不同形貌ZnSe的制备及光电化学性能

采用水热法制备了ZnSe纳米棒和微球, 用XRD, TGA-DTA和SEM等技术对其进行了表征, 提出了解释ZnSe微球的形成新机理. 研究结果表明, 纳米棒直径为50~100 nm, 棒长约为200~300 nm, ZnSe微球直径为3~10 μm.; 纳米棒在反应温度为240 ℃时具有闪锌矿和纤维锌矿型混晶结构, 微球在反应温度为210 ℃时具有闪锌矿结构; 将ZnSe纳米棒和微球均匀地涂在导电玻璃的导电面上, 于380 ℃煅烧40 min后制成膜电极, 并进行了光电化学研究, 纳米棒膜结构电极最高单色光的光电转换效率(IPCE)可达到9.09%.     

线性升温条件下纳米ZnSe的生成动力学

用非等温TG-DTG技术,在5.0、10.0、15.0和20.0 K•min－1 4个不同线性升温条件下,研究了从配合物ZnSe(C2H8N2)制备纳米ZnSe的过程动力学.结果表明: 该过程为三维扩散机理；机理函数为反Jander方程, f(α)＝ ，G(α)＝ ；表观活化能E=209.61 kJ•mol－1,指前因子A=1015.7 s－1,动力学方程为 ,并用结果解释了实验现象.初次报导了纳米ZnSe在420 ℃左右氧化为粒度低于40 nm的纳米ZnO.     

Ag∶InP/ZnSe纳米晶的合成与生物成像

采用高温热注入法,以P[N(CH_3)_2]_3为磷源合成了具有近红外荧光的Ag∶InP/ZnSe纳米晶.采用紫外-可见-近红外吸收光谱(UV-Vis-NIR)、荧光光谱、透射电子显微镜(TEM)、X射线衍射(XRD)等对产物的结构和光学性质进行了表征,并分析了Ag掺杂浓度和温度对InP纳米晶荧光性能的影响.通过调节Ag掺杂浓度和反应温度,发现当Ag掺杂量为6%,反应温度为200℃时,Ag∶InP纳米晶的发光效率最高.将制备的Ag∶InP的表面包覆ZnSe,粒子的荧光效率从原来的20%提高到45%.将具有近红外荧光的Ag∶InP/ZnSe纳米晶应用于细胞成像,结果表明制备的荧光纳米晶在细胞成像中清晰可见且毒性较低.     

Ag∶InP/ZnSe纳米晶的合成与生物成像

采用高温热注入法, 以P[N(CH3)2]3为磷源合成了具有近红外荧光的Ag∶InP/ZnSe纳米晶. 采用紫外|可见|近红外吸收光谱(UV|Vis|NIR)、 荧光光谱、 透射电子显微镜(TEM)、 X 射线衍射(XRD)等对产物的结构和光学性质进行了表征, 并分析了Ag掺杂浓度和温度对InP纳米晶荧光性能的影响. 通过调节Ag掺杂浓度和反应温度, 发现当Ag掺杂量为6%, 反应温度为200 ℃时, Ag∶InP纳米晶的发光效率最高. 将制备的Ag∶InP的表面包覆ZnSe, 粒子的荧光效率从原来的20%提高到45%. 将具有近红外荧光的Ag∶InP/ZnSe纳米晶应用于细胞成像, 结果表明制备的荧光纳米晶在细胞成像中清晰可见且毒性较低.     

ZnSe;Cu纳米晶/聚电解质多层膜制备和结构研究

采用分子沉积方法制备了ZnSe;Cu纳米晶/聚电解质多层膜,通过X射线光电子能谱(XPS)和透射电镜(TEM)等方法对薄膜的组成及结构进行了表征.XPS结果证实了回流处理对ZnSe;Cu微粒的表面结构以及铜离子价态的影响,从而很好地解释了经表面修饰后,微粒荧光增强的现象.TEM结果确定ZnSe;Cu的平均尺寸为3nm.X射线粉末衍射结果进一步确认ZnSe;Cu具有纤锌矿晶体结构.     

利用离子型Cd源制备ZnSe/CdSe核-壳结构纳米晶

在有机相体系中利用ZnSe前驱体纳米晶制备过程中的富Se环境,以引入Cd2+的方式在相对温和的环境下通过控制Cd2+离子的加入量及调节反应时间,成功制备了ZnSe/CdSe核-壳复合结构纳米晶.利用X射线衍射(XRD)、透射电镜(TEM)、紫外-可见吸收光谱(UV-vis)和荧光光谱(FL)对其结构形貌以及光学性质进行表征和分析的结果表明,CdSe以外延生长的方式包覆在ZnSe纳米晶表面从而形成具有良好结晶性的核-壳复合结构,其荧光发射始终保持良好单色性,同时实现了在500～620nm可见光范围内的连续可调.     

ZnSe:Mn/ZnSe纳米晶体中的Mn~(2+)离子扩散

以ZnSe:Mn/ZnSe纳米晶体为基础,分析了Mn~(2+)离子在纳米晶体中的扩散行为.通过电子顺磁共振(EPR)谱参数确定Mn~(2+)离子处在纳米晶体内部.考虑到合成过程,确定Mn~(2+)离子处于纳米晶体的核壳界面.通过荧光光谱来揭示不同退火温度和退火时间下的纳米晶体的光学性质.不同退火条件情况下纳米晶体中各元素的含量由电感耦合等离子体(ICP)发射光谱得到.随着退火温度的增加和退火时间的延长,相同物质的量的纳米晶体中Mn元素含量逐渐变小直到为零,Zn和Se的含量几乎不变.相同退火温度不同退火时间下的电子透射显微镜照片说明退火对纳米晶体的形貌和粒径几乎没有影响.     

Mn:ZnSe/ZnS核-壳结构纳米晶的无膦法制备和光学性质

以溶于十八烯的Se作为Se前驱体,在无膦条件下制备得到了具有较高量子产率的Mn:ZnSe纳米晶.为了进一步提高纳米晶的稳定性和发光强度,运用外延生长的方法进行ZnS壳层包覆并得到了具有核-壳结构的Mn:ZnSe/ZnS纳米晶.X射线衍射、透射电子显微镜及吸收和荧光光谱测试结果表明,该方法合成的Mn:ZnSe纳米晶以及核-壳结构Mn:ZnSe/ZnS纳米晶均为闪锌矿结构,具有良好的单分散性,包覆ZnS外壳层后量子产率可达到60%以上.此外,对ZnS壳层厚度和Mn2+的掺杂量对Mn:ZnSe/ZnS纳米晶发光强度的影响及发光机制也进行了初步讨论.     

Ag/ZnO/ZnSe三元异质结的合成及其可见光光催化性能

以Ag纳米线为模板,通过两步水浴法合成了Ag/ZnO/ZnSe三元异质结光催化材料。利用场发射扫描电子显微镜(FESEM)、X射线能谱仪(EDS)、X射线衍射仪(XRD)以及透射电子显微镜(FETEM)对样品的形貌和结构进行了表征。结果显示,Ag/ZnO/ZnSe三元异质结为蠕虫状的Ag/ZnO二元异质结外镶嵌着ZnSe小颗粒。在可见光下,对比纯Ag纳米线、纯ZnO纳米球、Ag/ZnO异质结对罗丹明B的可见光降解效率,结果发现Ag/ZnO/ZnSe异质结表现出了更高的光催化效率。其光催化性能的提高主要是由于Ag/ZnO/ZnSe异质结的作用促使电子空穴对的分离,降低了电子空穴对的复合机率,从而提高了材料的光催化效率。     

有机敏化剂插层层状氢氧化铽纳米复合体的合成与发光性质

选择两种有机物对苯二甲酸(TA)和苯甲酸(BA)作为敏化剂,通过在水热条件下的离子交换反应,成功将其以有机阴离子形式插层至层状铽氢氧化物而获得纳米复合体。荧光性质测定表明TA2-和BA-通过有效的能量转移均增强了Tb3+的特征绿色荧光发射,并且TA2-的敏化增强能力大于BA-。从能级匹配角度讨论了敏化剂和Tb3+之间能量转移的机理。     

CTAB辅助微波水热合成花簇状SnS微球

以氯化亚锡(SnCl2.2H2O)和硫代乙酰胺(TAA)为前驱物,十六烷基三甲基溴化铵(CTAB)为表面活性剂,采用微波水热法控制合成花簇状SnS微球。采用XRD和FESEM等分析手段对制备的样品进行表征。结果表明:合成的产物为正交晶系的SnS微晶,且结晶性良好;SnS微晶是由长方形纳米片自组装而成的花簇状微球。通过改变CTAB用量,可以实现花簇状SnS微晶的形貌和尺寸的调控,并初步分析了其形成过程。利用紫外-可见吸收光谱分析,产物的光学带隙约为1.51 eV;室温光致发光光谱表明,产物在832 nm处具有近红外发光特性。     

微观尺度高分子协同组装ZnO纳米片

以醇水混合体系作为反应介质,六水合硝酸锌和尿素为原料,聚乙烯吡咯烷酮(PVP)作为模板剂,经水热过程合成了由纳米片组装的花状微球碱式碳酸锌前驱体,经热处理得到相应的氧化锌(ZnO)产物。采用X射线衍射(XRD)和环境扫描电镜(SEM)对样品进行了表征,结果表明产物为六方纤维矿结构的ZnO,单分散花状微球直径约为2 μm,尺寸均一,组装成微球的纳米片构筑单元厚度为20 nm。红外分析表明PVP与Zn²⁺之间的化学配位作用发生在侧环的内酰基C=O键上的O位与Zn²⁺之间,研究表明PVP用量影响组装过程,在相同实验条件下,用聚乙二醇(PEG)代替PVP的模板作用,得到了粒径较大的纳米片组装的微球(φ～15 μm),在此基础上探讨了高分子结构对晶体生长和组装机制的影响。     

Selective synthesis of copper microsheets and ultralong microwires via a surfactant assisted hydrothermal process

The surfactant assisted hydrothermal process for selective preparation of copper nanosheets and ultralong microwires by reducing Cu²⁺ with 2-(bis-phosphonomethylamino)propionic acid (dpc) under the action of cetyltrimethylammonium bromide (CTAB) or polyvinyl pyrrolidine (PVP) is presented. X-ray powder diffraction (XRD) and energy dispersive X-ray analysis (EDX) indicate that the products are pure Cu of cubic phase. The effects of starting material concentration and reaction time on morphology of nanosheets have been studied by scanning electron microscopy (SEM). The presence of CTAB and PVP as capping agents is identified by EDX, transmission electron microscopy (TEM) and FT-IR. The possible growth process for ultralong microwires was studied by stopping the growth at a series of intermediate morphology stages based on SEM observations. Optical properties of Cu nanosheets and ultralong microwires were studied by UV-Vis spectrophotometry.     

Large-scale synthesis of ultrathin hexagonal tin disulfide nanosheets with highly reversible lithium storage

Ultrathin hexagonal SnS(2) nanosheets are synthesized via a simple hydrothermal reaction. The nanosheets have been applied as an anode for lithium-ion battery, which shows highly reversible capacity and good cycling stability with excellent capacity retention of 96% after 50 cycles.     

Hierarchical Hollow Hydroxyapatite Microspheres: Microwave‐Assisted Rapid Synthesis by Using Pyridoxal‐5′‐Phosphate as a Phosphorus Source and Application in Drug Delivery

Three‐dimensional (3D) hydroxyapatite (HAP) hierarchical nanostructures, in particular hollow nanostructures, have attracted much attention owing to their potential applications in many biomedical fields. Herein, we report a rapid microwave‐assisted hydrothermal synthesis of a variety of hydroxyapatite hierarchical nanostructures that are constructed by the self‐assembly of nanorods or nanosheets as the building blocks, including HAP nanorod‐assembled hierarchical hollow microspheres (HA‐NRHMs), HAP nanorod‐assembled hierarchical microspheres (HA‐NRMs), and HAP nanosheet‐assembled hierarchical microspheres (HA‐NSMs) by using biocompatible biomolecule pyridoxal‐5′‐phosphate (PLP) as a new organic phosphorus source. The PLP molecules hydrolyze to produce phosphate ions under microwave‐hydrothermal conditions, and the phosphate ions react with calcium ions to form HAP nanorods or nanosheets; then, these nanorods or nanosheets self‐assemble to form 3D HAP hierarchical nanostructures. The preparation method reported herein is time‐saving, with microwave heating times as short as 5 min. The HA‐NRHMs consist of HAP nanorods as the building units, with an average diameter of about 50 nm. The effects of the experimental conditions on the morphology and crystal phase of the products are investigated. The hydrolysis of PLP under microwave‐hydrothermal conditions and the important role of PLP in the formation of 3D HAP hierarchical nanostructures are investigated and a possible formation mechanism is proposed. The products are explored for potential applications in protein adsorption and drug delivery. Our experimental results indicate that the HA‐NRHMs have high drug/protein‐loading capacity and sustained drug‐release behavior. Thus, the as‐prepared HA‐NRHMs are promising for applications in drug delivery and protein adsorption.     

Hydrothermal synthesis of nickel hydroxide nanostructures in mixed solvents of water and alcohol

Nickel hydroxide nanosheets and flowers have been hydrothermally synthesized using Ni(CH₃COO)₂·4H₂O in mixed solvents of ethylene glycol (EG) or ethanol and deionized water at 200 °C for different time. The phase and morphology of the obtained products can be controlled by adjusting the experimental parameters, including the hydrothermal time and the volume ratio of water to EG or ethanol. The possible reaction mechanism and growth of the nanosheets and nanoflowers are discussed based on the experimental results. Porous nickel oxide nanosheets are obtained by heating nickel hydroxide nanosheets in air at 400 °C. The products were characterized by using various methods including X-ray diffraction (XRD), fourier transform infrared (FTIR), transmission electron microscopy (TEM), selected-area electron diffraction (SAED), field emission scanning electron microscopy (FESEM). The electrochemical property of β-Ni(OH)₂ nanosheets was investigated through the cyclic voltammogram (CV) measurement.     

Preparation of ZnSe Nanoparticles via Low‐Temperature Solid Phase Process

ZnSe nanoparticles were prepared from ZnCl₂, Se and KBH₄ in the presence of cetyltrimethyl ammonium bromide (CTAB) through a room temperature solid phase process. The products were characterized with x‐ray diffraction (XRD), transmission electron microscope (TEM), and energy dispersive analysis of x‐ray (EDAX). The results show that the cubic zincblende phase ZnSe nanoparticles can be obtained using this simple method. The size of nanoparticles was evaluated to be from 8 to 30 nm.     

Hydrothermal Synthesis and Primary Gas Sensing Properties of CuO Nanosheets

Uniformity nanosheets of CuO were prepared by a mild hydrothermal synthesis method. Phase analysis was carried out using x-ray diffraction (XRD) and the result confirmed the CuO nanosheets as a single phase. The field-emission scanning electron microscopy (FE-SEM) was used to observe the morphology of CuO nanosheets while the gas sensing properties of these unique CuO nanosheets were tested at a static state system. The results show that the CuO has uniformity nanosheets, and the gas sensing property show that the CuO nanosheets gas sensor has a stable gas response and the same gas sensitivity trend to tested gases. This method may be suitable for larger-scale production of these CuO nanosheets for practical applications.     

Complex wurtzite ZnSe microspheres with high hierarchy and their optical properties

Complex wurtzite ZnSe microspheres with hierarchical fractal structure and showing strong quantum-size effects can be prepared easily by a mild solvothermal reaction in a diethylenetriamine (DETA)-deionized water (DIW) binary solution. The ZnSe microspheres are made up of nanosheets, each formed by the face-to-face pairing of two individual nanosheets. In addition, high-order, flowerlike hierarchical structures are formed by the attachment of flexible, uniform nanofibers to the exposed faces of each nanosheet pair. The surface morphology of the nanosheets changed as reaction time increased and the detailed phase-transformation and shape-evolution processes were studied. This approach could provide an effective strategy for tuning the electronic and optical properties of semiconductors, with special advantages over the traditional high-temperature approach, and could be extended to access other semiconductor materials with unusual morphologies and structures.