A novel approach for the synthesis of superparamagnetic Mn3O4 nanocrystals by ultrasonic bath

In this study, the synthesis of Mn₃O₄ (husmannite) nanoparticles was carried out in two different alkali media under sonication by ultrasonic bath and conventional method. Manganese acetate was used as precursor, sodium hydroxide and hexamethylenetetramine (HMT) as basic reagents in this synthesis. An ultrasonic bath with low intensity was used for the preparation of nanomaterials. The as prepared samples were characterized with X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, transmission electron microscopy (HRTEM, TEM), energy-dispersive spectrum (EDS), and superconducting quantum interference device (SQUID) analysis. The XRD patterns exhibit the nanocrystals are in pure tetragonal phase. The chemical composition was obtained by EDS analysis and confirmed the presence of Mn and O in the sample. According to the TEM and HRTEM results, both nanorods and nanoparticles of Mn₃O₄ were obtained in the presence of ultrasonic irradiation. The average size of nanoparticles was 10 nm, and the size of nanorods was 12 nm in diameter and 100-900 nm in length for the samples prepared in basic medium with sodium hydroxide. In the conventional method with the same basic medium, the nanorod was not observed and the nearly cubic nanoparticles was appeared with an average size of 2.5 nm. The selected area electron diffraction (SAED) patterns revealed that the nanocrystals are polycrystalline in nature. When HMT was used as a basic reagent in the presence of ultrasonic irradiation, it was led to a higher size of nanoparticles and nanorods than when sodium hydroxide was used as a basic reagent. The average size of nanoparticles was about 15 nm and its shape was nearly cubic. The diameter for nanorods was 50 nm and the length was about a few micrometers.The magnetic measurements were carried out on the sample prepared in sodium hydroxide under ultrasonic irradiation. These measurements as a function of temperature and field strength showed a reduction in ferrimagnetic temperature (T_c = 40 K) as compared to those reported for the bulk (T_c = 43 K). The superparamagnetic behavior was observed at room temperature with no saturation magnetization and hysteresis in the region of measured field strength.     

Co3O4纳米晶的制备和表征

发现了一种新制备Co3O4纳米晶的新方法。这种方法是先将高分子聚乙烯吡咯烷酮(PVP)和乙酸钴溶解到溶剂中缓慢蒸发溶剂,然后干燥形成的前驱体,最后在400℃温度下煅烧制备了Co3O4纳米晶。生成的产物用XRD,SEM,TEM等测试方法进行了表征。结果发现在不同的溶剂中形成前驱体所制备的Co3O4纳米晶具有不同的形貌特征,使用乙醇溶剂时生成了大量的由Co3O4纳米晶自组装形成的Co3O4微米球;而使用水溶剂时则生成的全都是Co3O4纳米晶。实验结果表明在不同溶剂中形成的前驱体对于最终制备的Co3O4纳米晶形态有着很大的影响。     

Submicrocubes and highly oriented assemblies of MnCO3 synthesized by ultrasound agitation method and their thermal transformation to nanoporous Mn2O3

MnCO(3) submicrocubes and highly oriented MnCO(3) nanocrystal assemblies with an ellipsoidal morphology have been successfully prepared by an ultrasonic solution approach. The effect of surfactants of sodium dodecylsulfate (SDS) and aerosol OT (AOT) on the morphology of MnCO(3) was investigated. Highly oriented ellipsoidal assemblies composed of approximately 5 nm MnCO(3) nanocrystals with porous nanostructures were prepared in the presence of SDS. Both sonochemical irradiation and surfactant play an important role in the formation of these highly oriented assemblies. Nanoporous Mn(2)O(3) was obtained by thermal treatment of MnCO(3) at 600 degrees C in air. The shape of MnCO(3) was sustained after thermal transformation to form nanoporous Mn(2)O(3). The products were characterized by X-ray powder diffraction, transmission electron microscopy, selected-area electron diffraction, field emission scanning electron microscopy, thermogravimetric analysis and differential scanning calorimetric analysis.     

Er~(3+),Yb~(3+)共掺杂Y_2O_3纳米晶体粉末中1.5μm近红外发光增强现象的研究

用燃烧法制备了平均粒径为10和40nm的(Y0.96Er0.02Yb0.02)O3纳米晶体样品,并通过1200℃高温退火获得了同样组分的体材料样品。利用X射线衍射谱(XRD),傅里叶变换红外吸收光谱(FTIR),透射电镜(TEM)和透射电镜(SEM)照片对样品的晶体结构和形貌进行了表征。测量了不同样品980nm激发下的上转换发射光谱和近红外发射光谱。对实验结果的分析发现,随着粒径的减小,样品发射光谱中红光和近红外发射的成分增加。产生这一现象的原因是由于纳米材料具有比表面积大的特点,能够吸附更多的OH-(振动能量3200～3800cm-1),OH-数量的增加使电子从Er3+的4I11/2→4I13/2能级(能量差3600cm-1)的无辐射弛豫速率增大,这一无辐射弛豫过程减少了4I11/2上的电子布居数,使绿光发射减弱;同时增加了4I13/2上的电子布居数,使红光和近红外发射增强。40nm样品的1.5μm发射主峰强度是体材料的1.6倍,这一结果对纳米发光材料的实际应用是很有意义的。     

Ultrasound-assisted coating of silk yarn with sphere-like Mn3O4 nanoparticles

The growth of sphere-like trimanganese tetraoxide (Mn₃O₄) nanoparticles on silk fiber was achieved by sequential dipping in an alternating bath of potassium hydroxide and manganese(II) nitrate under ultrasound irradiation. Some parameters such as the effect of pH, numerous sequential dipping and ultrasonic irradiation on growth of the nanoparticles have been studied. The samples were characterized with powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and wavelength dispersive X-ray (WDX).     

Oxidative Precipitation as a Versatile Method to Obtain Ferromagnetic Fe3O4 Nano- and Mesocrystals Adjustable in Morphology and Magnetic Properties

Oxidative precipitation is a facile synthesis method to obtain ferromagnetic iron oxide nanoparticles from ferrous salts—with unexplored potential. The concentration of base and oxidant alone strongly affects the particle's structure and thus their magnetic properties despite the same material, magnetite (Fe₃O₄), is obtained when precipitated with potassium hydroxide (KOH) from ferrous sulfate (FeSO₄) and treated with potassium nitrate (KNO₃) at appropriate temperature. Depending on the potassium hydroxide and potassium nitrate concentrations, it is possible to obtain a series of different types of either single crystals or mesocrystals. The time-dependent mesocrystal evolution can be revealed via electron microscopy and provides insights into the process of oriented attachment, yielding faceted particles, showing a facet-dependent reactivity. It is found that it is the nitrate and hydroxide concentration that influences the ligand exchange process and thus the crystallization pathways. The presence of sulfate ions contributes to the mesocrystal evolution as well, as sulfate apparently hinders further crystal fusion, as revealed via infrared spectroscopy. Finally, it is found that nitrite, as one possible and ecologically highly relevant reduction product occurring in nature in context with iron, only evolves if the reaction is quantitative.     

磁性纳米级Fe3O4的氧气诱导、空气氧化液相合成与表征

氧气诱导、空气氧化液相合成出了粒径为20nm左右的磁性粉体Fe3O4。由X-ray衍射，红外光谱(IR)、透射电镜(TEM)及磁滞回线方法表征了粒子的结构组成。     

Co3O4纳米花的合成及其磁性

通过水热和热处理的方法，制备了产物Co3O4纳米花. 用X射线粉末衍射、场发射扫锚电镜、透射电镜和红外光谱等手段对产物进行了表征. 结果表明，产物纳米花是由大量的Co3O4纳米须组成，纳 米须的直径为20?40 nm，长度为100?500 nm，具有纳米孔结构，比表面积约为34.61 m2/g. 磁性测量表明，在零场冷却条件下，产物主要表现为反铁磁性；在加场冷却条件下，闭锁温度约为34K时，产物主要表现为铁磁性．     

Hydrothermal synthesis and optical characteristics of Eu in Zn2SnO4 nanocrystals

Zn₂SnO₄:Eu³⁺ nanocrystals were one-step synthesized by hydrothermal method for the first time. All the products were systematically characterized by powder X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), electron probe X-ray microanalyzer (EPMA), photoluminescence (PL) and photoluminescent excitation (PLE). The characteristic peak of Eu³⁺-doped in Zn₂SnO₄ nanocrystals was also detected. The luminescent properties of blank and Eu³⁺-doped Zn₂SnO₄ nanocrystals were reported.     

Sonochemical synthesis and characterization of Co3O4 nanocrystals in the presence of the ionic liquid [EMIM][BF4]

For the first time, a sonochemical process has been used to synthesis cobalt oxide Co₃O₄ nanoflowers and nanorods morphology in the presence of the ionic liquid 1-Ethyl-3-methylimidazolium tetrafluoroborate [EMIM][BF₄] as reaction media and morphology template. Different sonication time periods and different molar ratios of the ionic liquid (IL) were used to investigate their effects on the structural, optical, chemical and magnetic properties of the produced Co₃O₄ nanoparticles. During synthesis process brown powder contains cobalt hydroxide Co(OH)₂ and cobalt oxyhydroxide (Cobalt hydroxide oxide) CoO(OH) was formed, after calcination in air for 4 h at 400 °C a black powder of Co₃O₄ nanoparticles was produced. The produced Co₃O₄ nanoparticles properties were characterized by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), transmission electron microscopy (TEM), FTIR spectroscopy, UV–vis spectroscopy, and Vibrating Sample Magnetometer (VSM). To explain the formation mechanism of Co₃O₄ NPs some investigations were carried on the brown powder before calcination.     

Catalytic performance of Mn3O4 and Co3O4 nanocrystals prepared by sonochemical method in epoxidation of styrene and cyclooctene

A simple sonochemical method was developed to synthesis uniform sphere-like Co₃O₄ and Mn₃O₄ nanocrystals. Epoxidation of styrene and cyclooctene by anhydrous tert-butyl hydroperoxide over the prepared Co₃O₄ and Mn₃O₄ nanocatalysts was investigated. The results of conversion activity were compared with bulk Co₃O₄ and Mn₃O₄. Under optimized reaction conditions, the nanocatalysts showed a superior catalytic performance as compared to the bulk catalysts. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and BET surface area, were used to characterize and investigate the nanocatalysts.     

内嵌碳正八面体形貌Co3O4光催化活性研究

基于脱脂棉为牺牲模板,采用碳辅助法制备了内嵌碳的八面体形貌Co3O4,对其在模拟阳光下的光解水制氢气的能力进行了研究。X射线衍射（XRD）和扫描电镜（SEM）表征分析表明,制备的产物是具有规则正八面体形貌、粒径约为10 m的具有良好晶型的Co3O4。能谱（EDS）和光射线光电子能谱（XPS）结果表明,制备的产物内嵌无定形碳,碳源来自于脱脂棉制备过程中的不完全燃烧。实验结果表明制备的内嵌碳八面体形貌Co3O4具有良好的光解水制氢能力。     

One-step synthesis of Fe3O4 nanorods/graphene nanocomposites

A composite of graphene (GE) supported by rod-like Fe₃O₄ nanocrystals has been fabricated by a simple one-step chemical route. X-ray diffraction and transmission electron microscopy results show that the Fe₃O₄ nanorods with diameters in the range of 15?C20 nm and lengths of 150?C200 nm were firmly assembled on the GE nanosheet surface. Magnetic property investigation indicated that the Fe₃O₄/GE composites exhibit a ferromagnetic behavior and possess a saturation magnetization of 50.11?emu?g^?1. Moreover, Fe₃O₄/GE composites showed a very high adsorption capacity of Congo red.     

NaGdF4纳米晶多元醇法的合成、表征与NaGdF4：Eu3+和NaGdF4：Yb3+, Er3+纳米晶的发光

通过多元醇法(polyol method)合成出NaGdF₄:Eu³⁺和NaGdF₄:Yb³⁺,Er³⁺纳米晶,利用X射线衍射(XRD)、场发射扫描电镜(FE-SEM)和傅立叶变换红外吸收光谱(FT-IR)对合成的样品进行了表征。研究了Eu³⁺掺杂样品的下转换发光和Yb³⁺/Er³⁺共掺杂样品的上转换发光。对未经退火和经过退火的样品进行了比较。     

Ag/K_4Nb_6O_(17)异质结催化剂的制备、光谱分析及光催化性能研究

采用低温水热法成功制备了层状的K4Nb6O17半导体光催化材料。考虑到水热合成的K4Nb6O17表面多羟基(Nb—OH)和端氧(Nb O,Nb—O-)的特点,采用Ag(en)2+配合物前驱体法制备了高度均匀分散的Ag/K4Nb6O17异质结光催化剂,光催化性能评价结果表明,半导体K4Nb6O17表面负载极少量的Ag,其光催化降解甲基橙活性便得到大幅度提高,Ag的最佳负载量为0.5 at%。综合XRD,FTIR,UV-VisDRS,XRF和TEM表征结果,对Ag/K4Nb6O17异质结光催化剂的作用机制进行了较详细地阐述并获得如下结论:(1)K4Nb6O17提供了降解有机染料分子的电子和空穴;(2)K4Nb6O17纳米晶上Ag粒子作为光生电子接受器,促进了金属-半导体界面上电荷的转移,有效地分离了光生电子-空穴对,提高了光催化活性。     

Crystallization of CaAl4O7 and CaAl12O19 powders

Calcium is always present in alumina systems as an unintentional (or intentional) dopant, and yet the fundamental effect of its incorporation into the aluminas is not well understood, and is further complicated by the presence of Si. The synthesis of powders of two calcium aluminate phases (CaAl₄O₇, which is also known as CaO · 2Al₂O₃ or CA₂, and CaAl₁₂O₁₉, which is also known as CaO · 6Al₂O₃ or CA₆) has been investigated using low-temperature chemical-processing techniques. The crystallization of these powders from the amorphous precursor has been examined using various characterization techniques. The precursors for the powders were prepared by mixing stoichiometric proportions of the nitrate salts into a 5 wt% aqueous solution of poly(vinyl alcohol). Conversion of the amorphous precursors to crystalline powders and the subsequent phase transitions were monitored using differential thermal analysis (DTA), thermogravimetric analysis (TGA) and powder X-ray diffractometry (XRD). While powders with CA₂ stoichiometry crystallized directly at 883°C, amorphous powders with CA₆ stoichiometry first crystallized into an intermediate structure without partitioning and then transformed into CA₆ at 1175°C. Fully and partially crystallized powders were analyzed using transmission electron microscopy and electron energy-loss spectroscopy (EELS). Measured near-edge structures (Al–L_2,3, Ca–L_2,3 and O–K) are presented for the CA₂, γ-Al₂O₃ and CA₆ phases. The intermediate phase, identified as γ-Al₂O₃, was found to accommodate a significant concentration of Ca.     

Hydrothermal synthesis of CeF<Subscript>3</Subscript> nanocrystals and characterization

CeF₃ nanocrystals with plate-like and perforated morphologies were successfully synthesized via a facile hydrothermal route. The nanocrystals of CeF₃@silica can dispersed in aqueous solution were also prepared. The effects of fluoride sources on the morphology and microstructure of the nanocrystals were investigated by means of transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), and powder X-ray diffraction (XRD). Results indicate that the morphology of the rare earth compound nanocrystals can be well tuned by selecting proper fluoride sources. The ultraviolet (UV) absorption peak of the CeF₃ nanocrystals is slightly blue shifted along with the decrease of size. And the photoluminescence (PL) intensity of the CeF₃ nanocrystals is closely related to size and microstructure as well.     

纳米晶La2O3的制备及其红外吸收特性的研究

采用硬脂酸凝胶法制备了La2O3纳米晶,用X射线粉末衍射仪(XRD),透射电子显微镜(TEM)对La2O3纳米晶的粒径和形貌进行了表征.研究了不同热处理温度下纳米La2O3的红外吸收特性,结果表明,La2O3纳米晶的吸收峰的宽化、吸收峰发生蓝移和红移现象,同时La2O3纳米晶在1 000～1700 nm之间吸收较好,有可能用作激光隐身涂料的吸收剂.     

物理分析技术在无机氧化物晶体结构表征中的应用

以氯化锌和氢氧化钠为主要原料,采用简单液相法,通过改变反应液的组成,制备出了针状、棒状、片状和花状四种不同形貌的ZnO微/纳米晶体。应用X-射线粉末衍射仪（XRD）,扫描电子显微镜（SEM）、高分辨透射电子显微镜（HRTEM）及选区电子衍射仪（SEAD）对产物进行表征,获得了ZnO物相、形貌与微观结构的重要信息。     

NiFe_2O_4纳米粉末的制备及磁性研究

以硝酸铁、硝酸镍以及柠檬酸为原料,采用凝胶-热分解法制备了N iFe2O4纳米粉末。利用X射线衍射确定了粉体的相结构、比表面积和晶格常数,扫描电子显微镜(SEM)观察了颗粒的形貌,振动样品磁强计(VSM)测量样品的磁性能。结果表明:所制备的样品均为尖晶石结构,颗粒粒径为36nm~68nm,且颗粒的粒径随着热处理温度的升高而增大,样品的比饱和磁化强度最大可达54.63 emu/g。同时,文章也对反应的动力学原理进行了研究,得出N iFe2O4纳米颗粒形成的活化能为15.8kJ/mol。