J. Mater. Sci. Technol. ›› 2021, Vol. 95: 78-87.DOI: 10.1016/j.jmst.2021.03.067
• Research Article • Previous Articles Next Articles
Rahul Franklina,1, Weiheng Xub,1, Dharneedar Ravichandranb, Sayli Jambhulkarb, Yuxiang Zhub, Kenan Songc,*(
)
Received:2021-01-02
Revised:2021-03-24
Accepted:2021-03-27
Published:2021-12-30
Online:2021-05-24
Contact:
Kenan Song
About author:* E-mail address: kenan.song@asu.edu (K. Song).Rahul Franklin, Weiheng Xu, Dharneedar Ravichandran, Sayli Jambhulkar, Yuxiang Zhu, Kenan Song. Reinforcing carbonized polyacrylonitrile fibers with nanoscale graphitic interface-layers[J]. J. Mater. Sci. Technol., 2021, 95: 78-87.
Fig. 1. SEM images of as-obtained CNTs (a) and GNPs (b) with the magnified images of both materials (a1, b1).
| Fiber type | Fiber name | Compositions (wt%) | Processability and testability | |||||
|---|---|---|---|---|---|---|---|---|
| Interior and exterior layers | Middle layer | Spinnability# | Heat-treatment * | Mechanical testability+ | ||||
| PAN/DMF (wt%) | GNP | CNT | ||||||
| 1-phase | 15%PAN | 15 | N/A | N/A | N/A | Y | Hot drawing at 110, 130, and 150 °C; stabilization at 280 °C for 1.5 h, carbonization at 1250 °C for 10 min | Y |
| D-phase | 15%PAN/1%GNP-D | 15 | N/A | 1 | N/A | Y | N | |
| 3-Layered | 0%PAN/10%GNP-3 | 15 | 0 | 10 | 0 | Y | N | |
| 5%PAN/10%GNP-3 | 5 | 10 | 0 | Y | N | |||
| 10%PAN/10%GNP-3 | 10 | 10 | 0 | Y | N | |||
| 15%PAN/10%GNP-3 | 15 | 10 | 0 | N | Y | |||
| 15%PAN/1%GNP-3 | 15 | 1 | 0 | Y | Y | |||
| 15%PAN/1%CNT-3 | 15 | 0 | 1 | Y | Y | |||
Table 1 Summary of fiber terminology, compositions, processability, and testability.
| Fiber type | Fiber name | Compositions (wt%) | Processability and testability | |||||
|---|---|---|---|---|---|---|---|---|
| Interior and exterior layers | Middle layer | Spinnability# | Heat-treatment * | Mechanical testability+ | ||||
| PAN/DMF (wt%) | GNP | CNT | ||||||
| 1-phase | 15%PAN | 15 | N/A | N/A | N/A | Y | Hot drawing at 110, 130, and 150 °C; stabilization at 280 °C for 1.5 h, carbonization at 1250 °C for 10 min | Y |
| D-phase | 15%PAN/1%GNP-D | 15 | N/A | 1 | N/A | Y | N | |
| 3-Layered | 0%PAN/10%GNP-3 | 15 | 0 | 10 | 0 | Y | N | |
| 5%PAN/10%GNP-3 | 5 | 10 | 0 | Y | N | |||
| 10%PAN/10%GNP-3 | 10 | 10 | 0 | Y | N | |||
| 15%PAN/10%GNP-3 | 15 | 10 | 0 | N | Y | |||
| 15%PAN/1%GNP-3 | 15 | 1 | 0 | Y | Y | |||
| 15%PAN/1%CNT-3 | 15 | 0 | 1 | Y | Y | |||
Fig. 2. Manufacturing of 3-layered composite fibers and post-treatment at three stages (drawing, stabilization, and carbonization) (For interpretation of the references to color in this figure, the reader is referred to the web version of this article.).
Fig. 3. DSC curves of different heating rates for (a) 15%PAN, (b) 0%PAN/10%GNP-3, and (c) 10%PAN/10%GNP-3 fibers in nitrogen, followed by their corresponding re-runs in the air (d), (e), and (f). Plots of ln(φ/Tm2) versus 1/Tm according to the Kissinger method for activation energies of (g) cyclization, (h) oxidation, and (i) crosslinking reactions [33].
| 15%PAN | 0%PAN/10%GNP-3 | 10%PAN/10%GNP-3 | |
|---|---|---|---|
| Cyclization | 146.5 | 151.8 | 144.5 |
| Oxidation | 84.2 | 77.5 | 88.4 |
| Crosslinking | 138.5 | 112.1 | 132.4 |
Table 2 Activation energies determined from the Kissinger method (kJ/mol).
| 15%PAN | 0%PAN/10%GNP-3 | 10%PAN/10%GNP-3 | |
|---|---|---|---|
| Cyclization | 146.5 | 151.8 | 144.5 |
| Oxidation | 84.2 | 77.5 | 88.4 |
| Crosslinking | 138.5 | 112.1 | 132.4 |
Fig. 4. Cross-sectional SEM images of the pre-carbonized and post-carbonized (a1-a3) 0%PAN/10%GNP-3, (b1-b3) 5%PAN/10%GNP-3, (c1-c3) 10%PNA/10%GNP-3, and (d1-d3) 15%PAN/1%GNP-3 fibers with zoomed-in sections on the middle carbonized GNP/PAN layer.
Fig. 5. Mechanical properties of the fibers prior to stabilization. (a) The effect of increasing PAN concentration in the middle layer. (b) Comparison between 15%PAN and 1 wt% nanoparticle loaded fibers with and without layered structures. (c) Schematic of the change in GNP orientation resulted from the relative molecular movements on internal (blue) and external (red) surfaces of graphene layers, resulting in aligned the GNPs in the fiber axial direction. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)
| Pre- stabilized fibers | Carbonized fibers | |||||
|---|---|---|---|---|---|---|
| E (GPa) | σ (MPa) | ε (%) | E (GPa) | σ (MPa) | ε (%) | |
| 15%PAN | 9.3 ± 1.8 | 280.5 ± 44.6 | 8.1 ± 0.1 | 42.3 ± 11.4 | 320.4 ± 110.8 | 1.5 ± 0.5 |
| 15%PAN/1%GNP-D | 4.4 ± 0.8 | 190.2 ± 47.3 | 6.8 ± 6.2 | Non-collectable after carbonization due to fiber fracture in heat-treatment procedures (Fig. S4 in the Supporting Information) | ||
| 0%PAN/10%GNP-3 | 1.3 ± 0.2 | 39.8 ± 5.1 | 8.4 ± 0.6 | |||
| 5%PAN/10%GNP-3 | 4.5 ± 0.7 | 190.2 ± 26.9 | 10.2 ± 1.4 | |||
| 10%PAN/10%GNP-3 | 11.1 ± 0.9 | 420.2 ± 30.1 | 8.2 ± 1.1 | |||
| 15%PAN/1%GNP-3 | 9.0 ± 1.0 | 340.3 ± 25.7 | 9.4 ± 1.3 | 74.6 ± 17.6 | 440.2 ± 150.5 | 1.3 ± 0.6 |
| 15%PAN/1%CNT-3 | 9.8 ± 1.5 | 320.4 ± 41.2 | 9.6 ± 1.0 | 38.9 ± 22.2 | 290.7 ± 140.4 | 1.1 ± 0.9 |
Table 3 Mechanical properties before and after carbonization.
| Pre- stabilized fibers | Carbonized fibers | |||||
|---|---|---|---|---|---|---|
| E (GPa) | σ (MPa) | ε (%) | E (GPa) | σ (MPa) | ε (%) | |
| 15%PAN | 9.3 ± 1.8 | 280.5 ± 44.6 | 8.1 ± 0.1 | 42.3 ± 11.4 | 320.4 ± 110.8 | 1.5 ± 0.5 |
| 15%PAN/1%GNP-D | 4.4 ± 0.8 | 190.2 ± 47.3 | 6.8 ± 6.2 | Non-collectable after carbonization due to fiber fracture in heat-treatment procedures (Fig. S4 in the Supporting Information) | ||
| 0%PAN/10%GNP-3 | 1.3 ± 0.2 | 39.8 ± 5.1 | 8.4 ± 0.6 | |||
| 5%PAN/10%GNP-3 | 4.5 ± 0.7 | 190.2 ± 26.9 | 10.2 ± 1.4 | |||
| 10%PAN/10%GNP-3 | 11.1 ± 0.9 | 420.2 ± 30.1 | 8.2 ± 1.1 | |||
| 15%PAN/1%GNP-3 | 9.0 ± 1.0 | 340.3 ± 25.7 | 9.4 ± 1.3 | 74.6 ± 17.6 | 440.2 ± 150.5 | 1.3 ± 0.6 |
| 15%PAN/1%CNT-3 | 9.8 ± 1.5 | 320.4 ± 41.2 | 9.6 ± 1.0 | 38.9 ± 22.2 | 290.7 ± 140.4 | 1.1 ± 0.9 |
Fig. 6. Polarized Raman spectroscopy study on the orientation of GNPs and CNTs for the 3-layered structure. (a) Cross-sectional SEM images of the 15%PAN/1%GNP-3 with zoomed-in section showing aligned GNP. (b) Schematic showing the two Raman incident points on the middle and edge of the middle layer with optical images showing the rotation of 90° for both sections. The corresponding Raman signal for the edge and middle sections for (c1, c2) 15%PAN/1%GNP-3 and (e1 and e2) 15%PAN/1%CNT-3. (d1-d3) are the schematics for the orientations of GNP (For interpretation of the references to color in this figure, the reader is referred to the web version of this article.).
Fig. 7. Electrical and VOCs sensing performances. (a) The conductivity of three selected carbonized fibers at 1250 °C. (b) VOC sensing setup. Chemiresistive response of (c) HT-15%PAN/1%GNP-3 fiber and (d) HT-15%PAN fiber to various concentrations of methanol for 30 s. The zoomed-in sections are the response for 30 ppm concentration. (e) Response magnitude and their SNR with increasing concentrations for the two tested fibers. (f) The cyclical performance of the HT-15%PAN/1%GNP-3 fiber with various methanol concentrations.
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