ZnO准一维纳米结构生长形态的演化机理

利用气相生长系统,通过调控实验参数,制备了多种形貌的ZnO准一维结构,如纳米条带、[011-0]和[21-1-0]取向的单侧生齿的梳状纳米条带、微米尺度的梳状结构,由多节状六角棱柱和八角棱柱组装成的微米条带等.通过X射线衍射、扫描电子显微镜及其所加载的能谱分析和背散射电子衍射仪、高分辨透射电子显微镜等分析技术, 对其中具有代表性的介观结构进行了系统的形貌分析和细致的结构解析.分析出基本的结构单元及其复合体, 揭示了显微尺度下ZnO晶体的外形多样性以及其形态演化中的关联和规律,即ZnO纳米条带、梳状结构和多节状微米条带具有晶体结构上的同一性.     

Properties of Nd3+-doped and undoped tetragonal PbWO4, NaY(WO4)2, CaWO4, and undoped monoclinic ZnWO4 and CdWO4 as laser-active and stimulated raman scattering-active crystals

Spectroscopic, laser, and chi((3)) nonlinear optical properties of tetragonal PbWO(4), NaY(WO(4))(2), CaWO(4), and monoclinic CdWO(4) and ZnWO(4) were investigated. Particular attention was paid to Nd(3+)-doped and undoped PbWO(4) and NaY(WO(4))(2) crystals. Their absorption and luminescence intensity characteristics, including the peak cross sections of induced transitions, were determined. Pulsed and continuous-wave lasing in the two 4F(3/2)-->4I(11/2) and 4F(3/2)-->4I(13/2) channels was excited. For these five tungstates, highly efficient (greater than 50%) multiple Stokes generation and anti-Stokes picosecond generation were achieved. All the observed scattered laser components were identified. These results were analyzed and compared with spectroscopic data from spontaneous Raman scattering. A new crystalline Raman laser based on PbWO(4) was developed for the chi((3)) conversion frequency of 1-microm pump radiation to the first Stokes emission with efficiency up to 40%. We classify all the tungstates as promising media for lasers and neodymium-doped crystals for self-stimulated Raman scattering lasers.     

Microwave-assisted synthesis of barium tungstate nanosheets and nanobelts by using polymer PVP micelle as templates

Single-crystal BaWO₄ nanosheets and nanobelts have been successfully synthesized by using polymer PVP micelle as templates in a reflux system under microwave irradiation. Our result shows that the concentration of PVP aqueous solutions played an important role in the formation of BaWO₄ crystal with different morphologies. The products were characterized by X-ray powder diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM) and electron diffraction (ED).     

Spherulitic growth and recrystallization in barium silicate glasses

The growth and recrystallization of spherulites formed in barium disilicate glasses between 700 and 900° C has been studied by electron microscopy and electron diffraction. Spherulites formed at 700° C consist of fibrillar (～ 100 Å diameter) monoclinic crystals in confocal arrangement with preferred crystallographic growth axes. High temperature (900° C) spherulites are composites of radially oriented plate-shaped orthorhombic crystals with lateral growth of epitaxially nucleated fibrillar monoclinic crystals. At intermediate temperatures “axialites”, consisting of a single orthorhombic “midrib” crystal with monoclinic fibrillar side-growths, grow in competition with the low temperature spherulite morphology. The monoclinic fibrillar phase is believed to be an intermediate metastable structure which is able to grow more rapidly than the orthorhombic phase via cellular transformation in the presence of impurities. Brief comparison is made between the observed morphologies and theories for interface instability and cellular crystallization. Recrystallization, induced mainly by the large interfacial area of spherulite fibrils, produces faulted and twinned monoclinic grains which transform slowly to the orthorhombic stable crystal phase. A glassy intercrystalline residue becomes more prominant with grain growth.     

Synthesis and field emission of single-crystalline copper vanadate nanobelts

Single-crystalline nanobelts of a nonstoichiometric compound Cu(1.55)V(2)O(6.55), with a thickness of 40-60?nm, width of 50-300?nm and length of several micrometers, have been synthesized on a large scale by a hydrothermal method. The structures and morphologies of the nanobelts were characterized by x-ray powder diffraction, x-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy and high-resolution transmission electron microscopy. A probable growth mechanism has also been discussed. The nanobelts exhibit a turn-on field of 11.0?V?μm(-1), which is defined as the macroscopic field required to produce a current density of 10?μA?cm(-2). It is anticipated that the nanobelts can serve as a candidate material for future field emitters.     

聚丙烯酸钠或聚甲基丙烯酸调控下合成特殊形貌的PbWO4晶体

以聚丙烯酸钠（PAANa）或聚甲基丙烯酸（PMAA）为模板,Na2WO4为沉淀剂,在Pb（NO3）2溶液中合成具有特殊形貌的PbWO4晶体。PAANa、PMAA或PbWO4的浓度改变时,PbWO4晶体的形貌都将发生较大的变化。PbW04的浓度为0．0500mol／L时,PbWO4晶体为宝塔形;PAANa浓度增大后,PbWO4晶体变为枣核形;PMAA取代PAANa后,PbWO4晶体可变为有四条楞的枣核状晶体,但PbWO4晶体的晶型都没有改变。     

Fe(3)O(4) nanobelts: one-pot and template-free synthesis, magnetic property, and application for lithium storage

We report on the synthesis of Fe(3)O(4) nanobelts with good magnetic properties and lithium storage performances by using a one-pot and template-free hydrothermal method with Na(2)CO(3) and FeCl(2) as the reactants. By controlling the amount of Na(2)CO(3), we obtained pure Fe(3)O(4) nanobelts with widths of 0.1-2?μm, thicknesses of about 10 nm and lengths of 20-30?μm, showing a high aspect ratio. XRD and SAED patterns of the obtained sample demonstrated that the Fe(3)O(4) nanobelts were well crystallized. Nitrogen adsorption/desorption measurements showed that Fe(3)O(4) nanobelts manifested a BET surface area of 25.04?m(2)?g(-1). Further experiments demonstrated that the amount of Na(2)CO(3) played an important role in controlling both the morphologies and crystal structures of the products. The formation mechanism of Fe(3)O(4) nanobelts was also studied. More importantly, we found that the Fe(3)O(4) nanobelts showed magnetic properties with a magnetic saturation value of 77.0?emu?g(-1) and lithium storage performances with a high initial discharge capacity of 1090?mAh?g(-1) at a current rate of 500?mA?g(-1), and a reversible capacity of 404?mAh?g(-1) retained after 60 charge/discharge cycles. These results suggest that the Fe(3)O(4) nanobelts might be promising for magnetic and lithium battery applications.     

Simple template-free solution route for the synthesis of Ni(SO(4))(0.3)(OH)(1.4) nanobelts and their thermal degradation

Nanobelts of nickel hydroxyl sulfate have been prepared on a large scale via a simple template-free hydrothermal reaction on the basis of a complex [Ni(NH(3))(6)](2+) formed with Ni(2+) and ammonia in an ethanol-water solution. The as-synthesized nanobelts were single crystals, with several tens of microns in length and 50-150?nm in width. The nanobelts were enclosed by top surfaces (100) and side surfaces (001) and their growth direction was parallel to [010]. The function of aqueous ammonia and ethanol was discussed. Furthermore, nanostructures of a mixture of crystralline NiO and amorphous nickel sulfate with various morphologies, such as nanobelts, porous nanobelts, and nanoparticles, were obtained by the thermal treatment of the as-synthesized Ni(SO(4))(0.3)(OH)(1.4) nanobelts at different temperatures.     

Solid phase growth of tin oxide nanostructures

For the first time, single-crystalline SnO₂ nanostructures comprising of nanobelts, nanowires and nanosheets have been synthesised by solid phase crystal growth from tin oxide single crystals. The product was characterised by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, transmission electron microscopy, selected area electron diffraction, and Raman spectroscopy. The procedure consisted of two stages. In the first stage, a mixture of SnO₂ polyhedral single crystals attached with graphite particles were produced by heating a mixture of SnCl₂ and graphite. Then, the SnO₂ single crystals were grown into nanobelts, nanowires and nanosheets by further heating. The role of graphite in the process is also discussed to be the surface reduction of SnO₂ into oxides with lower oxygen content which provide a driving force for surface diffusion and subsequent crystal growth of tin oxide into the one and two dimensional nanostructures. The results provide insights for both fundamental research as well as technological production of SnO₂ nanostructures.     

Synthesis of BaTi2O5 nanobelts

BaTi₂O₅ nanobelts with 60–100 nm in thickness, 200–300 nm in width, and several micrometers in length have been successfully synthesized through a two-step hydrothermal reaction. Sodium titanate nanobelts are synthesized via the reaction of titania nanoparticles and NaOH aqueous solution at 180 °C for 24 h. After the reaction, resulting sodium titanate nanobelts are ion-exchanged with barium ions and then treated at 180 °C for 60 h under alkaline condition, BaTi₂O₅ nanobelts are formed. The morphologies and crystal structures of sodium titanate and BaTi₂O₅ nanobelts are characterized by field-emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM) and X-ray powder diffractometer (XRD), respectively.     

LiV3O8纳米带的低温熔盐合成及其电化学性能

为了改进三聚钒酸锂作为锂离子电池正极材料的电化学性能,以LiNO3、LiCl和NH4VO3作为反应原料,通过一种简单的低温熔盐合成方法（LT-MSS）在250℃温度条件下制备得到带状LiV3O8纳米材料.X射线衍射（XRD）和X射线光电子能谱（XPS）分析结果表明所得产物为单斜相LiV3O8.扫描电镜（SEM）、透射电镜（TEM）和高分辨透射电镜（HRTEM）照片显示该产物为单晶纳米带形貌,沿[001]方向生长.电化学测试表明该产物储锂量高,循环性能良好.实验结果表明采用低温熔盐合成法制备LiV3O8能够有效提高所得产物的结构、形貌和电化学性能.     

Temperature effect on electrospinning of nanobelts: the case of hafnium oxide

Electrospinning is a convenient and versatile method for fabricating different kinds of one-dimensional nanostructures such as nanofibres, nanotubes and nanobelts. Environmental parameters have a great influence on the electrospinning nanostructure. Here we report a new method to fabricate hafnium oxide (HfO(2)) nanobelts. HfO(2) nanobelts were prepared by electrospinning a sol-gel solution with the implementation of heating and subsequent calcination treatment. We investigate the temperature dependence of the products by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and energy-dispersive x-ray (EDX) spectroscopy. The heating temperature of spinning ambient is found to be crucial to the formation of HfO(2) nanobelts. By tuning the temperature, the morphological transformation of HfO(2) from nanowires to nanobelts was achieved. It was found that the rapid evaporation of solvent played an important role in the formation process of HfO(2) nanobelts. It is shown that nanobelts can only be obtained with the temperature higher than 50?°C and they are in the high quality monoclinic phase. A possible growth mechanism of the nanobelts based on phase separation is proposed. The enhanced photoluminescence (PL) of HfO(2):Eu(3+) nanobelts is also illustrated.     

钨酸铅(PbWO_4)晶体的发光均匀性研究

通过对下降法生长的全尺寸钨酸铅（ＰｂＷＯ４）晶体沿长轴方向不同点的透过率和光产额的测量、分段晶体的透过率和光产额的测量,研究了钨酸铅晶体的发光均匀性及其影响因素．结果表明：钨酸铅晶体发光均匀性主要由生长后期的钨酸铅晶体质量所决定,采用晶种为大头的加工取向有利于提高钨酸铅晶体的发光均匀性．     

Synthesis of manganese vanadate nanobelts and their visible light photocatalytic activity for methylene blue

Manganese vanadate nanobelts have been synthesised by a simple hydrothermal process using polymer polyvinyl pyrrolidone as the surfactant by adjusting the pH value. The X-ray diffraction, selected area electron diffraction and the high-resolution transmission electron microscopy (TEM) show that the manganese vanadate nanobelts are composed of a single crystalline monoclinic Mn₂V₂O₇ phase. Scanning electron microscopy and TEM observations show that the thickness, width and length of the nanobelts are 20 nm, 350 nm–1 μm and several dozens to several hundreds of micrometres, respectively. The photocatalytic activities of the manganese vanadate nanobelts have been evaluated by the photocatalytic degradation of methylene blue (MB) in an aqueous solution as a model pollutant under the solar light irradiation. After 4 h of the irradiation by the solar light, the MB solution with the volume of 10 mL and the concentration of 10 mg·mL^?1 can be totally degraded using 10 mg manganese vanadate nanobelts.     

Investigation of the drawing mechanism of UHMWPE fibers

The influence of draw ratios (DR) of gel-spun ultrahigh molecular weight polyethylene (UHMWPE) fibers on resultant morphologies, tensile, degrees of orientation, and crystal phase transition properties were investigated using wide-angle X-ray diffraction (WAXD), differential scanning calorimetry (DSC), and scanning electron microscopy (SEM). The anisotropic crystalline structure with full concentric circular rings originally shown on the WAXD patterns of the as-prepared and drawn UHMWPE fibers gradually transform into oriented fibers with azimuthal spots on the equator as their DR values increase from 1 to 20, in which their orthorhombic crystals, percentage crystallinity, crystalline orientation, and the birefringence values increase significantly. As evidenced by SEM and WAXD analysis, the chain-folded molecules originally present in kebab crystals of the as-prepared UHMWPE fiber specimens gradually transformed into shish-like crystals with relatively high orientation as their DR values increase from 1 to 20. In contrast, the crystallinity and crystal orientation values of the drawn UHMWPE specimens increase only slightly, as their DR values increase from 20 to 40, wherein both crystallinity values of orthorhombic and monoclinic crystals increase slightly. In fact, barely any oriented kebab but only shish crystals were observed on the surfaces of drawn UHMWPE fiber specimens with DR values higher than 20. The birefringence values increase only slightly with further increasing DR values, while crystallinity and crystal orientation values of the drawn UHMWPE fiber specimens remained relatively unchanged as their DR values increase from 40 to 150. In the meantime, the monoclinic crystals gradually grow at the expense of the orthorhombic form crystals as the DR values of drawn UHMWPE fiber specimens increase from 40 to 150. Possible reasons accounting for these interesting properties found for the drawn UHMWPE fibers with varying draw ratios are proposed in this study.     

碲化铜纳米材料的液相可控合成及其电导率

采用溶剂热法在不同溶剂中(二正丙胺、丙酮和环己酮)分别制备了不同形貌的Cu7Te4纳米结构,包括厚度为200 nm,长度达几十微米的纳米带、粒径为10~25 nm的纳米粒子和由约10 nm的纳米粒子聚集构成的微米片,并使用XRD、SEM、TEM和HRTEM等测试手段对其进行了表征.此外,在室温到400℃范围内测试了三种形貌样品的电导率随温度的变化曲线,研究表明,在相同的测试条件下,由Cu7Te4纳米带制备的块体材料的电导率显著高于另外两种形貌样品.最后,对反应机理和三种溶剂环境对产物形貌的影响进行了探讨.     

不同结构形貌BiVO4的水热制备及可见光催化性能

采用水热法,无需添加剂,通过调控反应液pH值和反应温度制备了不同结构和形貌的BiVO4可见光催化剂.利用X射线衍射(XRD)、扫描电子显微镜(SEM)、紫外可见漫反射(DRS)和低温氮吸附等手段对样品进行表征,结果显示:水热温度与反应液pH值对晶体结构有很大影响,180℃水热温度和酸性条件有利于单斜相的生成.反应液pH值对形貌也有很大影响,不同条件下得到了片状、立方状、棒状等不同形貌的BiVO4.同时以亚甲基蓝为降解对象,考察了所制备BiVO4的可见光催化活性.其中,pH值为2,反应液中制备的片状单斜相BiVO4具有最高的光催化活性(4 h达92.0%).此外,还考察了光催化剂用量、亚甲基蓝浓度和电子受体的存在对光催化过程的影响,结果表明:当催化剂用量为1.0 g/L,亚甲基蓝浓度为10 mg/L,KBrO3为电子受体时光催化效果最佳.     

Preparation of Manganese Oxide Nanobelts

Oriented nanobelts of manganese oxide have been firstly and successfully prepared by a microemulsion technique under controlled circumstances. The samples were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM). Influences of sodium chloride and annealed temperature on the synthesis of Mn3O4 nanobelts were investigated. It was found that NaCl is the key factor to synthesize oriented Mn3O4 nanobelts and 827 K is optimum temperature to produce fine nanobelts. Oriented growth mechanism of Mn3O4 nanobelts was discussed.     

钨酸铅晶体着色问题的实验研究

本计ＰｂＷＯ４（ＰＷＯ）晶体的着色问题进行了实验研究,以ＰｂＯ和ＷＯ３粉体为原料采用改进的Ｂｒｉｄｇｍａｎ法生长的ＰＷＯ晶体会呈现出浅黄色,通过对实验现象的分析,提出了ＰＷＯ晶体中同时存在Ｏ缺位和Ｐｂ缺位,其中,Ｏ缺位是导致ＰＷＯ晶体３５０ｎｍ率低的原因,Ｐｂ缺位是产生４２０ｎｍ吸收带使晶体着色的根源。     

钨酸盐晶体中负离子配位多面体的结晶方位与晶体的形貌

钨酸盐类晶体是重要的闪烁晶体．本文从钨酸盐类晶体中负离子配位多面体的结晶方位和相互联结的稳定性出发，探讨了钨酸盐类晶体中[WO4]2-等负离子配位多面体的结晶方位与晶体结晶形貌之间的关系；认为[WO4]2-四面体与金属阳离子（Ca2＋，Pb2＋，Zn2＋）结合时，由于晶体结构和生长条件（如籽晶取向等）的不同，在晶体各族晶面上的叠合速率和结构取向不同，晶体的结晶形貌迥然有别；四面体的面和梭的法线（L2）所对向的晶面，生长速率慢，顽强显露，均属晶体的板面；四面体的顶角所指向的晶面，生长速率快，显露面积小，经常消失．由此可以合理解释钨酸铅等闪烁晶体的生长特征．最后对ABO4型晶体的结构及习性特征进行了总结归纳．