Synthesis and magnetic properties of shuriken-like nickel nanoparticles

Shuriken-like nickel nanoparticles were successfully synthesized by a thermal decomposition method at 200 °C with Nickel(II) acetylacetonate (Ni(acac)₂) as the precursor and oleylamine (OAm) as the solvent and reductant, respectively. The phase structures, morphologies and sizes, and magnetic properties of the as-synthesized nickel products were characterized in detail by using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission-scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM). Some key reaction parameters, such as the reaction time, reaction temperature and surfactants, have important influence on the morphology of the final products. XRD pattern indicated that the products are well-crystallized face-centered cubic (fcc) nickel phase. SEM images demonstrated that the nickel nanoparticles are shuriken-like morphology with average size around 150 nm. The mechanism of shuriken-like Ni nanoparticles (NPs) is proposed. The magnetic hysteresis loops of shuriken-like and spherical nickel products illustrated the ferromagnetic nature at 300 K, indicating its potential applications in magnetic storage.     

多孔NiO纳米棒:可牺牲模板法制备及其磁性(英文)

本文基于微乳液法制备了长度几微米、直径20-100纳米的NiC2O4纳米棒,以此为可牺牲模板得到多孔NiO纳米棒,并采用FESEM、TEM、HRTEM、XRD、FTIR对产物的形貌和结构进行了表征。研究表明,所制多孔NiO纳米棒是由NiO颗粒组成,且NiO颗粒的直径可随热处理温度变化。同时研究了NiO纳米棒的磁性性能,制备的NiO纳米棒显示出随NiO颗粒尺寸变化的铁磁性特征。     

A new route to synthesis of γ-alumina nanorods

γ-Alumina single-crystalline nanorods have been successfully synthesized by thermal decomposition of boehmite precursor which was prepared by solvothermally treating AlCl₃ ⁎ 6H₂O, NaOH, sodium dodecyl benzene sulfonate in water and dimethylbenzene mixed solvents. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). Our experiments show that the surfactant plays an important role in the morphology and assembly of boehmite. Photoluminescence (PL) spectrum of the boehmite nanorods was also investigated.     

海藻酸钠调控羟基磷灰石纳米棒的低温快速合成

以海藻酸钠为晶体生长调节剂, 在水热条件下制备了形貌均匀、高长径比的羟基磷灰石(Hydroxyapatite, HA)单晶纳米棒。通过X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、场发射扫描电镜(FE-SEM)、透射电镜(TEM)以及同步热分析(TG/DSC)等测试方法对合成产物进行了表征, 探索了反应温度和时间对产物的结晶度、组成以及形貌的影响, 并提出了HA纳米棒的合理生长机理。研究表明, 80℃水热条件, 反应24 h, 对于均匀、低有机吸附量的HA单晶纳米棒合成较有利。对纳米棒的不同生长阶段的微结构分析表明: 晶体生长经历了成核、表面调控、继续生长和取向搭接四个阶段。     

Synthesis of single-crystal PbS nanorods via a simple hydrothermal process using PEO-PPO-PEO triblock copolymer as a structure-directing agent

Single-crystal PbS nanorods were successfully synthesized through a simple hydrothermal route using PEO-PPO-PEO triblock copolymer (P123) as a structure-directing agent. The XRD pattern indicates that the crystal structure of the nanorods is face-centre-cubic rocksalt. A SEM image shows that the nanorods have a diameter of 40-70 nm and a length of 200-600 nm, and both tips exhibit taper-like structures. HRTEM and SAED images reveal the single-crystalline nature of the nanorods with the growth along the (111) direction. The experimental results indicated that the P123 concentration and reaction temperature played important roles in controlling the morphology of the PbS nanostructures. The optical property of PbS nanorods was investigated by UV-Vis absorption spectroscopy and the band structure was calculated by the B3LYP hybrid density functional theory.     

水热合成与热分解法制备氧化铝纳米棒

以氢氧化铝和氢氧化锂为原料, 在120℃反应10～17d的水热条件下, 制备出Al(OH)₃·xH₂O前驱物. 此前驱物经400℃热分解1h, 得到了Al₂O₃纳米棒. 通过TEM、HRTEM、SAED和XRD等分析手段对产物进行了表征, 并以TGA分析Al(OH)₃·xH₂O前驱物受热分解时的热力学行为. 实验结果发现: 产物形貌为棒状, 呈现单晶特性. 纳米棒的成长符合Ostwald熟化与方向附着机制. 同时发现了碱液对纳米棒的形成有很大的影响, 以5mol/L KOH碱液取代原来的LiOH碱液时, 出现更细小形貌的纳米线, 尺寸为φ2nm×(10～25)nm.     

小型金纳米棒的制备

用种子生长法合成小型金纳米棒,改变合成参数可调控其形貌和性能。使用紫外-可见-近红外分光光度计和透射电子显微镜(TEM)测试和观察了金纳米棒的消光特性和形貌,研究了AgNO₃、十六烷基三甲基溴化铵(CTAB)和籽晶的用量对金纳米棒的形貌和性能的影响。结果表明：在不同条件下制备的金纳米棒具有良好的重现性。在(0.01 mol/L) AgNO3用量为0.035 mL、(0.1 mol/L) CTAB用量为11 mL、籽晶用量为1.1 mL的最佳条件下合成的金纳米棒,其长径比约为3.8,平均长度约为34 nm,形貌均匀性和分散性良好。这种小型金纳米棒可用于检测残留物福美双(Thiram)。     

氨基功能化磁性FeO(OH)纳米棒的制备研究

在获得表面修饰氨基官能团的磁纳米棒,为进一步偶联生物分子制备出磁生物双靶向纳米药物奠定基础.以部分氧化法制备了磁性FeO(OH)纳米棒,并在保持原有形貌的基础上对其进行硅胶包覆和氨基功能化,从而获得功能化磁纳米药物载体.磁纳米棒的形貌特征、晶体结构、磁性质和表面基团分别通过TEM(SAED)、XRD、VSM和FTIR进...     

双氮二甲基甲酰胺介导溶剂热合成CuS粉体及表征

以CuCl2.2H2O为铜源,N,N-二甲基甲酰胺(N,N-dimethylformamide,DMF)为溶剂,分别以L-半胱氨酸、硫脲、硫代乙酰胺为硫源采用溶剂热法在130℃下反应8h得到了不同形貌的硫化铜(CuS)纳米粉体。用X射线粉末衍射仪、X射线光电子能谱、场发射扫描电子显微镜、透射电子显微镜、紫外可见吸收光谱手段对粉体的结构、形貌、成分及光学性能进行表征。研究表明,硫源对产物的结构和形貌有较大的影响。采用L-半胱氨酸为硫源得到的产物多呈纳米颗粒无序堆积的无定形态,而采用硫脲和硫代乙酰胺为硫源得到的是纳米棒组成的球状粉体。讨论了不同硫源对CuS粉体的形成及其形貌的影响,并对各种形貌CuS粉体的形成机理进行了简单的探讨。     

Effect of Oxide Assisted Metal Nanoparticles on Microstructure and Morphology of Gallium oxide Nanowires

Several researches have been reported about the characteristic of β-Ga2O3 nanowires which was synthesized on nickel oxide particle. But indeed, recent researches about synthesis of β-Ga2O3 nanowires on oxide-assisted transition metal are limited to nickel or cobalt oxide catalyst. In this work, Gallium oxide (β-Ga2O3 ) nanowires were synthesized by a simple thermal evaporation method from gallium powder in the range of 700 - 1000℃ using the iron, nickel, copper, cobalt and zinc oxide as a catalyst, respectively. The β-Ga2O3 nanowires with single crystalline without defects were successfully synthesized at the reaction temperature of 850, 900 and 950℃ in all the catalysts. But optimum experimental condition in synthesis of nanowires varied with the kind of catalyst. As increasing synthesis temperature,the morphology of gallium oxide nanowires changed from nanowires to nanorods, and its diameter increased. From these results, we could be proposed that the growth mechanism of β-Ga2O3 nanowires was changed with synthesis temperature of nanowires. Microstructure and morphology of Synthesized nanowire was characterized by HR-TEM, FE-SEM, EDX and XRD.     

从天然辉锑矿中制备硫化锑纳米棒及其性能探究

以天然辉锑矿为原料, 在聚乙二醇(PEG)和N,N-二甲基甲酰胺(DMF)的辅助下, 利用水热法合成了硫化锑(Sb₂S₃)纳米棒。探讨了Sb₂S₃纳米棒的形成机理, 并系统研究了不同制备条件对产物形貌与性能的影响。采用一系列表征方法对产物的晶型、成分、形貌、光电性能进行了探究, 并以可见光为光源、甲基橙为目标降解物评价了纳米Sb₂S₃的光催化活性。研究表明, 经160℃水热反应12 h可得到厚约50 nm的Sb₂S₃纳米片, 在氮氛中400℃热处理1 h后, 纳米片将转变为宽100~200 nm, 长2~3 μm的Sb₂S₃单晶纳米棒。制备的Sb₂S₃纳米棒为直接半导体, 能带间隙为1.66 eV。光催化测试表明, 制备的Sb₂S₃纳米棒在可见光下对甲基橙的光催化降解率高于商业Sb₂S₃试剂, 60 min后, 甲基橙的降解率达87.6%, 表现出明显的可见光活性。     

Observation of magnetic, structural and surface morphological studies of triangle-like nickel nanoplates

Two-dimensional triangle-like nickel nanoplates have been synthesized by solvothermal method in the presence of triethylamine as a structure directing agent. The structure, morphology and magnetic properties of the as-synthesized products were characterized by X-ray diffraction, Atomic force microscopy and Superconducting quantum interference device magnetometer. The as-synthesized products have been confirmed to be phase-pure crystalline nickel with face centered cubic structure on the basis of X-ray diffraction characterization. Atomic force microscopy image demonstrated that the as-prepared nickel product possess two-dimensional triangle-like structure with edge length of about 65-85 nm. Magnetic measurements showed that the coercive forces at 4.2 K and 300 K for nickel nanoplates are 363.3 and 182 Oe, respectively. The nickel nanoplates exhibit a distinct enhanced coercive force due to the presence of shape anisotropy when compared with that of bulk. A possible mechanism for the formation of triangle-like Ni nanoplate structure is proposed.     

MnOOH纳米棒的低温水热合成

以KMnO₄ 和N₄ (CH₂)₆为主要原料, 在130℃反应16h, 水热法制备了MnOOH纳米棒, 并利用X射线粉末衍射(XRD)、透射电子显微镜(TEM)和高分辨透射电子显微镜(HRTEM)等手段对产物进行了表征. 探索了KMnO₄ 和N₄ (CH₂)₆间的摩尔比以及反应温度对合成产物的影响. 实验结果表明:产物为具有单斜结构的MnOOH纯相, 形貌为棒状, 呈现单晶特性.     

溶胶-凝胶法制备硼酸镁纳米棒

以硝酸镁、硼酸、柠檬酸为原料, 利用溶胶-凝胶法及不同温度后续煅烧制备了硼酸镁(MgB₄O₇和Mg₂B₂O₅)纳米棒. 用X射线衍射(XRD)分析了纳米棒的结构, 用扫描电子显微镜(SEM)和透射电子显微镜(TEM)观察了纳米棒的形貌. 实验结果表明, 750℃煅烧产物为MgB₄O₇纳米棒, 950℃煅烧产物为Mg₂B₂O₅纳米棒, 纳米棒的径长比可以通过调节原料硝酸镁和硼酸的比例来控制. 用自催化机理解释了硼酸镁纳米棒的生长机理.     

溶剂热技术制备硫化镍纳米粉体

分别以硝酸镍和硫脲作镍源及硫源、以乙二醇作溶剂,采用溶剂热技术成功地制备了Ni3S2,α-NiS和NiS2粉体。研究结果显示原料的配比及反应温度能够影响产物的物相组成及形貌。     

Synthesis of single-crystalline perovskite barium titanate nanorods by a combined route based on sol-gel and surfactant-templated methods

The single-crystalline perovskite barium titanate nanorods were successfully synthesized by a combined route based on sol-gel and surfactant-templated methods at low temperature. The synthesis was accomplished by using barium acetate (Ba(CH₃COO)₂) and tetrabutyl titanate (Ti[O(CH₂)₃CH₃]₄) as the starting materials and laurylamine as the surfactant, respectively. Well-isolated single-crystalline cubic perovskite BaTiO₃ nanorods with diameters ranging from 20 to 80 nm and lengths reaching up to > 10 μm can be easily fabricated by this route. The crystal form and morphology of the nanorods were characterized by X-ray diffraction, TEM and HRTEM. The mechanism of the formation of the single-crystalline cubic perovskite BaTiO₃ nanorods was discussed based on the theory of oriented attachment.     

溶胶模板法合成CdS纳米棒

以硝酸镉与硫代乙酰胺为起始物,采用DMF为溶剂,在低温(～50℃)下通过软化学法合成了CdS纳米棒,其直径为7～20nm,长度达500nm.通过XRD、TEM、SAED以及EDS对纳米棒的结构和成分进行了表征;通过引入乙酰丙酮(AcAc)控制钛酸丁酯水解,形成的溶胶中分子间网络孔道为CdS纳米棒提供了有效的生长模板.     

Synthesis and optical properties of single-crystalline GaN nanorods

Single-crystalline GaN nanorods were successfully synthesized on Si(1 1 1) substrates through ammoniating Ga₂O₃/Mo films deposited on the Si(1 1 1) substrate by radio frequency magnetron sputtering technique. The as-synthesized nanorods are confirmed as single-crystalline GaN with wurtzite structure by X-ray diffraction (XRD), selected-area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM). Scanning electron microscopy (SEM) displays that the GaN nanorods are straight and smooth with diameters in the range of 100-200 nm and lengths typically up to several micrometers. X-ray photoelectron spectroscopy (XPS) confirms the formation of bonding between Ga and N. The representative photoluminescence spectrum at room temperature exhibits a strong and broad emission band centered at 371.1 nm, attributed to GaN band-edge emission. The growth process of GaN nanorod may be dominated by vapor-solid (VS) mechanism.     

Characterization of Bi2S3 nanorods and nano-structured flowers prepared by a hydrothermal method

Bismuth sulfide nanorods and nano-structured flowers were synthesized by hydrothermal reaction of bismuth nitrate pentahydrate and thiourea solutions, containing 1 and 2 ml of 65% HNO₃, respectively. By using X-ray diffraction (XRD), selected area electron diffraction (SAED), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and high resolution TEM (HRTEM), the products were specified as orthorhombic Bi₂S₃ in the shapes of nanorods and flower-like clusters of nanorods, with the growth of nanorods in the [001] direction. A diffraction pattern was also simulated, and was in good accordance with the SAED pattern obtained from the experiment.     

Synthesis of single-crystalline alpha-FeOOH nanorods with semi-hard magnetic property

Goethite (α-FeOOH) nanorods were synthesized via hydrothermal method. The experimental results indicate that the uniform α-FeOOH nanorods, with length up to nearly 1 μm and diameter of ca. 50 nm, demonstrate perfect crystallinity and the growth direction of [001]. Owing to the characteristics of single-crystalline structure and high purity, the hysteresis loop of the resulting products shows semi-hard magnetic behavior compared to antiferromagnetic bulk with high-coercivity in nature.