Sc2O3: Nd,Sc2O3:Yb纳米粉体的制备和光致发光

以反滴定共沉淀方法制备了Sc2O3:Nd、Sc2O3 :Yb纳米粉体,用热重、差热分析、X射线衍射对前驱体相变及粉体结构进行了研究,并研究了其光致发光.Sc2O3:Nd、 Sc2O3:Yb前躯体的热重和差热曲线分别在73 ℃、77 ℃与434 ℃、436 ℃出现了明显的热失重和吸热峰,结合XRD表明约在450 ℃,前驱体粉体经γ-ScOOH相转变为立方Sc2O3相.Reitveld方法精修给出Sc、O的原子坐标.结果表明,掺杂离子导致了晶格畸变.在825 nm光激发下,粉体Sc2O3 :Nd的1084 nm主荧光峰为Nd3+的4F3/2→4I11/2跃迁;在937 nm光激发下,粉体Sc2O3:Yb的1044 nm主荧光峰为Yb3+的2F5/2→2F7/2跃迁.Sc2O3:Nd、Sc2O3:Yb的发光光谱表明激活离子处于较强晶场中,Stark能级分裂大,有利于降低Yb3+的激光阈值、提高激光热稳定性.     

Yb:CaF2透明陶瓷的制备与性能研究

采用共沉淀法合成5at;Yb:CaF2纳米粉体.该粉体为纯立方CaF2相,平均颗粒尺寸为45 nm.Yb:CaF2纳米粉体呈立方体状,具有较好的分散性.通过真空预烧结合热等静压烧结(HIP)后处理制备5at;Yb:CaF2透明陶瓷,研究了真空预烧温度对陶瓷物相、致密度、显微结构及光学透过率的影响.结果表明,不同温度真空预烧的陶瓷均为纯立方相,在650℃真空预烧的5at;Yb:CaF2陶瓷经HIP处理后具有最好的光学质量,其在1200 nm处的直线透过率达到87;(厚度为3 mm).     

溶胶-凝胶燃烧法合成Nd:GGG激光陶瓷粉体

采用溶胶-凝胶燃烧法成功合成了Nd:GGG激光陶瓷粉体,讨论了溶胶-凝胶的转化,并对Nd:GGG粉体进行了XRD、TG-DTA、SEM及荧光光谱分析.XRD分析表明1000℃是Nd:GGG粉体合成的最佳温度,并且随着煅烧温度的升高粉体的粒径长大,SEM观察发现在1000℃下粉体粒度均匀,平均粒径为100nm,荧光光谱测试结果表明荧光发射的最强峰位于1061.54nm处,是Nd3+的4F3/2-4I11/2谱相导致的荧光发射.     

炭吸附纳米氧化铁的制备及其可见光催化性能

采用炭吸附共沉淀法制备了氧化铁(Fe2O3)纳米粉体,通过热重分析仪(TG-DTA)、X射线衍射仪(XRD)、紫外可见分光光度计(UV-Vis)和透射电镜(TEM)等手段对催化剂的热稳定性、物相结构、吸光性能、形貌进行表征;以甲基橙(MO)为目标降解物,镝灯为可见光源,研究了Fe2 O3纳米粉体的光催化性能.结果表明,炭吸附共沉淀法制得的Fe2O3粉体粒径小、分布均匀、团聚较少;Fe2O3的吸收波长发生红移且在紫外光、可见光区域的吸收能力增强.光催化降解甲基橙结果显示,炭吸附共沉淀法制得的Fe2O3粉体在60 min内降解率达到74;,是沉淀法制备的Fe2O3粉体降解率的2.2倍.     

Y2O3∶Yb3+,Tm3+纳米粉体的制备及发光性能研究

以Y2O3为基质材料,Yb3+为敏化剂,Tm3+为激活剂,采用化学共沉淀法制备Y2O3∶Yb3+,Tm3+纳米粉体,通过差热、红外光谱、XRD、荧光、上转换发光和场发射电子显微镜等方法对样品进行表征.结果表明:Tm3+和Yb3+完全固溶到Y2O3立方晶格中,且粉体大小均匀,尺寸约50 nm;Yb3+浓度为4;(摩尔分数)、煅烧温度900 ℃时,荧光和上转换发光强度最强;Tm3+浓度为0.4;时绿光(5F4/5S2→5I8)和红光(2F5/2→2F7/2)荧光强度最强,浓度0.5;时蓝光(1G4→3H6)和红光(1G4→3F4)的上转换发射强度最大.     

Tm3+/Ho3+掺杂的Gd3Ga5O12～2.0μm波段红外激光晶体的生长和性能研究

采用提拉法生长了最大尺寸为φ25mm×(30～40)mm优质透明的Tm3+:GGG、Yb3+/Tm3+:GGG、Cr3+/Tm3+:GGG、Tm3+/Ho3+:GGG和Cr3+/Tm3+/Ho3+:GGG共五种晶体.在室温下测试了这些晶体的吸收光谱、荧光光谱及荧光衰减曲线等,详细研究了光谱性能,对部分晶体进行了Judd-Ofelt理论计算,得到强度参数等重要的光谱参数.计算了～2.0μm附近荧光峰值波长处相应的能级跃迁的发射截面、量子效率等.研究表明:Yb3+和Cr3+的掺入分别使得Tm:GGG晶体在980nm附近和451 nm、628 nm附近的吸收大大增强,有利于商业激光二极管和闪光灯泵浦.在Tm激活的Tm3+:GGG、Yb3+/Tm3+:GGG、Cr3+/Tm3+:GGG晶体中,～2.0μm波段附近发射强度和发射截面值最大的峰值对应的波长为2000nm;而在Ho激活的Tm3+/Ho3+:GGG和Cr3+/Tm3+/Ho3+:GGG晶体中,发射强度和发射截面最大的峰值对应的波长为2080 nm.用氙灯抽运键合的尺寸为φ5mm×45mm Cr3+/Tm3+/Ho3+:Gd3+ Ga5 O12晶体,在2.086～2.102μm波段实现了平均功率为170 mw的激光输出.     

Y2O3添加对Yb2Si2O7无压烧结致密化的影响

以Yb2O3粉末和溶胶-凝胶法制备的活性SiO2凝胶为原料,在1550℃保温4h合成了具有单斜结构的单相Yb2Si2O7粉体.采用无压烧结方法获得了Yb2Si2O7陶瓷.通过添加Y2O3烧结助剂,获得了气孔率为3.2;的致密Yb2Si2O7陶瓷.采用XRD、SEM方法对烧结体的结构、成分和形貌进行测试与表征.结果表明:烧结体均为单相的Yb2Si2O7,不含其它杂质相.Y2O3的添加大大降低了烧结体的气孔率,促进了烧结的致密化.所得致密Yb2Si2O7陶瓷的平均晶粒尺寸为1～2 μm,大部分晶粒为颗粒状晶粒.     

铝粉粒度对自蔓延高温合成AlB_2-Al_2O_3复合粉体的影响

以金属Al粉和B_2O_3粉为原料,采用自蔓延高温合成法(SHS)制备AlB_2-Al_2O_3复合粉体。采用X射线衍射仪、扫描电镜和能谱仪分析手段,对所制得的复合粉体进行了表征。研究了Al粉粒度(100目、300目和600目)对自蔓延高温合成方法制备AlB_2-Al_2O_3复合粉体的燃烧学、相组成及微观结构的影响。结果表明:铝粉粒度越小,燃烧温度越高、燃烧波速度越快,复合粉体中AlB_2相含量增加,实验测得600目铝粉反应的燃烧温度为2060 K,燃烧波速度为2.08 mm/s。复合粉体以AlB_2和Al_2O_3为主晶相,显微结构为数量较少、粒径约5μm的AlB_2粉弥散分布于粒径约2μm的Al_2O_3和Al的混合粉中。     

共沉淀法制备Ba(Fe0.5 Nb0.5)O3纳米粉体

以廉价的Nb2O5为铌源,采用共沉淀法制备了纳米Ba(Fe0.5Nb0.5)O3粉体.用XRD、TG-DSC、FT-IR、SEM等测试手段分析了烧结温度、保温时间、体系温度、pH值等对前驱体粉体的物相、形貌及晶粒大小的影响,并对粉体的磁学性能进行了表征.结果表明:合成温度在950℃,体系温度在30℃和50℃均可获得纯相立方钙钛矿结构的Ba(Fe0.5 Nb0.5)O3粉体,保温时间和pH值对粉体相结构变化无影响.在体系温度为30℃,pH=10,前驱体粉体在950℃煅烧2h后获得颗粒尺寸约30 nm的Ba(Fe05Nb0.5)O3粉体,且粉体具有弱的铁磁性.     

溶胶-凝胶法制备Nd:GGG透明陶瓷纳米粉体

溶胶-凝胶法制备出Nd3+∶Gd3Ga5O12(Nd:GGG)透明陶瓷纳米粉体.以TG-DTA、红外光谱、XRD、TEM、电子衍射和电子能谱等测试手段,对前驱体及烧成粉体的结构和形貌进行了研究.结果表明,Nd∶GGG超细粉体的最佳烧成温度为1000℃,粉体样品粒度小、粒径均匀,在70～100nm之间.     

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。     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

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.     

Photoluminescence characteristics of Mg- and Si-doped GaN thin films grown by MOCVD technique

We have studied the optical, structural and surface morphology of doped and undoped GaN thin films. The p- and n-type thin films have been successfully prepared by low-pressure MOCVD technique by doping with Mg and Si, respectively. The different carrier concentrations were obtained in the GaN thin films by varying dopant concentrations. Photoluminescence (PL) studies were carried to find the defect levels in the doped and undoped GaN thin films at low temperature. In the undoped GaN thin films, a low intensity and broad yellow band peak was observed. The donor–acceptor pair (DAP) emission and its phonon replicas were observed in both the Si or Mg lightly doped GaN thin films. The dominance of the blue and the yellow emissions increased in the PL spectra, as the carrier concentration was increased. The XRD and SEM analyses were employed to study the structural and surface morphology of the films, respectively. Both the doped and the undoped films exhibited hexagonal structure and polycrystalline nature. Mg-doped GaN thin films showed columnar structure whereas Si-doped films exhibited spherical shape grains.