Synthesis and characterization of a micro scale zinc oxide–PVA composite by ultrasound irradiation and the effect of composite on the crystal growth of zinc oxide

Micro scale zinc oxide-polyvinyl alcohol (ZnO–PVA) composite has been synthesized by ultrasound irradiation. The properties of the as-prepared ZnO–PVA composite material are characterized by X-ray diffraction (XRD), thermo gravimetric analysis (TGA), transmission electron microscopy (TEM), and diffuse reflection spectroscopy (DRS). A band gap of 3.25 eV is estimated from DRS measurements. The controlled crystal growth of zinc oxide has been studied by using the as-prepared micro scale ZnO–PVA composite as seeds for the crystal growth of ZnO.     

Thermal properties of nano crystalline CdS

Nano CdS samples are synthesized by precipitation method for different growth conditions. Thermal diffusivity and conductivity on these nano CdS are measured by photo acoustic technique. The results are compared with bulk and discussed. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Sol‐gel synthesis of electrospun BaO/MnO nanocomposite fibers and their magnetic characterization

A new approach, combining in‐situ sol‐gel process with electrospinning, was used to prepare magnetic barium acetate/manganese acetate/poly (vinyl alcohol) (PVA) composite nanofibers. The composite gel was synthesized by sol‐gel method in the presence of 10 wt.% PVA aqueous solution. PVA was used as stabilizer and polymeric matrix. The resultant barium acetate/manganese acetate/PVA composite nanofibers were calcined at 1023 K for 5 h. This formed BaO/MnO nanocomposite crystalline fibers with average diameter less than 100 nm and were characterized with Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Energy Dispersive X‐ray Analysis (EDAX), powder X‐ray diffractometer (XRD), UV‐Vis‐Spectroscopy (UV) and Vibrating Sample Magnetometer (VSM) respectively. These composite fibers exhibited a uniform cylindrical morphology, with the BaO/MnO nanoparticles implanted in the fibers. M‐H curves were obtained at 300 K and 20 K. From the M‐H curves, room temperature ferromagnetism was observed at 300 K. At low temperatures, the ferromagnetic behavior was masked by the paramagnetic behavior. The saturation magnetization at 300 K was found to be 0.004 emu /g and the saturation magnetization at 20 K was found to be 0.658 emu /g. The magnetization at 20 K was found to be very large and it was several times larger than at 300 K. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of doped lithium aluminate nanocrystalline particles by sol‐gel method

Nanocrystalline particles of Co²⁺doped lithium aluminate (Co²⁺:LAO) and Ni²⁺‐doped lithium aluminate (Ni²⁺:LAO) were synthesized by sol–gel method. The crystalline nature and particle size of the samples were characterized by X‐ray diffraction analysis (XRD). The morphology and the presence Co²⁺ and Ni²⁺ in the synthesized samples were analyzed by scanning electron microscope (SEM) and energy dispersive X‐ray analysis (EDAX). The presences of functional groups in the samples were analyzed using FT‐IR analysis. The optical absorbance of the synthesized samples were observed using UV absorption spectral analysis. The frequency dependent dielectric behaviour of the synthesized nano materials was analyzed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

纳微米复合HAp-ZrO2生物复合材料的制备与微观结构研究

本文主要对纳米氧化锆与羟基磷灰石(HAp)复合制备纳微米复合HAp-ZrO2复合材料的制备工艺及微观结构进行了初步研究.用XRD分析了原料及复合材料的相组成,用IR研究了HAp粉体的结构,发现所制备HAp纯度高,羟基稳定存在.用TEM观察了HAp粉体以及HAp与ZrO2复合粉体的形貌与颗粒大小,发现HAp粉体呈颗粒状,粒径在60～70nm,这表明用化学沉淀法可制备出纳米级的HAp粒子,但在后续过程中往往发生团聚而达到微米级;纳米ZrO2粒子加入后在HAp基体中分散均匀.SEM观察发现,纳米ZrO2粒子的加入可以起到抑制羟基磷灰石晶粒长大、改善材料微观结构的作用.     

Y_2O_3:Er~(3+)上转换纳米纤维的制备与性质研究

采用静电纺丝技术制备了PVA/[Y(NO_3)_3+Er(NO_3)_3]复合纳米纤维,将其在适当的温度下进行热处理,得到Y_2O_3∶Er~(3+)上转换纳米纤维.XRD分析表明,PVA/[Y(NO_3)_3+Er(NO_3)_3]复合纳米纤维为无定型,Y_2O_3∶Er~(3+)上转换纳米纤维属于体心立方晶系,空间群为Ia3.SEM分析表明,PVA/[Y(NO_3)_3+Er(NO_3)_3]复合纳米纤维的平均直径约为130 nm;经过600 ℃焙烧后,获得了直径约60 nm Y_2O_3∶Er~(3+)上转换纳米纤维.TG-DTA分析表明,当焙烧温度高于600 ℃时,PVA/[Y(NO_3)_3+Er(NO_3)_3]复合纳米纤维中水分、有机物和硝酸盐分解挥发完毕,样品不再失重,总失重率为80;.FT-IR分析表明,PVA/[Y(NO_3)_3+Er(NO_3)_3]复合纳米纤维的红外光谱与纯PVA的红外光谱基本一致,600 ℃时,生成了Y_2O_3∶Er~(3+)上转换纳米纤维.该纤维在980 nm激光激发下发射出中心波长为522 nm、561 nm的绿色和658 nm的红色上转换荧光,对应于 Er~(3+)的~2H_(11/2)/~4S_(3/2)→~4I_(l5/2)跃迁和~4F_(9/2)→~4I_(l5/2)跃迁.对Y_2O_3∶Er~(3+)上转换纳米纤维的形成机理进行了讨论,该技术可以推广用于制备其他稀土氧化物上转换纳米纤维.     

Size‐dependent spectroscopic,optical, and electrical properties of PbSe nanoparticles

Stable crystalline Lead Selenide nanoparticles (PbSe NPs) were prepared with a cubic (sphalerite) phase in polyvinyl alcohol (PVA) matrix. Moreover, XRD was used to characterize the PbSe NPs in PVA. The size were controlled by Pb:Se ions ratio in which the particle size was found to be inversely proportional to this ratio up to 16:1. FT‐Raman and FT‐IR measurements indicated the decrease of crystallization of PVA due to doping with PbSe NPs as indicated by the appearance of a peak at 1124 cm^‐1 that increases by size reduction of PbSe NPs. The Photoluminescence and electrical measurements monitored the interaction of PbSe NPs with PVA which increased by decreasing the particle size. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis from zinc oxalate,growth mechanism and optical properties of ZnO nano/micro structures

We report the synthesis of various morphological micro to nano structured zinc oxide crystals via simple precipitation technique. The growth mechanisms of the zinc oxide nanostructures such as snowflake, rose, platelets, porous pyramid and rectangular shapes were studied in detail under various growth conditions. The precursor powders were prepared using several zinc counter ions such as chloride, nitrate and sulphate along with oxalic acid as a precipitating agent. The precursors were decomposed by heating in air resulting in the formation of different shapes of zinc oxide crystals. Variations in ZnO nanostructural shapes were possibly due to the counter ion effect. Sulphate counter ion led to unusual rose‐shape morphology. Strong ultrasonic treatment on ZnO rose shows that it was formed by irregular arrangement of micro to nano size hexagonal zinc oxide platelets. The X‐ray diffraction studies confirmed the wurzite structure of all zinc oxide samples synthesized using different zinc counter ions. Functional groups of the zinc oxalate precursor and zinc oxide were identified using micro Raman studies. The blue light emission spectra of the various morphologies were recorded using luminescence spectrometer. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

碳热原位合成SiC_w/Al_2O_3复相陶瓷粉体的制备工艺及反应机理

本文以高岭土和纳米碳黑颗粒为原料,采用碳热还原原位合成工艺制备SiC_w/Al_2O_3复相陶瓷粉体.通过研究合成温度、保温时间、原料配比以及氩气流量对合成产物的影响,借助XRD、SEM等技术手段进行测试表征,得到了合成工艺的最优参数,并探讨了碳热还原反应的机理.实验结果表明:高岭土与碳黑的摩尔比为1∶ 8,氩气流量为80 mL/min,在1500 ℃下保温2 h,可获得纯净的SiC_w和Al_2O_3复相陶瓷粉体,SiC晶须的平均直径为300 nm左右,长度大于6 μm,长径比大于20,SiC晶须表面光洁,与氧化铝颗粒呈均匀分布.碳热还原高岭土合成SiC_w/Al_2O_3,包括碳热还原SiO_2 与碳热还原莫来石两个阶段,碳化硅晶须的生成遵循气-固(V-S)生长机理.     

Continuous preparation of decorated nano zinc oxide organic sols with intense luminescence

A sort of decorated nano ZnO organic sols have been successively prepared by pulsed laser ablation at the interface of ZnO target and a flowing liquid containing polymers. It is found that the decorated nano ZnO ethanol sols, the decorated nano ZnO-PS (polystyrene) cyclohexane sols and the decorated nano ZnO-PMMA (polymethyl methacrylate) ethyl butyrate sols all have strong fluorescence emission at 329 nm and 411 nm, 308 nm and 317 nm, and at 330 nm and 400 nm, respectively. The results show the decorating for nano ZnO will intensely affect their luminescence, and the wavelength and intensity of luminescence can be adjusted or controlled by the different decoration.     

葡萄糖为碳源的SiC-TiC复合粉末合成工艺研究

以硅溶胶、葡萄糖和TiO2为初始原料,采用碳热还原法在氩气气氛下合成SiC-TiC复合粉末.探讨了不同反应温度对SiC-TiC复合粉末的物相组成、粒径分布、显微形貌等方面的影响.采用X-射线衍射仪(XRD)、激光粒度分析仪、扫描电镜(SEM)等手段对所合成的SiC-TiC复合粉末进行表征.研究结果表明:SiC-TiC复合粉末适宜的合成条件为在1550℃保温2h.在1550℃下合成的SiC-TiC复合粉末主要由少量的片状颗粒、一定量的晶须以及大量的近似球状颗粒构成.粉末样品中SiC晶须的生长机理遵循气-固(VS)机理.     

Microwave assisted synthesis of hydroxyapatite nano strips

Synthesis of hydroxyapatite (HAP) nano strips was carried out by chemical precipitation method followed by microwave irradiation. The microwave assisted reactions proceed at fast rates. It is found that the presence of the complex reagent EDTA plays an important role in the morphological changes of nanostructure hydroxyapatite. EDTA acts as a hexadentate unit by wrapping itself around the Ca²⁺ metal ion with, four oxygen and two nitrogen atoms and forms several five member chelate rings. The relative specific surface energies associated with the facets of the crystal determines the shape of the crystal. Scanning electron microscopy revealed the presence of hydroxyapatite nano strips with the range 50‐100 nm in EDTA influenced HAP powders. Fourier transform‐infrared spectroscopy (FT‐IR) result combined with the X‐ray diffraction (XRD) indicates the presence of amorphous hydroxyapatite (HAP) in the as‐prepared material. X‐ray patterns collected on the powder after heat‐treatment at 1100 °C for 2 h in air exhibits single phase of HAP. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

聚乙烯醇改性磷酸银的光催化活性研究

在制备的磷酸银表面吸附少量的聚乙烯醇(PVA),并通过热处理制备了DPVA/Ag3 PO4复合材料.使用傅立叶红外光谱法(FT-IR)和荧光光谱法(PL)对DPVA/Ag3 PO4复合材料进行表征.分析得知,经聚乙烯醇复合改性的DPVA/Ag3 PO4复合微粒中存在共轭结构,光生电子-空穴对复合率降低,光催化活性得到显著提高.研究了不同条件(复合比例、热处理温度、热处理时间)下制备的复合光催化剂在可见光下催化降解甲基橙的光催化性能.当PVA与Ag3 PO4质量比为1:4000,热处理温度为190℃,热处理1 h时光催化效果最好.     

添加不同稳定剂制备的四方氧化锆晶型转变临界尺寸研究

以八水氧氯化锆(ZrOCl2·8H2O)为原料,以氨水(NH3·H2O)、氢氧化钠(NaOH)溶液为沉淀剂,采用溶胶-凝胶法制备纳米级氧化锆粉体,对前驱体加入不同的稳定剂,通过吸滤、干燥、煅烧等工艺,得到以四方氧化锆晶相为主、不同粒度组成、不同四方相含量的样品.利用激光纳米粒度分析仪、X-射线衍射(XRD)等分析手段分别对粉体的粒径、物相组成进行表征,分别采用晶面公式、谢乐公式对四方相含量、晶粒尺寸进行计算.分析了室温下加入不同稳定剂制备的氧化锆纳米粉体中四方相含量和颗粒粒径之间的关系.结果表明:氧化钇稳定的氧化锆纳米粉粒度更细、粒度分布更均匀.经400~1000 ℃×2 h煅烧后,通过氧化锆纳米粉晶粒尺寸累积分布与四方相含量的关系可以得出以氧化镁、氧化钙、氧化钇为稳定剂制备的氧化锆纳米粉相变临界粒径分别为24~28 nm、26~33.6 nm、18~22.6 nm.     

表面活性剂辅助法制备纳米Z nO及光催化性能研究

以Zn(NO3)2·6H2 O、氨水和不同的表面活性剂为原料,采用沉淀法制备了具有不同微观形貌和尺寸的纳米ZnO,研究表面活性剂对纳米ZnO光催化降解甲基橙性能的影响.通过X射线衍射仪(XRD)、扫描电镜(SEM)和紫外可见分光光度计(UV-Vis)等对所制备纳米ZnO的物相、形貌及光吸收性能进行表征,并对其进行光催化性能测试.结果表明,以CTAB为表面活性剂所制备的纳米ZnO,粒径均匀、分散性良好、无明显团聚现象,并且对甲基橙的光催化降解性能最好,在2 h内降解率可达90.6;.     

Al-Fe3O4体系在机械力化学过程中的物理化学变化

将纳米磁性粒子嵌入到绝缘基体中形成的磁性复合粒子,在许多方面具有重要意义.本文利用Al-Fe3O4通过机械力化学方法原位生成Fe/Al2O3 磁性复合粒子.通过对球磨不同时间的Al-Fe3O4粉末进行X射线衍射(XRD)和示差扫描量热(DSC)分析,结果表明Al-Fe3O4混合粉末通过机械力化学方法可获得Fe/Al2O3复合粒子.同时较为详细地研究了上述体系在机械力化学过程中的物理化学变化,并提出了机械力化学过程中Al-Fe3O4体系固相反应的方式.     

Photoluminescent hierarchical Zno micro‐flower and its surface wettability

The flower‐like ZnO with micro‐nano hierarchical structure is successfully obtained by a simple hydrothermal synthesis, using sodium dodecyl benzene sulfonate (SDBS) as a structure direct agent. The resulted ZnO micro‐flowers are very uniform in morphology with particle sizes around 1 µm. A number of techniques, including X‐ray diffraction (XRD), field emission scan electron microscopy (FESEM), energy‐dispersive spectroscopy (EDS), fourier transform infrared (FTIR) spectra and thermogravimetry analysis (TGA), are used to characterize the obtained ZnO. The self‐assemble of ZnO nano‐sheets under the direction of SDBS leads to the formation of ZnO micro‐flowers. The room temperature photoluminescence property of the obtained flower‐like ZnO exhibits a broad visible light emission. The surface of as‐made ZnO shows a very hydrophilic property, while the special micro‐nano hierarchical structure enables the ZnO micro‐flower a superhydrophobic surface after modification of fluoroalkylsilane.     

High‐performance gas‐sensing properties of octahedral NiO crystals prepared via one‐step controllable synthesis route

Octahedrally shaped NiO powders have been synthesized via a one‐step composite‐hydroxide‐mediated method without any surfactant. The synthesized materials are characterized by XRD, EDS, TEM and FESEM techniques. Each particle exhibited a nearly perfect octahedron shape with sharp edges and corners as well as smooth surfaces. The octahedral NiO particles performed better gas‐sensitivity toward ethanol than that of NiO nanopowders, which was attributed to the exposed ｛111｝ facets of octahedron. The result was confirmed by the first‐principle calculation which indicated that the (111) facet was more active than (100) and (110) facet.     

超声辅助脉冲电沉积Ni-TiN复合镀层制备工艺研究

采用超声辅助脉冲电沉积方法在45#钢表面制备NI-TiN复合镀层..利用X射线衍射仪(XRD)对复合镀层的物相组成进行检测分析,并利用原子力显微镜(AFM)、透射电镜(TEM)对Ni-TiN复合镀层的立体表面形貌及晶粒的分布进行观察分析.结果表明:当超声波功率为300 W时,所制备的Ni-TiN纳米复合镀层衍射峰强度最高,且含有Ni、TiN两相,Ni晶粒得到显著细化,TiN纳米颗粒分布较为均匀,无显著团聚现象发生.     

Tribochemical Synthesis of Magnesium Zirconate for Some Specific Purposes

MgZrO₃ was synthesized by tribochemical and thermal treating of a mixture of MgO and ZrO₂ corresponding to its stoichiometry. The gained compound is identified by chemical and X-ray analysis.