Hierarchical assemblies of Si3N4 nanostructures

In the present work, for the first time, we report the growth of hierarchical assemblies of Si₃N₄ nanostructures via catalyst-assisted pyrolysis of a polymeric precursor on the Si substrates. The synthesized products were characterized by using field emission scanning electron microscopy, X-ray diffraction, and transmission electron microscopy. It is found that the size of the catalytic droplet plays a critical role on the formation of hierarchical assemblies of Si₃N₄ nanostructures rather than common single nanowire. A mechanism based on the Vapor–Liquid–Solid (VLS) process was proposed for the assembly of hierarchical Si₃N₄ nanostructures.     

Epitaxial Growth and Thermoelectric Measurement of Bi2Te3/Sb Superlattice Nanowires

Superlattice nanowires are expected to show further enhanced thermoelectric performance compared with conventional nanowires or superlattice thin films. We report the epitaxial growth of high density Bi₂Te₃/Sb superlattice nanowire arrays with a very small bilayer thickness by pulse electrodeposition. Transmission electron microscopy, selected area electron diffraction and high resolution transmission electron microscopy were used to characterize the superlattice nanowires, and Harman technique was employed to measure the figure of merit (ZT) of the superlattice nanowire array in high vacuum condition. The superlattice nanowire arrays exhibit a ZT of 0.15 at 330 K, and a temperature difference of about 6.6 K can be realized across the nanowire arrays.     

不同取向的CoSb3纳米线阵列的电化学法制备

近年来,金属纳米线及其阵列由于其新奇的物理和化学特性和在纳米器件方面潜在的应用前景,越来越受到人们的关注。氧化铝模板合成一维纳米材料具有设备简单、制作方便等优点,因而成为近年来人们常用的一种方法。利用电化学沉积的方法在多孔氧化铝模板中沉积各种成分的纳米线已成为纳米材料制备的一种常见的方法。这种方法不仅可以得到大面积有序的纳米线阵列,还可以根据需要调节孔洞的大小来控制纳米线的直径[1￣3]。最近理论研究结果预言[4￣6],由于纳米材料的量子限域效应,热电材料的纳米线将有比其相应块体材料更高的品质因数n,这极大地激…     

铝热反应法制备双股类螺旋Zn2SnO4单晶纳米带

综合利用化学气相沉积、铝热反应法、汽-液-固生长法、极性面融合和稳态湍流动力学控制来大量制备双股类螺旋Zn₂SnO₄单晶纳米带. 该材料属于面心立方尖晶石型透明半导体, 在光伏器件和湿度与可燃气体传感器中有着广泛的应用. 扫描电镜、透射电镜、电子衍射、X射线衍射、拉曼光谱以及光发射等技术分析表明所得的双股类螺旋纳米带是由两个独立的Zn₂SnO₄纳米带通过扭曲纠缠和融合而成. 该双股类螺旋纳米带实际上是在轴向具有周期性的超晶格材料. 光致发光测量表明该纳米带在326.1 nm处出现强发射峰, 线宽约为1.5nm. 本研究所采用的综合制备法中的铝热反应法和稳态湍流微扰法可能有助于类似材料的控制制备.     

A conversion route towards tubular SiO2 using rod-like BaSiF6 as a novel template

A simple hydrothermal reaction between Ba(NO₃)₂ and K₂SiF₆ results in the formation of 1D rod-like BaSiF₆. The BaSiF₆ rods can act as efficient precursors for production of tubular SiO₂ by hydrothermal reaction in alkaline solutions. Powder X-ray diffraction (XRD), X-ray photoelectron spectra (XPS), transmission electron microscopy (TEM), high resolution electron microscopy (HRTEM), and field emission scanning electron microscopy (FESEM) were used to characterize the phase and morphology of the final product. The experiments indicated the amount of NaOH, reaction temperature, and reaction time played important roles in the transformation process. A possible growth mechanism of tubular silica was proposed.     

不同形貌Bi4Ti3O12粒子的可控合成及光催化性能

研究了用一步水热法制备的不同形貌的钛酸铋(Bi₄Ti₃O₁₂, BIT)粒子的光学和可见光催化性能, 并对其晶体结构和微观结构用X射线衍射(XRD)、场发射扫描电子显微镜(FESEM)、透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)等手段进行了表征. XRD结果表明, 所制备的BIT 样品为层状钙钛矿结构. FESEM结果表明, 通过控制水热过程的反应参数可以得到不同形貌的纳米粒子. 紫外-可见漫反射光谱(UV-Vis DRS)表明BIT 样品的带隙能约为2.88-2.93 eV. 利用可见光(λ>420 nm)照射下的甲基橙(MO)降解实验评价了BIT 样品的光催化性能. 结果表明, BIT 的光催化活性比掺氮TiO₂ (N-TiO₂)高得多. 研究了形貌对BIT 光催化性能的影响. 所制备的BIT纳米带光催化效率最高, 经可见光照射360 min, 甲基橙溶液的降解率可达到95.0%.     

Hydrothermal Synthesis of Rhombus-like SmCO3OH Microplates and Its Photoluminescence Property Doped with Eu3+

Rhombus-like SmCO₃OH microplates with the edge lengths ranging from 5 μm to 10 μm and the thickness about 1.5 μm were synthesized through a simple hydrothermal method using urea as the precipitance. The structure and properties of the rhombus-like SmCO₃OH microplates were characterized by X-ray diffraction, field-emission scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray photoelectron spectroscopy. The optical property of the rhombus-like SmCO₃OH microplates doped with Eu³⁺ was investigated by photoluminescence. A broad and strong emission band at 677 nm was obtained, which can be contributed to producing light conversion film.     

脉冲沉积制备Cu2O/TiO2纳米管异质结的可见光光催化性能

在用阳极氧化法制备有序排列TiO₂纳米管阵列薄膜的基础上,引入脉冲沉积工艺,成功实现了均匀、弥散分布的Cu₂O纳米颗粒修饰改性TiO₂纳米管阵列,形成Cu₂O/TiO₂ 纳米管异质结复合材料. 利用场发射扫描电镜（FESEM）、场发射透射电镜（FETEM）、X射线衍射（XRD）、X射线光电子能谱（XPS）和紫外-可见漫反射光谱（UV-Vis DRS）对样品进行表征,重点研究了Cu₂O/TiO₂ 纳米管异质结的光电化学特性和对甲基橙（MO）的可见光催化降解性能. 结果表明,Cu₂O纳米颗粒均匀附着在TiO₂纳米管阵列的管口和中部位置,所制备的Cu₂O/TiO₂ 纳米管异质结具有高效的可见光光催化性能;在浓度为0.01 mol·L^-1的CuSO₄溶液中制得的Cu₂O/TiO₂纳米管异质结表现出最好的电化学特性和光催化性能;另外,对Cu₂O纳米颗粒影响光催化活性的机理进行了讨论.     

三种化学方法合成K0.5Bi0.5TiO3粉体的机理比较

采用溶胶-凝胶法、水热法和溶胶-凝胶-水热法三种化学方法合成K_0.5Bi_0.5TiO₃ (KBT)无铅压电陶瓷粉体. 用X射线衍射(XRD)分析产物的结构, 用扫描电镜(SEM)和透射电镜(TEM)观察产物的形貌. 实验结果表明, 三种化学方法均可获得纯钙钛矿相KBT粉体, 但不同工艺获得的粉体在形貌和生成机制上有很大的不同. 溶胶-凝胶法属高温固相扩散机制, 需要700 ℃以上温度煅烧才可获得KBT纯相, 且粉体颗粒度大、团聚严重. 水热法符合溶解-结晶机制, 生长出四方形的KBT纳米片. 溶胶-凝胶-水热法利用了凝胶团聚体空间链状结构的模板作用, 通过原位结晶机制生长出KBT纳米线.     

Co-templating synthesis of highly dispersed 1D ZnO nanostructures in amorphous SiO2 under hydrothermal condition

One-dimensional (1D) ZnO nanostructures were grown in amorphous SiO₂ matrix by a co-templating method under hydrothermal condition. Using ethylenediamine (EDA) groups grafted mesoporous silica MCM-41 as a co-template, the growth of 1D ZnO nanostructures was oriented by soft EDA groups and confined inside the hard mesochannels of MCM-41. The microstructure and morphology of the 1D-ZnO-nanostructures/SiO₂ composite were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray energy dispersive spectroscopy (EDS). All these results indicate that the 1D ZnO nanostructures were synthesized and highly dispersed in the amorphous SiO₂ matrix. Blue-shifted exciton absorption was observed from the co-templating synthesized sample.     

N2流量对GaN的形貌及光学和电学性能的影响

采用化学气相沉积法(CVD)在Si(100)衬底上以Ni为催化剂, 金属Ga和NH₃为原料合成了GaN微纳米结构, 并研究了N₂流量对产物GaN的形貌及光学和电学性能的影响。利用场发射扫描电子显微镜(SEM)、透射电镜(TEM)、X射线衍射仪(XRD)、X-ray能谱仪(EDS)、光致发光谱(PL)和霍尔效应测试仪(HMS-3000)等测试手段对样品的形貌、结构、成分、光学和电学性能进行了分析。结果表明, 随着N₂流量的增加, 产物GaN的形貌发生了由微米棒到蠕虫状线再到光滑纳米线的转变;生成的GaN均为六方纤锌矿结构;样品均表现出383 nm的近带边紫外发射峰和470 nm左右的蓝光发射峰;所有样品均为n型;并对产物GaN的形貌转变机理进行了分析。     

Bi2Ti2O7/TiO2复合纤维：原位水热合成及光催化性能

采用静电纺丝技术制备的TiO2纤维作为模板和反应物,通过原位水热合成了具有异质结构的Bi2Ti2O7/TiO2复合纤维。利用X射线衍射(XRD)、扫描电镜(SEM)、能量散射光谱(EDS)、高分辨透射电镜(HRTEM)和紫外可见吸收光谱(UV-Vis)等分析测试手段对样品的结构和形貌进行表征。以罗丹明B为模拟有机污染物进行光催化降解实验。结果表明:花状Bi2Ti2O7纳米结构均匀地生长在TiO2纤维上,制备了Bi2Ti2O7与TiO2相复合的光催化材料,其光谱响应范围拓宽至可见光区,与纯TiO2纤维相比可见光催化活性显著提高,且易于分离、回收和循环使用。初步探讨了Bi2Ti2O7/TiO2异质结的生长机制和光催化活性提高机理。     

N2流量对GaN的形貌及光学和电学性能的影响

采用化学气相沉积法(CVD)在Si(100)衬底上以Ni为催化剂,金属Ga和NH3为原料合成了GaN微纳米结构,并研究了N2流量对产物GaN的形貌及光学和电学性能的影响。利用场发射扫描电子显微镜(SEM)、透射电镜(TEM)、X射线衍射仪(XRD)、Xray能谱仪(EDS)、光致发光谱(PL)和霍尔效应测试仪(HMS-3000)等测试手段对样品的形貌、结构、成分、光学和电学性能进行了分析。结果表明,随着N2流量的增加,产物GaN的形貌发生了由微米棒到蠕虫状线再到光滑纳米线的转变;生成的GaN均为六方纤锌矿结构;样品均表现出383 nm的近带边紫外发射峰和470 nm左右的蓝光发射峰;所有样品均为p型;并对产物GaN的形貌转变机理进行了分析。     

Highly ordered MnO2 nanowire array thin films on Ti/Si substrate as an electrode for electrochemical capacitor

AAO/Ti/Si substrate was successfully synthesized by a two-step electrochemical anodization of the aluminum film on the Ti/Si substrate and then used as template to grow nanowire arrays. The ordered MnO₂ nanowire arrays with about 40 nm diameters had been directly fabricated on AAO/Ti/Si substrate by direct current (DC) electrodeposition. The microstructure of the nanowire arrays was investigated by field-emission scanning electron microscopy, transmission electron microscopy and X-ray diffraction. Their electrochemical characterization was performed using cyclic voltammetry in 0.5 M Na₂SO₄ aqueous solution. The synthesized MnO₂ nanowires had amorphous nature until 400 °C. The deal capacitive behavior was obtained when the as-prepared sample was heat-treated at 200 °C. The specific capacitance of the electrode was about 254 F/g.     

氧化铟八面体、纳米带、锯齿状纳米线和纳米链的可控合成

在N₂/H₂O混合气流中将硅片上金覆盖的金属铟颗粒加热到800 ℃制备出了不同形貌的In₂O₃纳米结构, 在距铟源不同距离处依次得到In₂O₃的八面体、纳米带、锯齿状纳米线和纳米链. 采用拉曼光谱、扫描电镜、X射线衍射和透射电镜对产物进行了表征分析. 结果表明, 八面体、纳米带、锯齿状纳米线和纳米链均为立方相单晶结构的In₂O₃. 基于气-固和气-液-固生长机理详细分析了八面体、纳米带、锯齿状纳米线和纳米链的生长过程, 提出了不同形貌In₂O₃纳米结构的生长模式.     

The Crystal Structure of Sr2TiSi2O8

Sr₂TiSi₂O₈ single crystals were grown by Czochralski pulling and from a high-temperature solution. X-ray diffractometry revealed the modulated crystal structure of Sr₂TiSi₂O₈ to belong to the 5D superspace group P4bm (−α, α, 1/2; α, α, 1/2) with α=0.3. Atomic positions, anisotropic displacement factors and positional modulation parameters for Sr₂TiSi₂O₈ are determined and discussed. The positional modulation is further investigated by electron diffraction and high-resolution transmission electron microscopy. In the latter experiments, the 2D modulation appears to be superimposed by some 1D modulation waves. This effect is discussed in terms of growth conditions.     

稀碱溶液中水热法制备柔性TiO2纳米须薄膜的生长机制及表征

以柔性不锈钢基底上经磁控溅射沉积的钛膜为钛源, 在1 mol·L^-1的低浓度NaOH溶液中水热法制备了朝基底上方取向生长的大长径比柔性TiO₂纳米须薄膜, 考察了钛膜沉积条件对纳米须薄膜的影响, 系统研究了水热反应条件对薄膜生长过程的影响及TiO₂纳米须薄膜的形成机制. 通过场发射扫描电镜(FESEM)、X射线能谱仪(EDS)、高分辨透射电子显微镜(HRTEM)、X射线衍射仪(XRD)等对样品进行了表征. 结果表明, 与室温沉积的钛膜相比, 600 ℃下沉积的钛膜水热后得到的纳米线薄膜与基底的附着力更好. 所得TiO₂纳米须为单晶锐钛矿, 经由Na₂Ti₂O₄(OH)₂、H₂Ti₂O₅·H₂O转变而来. 纳米须形成于水热阶段, 平行于Na₂Ti₂O₄(OH)₂的(100)晶面择优取向生长, 纳米须经历了纳米片→纳米线束→纳米线的裂解生长过程. 朝基底上方取向生长的纳米须薄膜的形成是低浓度NaOH溶液与较高水热温度(220 ℃)协同作用的结果. 进一步在Na₂SO₄溶液中研究了薄膜电极的光电化学性能, 结果表明, TiO₂纳米须薄膜的光电性能明显优于零维纳米颗粒薄膜和二维纳米片薄膜, 显示了良好的应用前景.     

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.     

RGO/C_3N_4复合材料的制备及可见光催化性能

通过半封闭一步热裂解法和改进的Hummers法分别制备了类石墨氮化碳(C3N4)和氧化石墨烯(GO),再利用光还原方法制得还原氧化石墨烯/氮化碳(RGO/C3N4)复合材料。采用X射线衍射(XRD),场发射扫描电镜(FESEM),X射线光电子能谱(XPS),紫外-可见漫反射吸收光谱(DRS),光致荧光(PL)和傅里叶变换红外光谱(FTIR)等测试技术对复合材料进行表征。以罗丹明B(RhB)为探针分子在可见光下考察RGO/C3N4复合材料的光催化活性,结果表明:RGO的引入显著提高了C3N4的光催化活性,且6.0%RGO/C3N4复合物的光催化活性最高,可能的原因是RGO具有优良的接受和传导电子性能,抑制了C3N4光生电子-空穴的复合机率,进而提高了光催化活性。     

RGO/C3N4复合材料的制备及可见光催化性能

通过半封闭一步热裂解法和改进的Hummers法分别制备了类石墨氮化碳(C₃N₄)和氧化石墨烯(GO),再利用光还原方法制得还原氧化石墨烯/氮化碳(RGO/C₃N₄)复合材料。采用X射线衍射(XRD),场发射扫描电镜(FESEM),X射线光电子能谱(XPS),紫外-可见漫反射吸收光谱(DRS),光致荧光(PL)和傅里叶变换红外光谱(FTIR)等测试技术对复合材料进行表征。以罗丹明B(RhB)为探针分子在可见光下考察RGO/C₃N₄复合材料的光催化活性,结果表明：RGO的引入显著提高了C₃N₄的光催化活性,且6.0%RGO/C₃N₄复合物的光催化活性最高,可能的原因是RGO具有优良的传导和接受电子性能,抑制了C₃N₄光生电子-空穴的复合机率,进而提高了光催化活性。