溶胶-凝胶模板法合成MnO2纳米线

本文通过两步阳极氧化在 0 .5M硫酸和 5g L草酸混合溶液中制得多孔氧化铝膜 ,经 5wt%的磷酸扩孔处理得到具有孔径大小均一 ,排列有序 ,并具有一定厚度的阳极氧化铝模板 (AAO) ,以该氧化膜为模板 ,用溶胶 凝胶法在其微孔内合成了MnO2 纳米线。利用扫描电镜 (SEM)对模板和纳米线材料的形貌进行了表征 ,发现氧化铝模板微孔直径为 75± 2nm ,MnO2 纳米线直径在 70nm左右 ,长度为 5 0 0～ 70 0nm。通过X 射线衍射 (XRD)检测可知该纳米线为α MnO2 。循环伏安 (CV)表明α MnO2 纳米线在 2 .0mol L (NH4 ) 2 SO4 溶液中具有优良的电容行为 ,比电容达 1 6 5F g ,是一种理想的超级电容器电极材料。     

用AAO模板法制备硅纳米管

先用二步阳极氧化法制备纳米孔平均孔径约为100 nm的Al/Al_2O_3(AAO)模板,再以AAO为模板用溶胶-凝胶法合成管径约为60-80 nm的硅纳米管,并用扫描电镜和透射电镜观察了硅纳米管的形貌。结果表明,AAO模板的孔径分别随着二步阳极氧化法中电解温度、氧化电压、硫酸和草酸混酸浓度的增大而增大,硅纳米管的形成与硅烷溶胶的嵌入方法、凝胶形成时间和温度有较大的关系。     

氧化锌纳米线/管阵列的溶胶-凝胶模板法制备与表征

用溶胶-凝胶法在氧化铝模板中制备了直径约为15、30、50、60nm的有序氧化锌纳米线/管阵列.用扫描电镜(SEM)、透射电镜(TEM)和X射线衍射仪(XRD)对氧化锌纳米线/管的形貌、结构以及相组成进行了分析.结果发现,纳米线的形貌依赖于氧化铝模板中孔洞的形貌,纳米线的长度受控于氧化铝模板的厚度,外径与氧化铝模板的孔径相等.通过控制溶胶的浓度以及氧化铝模板在溶胶中的浸泡时间可以制备出纳米管.     

CoFe2O4纳米线阵列的合成及磁性

利用多孔阳极氧化铝模板和溶胶．凝胶法制备了CoFe2O4纳米线阵列。溶胶是通过真空注入法被填充到模板的纳米孔洞中的，通过高温热处理，形成CoFe2O4纳米线阵列。利用扫描电子显微镜（SEM）、X射线衍射仪（XRD）和振动样品磁强计（VSM）对CoFe2O4纳米线阵列的形貌、结构和磁性进行了研究。CoFe2O4纳米线的直径与模板孔径相等．其具有多晶的尖晶石结构。CoFe2O4纳米线阵列未表现磁各向异性，这是由其多晶结构和较大的磁晶各向异性常数决定的．     

模板浸润法制备可生物降解聚合物纳米管和纳米线

以孔径为200nm的阳极氧化铝（AAO）为模板，用简单的物理方法制备了生物可降解聚合物聚己内酯（PCL）的纳米管、线及其阵列结构。SEM和TEM测试结果表明：熔融法在120℃和140℃都能制得整齐的纳米管阵列结构，管径均匀，约300nm。在溶液法中，5％浓度的溶液制得了杂乱的纳米管，而10％浓度的溶液制得的是纳米线阵列，直径在200nm左右。     

钴铁氧体空心微球的模板法制备及其性能研究

用聚苯乙烯球作模板,硝酸铁和硝酸钴为起始反应试剂,通过沉积与表面反应法合成了CoFe2O4空心微球。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)对样品的结构和形貌进行了表征。结果表明,所制备的CoFe2O4空心微球为立方结晶石结构,其直径约为2.5μm,是由纳米颗粒组装而成。用振动样品磁强剂计(VSM)和网络矢量分析仪分别对该样品以及本实验室制得的CoFe2O4粉体的室温磁性和吸波性能进行了研究。结果表明,CoFe2O4空心微球比粉体的磁性和吸波性更好。其中,CoFe2O4空心微球的矫顽力达到182.70Oe;频率为6000MHz波段附近有1个明显的吸收峰,回损值大于-18db,并有继续增大的趋势。     

溶胶-凝胶法制备MgB_2超导纳米线

采用溶胶-凝胶法和在Ar气氛下热分解技术,制得了MgB2超导晶态纳米线。利用XRD对样品进行物相分析,表明有MgB2生成。通过扫描电子显微镜(SEM)对样品进行形貌分析,证实制备出了MgB2纳米线。样品的超导特性通过电阻随温度变化的测量得以证实,其超导临界转变温度Tc为19.4K。此外,对比分析了溶胶-凝胶法粉末和传统固相烧结粉末的异同。     

溶胶-凝胶法制备尖晶石锂锰氧正极材料

以丙氨酸为螯合剂采用软化学法制备了锂锰氧化物.XRD分析结果表明所合成的产物为尖晶石型锰酸锂;采用SEM对产物的形貌进行了表征,结果表明所合成产物主要为棒状,且颗粒大小分布均匀.通过FT-IR及TG/DTA等手段初步探讨了产物的合成机理.采用循环充放电测试考察了产物的电化学性能,结果表明采用此法制备的产物具有优异的电化学性能.     

CoFe2O4纳米线阵列的制备与磁性

在氧化铝模板的纳米孔洞中,用电化学的方法沉积钴铁合金纳米线,经过550℃、30h氧化处理,成功制备出钴铁氧体纳米线阵列.分别用透射电子显微镜(TEM)、X射线衍射仪(XRD)和振动样品磁场计(VSM)对样品的形貌、晶体结构和磁学性质进行了表征测试.TEM观察结果显示纳米线粗细均匀,直径约为70nm.XRD显示纳米线的物相结构为CoFe2O4;VSM测试结果表明,CoFe2O4纳米线阵列的磁滞回线矫顽力为1.190×105A/m,比氧化处理前的钴铁合金纳米线阵列有显著提高.     

钴铁氧体纳米管阵列制备及其磁学性能(英文)

为了研究一维钴铁氧体纳米管阵列的磁学性质,应用氧化铝模板具有的约束作用和毛细管作用,结合溶胶凝胶技术合成了钴铁氧体纳米管阵列.在140℃条件下,通过包含Fe(AO)3和Co(AO)2(物质的量之比为2∶1)的柠檬酸和乙二醇混合溶液(物质的量之比为1∶4)酯化反应得到溶胶.将氧化铝模板浸入溶胶几次后取出,取出充满溶胶的氧化铝模板,在大气气氛中,以0.6℃/min～5℃/min的升温速度将样品由室温升温至500℃,保温8 h.结果表明,在控制Fe3+离子浓度的条件下也可以合成钴铁氧体纳米线(Fe3+离子浓度大于1 mol/L)和"竹节"型纳米管(Fe3+离子浓度介于0.5 mol/L～1.0 mol/L),但重点进行了其纳米管阵列(Fe3+离子浓度小于0.5 mol/L)合成和磁学性能测试.透射电子显微镜(TEM)、高分辨电镜(HRTEM)的观察以及粉末X光衍射(XRD)测试结果表明纳米管组成为多晶结构.纳米管的直径取决于氧化铝模板的孔径,大约为200 nm,其长度约几个微米.应用样品振动磁强计对样品磁性进行了表征,结果表明纳米管阵列未表现出方向特性,矫顽力随着升温速率的降低而升高,在0.6℃/min的升温速率时,矫顽力达到最高的1 445 kOe,简单讨论了其形成原因.     

Synthesis of the nanocrystalline CoFe2O4 ferrite thin films by a novel sol-gel method using glucose as an additional agent

Polycrystalline and nanometer-sized CoFe₂O₄ ferrite thin films are successfully synthesized using glucose as an addition agent. The thermal gravimetric/differential thermal analyzer, X-ray diffractometer, electron diffraction, scanning electron microscope, atomic force microscope and vibrating sample magnetometer are used to characterize the effects of the calcination temperature on the crystalline structure, morphology and magnetic properties of the Co-ferrite thin films. CoFe₂O₄ ferrite thin films have a single phase inverse spinel structure and are crystallized at and above 300 °C which is much lower than the required temperature in the traditional ceramic method (about 500-600 °C). Co-ferrite thin films annealed at relative low temperature of 400 °C show very small particle size with average of 32 nm and excellent magnetic properties for information storage applications.     

CoFe2与CoFe2O4质量比及MgO稀释对CoFe2@CoFe2O4磁性的影响

采用金属有机盐热分解方法制备了MgO包覆的CoFe₂O₄纳米粒子（CoFe₂O₄@MgO）,然后将CoFe₂O₄@MgO在H₂中还原,接着在空气中氧化制备了一组CoFe₂@CoFe₂O₄@MgO样品;用盐酸溶液溶解CoFe₂@CoFe₂O₄@MgO中的MgO获得另一组样品（CoFe₂@CoF₂O₄）。测量并绘制了CoFe₂@CoFe₂O₄@MgO和CoFe₂@CoF₂O₄的磁化强度随外磁场及温度变化的关系曲线。随着氧化温度升高,CoFe₂@CoFe₂O₄@MgO和CoFe₂@CoF₂O₄的矫顽力H_c、饱和磁化强度M_s、剩磁比M_r/M_s及磁有序状态发生显著变化,这些变化强烈依赖于磁性粒子的各向异性及粒子间的偶极相互作用。     

Synthesis, characterization and magnetic properties of CoFe2O4 nanorods

In this work, we demonstrated a new precursor route to synthesize CoFe₂O₄ one-dimensional (1D) nanorods. CoFe₂O₄ nanorods were prepared via the thermal decomposition of CoFe₂(C₂O₄)₃ nanorod precursor, which was prepared by solvothermal method without the assistance of template or surfactant. The microstructure and magnetic property of the obtained products were characterized by x-ray powder diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), thermogravimetric (TG) and differential thermal analysis (DTA) and vibrating sample magnetometer (VSM). The results showed that the as-prepared CoFe₂O₄ nanorods were built by magnetic nanoparticles after calcining the precursor nanorods at different temperatures, and the size variation of magnetic nanoparticles with calcination temperatures leaded to variable magnetic properties.     

CoFe2O4纳米微粉的制备及磁性

以FeCl3和CoCl2为原料,制备出颗粒细小的CoFe2O4纳米微粉,利用X射线衍射确定了粉体的组成,利用振动样品磁强计测量了室温下粉体的磁性能,利用扫描电子显微镜观察了颗粒的形貌.     

Solvothermal synthesis of Co/CoFe2O4 nanobelts

A facile solvothermal route is used for the synthesis of Co/CoFe₂O₄ nanobelts by rationally manipulating the dosages of a surfactant Poly(vinylpyrrolidone) (PVP, MW 40000). PVP plays a pivotal role in preparing the Co/CoFe₂O₄ nanobelts. The optimal dosage for the synthesis of the Co/CoFe₂O₄ nanobelts is 0.5 g. Lower than this value, octahedral particles and nanobelts were coexistent; higher than this value, octahedral particles were obtained. Furthermore, the possible formation mechanism of Co/CoFe₂O₄ nanobelts was proposed. A small quantity of Co²⁺ ions are reduced by glycerol, which is the reason for the presence of metallic Co in the CoFe₂O₄ ferrite. The Co/CoFe₂O₄ nanobelts may be very attractive for potential applications because of their outstanding magnetic properties (Ms = 110 emu/g, Hc = 387 Oe).     

Synthesis of CaCu3Ti4O12 ceramic via a sol-gel method

The novel nano-ultrafine powders for the preparation of CaCu₃Ti₄O₁₂ ceramic were prepared by the sol-gel method and citrate auto-ignition method. The obtained precursor powders were pressed, sintered at 1000 °C to fabricate microcrystal CaCu₃Ti₄O₁₂ ceramic. The microcrystalline phase of CaCu₃Ti₄O₁₂ was confirmed by X-ray powder diffraction (XRD). The morphology and size of the grains of the powders and ceramics under different heat treatments were observed using scanning electron microscopy (SEM). The relative dielectric constant of the ceramic sintered at 1000 °C was measured with a magnitude of more than 10⁴ at room temperature, which was approaching to those of Pb-containing complex perovskite ceramics, and the loss tangent was less than 0.20 in a broad frequency region. The relative dielectric constant and loss tangent were also compared with that of CaCu₃Ti₄O₁₂ ceramic prepared by other reported methods.     

Oleic-acid-coated CoFe2O4 nanoparticles synthesized by co-precipitation and hydrothermal synthesis

Oleic-acid-coated CoFe₂O₄ nanoparticles were synthesized by co-precipitation and hydrothermal synthesis. The coprecipitation of the nanoparticles was achieved by the rapid addition of a strong base to an aqueous solution of cations in the presence of the oleic acid surfactant, or without this additive. The nanoparticles were also synthesized by a hydrothermal treatment of suspensions of the precipitates, coprecipitated at room temperature in the presence of the oleic acid, or without it. The influence of the synthesis conditions, such as the valence state of the iron cation in the starting aqueous solution, the temperature of the treatment and the presence of oleic acid, on the particles size was systematically studied. X-ray powder diffractometry (XRD) and transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) revealed that, although spinel forms at room temperature, a substantial amount of Co was incorporated within the secondary, feroxyhyte-like phase when the iron cation was in the 2+ state. In contrast, when iron was in the 3+ state, the spinel forms at elevated temperatures of approximately 60 °C. The presence of the oleic acid further increased the formation temperature for the stoichiometric spinel. Moreover, the oleic acid impeded the particles’ growth and enabled the preparation of colloidal suspensions of the nanoparticles in non-polar organic solvents. The nanoparticles’ size was successfully controlled by the temperature of the synthesis in the region where superparamagnetism dominates to the region where mono-domain ferrimagnetism dominates the magnetic properties.     

钴铁氧体/聚吡咯复合材料的制备及电磁性能

首先采用溶胶-凝胶法制备钴铁氧体,再使用水热原位合成钴铁氧体(CoFe₂O₄,CFO)/聚吡咯(polypyrrole,PPy)新型复合材料。采用X射线衍射仪(XRD)分析样品的相结构、扫描电子显微镜(SEM观察样品微观形貌、振动样品磁场计(VSM)测试样品磁性能表征样品磁性能、样品的电磁参数采用矢量网络分析仪分析,计算获得样品在(8～12)GHz频率范围内的反射损耗。结果表明:在以酒石酸为络合剂、pH=5左右、经650 ℃热处理,得到结晶度良好的尖晶石结构钴铁氧体,平均粒径为350 nm;原位聚合后得到的钴铁氧体/聚吡咯复合材料表现出良好的吸波性能,在涂层厚度1.5 mm,PPy含量为6%时,吸波性能最佳,在频率为8.66 GHz处达到-11.05 dB,小于-5 dB的频段范围为(7.49~11.43)GHz,其可作为一种轻质、宽频的雷达波吸收剂来使用。     

Chemistry of post-annealing of epitaxial CoFe2O4 thin films

CoFe₂O₄ thin films of different thicknesses were grown on SrTiO₃ substrates. The X-ray diffraction analysis and atomic force microscopy indicated both epitaxy and a granular microstructure. We studied the magnetic properties of these films as a function of oxygen post-annealing and film thickness. All as-deposited films exhibited similar magnetic properties with saturated magnetization (M_s) of approximately 50% of the bulk M_s, (80 Am² kg^− 1). After the post-annealing the M_s changes as a consequence of crystallographic restructuring of the film. Cation ordering in 100 nm thick films reduces M_s, whereas re-oxidation increases M_s for thinner films. 13 nm films, annealed for 1 h, reach the bulk M_s. For even thinner films the quantum-size effect reduces M_s. For a synthesis of ≥ 30 nm films an annealing cycle after deposition of every 15 nm layer is recommended.     

Salt-assisted Low Temperature Solid State Synthesis of High Surface Area CoFe2O4 Nanoparticles

A novel salt-assisted low temperature solid state method using CoCl₂?6H₂O, FeCl₃?6H₂O and NaOH as pre- cursor and using NaCl as a dispersant to synthesize high surface area CoFe₂O₄ nanoparticles, has been investigated. The effects of the molar ratio of added salt and calcination temperature on the characteristics of the products were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), vibrating sample magnetometer (VSM) and Brunauer, Emmett and Teller (BET) surface area analysis. Results showed that the introduction of leachable inert inorganic salt as a hard agglomeration inhibitor in the mixture precursor led to the formation of high dispersive CoFe₂O₄ nanoparticles; and the increase in specific surface area from 28.28 to 73.97 m²/g, and the saturation magnetization is 84.6 emu/g.