Two birds with one stone: Simultaneous fabrication of HfC nanowires and CNTs through efficient utilization of polymer-derived ceramics

doi:10.1016/j.jmst.2022.04.037

Abstract

Abstract:

Carbon nanotubes (CNTs) are fabricated in carbon cloth by ultilizing the waste gasses when fabricating hafnium carbide nanowires (HfC_NWs) through thermal pyrolysis of Hf-containing polymer precursor. The formed HfC_NWs are distributed uniformly on the surface of the carbon fibers in carbon/carbon (C/C) composites and display perfect single crystal appearance. The pyrolysis of the Hf-containing organic precursor provides hafnium and carbon source for the growth of HfC_NWs. The released waste gasses containing CO, CH₄ and CO₂ are the main carbon source for the growth of CNTs. Specifically, the flexural strength of HfC_NWs reinforced carbon/carbon (HfC_NWs-C/C) composites is enhanced by ∼105% compared with pure C/C, and the CNTs/carbon cloth also displays improved electrochemical performance with respect to capacitor applications. The present study introduces a novel sustainable and eco-friendly process related to polymer-derived ceramics to form advanced ceramic nanocomposites and proposes a deep understanding of the growth mechanism of CNTs.

Key words: HfC nanowires, Carbon nanotubes, Waste gasses, Effective utilization, Polymer-derived ceramics

Yanqin Fu, Yulei Zhang, Xuemin Yin, Liyuan Han, Qiangang Fu, Hejun Li, Ralf Riedel. Two birds with one stone: Simultaneous fabrication of HfC nanowires and CNTs through efficient utilization of polymer-derived ceramics[J]. J. Mater. Sci. Technol., 2022, 129: 163-172.

Figures/Tables 9

Fig. 1. Schematic diagram of the process for preparing HfCNWs and CNTs via one-step method.

Fig. 2. Typical SEM images and schematic illustrations of the as-prepared HfCNWs (S0) and CNTs synthesized in different temperature zones (1300, 1100, 900 and 700 °C) corresponding to S1, S2, S3 and, S4, respectively.

Fig. 3. Microstructure of the as-prepared HfCNWs. (a) Typical SEM image of HfCNWs, inset of (a): Schematic diagram of C/C composites with in situ grown HfCNWs; (b, c) Enlarged area with radially upright nanowires; (d) TEM image of single HfCNW, inset on the left shows the corresponding HRTEM image and SAED pattern, while the inset on the right depicts the amorphous HfOC layer; (e) XRD pattern of C/C with HfCNWs.

Fig. 4. TEM images of the in situ grown CNTs. (a, b) 900 °C; (d, e) 1100 °C; (g, h) 1300 °C; (c, f, i) Raman spectrum of S3, S2 and S1, respectively.

Table 1. Structure parameters obtained from Raman spectra of S1-S3.

Material	I_A/I_G	I_D’/I_G	I_D/I_G
S3	1.952±0.020	0.764±0.003	2.128±0.016
S2	2.235±0.041	0.463±0.010	1.892±0.012
S1	2.205±0.025	0.684±0.008	2.355±0.023

Fig. 5. Formation of CNTs. (a) in situ TG-MS study of the Hf-containing polymeric precursor [m/z = 16 (CH4); m/z = 28 (CO); m/z = 44 (CO2)]; (b) Gibbs free energy vs. temperature (Ellingham diagram) for the reaction of NiO with H2 and CO; (c) Schematic diagram of the HfCNWs and CNTs formation via one-step method.

Fig. 6. PLM images of the carbon substrate: (a) C/C composites; (b) HfCNWs-C/C composites.

Fig. 7. Mechanical property of C/C and HfCNWs-C/C composites. (a) Stress-strain curves of flexural strength; (b) Flexural modulus; (c) and (d) SEM images of the flexural fracture of C/C and HfCNWs-C/C composites; (e) and (f) Schematic diagram of the toughing mechanism of C/C and HfCNWs-C/C composites, respectively; (g) Related flexural performance of nano-reinforced C/C composites reported in other literatures [37], [38], [39], [40], [41], [42], [43], [44].

Fig. 8. Electrochemical performance of different samples. (a) CV curves of samples at 50 mV s?1 in a three-electrode system; (b) GCD curves of samples S1-S3 and carbon cloth electrodes at 1 A g?1; (c) Nyquist plots of the samples; (d) CV curves of sample S2 at different scan rates; (e) Variation of specific capacitance of sample S2 with current density, and (inset (e)) GCD curves of S2 at different current densities; (f) Cycling performance of S2 at a scan rate of 500 mV s?1 and (inset (f)) CV curves of S2 at 500 mV s?1 under different cycles.

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