气场压力对激光辐照制备石墨纤维微观结构与力学性能影响

doi:10.11949/0438-1157.20230769

摘要/Abstract

摘要：

在氩气压力0~0.3 MPa下对聚丙烯腈基碳纤维进行高功率激光快速辐照热传导制备了石墨纤维，研究了氩气压力对碳纤维石墨化性能的影响。结果表明，当气场压力为0 MPa时，高功率激光快速辐照下碳纤维发生了气胀现象：碳纤维中非碳元素以气体形式大量快速逸出、碳纤维直径增加，同时伴随着部分表层脱落。进一步增加高功率激光辐照时的气场环境压力，当气场压力为0.2~0.3 MPa时，碳纤维直径减小并逐渐稳定、表层脱落消失，碳纤维的石墨化程度和石墨微晶尺寸进一步增加，同时加压激光辐照后石墨纤维拉伸强度损失减小，杨氏模量增加。因此，施加0.2~0.3 MPa氩气压力是改善高功率激光辐照制备石墨纤维性能的一种有效方法。

关键词: 碳纤维, 激光, 热传导, 气体, 稳定性, 微观结构

Abstract:

Graphite fibers were prepared by rapid high-power laser irradiation heat conduction of polyacrylonitrile based carbon fibers under argon pressure of 0—0.3 MPa. The effect of argon pressure on the graphitization properties of carbon fibers was studied. The results show that when the gas field pressure is 0 MPa, the carbon fiber undergoes inflation under rapid irradiation with high-power laser: a large amount of non-carbon elements in the carbon fiber rapidly escape in the form of gas, the diameter of the carbon fiber increases, and at the same time, part of the surface layer falls off. Further increasing the gas field environmental pressure during high-power laser irradiation, when the gas field pressure is 0.2—0.3 MPa, the diameter of the carbon fiber decreases and gradually stabilizes, and the surface detachment disappears. The degree of graphitization of the carbon fiber and the size of graphite microcrystals further increased, at the same time, the tensile strength loss of graphite fibers decreased and the Young's modulus increased after pressurized laser irradiation. Therefore, applying 0.2—0.3 MPa argon gas pressure is an effective method to improve the performance of graphite fibers prepared by high-power laser irradiation.

Key words: carbon fiber, laser, heat conduction, gas, stability, microstructure

中图分类号:

TQ 342⁺.74

丁奇胜, 谭晶, 程礼盛, 张政和, 宋立健, 杨卫民. 气场压力对激光辐照制备石墨纤维微观结构与力学性能影响[J]. 化工学报, 2023, 74(12): 4988-4996.

Qisheng DING, Jing TAN, Lisheng CHENG, Zhenghe ZHANG, Lijian SONG, Weimin YANG. Effect of gas field pressure on the microstructure and mechanical properties of graphite fibers prepared by laser irradiation[J]. CIESC Journal, 2023, 74(12): 4988-4996.

图/表 10

图1 碳纤维激光石墨化装置和压力作用示意图

Fig.1 Schematic diagram of carbon fiber laser graphitization device and pressure action

表1 样品CF-0-0性能参数

Table 1 Performance parameters of CF-0-0 sample

去浆碳纤维	直径/µm	拉伸强度/MPa	杨氏模量/GPa
CF-0-0	7~7.5	3100	225

表2 CF-P-S系列样品元素含量

Table 2 Element content of CF-P-S series samples

样品	C/%	N/%	H/%	S/%
CF-0-0	92.68	5.28	1.286	0.862
CF-200-0	95.20	1.85	0.198	0.226
CF-200-0.1	94.60	1.75	0.21	0.265
CF-200-0.2	95.12	1.76	0.385	0.412
CF-200-0.3	94.40	2.02	0.769	0.621
CF-260-0	96.37	1.34	0.163	0.223
CF-260-0.1	95.70	1.42	0.122	0.322
CF-260-0.2	95.85	1.45	0.65	0.452
CF-260-0.3	95.53	1.98	0.82	0.763

图2 不同气场压力下200 W和260 W激光辐照后碳纤维SEM照片

Fig.2 SEM images of carbon fibers irradiated by 200 W and 260 W lasers under different gas field pressures

图3 不同气场压力下200 W和260 W激光辐照后碳纤维直径变化

Fig.3 Changes of carbon fiber diameter after 200 W and 260 W laser irradiation under different gas field pressures

图4 不同气场压力下200 W和260 W激光辐照后碳纤维Raman光谱

Fig.4 Raman spectra of carbon fibers irradiated by 200 W and 260 W lasers under different gas field pressures

表3 CF-P-S系列样品Raman光谱拟合参数

Table 3 Raman spectrum fitting parameters of CF-P-S series samples

样品	D峰		G峰		I_D	I_G	R
样品	峰位值/cm^-1	FWHM	峰位值/cm^-1	FWHM	I_D	I_G	R
CF-200-0	1356.13	44.37	1591.77	48.18	9068.05	13335.36	0.68
CF-200-0.1	1356.21	39.30	1589.13	39.21	7047.10	12812.90	0.55
CF-200-0.2	1353.33	38.25	1587.90	26.35	5271.12	14514.88	0.36
CF-200-0.3	1354.25	39.10	1588.78	28.07	3697.69	10829.36	0.34
CF-260-0	1346.57	42.37	1581.34	32.85	1410.91	7506.16	0.19
CF-260-0.1	1351.52	38.43	1586.13	25.76	1320.99	13293.37	0.10
CF-260-0.2	1351.94	36.13	1587.22	23.92	989.19	21982.01	0.04
CF-260-0.3	1357.43	34.46	1585.07	22.80	1039.34	18868.15	0.05

图5 不同气场压力下200 W和260 W激光辐照后碳纤维XRD赤道扫描谱图

Fig.5 XRD equatorial scanning spectra of carbon fibers after 200 W and 260 W laser irradiation under different gas field pressures

图6 不同气场压力下200 W和260 W激光辐照后碳纤维类石墨微晶尺寸变化

Fig.6 Size changes of carbon fiber like graphite microcrystals after 200 W and 260 W laser irradiation under different gas field pressures

图7 不同气场压力下200 W和260 W激光辐照后碳纤维力学性能变化

Fig.7 Changes in mechanical properties of carbon fibers after 200 W and 260 W laser irradiation under different gas field pressures

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