溶胶凝胶自燃烧法合成ZnS纳米颗粒及粒径控制

以硝酸锌、硫脲、乙二醇以及氨基乙酸等为原料,运用溶胶凝胶自燃烧法合成了尺寸和形貌均一性较好的ZnS多晶纳米颗粒.经X射线衍射仪、扫描电子显微镜、紫外-可见分光光度计等表征发现合成的ZnS纳米颗粒具有闪锌矿结构,其平均粒径为160nm且每个纳米颗粒均由约10nm的晶粒组成,且样品具有良好的光吸收性能,其能带带隙为3.46eV.还详细研究了前驱物中组分比例对ZnS纳米颗粒粒径分布的具体影响.研究表明前驱物中n(乙二醇)/n(氨基乙酸)是影响ZnS纳米颗粒粒径分布的主要因素.这一研究结果提供了一种基于自燃烧法的可靠的ZnS纳米颗粒合成工艺,并且实现了利用n(乙二醇)/n(氨基乙酸)独立优化纳米颗粒粒径均一性,有利于基于此工艺的功能材料设计和光电性能优化.     

FeNi/SiO2核 - 壳纳米球的制备及磁学性质

利用共沉淀结合氢气还原法制备球形核 - 壳结构的γ - FeNi/SiO2纳米复合材料.用X射线衍射(XRD)确定样品的相组成,用透射电子显微镜(TEM)观察样品的形貌,用振动样品磁强计(VSM)测定样品的磁性能.结果表明:pH值是影响核 - 壳纳米结构形貌的重要因素;pH值为9左右且还原温度为700 ℃,制备出的纳米粒子具有近似的球形核 - 壳结构:纳米颗粒是以γ - FeNi合金为核心,其平均粒径大约为80 nm,外面包覆非晶SiO2壳层的核 - 壳结构;随着SiO2质量分数增加,样品的饱和磁化强度明显下降.随着还原温度升高,纳米粒子的尺寸大小略有增加,其饱和磁化强度明显增大,但矫顽力下降,这主要归结于铁镍与铁镍氧化物界面存在交换耦合相互作用.     

沉淀法制备ZnO：Eu^3＋纳米晶及其发光性能的研究

分别以尿素、氨水作为沉淀剂,与Zn(NO3)2和Eu(NO3)3混合物反应,制备出不同尺寸的纳米ZnO:Eu3 晶.用X射线衍射仪(XRD)、扫描电子显微镜及荧光分光光度计对所制备的ZnO:Eu3 进行了分析.结果表明,以尿素为沉淀剂可以得到颗粒均匀、尺寸较小并且发光性能优良的ZnO:Eu3 纳米晶,主发射峰位置在611 nm处;随着Eu3 掺杂浓度的提高,ZnO:Eu3 粒径逐渐减小;利用均匀沉淀法(尿素为沉淀剂)制备的ZnO:Eu3 其发光性能优于直接沉淀法(氨水为沉淀剂)制备的ZnO:Eu3 .     

纳米氧化锡的制备与结构特性

采用金属醇盐羟化法制备了纳米氧化锡粉末，并研究了粉末的结构特性。这一制备纳米金属氧化物粉末的新技术具有设备与流程简单，成本低，污染小，产品纯度高，平均粒径小，颗粒均一，粉末的光电特性好等特点。     

As压调制的InAlAs超晶格对InAs纳米结构光学特性的影响

利用固源分子束外延(MBE)设备生长出InAs/InAlAs/InP(001)纳米结构材料,探讨了As压调制的InAlAs超晶格对InAs纳米结构光学特性的影响.结果表明,As压调制的InAlAs超晶格能有效地调整InAs纳米结构的形貌特性、发光峰位,改善发光线宽,提高辐射效率,从而有利于其在长波长光电器件方面的应用.     

溶剂热辅助法控制合成ZnO纳米结构及其光学性质研究

用溶剂热方法合成了znC2O4·2H2O纳米棒的中间体,在不同热处理条件下获得ZnO的玉米棒、颗粒片、链结构等不同形貌,从而实现对ZnO的形貌进行控制．室温下．ZnO在250nm的紫外光激发下,在400nm处出现一个近带发射峰．这种发光峰属于ZnO中的缺陷发光．对ZnO的形成机理做出了热重和红外分析,并对ZnO的形成机理提出了一种可能的解释．溶剂热方法获得的ZnC2O4·2H2O纳米棒在高温下分解成ZnO．在退火过程中,中间体会先形成空洞,然后形成带颗粒的纳米棒;但是这种纳米棒开始会粘接在一起形成片状,然后纳米片会卷曲成玉米棒结构,最终玉米棒散掉,形成纳米链．     

环氧树脂作还原剂制备Li3V2(PO4)3的结构和性能

采用高温固相法，以环氧树脂为还原剂合成锂离子电池正极材料Li3V2(PO4)3.通过X射线衍射分析和扫描电子显微镜对样品的晶体结构和微观形貌进行表征，并用恒电流充放电和循环伏安实验研究材料的电化学性能.结果表明所制备的Li3V2(PO4)3为结晶完善的单斜结构，颗粒分布均匀且粒径较小，0.2 C时在3.0V~4.3V电压范围的首次放电比容量为126.9 mAh/g，30次循环后的比容量为126.0 mAh/g，容量保持率达到99.29%.     

基于粒径和形貌视角下探究微乳剂是否为纳米农药

我们针对当前关于“微乳剂是不是纳米农药吗”的质疑,从粒径大小和形貌特征视角下分别对市场上常见的几种微乳剂进行研究,首次通过动态光散射激光粒度仪结合扫描电子显微镜,以前期制备的ZIF纳米农药为对照,分别测试和对比分析了微乳剂稀释不同浓度后的粒径变化和颗粒分散后的微观形貌。结果表明,常规微乳剂处于动态平衡中,不同浓度稀释后,粒径发生无规律变化,尤其在扫描电镜下观察含药液滴干燥后颗粒分布不均,有聚集、大颗粒析出现象,而纳米农药不同浓度稀释后粒径变化不大,均在1~300 nm,并且在扫描电镜下观察微观形貌也是单分散纳米状态,不会聚集。因此,单靠动态光散射测定的粒径不能判断微乳剂就是纳米农药,还需要借助电镜技术观察微观下的分散状态和粒径分布。     

熔盐法合成Yb3+、Ho3+掺杂CaBi4Ti4O15及其上转换发光温敏性研究

通过熔盐法合成了Yb³⁺、Ho³⁺共掺杂CaBi₄Ti₄O₁₅荧光粉,研究其结构、形貌、上转换荧光和荧光温度传感特性。X射线衍射结果显示,所有样品都为纯相的铋层氧化物结构,随着Ho³⁺掺杂浓度的提高,晶格收缩,引起了(119)衍射峰向高角度偏移。扫描电镜照片显示合成的粉末样品呈片状结构,长宽分布从百纳米到微米量级,厚度小于200 nm。合成的荧光粉末材料在980 nm红外激光激发下,发出明亮的可见光,其上转换发光对温度变化有明显的响应。基于归一化荧光强度的温敏发光实验结果表明,基于绿光发射带的温敏特征在488 K时有最大灵敏度0.004 97 K^-1,在583 K时有最大相对灵敏度1.01%K^-1。研究表明,熔盐法合成的具有片状结构的Yb³⁺、Ho³⁺共掺杂CaBi₄Ti₄O₁₅荧光粉在上转换荧光温度传感...     

表面活性剂对纳米氧化锌合成及分散性的影响

在比较了各种合成方法后，我们采用固相合成法来制备纳米氧化锌，并对其提出了改进．通过在固相反应过程中加入表面活性剂对纳米氧化锌进行了表面改性，制备出了粒径更小、分散性更好的氧化锌．用X-射线粉末衍射仪、扫描电镜表征产物的结构和形貌，用分光光度计研究其分散性．结果表明，改性后产物的分散性得到了显的改善，较之未改性样品，其吸光度均有不同程度的增加，且在不同极性溶剂中的分散性随表面活性剂种类和用量的不同而不同．     

Nanoengineering of inorganic and hybrid hollow spheres by colloidal templating

Hollow silica and silica-polymer spheres with diameters between 720 and 1000 nanometers were fabricated by consecutively assembling silica nanoparticles and polymer onto colloids and subsequently removing the templated colloid either by calcination or decomposition upon exposure to solvents. Scanning and transmission electron microscopy images demonstrate that the wall thickness of the hollow spheres can be readily controlled by varying the number of nanoparticle-polymer deposition cycles, and the size and shape are determined by the morphology of the templating colloid. The hollow spheres produced are envisioned to have applications in areas ranging from medicine to pharmaceutics to materials science.     

Fly ash collected from electrostatic precipitators: microcrystalline structures and the mystery of the spheres

Scanning electron micrographs demonstrate the presence of microcrystalline structures on the surface of coal-derived fly ash samples taken from electrostatic precipitator hoppers. Cenospheres (hollow spheres) were found to be packed with smaller cenospheres, which were also packed with spheres. Microspheres, apparently formed by uneven heating, are encapsulated in the parent sphere. Chemical analyses provide a basis for the postulation of a mechanism of formation for plerospheres (hollow spheres packed with spheres) and microcrystals.     

具有介孔结构的Co/SiO2空心球的制备及其催化性能研究

以二氧化硅为模板,采用牺牲模板法制备具有介孔结构的碱式硅酸钴空心球.采用扫描电子显微镜(SEM),透射电子显微镜(TEM)、X射线衍射(XRD)、氮气吸脱附曲线(BET)和程序升温还原(TPR)等方法,对样品的结构和形貌作了表征.探索了碱式硅酸钴空心球的还原规律,研究了Co/SiO2作催化剂的催化性能.结果表明,180℃下反应1 h时,碱式硅酸钴即为空心球结构;在800℃氢气气氛中反应5 h,碱式硅酸钴完全被还原为Co/SiO2,还原前后仍为空心球结构,比表面积和孔容均有所减小,孔径增大.以Co/SiO2空心球做催化剂进行硝基苯加氢催化,1 h后硝基苯的转化率为56%,比商用Raney Ni提高约14%.     

Shape-controlled synthesis of gold and silver nanoparticles

Monodisperse samples of silver nanocubes were synthesized in large quantities by reducing silver nitrate with ethylene glycol in the presence of poly(vinyl pyrrolidone) (PVP). These cubes were single crystals and were characterized by a slightly truncated shape bounded by [100], [110], and [111] facets. The presence of PVP and its molar ratio (in terms of repeating unit) relative to silver nitrate both played important roles in determining the geometric shape and size of the product. The silver cubes could serve as sacrificial templates to generate single-crystalline nanoboxes of gold: hollow polyhedra bounded by six [100] and eight [111] facets. Controlling the size, shape, and structure of metal nanoparticles is technologically important because of the strong correlation between these parameters and optical, electrical, and catalytic properties.     

CdS纳米颗粒的合成、表面修饰及光学特性研究

用一步室温固相化学反应法合成CdS纳米颗粒，并以氨催化水解法对其表面进行了修饰，得到了具有CdS／SiO2核／壳结构的纳米微球，以透射电子显微镜和X-射线衍射仪对其结构和物相进行了表征，并研究了其光致发射光谱的性质，研究结果表明：固相反应完全，产物为纯相CdS，室温固相化学反应法避免了传统湿法存在的团聚现象的缺点，具有产率高、无污染、节能等优点；而且CdS纳米颗粒表面经SiO2修饰后，其带边发射显增强，缺陷发射减弱，且在一定范围内随着SiO2包覆层厚度的增加，荧光强度增加。     

Origin of corn: pollen evidence

The origin of Indian corn remains controversial. Its closest wild relative is teosinte, with which it hybridizes freely to produce fertile progeny. Teosinte ears are smaller and simpler than those of corn. Searches for a more likely living ancestor have failed, but nine of its assumed pollen grains have been recovered in deep drillcore samples obtained from a stratum of soil under Mexico City, which is believed to antedate man in the Western Hemisphere. These nine largest grains are indistinguishable from pollen of modern corn. It has been assumed to be that of a postulated wild corn other than that of teosinte, but this does not account for the possibility that the pollen grains are those of a tetraploid teosinte-producing pollen with two sets of chromosomes. This likelihood has been examined by treating modern teosinte plants with colchicine, which induces tetraploidy. The result has been many teosinte pollen grains indistinguishable in size from modern corn. In interpreting thrs outcome it is important also to know that heat treatment of corn and other plants induces polyploidy, and that the deep drill-core pollen was recovered in a stratum of volcanic clay indicating the high temperature known to favor doubling of corn pollen volumes.     

磁性纳米颗粒在DNA分离纯化中的应用

为了解磁性纳米颗粒在DNA分离纯化中的应用,采用文献综述和归纳总结的方法,阐述了1997—2021年以铁氧化物为核心的磁性纳米材料的研究进展,同时比较了材料结构和表面相关活性官能团的修饰对DNA提取效率的影响。结果表明：1）应用磁性纳米颗粒的固相萃取有着安全无毒、操作简单、可重复使用、能够实现自动化与高通量操作等多种优势,提取DNA效率相比于商业化试剂盒也有优势。2）目前磁性纳米材料已有比较全面的研究。磁性纳米颗粒的尺寸、孔径大小、磁化强度及引入的活性官能团不同等性质均对DNA的提取效率有影响,改变这些性质研发新型且高效的功能化磁性纳米颗粒或改变磁性纳米材料的制备方法、所提取DNA的形态性质、溶液的pH或盐浓度等试验条件,以提高DNA与材料的解吸率,不断优化磁性分离过程,提高DNA分离效率和质量。3）发展高通量商业化的核酸提取程序,是磁性固相萃取可观的发展前景。4）磁性纳米颗粒除了在核酸提取中的应用,在其他生物医学应用中也有着广泛的研究。以上结果均表明磁性纳米材料有着极强的研究发展前景。     

可视化研究银纳米颗粒与柑橘类农药杀扑磷的相互作用

为检测柑橘类农药杀扑磷,选择具有独特局域表面等离子体共振吸收和散射特性的银纳米。用合成70 nm大小的银纳米颗粒结合Britton-Robinson缓冲溶液研究银纳米与杀扑磷农药的相互作用,发现银纳米颗粒与杀扑磷农药反应形成Ag-S键,检测限达0.2×10~(-6) mol/L,表明用银纳米检测杀扑磷农药是一种成本低、简捷、易操作的好办法,以期为杀扑磷农药的检测提供新的思路和基础。     

Defects in carbon nanostructures

Previous high-resolution electron microscopy (HREM) observations of the carbon nanotubes have led to a "Russian doll" structural model that is based on hollow concentric cylinders capped at both ends. The structures of the carbon nanotubes and particles were characterized here by bulk physical and chemical property measurements. The individual nanostructure is as compressible as graphite in the c axis, and such nanostructures can be intercalated with potassium and rubidium, leading to a saturation composition of "MC(8)." These results are counter to expectations that are based on a Russian doll structure. HREM after intercalation with potassium and deintercalation indicates that individual nanoparticles are a "paper-mache" of smaller graphite layers. Direct current magnetization and electron spin resonance measurements indicate that the electronic properties of the nanostructures are distinctly different from those of graphite. Although the nanostructures have distinct morphologies and electronic properties, they are highly defective and have a local structure similar to turbostratic graphite.