Magnesium oxide nanocrystals via thermal decomposition of magnesium oxalate

The present work reports the synthesis of magnesium oxide (MgO) nanocrystals via a thermal decomposition route and the study of physicochemical properties of products. The MgO nanocrystals were prepared from magnesium oxalate powders as precursor. Transmission electron microscopy (TEM) analysis demonstrated MgO nanocrystals with an average diameter of about 20−25 nm. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electronic diffraction (SAED), and Fourier transform infrared (FT-IR) spectroscopy. Optical absorption and photoluminescence emission properties of MgO nanocrystals were investigated.     

物理分析技术在无机氧化物晶体结构表征中的应用

以氯化锌和氢氧化钠为主要原料,采用简单液相法,通过改变反应液的组成,制备出了针状、棒状、片状和花状四种不同形貌的ZnO微/纳米晶体。应用X-射线粉末衍射仪（XRD）,扫描电子显微镜（SEM）、高分辨透射电子显微镜（HRTEM）及选区电子衍射仪（SEAD）对产物进行表征,获得了ZnO物相、形貌与微观结构的重要信息。     

Direct ultrasonic-assisted synthesis of sphere-like nanocrystals of spinel Co3O4 and Mn3O4

A simple sonochemical method was developed to synthesize uniform sphere-like or cubic Co(3)O(4) and Mn(3)O(4) nanocrystals by using acetate salts and sodium hydroxide or tetramethylammonium hydroxide (TMAH) as precursors. Influence of some parameters such as time of reaction, alkali salts, and power of the ultrasound and the molar ratio of the starting materials on the size, morphology and degree of crystallinity of the products was studied. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), FTIR spectroscopy, Thermal gravimetry analysis and differential thermal analysis (TGA/DTA) were used to characterize the nanocrystals.     

溶剂热再结晶合成由纳米颗粒自组装成的一维CdS纳米棒

采用两种不同的溶剂热路径合成出了不同形貌和尺寸的CdS纳米晶, 一种是以无水乙二胺(en) 为溶剂, CdCl₂·2.5H₂O和硫脲(H₂NCSH₂N) 为镉源和硫源, 在不同反应温度(160 ℃-220 ℃ 下制备出了CdS纳米晶, 讨论温度对CdS纳米晶生长的影响; 另一种是以en为溶剂, 将在160 ℃下合成的产物在200 ℃下原位再结晶生长2-8 h, 分析原位生长时间对CdS纳米晶生长的影响. 通过X射线衍射(XRD)、 扫描电子电镜(SEM) 和透射电子电镜(TEM) 等表征产物的物相、 形貌和微结构, 分析可知: 两种路线合成的产物均为六方相CdS; 当温度为160 ℃时, 产物形貌为纳米颗粒状, 当温度高于160 ℃时, 产物为CdS纳米棒状; 同时, 在200 ℃下原位再结晶生长不同时间后发现产物形貌由纳米颗粒转变为纳米棒, 通过场发射扫描电镜(HRTEM) 分析可知: 纳米棒是由零维纳米颗粒自组装而成. 最后, 讨论了影响产物CdS纳米晶形貌转变的因素和纳米棒的生长机理.     

Barium molybdate and barium tungstate nanocrystals synthesized by a cyclic microwave irradiation

BaMoO₄ and BaWO₄ nanocrystals were synthesized from Ba(NO₃)₂ and Na₂MeO₄ (Me=Mo and W) solutions using 50% of 600 W microwave irradiation for 20 min. The products were characterized using X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), selected area electron diffraction (SAED) and photoluminescence (PL) spectrophotometry. They show that the products are good dispersed nanocrystals (poly-nanocrystals) of single-phase scheelite tetragonal structure with the vibration modes corresponding to the molybdate and tungstate compounds. Their photoluminescence was detected at 415 and 392 nm for BaMoO₄ and BaWO₄, respectively.     

Hydrothermal synthesis and optical characteristics of Eu in Zn2SnO4 nanocrystals

Zn₂SnO₄:Eu³⁺ nanocrystals were one-step synthesized by hydrothermal method for the first time. All the products were systematically characterized by powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron probe X-ray microanalyzer (EPMA), photoluminescence (PL) and photoluminescent excitation (PLE). The characteristic peak of Eu³⁺-doped in Zn₂SnO₄ nanocrystals was also detected. The luminescent properties of blank and Eu³⁺-doped Zn₂SnO₄ nanocrystals were reported.     

爆轰法合成碳包覆镍纳米颗粒的研究

 采用自制的负氧平衡复合炸药前驱体,在密闭容器中充氮气保护下爆轰合成了碳包覆镍纳米颗粒。利用X射线衍射、X射线荧光、透射电镜和拉曼光谱等技术,对爆炸产物的组成成分、结构形貌等进行了观测。结果表明,爆轰产物主要由具有面心立方结构的镍晶核和碳元素构成,此外还含有其它微量元素;合成的纳米颗粒呈球形或椭球形状,颗粒尺寸主要分布在10~25 nm范围,包覆的碳壳厚度约1~2 nm,核壳结构完备。结合观测结果,对爆轰法合成碳包覆纳米颗粒的形成机制进行了简单的讨论。     

PEI/CeF3 : Tb3+纳米晶体的简易合成及荧光特性

用水热法制备了PEI/CeF₃ : Tb³⁺纳米晶体,运用透射电子显微镜,X射线衍射,傅立叶变换近红外光谱,对样品进行了表征。结果表明:所得纳米晶体平均粒径为10 nm,呈比较规则的立方体形;纳米晶体表面包覆有PEI,因而具有较好的水溶性和潜在的生物应用价值。我们给出了该纳米晶体的荧光激发谱与发射谱,详细说明了各发光峰对应能级的跃迁及其发光机理,分析了不同掺杂浓度对其荧光强度的影响。结果表明:所制备的纳米晶体在紫外光激发下,显示出明亮的绿色荧光。当Tb³⁺离子掺杂摩尔分数20%左右时,样品的荧光强度达到最大值。     

Ultrasonic-assisted size-controllable synthesis of Bi2Te3 nanoflakes with electrogenerated chemiluminescence

Bi(2)Te(3) hexagonal nanoflakes with controllable edge length ranging from approximately 150 nm to as small as approximately 10nm were synthesized via an ultrasonic-assisted disproportionation route, using Te powder and Bi(NO(3))(3).5H(2)O as raw materials. The mechanochemical effects of the ultrasonic irradiation accelerated the reaction and were helpful to obtain relatively small and uniform nanocrystals. The products were characterized by X-ray powder diffraction, X-ray photoelectron spectra, transmission electron microscopy, and selected area electron diffraction techniques. Electrogenerated chemiluminescence of as-prepared Bi(2)Te(3) was also reported for the first time.     

Controllable synthesis and characterization of CuO, β-Ni(OH)2 and Co3O4 nanocrystals in the MCln-NH4VO3-NaOH system

In this study, we demonstrate a general but efficient solution-phase approach for preparing CuO, β-Ni (OH)₂ and Co₃O₄ nanocrystals selectively by simply adjusting the amount of NaOH in the reaction system of MCl_n-NH₄VO₃-NaOH. The experimental results revealed that the amount of NaOH is crucial in the formation of desirable products. The as-obtained nanocrystals were characterized by means of X-ray powder diffraction, transmission electron microscope, high resolution transmission electron microscope, selected area electron diffraction and electrochemical techniques. The as-prepared CuO are nanorods with 15 nm in diameter and 50 nm in length. The as-prepared Ni (OH)₂ nanocrystals have the flocculent feature and Co₃O₄ nanocrystals are composed of irregular particles. It should be pointed out that some traditional metal vanadates occur in these reaction systems, which were usually prepared by the solid-state routes. On the other hand, the electrochemical properties of the obtained products were studied in brief. Electrochemical performances of CuO, β-Ni (OH)₂ and Co₃O₄ nanocrystals were measured with Li metal as the reference anode, which indicates their excellent capacities of Li-deposited for Li-ion batteries.