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Materials 2019, 12, 1281 10 of 14 addition of both 25% and 50% CTP cannot change the size of the (0 0 2) crystallographic planes and it remained at 1.07 nm. However, the crystallographic structure of three samples evolved differently after carbonisation at 1200 ◦C as shown in Table 4. High-temperature carbonisation did not improve the size of the (0 0 2) crystalline plane at the U0 and U2 samples compared to low-temperature carbonisation. This is while the size for the U4 sample decreased to 1.04 nm at 1200 ◦C, the resultant reduction in the size of the crystallite in the U4 sample shows the better integrity between CTP and PAN at a lower Materials 2019, 12, x FOR PEER REVIEW amount of CTP e.g., 25% in the spinning dope. (a) (b) 10 of 14 U4 ES U2 ES U0 ES CTP (c) 10 15 20 25 30 35 40 10 15 20 25 30 35 40 10 15 20 25 30 35 40 2theta (Degree) 2theta (Degree) 2theta (Degree) Figure 7. X-ray diffraction (XRD) patterns of precursors (a), and carbonised fibre at 850 ◦ C (b) and 850 ◦ C Figure 7. X-ray diffraction (XRD) patterns of precursors (a), and carbonised fibre at 850 °C (b) and (c) for U0, U2 and U4 samples. 850 °C (c) for U0, U2 and U4 samples. Table 4. The results extracted from XRD patterns and calculated size of crystallites for precursor, low temperature and high-temperature carbonised samples. Table 4. The results extracted from XRD patterns and calculated size of crystallites for precursor, low Samples 2θ (Degree) FWHM (Degree) temperature and high-temperature carbonised samples. CTP Samples 20.15 9.36 Lc (nm) N/A 2.59 N/A 2.59 2.63 2.74 1.07 1.07 1.07 1.07 1.07 1in.0c4lusion of CTP as an CTP Precursor Carbonised @850 ◦C Carbonised @850 °CU0 Carbonised @1200 ◦C U2 U4 16.83 Precursor 20.15 9.36 16.81 3.01 2.63 2.74 U0 U2 U4 U2 U4 U0 U2 U4 U0 U2 24.43 7.55 1.07 1.07 1.07 2Θ (Degree) FWHM (degree) Lc (nm) U0 U2 16.81 U4 U0 16.8316.82 3.06 3.06 3.01 2.90 16.8224.41 2.90 24.41 7.51 24.43 7.55 24.4124.24 7.47 7.48 7.49 1.07 1.07 1.04 7.47 24.4124.33 7.51 24.05 7.71 24.24 7.48 Carbonised @1200 °C 24.33 7.49 Raman spectroscopy was also cUar4ried ou2t4t.o05investigate th7e.7i1nfluence of additive to the PAN spinning dope. As shown in Figure 8, a notable reduction in D-band (defect As presented in Table 4, calculated size of (1 0 0) crystallographic plane for U0, U2 and U4 structure) was observed after increasing carbonisation temperature from 850 ◦C to 1200 ◦C. Higher samples showed an increase in the size of the (1 0 0) crystalline plane from 2.59 nm in the U0 sample intensity of G-band (graphitic structure) at 1200◦C is attributed to the developing sp2 carbon atoms at to 2.63 nm and 2.74 nm in the U2 and U4 precursor samples, respectively. As all samples were a higher temperature, which demonstrates higher graphitic like carbon atoms. prepared under the same experimental conditions, a slight growth in the size of the crystallites is described by adding CTP as the dope additive. Adding CTP as a dope additive decreases the strong dipole-dipole interaction between cyanide groups in PAN chains. Therefore, the presence of CTP reduces the strong cohesive bonding between PAN chains which causes the formation of PAN clusters in the spinning dope. The higher CTP load in the spinning dope resulted in the lower polymer chains interaction and this resulted in the formation of larger PAN crystallites in the electrospun fibres, as presented in Table 3. The reduction of interaction in PAN chains due to the addition of CTP was also confirmed by observation of the shear-thinning behaviour in PAN/CTP solutions. Low-temperature carbonisation of stabilised fibres at 850 °C did not reveal a distinguishable difference between samples as shown in Figure 7b. Further calculation and quantification of low-temperature carbonised samples revealed that addition of both 25% and 50% CTP cannot change the size of the (0 0 2) crystallographic planes and it remained at 1.07 nm. However, the crystallographic structure of three samples evolved differently after carbonisation at 1200 °C as U4 850 U2 850 U0 850 U4 1200 U2 1200 U0 1200PDF Image | Low-Cost Carbon Fibre Derived from Sustainable Coal Tar Pitch and Polyacrylonitrile
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