Zhang Hong-Gang, Zhuo Ya-Qi, Zhang Xiao-Min, Zhang Leng, Xu Piao-Yang, Tian Han-Rui, Lin Shui-Chao, Zhang Qianyan, Xie Su-Yuan, Zheng Lan-Sun
State Key Laboratory for Physical Chemistry of Solid Surfaces, iChEM (Collaborative Innovation Center of Chemistry for Energy Materials), Department of Chemistry, Xiamen University, Xiamen 361005, China.
Nanomaterials (Basel). 2021 Nov 12;11(11):3033. doi: 10.3390/nano11113033.
The flash vacuum pyrolysis (FVP) technique is useful for preparing curved polycyclic aromatic compounds (PAHs) and caged nanocarbon molecules, such as the well-known corannulene and fullerene C. However, the operating temperature of the traditional FVP apparatus is limited to ~1250 °C, which is not sufficient to overcome the high energy barriers of some reactions. Herein, we report an ultrahigh-temperature FVP (UT-FVP) apparatus with a controllable operating temperature of up to 2500 °C to synthesize fullerene C from a nonaromatic single carbon reactant, i.e., chloroform, at 1350 °C or above. Fullerene C cannot be obtained from CHCl using the traditional FVP apparatus because of the limitation of the reaction temperature. The significant improvements in the UT-FVP apparatus, compared to the traditional FVP apparatus, were the replacement of the quartz tube with a graphite tube and the direct heating of the graphite tube by impedance heating instead of indirect heating of the quartz tube using an electric furnace. Because of the higher temperature range, UT-FVP can not only synthesize fullerene C from single carbon nonaromatic reactants but sublimate some high-molecular-weight compounds to synthesize larger curved PAHs in the future.
闪蒸真空热解（FVP）技术对于制备弯曲的多环芳烃（PAHs）和笼状纳米碳分子很有用，比如著名的碗烯和富勒烯C。然而，传统FVP装置的操作温度限制在~1250°C，这不足以克服某些反应的高能量壁垒。在此，我们报道一种超高温FVP（UT-FVP）装置，其操作温度可控制高达2500°C，用于在1350°C或更高温度下由非芳香族单碳反应物即氯仿合成富勒烯C。由于反应温度的限制，使用传统FVP装置无法从CHCl获得富勒烯C。与传统FVP装置相比，UT-FVP装置的显著改进是用石墨管代替石英管，并通过阻抗加热直接加热石墨管，而不是用电炉间接加热石英管。由于温度范围更高，UT-FVP不仅可以从单碳非芳香族反应物合成富勒烯C，而且未来还可以升华一些高分子量化合物以合成更大的弯曲PAHs。
