Controllable synthesis of NiC2O4·2H2O nanorods precursor and applications in the synthesis of nickel-based nanostructures

A controllable synthesis of NiC₂O₄·2H₂O nanorods precursor was obtained via the microemulsion-mediated solvothermal method and a further synthesis of β-Ni(OH)₂ nanorods, nickel oxide (NiO) sub-microtubes, Ni nanospheres and flower-like nickel complexes nanostructures by using the precursor. The morphologies and crystalline structures were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and the X-ray powder diffraction (XRD). The morphologies and sizes of the precursors can be readily tuned by adjusting experimental parameters of the reverse microemulsion system. The synthesized β-Ni(OH)₂ nanorods composed of fine nanosheets shown excellent electrochemical performance as an electrode material in rechargeable battery systems.     

La(OH)3和 La2O2CO3纳 米 棒 的 合 成 及 其 催 化 Claisen-Schmidt缩合反应性能简

通过调节溶液的pH值,在水热条件下合成出长径比为2-45的La（OH）₃纳米棒. 对水热合成过程中间体的结构演变分析,发现高碱度有利于小尺寸晶核的形成,La（OH）₃晶体结构的各向异性导致这些晶种沿着C轴方向生长,进而形成纳米棒结构. 将La（OH）₃纳米棒前驱体于773 K焙烧可以得到长径比为2-20的La₂O₂CO₃纳米棒. 随着长径比的增加,La₂O₂CO₃纳米棒暴露的（110）晶面逐渐增加,La³⁺-O^2-碱性位的数目也从0.08增加到0.24 mmol/g. 因此,在Claisen-Schmidt缩合反应中,La₂O₂CO₃纳米棒催化剂上的反应速率随着长径比的增加而逐渐增大.     

Direct synthesis of porous/hollow magnesium carbonate hydroxide spindly nanorods and their application in water treatment

Spindly Mg₅(CO₃)₄(OH)₂·4H₂O nanorods with porous and hollow nanostructures were synthesized in a water-in-oil reverse microemulsion system of cetyltrimethylammonium bromide (CTAB)/water/cyclohexane/n-pentanol. These nanorods were characterized by a number of physical techniques, including powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). Comparison experiments showed that fundamental experimental parameters, such as the molar ratio of H₂O to CTAB and the concentration of reactants, were important in the morphological control of Mg₅(CO₃)₄(OH)₂·4H₂O nanostructures. The potential applications of the as-synthesized Mg₅(CO₃)₄(OH)₂·4H₂O nanorods in water treatment were also investigated.     

超级铝热剂Al/Fe2O3的制备、表征及对环三亚甲基三硝胺热分解的影响

采用水热法制备了中空短棒状纳米Fe2O3,并用超声分散法将其与纳米Al颗粒复合为单金属氧化基超级铝热剂.利用X射线粉末衍射(XRD)、傅里叶变换红外(FTIR)光谱、扫描电镜及能量散射光谱仪(SEM-EDS)对样品进行表征.并运用差示扫描量热法(DSC)对比研究了超级铝热剂Al/Fe2O3、Al粉和纳米Fe2O3对环三亚甲基三硝胺(RDX)热分解特性的影响.结果表明:超级铝热剂的加入改变了RDX的热分解过程,并加剧了RDX的二次气相反应;随着超级铝热剂含量的增加,RDX的分解峰峰形发生了明显的改变;Al/Fe2O3、Al粉和Fe2O3对RDX热分解的作用主要表现为二次分解峰逐渐明显且峰温降低.     

双功能化磁性纳米修复剂对多重金属的快速、高效钝化行为

采用“一锅法”制备了四氧化三铁/半胱氨酸（Fe₃O₄/Cys）磁性纳米微球,随后对Fe₃O₄/Cys进行亚氨基二乙酸（IDA）修饰得到Fe₃O₄/Cys/IDA磁性双功能化纳米微球。研究发现Fe₃O₄/Cys中的L-Cys是通过—SH基团接枝到Fe₃O₄表面的,随后IDA分子中的羧基与Fe₃O₄/Cys中的—NH₂形成酰胺键,最终形成多支链多羧基的Fe₃O₄/Cys/IDA磁性纳米修复剂。基于修复剂表面短支链-长支链交替的多羧基结构,实现了羧基基团的高密度接枝。同时,Fe₃O₄/Cys/IDA磁性纳米微球对Pb²⁺、Cd²⁺、Cu²⁺、Co²⁺、Ni²⁺、Zn²⁺为专性吸附,而对Hg²⁺属于非专性吸附,且吸附重金属后得到的钝化产物均表现了良好的稳定性。另外,Fe₃O₄/Cys/IDA对重金属离子的吸附符合Langmuir模型,属于单层均相吸附,其吸附过程符合准二级动力学模型,最大吸附量为49.05 mg·g^-1。     

泡沫镍负载Fe2O3@Ni3S2纳米线网状结构电极的制备及其电催化析氧性能

通过两步水热法制备泡沫镍(NF)负载Fe_2O_3纳米粒子@Ni_3S_2纳米线网状结构电极(Fe_2O_3@Ni_3S_2/NF)。运用X射线衍射(XRD)、X射线光电子能谱(XPS)、透射电子显微镜(TEM)、N_2吸附-脱附测试等方法对电极材料的物相和微观结构特征等进行了表征。水热条件下原位表面化学刻蚀生成的Ni_3S_2纳米线与三维多孔NF基体间拥有强结合力和低界面电阻,Fe_2O_3粒子均匀分布在纳米线的表面。在1 mol·L~(-1)的KOH溶液中,运用线性扫描伏安测试(LSV)、计时电位法、电化学交流阻抗测试(EIS)等对电极的电催化析氧(OER)性能进行了测试。结果表明:在100 mA·cm~(-2)的超高电流密度下,Fe_2O_3@Ni_3S_2/NF电极的OER过电势仅为223 mV,比Ni_3S_2/NF材料的过电势降低了285 mV;经过10 h计时电位测试,性能保持率高达80%。     

Preparation and optical properties of SrF2:Eu nanospheres

SrF₂:Eu³⁺ nanospheres with homogeneous diameter have been synthesized by a microemulsion-mediated hydrothermal method for the first time, in which quaternary microemulsion of CTAB/water/cyclohexane/n-pentanol was used. The possible reaction mechanism and the luminescent properties of SrF₂:Eu³⁺ nanospheres were also investigated in this paper. The morphology and grain sizes of final products were characterized by field emission scanning electron microscopy and transmission electron microscopy, indicating that most of the products were nanospheres with an average diameter of ∼50 nm. Room-temperature emission spectra, recorded under 394-nm excitation, showed that the transition of ⁵D₀ → ⁷F₁ emission be dominating in SrF₂:Eu³⁺ nanospheres. From the dependence of the luminescence intensity on the concentration of Eu³⁺ ions, the optimal dopant concentration is 2 mol%.     

Thermal oxide synthesis and characterization of Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanorods and Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanowires

Fe₃O₄ nanorods and Fe₂O₃ nanowires have been synthesized through a simple thermal oxide reaction of Fe with C₂H₂O₄ solution at 200–600°C for 1 h in the air. The morphology and structure of Fe₃O₄ nanorods and Fe₂O₃ nanowires were detected with powder X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The influence of temperature on the morphology development was experimentally investigated. The results show that the polycrystals Fe₃O₄ nanorods with cubic structure and the average diameter of 0.5–0.8 μm grow after reaction at 200–500°C for 1 h in the air. When the temperature was 600°C, the samples completely became Fe₂O₃ nanowires with hexagonal structure. It was found that C₂H₂O₄ molecules had a significant effect on the formation of Fe₃O₄ nanorods. A possible mechanism was also proposed to account for the growth of these Fe₃O₄ nanorods. Supported by the Fund of Weinan Teacher’s University (Grant No. 08YKZ008), the National Natural Science Foundation of China (Grant No. 20573072) and the Doctoral Fund of Ministry of Education of China (Grant No. 20060718010)     

Ni2P@CoP3核壳纳米球的制备、表征及其用于超级电容器性能

利用水热技术先后获得Ni纳米球和Ni@Co(OH)_2海胆状核壳纳米球前驱体,通过高温煅烧法获得NiO@CoO核壳纳米球,再以次磷酸钠为原料,通过高温磷化法最终获得Ni_2P@CoP_3核壳纳米球。利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、高角度环形暗场像扫描透射电子显微镜(HAADF-STEM)、X射线粉末衍射仪(XRD)、能谱仪(EDS)及X射线光电子能谱(XPS)对产物的形貌、结构和组成进行表征。采用循环伏安(CV)、恒电流充放电(GCD)以及循环稳定性实验探索了电极材料的电化学性能。结果表明,Ni_2P@CoP_3核壳纳米球的直径约为400 nm,由六方系Ni_2P纳米核和立方相CoP_3纳米壳构成。相比单纯的Ni_2P或CoP_3纳米球,Ni_2P@CoP_3核壳纳米球发挥了复合结构的协同效应,更加有利于电解液的质子传递,促进了赝电容反应,表现出更高的比容量、稳定性和更长的循环寿命。     

多孔朵状Fe_3O_4纳米微球的制备及其性能研究

<正>众所周知,纳米材料的尺寸大小、晶型、形貌构型等结构特征对材料的化学物理性能有重要的影响[1],由于特殊形貌的新材料所具有独特、新颖、高效的化学物理等方面的性质以及在众多领域中的潜在应用[2],特别是3D花状空心纳米结构新物质[3-4],新形貌物质的纳米材料的制备方法和应用特性已经吸引了世界上材料领域的广泛兴趣和关注[5]。目前为止,合成3D纳米结构的方法有自组装法、三维导向连接法以及水热法等,即通过使用有     

Flash microwave synthesis of trevorite nanoparticles

Nickel ferrite nanoparticles have several possible applications as cathode materials for rechargeable batteries, named “lithium-ion” batteries. In this study, NiFe₂O₄ was prepared by microwave induced thermohydrolysis. The obtained nanoparticles were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), BET method, transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS). All the results show that the microwave one-step flash synthesis leads in a very short time to NiFe₂O₄ nanoparticles with elementary particles size close to 4-5 nm, and high specific surfaces (close to 240 m²/g). Thus, microwave heating appears as an efficient source of energy to produce quickly nanoparticles with complex composition as ferrite.     

Sensitive electrochemical immunoassay for chlorpyrifos by using flake-like Fe3O4 modified carbon nanotubes as the enhanced multienzyme label

A highly sensitive electrochemical immunoassay of chlorpyrifos (CPF) was developed by using a biocompatible quinone-rich polydopamine nanospheres modified glass carbon electrode as the sensor platform and multi-horseradish peroxidase-flake like Fe₃O₄ coated carbon nanotube nanocomposites as the signal label. Due to the quinone-rich polydopamine nanospheres, the platform exhibited excellent fixing capacity by simple coating of sticky polydopamine nanospheres and subsequent oxidization. By coprecipitation of Fe³⁺ and Fe²⁺ on polydopamine modified carbon nanotubes (CNTs) with the aid of ethylene glycol (EG), the flake-like Fe₃O₄ coated CNTs (CNTs@f-Fe₃O₄) were synthesized and chosen as the carrier of multi-enzyme label due to the high loading of secondary antibody (Ab₂) and horseradish peroxidase (HRP) and also the peroxidase-mimic activity of Fe₃O₄. Under the optimum conditions, the immunosensor can detect CPF over a wide range with a detection limit of 6.3 pg/mL. Besides, the high specificity, reproducibility and stability of the proposed immunosensor were also proved. The preliminary application in real sample showed good recoveries, indicating it holds promise for fast analysis of CPF in aquatic environment.     

Facile Synthesis and Catalytic Properties of β-Co（OH）2 and Mg（OH）2 Nanoplates

β-Co(OH)2 and Mg(OH)2 nanoplates were synthesized via a facile template-free hydrothermal approach.The different conditions of preparation and catalytic properties of the products were studied and discussed.The products were characterized by X-ray diffraction,transmission electron microscopy,scanning electron microscopy,selected area electron diffraction(SAED),and gas chromatograph.     

Synthesis of Gd3PO7:Eu nanospheres via a facile combustion method and optical properties

Eu³⁺-doped Gd₃PO₇ nanospheres with an average diameter of ∼300 nm and a narrow size distribution have been prepared by a facile combustion method and structurally characterized by X-ray diffraction and field emission scanning electron microscopy. The luminescent properties were systemically studied by the measurement of excitation/emission spectra, and emission spectra under different temperatures, as well as by photostability. The strong red-emission intensity peaking at 614 nm originates the ⁵D₀→⁷F₂ transition and is observed under 254-nm irradiation, indicating that Eu³⁺ ions in Gd₃PO₇ mainly occupied non-centrosymmetry sites. The CIE1931 XY chromaticity coordinates of Gd₃PO₇:Eu³⁺ nanospheres are (x=0.654, y=0.345) in the red area, which is near the National Television Standard Committee standard chromaticity coordinates for red. Thus, Gd₃PO₇:Eu³⁺ nanospheres may be potential red-emitting phosphors for PDP and Xe-based mercury-free lamps.     

镁二次电池正极材料纳米Fe3S4的电化学性能

首次将尖晶石相的纳米Fe₃S₄材料用作镁二次电池的正极材料。采用水热法一步合成了具有纳米结构的Fe₃S₄材料, 并采用XRD、SEM测试手段对产物的物相、形貌进行了表征。实验结果表明, 在160 ℃能够合成纯相的Fe₃S₄材料, 该材料具有银耳状纳米结构。电化学测试结果显示, 水热法合成的纳米Fe₃S₄材料能够在镁二次电池体系中进行有效的可逆充放电, 放电平台电压为0.9 V, 首次放电容量高达267 mAh·g^-1, 50次循环后衰减至110 mAh·g^-1。电化学交流阻抗测试结果表明镁离子能够在Fe₃S₄晶格中扩散。     

Photocatalytic Activity of High Aspect Ratio TiO2 Nanorods

In this article, TiO₂ nanorods (aspect ratio >20) were prepared through a polyol process and doped with metal ions (Cu²⁺, Ni²⁺, Fe³⁺, and Cr³⁺). Compared with TiO₂ nanoparticles, the TiO₂ nanorods displayed relatively higher photocatalytic activity for the degradation of copper sulfophthalocyanine. Moreover, the photocatalytic activity was greatly enhanced when the metal ions were doped in the TiO₂ nanorods.     

Boron and nitrogen-codoped TiO2 nanorods: Synthesis, characterization, and photoelectrochemical properties

Boron and nitrogen codoped TiO₂ nanorods (BNTRs) were synthesized via two-step hydrothermal reactions using TiN as a starting material. The as-prepared samples were characterized by X-ray diffraction, field-emission scanning electron microscope (SEM), transmission electron microscopy and X-ray photoelectron spectroscopy techniques. The results showed that TiO₂ nanorods with the diameter of approximately 50–100 nm and the length of several micrometers were doped by the interstitial N and B. The nanorods were firstly formed in the hydrothermal synthesis of nitrogen doped TiO₂. The growing process of nanorods was observed by SEM and a most probable formation mechanism of the trititanate nanorods was proposed. The BNTRs showed a higher photocatalytic activity and a bigger photocurrent response than N–TiO₂ nanorods under visible light irradiation.     

可回收Fe3O4@SiO2-Ag磁性纳米微球对染料污染物的快速脱色处理

介绍了一种采用无毒廉价的前驱物制备Fe₃O₄@SiO₂-Ag磁性纳米微球的快捷方法,制备的Fe₃O₄@SiO₂-Ag纳米微球在NaBH₄存在下可以催化还原染料污染物.实验结果表明,Fe₃O₄@SiO₂-Ag磁性纳米粒子保持了Ag纳米粒子和Fe₃O₄纳米粒子的双重优点,不仅对染料罗丹明B和曙红Y具有良好的催化还原效率,而且可以在外加磁场作用下从溶液中快速有效的分离.催化还原反应速率与反应温度及Fe₃O₄@SiO₂-Ag催化剂用量有关,反应体系中表面活性剂和无机盐(Na₂SO₄)的存在也会影响催化剂的催化活性.该Fe₃O₄@SiO₂-Ag磁性纳米粒子在工业染料污染物处理方面具有应用前景.     

Microscopic studies of a SnO2/α-Fe2O3 architectural nanocomposite using Mössbauer spectroscopic and magnetic measurements

A SnO₂/α-Fe₂O₃ architectural nanocomposite, which was evidenced as SnO₂ nanorod arrays assembled on the surface of α-Fe₂O₃ nanotubes in our previous study, was investigated microscopically by means of Mössbauer spectroscopic and magnetic measurements. It was found for the SnO₂ nanorods that Fe³⁺ ions substituted slightly to Sn_0.998Fe_0.002O₂. Concerning the α-Fe₂O₃ tubes, the Morin transition, which was completely suppressed in the mother, SnO₂-free α-Fe₂O₃ nanotubes, was found to be recovered locally. We speculate that it takes place in the interface area as a result of structural modification needed for the connection with the SnO₂ nanorods.     

Preparation of a new pyrochlore-type compound Na0.32Bi1.68Ti2O6.46(OH)0.44 by hydrothermal reaction

A new pyrochlore-type Na_0.32Bi_1.68Ti₂O_6.46(OH)_0.44 with the cubic cell of a=10.339(5) Å was prepared by hydrothermal reaction using TiO₂ (anatase) and Bi₂O₃ in NaOH solution. This compound was obtained when the molar ratio of NaOH/TiO₂ was above 2 and the reaction temperature was above 240 °C. The TG-curve of as-prepared sample showed a mass loss of 0.8 mass% which was caused by release of OH group. This compound decomposed to a pyrochlore-type compound and a layered-type Na_0.5Bi_4.5Ti₄O₁₅ above 800 °C. The optical band gap of Na_0.32Bi_1.68Ti₂O_6.46(OH)_0.44 was estimated to be 2.5 eV.