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The Preparation And Growth Mechanism Of One-Dimension Fullerene C60 Nanomaterials

Posted on:2011-08-19Degree:DoctorType:Dissertation
Country:ChinaCandidate:G B LiFull Text:PDF
GTID:1101360308975878Subject:Materials science
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The new fullerene materials have many unusual features, which show potential applications in the fields of modern technology, such as solar cells, photoconductor, molecular electronic devices, drugs and catalysts. Currently, with the continuous development of fullerene materials research, the research of nano-structured fullerene materials in the field of novel materials has attracted widespread attentions. Fullerenes, especially C6o can form a new aggregate structure under certain conditions and form a stable shape controlled growth of the "pipe", "line", which are concerning for the worldwide materials scientists. Fullerene C6o nanotubes and nanowires both possess conjugatedπelectronic structure. These novel C60 materials not only maintain the structure and properties of fullerene molecules, but also possess the characteristics of quasi one-dimensional material. The main work of this thesis is the synthesis of one-dimensional fullerene C60 nanomaterials using colloidal precipitation method. A variety of different morphologies of fullerene C60 nanomaterials has been successfully prepared and their structure and composition were detailed characterized. The optical anisotropy, thermal stabilities, electrochemical properties and magnetic properties of fullerene C60 nanotubes were also characterized. As the same time, based on the above results, the growth mechanism of one dimensional fullerene C60 nanomaterials was discussed. The main contents were described as follows:(1) In this paper, fullerene C60 nanotubes were first successfully synthesized using colloidal precipitation. The C60 nanotubes morphology and structure was characterized by POM,SEM,TEM and AFM. The obtained results showed that the C6o nanotubes possessed two structures:the symmetry and non-symmetry wall C6o nanotubes in accordance with the position of the hollow structure. Their diameter is between 300-500nm, the minimum diameter of C6o nanotube is about 150nm, the length is about tens to hundreds of microns with high aspect ratio. The SEAD and XRD results showed that the C6o nanotube's wall was composed of single crystal C60 molecules. The growth direction of C6o nanotubes was along the [110] surface of C6o molecules. The Raman and IR spectra confirmed that the C60 nanotubes were composed of pure C60 molecules.(2) The influence of different preparation conditions on the growth of C60 nanotubes was studied. The results showed that light can accelerated the complex of pyridine and C6o molecule and promote the growth of C6o nanotubes. It is easier to obtain C6o nanotubes using the blue and green light saturated the C60-pyridine solution, the content of nanotubes was higher, and the nanotubes'wall was smoother. Meanwhile ultrasonic irradiation can also accelerated the complex of pyridine and C60, thereby reducing the formation time of C60 nanotubes. For the first time we got a series of C60 nanotubes with the aspect ratio range from 3 to 1000 using ultrasonic cutting technology.(3) We investigated the properties of fullerene C60 nanotubes. The results showed that C6o nanotubes had optical anisotropy. At the same time, the C60 nanotubes can be patterned in a magnetic field. In addition, the thermal stabilities of C60 nanotubes were studied in air and nitrogen atmosphere respectively. The results showed that C6o nanotubes were more stable in nitrogen atmosphere. The electrochemical properties of C60 nanotubes were tested. The voltammogram oxidation peak of C60 nanotubes did not appear which means that the reduced C60 nanotubes can not be electro-oxidation under the experimental conditions. The big difference of packing state between one-dimensional structure and molecular induced the difference of electronic structure between C6o nanotubes and C60 molecular.(4) The Raman spectra and thermal stabilities of C6o nanotubes and nanofibers were compared. The Raman spectra revealed that the solution state of C60 nanotubes and C6o nanofibers were similar, the dried C6o nanotubes were more easily graphite than C6o nanofibers under the same laser irradiation conditions, and the C6o nanotubes were more likely to photo-polymerization. Therefore, Raman spectroscopy can be used to distinguish C60 nanotubes and C60 nanofibers. The thermal stabilities of C60 powders, C60 nanotubes and nanofibers were studied in air and nitrogen atmosphere respectively. The initial decomposition temperature of C60 nanotubes, C60 powders and C60 nanofibers was about 150,320 and 490℃in air atmosphere, which in turn increases of thermal stability, This is due to the different aggregation structure of C60 molecules. In nitrogen atmosphere, the initial decomposition temperature of C60 nanotubes, C60 powders and C60 nanofibers was 160,340 and 700℃respectively. When the temperature reached 900℃, the C60 powders, C60 nanotubes and C60 nanofibers residues was:0,20% and 10%.(5) The growth mechanism of C60 nanotubes was investigated. The complex reaction was occurred between C60 and pyridine molecules, and then formed a charge transfer complex, which was necessary to prepare C60 nanotubes.(6) The C60 nanofibers were rapidly prepared using modified liquid-liquid interface deposition (colloidal precipitation) method. The C60 nanofibers morphology was characterized by POM, SEM, TEM and other tests, the results showed that:C60 nanofibers diameter was uniform and their surface was smooth. The Raman and IR spectra proved that C60 nanofibers were composed of pure C60.The thermal stability of C60 nanofibers was studied. The growth mechanism of C60 nanofibers was deduced:the complex reaction between C60 and toluene did not occur, which can not form charge transfer complex. But the dispersion of C60 in toluene solution can form colloidal solution and light can promote the formation of colloidal solution, thus the growth of C60 nanofibers was accelerated.(7) Fullerene C60 nanoparticles were prepared using a colloidal precipitation method. Their diameter was about 300-500nm. The C60 nanoparticles were solid structure, the size of nanoparticles was different; the larger size of nanoparticles the surface smoother; the smaller size of nanoparticles the surface rougher. The C60 micron/nanometer rods were prepared using soft template method, their diameter was in micron scale in the case of not mixing preparation, and some of rods diameter in nanometer scale, the length of rods can reached tens to hundreds micrometers. In the case of mixing C60 nanorods showed overlapping cluster of physical state, most of the diameter was 300nm, and length of 2-4 microns, the size distribution was more uniform. The C60 nanorods surface was smooth. They showed hexagonal cross section. The flower cluster and dendritic-like structure of C60 micro/nanometer structures was prepared by slowly dropping in toluene-C60 system.(8) The C60/C70 nanofibers were synthesized with a mixture of fullerenes C60/C70 powders. The C60/C70 nanofibers were characterized. The results showed that part of C60/C70 nanofibers was solid structure, others with hollow structure or the hollow structure was not continuous. The fibers possessed optical anisotropy; the average diameter of fibers was about 1000nm, their surface was smooth. In this experiment, we first discovered spiral structure of C60/C70 nanofibers with diameters of about 200nm.
Keywords/Search Tags:one-dimensional nanomaterials, fullerene (C60), C60 nanotubes, C60 nanofibers, growth mechanism, colloidal precipitation
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