电子辐照诱发固态相变导致的氮化硼纳米结构生长

报道了N+离子轰击产生的氮化硼(BN)纳米结构,及在电子辐照时结构演化的高分辨透射电子显微镜的原位测定结果.应当强调的是,这种类富勒烯和发夹结构的演化,实际上是电子辐照诱发固态相变的发展,观察中发现的一些BN颗粒、卷曲物,可以被认为是类富勒烯等纳米结构形成的前体或早期阶段.提出了一种类富勒烯等结构的电子辐照动力学模型,并进行了讨论. 关键词： 氮化硼 电子辐照 透射电子显微镜 氮化硼纳米形成物     

竹节状α-Fe2O3纳米棒的制备、表征和性能研究

以硝酸铁为铁源,氨水为沉淀剂,聚乙二醇(PEG)为分散剂,采用共沉淀法制备氢氧化铁前驱体,然后将获得的前驱体在450℃、氮气保护下热处理2 h,最后利用透射电镜、X射线衍射、拉曼光谱和近边X射线精细结构光谱(NEXAFs)表征样品的形貌和结构,并使用HH-50型振动样品磁强计测量样品在室温下的磁学行为.透射电镜结果显示,获得的样品由氧化铁纳米颗粒和竹节状氧化铁纳米棒组成,纳米颗粒的粒径范围为50～100 nin,纳米棒的直径大约为10 nin.XRD表征显示样品中氧化铁纳米棒和纳米颗粒为赤铁矿型α-Fe2O3;光谱实验结果证实了样品中氧化铁纳米颗粒和纳米棒的结构是α-Fe2O3;磁学性能测试表明获得的样品表现为典型铁磁性材料的磁滞回线,其饱和磁感应强度约为64.65 emu·g-1,矫顽力的大小约为15.13 Oe.     

SDBS对氧化铜纳米颗粒悬浮液粘度的影响

由氧化铜纳米颗粒、分散剂和水组成的悬浮液粘度是研究其流动与换热的重要基础数据。本文通过实验得出分散剂是影响纳米悬浮液粘度的决定性因素这一结论。研究表明,本文采用的纯分散剂溶液即十二烷基苯磺酸钠(SDBS)水溶液的粘度对温度变化很敏感,氧化铜纳米颗粒质量分数的增加对粘度的影响并不明显,而分散剂浓度对粘度的影响远远超过纳米颗粒质量分数对粘度的影响。     

大气可吸入肺纳米颗粒的SEM及X射线微分析研究

以大气中可吸入肺纳米颗粒为研究对象,利用场发射扫描电子显微镜(FSEM)和X射线能谱仪对其形态和常量组分进行了系统研究。研究结果表明:大气可吸入物中的纳米颗粒大多为类球与椭球形,表面较为光滑,结构紧密,较小的纳米颗粒聚集成团呈松散絮状,粒度大小约在30~100 nm之间,纳米颗粒物中含有的常量元素同大颗粒污染物基本一致,主要含有C,O,Al,Si,Na,Mg,K,Ca,Fe,S,Cl等元素,能量色谱仪(EDS)的点分析研究证实一些纳米颗粒物中Cl和S元素的含量明显增大,而另一些颗粒主要为C和O元素,分析其原因,认为主要是气溶胶在形成过程中,以纳米无机灰尘颗粒为中心表面吸附了大气污染物中的有机排放物所致,从而形成了具有核壳结构的纳米颗粒污染物。因此,减少人为有机污染物的排放,对于减少可吸人肺有害纳米颗粒的形成具有很大的影响。     

Gd_2O_3:Eu纳米晶的制备及其光谱性质研究

以EDTA为络合剂,聚乙二醇为有机分散剂,用络合溶胶-凝胶法制备出Gd_2O_3:Eu纳米晶。用XRD,SEM,X-射线能量色散谱仪(EDS),荧光分光光度计等分析手段对Gd_2O_3:Eu的纳米晶结构、形貌、组分的均匀性以及发光特性进行了研究。结果表明:EDTA-M凝胶仅在800℃焙烧即可得到颗粒细小、组分均匀、纯立方相的Gd_2O_3:Eu纳米晶,颗粒基本呈球形,粒径为30nm左右。对样品的激发光谱、发射光谱测定表明:Gd_2O_3:Eu纳米晶在269nm光激发下发红光,发射光谱谱峰在611nm,与体材料基本相同;激发光谱中电荷迁移带(CTB)明显红移,从体材料的255nm移至269nm,移动了约14nm;猝灭浓度从体材料的6％提高到8％。     

纳米冷冻油的分散稳定性和黏度实验研究

本文以纳米冷冻油为研究对象,通过沉降观察和分光透射比实验对几种非离子表面分散剂进行了优选,研究发现,当分散剂的亲水亲油平衡值在3～6范围时效果最佳。分散剂浓度对纳米冷冻油的稳定性影响较大,随着分散剂浓度的增加,纳米冷冻油的分散越稳定。在小配比分散剂浓度下,分散剂的加入对纳米冷冻油的黏度影响很小。利用TiO_2纳米冷冻油的黏度实验数据,比较了几种纳米流体黏度模型,并拟合了TiO_2纳米冷冻油的黏度公式,通过黏度公式预测TiO_2纳米颗粒团聚体的直径为原始颗粒的14.4倍。     

Gd2O3:Eu纳米晶的制备及其光谱性质研究

以EDTA为络合剂，聚乙二醇为有机分散剂，用络合溶胶—凝胶法制备出Gd2O3:Eu纳米晶。用XRD，SEM，X—射线能量色散谱仪(EDS)，荧光分光光度计等分析手段对Gd2O3:Eu的纳米晶结构、形貌、组分的均匀性以及发光特性进行了研究。结果表明：EDTA—M凝胶仅在800℃焙烧即可得到颗粒细小、组分均匀、纯立方相的Gd2O3:Eu纳米晶，颗粒基本呈球形，粒径为30nm左右。对样品的激发光谱、发射光谱测定表明：Gd2O3:Eu纳米晶在269nm光激发下发红光，发射光谱谱峰在611nm，与体材料基本相同；激发光谱中电荷迁移带(CTB)明显红移，从体材料的255nm移至269nm，移动了约14nm；猝灭浓度从体材料的6％提高到8％。     

用软刻蚀方法制备PbS纳米晶复合聚丙烯酸微图形

利用软刻蚀方法制备了包裹有硫化铅纳米颗粒的聚丙烯酸微图形 .首先通过毛细微模塑法制备了丙烯酸铅的微条纹 ,并使之在γ射线引发下固态聚合 ,最后用硫化钠溶液处理聚合物微条纹 ,将铅离子转化为包埋在聚合物体系中的硫化铅颗粒 ,得到了包裹有硫化铅纳米颗粒的高清晰度的聚丙烯酸微图形 .利用X射线衍射(XRD)、X射线光电子能谱仪 (XPS)、透射电镜 (TEM)对其结构和性质进行了表征 .结果表明包埋在聚合物体系中的PbS颗粒直径小于 2 0nm .     

电化学方法制备ZnO纳米颗粒掺杂类金刚石薄膜及其场发射性能研究

采用液相电化学沉积技术制备了ZnO纳米颗粒掺杂的类金刚石(DLC)薄膜, 研究了ZnO纳米颗粒掺杂对DLC薄膜场发射性能的影响. 利用X射线光电子能谱、透射电子显微镜、Raman光谱以及原子力显微镜分别对薄膜的化学组成、 微观结构和表面形貌进行了表征. 结果表明: 薄膜中的ZnO纳米颗粒具有纤锌矿结构, 其含量随着电解液中Zn源的增加而增加. ZnO纳米颗粒掺杂增强了DLC薄膜的石墨化和表面粗糙度. 场发射测试表明, ZnO纳米颗粒掺杂能提高DLC薄膜的场发射性能, 其中Zn与Zn+C的原子比为10.3%的样品在外加电场强度为20.7 V/μm时电流密度达到了1 mA/cm². 薄膜场发射性能的提高归因于ZnO掺杂引起的表面粗糙度和DLC薄膜石墨化程度的增加.     

氮对类金刚石薄膜的微观结构内应力与附着力的影响

采用原子力显微镜(AFM)、俄歇电子能谱(AES)和显微压痕分析等手段对射频等离子体增强化学气相沉积法制备的掺氮类金刚石(DLC：N)薄膜的微观结构和力学性能进行了研究.结果表明,随着含氮量的增加,DLC薄膜的AFM表面形貌中出现了几十纳米的颗粒,原子侧向力显微镜和AES分析表明这种纳米颗粒是x大于0.126的非晶氮化碳CN_x结构.这种非晶DLC/CN_x的纳米复合结构,减小了薄膜的内应力,从而提高了薄膜与衬底的附着力. 关键词： 类金刚石碳膜 微观结构 附着特性     

Synthesis and characterization of MoO<Subscript>3</Subscript> nanostructures by solution combustion method employing morphology and size control

Molybdenum oxide nanostructures were synthesized utilizing the solution combustion method where the ammonium molybdate powder and an organic additive were used as precursors. Different organic additives including ethylene diamine tetra-acetic acid (EDTA), polyethylene glycol 200 (PEG 200), sorbitol and urea were used as surfactants in order to investigate the effect of additive structure on morphology and particle size of products. Also various reaction parameters such as the additive/Mo molar ratio, concentration of metal ion in solution, pH of the reaction, and temperature of the synthesis media were changed to study effects on product morphology and size. Outcomes were characterized by Scanning Electron Microscopy (SEM), X-ray diffraction, and Transmission Electron Microscopy (TEM) techniques. Results show a variety of MoO₃ nanoparticles and nanorods produced within the size range of 10–80 nm. Furthermore, microrods and microsheets were also obtained through this method whose length varied in the order of microns.     

基于硫蒸气处理转移的单层二硫化钼的荧光增强

采用化学气相沉积法在SiO2/Si衬底上制备了单层MoS2,再通过300℃硫蒸气处理用聚甲基丙烯酸甲酯(Polymethyl Methacrylate,PMMA)转移下的单层MoS2.使用原子力显微镜、真空荧光检测和拉曼光谱等手段表征了样品的形貌和光致发光性能.结果表明:经过硫蒸气处理转移后的单层MoS2的光致发光强度比由化学气相沉积法制备的未处理的单层MoS2的光致发光强度增强了约5倍.光致发光强度增强是由于在硫蒸气处理过程中,单层MoS2的部分硫空位被硫原子纳米团簇所填补,从而提高了光致发光效率.此外,分别将单层MoS2转移到SiO2/Si衬底、石英、三氧化铝及氟化镁衬底再经过硫处理后,也观察到了类似的荧光增强现象.     

Preparation of metal–ceramic composites by sonochemical synthesis of metallic nano-particles and in-situ decoration on ceramic powders

Copper and nickel nanoparticles were synthesized using reducing agents in the presence of direct high energy ultra-sonication. The metallic nanoparticles were decorated on various ceramic substrates (e.g. α-Al₂O₃, and TiO₂) leading to metal reinforced ceramics with up to 45% metallic content. Different parameters, such as the amount of precursor material or the substrate, as well as the intensity of ultrasound were examined, in order to evaluate the percentage of final metallic decoration on the composite materials. All products were characterized by means of Inductively Coupled Plasma Spectroscopy in order to investigate the loading with metallic particles. X-ray Diffraction and Scanning Electron Microscopy were also used for further sample characterization. Selected samples were examined using Transmission Electron Microscopy, while finally, some of the powders synthesized, were densified by means of Spark Plasma Sintering, followed by a SEM/EDX examination and an estimation of their porosity.     

Corrosion behaviour of sintered NdFeB coated with Al/Al2O3 multilayers by magnetron sputtering

Al/Al₂O₃ multilayers were deposited on sintered NdFeB magnets to improve the corrosion resistance. The amorphous Al₂O₃ films were used to periodically interrupt the columnar growth of the Al layers. The structure of the multilayers was investigated by Scanning Electron Microscopy (SEM) and High Resolution Transmission Electron Microscopy (HRTEM). It was found that the columnar structure was effectively inhibited in the multilayers. Subsequent corrosion testing by potentiodynamic polarization in 3.5 wt.% NaCl and neutral salt spray test (NSS) revealed that the Al/Al₂O₃ multilayers had much better corrosion resistance than the Al single layer. Furthermore, for multilayers with similar thickness, the corrosion resistance was improved as the period decreased.     

Generating porosity in metal oxides thin films through introduction of polymer micelles

The generation of porosity in Nb₂O₅ sol–gel films through introduction of polymer micelles of commercially available copolymer Pluronic PE6800 [poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol)] was studied using direct observation of film morphology by Transmission Electron Microscopy and indirect calculations of free volume fraction by optical means. Mesoporous Nb₂O₅ films were deposited by the sol–gel and spin-coating methods and templated with aqueous solutions of Pluronic PE6800 with concentrations below and above critical micelle concentration determined by the modified dye solubilization method. The influence of the duration of the postdeposition annealing on total pore volumes was investigated by reflectance measurements and consequent calculation of optical properties and free volume fraction by Bruggeman effective medium theory. The possible application of the films in optical sensing of vapors has been demonstrated through reflectance measurements prior to and after acetone vapors exposure.     

Oriented Growth of Nanocrystalline Gamma Ferric Oxide in Electrophoretically Deposited Films

Films of nanocrystalline γ-Fe₂O₃ were deposited on silicon substrates by using the technique of electrophoretic deposition. The precursor powder was nanocrystalline γ-Fe₂O₃, which was synthesized, using DC arc plasma in the oxygen ambient by vapour–vapour interaction in gas phase condensation; at a stabilized arc current of 40 A. This powder was characterized by X-ray diffraction, Transmission Electron Microscopy, Vibrating Sample Magnetometer and Mössbauer Spectroscopy. An increase in directional coercivity was observed in case of films deposited on silicon substrates, which is dramatically significant. Preferred orientation of almost similar sized nanocrystalline magnetic domains in deposited films is evident from the results of X-ray diffraction and Transmission Electron Microscopy results. The preferred alignment of the nanocrystallites seems to be responsible for the significant changes observed in magnetic properties of films.     

Switching of hydrophilic to ultra hydrophilic properties of flower-like gold nanostructures

Flower-like morphologies of gold nanostructures were obtained via chemical method by controlling molar concentration ratio of reducing agent and precursor. Chloroauric acid was used as a metal precursor while tri-sodium citrate as the reducing agent. These flower-like structures were characterized by UV-vis spectroscopy, Scanning Electron Microscopy (SEM) and X-ray Diffraction (XRD) techniques. The basic crystallite size calculated via XRD measurement was found to be ∼10 nm and remain unaffected by the different concentration ratios. The coating of these structures was made over clean glass substrate and analyzed for wettability by measuring their water contact angles. Our analysis indicates that the coatings of hierarchical flower-like structures of gold are able to provide ultra hydrophilic properties to glass substrate.     

Densification and nanocrystallisation of sol-gel ZrO 2 thin films studied by surface plasmon polariton-assisted Raman spectroscopy

Very thin ZrO ₂ films (few nanometers) have been prepared by sol-gel process. These films were deposited onto a stack of a thin silver layer evaporated on a glass substrate for Surface Plasmons Resonance (SPR) experiments. The first aim of this work is to study the high densification of the sol-gel films followed by the refractive index and thickness accurate measurements at each step of the annealing procedure, using an optical set-up based on SPR. Secondly, SPR excitation coupled with micro-Raman experiment has also been performed to determine the thin films structure depending on layer thickness. Finally, Conventional Transmission Electron Microscopy (CTEM) and High Resolution (HRTEM) studies have been conducted to check and complete Raman spectroscopy results. A discussion compares the optical results and the Transmission Electron Microscopy observations and shows that ultra thin layers structure is strongly depends on films thickness. Received 14 May 2001 and Received in final form 2 January 2002     

掺镧TiO2纳米薄膜材料的制备与光催化性能研究

用溶胶-凝胶法研究了掺镧TiO_2纳米薄膜材料。在钛醇盐溶液前驱体中,通过提拉方式镀膜在玻璃上,从而形成自净玻璃。论文对不同的掺镧量、不同的聚乙二醇加入量以及不同镀膜次数的TiO_2材料的透光性、光催化降解性分别进行了测试和研究,并对相关机理进行了探讨。研究表明:对于单层膜的TiO_2材料,掺镧与不掺镧对透光性的影响不大,但掺镧后光催化活性大大提高;对于单层膜的TiO_2材料,随着聚乙二醇的增多,透光率整体呈下降趋势,催化活性先增加后减小。对于多层膜的TiO_2材料,随着层数增加,在紫外光区,透光性变化不大,在可见光区,透光性有所下降。在两层膜后,层数的增多对催化活性影响不大。由实验知:在100mL基体溶液中,当掺入0.5gLa(NQ_3)_3·nH_2O,加入0.2g聚乙二醇,镀膜两层时,透光性好且光催化活性也高。     

Structure and electrical conduction of WO3 nanorods epitaxially grown on mica

Tunsten oxide nanorods are grown on mica substrate in air from WO₃ vapor at 590 °C. They are epitaxially oriented on the substrate in three directions according to the hexagonal symmetry of the mica. Their morphology was investigated by Atomic Force Microscopy (AFM), their structure by Electron Diffraction (ED) and High Resolution Electron Microscopy (HRTEM). The energy dispersive X-ray analysis (EDX) associated with the TEM revealed the presence of potassium in the first step of the nanostructures growth suggesting the formation of a tungsten bronze. According to their thickness the nanorods have a structure either hexagonal or monoclinic. The structural investigations showed that numerous kinds of planar defects parallel to the growth direction are formed. The electrical conduction was analyzed with a Conductive Atomic Force Microscopy (CAFM) method which allows to obtain either an image of the resistance variations along the nanorods or a current-voltage response. The result demonstrates that the WO₃ nanorods form electrically networks suitable for gas sensing experiments.