大尺寸弛豫铁电单晶PIMNT的坩埚下降法生长

PIMNT单晶是近年来最新发现的弛豫铁电晶体材料,该三元固溶体单晶具有比较理想的压电、铁电和介电性能,本文报道了大尺寸PIMNT单晶的熔体坩埚下降法生长的实验研究结果。采用固相合成钙钛矿相多晶料,采用垂直坩埚下降法成功生长出最大直径为3英寸的PIMNT单晶;从所生长单晶原胚的三方相区段切割加工出(001)取向晶片,就(001)晶片的介电、压电及铁电性能进行了测试表征,表明其材料性能能够满足相关超声换能器件制作的实用需求。本论文还着重讨论了PIMNT单晶生长所涉及的系列关键技术问题,如富铅熔体对铂金坩埚的侵蚀、晶体原胚的单晶性表征、晶体生长过程的组分偏析与单晶原胚的性能分布等。     

宽禁带半导体碳化硅单晶生长和物性研究进展

本文介绍了最近几年在SiC单晶生长和晶片加工技术产业化进程中的系列进展。研究出SiC单晶生长的扩径技术,4英寸SiC晶体单晶直径达105 mm。晶体质量逐步提高,至2011年,大部分晶片微管密度小于1个/cm2,反映晶体结晶质量的X射线摇摆曲线半高宽小于20″;生长的导电型SiC晶体电阻率小于0.02Ω.cm,半绝缘型SiC晶体电阻率大于108Ω.cm,电阻率分布均匀性良好。研究出即开即用SiC晶片批量加工技术,晶片表面粗糙度低于0.2 nm,翘曲度和总厚度变化满足工业化批量生产要求。与此同时,在基础物性研究方面也取得了系列研究成果。首次在实验上给出了直接证据证明SiC晶体中的双空位能够诱导出磁性,并从理论上予以证明。利用多种方法在SiC衬底上成功制备出大面积、高质量、性能优异的石墨烯。     

PIMNT单晶生长用多晶料的固相合成

以In2O3、Nb2O5、4MgCO3·Mg(OH)2·4H2O、TiO2、PbO为初始试剂,先合成出前体化合物MgNb2O6和InNbO4;按照0.25Pb( In1/2 Nb1/2) O3-0.44Pb( Mg1/2 Nbv3)O3-0.31PbTiO3的组分比例,添加1.5 mol％过量PbO,通过高温固相反应合成出PIMNT多晶料.X射线粉末衍射、差热/热重分析表明,PIMNT多晶系钙钛矿结构的固溶体化合物.采用本实验合成PIMNT多晶料锭,通过坩埚下降法成功生长出25mm直径的PIMNT单晶,证实采用预先合成多晶料有助于钙钛矿相PIMNT单晶的稳定生长.     

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.     

化学气相传输法生长ZnO单晶及性质研究

利用化学气相传输法生长了ZnO单晶.在无籽晶自发成核的条件下,使用碳辅助增强质量传输方法,得到了晶粒尺寸达4mm×10mm的ZnO晶体.利用长有GaN层的蓝宝石晶片作为衬底,得到了直径为30mm、厚2mm左右的ZnO单晶体.比较了不同温度条件下晶体生长的结果并进行热力学过程和现象了分析.用光荧光谱和X射线双晶衍射研究了ZnO晶体的性质.     

纯镁单晶制备研究

利用自制的硅碳棒加热单晶生长炉,采用改进的坩埚下降法,在最高温度900℃,坩埚相对下降速度约为1.7cm/h条件下,生长出直径约为φ50mm的纯镁单晶.通过X射线衍射、金相观察和测量电导率等手段研究分析了所生长镁单晶的晶体质量.     

连续铸造铜单晶的晶体取向与竞争生长

本文采用自制单晶连铸设备和X射线衍射方法研究连铸铜单晶的晶体取向与竞争生长.结果表明,在晶体演化过程中逐渐淘汰的晶面为(311)、(200)和(111),最后单晶生长的晶面为(200),连铸铜单晶的晶体生长方向为[100],晶体取向[100]与晶轴的偏离度小于10°.单晶生长时固液界面向熔体呈凸出形状,这有利于晶体生长过程中的竞争和淘汰.还发现了连铸铜单晶取向在一定范围内,并不是唯一取向的单晶.     

垂直布里奇曼法生长铜单晶体的研究

Cu单晶在中子和X射线单色器及激光核聚变靶材等领域有重要应用前景.本文采用自制的硅钼棒单晶生长炉和特制的镀碳石英生长坩埚,采用垂直布里奇曼法在30 ℃/cm的温度梯度下,以10 mm/d的下降速度生长出较高质量的铜单晶体.生长的晶体经多次研磨抛光腐蚀处理后进行X射线衍射分析和金相分析,显示出(200)晶面尖锐的X射线衍射峰和规则的方形蚀坑,表明生长的晶体结构完整.     

蓝宝石晶体的生长方向研究

本实验采用提拉法,在中频感应加热单晶炉内,进行了不同生长方向蓝宝石晶体的生长工作,分别取[11-20]和[0001]生长的晶体c面(0001)的晶片.通过应力仪、显微观测和X射线衍射等方式对晶片的位错密度等微观缺陷以及晶体结构进行了检测.实验表明:不同的生长方向生长得到的蓝宝石晶体的质量存在一定的差别,一般情况下,[11-20]方向生长的蓝宝石晶体质量优于[0001]方向生长的晶体.     

闪烁单晶钨酸锌的坩埚下降法生长

通过高温固相反应或湿化学法合成ZnWO4多晶料,采用垂直坩埚下降法生长出φ25 mm× 60 mm的透明完整钨酸锌单晶.应用X射线粉末衍射分析证实了所制备钨酸锌多晶与单晶的结晶物相,测试了钨酸锌单晶的紫外可见透射光谱、光致发射光谱和X射线激发发射光谱,讨论了此闪烁单晶的氧气氛退火效应.结果表明,该单晶的透射光谱在400～800 nm波长区域呈现典型光学透过性,其吸收截止边位于380 nm左右,在紫外激发光或X射线激发作用下,此单晶具有峰值波长位于470 nm的荧光发射;此单晶经980℃温度下的氧气氛退火处理,其晶体着色有所变浅而光学透过性得以明显改善.     

改进的升华法制备氮化铝单晶体

采用改进的升华法在氮气环境下制备氮化铝单晶体.通过优化实验条件制备出了六角形的高质量的氮化铝单晶体.实验发现,在坩埚的不同区域得到的氮化铝晶体的大小和形态有所不同.讨论了温度梯度对氮化铝晶体尺寸大小和形态的影响.     

异质结构光子晶体的制备与带隙特性研究

本文采用多次垂直沉积法制备出了可见光范围的多重异质结构光子晶体,并对其形貌特征和带隙特性进行了分析.扫描电镜图像表明:所制备的异质结构光子晶体排列规整、不同结构间界面明显.光学吸收光谱分析结果表明:异质结构光子晶体与各单一结构光子晶体带隙相比,带隙明显增大,为各单一结构光子晶体带隙的叠加,且与不同结构的叠加顺序无关.     

An effective growth method to improve the homogeneity of relaxor ferroelectric single crystal Pb(In1/2Nb1/2)O3‐ Pb(Mg1/3Nb2/3)O3‐PbTiO3

Compositional segregation usually has negative effects on the growth of solid solution ferroelectric single crystals of Pb(In_1/2Nb_1/2)O₃‐Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ (abbr. PIN‐PMN‐PT or PIMNT). A modified Bridgman method was adopted in this work to control the segregation and improve the compositional homogeneity significantly. The characteristic of this work is to use multiround growths and gradient composition raw materials in order to keep the PbTiO₃ concentration constant during the crystal growth. As an example, the two‐round growth of ternary PIN‐PMN‐PT single crystal is conducted in the same Pt crucible with gradient raw materials, where the first‐round boule was used as the seed crystal for the second‐round growth. Our results show that the as‐grown (Ф80 mm × 270 mm) PIN‐PMN‐PT crystals exhibit higher phase transition temperatures (T_c∼180 °C, T_r/t∼110 °C) and larger coercive field (E_c∼5–5.5 kV/cm), which are much better than the performances of Pb(Mg_1/3Nb_2/3)O₃‐PbTiO₃ crystals, and similar dielectric and piezoelectric performances (ε∼5000, tanδ∼1.25%, d₃₃∼1500 pC/N, k_t∼60%). And about 85 percent of the crystal boule grown by the two‐round growth technique could maintain its compositions around the morphotropic phase boundary.     

降温速率对DAST单晶生长的影响

使用籽晶法通过调整降温速率生长出高质量4-N,N-二甲胺基-4′-N′-甲基-氮杂芪对甲苯磺酸盐(DAST)晶体,研究了降温速率对DAST晶体结晶质量、光学特性及太赫兹输出特性的影响.通过核磁共振分析表征了合成原料的结构和纯度.使用X射线衍射仪对生长晶体的(001)面进行X射线摇摆曲线测试,测试结果表明在降温速率为0....     

Understanding the growth mechanism of CuI crystals during gel growth experiments

Cuprous iodide crystals have been grown with decomplexation method in silica gel. Various crystal morphologies, such as polycrystalline aggregate, skeletal, dendrite, hopper crystals and regular tetrahedron crystals, were observed in different growth regions with an optical microscope. Their surfaces were photographed using a binocular metallographic microscope and the results were explained with the crystal growth mechanism which was determined by supersaturation. These observations support the general hypothesis that the concentration of reactant affects the relative growth rate by controlling the nucleation and diffusion. The mutual influence of the crystals grown in different regions was also discussed. Additionally, the suitable condition for getting regular tetrahedron crystals or large hopper crystals was obtained by changing the concentration of CuI·HI complex in the later period of crystal growth. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

对三联苯有机晶体的生长及性能

对三联苯是一种常见的有机闪烁剂,通常用作闪烁计数器的发光材料。对三联苯闪烁晶体具有对中子探测效率高以及不易潮解等特性,这使其在实际应用中具有广阔的前景。本文采用坩埚下降法,使用单层安瓿成功生长出φ12 mm×30 mm对三联苯晶体。在生长开始前通过差热分析,确定晶体的生长温度。生长完成后测试了晶体粉末的X射线衍射谱、摇摆曲线、红外光谱、荧光光谱和拉曼光谱。X射线衍射结果表明,生长的晶体为纯对三联苯相。从摇摆曲线结果可以看出,生长晶体质量良好。红外和拉曼分析结果显示,峰位并没有出现明显的偏移,表明晶体中杂质含量较少并未引起晶体分子化学结构的变化。荧光光谱没有杂质峰的出现也说明对三联苯晶体存在较少杂质或晶格缺陷。     

Growth of YCOB single crystals by flux technique and their characterization

Nonlinear optical single crystals of YCOB with good optical quality were grown by the flux technique for the first time. Polycrystalline YCOB samples were synthesized by solid state reaction method. The thermal analysis of the sample was performed with lithium carbonate flux in different weight proportions and the growth temperature was optimised. Single crystals of YCOB with dimensions 3 × 3 × 5 mm³ were obtained by the method of ‘slow‐cooling’. The grown crystals were characterized by XRD, UV‐VIS‐NIR, EDAX, FTIR and etching studies. The powder XRD pattern revealed the formation of YCOB compound. The lattice parameters were identified through single crystal XRD studies. The UV‐VIS‐NIR results showed that the crystal has a sharp cutoff at 220 nm and is nearly 55% transparent over a wide wavelength range enabling applications in the UV region. The EDAX measurement revealed the ‘flux‐free’ crystal formation. The presence of the functional groups belonging to the YCOB crystals was identified by the FTIR results. ‘Hillock‐like’ patterns are observed in the etching studies. The primary emphasis in this study is laid to describe ‘flux technique’ as an alternative method to grow YCOB crystals. The results are presented and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Yb3+:YVO4晶体的生长及光谱性能研究

采用提拉法生长出光学质量优良的Yb3+:YVO4晶体,研究生长过程中工艺参数的控制.测得掺杂浓度为18.1;Yb3+:YVO4晶体中Yb3+离子的有效分凝系数Keff为0.96.测定了不同Yb3+离子掺杂浓度晶体的吸收光谱和荧光光谱,并分别计算了不同掺杂浓度下Yb3+:YVO4晶体的光谱参数.本文总结和解释了掺杂浓度影响其性能的规律,讨论了Yb3+:YVO4晶体作为激光晶体的优点.     

Bridgman法生长TeO2晶体的缺陷分析

采用Bridgman法生长了二氧化碲(TeO2)晶体,运用光学显微镜、电子衍射光谱、化学腐蚀等方法分析了该方法生长TeO2晶体内部的缺陷.初步讨论了散射点、微裂纹、气泡和黑点、条纹以及腐蚀坑等微缺陷的形成机理.结果表明:晶体内部的散射点来自于原料中杂质,条纹主要是由于晶体内应力引起,晶体内的气泡和黑点和晶体生长的温度密切相关,并就如何减少这些微缺陷进行了初步探讨.     

Growth and Structure of Doped KLN Crystal

KLN, Fe:KLN, Mn:KLN and Cu:KLN crystals were grown by Czochraski method. The structure of crystal was measured by X‐ray diffraction technique. The results indicated that the doped crystals kept the same structural characteristics as the pure KLN crystal, but the lattice constants of Fe:KLN and Mn:KLN crystals became smaller than that of pure KLN crystal, and that values of Cu:KLN crystal became larger than that of pure KLN crystal. This indicated that Fe and Mn cations replaced Nb cation, and Cu cation replace K cation after they entered into the lattice of KLN crystal. The result of ultraviolet‐visible absorption spectra was identified with that of X‐ray diffraction analysis.