以预锂化多壁碳纳米管为负极的锂离子电容器性能

采用内部短路方式对多壁碳纳米管负极进行不同程度的预嵌锂处理,预嵌锂时间为5,30,60min,以预嵌锂多壁碳纳米管极片作为负极,活性炭极片作为正极,组装成锂离子电容器。利用扫描电子显微镜(SEM)、透射电子显微镜(TEM)对多壁碳纳米管及电极极片进行表征分析,采用恒流充放电(GCD)和交流阻抗谱(EIS)研究预嵌锂多壁碳纳米管负极和未预嵌锂处理多壁碳纳米管负极锂离子电容器的性能。电化学测试结果表明,多壁碳纳米管负极预嵌锂大幅提高了电容器充放电性能,对比未嵌锂多壁碳纳米管电容器,在相同的电流密度下(100mA/g),能量密度提高400%。预嵌锂60min,电流密度100mA/g时,其比容量达到57F/g。在电流密度为100～3200mA/g范围内,其最高能量密度与功率密度分别达到90Wh/kg,4130W/kg。1000次充放电循环后,容量保持率维持在85%以上,表现出良好的超级电容器性能。     

用二胺在碳纳米管上引入胺基团的研究

为了在碳纳米管上引入胺基团，先对CVD法制备的多壁碳纳米管进行了有效的纯化和功能化，用TEM观察了纯化过程中的杂质变化和碳纳米管的形态结构，然后用二环己基碳二亚胺(DEC)缩合剂使功能化了的多壁碳管和乙二胺反应，并采用FF-IR红外光谱和Raman光谱对反应前后的碳管进行了表征。红外光谱测试结果表明：反应前红外光谱中在1709cm^-1处有羧基的吸收峰，说明碳纳米管的端口及侧壁已被有效功能化；反应后在1581cm^-1出现吸收峰表明二者通过酰胺键连接起来，增强了碳纳米管在有机溶剂中的溶解性；Raman光谱中反应前后D峰和G峰无明显区别，表明反应前后碳纳米管结构未发生变化。     

球磨时间对镁碳复合储氢材料结构和性能的影响

采用氢气气氛中高能球磨反应法,制备了40Mg60C镁碳复合储氢材料,研究了球磨时间对材料粒度、晶体结构和放氢性能的影响.结果表明,球磨2h材料的粒度即可达纳米级,约10～20nm,球磨时间再延长,材料团聚程度加重;球磨2h的材料为纳米晶和非晶结构,当球磨时间增加到4h时,材料几乎成为非晶结构;球磨时间4h时,材料储氢量已趋于饱和,最大放氢量为3.15%(质量分数);材料放氢温度随球磨时间的增加而降低,球磨5h材料的初始放氢温度和放氢峰温降为275.18和314.94℃.     

催化化学气相沉积法制备螺旋形多壁碳纳米管(英文)

以乙炔为碳源、FeMo/MgO催化剂为模板,采用催化化学沉积法制备了螺旋状多壁碳纳米管(hs-MWC-NTs)。其中FeMo/MgO模板,由作为发泡和助燃剂的柠檬酸燃烧而制成。FeMo/MgO催化剂的XRD谱图揭示其具有微晶的通性。应用SEM、TEM和Raman光谱剖析了合成的炭材料。SEM和TEM观察表明获得了hs-MWC-NTs;Raman光谱的D峰和G峰确认了所获碳纳米管(CNTs)的结晶状态。结果表明:此法乃是合成直径10nm～20nm螺旋形多壁碳纳米管的最容易和简便方法。     

高能球磨对多壁纳米碳管结构及场发射性能的影响

用振动磨进行了铁粉和多壁纳米碳管的混合物共同粉磨的试验研究,用XRD、Raman光谱和HRSEM对球磨不同时间的纳米碳管的形貌、结构及场发射性能进行了测定。结果表明,球磨8h后,部分纳米碳管的封闭端被打开,且被打开的封闭端的数量随球磨时间的增长而增多。场发射测定结果证明,铁微粒的存在可大大改善纳米碳管的场发射性能。     

水分散多壁碳纳米管紫外光谱特征及其应用

研究了多壁碳纳米管水分散体系的紫外光谱特征及其影响因素,并将其应用于碳纳米管对环境污染物五氯苯酚的吸附过程。结果表明:水分散多壁碳纳米管的主吸收带在190~250nm;最大吸收峰位于190~207nm,且随碳纳米管管外径的增加向短波方向偏移;抽滤次数n影响水分散体系中碳纳米管的浓度及其紫外光谱强度,n≥4时吸收强度趋于稳定低值。紫外光谱法研究碳纳米管吸附五氯苯酚的体系中,选用232nm作为测定波长可得到良好的线性关系且避免碳纳米管背景浓度的干扰。     

球磨对滑石、绿泥石、菱镁石和刚玉X射线衍射峰强度的影响

采用球磨工艺,获得了不同粒度的滑石、绿泥石、菱镁石和刚玉粉末样品,用来研究球磨时间对试样衍射峰强度的影响.试验表明,采用球磨法制得的样品的X射线衍射峰严重变形,随着球磨时间的延长,变形更加严重.辽宁产滑石和绿泥石,球磨4h,其衍射强度衰减不大,可以满足X射线定量分析的精度要求.菱镁石在球磨条件下迅速粉化,X射线衍射法定量分析时不宜采用.刚玉是一种较好的耐球磨物质,宜优先用作参比物质.     

新型纳米晶FexC系软磁合金粉末的制备及磁性研究

用机械球磨方法(MA)制备纳米晶FexC系软磁合金粉末(其中x=1、3、4、8),球磨时间分别为60、120、180、255、300h.用X-ray衍射谱分析样品的物相及其晶格结构,用振动样品磁强计测量粉末样品的磁性.对不同球磨时间而言,发现当球磨时间在小于120h范围内,随着球磨时间的增加,样品的软磁特能不断提高,当球磨时间达120h时,材料有最佳的软磁特能,对不同球磨成分而言,随着C含量减少(Fe含量的增加),其磁性能进一步提高,当x=8时,材料的饱和磁化强度σs达178.24emu/g,矫顽力降为1.76kA/m.其优良的软磁特性可与传统的FeNi、FeCo合金粉末相比.当球磨时间大于120h,样品的软磁性能开始变差.从X-ray衍射谱的分析可看出,这是由于样品发生了相变,从单相体心立方结构的α-Fe(C)固溶体向FeC金属间化合物转变.x=1的样品,经255h球磨后,样品成为单相Fe5C2金属间化物,它具有单斜晶体结构.这说明随着球磨时间的增加,材料由软磁性向硬磁性转化.同时发现样品随C含量增加时材料的抗氧化能力也提高了.并对上述实验结果进行了讨论.     

多壁碳纳米管在硫酸溶液中的γ辐射剪切

在硫酸溶液中系统地研究了γ辐射法剪切多壁碳纳米管,以及影响碳管长度的反应条件,详细讨论了多壁碳纳米管的剪切机理.采用透射电子显微镜(TEM)、傅立叶变换红外光谱(FT-IR)、紫外可见分光光度计(UV-Vis)和Raman光谱对短多壁碳纳米管进行了分析与表征,分析了多壁碳纳米管浓度与其对UV270nm吸光度的关系,得出了多壁碳纳米管质量浓度与其对UV270nm吸光度的线性回归方程.结果表明,γ辐射和硫酸氧化作用在剪切多壁碳纳米管的过程中存在协同效应.随着辐射剂量和酸浓度的增加,剪切后的碳管长度不断缩短.当辐射剂量增加到200kGy、酸浓度为5mol/L时,短多壁碳纳米管长度为200～300nm.辐射剪切的方法在碳纳米管外侧及末端引进C-OH、-COOH等官能团,从而对MWNTs的石墨型结构造成微弱损伤.另外,制备的短多壁碳管在水中可以均匀分散2周而不出现沉淀.     

空气中多壁碳纳米管的稳定性

采用化学气相沉积法(CVD),以二甲苯为碳源,二茂铁为催化剂制备了多壁碳纳米管(MWCNTs)。考察了纯化后的多壁碳纳米管在空气中的结构稳定性,利用电子显微技术及体积电阻率法研究了多壁碳纳米管在空气中的特性变化。结果表明:多壁碳纳米管在空气中存放时会被缓慢氧化而变短,氧化程度随空气中放置时间的延长而增加,15d后几乎完全转化为无定形碳。体积电阻率随氧化程度不同而不同。多壁碳纳米管在空气中不稳定,容易氧化,需要密闭保存。     

Electrophoretic deposition of HA/MWNTs composite coating for biomaterial applications

A composite coating of hydroxyapatite (HA)/multi-walled carbon nanotubes (MWNTs) has been fabricated by electrophoretic deposition (EPD). The nano powders of HA and MWNTs were dispersed in ethanol with total concentration of 0.005 g/mL and MWNTs 20% and 30% contents (wt). And the pH value of suspension was adjusted in a range from 4 to 5. After stabilization the mixture was ultrasonically treated for 3 h to form a stable suspension. Prior to the electrophoretic deposition, the titanium substrate was hydrothermally treated at 140 in NaOH (10 mol/L) solution for 6 h. A titanium sheet and circinal net of stainless steel were used as a cathode and an anode respectively, and a constant deposition voltage of 30 V was applied for 50-60 s in the EPD process. The thickness of the coatings was controlled from 10 mum to 20 mum. The samples of composite coating were then sintered in a resistance tube furnace in flowing argon at 700 for 2 h. The structure of the as prepared coating was characterized by SEM and XRD, and the bonding force of the coating/substrate was measured by an interfacial shear strength test. It is shown that the bonding strengths between the coating and the titanium substrate is as high as 35 MPa. The cell culture experiments indicate that the prepared composite coating of HA/MWNTs possesses good biocompatibility.     

PARTICLE SIZE ANALYSIS FOR OFLOXACIN, PREDNISOLONE ACETATE, AND AN OPHTHALMIC SUSPENSION CONTAINING THE OFLOXACIN/STEROID DRUG COMBINATION

Image analysis (LA), Photon Correlation Spectroscopy (PCS), and Single Particle Optical Sizing (SPOS) have been applied to the analysis of particle size for ofloxacin, prednisolone acetate and an ofloxacin/prednisolone acetate ophthalmic suspension. LA shows that ofloxacin particles suspended in mineral oil are on the order of 10 µor less. LA of prednisolone acetate in H₂O shows that the steroid particles are agglomerated and range in size from 20 to 50 µ. SPOS is used to verify LA results for prednisolone acetate. LA of the ofloxacin/steroid balled milled suspension yields a particle size of ∼ 1 µ with a few particles on the order of 5 µ, PCS analysis of three batches of ball-milled ofloxacin/steroid suspension shows that increased ball-milling time increases the reproducibility of the mean diameter value as determined by PCS. It is also observed by PCS that the mean diameter of the steroid achieves a constant value with ball-milling from 11 to 14 days (1386.4 to 1383.4 nm). Extended ball-milling past the 14 day time point (18 days) appears to reduce sample inhomogeneity, thereby eliminating larger particulates with a subsequent reduction in the mean diameter to 1097.4 nm, Results for PCS analysis of the ball-milled ofloxacin/steroid suspension are verified by SPOS.     

Field emission properties of carbon nanotube pastes examined using design of experiments

Field emission properties of screen-printed carbon nanotube (CNT) pastes were investigated by design of experiments (DOE) using three, two-level, input factors. Characterization showed that the multi-walled carbon nanotubes (MWNTs) with a diameter of approximately 5 nm containing 5 wt. % of carbonaceous impurities were almost completely burnt out after heating to 600°C in air, while 96% of the sample remained even up to 800°C in a nitrogen atmosphere. Experimental measurements using a diode structure for eight sample groups revealed an emission current density of 52–87 μA/cm² in an electric field of 5 V/μA and a field enhancement factor of 12,079–16,922, assuming the work function of MWNTs to be 5 eV, thereby demonstrating superior emission properties with the sample containing a larger amount of MWNTs. A long-term, 110-h reliability test showed a stable emission property with a half-life of 6,000 h.     

Exothermic reaction characteristics of continuously ball-milled Al/Ni powder compacts

Self-propagating reactions in compacted pellets of continuously low-energy ball-milled aluminium (Al) and nickel (Ni) powders at a composition corresponding to AlNi₃ were investigated. The formation of a bi-modal structure with nanoscale lamellae of Al and Ni surrounding thicker Ni layers was observed. The milled powder sizes decreased for milling durations longer than 4 h, but the pellet green densities remained mostly constant for longer than 2 h of milling. The ignited pellets observed using high-speed optical and infrared imaging revealed that the thermal wave velocity, maximum reaction temperature, ignition initiation duration and ignition temperature decreased with increasing milling times due to solid-state diffusion. X-Ray Diffraction (XRD) analysis after ignition tests showed that the AlNi₃ amount increased with milling time. Thermal analysis using interrupted Differential Scanning Calorimetry (DSC) in combination with XRD revealed that the ball-milled pellets have similarities to nanoscale magnetron sputtered multilayer foils in terms of phase formation sequence and exothermic peak shifts.     

Electrochemical properties of carbon nanotube (CNT) film electrodes prepared by controllable adsorption of CNTs onto an alkanethiol monolayer self-assembled on gold electrodes

This paper describes electrochemical properties, such as electrode reactivity, electrode dimensions, and interfacial capacitance, of multiwalled carbon nanotube (MWNT) film electrodes prepared by controllable adsorption of the MWNTs onto the self-assembled monolayer (SAM) of n-octadecyl mercaptan (C18H37SH) deposited onto Au electrodes. The adsorption of the MWNTs onto the SAM-modified Au electrode substantially restores heterogeneous electron transfer between bare Au electrode and redox species in solution phase that is almost totally blocked by the SAM of C18H37SH, and as a result, the prepared MWNT/SAM-modified electrode possesses good electrode reactivity without a remarkable barrier to heterogeneous electron transfer. In addition, the surface coverage of the MWNTs is readily controlled by adjusting the immersion time for the adsorption of the MWNTs onto the SAM of C18H37SH, which essentially endows the prepared MWNT/SAM-modified electrodes with tunable electrode dimensions ranging from a nanoelectrode array to a macro-sized conventional electrode. On the other hand, the MWNT/SAM-modified electrode is found to possess a largely reduced interfacial capacitance, as compared with the MWNT film electrodes prepared with existing methods by directly confining the MWNTs onto electrode surface. This demonstration offers a new approach to fabrication of stable MWNT film electrodes with excellent electrochemical properties that are believed to be very attractive for electrochemical studies and electroanalytical applications.     

Neuroblastoma cells displacement by magnetic carbon nanotubes

In this paper, as-produced multiwall carbon nanotubes (MWNTs) have been analyzed by scanning electron microscopy and energy dispersive X-ray spectrometry, revealing the presence of Fe, Al, and Zn residuals and impurities. MWNTs have then been dispersed in Pluronic F127 aqueous solution and used to seed neuroblastoma cell lines (HN9.10e and SH-SY5Y) for three days. We found that MWNTs interact with cells and induce, under a permanent constant magnetic field, the cell displacement toward the magnetic source.     

Preparation and properties of the polyimide/multi-walled carbon nanotubes (MWNTs) nanocomposites

The polyimide/multi-walled carbon nanotubes (MWNTs) nanocomposite films were prepared by mixing of poly(amic acid) (PAA) solution and MWNTs/DMAc suspension follow by mixture casting, evaporation and thermal imidization. To increase the chemical compatibility between polyimide matrix and MWNTs, MWNTs were modified with mixed strong acid. The results show that the dispersion of the MWNTs is improved greatly in the polyimide matrix after acid modification. The modified MWNTs are dispersed homogeneously in the polyimide matrix while the structure of the polyimide and MWNTs structures is stable in the preparation process. With the incorporation of MWNTs, the mechanical properties of the resultant nanocomposite films were greatly improved due to the strong interfacial interaction between the modified MWNTs and the polyimide matrix. The thermal stability of the nanocomposites was lower a little than pure polyimide because of the drop of thermostability of MWNTs through acid-treatment. The electrical conductivity and the dielectric constant of the nanocomposites were also having sharp increase, which is favorable for practical use in anti-static materials and embedded capacitors.     

镁钼氧化物催化剂制备多壁纳米碳管的初步研究

采用溶胶-凝胶法合成了可用来催化裂解甲烷大量制备高质量和较高纯度的多壁纳米碳管的镁钼氧化物催化剂. 实验表明该催化剂具有较高的活性和催化效率, 反应2h后, 制备的多壁纳米碳管的量接近原始催化剂量的30倍. 并用透射电镜、高分辨透射电镜、激光拉曼和热重分析对制得的粗产品进行了表征, 结果表明: 碳管的直径在10～22nm之间, 且随着反应时间的延长, 制备的纳米碳管石墨化程度增加, 反应1h后, 粗产品中碳管含量达95%, 同时, 对催化剂的特殊催化生长机理作了讨论, 生长过程中多层Mo颗粒析出在MgO载体表面是碳管成束的主要原因.     

Effects of high-energy ball milling on the morphology and the field emission property of multi-walled carbon nanotubes

The effects of grinding time in a vibration mill on the morphology and the field emission property of multi-walled carbon nanotubes (MWNTs) were studied using XRD, Raman spectra and high-resolution transmission electron microscopy (HRTEM). The results show that the closed ends of MWNTs are partly broken when ground for 4 h. The number of broken ends increases with grinding time. The field emission measurement results indicate that the presence of Fe particles can improve the field emission property of ground MWNTs.     

Study on the structural formation of new useful multiporous material ‘nano–meso ZSM-5’ and its application in producing biofuel

New ‘nano–meso ZSM-5’ (NM-ZSM-5) material was successfully synthesised by hydrothermal treatment using silica derived from rice husk. The synthesis of the material involves two steps of crystallisation, including the formation of ZSM-5 zeolite seed and mesoporous structure. The effect of crystallisation time on the formation of mesoporous structure was studied in the range 0–40?h. Samples were characterised by X-ray diffraction, infrared spectroscopy, transmission electron microscopy, Brunauer–Emmett–Teller and ²⁷Al-NMR methods. The results show that the best time for crystallisation is 14?h. The synthesised material has a multiporous structure, including micropore system of ZSM-5 zeolite, mesopore system of MCM-41 and another pore system which has a diameter in the range 10–50?nm (mesoporous system) due to the burning of organic compounds that remain in the material during the calcination process. In addition, the synthesised NM-ZSM-5 achieves crystallinity of approximately 100%. The catalytic performance of NM-ZSM-5 material was evaluated by the catalytic cracking reaction to produce biofuel from vegetable oil sludge. The research proved that NM-ZSM-5 is one of the most suitable catalysts for this process. The catalytic cracking reaction over NM-ZSM-5 yields products that are similar to those of the petroleum cracking process, such as dry gases, liquefied petroleum gas, gasoline, light cycle oil and heavy cycle oil.