一维Sm2O3纳米晶的可控合成及其光学性能研究

以有机碱二乙烯三胺(EDTA)为碱源,Sm(NO3)3·6H2O为钐源,在不同模板剂辅助条件下采用水热-热处理相结合的方法进行Sm2O3纳米晶的可控合成.利用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)和Lambda 950分光光度计分别对产物的物相、形貌和光学性能进行表征,并研究了未添加模板剂和分别以六亚甲基四胺(HMTA)、聚乙烯吡咯烷酮(PVP)和十六烷基三甲基溴化铵(CTAB)为模板剂条件下对产物的物相、形貌及光学性能的影响.结果表明:以HMTA为模板剂条件下得到了长条状结构的Sm2O3纳米晶,未添加模板剂和分别以PVP和CTAB为模板剂条件下得到了尺寸可控的棒状结构的Sm2O3纳米晶.不同模板剂会影响产物的微观结构及尺寸,进而对其光学性能产生有较大的影响,其中以HMTA为模板剂时所得长条状结构的Sm2O3纳米晶的禁带宽度较小为4.775 eV.     

硫化锌纳米晶的合成及性能表征

采用水热法以油酸和十二烷基硫酸钠(简记为SDS)作为复合型表面活性剂制备ZnS纳米晶,并对制备的ZnS纳米晶进行了表征.通过正交实验考察了油酸用量、SDS用量、反应温度、反应时间及pH值对ZnS发光性能的影响,确定了最佳工艺条件.结果表明,制备的ZnS为闪锌矿结构,单分散,粒径尺寸为6 nm,ZnS纳米晶表面的亲水性得到了有效的改善.所以,复合型表面活性剂的使用既可以提高ZnS纳米晶的发光性能又起到表面改性的作用.     

PbS/CdS纳米晶共敏化ZnO纳米线太阳能电池的性能研究

以Zn (Ac)2·2H2O为原料在强碱性条件下合成一维结构的ZnO纳米线,SEM结果表明合成的纳米线尺寸、形貌、长径比均一;并以油胺为单一溶剂采用热注射法制备了形貌、尺寸均匀的PbS纳米晶;构建PbS纳米晶敏化ZnO纳米线基太阳能电池,同时为了改善电池的光电转换效率并构建了PbS/CdS纳米晶共敏化电池,并测试了电池的光电流密度-光电压(J-v)曲线以及Nyquist曲线图,结果表明PbS/CdS纳米晶共敏化电池性能明显优于单纯的PbS纳米晶敏化ZnO纳米线太阳能电池.     

Bi2Te3纳米晶溶剂热合成及表征

采用溶剂热方法,在水合肼溶剂中通过添加适量表面活性剂十二烷基硫酸钠(SDS),在180 ℃下反应10 h后成功地制备了不同形貌的纯相Bi2Te3纳米晶,包括纳米颗粒、纳米棒和花瓣状纳米片.用X射线衍射(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、能量色散谱仪(EDS)对产物进行了表征,探讨了表面活性剂用量和温度对产物形貌的影响,提出了可能的形成机理.     

钙钛矿型SrSnO3纳米棒的合成

采用表面活性剂CTAB(十六烷基三甲基溴化铵)辅助水热法制备了SrSn(OH)6前躯体,将SrSn(OH)6前躯体600 ℃热处理3 h合成了钙钛矿立方SrSnO3一维纳米棒.通过热重-差热分析(TG-DTA)、X射线衍射图谱(XRD)、红外光谱(IR)、透射电子显微镜(TEM)对所合成样品进行了表征.结果表明,水热体系的pH值以及水热温度是影响所得产物纯度和结晶度的重要因素.在合成过程中,表面活性剂CTAB对样品纳米棒结构的生长具有关键作用.     

DMF体系中Cu2O球晶的制备及形貌分析

以N,N-二甲基甲酰胺(DMF)为溶剂,通过改变铜源和表面活性剂,调控反应参数,溶剂热条件下制备了三维十字形、空心及实心的Cu₂O球晶。利用XRD、SEM等表征手段,分析探讨了工艺条件变化对Cu₂O球晶形貌的影响。研究表明,随着DMF浓度的增大,体系的还原能力增强,Cu⁺增多,溶液的过饱和度增大,Cu₂O晶体集合体形态由晶体结构控制的各向异性与对称性的球晶逐渐向各向同性球晶演变。十二烷基硫酸钠(SDS)、十六烷基三甲基溴化铵(CTAB)、聚乙烯吡咯烷酮(PVP)等表面活性剂有助于降低溶液的过饱和度,增加结晶质的表面扩散能力,有利于规则形态Cu₂O晶粒的形成。反应体系中,Cu(Ac)₂·H₂O水解生成的羧基与DMF中的甲酰基在高温下发生脱羧反应产生CO₂气体以及SDS发泡作用产生的气体是形成空心Cu₂O球晶的重要原因。     

表面活性剂对钨酸铅低维粉体形貌的影响

以钨酸钠和醋酸铅为原料,分别加以表面活性剂聚乙二醇200和十六烷基三甲苯溴化铵,用沉淀法合成出钨酸铅纳米晶和菱形微晶.对样品进行X射线分析,结果显示样品结晶良好.对样品进行透射电子显微镜分析,结果显示钨酸铅纳米晶和菱形微晶成形良好,且分散性良好、无团聚发生.讨论了表面活性剂对钨酸铅低维粉体形貌的影响,认为PEG200对分散性良好的钨酸铅纳米晶的生成起了关键作用,而CTAB则促进了成形良好的菱形钨酸铅微晶的生成.     

不同表面活性剂对La2Ce2O7纳米晶体生长活化能的影响

以La2O3和Ce(NO3)3·6H2O为原材料,以SDBS和CTAB为表面活性剂,采用水热合成法制备了La2Ce2O7纳米晶体.通过XRD、Raman、SEM和TEM对粉体的物化性能进行了分析,讨论了不同表面活性剂对晶体生长活化能的影响.结果表明:添加两种表面活性剂的样品均为萤石结构,以CTAB为表面活性剂的样品晶粒尺寸为11.4 nm,比表面积为187.53 m2·g-1,其晶体生长活化能(16.33±0.02 kJ·mol-1)要大于添加阴离子表面活性剂(SDBS)的样品(13.47±0.03 kJ·mol-1).     

Fe3+诱导囊泡相磁流体的形成及性能

以阳离子表面活性剂N,N-二甲基十二烷基氧化胺(DDAO)和阴离子表面活性剂硬质酸铁(STFE)为原料,通过Fe3+诱导形成囊泡,并以其为微反应器,促使Fe2+在囊泡内发生反应,得到平均粒径为15 nm的Fe3O4纳米晶,该纳米晶分散于囊泡内,得到稳定磁流体.采用广角X射线衍射(XRD),X射线光电子能谱(XPS)、透射电镜(TEM)、扫描电镜(SEM)、磁滞回线(VSM)等对合成的Fe3O4纳米晶以及磁流体进行分析表征.结果表明,以Fe3+诱导囊泡为微反应器形成的磁流体稳定性优良,在磁场反复作用后,仍具有良好的稳定性,其中的Fe3O4纳米粒子颗粒均匀,具有超顺磁性特征,磁饱和度达到79.98 emu/g.     

表面活性剂对水热法合成ZnS:Cu,Al纳米晶光致发光特性的影响

采用水热法直接合成了ZnS∶Cu,Al纳米荧光粉,并且系统研究了加入表面活性剂在不同S/Zn下,清洗样品和不清洗样品的结晶性、傅立叶红外光谱(FT-IR)及光致发光(PL)光谱.XRD和TEM测试结果表明:合成纳米晶为纯立方相结构,球形纳米晶尺寸约15 nm, 尺寸分布窄,分散性好.未清洗样品的结晶性比清洗样品的好,且加入表面活性剂和未清洗都导致粒径增大,影响纳米材料的表面态.改变[S~(2-)]/[Zn~(2+)]物质的量比、清洗和加入表面活性剂都会影响材料的PL强度.这说明其发光机理为紫外光激发材料表面的发光中心,即PL强度决定于纳米材料的表面态.     

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。     

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.     

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)     

Solubility of Ag2O into the Na2O–B2O3–Al2O3 system

The solubility of Ag₂O was measured for the Na₂O–B₂O₃ and Na₂O–B₂O₃–Al₂O₃ system with the rotating crucible method and static method, respectively, under air atmosphere at temperatures ranging from 1273 to 1423 K. The contamination of melts from crucibles could be avoided by the rotating crucible method, with which it became possible to measure the solubility of Ag₂O for the Na₂O–B₂O₃ system above the melting point of Ag for the first time. It was found that the addition of Na₂O decreases the solubility of Ag₂O while the addition of Al₂O₃ had little effect on the solubility. The effect of Na₂O and Al₂O₃ on the solubility of Ag₂O is expressed by interaction coefficients and is analyzed in terms of the basicity of melts. The solubility of Ag₂O in Na₂O–B₂O₃–Al₂O₃ melts increased with increased temperature. This phenomena was explained by a small enthalpy change in oxidation of silver.     

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.     

Considerations on the structure and physical properties of B2O3-SiO2 and GeO2-SiO2 glasses

Data of density, refractive index and thermal expansion coefficient for B₂O₃-SiO₂ and GeO_2-SiO₂ glasses have been analyzed. The volumes of the structural units are the same found for the vitreous B₂O₃, GeO₂ and SiO₂. The volume of any structural unit is constant over the entire composition region of the glass system. The same has been found for the differential refraction and unit refraction of the structural units in these glasses. Different features are observed for the differential expansion of the structural units. There is a considerable change with composition in the differential expansion of BO₃, GeO₄ and SiO₄ units. The effect is attributed to a change in the asymmetry of vibrations with the number of Si-O-B or Si-O-Ge linkages in the matrix. The thermal expansion coefficient is mainly determined by the contribution of B₂O₃ or GeO₂ in the concerned glasses.