Carbon based materials now actually dominate the earth, ranging from living matter, natural coal, to newly-synthesized next-generation nano-carbon materials, leading to the prosperity of the future world. While the sp2 carbon materials, showing extraordinary stability, strength, electronic and thermal superiority due to their unique bonding and hybridization strategy, is the most promising for future applications. Thus the focus of the thesis is the growth mechanisms of low-dimensional sp2 carbon materials, including 0D fullerene, 1D CNT, and 2D graphene.
In the first chapter, excellent properties of the sp2 carbon materials were introduced including the structural, chemical, thermal, electronic and mechanical properties, following up with the trends in the synthetic approaches dated back from the discoveries of the three star materials.
Drawbacks on the current synthetic methods and challenges on the improvement and development of these methods were discussed in details. Subsequently current theories and progresses on the formation mechanisms of fullerene, CNT, and graphene were introduced, accompanied with simulations and calculations. However, due to the limitation of the current experimental and computational tools, a comprehensive understanding on the growth of the materials from nucleation, elongation or enlargement, to completion or termination from atomic-scale perspective is still pending. Therefore, in the following three chapters, we presented our studies on the growth mechanisms of fullerene, CNT and graphene, respectively.
In the second chapter, to build a complete growth mechanism of fullerene in its arc discharge synthesis and to simulate the experimental mass spectra result of the final product, following works were done.
i) A simple carbon-cluster-evolution model was introduced considering the collisions happen during the arc discharge fullerene synthesis. With the preliminary model, the influence of various experimental conditions such as the buffer gas, pressure, temperature, initial carbon velocity, etc. to the growth and yield of fullerene can be explained;
ii) Thermodynamic stabilities of various carbon clusters at different temperatures were estimated using first principle calculation, vibrational entropy estimation, and numerical fitting. It was found that at high temperature (5000 K), carbon mostly remains as small carbon fragments like C2, C3, and C4. With the decreasing of temperature, the stability of chains/rings increases. At ~3000 K, stability of large fullerenes increases, but a high transition barrier from chains/rings to fullerenes obstacles the fullerene formation. It is until the temperature reaches ~2500 K that the
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barrier becomes lower and can be overcome. At lower temperature, though fullerenes are the most stable species, lack of kinetic energy for the annealing of fullerene also prevents its formation;
iii) Kinetic processes during the fullerene formation were tested using DFT-MD simulations and DFT calculations. It was found that collisions between fullerene cages cannot result into coalescence while the collisions between fullerenes and rings/chains lead to the enlargement of fullerene cages where chains/rings could pass C atoms to the fullerenes. In addition, the transformation between non-IPR fullerene and IPR fullerene is also intermediated by carbon chains/rings since chains/rings could help lower the transition barrier;
iv) An advanced kinetic model for the arc-jet fullerene formation was proposed based on the initial simple cluster-evolution model by incorporating both thermodynamic calculation and kinetic simulation results. With this model, the final cluster distribution after the simulation successfully resembles the experimental mass spectra result.
In the third chapter, growth mechanism of CNT was extensively studied mainly using DFT-MD simulations, following with some DFT calculations and classical MD simulations.
i) A complete CNT cap formation process was simulated on the Fe particle using DFT- MD simulation. The formation of carbon chains is found to be very crucial to the nucleation of CNT. It initially triggers the cap formation by the entanglement of multiple chains. But with too many chains, it tends to poison the particle surface and stops the further nucleation. Only by deleting the excessive carbon chains, the formation of the nucleus would restart, and the nucleation could complete;
ii) DFT-MD simulations showed that only very strong CNT-catalyst binding would sustain the open end of a CNT and support the continuous growth. For catalysts that have weak binding with the CNT, the grown tube would become narrower and tend to close. But the addition of H could help stop the narrowing and maintain the tube growth by preventing the formation of excessive long chains;
iii) CNT-catalyst interface was studied using DFT calculation and classical MD simulations. It was found that the formation of the carbon chains at the interface during the MD simulations is because of the limited time scale of the MD simulation methods.
By decreasing carbon feeding rate and increasing simulation time to approach real experimental time scale, the carbon chains would all transform into hexagons at the tube edge and become the tube wall;
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iv) Using DFT calculations, on regular tube edge consisting of only armchair, zigzag, and kink sites, the most stable edge configuration was searched. It was found the it was found that the conventional flat edge (A-Z alternatively separated) with dangling carbon attached is with similar stability as the newly reported tilted edge (A-Z segregated), or even more stable than it. The energy fluctuation among various interface configurations is not very significant but large enough not to be degenerated.
v) A CNT-catalyst contact induced phase separation of the alloy catalyst during CNT growth was observed by DFT-MD simulations. The phase separated alloy catalyst could prevent the deactivation of the particle, and lead to a oriented carbon source diffusion, which results in the fast growth of CNT and the prevention of the tube closure due to the graphitic encapsulation;
vi) During the CNT nucleation, the addition of the 6th pentagon determines the chirality of the grown CNT. While our DFT calculation showed that it is a kinetic process that beyond the nucleation size, and therefore, it is impossible to achieve chirality selective growth because on a liquid catalyst it is with equal environmental condition and thus equal probability to grow into a CNT with a specific chirality;
In the fourth chapter, mechanisms of fast and self-limited growth of graphene CVD synthesis on Cu foils were studied collaborated with experimental works using DFT calculations.
i) While fast growth of graphene with oxygen supply is due to the reduced the methane decomposition barriers by the assistance of oxygen on Cu surface, the mechanism of superfast growth of graphene with the modulation of fluorine in a confined space in the CVD system is quite different. It is the easy decomposition of fluoromethane on Cu surface, which is from the substitution of H atom in the methane gas flow by the F released from the metal fluoride, that greatly increases the concentration of carbon species, which further promotes the graphene growth rate;
ii) A new mechanism for the self-limited graphene growth where the graphene coverage on metal substrate cannot reach 100% was proposed. The failure of a full coverage is attributed to the existing of a newly-recognized parameter—the concentration of gas phase precursors which is distinguished from that of the surface precursors. Therefore, to achieve a controllable synthesis of high-quality full-coverage graphene film on metal substrate, careful controlling the concentration of gas phase precursors by changing the experimental parameters is very crucial.
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This thesis carefully studied the growth mechanisms of fullerene, CNT, and graphene by researching the detailed processes during the formation of the materials using very accurate DFT-MD simulations and subtle DFT calculations which finally forms a general picture for our deeper understanding. During the studies, it is gradually found that there are actually more similarities among the formation mechanisms of the three materials than we thought. For example, at the very beginning of the fullerene and CNT nucleation, there is always the formation of the first pentagon by the entanglement of the carbon chains which triggers the nucleation. This, in turn, contributes to our studies to better understand the simulation results.
In the three main chapters, all the simulations and calculations either help to understand the experimental results, or build us a clearer picture on how fullerene/CNT/graphene is nucleated, elongated/enlarged, and completed/terminated, which further feed back to the experimental scientists for the realization of ultimate production of high quality materials.
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