8～12μm长波红外材料ZnS多晶的制备

真空热压烧结法是最经济、高效地制备ZnS多晶的方法之一.ZnS多晶的红外透过率是衡量材料品质的重要参数.本文运用TEM、XRD和化学分析方法,研究了原料粉末特性和热压工艺参数对热压ZnS多晶红外透过率的影响,并确定了合理的热压工艺参数.运用该方法制备的ZnS多晶6mm厚的试样,8～12μm波段平均红外透过率为66.7;.     

N型赝三元热压热电材料的微观结构和电学性能

通过熔炼/研磨技术和热压方法制备N型赝三元热压块体材料.通过SEM和XRD研究了由不同粒度粉末制备的热压块体材料的微观结构,在室温条件下测量了热压材料样品的电学性能.结果表明热压块体材料在微观结构和电学性能上存在各向异性,从而预示能够在增强材料机械强度的同时提高其热电性能.     

用化学气相沉积法制备红外体块晶体ZnS

本文报道了采用化学气相沉积法制备红外ZnS体块晶体的工艺及其性能.并用傅立叶红外光谱仪测试了材料的红外性能,研究了晶体缺陷对材料红外透过率的影响.结果表明:通过优化生长工艺,使反应室的压力在500～1000Pa之间变化,沉积温度控制在550～650℃之间,可以制备出厚度均匀,红外透过率(3-5μm和8～12μm)在70;以上,尺寸达250mm×250mm×15mm高质量的ZnS体块晶体.     

AgGa1-xInxSe2晶体退火改性研究

采用改进布里奇曼法生长出外观完整的AgGa1-xInxSe2(x=0.2)单晶锭,晶体的红外透过率低,不能直接用于红外非线性光学器件制备.采用TA公司生产的SDTQ-600热分析仪进行DSC-TGA测试,发现其熔点为826.69℃,结晶点为750.86℃,总失重约为3.9217;.采用同成份粉末源包裹晶体,在抽空封结后进行退火处理.退火处理后晶体的红外透过率有明显改善.在4000cm-1～7000cm-1范围内红外透过率由原先低于25;改进到高于40;;在750cm-1～4000cm-1范围的红外透过率由原先低于45;改善到超过50;,在2000cm-1 ～750cm-1区域甚至高达60;.结果表明:采用同成分粉末源包裹,在抽空封结后退火处理能有效提高AgGa1-xInxSe2晶体的红外透过率,改善晶体的光学均匀性,退火后的晶体适合红外非线性光学器件制备.     

CuO/氧化石墨烯复合材料合成、表征及光催化研究

以醋酸铜Cu(Ac)2和氧化石墨烯(GO)为原料,去离子水作溶剂,十六烷基三甲基溴化铵(CTMAB)为表面活性剂,通过水热反应制备了CuO/GO纳米复合材料.傅里叶红外光谱(FT-IR)、X-射线粉末衍射(XRD)以及光电子能谱仪(XPS)和透射电镜(TEM)对合成的复合材料结构表征以及形貌分析,结果发现CuO纳米粒子均匀地分散在GO上.并将制备的复合材料对罗丹明B溶液进行光催化降解研究,结果发现在光反应80 min后,罗丹明B的浓度降低率达到85;,因此CuO/GO复合材料对罗丹明B表现出了良好的光催化性能.     

磷锗锌晶体的热处理研究

采用改进垂直布里奇曼法生长出的磷锗锌(ZnGeP2,ZGP)晶体中存在各种缺陷,导致其红外透过率较低,刚生长的晶体不能直接用于制备红外非线性光学器件.分别采用真空、同成分粉末包裹和真空-同成分粉末包裹的复合退火工艺对生长的ZGP晶体进行了退火热处理研究.应用傅立叶红外光谱仪(FTIR)、高阻仪(HRM)、X射线能谱仪(EDS)等对退火前后的晶体性能和成分进行了测试分析.结果表明,三种方法退火后晶体的红外透过率和电阻率都得到改善,其中复合退火工艺的改善效果最为显著,晶体红外透过率由41;提高到60;,电阻率由2.5×108 Ω·cm提高到7.2 ×108 Ω·cm,晶体成分接近ZGP理想化学配比,退火后晶体的光学和电学性能得到显著改善,可用于ZGP-OPO器件制作.     

用化学气相沉积(CVD)法制备硫化锌(ZnS)体块材料中晶体缺陷和生长工艺的研究

本文报道了用化学气相沉积(CVD)法制备高质量红外光学体块材料硫化锌(ZnS)的制备工艺,研究了晶体缺陷对其光学性能的影响.XRD,XEM及IR表明,采用优化的沉积工艺和热等静压后处理,减少晶体中杂质、微孔、六方结构ZnS及Zn-H键的形成,使生长的CVD ZnS具有高的红外透过率,提高了材料的光学品质.     

热压工艺参数对N型(Bi2Te3)0.90(Sb2Te3)0.05(Sb2Se3)0.05热电材料电学性能的影响

通过熔炼/研磨/热压方法制备了N型(Bi2Te3)0.90(Sb2Te3)0.05(Sb2Se3)0.05热压合金样品,测量了由不同工艺参数(热压温度、热压压力)制备的样品的Seebeck系数和电导率.分析了热压参数对热电性能产生的影响.特别是发现了在实验压力范围内增加热压压力会使热压样品的Seebeck系数和电导率都有所提高,这与Seebeck系数和电导率通常变化趋势相反的规律有显著差异,其结果对热压样品的电学性能提高有积极的影响.     

红外非线性光学晶体CdSe生长与性能表征

采用垂直无籽晶气相法(VUVG)生长出尺寸达26 mm×45 mm的CdSe单晶体,对CdSe晶体的稳态气相生长速率进行了深入讨论.采用气相升华法提纯后的CdSe多晶原料的X射线粉末衍射谱与PDF卡片值(65-3436)吻合,生长出的单晶体{100}和(110)面XRD衍射峰尖锐,无杂峰,且{100}面出现3级衍射峰.晶锭密度为5.74 g/cm3,与理论计算值接近.退火处理后的晶片在1000～7000 cm-1 红外波段范围内透过率达到70;.采用VUVG法生长的CdSe单晶体,结晶性能好、结构致密、尺寸大和红外透过率高,可用于制备红外非线性光学器件.     

水基流延成型和热压烧结制备碳化硼陶瓷及性能研究

以工业碳化硼粉末为原料、采用Si3N4磨球磨损法引入Si3N4烧结助剂,采用水基流延成型和热压烧结方法制备了碳化硼陶瓷.研究了氧含量、分散剂、pH值等因素对B4C陶瓷浆料分散性能的影响,采用XRD、SEM等对碳化硼陶瓷的物相、显微结构和第二相分布进行了表征,并测试了样品的维氏硬度、断裂韧性、抗弯强度和弹性模量.结果表明:经醇洗后的碳化硼粉末中氧化硼含量降低,有利于B4C陶瓷浆料的分散稳定.采用球磨磨损引入了Si3N4粉,在B4C基体中通过原位反应形成第二相SiC和BN,SiC和BN第二相颗粒在B4C基体中弥散分布均匀.在2100 ℃热压烧结样品的维氏硬度、抗弯强度、断裂韧性和弹性模量分别达到30.2 GPa、596.5 MPa、3.36 MPa·m1/2和362.3 GPa.     

EDTA和KCl掺杂对KDP晶体光学质量的影响

通过传统降温法生长了不同EDTA和KCl剂量掺杂的KDP晶体,并观察了晶体的光散射情况,测定了晶体柱区样品的透过率和晶体中Fe、Cr、Cl三种杂质元素的含量,结果表明:低浓度的EDTA(0.01 mol;)和KCl(＜1.5 mol;)掺杂可以提高晶体的透过率,但高浓度掺杂(0.01 mol;EDTA, 2.0 mol; KCl)会导致晶体散射严重,透过率降低,KCl浓度达到2.5 mol;后晶体生长受到抑制,晶体缺陷严重;晶体中铁Fe3+、Cr3+的总含量随着掺杂浓度的增加而减少,晶体中并没有发现Cl元素存在.     

Growth improvement and quality evaluation of ZnGeP2 single crystals using vertical Bridgman method

ZnGeP₂ single crystals were grown using two-temperature zone vertical Bridgman method. The effect of crucible material, crucible shape, and cooling program on the growth of the ZnGeP₂ crystal was investigated. The qualities of the crystals were evaluated by high resolution X-ray diffraction, X-ray fluorescence spectrometry, and IR transmittance spectra. The results show that the full width at half maximum of the rocking curves for (200), (004), and (220) faces are 45″, 37″, and 54″, respectively. The concentration of the P, Zn and Ge are almost homogeneous along the growth axis, but P and Zn are slightly deficient compared with Ge in the as-grown ZnGeP₂ crystals. The increase of annealing temperature from 600 °C to 700 °C has little effect on the reduction of the absorption losses in ZnGeP₂ powders, and has negative effect on the reduction of the absorption losses in ZnP₂ powders. Annealed in ZnP₂ powders at 600 °C for 300 h, the optical absorption loss at 2.05 μm reduce by 37%, compared with that of 27% reduction annealed in ZnGeP₂ powders.     

Purification and mechanical nanosizing of Eu-doped GaN

Eu:GaN powder synthesized using a high temperature ammonothermal process is known to be dark in appearance due to presence of Eu-containing absorbing particles. Improvement of the visual quality of the Eu:GaN powder is achieved by rinsing in dilute acids. Acid-rinsed Eu:GaN has photoluminescence (PL) enhanced by a factor of 3 when compared to as-prepared Eu:GaN. Such visually clear powders are used for making Eu:GaN nanoparticles of sizes 30–50 nm using a soft ball-milling technique. The particle size was determined using X-ray diffraction, scanning electron microscopy and a dynamic light scattering system. Longer durations of a “soft” ball-milling technique results in particle size reduction. These nanopowders show significant photoluminescence intensity with no yellow luminescence, and have a reduced PL intensity with increasing ball-milling time. Eu:GaN nanopowder embedded in a KBr matrix shows at least a 10× improvement in transmittance when compared to as-prepared powders. The improvement of transmittance depends on both the concentration and particle size. This improved transmittance suggests that such a transparent matrix could be used as a laser gain medium.     

钨酸铅闪烁晶体的双掺杂性能研究

本文采用坩埚下降法生长出了PbWO4:(F,Er)晶体和PbWO4:(F,Nd)晶体,并且对此两种晶体透过性能和闪烁发光性能进行了测试分析.透过光谱结果显示,PbWO4:(F,Er)晶体和PbWO4∶(F,Nd)晶体在350 nm至700nm范围内的透过率比纯的钨酸铅均有较大的提高.紫外激发发射光谱测试结果表明,通过双掺杂可以提高钨酸铅晶体闪烁发光的强度,并且PbWO4:(F,Er)双掺杂晶体在波长为527 nm处和546 nm处均形成了较强的发光峰.通过对掺杂晶体进行XRD分析可知,阴阳离子的同时掺入并未引起钨酸铅晶体结构的明显改变.     

Growth and characterization of undoped and thallium doped cesium iodide single crystals

Single crystals of pure and thallium (Tl) doped cesium iodide (CsI) have been grown by melt growth (Bridgman) technique. The grown crystals were subjected to powder X-ray diffraction and high-resolution XRD analysis. The cut and polished crystals were characterized for luminescence studies. UV-visible transmission studies have been carried out on the grown crystal in the wavelength range 200–650 nm. From the transmission spectrum it was found that the cut off wavelength increases with increase in Tl concentration and the transmittance is about 70%. The 0.06 mol% of Tl doped CsI crystal shows a good energy resolution of 7.6%. The hardness decreases for increasing the doping concentration. Etching studies have been carried out on doped and undoped crystals using methanol and water as etchant.     

水热法生长非线性光学晶体K4Gd2(CO3)3F4

采用水热法,探索了 K4Gd2(CO3)3F4晶体的析晶条件,诸如生长原料及配比、生长温度、生长周期等,并成功生长了毫米级的透明单晶.对生长的晶体进行了XRD、UV-Vis-NIR、SHG等测试,结果表明,K4Gd2( CO3)3F4晶体在380～2000 nm波段的透过率超过80;,紫外吸收截止边低于200nm;其二阶非线性光学效应约为KDP的3.5倍.     

基于负折射率材料一维光子晶体可调节的频率和方向滤波器

为实现可调节的频率和方向滤波器,设计基于负折射率材料含空气层缺陷的一维光子晶体.用特征矩阵的方法研究电磁波在此种结构中的透射系数.研究发现在零平均折射率带隙内存在缺陷模,在正入射条件下缺陷模位置通过改变空气层厚度来调节.对在零平均折射率带隙内某个频率的电磁波,有某个特定方向让其透射,该方向也可以通过改变空气层厚度来调节.研究结果为设计可调节的频率和方向滤波器提供了理论依据.     

Improvement of growth habit and optical properties of rapidly grown KDP crystal by adding diethylene triamine pentacetate acid in growth solution

By altering the concentration of a new additive ‐ diethylene triamine pentacetate acid (DTPA) in the growth solution, a series of KDP crystals were obtained by the “point seed” rapid growth method. The growth rates up to about 20 mm/day. Effects of DTPA on the growth habit and optical properties of these as‐grown KDP crystals were investigated. The results reveal that, with the increase of DTPA concentration in growth solution, the contents of impurity metal ions incorporated into crystal and aspect ratio of crystal morphology were both decreased gradually, while the UV transmittance of crystal was enhanced continually. In the presence of moderate concentration of DTPA (100–200 ppm), the solution stability was increased and optical properties of crystal (including optical homogeneity, light scattering and laser damage threshold) were all improved. However excessive doping (>500 ppm) has opposite effects. The impact mechanism was also analyzed combining with the structure of KDP crystal and chemical characteristics of DTPA molecular.     

KCaCl3:Ce晶体的生长及发光性能

采用坩埚下降法生长出不同摩尔分数Ce³⁺(1%、2%、4%、6%、8%)掺杂的KCaCl₃:Ce单晶。晶体属于正交晶系,晶胞参数为a=0.756 0 nm,b=1.048 2 nm,c=0.726 6 nm。热重分析仪测得熔点为740 ℃,透过率测试显示晶体在可见光波段均具有较好光学透过率。对晶体的光致发光光谱、光致衰减时间、X射线激发发射光谱、透过率等光学性能进行了表征。光致发光光谱显示KCaCl₃:Ce晶体在358 nm和378 nm波长左右有宽的发射峰,符合Ce³⁺的5d₁→²F_5/2和5d₁→²F_7/2能级跃迁,通过拟合,KCaCl₃:Ce晶体的衰减时间在30 ns左右。晶体在X射线激发下均表现出优异的X射线发光性能。     

Zn2+掺杂对TiO2相变温度和晶粒尺寸的影响

采用溶胶-凝胶法制备了不同含量Zn2+掺杂的氧化钛粉体,利用TG-DTA、XRD测试技术检测了锌离子掺杂对锐钛矿和金红石相变及其晶体尺度的影响.试验结果表明,锌离子的掺入抑制了锐钛矿和金红石的相变,使相变温度提高,而且显著阻碍晶体的生长,从而获得纳米晶体.