二茂铁在高温热解乙二胺制备CNx纳米管过程中的催化性能研究

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二茂铁在高温热解乙二胺制备CN_x纳米管过程中的催化性能研究

采用高温热解法 ,以二茂铁 乙二胺有机溶剂为前驱液制备CNx 纳米管过程中 ,改变前驱液配比 ,对 86 0℃ ,不同二茂铁含量条件下制备出的CNx 纳米管进行了产量统计、形貌结构观察和拉曼光谱研究。结果显示 :随着前躯液中二茂铁含量的相对增大 ,不但CNx 纳米管产量随之增加 ,而且产物中“竹节状”结构纳米管相对“中空”结构纳米管的比重也增大 ;拉曼光谱结果进一步证实了由于“竹节状”结构CNx 纳米管的含量或比重增加所带来的纳米管样品整体或平均含氮量的升高而导致的样品结晶有序程度的降低。对单独钴粉和二茂铁催化条件下生成CNx 纳米管的形貌观察进一步证实 :二茂铁在热解法制备“竹节状”结构CNx 纳米管过程中的浮动催化作用显著 ,有利于实现含氮量较高、结构均匀的CNx 纳米管的可控制生长。     

拉曼光谱研究聚噻吩微米/纳米管

分别具有 2 0 0nm和 2 0nm管径的聚噻吩微米 /纳米管通过用微孔氧化铝过滤膜作为模板在三氟化硼乙醚溶液中电解聚合噻吩制得。在一张厚度约为 2 0nm的金箔上这些具有单分散长度的微米管能很好平行站立起来形成阵列 ,而纳米管则相互粘附不能形成很好的阵列。用 6 3 3nm激发的拉曼光谱研究表明 :微米管具有较高的掺杂程度 ,而纳米管的掺杂程度很低。这主要是由于两种管子的壁厚不同引起的     

拉曼光谱研究聚噻吩微米/纳米管

分别具有 2 0 0nm和 2 0nm管径的聚噻吩微米 /纳米管通过用微孔氧化铝过滤膜作为模板在三氟化硼乙醚溶液中电解聚合噻吩制得。在一张厚度约为 2 0nm的金箔上这些具有单分散长度的微米管能很好平行站立起来形成阵列 ,而纳米管则相互粘附不能形成很好的阵列。用 6 3 3nm激发的拉曼光谱研究表明 :微米管具有较高的掺杂程度 ,而纳米管的掺杂程度很低。这主要是由于两种管子的壁厚不同引起的     

硼碳氮纳米管的拉曼光谱研究

对不同温度和不同催化条件下用高温热解法制备的硼碳氮(BCN)纳米管的拉曼光谱进行了分析。随着制备温度的升高,拉曼光谱中D带和G带的强度比I_D/I_G由小变大,而后又变小,说明存在一个最佳温度,在该温度下生成的BCN纳米管中B、N元素掺杂浓度最大。不同催化剂对BCN纳米管的拉曼光谱也有影响,当以钴/二茂铁和镍/二茂铁为催化剂时的I_D/I_G值比以钴、镍和钴/镍为催化剂时大,说明这时的B、N的掺杂浓度较高,纳米管的质量较好,这与透射电子显微镜观察结果一致。     

CNx纳米管的制备、结构观察及低场致电子发射性能研究

采用高温热解法，以乙二胺为前驱液，在沉积有铁催化剂的p型硅（111）基底上制备出了定向生长的CNx纳米管.利用扫描电子显微镜、高分辨率透射电子显微镜和拉曼光谱对CNx纳米管进行了形貌观察和表征.CNx纳米管的高度在20?μm左右，直径在50—100nm之间，具有明显的“竹节状”结构，结晶有序度较差.对CNx纳米管薄膜进行低场致发射性能测试：外加电场为1.4V/μm，观察到20?μA /cm2发射电流，外电场升至2.54V/μm时发射电流达到1.280mA/cm2，在较高外电场下，没有发现电流“饱和”.这比 关键词： CNx纳米管 高温热解 “竹节状”结构 场致发射     

碳纳米管的热解法制备、电子显微镜观察及拉曼光谱研究

以二茂铁和二甲苯为原料在Ar和H2 气氛中不同温度下热解制备出了不同直径分布的碳纳米管。在 740℃、780℃、82 0℃和 880℃下制备出的碳纳米管的外径分布分别为 1 7-80nm、2 0 - 73nm、40 - 70nm、1 7- 2 7nm。拉曼光谱和透射电子显微镜 (TEM )观察表明 ,在82 0℃下制备的碳纳米管晶形最完整     

硼碳氮纳米管的热解法制备及生长机理研究

以乙二胺、二茂铁和硼氢化钠为原料,以N2和H2为辅气,用钴作催化剂,在不同温度下制备出了具有竹节状结构的硼碳氮(BCN)纳米管.根据透射电子显微镜观察,分析了BCN纳米管的生长机理.B和N的同时掺杂,所形成的五边形结构比单独N掺杂时具有更低的形成能,是竹节状结构形成的主要原因.用Raman光谱可以用来表征BCN纳米管中B和N的掺杂程度及纳米管的质量.分析表明,在860℃下制备的BCN纳米管竹节状结构最密集,质量最好,产率最高.扫描俄歇微探针分析表明,在860℃下制备的BCN纳米管的元素组成比为B∶N∶C= 关键词： BCN纳米管 热解 透射电子显微镜 Raman光谱     

二茂铁催化制备CNx纳米管的研究

采用浮动催化法,选用二茂铁做催化剂,在800 ~1040℃热解乙二胺/二茂铁前驱液制备CNx纳米管对不同温度下制备出的CNx纳米管进行了透射电镜观察、拉曼光谱研究以及产量统计,结果表明,二茂铁催化制备出的CNx纳米管具备较均匀的“竹节状”结构,并随制备温度的升高, CNx纳米管的平均直径增大,结晶有度提高,产量也增加.X射线光电子谱测试分析进一步验证了纳米管中氮原子的掺杂.还对CNx纳米管生长过中二茂铁的催化机理进行了探讨.     

不同氮源制备CNx纳米管薄膜及其低场致电子发射性能

采用高温热解法，分别以氯化铵(NH₄Cl)和乙二胺(C₂H₈N₂)为氮源在洁净的硅片上沉积生长CN_x纳米管薄膜.利用扫描电子显微镜、高分辨率透射电子显微镜和拉曼光谱对CN_x纳米管进行形貌观察和表征.结果显示不同氮源制备出的CN_x纳米管薄膜的洁净度、有序度以及纳米管的结构明显不同.热解乙二胺(C₂H₈N₂)/二茂铁(C₁₀H₁₀Fe)制备出的结晶度较低的“竹节状” 结构CN_x纳米管平行基底表面有序生长，而且低场致电子发射性能优越,开启电场1.0V/μm，外加电场达到2.89V/μm时发射电流密度为860μA/cm². 关键词： x纳米管')" href="#">CN_x纳米管 高温热解 “竹节状”结构 场致发射     

Raman study on electrochemical lithium insertion into multiwalled carbon nanotubes

We have carried out in situ Raman studies during the electrochemical insertion of lithium ions (Li⁺) into pristine and thermally treated multiwalled carbon nanotubes (MWNTs). We found an improved structural integrity as well as the removal of defects in the thermally treated tubes. The different Li⁺ insertion behaviors above 0.5 V in as‐grown and thermally treated tubes could be explained by the presence of defects on the outer surface of the tubes. No change of Raman spectra from 2.8 to 0.8 V is characterized by the coverage of Li⁺ on the outer surface of tubes, whereas the upshift of G band and the absence of a separated G band below 0.75 V indicate the formation of diluted graphite intercalation below the stage‐2 phase (LiC₁₂). Copyright © 2008 John Wiley & Sons, Ltd.     

不同催化剂对热解法制备CNx纳米管的影响

利用铁、钴、镍以及二茂铁为催化剂在高温下热解乙二胺制备CNx纳米管,研究了不同催化剂对CNx纳米管的形貌、结构及产量的影响,并对其催化机理进行了初步讨论.二茂铁和铁催化都能制备出“竹节状”结构的CNx纳米管,但产量较低.钴催化生成CNx纳米管多弯曲,管壁多褶皱,产量较高.镍催化只生成了直径500nm左右的螺旋管.拉曼光谱研究进一步表明,二茂铁催化生成“竹节状”结构CNx纳米管由于氮的掺杂程度相对较高而结晶有序度较低.     

Raman spectroscopic study of various types of tourmalines

Both polarized and unpolarized Raman scattering studies of seven tourmalines from the Lucyen mines in Vietnam are presented. These tourmalines, according to their chemical compositions, can be classified into four groups: G1, liddicoatite; G2, elbaite; G3, uvite; and G4, feruvite. The Raman spectra were recorded in two spectral ranges, i.e. 150–1600 cm⁻¹ and 3000–4000 cm⁻¹. In the lower spectral range, which covers the metal ion‐oxygen bond vibrations, all the observed A₁ and E modes are identified. In the higher spectral range, we investigated the OH stretching vibrations and showed that all the observed OH stretching modes have the A₁ character. In both spectral ranges, we found that the same group classification of tourmalines can be applied, and the grouping characterizations are consistent with the chemical composition results. Copyright © 2011 John Wiley & Sons, Ltd.     

Plasmon‐enhanced Raman scattering by suspended carbon nanotubes

We report plasmon‐enhanced Raman scattering of the order of 10³ by a metallic carbon nanotube partially suspended inside a near‐field cavity. The tube is part of a small bundle, and is interfaced with an Au nanodisc dimer using a recently developed assembly scheme based on dielectrophoretic deposition. Spatially resolved Raman measurements with two excitation wavelengths and two orthogonal polarizations confirm that the enhancement arises from a 65 nm long suspended tube segment. We show that the orientation of the tube inside the cavity can be as effective for generating enhancement as placing the nanotube precisely in a plasmonic hotspot. Position and shape of the G‐peak show that the suspended part of the tube is free of strain and doped with a Fermi energy shift ≤40 meV. (© 2014 WILEY‐VCH Verlag GmbH &Co. KGaA, Weinheim)     

Raman evidence of the interaction between multiwalled carbon nanotubes and nanostructured TiO2

Nanocomposites of carbon nanotubes and titanium dioxide (TiO₂) have attracted much attention due to their photocatalytic properties. Although many examples in the literature have visualized these nanocomposites by electron microscopic images, spectroscopic characterization is still lacking with regard to the interaction between the carbon nanotube and TiO₂. In this work, we show evidence of the attachment of nanostructured TiO₂ to multiwalled carbon nanotubes (MWNTs) by Raman spectroscopy. The nanostructured TiO₂ was characterized by both full‐width at half‐maximum (FWHM) and the Raman shift of the TiO₂ band at ca 144 cm⁻¹, whereas the average diameter of the crystallite was estimated as approximately 7 nm. Comparison of the Raman spectra of the MWNTs and MWNTs/TiO₂ shows a clear inversion of the relative intensities of the G and D bands, suggesting a substantial chemical modification of the outermost tubes due to the attachment of nanostructured TiO₂. To complement the nanocomposite characterization, scanning electronic microscopy and X‐ray diffraction were performed. Copyright © 2011 John Wiley & Sons, Ltd.     

Probing structural stability of double-walled carbon nanotubes at high non-hydrostatic pressure by Raman spectroscopy

Theoretical calculations predict that the collapse pressure for double-walled carbon nanotubes (DWCNTs) is proportional to 1/R ³, where R is the effective or average radius of a DWCNT. In order to address the problem of CNT stability at high pressure and stress, we performed a resonance Raman study of DWCNTs dispersed in sodium cholate using 532 and 633 nm laser excitation. Raman spectra of the recovered samples show minor versus irreversible changes with increasing I _D/I _G ratio after exposure to high non-hydrostatic pressure of 23 and 35 GPa, respectively. The system exhibits nearly 70% pressure hysteresis in radial breathing vibrational mode signals recovery on pressure release which is twice that predicted by theory.     

不同激发波长下单壁碳纳米管与多壁碳纳米管的拉曼光谱比较

对不同激发波长下单壁和多壁碳纳米管的激光拉曼光谱进行了比较。发现单壁碳纳米管D峰强度和G峰强度的比值(ID/IG)几乎不随激发光子能量的改变而变化,多壁碳纳米管ID/IG值随着激发光子能量的增加以斜率0 3/eV减小。并对此现象进行了初步的分析。此外,还发现在1064nm激发波长下,单壁和多壁碳纳米管2500-3500cm-1之间拉曼峰的相对强度随着入射激光功率的增加而增加。     

Synthesis of nitrogen-doped single-walled carbon nanotubes and monitoring of doping by Raman spectroscopy

Nitrogen-doped single-walled carbon nanotubes （CNx-SWNTs） with tunable dopant concentrations were synthesized by chemical vapor deposition （CVD）, and their structure and elemental composition were characterized by using transmission electron microscopy （TEM） in combination with electron energy loss spectroscopy （EELS）. By comparing the Raman spectra of pristine and doped nanotubes, we observed the doping-induced Raman G band phonon stiffening and 2D band phonon softening, both of which reflect doping-induced renormalization of the electron and phonon energies in the nan- otubes and behave as expected in accord with the n-type doping effect. On the basis of first principles calculations of the distribution of delocalized carrier density in both the pristine and doped nanotubes, we show how the n-type doping occurs when nitrogen heteroatoms are substitutionally incorporated into the honeycomb tube-shell carbon lattice.