熔盐法和水热法KTP晶体的晶胞参数及拉曼光谱特征

利用X射线衍射和显微激光拉曼光谱研究熔盐法自发结晶的KTP晶体、顶部籽晶熔盐法KTP晶体和水热法KTP晶体的晶胞参数和拉曼光谱特征,分析和比较不同方法生长的KTP晶体的晶体结构与化学键特征峰.研究表明:KTP晶体的晶胞参数与晶体生长方法有关,熔盐法自发结晶的KTP晶体生长过程中降温速率较快,晶胞体积相对较小;熔盐法和水热法KTP晶体中部分拉曼特征峰的位置因生长方法不同呈现一定的差异,水热法KTP晶体在782 cm-1、744 cm-1和515 cm-1处出现的特征峰可视为水热法KTP晶体的标志峰,借此可将其与熔盐法晶体相区分.     

水热法掺铌KTiOPO4晶体的形貌和缺陷研究

采用水热法在双温区加热炉中以Z-切向晶片为籽晶生长了掺铌KTiOPO4单晶(Nb∶KTP),得到尺寸为24.7mm×14.7 mm×42.6 mm的透明晶体。研究了Nb∶KTP水热条件下的生长习性和宏观、微观缺陷,通过其与纯KTP的透过谱的对比,对晶体质量进行了初步评估,与高质量的水热高抗灰迹KTP晶体有相当的质量。     

Nb∶KTiOPO4晶体的生长和倍频性能

通过研究晶体生长工艺参数对Nb∶KTiOPO4(Nb∶KTP)晶体生长的影响,用熔盐顶部籽晶法获得尺寸为55mm×25mm×5mm的Nb∶KTP透明单晶.研究中发现熔体的温度梯度、籽晶和降温速率将严重影响Nb∶KTP晶体的生长.Nb离子的引入不利于Nb∶KTP晶体的生长,尤其是造成晶体易开裂,且沿a轴方向生长速度非常缓慢.同时,Nb的引入大大改变Nb∶KTP晶体的倍频性能.掺杂Nb浓度的摩尔分数为13;时,Nb∶KTP晶体的倍频的Ⅱ型相位匹配的截止波长缩短至937nm,且有效产生469nm倍频蓝光;掺杂Nb浓度的摩尔分数为3;时,Nb∶KTP晶体对Nd∶YAG的1.0642μm激光倍频的最佳相位匹配角为θ=88.32°,()=0°,非常接近90°非临界相位匹配方向.     

Nb：KTiOPO4晶体的生长和倍频性能

通过研究晶体生长工艺参数对Nb∶KTiOPO4(Nb∶KTP)晶体生长的影响,用熔盐顶部籽晶法获得尺寸为55mm×25mm×5mm的Nb∶KTP透明单晶.研究中发现熔体的温度梯度、籽晶和降温速率将严重影响Nb∶KTP晶体的生长.Nb离子的引入不利于Nb∶KTP晶体的生长,尤其是造成晶体易开裂,且沿a轴方向生长速度非常缓慢.同时,Nb的引入大大改变Nb∶KTP晶体的倍频性能.掺杂Nb浓度的摩尔分数为13%时,Nb∶KTP晶体的倍频的Ⅱ型相位匹配的截止波长缩短至937nm,且有效产生469nm倍频蓝光;掺杂Nb浓度的摩尔分数为3%时,Nb∶KTP晶体对Nd∶YAG的1.0642μm激光倍频的最佳相位匹配角为θ=88.32°,()=0°,非常接近90°非临界相位匹配方向.     

激光晶体Nd:KGW晶体的表面缺陷观察

本文采用助熔剂籽晶提拉法生长出了Nd:KGW激光晶体.利用光学显微镜对晶体表面进行观察、并拍摄到晶体裂缝、生长丘、生长条纹和包裹物等缺陷的照片.分析其原因,是由于晶体生长工艺的不稳定,尤其是晶体生长过程中的温度梯度不够合适、提拉速度过快、降温速率偏快等所致.并由于生长体系粘度较大,容易形成包裹,晶体包裹物经XRD分析认为其中主要是熔体.     

CZ法生长参数对TeO2晶体质量的影响

本文主要讨论CZ法生长TeO2晶体中温度梯度、拉速、转速等工艺参数对晶体质量的影响,分析了晶体开裂、包裹物等宏观缺陷以及位错等微观缺陷的形成机理.从晶体形态、包裹体和位错密度变化等方面探讨了晶体生长参数与晶体缺陷之间的内在关系.     

点状籽晶法生长DKDP晶体的研究

本文研究了影响溶液稳定性的因素,主要包括溶液的纯度、饱和点和过饱和度等,并对DKDP的点状籽晶法生长进行了初步研究.同时比较了不同生长速度生长的晶体质量.结果表明:经超细过滤的高纯度溶液稳定性有很大提高,而此时生长速度对晶体质量的影响不大.最后,获得了X、Y向生长速度达3.8mm/d的点状籽晶,生长出尺寸为44mm×44mm×48mm的高质量DKDP晶体,并对晶体生长的表面进行了微观观察,分析了DKDP晶体生长的微观机制.     

浸没籽晶法生长La2CaB10O19单晶的研究

采用浸没籽晶法以CaO-Li2O-B2O3为助熔剂生长出La2CaB10O19单晶.籽晶的方向对晶体质量有较大的影响.晶体结构导致生长出的晶体均呈现板状外形,并且容易沿(001)面解理;捆绑晶体的铂丝嵌入晶体加剧了晶体的解理.然而解理和铂丝嵌入对不同方向籽晶生长出晶体的质量影响各不相同,对于晶体生长过程溶质输运的影响也不相同,实验发现,[101]方向为本实验条件下最佳的晶体生长方向.     

ADP晶体的全方位生长装置

本论文研究的全方位生长装置能解决常规的ADP晶体的单向生长问题.在这套装置中,籽晶完全位于溶液中央,籽晶可以首先恢复其理想的结晶学外形.在晶体生长过程中,晶体在各个方向的生长均为自由生长,且育晶器中央的溶液稳定性也明显高于育晶器顶部和底部.这些因素都有利于ADP晶体的优质快速生长.实验所得晶体的质量通过透过率、晶体内缺陷位错密度、高分辨率X射线衍射表征,并将所得结果与常规方法进行了比较.     

LaFeO_3晶体缺陷研究

以La2O3和Fe2O3粉体为原料,在1400℃烧结24 h制备出了LaFeO3多晶料棒,采用浮区法生长出LaFeO3晶体。从晶体开裂、晶体中孔洞、晶体生长层、晶体内包裹物和晶体位错几方面,系统地研究了LaFeO3晶体的缺陷形成。通过分析晶体缺陷产生的原因,提出了有效减少缺陷和控制缺陷的方法。同时,优化了晶体生长工艺,提高了LaFeO3晶体质量。     

KTP晶体的水热法生长及其光学性能的测量

使用水热法成功生长出大尺寸、高质量的KTP晶体,对该晶体的光学性能进行测量分析.由LambDA900分光光度计测量得到的水热法生长KTP晶体的透过率曲线表明晶体具有良好的光透过性能,其透过短波下限与熔盐法生长的KTP晶体基本相当.利用自准直法精确测量水热法生长KTP晶体的折射率,拟合得到30℃下折射率的Sellmeier方程的系数,并计算532nm与1319nm波长对应的主轴折射率,计算值与实验值相吻合.     

KTP晶体的电光研究进展

本文简述了KTP晶体的电光性能并与KD*P、LN晶体进行了比较。概括了KTP晶体电光器件研究的主要进展。对水热法生长的KTP晶体和熔剂法生长的KTP晶体在电光应用中的优缺点进行了分析。最后介绍了熔剂法生长的低电导率KTP晶体在电光领域的应用研究。     

KTP crystal growth from the starting materials reacted in solution

Using the solution‐reacted materials, potassium titanyl phosphate (KTiOPO₄, KTP) crystal was grown by the top‐seeded solution growth (TSSG) method. The solution‐reacted precursor was characterized by scanning electron microscope, and the solubility of KTP in K₈P₆O₁₉ was measured. The crystals were investigated by synchrotron radiation X‐ray topography, scattering centers measurement, weak absorption test and damage threshold test. The results showed that dispersion was better and solubility was higher than those by solid‐reacted method. Compared with the conventional crystal, KTP crystal grown from the solution‐reacted precursor had fewer defects, fewer scattering centers, lower weak absorption and higher damage threshold.     

单掺Rb+和Cs+的KTP晶体生长及其电导率

采用高温溶液降温法在掺质浓度均为5mol;的KTP-K4溶液中分别生长了单掺Rb+和Cs+的KTP晶体,发现掺质改变了晶体生长习性,在相应生长体系中掺质Rb+和Cs+的分配系数分别为O.646和0.08,掺质KTP晶体的晶胞参数a0和b0比纯KTP晶体者略有增长.通过掺Rb+或Cs+,KTP晶体的c向电导率明显降低,但晶体在350～1100nm范围内的光透过性质未受影响.     

Reducing Inversion Twinning in Single Crystal Growth of GaPO4

Gallium orthophosphate (GaPO₄) single crystals were grown by the reverse temperature gradient method from phosphoric acid solutions under hydrothermal conditions. Twins after (110) were studied by etching faces having been cut perpendicular to one of the twofold axes. Based on the determination of the twin boundary position as well as on the knowledge of the growth rates of different crystallographic forms, a few faces have been chosen to be quite promising for growing high‐quality GaPO₄ single crystals if they are offered at the referring seed crystal. From the characterization of the grown crystals conditions have been found, which may lead to the reduction of the inversion twin number during the growth process.     

Growth of KTiOPO<Subscript>4</Subscript> crystals doped with zinc and studies of their physical properties and specific structural features

A series of potassium titanyl phosphate single crystals doped with zinc (KTP: Zn) is grown by spontaneous flux crystallization. Their properties and the way the additive is implanted in the crystal lattice are studied. The inclusion of zinc atoms in the KTP structure is evidenced by the data of chemical analysis and the results of studies of electrophysical properties (the growth of conductivity and increase of relaxation anomalies). Precision X-ray diffraction studies of KTP: Zn single crystals reveal changes in the channel of the structure which correlate with the physical properties of this crystal series. No substitution of zinc atoms for titanium, phosphorus, or potassium atoms is found in the structure. Zinc atoms can be located at structural defects, domain walls, and the crystal surface.     

A survey of research on KTP and its analogue crystals

This paper reviews the growth and properties of KTiOPOP₄ (KTP) and its analogue crystals including its isomorphous crystals and doped crystals. Based on the calculation of the refractive indices and phase matching of KTP crystals, it is shown that non-critical phase matching can be achieved theoretically. In a 4%Nb-doped KTP crystal, non-critical phase matching was obtained with a pulsed Nd:YAG laser in an efficiency of ca. 4%. Most of the isomorphous and doped KTP crystals possess similar physical, optical and nonlinear optical properties as those of KTP.RbTiOPO₄, KTiOASO₄ and RbTiOASO₄ crystals have better electrooptical figure of merit and RbTiOPO₄ crystals have a fast ion conductor character. Some doped KTP crystals have shown high second harmonic generation efficiencies and damage thresholds. But the homogeneity of KTP analogue crystals is poorer than that of KTP. On the base of damage threshold tests using a CW Argon laser, it is concluded that the best second harmonic generation crystal among all the KTP analogue crystals is still KTP itself. Special care must be taken to eliminate impurity centers to avoid the formation of gray track and photorefractive centers.     

Growth,Characterization and Non-Critical Phase-Matching of Niobium-Doped KTP Crystals

A series of niobium doped KTP (Nb: KTP) crystals has been grown. XRD and DTA experiments show that the Nb: KTP crystal structures do not differ from that of KTP (within experimental error) and that the melting points of the crystals increase with increasing Nb content. Synchrotron radiation topography revealed that the main defects of the crystals were growth sector boundaries, growth striations, inclusions and dislocations. Second harmonic generation experiments were performed using a 12.2% Nb:KTP and the d₁₅ and d₂₄ values of csystal were determined to be (3.7 ± 0.4) and (8.3 ± 0.8) × 10⁻⁹ esu, respectively. The relationship between phase-matching angle and Nb content for a 1.064 μm laser was determined and in the case of a 4.0% Nb:KTP crystal, non-critical phase matching was realized.     

Growth imperfections in oriented grown KDP crystals by X‐ray topographic analysis

Potassium dihydrogen phosphate (KDP) crystals were restrained to grow in two dimensions only, using a specially designed platform. This enables us to grow the blanks of frequency conversion elements that satisfy type‐II phase matching direction out of a type‐II phase‐matched seed crystal. Synchrotron radiation topography was used to study the growth mechanism of these profiling grown KDP crystals. It is found that both dislocation growth mechanism and layer growth mechanism were involved in the growing process. Inclusions, growth striations and dislocations were the main defects that influenced the crystalline quality of these crystals. High‐resolution X‐ray diffraction was employed to study the lattice integrality of the crystal.