氧化锌铝包覆硼酸钐粉体的制备及性能表征

为了获得具有较低红外发射率和激光反射率的复合材料,通过将氧化锌铝复合于硼酸钐表面的方法,获得了复合效果较好、红外发射率和激光反射率都相对较低的氧化锌铝/硼酸钐纳米复合粒子。用共沉淀法制备了氧化锌铝包覆硼酸钐纳米复合粉体,从包覆前后的电镜照片可以看到包覆层的厚度约为250nm。并且研究了包覆过程中m(硼酸钐):m(氧化锌)、处理硼酸钐所用盐酸的浓度和包覆前驱体的煅烧温度等因素对红外发射率和激光反射率的影响。结果表明,m(硼酸钐):m(氧化锌)为1.5:1、盐酸浓度为0.4mol/L、煅烧温度为650℃时红外发射率和激光反射率最低,最低的红外发射率为0.70、最低的激光反射率为0.73%。     

沉淀法制备氧化锌粉体

以碳酸钠和硫酸锌为原料,采用沉淀法制备前驱体碱式碳酸锌,前驱体经过热分解得到氧化锌粉体。采用热重分析（TG-DTG-DTA）、X射线衍射（XRD）、红外光谱（IR）和扫描电镜（SEM）等方法对前驱体和产品氧化锌进行表征。结果表明：制备的前驱体为碱式碳酸锌Zn4（OH）6CO3;以水、乙二醇为溶剂及聚乙二醇（PEG）为分散剂,均可制备出较为纯净的氧化锌;乙二醇为溶剂和PEG为分散剂,改善了氧化锌的形貌和分散性,避免了氧化锌团聚。     

微波水热法用于制备纳米氧化锌粉体的研究

以氯化锌和氢氧化钠为原料,采用微波水热法制备了纳米氧化锌粉体,并采用X射线衍射（XRD）和透射电镜（TEM）对粉体的粒度、形貌、纯度进行了表征。通过单因素实验考察了反应温度、微波反应时间、微波功率、锌离子与氢氧根的浓度比等因素对氧化锌粉体的产率和粒径的影响,再通过正交试验得到最优制备条件。最佳制备工艺条件：锌离子与氢氧根的浓度比为1∶1.2、反应温度为 120 ℃、反应时间为 10 min、微波功率为500 W。在此条件下所得氧化锌粉体的晶型为六方晶相,产率达到93.5%,平均粒度约70 nm,粒径分布较窄,结晶完整。     

利用水热法和添加籽晶制备纳米AlOOH粉体

以Al(NO3)3·9H2O和氨水为原料,以水为反应介质,采用水热法制备纳米AlOOH粉体.通过DSC/TG和XRD分析了不同热处理温度下粉体的晶型转变和成分.利用SEM和粒度仪分析了不同水热温度以及不同籽晶对晶粒形貌的影响.结果表明,当水热反应温度低于380℃时,所获得的粉体成分均为AlOOH,颗粒均为纳米尺度;水热反应温度的提高有利于获得形貌规则的晶粒;加籽晶比不加籽晶所得粉体的粒径小且分布均匀;加纳TiO2作籽晶比加纳米α-Al2O3作籽晶所得粉体的粒径小.     

管式气体分散式反应器制备纳米碳酸钙

以石灰石为原料，利用管式气体分散式反应器新工艺制备出了粒径30～70nm的碳酸钙粉体。采用X射线衍射（XRD）、扫描电镜（SEM）、粒度分布仪及红外光谱仪（Fr-IR）等测试手段，对产品的物相、形貌和粒度分布进行了表征。X射线衍射表明产物为六方晶系方解石型碳酸钙并且产品结晶性能良好；扫描电镜及粒度分析表明粒度大小均匀、分散性良好；红外光谱表明改性后硬脂酸钠已吸附在碳酸钙表面，碳酸钙颗粒基本呈单分散状态。管式气体分散式反应器制备纳米碳酸钙粉体的优点是工艺简单，操作容易，原料易得，生产的产品粒径小，粒度分布窄，易于工业化生产。     

纳米氧化亚镍包覆Al复合粒子的制备

为了获得具有良好红外吸收特性及低发射率复合颜料,通过将纳米NiO复合于片状金属铝粉表面的方法,获得了复合效果好的纳米NiO/Al复合粒子.为了保证复合物的红外伪装性能,通过对复合前驱体Ni₂CO₃(OH)₂/Al的热分析,确定了对复合物的热处理温度.通过对复合物热处理前后的电镜照片分析,发现热处理前复合物表面是由线状的Ni₂CO₃(OH)₂交织而成的,而热处理后则变成了由纳米球状NiO粒子连接而成的球链.这种现象在同类研究中尚未见报道.对比所制备的纳米NiO/Al和NiO的XRD图谱,发现纳米NiO/Al中的NiO衍射峰宽化,表现出纳米粒子的特征,由半高宽计算出其晶粒粒径为12 nm.     

水/油微乳液技术制备单分散纳米CeO2

在十六烷基三甲基溴化铵 正丁醇/环己烷/水溶液组成的水/油型微乳液体系中,运用微乳液制备纳米粒子的原理,利用改进的两相液液法,测定了水/油微乳液的区域,并制备了纳米CeO2粉体.对制备得到的CeO2粉末的形貌特征、物相结构、成分等用透射电子显微镜、X射线衍射分析、热重-差示扫描量热法和红外光谱测试进行了表征.结果表明:在测定的微乳液区内能制备出颗粒分散性好,粒度分布均匀的纳米CeO2粒子,所得颗粒尺寸为3 nm左右.     

Ni(OH)_2水浆蒽醌催化水热还原制备超细镍粉

以蒽醌作催化剂，水热加氢还原从Ni（OH）2水浆制备了超细镍粉．研究了催化剂量、温度、时间、氢分压、浓度和pH等因素对还原速度和粉末粒度的影响，还原率通过X-射线衍射分析本被还原的镍来确定．用扫描电镜观察分析了粉末的粒度与形貌.研究表明，在温度高于200℃的条件下，蒽醌对Ni（OH）2浆料还原成金属镍粉是一种良好的催化剂．所得的粉末是平均粒径约为300nm的球状超细镍粉.     

利用水热法和添加籽晶制备纳米AIOOH粉体

以Al(NO3)3·9H2O和氨水为原料,以水为反应介质,采用水热法制备纳米AlOOH粉体。通过DSC/TG和XRD分析了不同热处理温度下粉体的晶型转变和成分。利用SEM和粒度仪分析了不同水热温度以及不同籽晶对晶粒形貌的影响。结果表明,当水热反应温度低于380℃时,所获得的粉体成分均为AlOOH,颗粒均为纳米尺度;水热反应温度的提高有利于获得形貌规则的晶粒;加籽晶比不加籽晶所得粉体的粒径小且分布均匀;加纳米TiO2作籽晶比加纳米αAl2O3作籽晶所得粉体的粒径小。     

镧掺杂钛酸钡粉体的水热改性

以固相法合成的BaTiO3粉体和La(NO3)3溶液为反应前驱物,NaOH为矿化剂,对BaTiO3粉体表面进行镧掺杂水热改性。利用X射线衍射仪、扫描电镜、Fourier红外光谱仪和透射电镜等研究了水热处理后BaTiO3粉体及陶瓷的相组成、晶粒尺寸、颗粒形貌及电性能。结果表明:对不同镧掺杂浓度的BaTiO3粉体进行水热处理后,粉体粒径变小,粒度分布范围变窄,颗粒形貌变得圆整,实现了高温、高压条件下的水热"整形"作用。在BaTiO3粉体颗粒表层形成了一层约50nm厚的富镧层,实现了高温高压下对BaTiO3陶瓷粉体的改性。将改性后的BaTiO3粉体制成陶瓷,其室温电阻率测试结果表明,经水热处理后的粉体改善了镧在钛酸钡陶瓷中的掺杂均匀性,掺杂半导化浓度范围加宽。     

Preparation and Characterization of Sn-doped ZnO Particles with Low Infrared Emissivity

Sn-doped ZnO particles were successfully synthesized by chemical co-precipitation method. Their morphology, phase, microstructure and infrared emissivity were characterized. The results show that the Sn-doped ZnO particles are of ellipsoid shape, their crystalline structure changed with thermal process temperature, the optimal thermal process temperature and Sn-doped proportion are 1000℃ and 15%, respectively, the minimum emissivity values are 0.42, 0.28, 0.46 and 0.48 corresponding to the infrared wavelengths of 0~∞, 3~5, 8~14 and 14~20 mm, which indicates that the Sn-doped ZnO particles have the application potential as low infrared emissivity material.     

超声辅助均匀沉淀法由前躯体ZnS制备ZnO纳米颗粒及其表征

前躯体ZnS在超声辅助60℃的低温条件下,采用醋酸锌为锌源、硫代乙酰胺为硫源来制备,然后采用在空气中热处理前躯体ZnS的方法制备了直径约为20~40 nm的ZnO纳米颗粒。所得产物分别采用红外光谱(FTIR)、热重-差热分析(TGA-DTA)、X射线衍射(XRD)、场发射扫描电镜(FE-SEM)、透射电镜(TEM)、电子能谱(EDS)和荧光光谱(PL)进行表征。实验结果表明,所得产物ZnO为六方纤锌矿结构,且结晶性很好,并且随着超声时间的延长其粒径有所降低。室温PL光谱表明,样品在400~550 nm内有3个较强的荧光发射峰。     

Al掺杂对甲醇醇解法合成ZnO纳米粉体的影响

采用醇解法,在130℃的甲醇溶液中分别合成纯的和Al掺杂纳米氧化锌(ZnO)晶体.使用X射线衍射仪,透射电子显微镜,Fourier红外光谱和偏振稳态荧光光谱对其晶体结构和光学性能进行了表征.结果表明:在甲醇溶液中,在较低的温度(130℃)下,成功制备出纳米ZnO晶体.Fourier红外吸收光谱表明醇解法合成的ZnO纳米晶体含有较少的有机物杂质.荧光光谱结果可以看出,纯ZnO和Al掺杂的ZnO纳米晶体在可见光范围(400nm～700nm)内有一个高的蓝光发光带(峰位为440nm)和一个绿光发光带(纯的和Al掺杂的峰位分别为520nm和530nm).通过对比发现掺杂Al可以有效的改变ZnO纳米粉体的可见光发光特性.     

Growth and optical properties of hierarchical flower-like ZnO nanostructures

The integration of low dimensions nanoscale building blocks into 3D architectures has attracted great scientific attention. We have obtained the novel hierarchical flower-like ZnO nanostructures self-assembled by nanorods via a facile hydrothermal method. The as-synthesized samples were characterized with various technologies. The field emission scanning electron microscope (FESEM) images indicated that hydroxide ions play a significant role on the formation of hierarchical flower-like ZnO nanostructures. The X-ray diffraction (XRD) result proved that the nanocrystals were well crystallized hexagonal wurtzite structure. A possible growth mechanism of the nanostructures was proposed based on the effects of hydroxide ions. And the TEM imagines provided some important evidence for the proposed growth mechanism. UV–vis adsorption and photoluminescence (PL) spectra results indicated that the obtained ZnO nanostructurs have a good optical-absorption and photoluminescence property. The as-synthesized ZnO nanostructures exhibited superior photocatalytic performance, which was higher than that of commercially available ZnO.     

Temperature-dependent infrared emissivity property of Ce-doped ZnO nanoparticles

The low infrared emissivity materials with good high-temperature properties remain a challenge for the infrared stealth of hot targets in 3–5 μm waveband. To further decrease the infrared emissivity of ZnO, the Ce-doped ZnO nanoparticles were prepared by a facile sol-gel method and the infrared emissivity properties in 3~5 μm waveband in high temperature conditions were deeply investigated by doping different concentration of Ce in ZnO. The influences of Ce dopant concentration on the microstructure, morphology, conductivity, lattice vibration and high-temperature infrared emissivity properties of Ce-doped ZnO were systematically studied, as well as the detailed analysis of temperature-dependent infrared emissivity properties through the conductivity and lattice vibration based on the theory of solid state physics. When the Ce dopant concentration is 3%, the infrared emissivity of Ce-doped ZnO decreases dramatically from room temperature to 800 °C in comparison with undoped ZnO and reaches the lowest value of 0.329 at 500 °C. It is indicated that the excess doping of Ce would produce an impurity phase of CeO₂ in the crystal, therefore decreases the conductivity, and causes extra lattice vibration in infrared region, and results in the increase of infrared emissivity. The infrared emissivity versus temperature exhibits a “U” type curve, which is caused by the competition effects of the conductivity and lattice vibration at elevated temperature.     

Fabrication and properties of ZnO/GaN heterostructure nanocolumnar thin film on Si (111) substrate

Zinc oxide thin films have been obtained on bare and GaN buffer layer decorated Si (111) substrates by pulsed laser deposition (PLD), respectively. GaN buffer layer was achieved by a two-step method. The structure, surface morphology, composition, and optical properties of these thin films were investigated by X-ray diffraction, field emission scanning electron microscopy, infrared absorption spectra, and photoluminiscence (PL) spectra, respectively. Scanning electron microscopy images indicate that the flower-like grains were presented on the surface of ZnO thin films grown on GaN/Si (111) substrate, while the ZnO thin films grown on Si (111) substrate show the morphology of inclination column. PL spectrum reveals that the ultraviolet emission efficiency of ZnO thin film on GaN buffer layer is high, and the defect emission of ZnO thin film derived from Zn_i and V_o is low. The results demonstrate that the existence of GaN buffer layer can greatly improve the ZnO thin film on the Si (111) substrate by PLD techniques.     

铅笔状ZnO生长机理的研究及光催化性能表征

用水热法于175℃合成了铅笔状ZnO。并通过XRD、EDS、SEM、TEM和HRTEM对不同碱性条件下合成的ZnO的形貌进行了分析,结果表明,n(OH-)∶n(Zn2+)=4∶1时,ZnO的形貌为平均厚度90nm的片状结构;当n(OH-)∶n(Zn2+)=10∶1时,ZnO的形貌为直径200nm、长度2.5μm的铅笔状结构。探讨了不同形貌的ZnO的形成机理。用UV-vis吸收光谱和PL光谱分析了ZnO的形貌对次甲基蓝光催化降解的影响,结果发现,铅笔状氧化锌的光催化性能优于片状氧化锌。     

Tailoring the properties of cerium doped zinc oxide/reduced graphene oxide composite: Characterization,photoluminescence study,antibacterial activity

Ce doped ZnO/rGO composite materials were prepared by a one-pot hydrothermal process without any surfactant. The size, crystallography and morphology of the composite were investigated in detail by X- ray diffraction (XRD) studies, Raman spectroscopy, scanning electron microscopic (SEM), transmission electron microscopic (TEM) studies, UV–Vis spectroscopic analysis and X-ray photoelectron spectroscopic (XPS) analysis. The XRD pattern substantiates the formation of Ce doped ZnO/rGO composite revealing the wurtzite structure of ZnO. The SEM micrograph illustrates flower-like morphology for ZnO/rGO composite which coalesced further after cerium incorporation. Additionally, TEM image illustrated that ZnO hexagons were disoriented from its flower structure in Ce/ZnO/rGO composite. The XPS spectra further reaffirm the formation of cerium doped ZnO/rGO composite. The photoluminescence (PL) spectra confirms that emission occurs in the UV and visible region and several active sub-levels were observed in visible region on deconvolution, due to the incorporation of cerium. Antibacterial activity towards B. subtills and V. harveyi affirmed that the incorporation of Ce in ZnO/rGO composite leads to an improved antibacterial activity.     

Hydrothermal Synthesis of CdMoO4 Nano-Particles

CdMoO₄ nano-particles were successfully synthesized by a hydrothermal process at a low temperature of 90°C, and the powders were characterized in detail by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, and photoluminescent spectra techniques (PL), respectively. CdMoO₄ particles could be obtained under the hydrothermal condition from micrometer to nanometer sizes by varying their precursors. The PL spectra results showed that the optical properties of CdMoO₄ crystallites obviously relied on their particle sizes.     

A green and facile one-pot synthesis of Ag–ZnO/RGO nanocomposite with effective photocatalytic activity for removal of organic pollutants

In this study, Ag–ZnO/reduced graphene oxide (Ag–ZnO/RGO) composite was synthesized by a green and facile one-step hydrothermal process. Aqueous suspension containing Ag and ZnO precursors with graphene oxide (GO) sheets was heated at 140 °C for 2 h. The morphology and structure of as-synthesized particles were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman spectroscopy, and Photoluminescence (PL) spectroscopy which revealed the formation of composite of metal, metal oxide and RGO. It was observed that the presence of Ag precursor and GO sheets in the hydrothermal solution could sufficiently decrease the size of ZnO flowers. The hybrid nanostructure, with unique morphology, obtained from this convenient method (low temperature, less time, and less number of reagents) was found to have good photocatalytic and antibacterial activity. The perfect recovery of catalyst after reaction and its unchanged efficiency for cyclic use showed that it will be an economically and environmentally friendly photocatalyst.