     

导模提拉法生长Tb3Sc2Al3O12(TSAG)晶体及性质表征

本文采用导模提拉法成功生长了Tb3Sc2Al3O12 (TSAG)晶体,并对所生长晶体进行了物相分析和单晶结构分析,探讨了多晶原料的烧结温度对晶体颜色的影响.Sc3+和Al3+的浓度分布测试表明,导模提拉法能较好地克服因分凝效应引起的Sc3+浓度分布不均,可以生长获得浓度分布均匀的TSAG晶体.磁光性能测试表明,Sc3+掺入对晶体在400～1100 nm波长范围内的磁光性能影响不大,所生长TSAG晶体的费尔德常数仅比Tb3Al5O12 (TAG)晶体低6; ～8;.     

提拉法与温梯法Yb∶YAG晶体性能的比较

采用提拉法和温梯法生长出掺杂浓度为 5 %原子分数的Yb∶YAG激光晶体 ,比较了两种不同生长方式的晶体在晶胞参数、Yb离子纵向分布以及吸收光谱上的差异 ,发现温梯法生长对晶体晶胞结构影响较少 ,但是Yb离子纵向分布相差较大。指出提拉法生长的晶体在 2 5 6nm处的弱吸收是由于Fe3 + 引起的。     

提拉法与温梯法Yb:YAG晶体性能的比较

采用提拉法和温梯法生长出掺杂浓度为5;原子分数的Yb∶YAG激光晶体,比较了两种不同生长方式的晶体在晶胞参数、Yb离子纵向分布以及吸收光谱上的差异,发现温梯法生长对晶体晶胞结构影响较少,但是Yb离子纵向分布相差较大.指出提拉法生长的晶体在256nm处的弱吸收是由于Fe3+引起的.     

大尺寸Y方向钽酸镓镧压电晶体生长及性能研究

成功采用提拉法生长了尺寸φ80 mm×100 mm的Y方向钽酸镓镧压电晶体,晶体整体透明、无包裹体.采用LCR电桥测量了晶体的相对介电常数,采用谐振-反谐振法测量了压电应变常数.研究了头尾之间性能差异性,头尾频率常数均匀性达到99.95;,表明晶体存在良好的性能均匀性.此外,还对(010)晶面进行了摇摆曲线和频率温度系数测试,测得FHMW和TCF值分别为38.5"、1.23ppm/K.     

Sm∶YCOB晶体生长及吸收光谱表征

采用熔体提拉法生长了高质量Sm3+掺杂YCa4O(BO3)3(YCOB)晶体.通过X射线粉末衍射、高分辨X射线衍射摇摆曲线、ICP-AES、吸收光谱等对晶体的性能进行了研究.发现生长的Sm∶ YCOB晶体与YCOB晶体具有相同的结构,结晶质量较好,半高宽可达31弧秒;5at;浓度掺杂时Sm3+在YCOB晶体中分凝系数为0.773;晶体在1400～1600 nm范围内有若干较强的吸收峰.     

助熔剂籽晶提拉法生长化学计量比LiTaO3晶体

利用助熔剂籽晶提拉法,在同成份LiTaO3熔体中掺入一定剂量的K2O,生长出了近化学计量比LiTaO3晶体.对晶体进行畴结构、居里温度以及光谱分析,结果表明与同成份比LiTaO3晶体相比较,畴结构为规则的六边形,紫外吸收边出现明显蓝移,晶体居里温度也随之提高,晶体头部居里温度为681.2℃,尾部为684.8℃.     

Czochralski Growth of Potassium Lithium Niobate Single Crystals with Low Li Content and Their Characterization

Single crystalline and crack free potassium lithium niobate (KLN) single crystals with low Li content were grown by the Czochralski method. The crystal composition can be written as K_2.60Li_1.17Nb_5.44O₁₅ (=K_2.95Li_1.33Nb_6.17O₁₇) which contain relatively fewer Li ions than ferroelectric K₃Li₂Nb₅O₁₅ crystals. All experimental results show that the deficiency of the Li ions in the KLN crystals strongly influences their physical properties. Especially, the as‐grown crystals do not indicate any signature for a ferroelectric phase transition in contrast to the ferroelectric K₃Li₂Nb₅O₁₅ crystals. However, due to ionic conduction, the temperature dependence of the dielectric constant of such KLN‐2 crystals show a broad anomaly near 300°C. In addition, the existence of proton defects can be revealed by infrared absorption spectroscopy near 3500 cm^‐1 in as‐grown crystals.     

The Czochralski Method ‐ where we are 90 years after Jan Czochralski’s invention

The Czochralski method, i.e. pulling a crystal from the melt, became the most important technology for the production of large semiconductor (Si, GaAs, InP, GaP …) and optical crystals (oxides, CaF₂ …). The present status is achieved by a profound analysis of the mechanisms of heat and species transport which are relevant for the stability of the Czochralski growth process and the performance of the growing crystal. It was clearly demonstrated in the last few years that modeling by numerical simulation is an indispensable tool to analyze the Czochralski process and to understand the governing mechanisms. The contribution presents examples of this kind of modeling the Czochralski technique in correlation with experimental investigations in order to illustrate the present status of understanding relevant processing phenomena. Furthermore, it is shown what problems need still to be solved in the future in order to further improve the yield and quality of Czochralski‐grown crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Domain structures and etching morphologies of lithium niobate crystals with different Li contents grown by TSSG and double crucible Czochralski method

Stoichiometric lithium niobate single crystals with different Li contents have been grown both by the top‐seeded solution growth (TSSG) method from potassium containing flux and by the double crucible Czochralski (DC Cz) method. Spectroscopic properties (e.g. the UV absorption edge, Raman linewidth) and the Curie temperature measurement have been used for the characterization of the crystal composition. The double crucible Czochralski method is found to be suitable for mass production of stoichiometric LiNbO₃ with Li content larger than 49.7 mol% and homogeneity of 0.03 mol%. The domain structures and etching morphologies on negative and positive c‐surface were also investigated by chemical etching method. A new domain structure of three‐fold symmetric sectors were observed in near‐stoichiometric LiNbO₃ grown by TSSG method. The straight line arrangement hillocks on negative c‐surface and the net‐like arrangement etch lines were observed and explained by stress etching mechanism. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

提拉法生长高质量氟化镁单晶

设计了适合提拉法生长氟化镁单晶体的温场,采用提拉法成功生长出了直径100 mm的高质量氟化镁单晶.晶体内无气泡等宏观缺陷、无开裂;通过精密退火处理后,晶体透过率达到95;,平均应力双折射小于0.5 nm/cm.上述结果表明采用提拉法可以生长高质量的氟化镁单晶.     

大尺寸YVO4晶体的自动控径提拉法生长

本文报道了在自动控制直径条件下大尺寸YVO4晶体的提拉法生长研究.利用改进的上称重法生长大尺寸YVO4晶体,在提拉法单晶生长过程中,晶体扩肩部分采用斜率积分模式,转肩部分采用斜率积分过渡到直径积分模式,等径部分采用直径积分模式,应用这种分段控制方式成功地实现了YVO4晶体的自动化生长.采用4台50型自动化生长炉对YVO...     

三坩埚提拉法生长铽镓石榴石单晶研究

采用三坩埚提拉法生长出高质量铽镓石榴石(Tb3Ga5O12,TGG)单晶,晶体尺寸为φ25 mm×40 mm.通过X射线衍射、双晶衍射分析讨论TGG单晶的晶体结构和单晶性,并采用He-Ne激光费尔德常数测试装置测定TGG单晶的费尔德常数.结果表明:采用三坩埚提拉法生长的TGG单晶具有＜111＞取向、强度高,双晶摇摆曲线半峰宽为17 s;晶体在632.8 nm处的费尔德常数为0.553 min/cm·Oe.     

Growth and spectroscopic characterization of Zr:Fe:LiNbO3 crystals with various Li/Nb ratios

In this paper, Zr:Fe:LiNbO₃ crystals with various Li/Nb ratios were grown by the Czochralski method from melts having compositions varying between 48.6 and 58 mol% Li₂O. X-ray powder diffraction (XRD), inductively coupled plasma optical emission/mass spectrometry (ICP-OE/MS), ultraviolet–visible (UV–vis) absorption and the infrared (IR) spectrum were measured and are discussed in terms of the spectroscopic characterization. It was found that as the Li/Nb ratio increases in the melt, the Li/Nb ratio in the crystal also increases, the distribution coefficients of Fe and Zr ions decrease, the absorption edge shifts to a shorter wavelength, and the ZrO₂ threshold concentration of the samples decreases.     

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     

提拉法生长镓酸锂晶体及缺陷研究

研究了提拉法生长的镓酸锂单晶的生长习性和结晶质量.晶体表面呈乳白色且表面粗糙.通过光学显微镜、四晶X射线衍射、透射光谱和电感耦合等离子体发射光谱对样品进行了表征,结果表明,在(001)面的抛光样品上存在三种缺陷: [110]和[-110]方向的十字线、[010]方向排列的气泡包裹物以及平行于(010)面的界面,界面的产生起因于(010)晶面的滑移;晶体的结晶质量从顶部到底部逐渐下降,这是由于在生长过程中氧化锂的挥发导致熔体成分偏离化学计量比造成的.     

Growth and photorefractive properties of Mg:Ce:Cu:LiNbO3 crystals grown by Czochralski method

In this paper, photorefractive properties of Mg:Ce:Cu:LiNbO₃ crystals were studied. The crystals doped with different concentration of Mg ions have been grown by the Czochralski method. Mg concentrations in grown crystals were analyzed by an inductively coupled plasma optical emission spectrometry (ICP‐OE/MS). The crystal structures were analyzed by the X‐ray powder diffraction (XRD), ultraviolet‐visible (UV‐Vis) absorption spectra and infrared (IR) transmitatance spectra. The photorefractive properties of crystals were experimentally studied by using two‐beam coupling. In this experiment we determined the writing time, maximum diffraction efficiency and the erasure time of crystals samples with He‐Ne laser. The results showed that the dynamic range (M/#), sensitivity (S) and diffraction efficiency (η) were dependent on the Mg doping concentration, and the Mg(4.58mol%):Ce:Cu:LiNbO₃ crystal was the most proper holographic recording media material among the six crystals studied in the paper. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)