ZnO纳米片自组装空心微球的无模板水热法制备与发光性质

报道了一种简单的制备ZnO纳米片自组装成空心微球的无模板水热法. 即通过醋酸锌与水和乙二醇混合溶剂(V_水/V_乙二醇 = 1/20)在100℃水热反应12 h合成了ZnO空心微球. 利用扫描电子显微镜、透射电子显微镜、X 射线衍射仪和红外光谱对产物进行了表征和分析. 结果表明, 所制备ZnO空心微球的直径为2~5 μm, 它是由直径为10~20 nm纤锌矿结构的ZnO纳米片自组装而成. 研究了水与乙二醇的体积比及反应时间对产物形貌的影响, 结果表明乙二醇在ZnO纳米片的形成与自组装过程中起着关键作用, 并提出了可能的生长机理. 在波长为300 nm光的激发下, 发现ZnO空心微球具有发光峰位于397 nm强的紫外光发光和486 nm弱的蓝绿光发光, 这两种发光分别起源于ZnO宽带隙的激子发射和氧空位与间隙氧之间的跃迁.     

ZnO纳米片组装的微球和层状集聚体的控制合成及其发光性质

通过锌片与水分别在乙二醇和乙二胺中120 ℃反应12 h,直接在锌片上原位合成出ZnO纳米片组装的微球和层状集聚体。利用X射线粉末衍射、扫描电子显微镜、透射电子显微镜和红外光谱对产物进行了表征和分析。结果表明,在乙二醇中得到的直径为0.3～2 µmZnO微球是由直径为30～50 nm纤锌矿结构的ZnO纳米片通过氢键组装而成;在乙二胺中得到的层状集聚体是由20～30 nm的纤锌矿结构的ZnO纳米片通过氢键组装成尺寸约为450×900 nm纳米片,这些较大尺寸纳米片再通过范德华力组装而成。研究了乙二醇和乙二胺在ZnO微球和层状集聚体形成过程中的作用并提出了可能的生长机理。在波长为300 nm光的激发下,发现ZnO微球和层状集聚体具有发光峰位于397 nm强的紫外光发光、485和520 nm弱的蓝绿光发光,它们分别起源于ZnO宽带隙的激子发射,氧空位与间隙氧之间的跃迁以及表面上离子化氧空位中的电子与价带中光激发的空穴之间的复合。     

氧化锌微球和层状集聚体的控制合成及其光致发光

通过锌片与水分别在乙二醇和乙二胺中120℃反应12 h,直接在锌片上原位合成出ZnO微球和层状集聚体.利用X射线粉末衍射、扫描电子显微镜、透射电子显微镜和红外光谱对产物进行了表征和分析.结果表明,在乙二醇中得到的直径为0.3～2 μm ZnO微球是由直径为30～50 nm纤锌矿结构的ZnO纳米片通过氢键组装而成;在乙二胺中得到的层状集聚体是由20～30 nm的纤锌矿结构的ZnO纳米晶通过氢键组装成尺寸约为450 nm×900 nm纳米片,这些较大尺寸纳米片再通过范德华力组装而成.研究了乙二醇和乙二胺在ZnO微球和层状集聚体形成过程中的作用并提出了可能的生长机理.在波长为300 nm光的激发下,发现ZnO微球和层状集聚体具有发光峰位于397 nm强的紫外光发光、485和520 nm弱的蓝绿光发光,它们分别起源于ZnO宽带隙的激子发射,氧空位与间隙氧之间的跃迁以及表面上离子化氧空位中的电子与价带中光激发的空穴之间的复合.     

ZnO纳米片组装的微球和层状集聚体的控制合成及其发光性质

通过锌片与水分别在乙二醇和乙二胺中120 ℃反应12 h,直接在锌片上原位合成出ZnO纳米片组装的微球和层状集聚体。利用X射线粉末衍射、扫描电子显微镜、透射电子显微镜和红外光谱对产物进行了表征和分析。结果表明,在乙二醇中得到的直径为0.3～2 µmZnO微球是由直径为30～50 nm纤锌矿结构的ZnO纳米片通过氢键组装而成;在乙二胺中得到的层状集聚体是由20～30 nm的纤锌矿结构的ZnO纳米片通过氢键组装成尺寸约为450×900 nm纳米片,这些较大尺寸纳米片再通过范德华力组装而成。研究了乙二醇和乙二胺在ZnO微球和层状集聚体形成过程中的作用并提出了可能的生长机理。在波长为300 nm光的激发下,发现ZnO微球和层状集聚体具有发光峰位于397 nm强的紫外光发光、485和520 nm弱的蓝绿光发光,它们分别起源于ZnO宽带隙的激子发射,氧空位与间隙氧之间的跃迁以及表面上离子化氧空位中的电子与价带中光激发的空穴之间的复合。     

NiO纳米片和多孔纳米片自组装的空心微球的无模板水热法制备与磁学性质

报道一种非常简单的制备NiO和Ni(OH)₂空心微球的无模板水热法, 即通过NiCl₂与氨水在140 ℃水热反应12 h, 制备了Ni(OH)₂纳米片自组装的空心微球, 经400 ℃热处理2 h得到了NiO空心微球. 采用X射线衍射仪、扫描电镜和透射电子显微镜对产物进行表征, 并在室温下测试了它的磁学性能, 结果表明, Ni(OH)₂空心微球的直径约为3～4 μm, 它是由尺寸1.1～1.3 μm左右的六方相结构的Ni(OH)₂纳米片组装而成; NiO空心微球是由立方相纳米片和多孔纳米片组装而成, 它具有弱的铁磁性, 其矫顽力为583 Oe, 剩余磁化强度为0.213 emu/g. 研究了氨在Ni(OH)₂纳米片的形成与组装过程中的作用, 提出了可能的生长机理.     

HAP自组装球的简易合成及其光催化增效作用

选择生物协同模板,通过简单的控制组装工艺,制备出结构均一有序的羟基磷灰石(HAP)纳米组装球.该纳米组装球整体尺寸约5-6 μm,球体中心部分尺寸约为2.5-3 μm.通过X射线粉末衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、傅里叶变换红外(FT-IR)光谱、比表面积(BET)测试等手段对产物形貌、结构和比表面积进行了表征.产物作为催化剂载体,对氧化锌催化降解罗丹明B (RhB)的催化效率提高了125%,催化剂回收率提高了23.1%,有效降低了催化剂的用量,在有机物降解领域具有潜在的应用价值.同时还对产物的控制生成过程和催化增效机理做了初步探讨.     

α-Fe_2O_3纳米立方体和纳米棒组装空心微球的可控合成及其磁学性能

在0.15mol/LCl-和0.05mol/LSO42-的存在下,通过Fe3 溶液140℃水热反应12h分别得到α-Fe2O3纳米立方体和α-FeOOH纳米棒自组装的微球,将得到的α-FeOOH纳米棒自组装微球经600℃热处理2h后转化为α-Fe2O3纳米棒组装空心微球.利用X射线衍射仪、扫描电子显微镜、透射电子显微镜和红外光谱对所得产物进行表征和分析.结果表明,所制备的单分散的α-Fe2O3纳米立方体为六方单晶结构,其边长为500nm.直径为2~4.5μm的空心微球是由直径约150nm的α-Fe2O3纳米棒组装而成.研究了Cl-和SO42-在纳米立方体和空心微球形成过程中的作用,提出了可能的生长机理.在室温下测试了α-Fe2O3纳米立方体和α-Fe2O3纳米棒自组装微球的磁学特性,其矫顽力和剩余磁化强度分别为2858.3Oe(1Oe=79.58A/m)和0.195emu·g-1(1emu·g-1=15.7914×10-9A·m2·kg-1),218.87Oe和0.071emu·g-1.     

水热法制备聚苯胺及其铁氧化物纳米复合材料

利用水热法与无模板自组装法相结合, 以三氯化铁为氧化剂、 掺杂剂和反应物, 制备了聚苯胺及其铁氧化物纳米复合材料. 结果表明, 通过改变三氯化铁的浓度可以调控产物的微观结构和组成. 当三氯化铁的浓度≤0.13 mol/L时, 产物组成为未掺杂的低聚苯胺与α-Fe₂O₃的复合纳米材料, 其微观结构为纳米颗粒组装成的椭球体和准立方体; 当三氯化铁的浓度≥0.20 mol/L时, 产物组成为掺杂态聚苯胺, 其微观结构为纳米片层结构组装成的微米级大丽花球; 并且产物的粒径随三氯化铁浓度的增大而增大. 利用扫描电子显微镜、 红外光谱、 紫外-可见光谱、 X光电子能谱及X射线衍射等手段对产物的微观结构和组成进行了表征, 并探讨了产物的形成机理.     

wo2.50纳米组装片的制备、表征及其在导电涂料中的应用

利用内在还原法制备了长0.7～1.2μm,宽180～250 nm的WO2.50纳米组装片。通过透射电子显微镜观察发现,该纳米组装片是由直径约45 nm的纳米粒子组装而成的。产物由WO2.00和WO2.90两相组成,具有良好的结晶度,其比表面积为13.6 m2/g。产物具有良好的导电性(电阻率为0.1Ω.cm)和与树脂的亲和性。产物的红外光谱中,νW—O吸收峰发生了33 cm-3的红移。采用热重-差示扫描量热测试技术对前驱物进行了热分析,对实验条件进行了探索,确定最佳制备温度为750℃。对WO2.50纳米组装片的形成机理作了探讨,将其应用在导电涂料领域,测得漆膜的表面电阻率为5Ω.cm。     

杨桃状ZnO纳米片微球的制备及气敏性能的研究

以六水合硝酸锌和尿素为原料,水为反应介质,油酸作为表面活性剂,经水热过程合成了由纳米片组装的碱式碳酸锌微球前驱体,经煅烧后得到形貌一致的氧化锌(ZnO)纳米片组装的杨桃状微球。采用X射线衍射仪(XRD)和环境扫描电镜(SEM)对样品进行表征,结果表明产物为六方纤维矿结构的ZnO,微球尺寸比较均一,直径约为20μm,组装单元扇形ZnO纳米片均匀排列,单元之间存在均匀空隙,BET测试显示纳米片呈现多级介孔结孔结构,比表面积为18.9m2·g-1,室温下的光致发光性能表明其结构表面存在大量氧空位,对产物ZnO气敏元件进行了乙醇和丙酮气体敏感性测试。     

Facile Synthesis and Catalytic Properties of β-Co（OH）2 and Mg（OH）2 Nanoplates

β-Co(OH)2 and Mg(OH)2 nanoplates were synthesized via a facile template-free hydrothermal approach.The different conditions of preparation and catalytic properties of the products were studied and discussed.The products were characterized by X-ray diffraction,transmission electron microscopy,scanning electron microscopy,selected area electron diffraction(SAED),and gas chromatograph.     

BiOCl nanostructures with different morphologies: Tunable synthesis and visible-light-driven photocatalytic properties

BiOCl nanostructures including microspheres,microflowers,microplates,and nanoplates,have been synthesized by a simple solvothermal method using bismuth nitrate and sodium chloride as raw materials without adding any additives.Structure and morphology of the products were characterized by powder X-ray diffraction,scanning electron microscopy,and transmission electron microscopy.The results indicated that the as-prepared microspheres and microflowers were composed of nanosheets.Although with different shape and lateral size,the nanoplates and microplales were all single-crystalline plates with exposed {001) facets.It was found that the volume ratio of polyethylene glycol 400 and H₂O in the solvent played a key role in the morphology of the products,and the possible growth mechanism was also discussed.The photocatalytic measurements indicated that the BiOCl samples exhibit good photocatalytic properties towards Rhodamine B.     

简单的溶剂热法制备分层的碲化铋微米结构

采用简单的溶剂热法制备出高纯度的由纳米片自组装而形成的碲化铋微米结构。在碲化铋的形成中,乙二醇不仅作为溶剂,而且还作为还原剂。研究发现,聚乙烯吡咯烷酮(PVP)和硝酸在碲化铋的形成中起到了很重要的作用。通过X-射线衍射(XRD)、X-射线光电子能谱(XPS)、扫描电镜(SEM)、透射电镜(TEM)、高分辨透射电镜(HRTEM)、选区电子衍射(SAED)对其进行表征及研究。最后,利用时间演化实验对碲化铋的形成机理进行了探讨。     

Facile Synthesis and Catalytic Properties of β-Co(OH)2 and Mg(OH)2 Nanoplates

β-Co(OH)2 and Mg(OH)2 nanoplates were synthesized via a facile template-free hydrothermal approach. The different conditions of preparation and catalytic properties of the products were studied and discussed. The products were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, selected area electron diffraction(SAED), and gas chromatograph.     

Microwave-assisted synthesis and characterization of hexagonal Fe3O4 nanoplates

Hexagonal magnetite (Fe₃O₄) nanoplates with an average edge length of 80 nm were successfully prepared in large quantities by a facile microwave-assisted route. The influences of experiment parameters such as reaction time, microwave power, and concentration of NaOH and other additive agents on the morphology and size of final products were investigated in detail. Phase structure, morphology and magnetic properties of products were carefully studied by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED), high-resolution transmission electron microscope (HRTEM), and vibrating sample magnetometer (VSM). Magnetic studies revealed that hexagonal Fe₃O₄ nanoplates have low saturation magnetization of 36.4 emu/g and the possible reason has been proposed.     

Mn3O4 nanoplates and nanoparticles: Synthesis, characterization, electrochemical and catalytic properties

Mn₃O₄ hexagonal nanoplates and nanoparticles were synthesized via a solvent-assisted hydrothermal oxidation process at low temperature and a solvothermal oxidation method, respectively. The synthesized product was characterized by powder X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM), electron diffraction (ED), Fourier transform infrared (FT-IR) spectroscopy. Their capability of catalytic oxidation of formaldehyde to formic acid at room temperature and atmospheric pressure and electrochemical properties by cyclic voltammogram (CV) were compared. The results showed that Mn₃O₄ hexagonal nanoplate is a better catalyst, and the hexagonal nanoplates and nanoparticles modified electrodes blended with carbon black have a higher specific capacitance.     

沉淀转化法制备多孔片状纳米LaF3

采用实验中所合成的LaPO4纳米棒为前驱体,通过沉淀的转化作用,大面积地制备了单分散的片状纳米LaF3。采用扫描电镜(SEM)、透射电镜(TEM)、X射线衍射仪(XRD)、BET(Brunauer-Emmett-Teller)测试对片状纳米LaF3的形貌、结构、相组成及表面性质进行了分析。片状纳米LaF3底边长约为40 nm,片的厚度约为35 nm,大小均一,具有多孔结构。通过改变反应溶剂,可以控制LaF3粒子的成核、生长和团聚,从而有效地调控多孔片状纳米LaF3的颗粒尺寸和分散性。对多孔片状纳米LaF3的生长机制进行了研究,结果表明LaPO4和LaF3的溶度积常数差导致了片状纳米LaF3的生成;体系中自身存在的Ostwald ripening作用使片状纳米LaF3出现了多孔结构。     

Preparation of monodispersed microporous SiO2 microspheres with high specific surface area using dodecylamine as a hydrolysis catalyst

A novel and simple method for the synthesis of monodispersed microporous SiO₂ microspheres with high specific surface area was developed by hydrolysis of tetraethoxysilane (TEOS) in a water-ethanol mixed solution and using dodecylamine (DDA) as hydrolysis catalyst and template. The as-prepared products were characterized with differential thermal analysis-thermogravimetry, scanning electron microscopy, high-resolution transmission electron microscopy, small angle X-ray diffraction and nitrogen adsorption. The effects of experimental conditions including hydrolysis temperatures, calcination temperature and concentrations of TEOS and DDA on the morphology and pore parameters of the as-prepared SiO₂ microspheres were investigated and discussed. The results showed that hydrolysis temperature and concentrations of TEOS and DDA are important parameters for the control of size and morphology of particles. The specific surface area and specific pore volume of the as-prepared SiO₂ microspheres increased with increasing DDA concentration and calcination temperature. DDA may act not only as a good hydrolysis catalyst but also as a template for the formation of monodispersed SiO₂ microspheres with high specific surface area. This research may provide new insight into the synthesis of monodispersed microporous SiO₂ microspheres.     

Hydrothermal synthesis and photocatalytic property of porous CuO hollow microspheres via PS latex as templates

Porous copper oxide (CuO) hollow microspheres have been fabricated through a simple hydrothermal method using PS latex as templates. The as-obtained samples were characterized by means of scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffractometry (XRD) and Fourier transform infrared spectroscopy (FTIR). The influences of the mole ratio of Ethylenediamine (C₂H₈N₂) and copper acetate (Cu(Ac)₂·H₂O), hydrothermal temperature and time on the size and morphologies of the final products have been investigated. The possible formation mechanism of porous CuO hollow microspheres has been proposed and the specific surface area of the hollow microspheres with 81.71 m²/g is measured by BET method. The band gap value calculated from a UV–vis absorption spectrum of porous CuO hollow microspheres is 2.71 eV. The as-synthesized product exhibits high photocatalytic activity during the photodegradation of an organic dyestuff, rhodamine B (RhB), under UV-light illumination.