Synthesis and magnetic properties of carbon-coated Ni/SiO_2 core/shell nanocomposites

A simple method for the synthesis of carbon-coated Ni/SiO2 core/shell nanocomposites is reported. The Ni nanoparticles were coated with silica layers via a combined procedure of sol-gel fabrication and hydrogen reduction prior to carbon coating via acetylene decomposition at an appropriate temperature. It was found that the anti-acid ability of the Ni/SiO2 composites was greatly enhanced after carbon coating. The results of magnetization measurement show that the real part (μ′) of complex permeability of the as-obtained sample is almost independent of frequency, and the imaginary part (μ″) stays small up to a frequency of 1 GHz. The encapsulation of Ni particles with SiO2 results in the rise of Ni nanoparticles resistivity. The outcome is the reduction in effect of eddy current at high frequency, making the real part μ′ almost constant and the imaginary part μ″ very small. Thus, this simple method may be effective for preparing composites of soft magnetic properties, especially in the high-frequency range.     

强流脉冲电子束诱发纯镍表层纳米结构的形成机制

利用强流脉冲电子束（HCPEB）技术对多晶纯镍进行了表面处理,并采用扫描电镜和透射电镜对强流脉冲电子束诱发的表面及亚表面的微观组织结构进行了分析.实验结果表明,HCPEB辐照后表面熔化,形成了深度约为2 μm的重熔层,快速的凝固使重熔层中形成晶粒尺寸约为80 nm的纳米结构.位于轰击表面下方5—15 μm深度范围内强烈塑性变形引起的位错墙和其内部的亚位错墙结构是该区域的主要结构特征.这些缺陷结构通过互相交割细化晶粒,最终导致尺寸约为10 nm的纳米晶粒的形成. 关键词： 强流脉冲电子束 纳米结构 多晶纯镍 位错墙     

制备因素对Ni/C催化剂上乙醇气相羰基化反应性能的影响

采用等体积浸渍法制备负载型Ni/C催化剂,考察了制备因素对乙醇直接气相羰基化反应的影响。实验结果表明,催化剂最佳制备因素为,Ni的质量分数为5%,活性炭采用水洗预处理,控制浸渍液的pH值为8.0～9.0,焙烧温度为450℃,H₂还原温度为400℃。采用上述参数制备的Ni/C催化剂,其乙醇转化率和丙酸选择性分别为96.14%和95.71%。利用N₂物理吸附法研究载体预处理对催化剂比表面积、孔容及孔径的影响和X射线衍射法(XRD)研究了活性组分在惰性气氛中焙烧时的分散状况。     

Two Nickel(Ⅱ) Complexes Constructed by Novel Bis(3-methoxy-2-pyridyl)ether-6,6"-dicarboxylic Acid Ligand: Lattice Water Control of Structure

Under given conditions, two complexes of [Ni(H2O)2BEDA]·2H2O 1 and [Ni(Py)2-sized and characterized by elemental analysis and X-ray single-crystal diffraction. Crystal data for 1:C14H18NiN2O11, monoclinic C2/c, a = 14.3844(17), b = 12.9900(15), c = 9.6309(11) (A°),β=104.3350(10)°, V = 1743.5(4) (A°)3, Z = 4, Dc= 1.711 g/cm3, F(000) = 928,μ= 1.179 mm-1, Mr=449.01, the final R = 0.0228 and wR = 0.0625. Crystal data for 2: C24H32NiN4O13, triclinic P1, a=9.423(2), b = 11.863(3), c = 13.089(3) (A°), α = 91.511(3), β= 92.465(3), γ = 100.696(2)°, V =1435.6(6) (A°)3, Z = 2, Dc= 1.488 g/cm3, F(000) = 672,μ= 0.748 mm-1, M,= 643.25, the final R =0.0400 and wR = 0.0975. Interestingly, in the two complexes, lattice water molecules dominate its crystal structures. Therefore, extensive intermolecular hydrogen bonds assemble 1 and 2 into 2D extended sheets and a 3D open framework, respectively. Furthermore, water molecules present in 2 are associated to form water clusters.     

Partial oxidation of methane to syngas catalyzed by a nickel nanowire catalyst

A nickel nanowire catalyst was prepared by a hard template method,and characterized by transmission electron microscopy (TEM),N2 physical adsorption,X-ray photoelectron spectrometry (XPS),X-ray diffraction (XRD) and H2 temperature-programmed reduction (H2-TPR).The catalytic properties of the nanowire catalyst in the partial oxidation of methane to syngas were compared with a metallic Ni catalyst which was prepared with nickel sponge.The characterization results showed that the nickel nanowire catalyst had high specific surface area and there was more NiO phase in the nickel nanowire catalyst than in the metallic Ni catalyst.The reaction results showed that the nickel nanowire catalyst had high CH4 conversion and selectivities for H2 and CO under low space velocity.     

镍纳米粒子-离子液体修饰碳糊电极的制备及其对多巴胺的测定

制备了镍纳米粒子-离子液体修饰电极,在0.1 mol/L磷酸缓冲溶液(pH 6.0)中研究了多巴胺(DA)在修饰电极上的电化学行为.与裸电极相比,DA在该修饰电极上的氧化还原电位明显降低,氧化还原反应的峰电流明显增大,DA的峰电流与其浓度在2.0×10~(-8) ～1.0×10~(-4) mol/L范围内呈良好的线性关系,检出限为6.5×10~(-9) mol/L.该修饰电极对抗坏血酸具有明显的抗干扰能力.     

Hydrocracking of Tar Components from Hot Coke Oven Gas over a Ni/Ce-ZrO2/γ-Al2O3 Catalyst at Atmospheric Pressure

Ni/Ce-ZrO₂/γ-Al₂O₃ catalysts with different Ce-ZrO₂ contents and Ni loadings were prepared by a two step impregnation method and characterized by X-ray diffraction, transmission electron microscopy, N₂ adsorption, and temperature-programmed reduction. The catalysts were used for the hydrocracking of toluene and naphthalene, which were model tar compounds in hot coke oven gas, under atmospheric pressure at 800 °C. They showed excellent catalytic activity, stability, and some sulfur tolerance. Both toluene and naphthalene was converted into light fuel gases even at a low mole ratio of steam to carbon (S/C = 0.44). During the testing period of 7 h, no coke deposition was observed on the surface of the catalysts. The results indicated that the addition of Ce-ZrO₂ limited the sintering of Ni particles and enhanced the catalytic activity. The Ni/Ce-ZrO₂/γ-Al₂O₃ catalyst is promising for the direct removal of tar compounds in hot coke oven gas with low S/C ratios.     

新型Ni/TiO_2催化剂用于对硝基苯酚催化加氢

以介孔氧化钛晶须为载体,采用等体积浸渍法制备了Ni/TiO2催化剂,通过扫描电镜、X射线衍射、N2吸附脱附、热重分析和程序升温还原技术对催化剂及其前驱体进行了表征,考察了催化剂中Ni含量及焙烧和还原温度对催化剂催化对硝基苯酚加氢反应性能的影响.结果表明,Ni/TiO2催化剂不仅具有晶须状形貌和高结晶度的锐钛晶型,还保持了高比表面积和介孔结构.随着Ni/TiO2催化剂中镍负载量的增加,对硝基苯酚转化率逐渐增加,当镍负载量超过10%时,催化剂活性和选择性没有明显变化.当镍负载量为10%,焙烧和还原温度分别为500和450 ℃时,Ni/TiO2催化剂的加氢活性最佳,是Raney Ni的4倍.该催化剂循环使用7次后未发现明显失活.     

漆原镍催化剂用于硝基化合物催化加氢

采用锌粉还原氯化镍制备了漆原镍催化剂,并将其用于催化间二硝基苯加氢制间苯二胺和2,5-二氯硝基苯加氢制2,5-二氯苯胺反应.运用X射线衍射、电感耦合等离子体发射光谱和透射电子显微镜等技术对催化剂进行了表征.考察了锌粉、展开剂和制备温度对催化剂活性的影响,以及压力、溶剂等对加氢反应速率的影响,确定了适宜的催化剂制备条件.结果表明,在间二硝基苯和2,5-二氯硝基苯加氢反应中,漆原镍催化剂表现出很高的活性和选择性,在乙醇溶剂中加入适量的水能够大大提高反应速率,适量的脱氯抑制剂能够有效加快2,5-二氯硝基苯加氢速率并提高2,5-二氯苯胺选择性.漆原镍催化剂重复使用5次后其性能基本保持不变.