初始温度及碳源对碳纳米管气相爆轰法合成的影响

改变初始温度以及分别使用甲烷和乙炔气体作碳源时气相爆轰合成碳纳米管,研究了初始温度与不同碳源对碳纳米管的影响。利用X射线衍射(XRD)、透射电镜(TEM)、拉曼(Raman)光谱等对碳纳米管进行表征。结果表明,随着初始温度的升高,所合成的碳纳米管的产量减少且石墨化程度降低,但管壁会变得光滑且管径有所增加。当使用乙炔时,所合成的产物中没有碳纳米管,而是合成了石墨化程度较高的无定形碳,随着催化剂量的增加,产物中碳包覆颗粒增多且包覆层清晰可见,但存在结构缺陷。当初始温度在110~130 ℃时,使用甲烷气体运用气相爆轰的手段是合成碳纳米管的较佳方案。     

纳米二氧化钛粉体的气相爆轰制备

 介绍了利用氢氧混合气体为原料、以四氯化钛为前驱体、气相爆轰制备纳米二氧化钛粉体的方法。利用XRD衍射结果分析证明,产物为金红石相和锐钛矿相的二氧化钛混晶,其晶粒尺度为纳米量级。通过XRD、SEM、TEM分析可以得出,粒子基本为球形,大部分粒子粒径为10~20 nm,也有少量的100 nm左右的粒子产生。分析后发现,反应发生在爆燃转爆轰的过程中和爆轰管中的湍流现象是导致大粒子产生的主要原因。在对在氢过量和氧过量两种状况下,对爆轰所产生的产物的形貌进行了对比,分析发现两种状况产生纳米二氧化钛粉末粒径分布和形貌并没有太大变化。     

二茂铁质量对气相爆轰法合成碳纳米管的影响

以甲烷和氧气作为爆源,二茂铁为前驱体,探究了不同前驱体质量对所合成的碳纳米管的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)等手段对碳纳米管的形貌和结构进行表征,结果发现:当二茂铁量较少时,只有碳包覆铁纳米颗粒存在;随着二茂铁质量的增加,逐渐有碳纳米管生成,其管径大多分布在10~50nm之间,为多壁碳纳米短管。随着前驱体质量的增加,碳纳米管的石墨化程度提高,结构缺陷也变少。通过对合成产物的热重分析可得,气相爆轰法所制备的碳纳米管具有强烈吸氧性,所得样品中碳纳米管的质量分数为26%左右。     

化学气相沉积法制备定向碳纳米管阵列

以二茂铁和二甲苯分别作为催化剂和碳源，采用一种无模板的化学气相沉积法，使用单温炉设备，成功地制备了高度定向的碳纳米管阵列.分别用扫描电子显微镜、透射电子显微镜和电子能量散射谱、拉曼光谱对碳纳米管阵列进行形貌观察和表征, 并研究了不同工艺参数对碳纳米管阵列形貌的影响.结果表明：在生长温度为800℃，催化剂浓度为0.02g/mL，抛光硅片上容易获得高质量的定向碳纳米管阵列，在此优化条件下生长的定向碳纳米管的平均生长速率可达25μm/min.     

气相/凝聚炸药爆轰合成的碳包铜纳米颗粒特征

采用凝聚炸药爆轰和气相爆轰分别制备碳包铜纳米颗粒,并利用XRD,Raman和TEM等方法对合成纳米产物进行对比分析。其中凝聚炸药爆轰法以柠檬酸铜干凝胶、油酸和黑索金为原料按照一定比例配成爆炸源,在氮气的保护氛围中引爆;而气相爆轰法以乙酰丙酮铜为原料,分别以H2和O2,H2和空气为爆炸源,在负氧条件下引爆。通过XRD,Raman和TEM分析结果表明,两类爆轰法均可得到分散性良好的碳包覆铜纳米颗粒,碳壳石墨化程度较高。气相爆轰可以合成10 nm以下的纳米晶粒,而凝聚炸药爆轰合成的晶粒尺寸在20~40 nm,且存在较多空壳结构;气相爆轰产物其碳壳尺寸在2~3 nm,凝聚炸药爆轰产物其碳壳尺寸在2~5 nm。     

气相/凝聚炸药爆轰合成的碳包铜纳米颗粒特征

采用凝聚炸药爆轰和气相爆轰分别制备碳包铜纳米颗粒,并利用XRD,Raman和TEM等方法对合成纳米产物进行对比分析。其中凝聚炸药爆轰法以柠檬酸铜干凝胶、油酸和黑索金为原料按照一定比例配成爆炸源,在氮气的保护氛围中引爆;而气相爆轰法以乙酰丙酮铜为原料,分别以H2和O2,H2和空气为爆炸源,在负氧条件下引爆。通过XRD,Raman和TEM分析结果表明,两类爆轰法均可得到分散性良好的碳包覆铜纳米颗粒,碳壳石墨化程度较高。气相爆轰可以合成10 nm以下的纳米晶粒,而凝聚炸药爆轰合成的晶粒尺寸在20~40 nm,且存在较多空壳结构;气相爆轰产物其碳壳尺寸在2~3 nm,凝聚炸药爆轰产物其碳壳尺寸在2~5 nm。     

爆轰法合成纳米氧化铈粒径的控制

为获得爆轰合成过程中纳米氧化铈粒径的控制方法,采用乳化炸药爆轰法合成了纳米氧化铈粉末,研究了乳化炸药基质中水相液滴的尺寸对乳化炸药爆速和纳米氧化铈粒径的影响。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射仪(XRD)和激光粒度仪,对不同乳化条件下得到的乳化炸药基质和相应的纳米氧化铈进行表征。结果表明,乳化炸药基质中水相液滴的尺寸对乳化炸药爆速和纳米氧化铈粒径均有较大的影响,乳化炸药基质中水相液滴的尺寸越小,相应的乳化炸药爆速越高,爆轰合成的纳米氧化铈的粒径越小,且粒径分布越均匀。     

激波管内氢-氧混合气体爆轰温度的测量

 以光纤传输光能，用多通道光学高温计，在垂直和平行于爆轰波传播方向上，测量了激波管中氢氧（或含氮）混合气体的爆轰温度。在20~53 kPa压力范围内，进行了六种初始压力氢氧混合气体的爆轰，分别测出横向温度和纵向温度；这两种温度在实验测量的误差范围内是一致的，并与正常爆轰的理论值符合得相当好。     

碳包覆铁纳米颗粒的气相爆轰合成北大核心CSCD

以粉末状与气态二茂铁为原料,以氢气和氧气混合气体为爆轰能源,采用气相爆轰法进行了合成碳包覆铁纳米颗粒实验。XRD和TEM实验结果表明,采用两种不同状态的二茂铁,均得到了纳米碳包覆铁颗粒。该包覆颗粒的组成核为铁或铁碳化合物,外层壳主要由石墨碳组成,大部分球形纳米颗粒尺寸分布于5-30 nm之间。通过对比发现,采用气态二茂铁爆轰时,所得到的碳包铁粒度分布较为集中,壳层厚度比较均匀,且粒子具有较好的球形状。最后结合铁碳合金相图,从热处理角度对气相爆轰合成碳包覆铁纳米颗粒的机理进行了分析,得出产物中α-Fe与Fe_3C的形成过程。分析了碳包覆铁纳米颗粒的磁滞回线,其表现出硬磁性与顺磁性双重性质。     

爆轰法合成碳包覆镍纳米颗粒的研究

 采用自制的负氧平衡复合炸药前驱体,在密闭容器中充氮气保护下爆轰合成了碳包覆镍纳米颗粒。利用X射线衍射、X射线荧光、透射电镜和拉曼光谱等技术,对爆炸产物的组成成分、结构形貌等进行了观测。结果表明,爆轰产物主要由具有面心立方结构的镍晶核和碳元素构成,此外还含有其它微量元素;合成的纳米颗粒呈球形或椭球形状,颗粒尺寸主要分布在10~25 nm范围,包覆的碳壳厚度约1~2 nm,核壳结构完备。结合观测结果,对爆轰法合成碳包覆纳米颗粒的形成机制进行了简单的讨论。     

Influence of pyrolysis temperature on the growth of Y-junction carbon nanotubes

Y-junction carbon nanotubes, grown through thermal pyrolysis of acetylene over nanocrystalline Ni-P deposited SiC whiskers, were investigated by transmission electron microscopy. The pyrolysis temperature, which ranged from 800 °C to 1000 °C, was found to be crucial for the growth of different Y-junction carbon nanotubes. At pyrolysis temperatures below the partial melting point of the Ni-P alloy catalyst, only single-junction nanotubes could be synthesized. Whereas, due to partial melting of the alloy catalyst at higher pyrolysis temperatures, liquid-assisted growth of multiple Y-junction nanotubes could occur. PACS 61.46.+w; 61.48.+c; 68.37.Lp     

Influence of temperature change on column buckling of multiwalled carbon nanotubes

Based on theory of thermal elasticity mechanics, an elastic multiple column model is developed for column buckling of MWNTs with large aspect ratios under axial compression coupling with temperature change. In this model, each of the nested concentric tubes is regarded as an individual column and the deflection of all the columns is coupled together through the van der Waals interactions between adjacent tubes. The thermal effect is incorporated in the formulation. Following this model, an explicit expression is derived for the critical buckling strain for a double-walled carbon nanotube. The influence of temperature change on the buckling strain is investigated. It is concluded that the effect of temperature change on the buckling strain is dependent on the temperature changes, the aspect ratios, and the buckling modes of carbon nanotubes.     

采用旋转涂膜法制备基底生长的定向碳纳米管阵列

 采用化学气相沉积技术,利用旋转涂膜法制备催化剂基底材料,通过对涂膜过程中的角速度、旋转时间以及基底还原过程中温度的控制改变催化剂颗粒的分布状态,获得了粒径均匀分布的催化剂基底,该基底上催化剂颗粒集中分布在47～62 nm区间,再利用该基底生长出定向碳纳米管阵列。运用扫描电镜、透射电镜、拉曼光谱仪对样品进行了表征。结果表明旋转涂膜法制备的基底平整性好于普通的滴膜法,且较其它基底制备方法具有简单易控、可使催化剂均匀分散等特点。利用该基底制备的碳纳米管阵列定向性良好。     

Morphologies and microstructures of carbon nanotubes prepared by self—sustained arc discharging

We have investigated the morphology and microstructure of carbon nanotubes and nanoparticles in cathode deposits prepared by self-sustained arc discharge. Scanning electron microscopy images indicate that there are two regions exhibiting different morphologies on the top surface of the cathode deposits. In the central region, there is a triangular pattern of spots with a diameter up to 100μm, which consists of carbon nanotubes and nanoparticles. In the fringe region, carbon nanotubes and nanoparticles are distributed randomly. In addition, carbon nanotubes in the central region have a larger inner diameter, compared with those in the fringe region. The outer diameter distribution of tubes in the central region is narrower than that of tubes in the fringe region, while the former has a smaller peak value than the latter. For the nanoparticles, they exhibit a different behaviour from the tubes existing in the same region. The difference between the microstructure of tubes or particles in the two regions is attributed to the different temperatures and temperature gradients during their formation.     

Structural peculiarities of carbon nanolayers prepared by deposition from a gaseous phase on Ni

Physics of the Solid State - The surface structure and the mechanical and electrical properties of graphite nanolayers (1–2 nm thick) obtained by the carbon deposition from a gaseous phase on...     

Effect of temperature on growth and structure of carbon nanotubes by chemical vapor deposition

The effect of temperature on growth and structure of carbon nanotubes (NTs) using chemical vapor deposition (CVD) has been investigated. Iron embedded silica was used to grow NTs in large quantity at various temperatures from 600 to 1050 °C with gas pressure fixed at 0.6 and 760 Torr, respectively. The growth and structure of the NTs are strongly affected by the temperature. At low gas pressure, the NTs are completely hollow at low temperature and bamboo-like structure at high temperature. While at high gas pressure, all the NTs are bamboo-like structure regardless of temperature. The diameter of NTs increases significantly with temperature. At low gas pressure the diameter gets bigger by mainly increasing the number of graphene layers of the wall of NTs, whereas at high gas pressure the diameter gets bigger by increasing both the number of graphene layers of the wall and the inner diameter of the NTs. This result indicates that the growth temperature is crucial in synthesizing NTs with different structures. The findings here are important for realizing controlled growth of NTs for their applications in different fields. Received: 20 November 2001 / Accepted: 21 November 2001 / Published online: 4 March 2002