Er~(3+)/Yb~(3+): KY(WO_4)_2晶体光谱的各向异性分析

在室温下测量和分析Er~(3+)/Yb~(3+): KY(WO_4)_2晶体三个折射率主轴方向上的吸收光谱和荧光光谱,其吸收光谱和荧光光谱谱带强度明显呈现各向异性;用修正的Judd-Ofelt理论计算Er~(3+)/Yb~(3+): KY(WO_4)_2晶体中Er~(3+)在三个折射率主轴方向上的强度参量Ω_t (t=2,4,6)和各吸收谱带的电偶极跃迁振子强度,同时计算了Yb~(3+)在三个轴向上980 nm波长处的积分吸收截面.结果表明:Er~(3+)/Yb~(3+): KY(WO_4)_2晶体吸收光谱和荧光光谱存在各向异性,N_p轴为Er~(3+)/Yb~(3+): KY(WO_4)_2激光晶体的最佳泵浦轴向.     

0.5at;Yb∶YAG晶体光谱与激光性能研究

采用提拉法生长yb3+掺杂浓度为0.5at;高质量的Yb∶Y3 Al5O12(Yb∶YAG)晶体.对晶体的结晶质量、分凝系数和光谱和激光性能进行了表征.结果表明:所生长的晶体结晶质量较好,在空气中退火后晶体吸收系数略有增加,晶体中自吸收效应的影响很小,具有宽的发射带.Yb∶YAG晶体和Yb∶YAG/YAG复合晶体分别在抽运功率为7.1W和6.15W的LD抽运下,获得2.19W和1.354 W的连续激光输出,斜率效率分别为34.58;和25.9;.     

掺镱钆镓石榴石激光透明陶瓷纳米粉体的研究

以Gd_2O_3、Yb_2O_3和Ga_2O_3为初始原料,碳酸氢铵为沉淀剂,硫酸铵为分散剂,采用均相共沉淀方法制备了Yb~(3+): Gd_3Ga_5O_(12) (Yb: GGG).用差热-热重分析仪、X 射线衍射仪、红外光谱分析仪、扫描电镜、透射电镜等测试方法对Yb: GGG粉体进行了表征.结果表明:前驱体经过900 ℃煅烧8 h 后已完全转变成纯立方相GGG多晶样品,所得的粉体分散性好,团聚轻,颗粒尺寸在50～100 nm之间.本文亦对均相共沉淀法合成Yb: GGG的反应过程进行了探讨.     

Ce∶LuAG闪烁晶体的生长研究

Ce∶LuAG晶体是一种性能优良的闪烁材料,但采用提拉法生长Ce∶LuAG时,经常出现开裂和包裹物缺陷。本文通过理论与实践相结合的方式分析了温度梯度、提拉速度、晶体旋转速度和热应变等因素对晶体产生缺陷的影响,并提出了解决办法,给出了适合生长优质Ce∶LuAG晶体的工艺参数:熔体上方温度梯度在5 ℃/mm左右,放肩角度在30°~60°,提拉速度1.0~1.5 mm/h,晶体旋转速度15~25 r/min。最后成功生长出直径30 mm、等径长50 mm质量较为完好的Ce∶LuAG单晶,晶体内核心面积小。     

Yb: YAG微晶玻璃的制备与性能研究

本文采用高温熔融工艺,制备Yb~(3+)掺杂的32CaO-(13-x)Y_2O_3-24Al_2O_3-31SiO_2-xYb_2O_3 (x＝0.5～2)系统玻璃,并在高温下进行去应力退火.用DTA确定样品的热处理温度,XRD分析热处理后样品的相变.用TEM观察1000 ℃热处理后的样品,在室温下测试1000 ℃热处理后玻璃的吸收光谱.结果表明:玻璃在1000 ℃热处理24 h后,产生单一的YAG相微晶颗粒;热处理前后样品光谱特性的变化表明热处理后掺杂的Yb~(3+)择优进入YAG晶格中,得到了透明的Yb: YAG微晶玻璃.     

镥铝石榴石(Lu3Al5O12∶Pr)晶体的生长及发光性能

用提拉法生长出了直径45 mm的Lu3Al5O12:1; Pr(LuAG: Pr)石榴石闪烁晶体.测试了该晶体不同部位样品的吸收谱、激发发射光谱和多道能谱等.对晶体的吸收波段、发光峰位和激发波长及其对应的Pr离子中电子的跃迁能级进行了指认.测得LuAG: Pr晶体在137Cs放射源激发下的闪烁衰减时间为29 ns,光产额约为10800±540photons/MeV,光致发光衰减时间为21.93 ns.LuAG: Pr晶体样品的热释光(TSL)曲线证实晶体中存在较多的能够束缚电子的浅陷阱.     

(Nd3+,Yb3+):Ca3(VO4)2晶体的极化研究

本文回顾了(Nd3+,Yb3+):Ca3(VO4)2晶体的研究历程,通过对晶体结构和对晶体激光性能研究年代的对比,认为高的泵浦阈值是由于晶体中存在的对泵浦光和激光散射很强的畴壁结构未被发现而造成的.讨论了极化的原理、建立了极化装置,采用Laue定向法和X射线定向仪定向法结合解决了(Nd3+,Yb3+):Ca3(VO4)2这种大晶格常数(c＝3.8029nm)晶体的定向问题.把晶体的抛光面放入0.5mol;的温度为30℃的硼酸中腐蚀样品1h,用显微镜可以观察到畴结构.在～1100℃和电流密度为～10μA/mm2的条件下极化2h即可完成极化.变黑的极化样品可以通过把晶体放入马福炉中升温至850℃,保持1h,然后降至室温即可消除.     

新型( Yb3+,La3+)∶Gd2SiO5和(Yb3+,Tb3+)∶GdTaO4单晶生长及分凝研究

采用提拉法生长了尺寸为φ30 mm × 50 mm的(Yb3+,La3+)∶Gd2SiO5单晶和尺寸为φ24 mm×57 mm的( Yb3+,Tb3)∶GdTaO4单晶,用X射线荧光法测量了掺杂样品的组分浓度在晶体中的分布,拟合了掺杂离子的有效分凝系数,结果表明:Yb3+在Gd2SiO5晶体中的分凝系数为1.185(15),接近单位1,而La3+则为0.68 (10),偏离单位1较多,对晶体的光学均匀性会有较大的影响;Yb3+和Tb3+在GdTaO4中的分凝系数为0.84(14)和0.84(5),接近单位1,对晶体的光学均匀性影响较小.     

不同Yb掺质浓度的Yb:Y3Al5O12晶体激光性能的比较

采用提拉法生长了Yb3+掺质浓度为5;原子分数、 50;原子分数和100;原子分数的Yb:Y3Al5O12(Yb: YAG)晶体,系统地分析了不同Yb3+掺质浓度晶体的吸收光谱和荧光光谱.从吸收峰和吸收系数可以看出采用940nm LD泵浦三种不同浓度的Yb:YAG晶体都比较合适.随着Yb3+离子掺质浓度的增高,晶体中出现的自吸收现象越为明显.通过对三种不同Yb掺质浓度晶体激光性能参数的计算,得出高掺质浓度Yb:YAG和YbAG晶体是有前景的激光增益介质.     

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.     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

Selinidin: Crystal structure generated by C–H···O, C–H···π and π-π interactions

The title compound, 9,10-dihydro-8,8-dimethyl-2-oxo-2H,8H-benzo[1,2-b:3,4-b']dipyran-9-yl-2-methyl-2-butenoate, C₁₉H₂₀O₅, was isolated from the roots of Selinum vaginatum. The compound crystallizes into monoclinic space group P2 ₁ with unit cell parameters: a = 12.830(2) Å, b = 9.041(1) Å, c = 14.983(1) Å, β = 95.09(1)°, Z = 4. The crystal structure has been determined using direct methods and refined by full-matrix least-squares to a final R value of 0.0529 for 3142 observed reflections. There are two independent molecules, A and B, per asymmetric unit. In both the molecules, the coumarin nucleus is planar. However pronounced differences are observed in the conformation of dihydropyran ring which has a half-chair conformation with an 8β-9α orientation in molecule A and is intermediate between half-chair and sofa in molecule B. Differences also occur in the conformation of the 2-methylbutenoyloxy side chain at C9 due to the different geometry of C–H···π interactions in molecules A and B. Molecules A and B are connected by π–π interactions between their coumarin fragments forming dimers. The dimers interact through C–H···O and C–H···πhydrogen bonds.     

Chromene and Imidazole Based D-π-A Chemosensor Preparation and Its Anion Responsive Effects

We have designed and synthesized the colorimetric chemosensor through the reactions of 2-(4H-chromen-4-yildene)malonitrile and 4-imidazolecarboxaldehyde. Due to its well conjugated D-π-A system and the existence of NH- fragment in structure, we expected that the chemosensor can detect anion using NH- fragment in the imidazole moiety of the structure. In this regard, UV-Vis absorption spectra were measured to investigate sensing properties of the probe toward different anions in DMSO. This chemosensor can detect both fluoride and cyanide ion with absorption change in intensity. In addition, pH sensing property was also investigated upon the addition of hydroxide ion. These properties are related to the deprotonation effect. The ICT system in this molecule was also observed by the computational approach using Material Studio 4.3 package.     

电子显微分析在表征纳米晶体化学组分中的应用

纳米材料的化学组分及含量影响其光、电、声、热、磁等物理性能,电子显微分析是表征纳米晶体化学组分的重要方法之一.本文综述了X-射线能谱(EDS)、X-射线波谱(WDS)、电子能量损失谱(EELS)和选区电子衍射(SAED)等现代电子显微分析技术在表征纳米晶体化学组分、形貌、尺寸和结构等方面的应用及其研究进展,并比较了这些分析方法存在的差异,提出了其应用中存在的不足及今后的研发方向.     

4- and 5-nitroindane

Mononitration of indane produces a mixture of 4- and 5- nitroindanes. Crystallization from mixtures occurs after distillation improves composition of a major component to above 80%. 4-Nitroindane: triclinic, space group (#2),a=7.332(4) Å,b=8.304(4) Å,c=8.358(4) Å, =61.43(4)°, =67.60(4)°, =70.15(4)°,V=405.4(4) ų,Z=2. Non-H-atoms are nearly planar, aliphatic H's are eclipsed. 5-Nitroindane: monoclinic, space groupP2₁/c (#14),a=10.946(8) Å,b=15.643(10) Å,c=9.415(6) Å, =92.34(5)°,V=1611(2) ų,Z=8. Non-H-atoms in the two molecules differ in torsion of the nitro group with respect to indane and fold of the nonbenzylic methylene group. Semiempirical calculations (PM3) suggest that distorsion from planarity may be associated with the two lowest energy vibrational modes. Uv, ir, ms, proton, and¹³C-nmr spectra are correlated with the solid state structures.     

6<Emphasis Type="Italic">S</Emphasis>,8α-Dihydroxy-14,15-Dihydrocarapin (Khayanone) from the Stem Bark of <Emphasis Type="Italic">Khaya Senegalensis</Emphasis> (Meliaceae): Isolation and its Crystal Structure

Khayanone was isolated from the stem bark of African mahogany, Khaya senegalensis (Meliaceae), and characterized as 6S,8α-dihydroxy-14,15-dihydrocarapin on the basis of spectral analysis and single crystal X-ray diffraction study. The compound crystallizes in the tetragonal space group P4 ₁ 2 ₁ 2 with unit cell parameters: a = 13.2315(19) Å, c = 29.118(6) Å, Z = 8. The crystal structure has been solved by direct methods and refined to R = 0.0375 for 4552 unique reflections. The six-membered rings A and B exist in boat conformations, rings C and D in chair conformations, and the furan ring is planar. The crystal structure is stabilized by O-H···O and C-H···O interactions. This is the first report about 6S configuration of mexicanolide revealed by X-ray diffraction analysis. The configuration of oxygenated C-6 in mexicanolide-group limonoids is discussed.     

Nuclear magnetic resonance: a powerful tool to study liquid crystals

Nuclear magnetic resonance (NMR) is a spectroscopic technique widely used to investigate materials and soft matter in particular. In this brief review, the main uses of NMR techniques to investigate different aspects of liquid crystals, such as the orientational and dynamic properties, the supramolecular structure and average molecular conformations, are described. In the second part of the paper, the case study of a ‘de Vries’ liquid crystal is reported and the main results obtained by combining different NMR techniques are discussed.     

X-ray analysis of sideroxol from <Emphasis Type="Italic">Sideritis leptoclada</Emphasis>

Sideroxol (1), a kaurane diterpene which has the ent-7α,18-dihydroxy-15β,16β-epoxykaurane structure (MW = 320.47, C₂₀H₃₂O₃) was obtained from the acetone extract of Sideritis leptoclada plant as well as from some other Sideritis species. It crystallizes in the orthorhombic space group P2₁, 2₁, 2₁ with a = 10.967(3), b = 24.555(5), c = 6.372(4) Å, Dc = 1.240 g cm⁻³, Z = 4, and refines to R = 0.065 for 721 independent reflections. The skeleton consists of three fused six-membered rings and a five-membered ring with fused epoxide. The six membered rings exhibited slightly distorted chair conformation. In addition to sideroxol, two kaurane and five kaurene diterpenes were isolated from the hexane and acetone extracts of the studied plant.     

New zeotype borophosphates with chiral tetrahedral topology: (H)0.5M1.25(H2O)1.5[BP2O8]·H2O (M = Co(II) and Mn(II))

Two new isostructural open‐framework zeotype transition metal borophosphate compounds, (H)_0.5M_1.25(H₂O)_1.5[BP₂O₈]·H₂O (M = Co(II) and Mn(II)) were synthesized by mild hydrothermal method. The structure of compounds were characterized by single‐crystal X‐ray diffraction which have ordered, alternating, vertex‐sharing BO₄, PO₄, and (MO₄)OM(H₂O)₂ groups with hexagonal, P 6₁ 2 2 (No 178) space group and unit cell parameters for Co a = 9.4960(6) Å, c = 15.6230(13) Å, for Mn a = 9.6547(12) Å, c = 15.791(3) Å, Z = 1 for both of them. TGA/DTA analysis, IR spectroscopy were used for characterization. Magnetic susceptibility measurements for both of the compound indicate strong antiferromagnetic interaction between metal centers. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)