SnS片状纳米晶的制备及其表征

用水热法制备了SnS片状纳米晶.通过X射线衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM),X射线能谱(EDS)等方法对所制备的样品SnS粉晶的结构形貌及组分进行了表征.研究了影响合成SnS片状纳米晶的几个因素,讨论了片状纳米晶生长过程与(040)晶面择优取向的关系,并分析了SnS片状纳米晶的合成机理.     

星状VO2纳米结构的制备及电化学性能研究

以草酸和五氧化二矾为原料,通过水热法制备出电化学性能优异的星状VO2纳米材料.应用X-射线衍射仪(XRD)、X-射线光电子能谱仪(XPS)和扫描电子显微镜(SEM)等设备分别对样品的物相、元素组成及价态和形貌进行表征.电化学结果显示,星状VO2纳米结构在0.2 A· g-1的电流密度下,其比电容高达574.75 F· g-1,且能量密度为51.09 Wh· kg-1.经过4250次循环充放电后,星状VO2比电容仍保持90.2;,表现出极高的电容性能.     

三硒化二铋微/纳米晶的可控合成

采用溶剂热法,在N,N-二甲基甲酰胺和乙二醇的混合溶剂中,无碱条件下,通过添加适量聚乙烯吡咯烷酮(PVP),成功制备出硒化铋微/纳米晶.采用X射线衍射(XRD)、扫描电子显微术(SEM)、透射电子显微术(TEM)、选区电子衍射(SAED)、高分辨透射电镜(HRTEM)和X射线光电子能谱(XPS)对产物进行了表征,结果表明获得了Bi2Se3单晶纳米片结构,边长约为300～1100 nm,厚度约为200～500 nm,讨论了PVP添加量对产物形貌的影响,并研究了六方片状硒化铋产物的产生机理.     

Cu2ZnSnS4纳米片的两步法制备及其光学性能

先后利用化学气相沉积法和液相离子交换法,在FTO导电玻璃基底上两步法制备Cu2ZnSnS4 (CZTS)纳米片,并通过X射线衍射仪(XRD)、拉曼光谱仪(Raman)、扫描电镜(SEM)、透射电镜(TEM)、X射线能谱(EDS)和紫外-可见吸收光谱仪(UV-vis)等表征手段对所得样品的物相结构、微观形貌、化学组分及光学性能进行测试分析.研究结果表明,所得样品为四方晶型CZTS纳米片,对可见光具有良好的全波段吸收,经计算其禁带宽度约1.51 eV.此外,对CZTS纳米片的形成机理进行初步探讨.     

Cu2ZnSnS4纳米晶的溶剂热法制备和表征

利用溶剂热制备了Cu2ZnSnS4 (CZTS)球形纳米晶.采用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、能量色散谱(EDS)和紫外-可见分光光度计对产物的物相结构、形貌、化学组分及光学性能进行表征.结果表明:所制备的CZTS球形纳米晶具有锌黄锡矿结构,球形颗粒的直径为190～300 nm,每个球形颗粒是由很多平均尺寸大约24 nm的纳米晶构成.纳米晶具有锌黄锡矿结构,其禁带宽度约为1.55 eV.同时研究了反应前驱溶液中不同量的硫脲和氯化锌对所制备的CZTS纳米颗粒的结构、原子组分比和形貌的影响规律,并对其形成机理进行了初步探讨.     

La-TiO2/ZnO异质结纳米复合材料的光催化性能

利用溶胶-凝胶法与固相混合法制备了掺La超微纳米晶TiO2负载ZnO异质结纳米复合材料La-TiO2/ZnO.采用比表面积(BET和BJH)、X-射线衍射(XRD)、紫外-可见光吸收(UV-vis)、高分辨透射电镜(HRTEM)和X-射线光电子能谱(XPS)表征催化剂的物理化学性能.La-TiO2/ZnO异质结光催化活性通过紫外光降解亚甲基蓝(MB)来评价,当nTiO2:nLa∶ nZnO=1∶0.015∶0.5时,光催化活性最佳.其主要原因是掺La超微纳米晶TiO2在ZnO表面形成多异质结,可有效抑制光生电子空穴对的复合.本文探讨了光催化活性较高的催化机理.     

溶胶-凝胶法制备CoTiO3纳米晶及其合成活化能研究

以六水合硝酸钴和酞酸丁酯为主要原料,乙二胺四乙酸(EDTA)为络合剂,用溶胶-凝胶法制备出CoTiO3纳米晶.用差热-失重热分析(TG-DSC)、X-射线衍射(XRD)、透射电子显微镜(TEM)等测试手段,对凝胶前驱体及产物进行了表征.研究了煅烧温度、前驱体pH值对产物组成和结构形貌的影响,并用Kissinger法计算CoTiO3纳米晶的表观活化能.结果表明:溶胶pH值为2.0～4.0,凝胶经700℃煅烧2h,获得均匀分布的CoTiO3纳米晶、平均粒径约50 nm.CoTiO3纳米晶的表观活化能为80.43 kJ/mol.     

纳米碳酸钙基浅色导电粉的制备及性能研究

以纳米碳酸钙为核体,用聚电解质对其表面改性后,采用均相共沉淀法制备了锡掺杂氧化铟(ITO)包覆的碳酸钙基浅色导电粉.通过改变聚电解质层数、ITO的包覆量及煅烧时间等实验条件,探究了制备纳米碳酸钙基浅色导电粉的最佳条件.用X-射线粉末衍射仪、扫描电子显微镜、X-射线电子能谱以及粉末电阻率测试仪等对样品的结构、形貌、化学组成及电阻率等进行分析.结果表明:聚电解质层数为5层,CaCO3与ITO的质量比为6∶1,500℃煅烧4.5h制备的粉末具有最佳的导电性能,其电阻率为3.8×103 Ω·cm.     

分等级结构氧化镍花状微球的制备及其机理研究

以六水合硝酸镍为原料,采用简易溶剂热法制备了具有分等级结构的氧化镍纳米片-花状微球.采用X-射线衍射(XRD)、扫描电镜(SEM)和高分辨率透射电镜(HR-TEM)、傅立叶变换红外光谱(FT-IR)等测试技术对其物相形貌进行分析表征.结果表明:在脲素存在条件下,利用醇热法可以合成花状碱式硝酸镍前驱体,在经400℃热处理2h后,形成了由薄片组成的花状微球,并且由于二次结晶过程,在原来的球体表面形成了扇面状平滑单晶薄片,厚度约为几十纳米.整个晶体生长过程,出现了溶解-再结晶的现象,即可以通过溶解-再结晶的过程来实现对氧化镍微观形貌的调控;并初步探讨了这种具有分等级结构的纳米片-花球结构的形成机理.     

超细Si/SiOx纳米线和纳米花等离子体辅助生长及光致发光

采用等离子体辅助直流弧光放电技术,以Si粉和SiO2粉为反应原料,制备了不同形貌的超细Si/SiOx纳米线和纳米花.通过X射线衍射(XRD)、透射电子显微镜(TEM)、能量色散X射线光谱(EDS)对Si/SiOx纳米线的形貌和组分进行表征与分析.Si/SiOx纳米线紫外可见吸收光谱证实了样品的光学带隙为4.58 eV.Si/SiOx纳米线光致发光光谱(PL)表明其在305 nm、495 nm处有较强的发光峰,具有良好的发光性能.     

The crystal structure and chemistry of several palygorskite samples with different geneses

The structure, chemical composition, and properties of palygorskites from several deposits in the Russian Federation, Ukraine, Uzbekistan, and Slovakia have been investigated by transmission electron microscopy, microanalysis, X-ray diffraction, IR spectroscopy, and thermal analysis. It is shown that the palygorskites formed under different physicochemical conditions may significantly differ in chemical composition, morphology, and defect structure. Depending on the formation conditions, palygorskites decompose differently upon heating.     

Effect of nanosized titania on the structure and properties of the composites based on butadienenitrile rubber

Nanocomposites based on butadienenitrile rubber (butadiene copolymer with 28% acrylonitrile) with functional titania nanoparticles of different nature have been obtained, and their complex study by X-ray diffractometry, small-angle X-ray scattering, scanning electron microscopy, electron probe X-ray microanalysis, and X-ray energy-dispersive spectroscopy has been performed. Differences in the morphology and composition of the surface and transverse cuts of nanocomposites in dependence of nanoparticle characteristics are established. It is found that the nanocomposites with the largest crystallite sizes have the lowest viscosity. It is also revealed that the nature of titania nanoparticles barely affects the vulcanization kinetics, and that the optimal vulcanization time for the composites is 25 min. Uniaxial extension tests have shown that nanocomposites with the best properties can be fabricated by introducing amorphous titania into the polymer (butadienenitrile rubber).     

Methods of chemical and phase composition analysis of gallstones

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.     

A HREM study of CdSe-glass coloration

The mechanism of coloration in CdSe-glass was investigated by HREM (high resolution electron microscopy) and microanalysis of X-ray dispersive spectroscopy. The results indicate that the colorations of CdSe-glass arise from both non-crystalline and crystalline forms of the CdSe particles.     

Electron microscopy methods in studies of cultural heritage sites

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.     

Spontaneous growth of single crystals of various shapes in tin-fullerite films

Changes in the structure and elemental and phase compositions of tin-fullerite films after their storage in air are investigated by X-ray diffraction, scanning electronic microscopy, atomic force microscopy, X-ray spectroscopic microanalysis, and Auger electron spectroscopy. Formation of the new phase Sn_xC₆₀, whisker tin and Sn_xC₆₀ crystals, and petal and flowerlike fullerite crystals under the action of internal stress is established.     

结晶β-C3N4薄膜的制备和特性研究

用电子回旋共振等离子体化学汽相沉积(ECR CVD)法, 在单晶硅(100)衬底上沉积生长出了具有{221}结构特性的连续的结晶态β-C3N4薄膜.使用扫描电镜(SEM)观测了沉积薄膜的形态;采用X射线光电子光谱(XPS),X射线衍射(XRD)和拉曼散射表征薄膜的结构.研究表明,沉积结晶态β- C3N4薄膜具有{221}结构特性.     

SiCN薄膜在Si衬底上的沉积

本文采用微波等离子体化学气相沉积(MPCVD)系统,在单晶Si衬底上制备出了SiCN薄膜.所采用的源气体为高纯CH4和N2,而Si源来自于Si衬底、SiH4和Si棒.用场发射扫描电镜(SEM)、X射线光电子能谱(XPS)和X射线衍射谱(XRD)对样品进行了表征与分析.结果表明,外加Si源、高的衬底温度、高流量N2有助于提高样品的成膜质量.所得到SiCN样品是新型的六方结构三元化合物.     

一维ZnE(E=S,Se)网状微米晶须的化学气相合成及生长机理研究

以Zn粉为原料,在CuE(E=S, Se)微米球的辅助下,采用化学气相沉积(CVD)法在Si衬底上成功制备出微米级ZnE(E=S, Se)网状晶须.用XRD,EDS,SEM和PL谱分别对产物的结构、成分、形貌和结晶质量进行了测试和分析.结果表明:生长的ZnS和ZnSe微米晶须均为立方闪锌矿结构,长度达300 μm以上,具有接近理想化学计量比的成分和较高的结晶质量.ZnE微米晶须的生长符合氧化还原反应下的气-液-固生长机制,Cu3Zn合金充当了实际的微米晶须生长催化剂,在晶须生长过程中Cu3Zn合金汇聚在一起使ZnE微米晶须形成交叉网状结构.     

Electron microscopy study of the microstructure of Ni–W substrate surface

The surface microstructure of Ni–W alloy tapes, which are used as substrates to form films of high-temperature superconductors and photovoltaic devices, has been studied. Several samples of a Ni₉₅W₅ tape (Evico) annealed under different conditions were analyzed using scanning electron microscopy, energy-dispersive X-ray microanalysis, electron diffraction, and electron energy-loss spectroscopy. NiWO₄ precipitates are found on the surface of annealed samples. The growth of precipitates at a temperature of 950°С is accompanied by the formation of pores on the surface or under an oxide film. Depressions with a wedge-shaped profile are found at the grain boundaries. Annealing in a reducing atmosphere using a specially prepared chamber allows one to form a surface free of nickel tungstate precipitates.