LiInS_2多晶原料的合成与性能(英文)

本文研究了高纯LiInS2多晶原料的合成及性能。LiInS2晶体是一种极具吸引力的晶体,可以应用于红外区域的非线性光学频率变换。一般来说,含锂硫族化合物制备非常困难,因为锂极易被氧化,且腐蚀石英管。而且,硫族元素高的蒸气压会导致石英安瓿爆炸。本文采用两种方法合成了LiInS2多晶原料,对所获LiInS2多晶原料进行了X射线粉末衍射和差示扫描量热分析。     

大尺寸红外非线性光学晶体LiInS2的生长与性能研究

采用高压釜法合成了单相、致密的LiInS2多晶原料,采用改进的Bridgman晶体生长技术进行红外非线性光学晶体LiInS2的生长研究,获得了12 mm×40 mm的高质量完整单晶.对所获得的LiInS2晶体进行了组分分析、高分辨X射线衍射、激光损伤阈值等测试表征,测试结果表明:晶体存在硫过量和锂不足(NLi: N In＜1),各组分稍微偏离化学计量比;LiInS2晶体的 (040)面的半峰宽为78.84',表明晶体具有较好的完整性;晶体的激光损伤阈值为109 MW/cm2,有待于通过提高晶体质量和晶体表面的质量来进一步提高.     

加速坩埚旋转下降技术生长LiInS2晶体

本论文采用新的合成方法-高压釜法,利用高纯单质Li(3N)、 In(4N)、 S(sublimed)为原料,在1120℃下合成了单相、致密的LiInS2多晶料,并对其做了XRD表征.对传统的Bridgman-Stockbarger生长技术进行了改进,实现了加速坩埚旋转下降技术(ACRT),从而获得了较大尺寸的红外非线性光学晶体LiInS2,并对晶体的结构进行了表征.     

正钒酸钙晶体原料的合成与生长

本文通过固相合成方法直接合成正钒酸钙晶体原料.并用红外光谱、X射线多晶粉末衍射对所合成的原料进行表征.结果表明,固相合成法可获得纯度较高的正钒酸钙晶体原料.使用该方法合成的原料采用Czochralski高温提拉法生长出φ20mm×25mm的Ca3(VO4)2单晶.     

新型红外非线性光学晶体LiGaTe2的多晶合成与晶体生长

采用直接合成方法无法得到纯相的碲镓锂( LiGaTe2)多晶原料,因此提出了两步合成法进行LiGaTe2多晶原料合成,即先合成二元相Ga2Te3,再以Ga2Te3、Li、Te为原料按化学计量比配料在较低温度(850℃)下合成纯相的碲镓锂多晶料,并对具体的反应机理进行了讨论.对所得碲镓锂多晶料进行了XRD分析,结果显示合成的多晶为单相高纯LiGaTe2.差示扫描量热分析(DSC)表明,LiGaTe2的熔点为674.78℃.初步开展了LiGaTe2晶体的生长研究,对晶体生长结果进行了探讨.     

钽酸锂晶体高温富锂扩散工艺的研究

为了采用扩散法制备大厚度近化学计量比钽酸锂(nSLT)晶体,本文从富锂多晶料配比及合成工艺、极化工艺和扩散条件等方面对钽酸锂晶体高温富锂扩散工艺进行了研究,对处理后晶片组分、畴反转电压和光学均匀性进行了表征,研究了扩散条件对晶体组分的影响.结果表明,富锂多晶料锂钽为60/40时较佳,多次使用对所制备晶片组分、畴反转电压和光学质量无明显影响.在研究基础上,制备了系列nSLT晶片,晶片厚度最大为3.2 mm,其组分达到化学计量比且组分均匀,矫顽场约为152 V/mm,晶体光学质量满足实用需求.     

部分硫/硒(S/Se)红外非线性晶体原料的快速合成方法研究

含有硫/硒(S/Se)元素的部分化合物在现有中红外非线性晶体材料中占据相当重要的地位.高纯多晶原料是生长优质S/Se光学晶体的基础,但常规合成方法存在周期长、数量少等缺点.为此,针对部分S/Se化合物,我们对传统的合成方法进行优化、改进,实现GaSe,AgGaSe2,AgGaGeS4,AgGaGe5Se12等的快速合成,单次合成原料200～300 g,合成周期小于48 h,经过粉末衍射(XRD)测试表明合成的原料质量较好,能够生长出较大尺寸单晶.文中对快速合成方法的机理、存在的问题等也进行了相关讨论.     

坩埚旋转下降法生长硒镓银单晶体

本文报道了硒镓银多晶原料合成与单晶生长的新方法--熔体温度振荡法和坩埚旋转下降法.5～6N高纯Ag、Ga、Se单质按AgGaSe2化学配比富0.5;Se配料,1100℃下合成并在熔点附近进行温度振荡,获得了高纯单相致密的AgGaSe2多晶材料.用合成的多晶为原料,采用坩埚旋转下降法生长出φ22×80mm的AgGaSe2单晶锭.晶体外观完整,在10.6μm附近红外透过率达62.4;,吸收系数低于0.01cm-1,对10.6μm CO2激光实现倍频,能量转换效率达12;.     

ZnGeAs2多晶合成与表征

ZnGeAs2是黄铜矿结构的三元化合物半导体材料,在红外非线性光学方面有重要应用前景.本文探讨了ZnGeAs2多晶的形成途径和合成机理,报道了一种ZnGeAs2多晶合成方法.以高纯(6N)Zn、Ge、As单质为原料,按化学计量比,富Zn1‰和As2‰配料,采用双温区合成方法,辅以机械、温度振荡和梯度降温的合成工艺,合成出均匀致密的单相ZnGeAs2多晶.经XRD和EDS分析表明:合成产物为黄铜矿结构的单相ZnGeAs2多晶,晶胞常数为a=b=0.56745 nm,c=1.11580 nm,与标准PDF卡片(No.730397)一致;各组成元素的原子比Zn∶Ge∶AS=1.00∶0.98∶1.95,接近理想化学计量比.上述分析结果表明,合成产物可用于ZnGeAs2单晶生长,为进一步研究ZnGeAs2晶体的非线性光学性能和应用奠定了较好的基础.     

气体高压合成炉的设计及在小批量合成高纯ZnSe多晶中的应用

选择ZnSe多晶合成中具有最大气体总压力的Zn-Se-NH4Cl体系,通过在合成温度下减小石英坩埚内外压力差的途径,设计了专门的气体高压晶体合成炉,研究了所建立的高压炉的基本高温高压性能.并在此基础上成功小批量合成了的高纯的ZnSe多晶,结果表明自行设计建造的高压炉批量合成ZnSe高熔点化合物多晶材料是可行的,并且该设备也可以用于其它Ⅱ-Ⅵ族高熔点非氧化物高纯多晶的合成.     

Synthesis of dense polycrystalline GaN of high purity by the chemical vapor reaction process

A process for producing high-purity, dense polycrystalline gallium nitride is proposed. Dense polycrystalline gallium nitride was produced by the reaction of ammonia, gallium metal, and a halide source in a quartz boat containing metallic gallium. The process is called the chemical vapor reaction process. The hard crust-like pieces of polycrystalline GaN obtained are of high purity, can be used as source material for single-crystal growth by the ammonothermal technique, sublimation, sputtering, and pulse laser deposition.     

Structure and lithium ion diffusion in lithium silicate glasses and at their interfaces with lithium lanthanum titanate crystals

Solid state lithium ion electrolytes are important to the development of next generation safer and high power density lithium ion batteries. Lithium containing glasses such as lithium silicate glasses have been widely studied due to their high ionic conductivity. Recently, lithium silicate glasses were introduced in polycrystalline lithium lanthanum titanate (LLT) ceramics as intergranular thin films between the crystalline grains to achieve higher lithium ion conductivities in these solid state electrolytes. In this work, we present investigations of the structure and diffusion behavior of lithium silicate glasses and their interfaces with LLT crystals using molecular dynamics simulations. The short and medium range structures of the lithium silicate glasses were characterized and the ceramic/glass interface models were obtained using MD simulations. Lithium ion diffusion behaviors in the glass and across the glass/ceramic interfaces, as well as the effect of atomic structure on diffusion behaviors, were investigated. It was found that there existed a minor segregation of lithium ions at the glass/crystal interface. The interface lithium ion diffusion energy barrier was found to be dominated by the glass phase.     

Terahertz time-domain spectroscopy: A new tool for the study of glasses in the far infrared

Terahertz time-domain transmission spectroscopy was used to obtain the absorption coefficients and refractive indices of polycrystalline quartz, amorphous silica, Pyrex and BK7 glasses. The results were analyzed in terms of the power-law model of far-infrared absorption. Evidence of the Boson peak was seen in the absorption spectra. Relationships were observed between THz absorption and refractive indices on the one hand, and glass structure and properties on the other. THz TDS is demonstrated to be a useful tool in the study of far-infrared transmission properties of glasses, producing low-noise, high resolution measurements of absorption coefficients and refractive indices.     

Mechanism and control of crack generation in glass substrates during crystallization of a-Si Films by flash lamp annealing

We investigate the impact of the materials of glass substrates on crack formation during flash lamp annealing (FLA) of 4.5 μm-thick precursor amorphous silicon (a-Si) films for the formation of polycrystalline Si (poly-Si) films. The use of soda lime glass substrates, with the largest thermal expansion coefficient (α) and the lowest glass transition temperature (T_g) in glass materials attempted in this study, results in the serious formation of cracks on and inside the glass substrates. Cracks are also seen on the surface of quartz glass substrates, which have much smaller α and higher T_g, after FLA. Furthermore, flash-lamp-crystallized (FLC) poly-Si films have linearly-connected low-crystallinity regions only when quartz glass substrates are used. These facts indicate that the expansion of Si films induces cracks in quartz glass substrates, while the expansion of the upper part of glass is the cause of the crack formation in glass substrates with large α. The generation of cracks is most significantly suppressed when we use alkali-free glass substrates, with a moderate α and a relatively high T_g, which will contribute to the realization of high-quality poly-Si films and high-performance solar cells.     

Optical and electrical properties of lithium doped nickel oxide films deposited by spray pyrolysis onto alumina substrates

Non-doped and lithium doped nickel oxide crystalline films have been prepared onto quartz and crystalline alumina substrates at high substrate temperature (600 °C) by the pneumatic spray pyrolysis process using nickel and lithium acetates as source materials. The structure of all the deposited films was the crystalline cubic phase related to NiO, although this crystalline structure was a little bit stressed for the films with higher lithium concentration. The grain size had values between 60 and 70 nm, almost independently of doping concentration. The non-doped and lithium doped films have an energy band gap of the order of 3.6 eV. Hot point probe results show that all deposited films have a p-type semiconductor behavior. From current–voltage measurements it was observed that the electrical resistivity decreases as the lithium concentration increases, indicating that the doping action of lithium is carried out. The electrical resistivity changed from 10⁶ Ω cm for the non-doped films up to 10² Ω cm for the films prepared with the highest doping concentration.     

石英晶体板非线性高频振动的拓展伽辽金法分析

针对考虑几何和材料非线性的石英晶体板厚度剪切振动和弯曲振动的方程组,利用扩展伽辽金法对该方程组进行转化和求解,分别获得了强烈耦合的厚度剪切振动模态和弯曲振动模态的频率响应关系,绘制了不同振幅比和不同驱动电压影响下的频率响应曲线图。数值计算结果表明可以选取石英晶片的最佳长厚比尺寸来避免两种模态的强烈耦合。驱动电压的变化将引起石英晶体谐振器厚度剪切振动频率的明显改变,必须将振动频率的漂移值控制在常用压电声波器件的允许值之内。扩展伽辽金法对石英晶体板非线性振动方程组的求解为非线性有限元分析和偏场效应分析奠定了基础。     

溶胶凝胶法制备WS2-SiO2可饱和吸收体的探究

WS2二维材料独特的光吸收体特性使其成为可饱和吸收体的优选材料。溶胶凝胶法具有操作方便、设备简单、成本低廉等优点。利用溶胶凝胶法在石英基片上制备SiO2材料为主体的WS2-SiO2薄膜是一种实现可饱和吸收体的新思路。本文通过改变实验过程中原料配比、热处理条件、旋涂速度等实验参数确定出溶胶凝胶法制备SiO2薄膜的最佳条件,在此基础上再加入WS2溶液制备出WS2-SiO2薄膜可饱和吸收体,通过共聚焦显微镜、透射电子显微镜、拉曼光谱、X射线衍射等方法对制备的样品进行了测试分析,结果表明采用本文提出的制作方法可以得到外观良好的WS2-SiO2薄膜可饱和吸收体、WS2在 SiO2薄膜中呈多层的多晶颗粒,晶面指数主要为(002)、(004)、(101)、(103)、(006)、(105)。     

红外LED用GaAs单晶的垂直梯度凝固制备研究

GaAs单晶是当前光电子器件的主要衬底材料之一，在红外LED中有着重要应用。但杂质浓度高、迁移率低等缺点会严重影响红外LED器件性能。为生产出低杂质浓度、高迁移率、载流子分布均匀、高利用率的红外LED用掺硅垂直梯度凝固(VGF)法GaAs单晶，本文研究了热场分布、合成舟和炉膛材质、工艺参数对单晶的成晶质量、杂质浓度、迁移率、载流子分布的影响。利用CGSim软件对单晶生长热场系统进行数值模拟研究，温区一至温区六长度比例为8∶12∶9∶5∶5∶7时，恒温区达到最长，位错密度达到1 000 cm^-2以下，成晶率达到85%。采用打毛石英合成舟进行GaAs合成，用莫来石炉膛替代石英炉膛，可以获得迁移率整体高于3 000 cm²/(V·s)的GaAs单晶，满足红外LED使用要求。对单晶生长工艺参数展开研究，采用提高头部生长速度、降低尾部生长速度的方式提高单晶轴向载流子浓度均匀性，头尾部载流子浓度差降低33%,尾部迁移率从2 900 cm²/(V·s)提高到3 560 cm²/(V·s)。单晶有效利用长度提高33...