沉淀法制备钨酸铅微晶及形成机理研究

以硝酸铅和钨酸钠为原料,以聚乙二醇400为分散剂,采用沉淀法制备出不同形貌的钨酸铅微晶.采用X射线衍射(XRD)、扫描电镜(FESEM)测试、能量分散光谱(EDS)、荧光光谱(PL)对样品进行了表征.结果表明:在80℃烘干后,得到结晶性能良好的纯相PbWO4;随着聚乙二醇-400量的增加,钨酸铅微晶形貌由塔状变向梭子状转变,且分散性良好、无团聚发生;PbWO4微晶在350 ～ 650 nm范围内具有较宽的发射谱带,由三组主要的发光峰构成,分别在430 nm、465 nm左右的蓝色发光峰和560 nm左右的弱的黄绿色发光峰.最后研究了PEG-400在PbWO4微晶生长阶段的控制作用,并提出了PbWO4有序微晶结构的形成机理.     

钨酸锌微纳米材料的水热合成及发光性能研究

以Zn(NO3)2·6H2O和Na2WO4·2H2O为原料,草酸为沉淀剂,采用水热法在180℃反应4h制备了ZnWO4粉体,并考察了前驱体溶液pH值对ZnWO4发光性能的影响.通过X射线衍射(XRD),场发射扫描电子显微镜(SEM)和荧光光谱(PL)等测试手段对样品的物相、微观形貌和发光性能进行表征.结果表明:pH值为7～9时适宜合成ZnWO4粉体,pH =7、8时,得到的是星状结构ZnWO4粉体;pH =9时分别得到的是由长度为500 nm,直径为100 nm的纳米棒交叉组装而成的镂空结构ZnWO4粉体.相比之下,由纳米棒交叉组装而成的镂空片的发光性能最佳.     

钇掺杂多孔结构氧化锌纳米棒的制备与性能研究

采用两步法在二氧化锡掺氟(SnO2:F,FTO)导电玻璃基板上制备出钇(Y)掺杂多孔结构氧化锌(ZnO)纳米棒,首先利用浸渍-提拉法在FTO导电玻璃基板上制备ZnO晶种层,然后利用水热法在ZnO晶种层上生长Y掺杂ZnO纳米棒.研究了不同浓度Y掺杂ZnO纳米棒的晶相结构、微观形貌、化学组成及光学性能.实验结果表明:所制备的Y掺杂ZnO纳米棒为沿c轴择优取向生长的六方纤锌矿结构,随着Y掺杂浓度的增加,ZnO纳米棒(002)衍射峰强度先增大后减小,纳米棒的平均长度由1.3μm增加到2.6μm.ZnO纳米棒的形貌由锥状结构向柱状结构演化,纳米棒侧面的孔洞分布密度增加.所制备的Y掺杂ZnO纳米棒具有一个较弱的紫外发光峰和一个较强的宽可见发光峰.所制备样品的光学带隙随着Y掺杂浓度的增加而减小,其光学带隙在3.29～3.21 eV之间变化.利用Y掺杂ZnO纳米棒作为量子点敏化太阳能电池的光阳极可极大提高太阳电池的光电转换效率.     

大尺寸PWO:(Mo,Y)晶体发光均匀性的研究

报道了用改进的Bridgman法生长的大尺寸PbWO4:(Mo,Y)晶体发光均匀性的表征研究.通过对大尺寸的PbWO4:(Mo,Y)晶体不同部位的透射光谱、X射线激发发射光谱、光产额和抗辐照损伤能力等光学和闪烁性能的测试,结果表明在实验所涉及的掺杂浓度范围,Mo、Y双掺杂能显著改善PbWO4晶体的发光均匀性,增强其抗辐照损伤能力.     

CoC2O4·2H2O纳米晶形貌可控合成

通过简单调节反应介质热塑性酚醛树脂与乙二醇配比,选择性地制备了CoC2O4·2H2O纳米棒和纳米片晶体或其两种形貌晶体混合物.样品热重和差示扫描量热(TG-DSC)、X射线粉体衍射(XRD)、场发射扫描电镜( FESEM)实验表明:以热塑性酚醛树脂为反应介质得到了COC2O4·2H2O纳米棒;以乙二醇为反应介质得到了CoC2O4·2H2O纳米片;逐渐增大乙二醇和酚醛树脂质量比,实现了CoC2O4·2H2O形貌由纳米棒形貌转变为纳米片形貌.基于不同晶体形貌和实验结果,提出了棒状和片状COC2O4·2H2O可能的形成机理模型以解释两种形貌COC2O4·2H2O纳米晶的生长行为.     

NaF、LiF掺杂钨酸铅晶体的性能研究

采用坩埚下降法生长了NaF、LiF掺杂钨酸铅(PbWO4)晶体,研究了掺杂晶体的透射光谱、光产额和X射线激发发射谱等发光性能.结果表明:与未掺杂PbWO4晶体相比,NaF掺杂可以显著提高PbWO4晶体在350nm附近的透过率,其X射线激发发射谱中出现新的发光峰;而LiF掺杂引起了晶体可见光范围内的强烈吸收,造成PbWO4晶体光产额的显著下降.基于影响PbWO4晶体闪烁性能的原因分析,提出了采用其它价态金属氟化物掺杂来提高PbWO4晶体光产额的新思路.     

Co掺杂浓度对ZnO纳米棒结构和光学性能影响研究

采用水热法以不同浓度Co掺杂合成了具有六方纤锌矿结构的ZnO纳米粉体,通过X-射线衍射(XRD)、扫描电镜(SEM)、拉曼光谱、X射线光电子光能谱分析法(XPS)、(光致发光)PL谱等分别对样品的形貌、结构、光学性能进行了测试和表征.结果 表明:随着Co掺杂浓度的增大,纤锌矿ZnO的晶体结构没有改变,且Co以二价离子Co2+的形式掺杂进入ZnO晶格;同时花状ZnO纳米棒的均匀性变差,不同浓度Co掺杂ZnO纳米棒中均出现了少量且尺寸较小的单根纳米棒.PL光谱显示:随着Co掺杂浓度增大,样品的紫外发光峰没有明显地变化,而可见发光峰的强度先减小再增大,说明样品的缺陷先降低再提高.当Co掺杂的浓度为2.0;时,所制备的ZnO花状纳米棒可见发光峰相对最低,其具有较小的缺陷.     

PLD制备的籽晶层对ZnO纳米棒形貌及性能的影响

本文研究了脉冲激光沉积法(PLD)制备的不同籽晶层对水热生长ZnO纳米棒的形貌及发光性能的影响,通过比较得出,籽晶层是获得高度取向,排列有序的ZnO纳米棒的基础.电子回旋共振(ECR)氧等离子体参与沉积,有利于获得表面均匀且光滑平整的籽晶层,进而得到形貌及结晶质量较好的ZnO纳米棒.籽晶层的厚度不仅能够改变纳米棒的疏密程度,而且还能够改善纳米棒的取向性.通过调节籽晶层的退火温度可以调节纳米棒直径的大小,恰当的籽晶层退火温度也是获得形貌优良的ZnO纳米棒的一个关键因素.     

溶剂热法制备InP纳米球及其生长机理研究

以氯化铟(InCl3·4H2O)和白磷(P4)为反应物,硼氢化钠(NaBH4)为还原剂,在较低的反应温度下采用溶剂热法制备出了InP纳米球.利用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)和光致发光光谱(PL)对所制备产物的结构、形貌和发光性能进行了分析和表征.结果表明:在适当的温度下可以制备出尺寸为300 nm左右的纳米球,通过改变反应条件可以改变产物的尺寸、形貌.同时,从动力学方面对溶剂热法制备InP纳米球的反应机理进行了初步探讨.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.     

Fe_3O_4单晶纳米棒和量子点的水热合成与表征

本文以FeSO_4·7H_2O为铁源,采用LSS反应机制控制合成了Fe_3O_4单晶纳米棒和量子点,并根据不同反应条件下反应生成的产物形貌推断了反应机理.采用X-射线衍射仪(XRD)、透射电子显微镜(TEM)对产物进行表征.室温下分别测试了Fe_3O_4单晶纳米棒和量子点的磁滞回线,检测得到纳米棒和量子点饱和磁化强度磁化率(Ms)分别为44.26 emu/g和60.09 emu/g,矫顽力(H_c)分别为132.3 Oe和143.2 Oe.     

钨酸铅闪烁晶体的双掺杂性能研究

本文采用坩埚下降法生长出了PbWO4:(F,Er)晶体和PbWO4:(F,Nd)晶体,并且对此两种晶体透过性能和闪烁发光性能进行了测试分析.透过光谱结果显示,PbWO4:(F,Er)晶体和PbWO4∶(F,Nd)晶体在350 nm至700nm范围内的透过率比纯的钨酸铅均有较大的提高.紫外激发发射光谱测试结果表明,通过双掺杂可以提高钨酸铅晶体闪烁发光的强度,并且PbWO4:(F,Er)双掺杂晶体在波长为527 nm处和546 nm处均形成了较强的发光峰.通过对掺杂晶体进行XRD分析可知,阴阳离子的同时掺入并未引起钨酸铅晶体结构的明显改变.     

氧化锌纳米棒的制备及其光电性能的研究

以硝酸锌Zn(NO3)2·6H2O和六次甲基四胺(HMT)为原料,通过水热法制备出氧化锌纳米棒,研究了反应时间和冷却时间对产物形貌和尺寸的影响.采用扫描电子显微镜(SEM)、X射线衍射(XRD)、光致发光谱(PL)、紫外-可见光谱、红外光谱(FT-IR)表征产物的结构和性能.结果表明,反应时间为6 h和急速冷却至室温条件下合成样品为六方纤锌矿氧化锌纳米棒,平均直径为300 nm;样品具有良好的结晶质量和发光性能,样品在200～400nm有较强的紫外吸收性能;FT-IR图谱表明产物在430 cm-1左右出现了Zn-O特征吸收峰,并有所红移;样品的开启场强为2.2 V/μm,场增强因子为2550,当场强为4.75 V/μm时,电流密度可以达到0.7 mA/cm2,是一种性能优良的冷阴极电子发射源.     

Structural and optical property studies of CdSe crystalline nanorods synthesized by a solvothermal method

CdSe nanorods are synthesized via a simple solvothermal method at a moderate temperature of 180 °C. The influences of introducing hydrazine hydrate (N₂H₄·H₂O) as the reducing agent, and ammonia (NH₃·H₂O) as the complexing agent and also the reaction temperature, on the morphology and size of the obtained CdSe nanorods are investigated and reported. CdSe nanorods with a mean diameter and length of 25 and 82 nm, respectively, are synthesized and the problem of handling the stacking faults present in the long CdSe nanorods is analyzed. The use of increased quantity of hydrazine hydrate and also prolonged reaction time is found to reduce the stacking faults on the synthesized nanorods. The morphology, phase and the optical properties of CdSe nanoparticles are studied using powder X-ray diffraction, TEM and high-resolution transmission electron microscope (HRTEM), UV–visible absorption spectroscopy and photoluminescence (PL) spectroscopy. The low-resolution TEM images confirm the formation of CdSe nanorods, and also the agglomeration of nanoparticles and the presence of few spherical nanoparticles. The strong PL intensity from the CdSe nanorod at 702 nm confirms a blue shift of 14 nm, when compared with the bulk wurtzite CdSe.     

Low temperature hydrothermal growth and optical properties of ZnO nanorods

Well‐faceted hexagonal ZnO nanorods have been synthesized by a simple hydrothermal method at relative low temperature (90°C) without any catalysts or templates. Zinc oxide (ZnO) nanorods were grown in an aqueous solution that contained Zinc chloride (ZnCl₂, Aldrich, purity 98%) and ammonia (25%). Most of the ZnO nanorods show the perfect hexagonal cross section and well‐faceted top and side surfaces. The diameter of ZnO nanorods decreased with the reaction time prolonging. The samples have been characterized by X‐ray powder diffraction (XRD) and scanning electron microscopy (SEM) measurement. XRD pattern confirmed that the as‐prepared ZnO was the single‐phase wurtzite structure formation. SEM results showed that the samples were rod textures. The surface‐related optical properties have been investigated by photoluminescence (PL) spectrum and Raman spectrum. Photoluminescence measurements showed each spectrum consists of a weak band ultraviolet (UV) band and a relatively broad visible light emission peak for the samples grown at different time. It has been found that the green emission in Raman measurement may be related to surface states. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Facile electrochemical synthesis of tellurium nanorods and their photoconductive properties

Tellurium nanorods have been successfully fabricated by template and surfactant‐free electrochemical technique from an aqueous solution at room temperature. The as‐prepared tellurium nanorods were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectrometry, UV‐vis spectroscopy and photoluminescence spectroscopy. Films based on tellurium nanorods were constructed to study the photoresponse and I‐V curves. These photoresponse measurements demonstrate that tellurium nanorods exhibited enhanced conductivity under illumination compared to in the dark measurement.     

Synthesis and growth mechanism of ZnO rod‐like nanostructures by a microwave‐assisted low‐temperature aqueous solution route

A zinc oxide (ZnO) nanoarray (rod‐like nanostructure) was successfully synthesized through a low‐temperature aqueous solution and microwave‐assisted synthesis using zinc nitrate hexahydrate (Zn(NO₃)₂·6H₂O) and hexamethylenetetramine (HMTA) as raw materials, and using FTO glass as substrate. The effects of parameters in the preparation process, such as solution concentration, reaction temperature and microwave power, on the morphology and microstructure of ZnO nanoarray were studied. Phase structure and morphology of the products were characterized by X‐ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The results indicated that hexagonal wurtzite structure ZnO nanoarray with good crystallization could be prepared through a low‐temperature solution method. When the concentration of the mixed solution was 0.05 M, the reaction temperature was 95 °C, and the reaction time was 4 h, high‐density ZnO regular nanorods of 200 nm diameter were obtained. A possible mechanism with different synthesis methods and the influence of microwave processing are also proposed in this paper.     

Single step synthesis of CdSeS nanorods with chemical composition gradients

We report a simple method of fast synthesis of CdSeS nanorods with chemical composition gradients. The CdSeS nanorods were prepared by single-step addition of Se and S source mixture into Cd precursor solution at elevated temperatures. The size of the nanorods can be tuned by changing the S/Se feed molar ratio. As a result of the reactivity difference between Se and S precursors, the nanorods have a core/shell structure with chemical composition gradients, leading to enhancements of their photoluminescence quantum yield and photostability, which make them attractive for use in optoelectronic devices and bio-labeling.