Kandola Baljinder K, Hewage Trishan A M, Hajee Muhammed, Horrocks A Richard, Culebras Mario, Collins Maurice N
Institute for Materials Research and Innovation, University of Bolton, Deane Road, Bolton BL3 5AB, UK.
Institute for Materials Research and Innovation, University of Bolton, Deane Road, Bolton BL3 5AB, UK; Colorplas Ltd., Moss Bridge Road, Rochdale, Lancashire OL16 5PQ, UK.
Int J Biol Macromol. 2025 Sep;321(Pt 4):146553. doi: 10.1016/j.ijbiomac.2025.146553. Epub 2025 Aug 5.
The thermal stability of melt-spun hydroxypropyl-modified lignin/polyamide (PA1010) 50:50 wt% blended precursor fibres, crucial for the thermal stabilisation stage in carbon fibre production, was enhanced by pre-treating the fibres with a graphene oxide (GO) suspension, synthesized via the modified Hummers method. This pre-treatment allowed the fibres to be subsequently thermally stabilised at a faster heating rate of 20 °C/min, compared to the typical 0.1-0.25 °C/min used for lignin-based fibres, thereby reducing overall thermal stabilisation time from 29 h to 2.5 h. The stabilised filaments were successfully carbonised at 950 °C, yielding coherent, void-free carbon fibres without inter-filament fusion. The tensile modulus of GO-treated filaments improved from 1.3 GPa to 2.3 GPa after thermal stabilisation. However, derived carbon fibres were brittle in nature. Various characterisation techniques, including DSC, TGA, FTIR, SEM-EDX, AFM, XPS, and tensile testing, were used to analyze the physico-chemical changes. DSC showed that GO improved the polycrystallinity of the precursor filaments and contributed to the formation of a three-dimensional cross-linked network during heat stabilisation, suppressing the PA melt endotherm. TGA confirmed that GO-treated filaments had higher char yields (∼40 %) than untreated fibres (∼30 %), further supporting GO-induced crosslinking reactions. FTIR, SEM-EDX, and AFM confirmed an even GO coating. A study of GO pre-treatment variables suggested that a reduction in GO concentration is required to reduce resulting carbon fibre brittleness at the expense of increased thermal stabilisation time.
通过用改进的Hummers方法合成的氧化石墨烯(GO)悬浮液对熔纺羟丙基改性木质素/聚酰胺(PA1010)50:50重量比的共混前驱体纤维进行预处理,增强了其热稳定性,这对于碳纤维生产中的热稳定阶段至关重要。与用于木质素基纤维的典型加热速率0.1-0.25℃/分钟相比,这种预处理使得纤维随后能够以20℃/分钟的更快加热速率进行热稳定化,从而将总的热稳定时间从29小时减少到2.5小时。稳定后的长丝在950℃成功碳化,得到了连贯、无空隙且无丝间融合的碳纤维。热稳定后,经GO处理的长丝的拉伸模量从1.3 GPa提高到了2.3 GPa。然而,所得碳纤维本质上是脆性的。使用了包括DSC、TGA、FTIR、SEM-EDX、AFM、XPS和拉伸测试在内的各种表征技术来分析物理化学变化。DSC表明,GO提高了前驱体长丝的多晶性,并有助于在热稳定过程中形成三维交联网络,抑制了PA的熔融吸热。TGA证实,经GO处理的长丝比未处理的纤维具有更高的炭产率(约40%),进一步支持了GO引发的交联反应。FTIR、SEM-EDX和AFM证实了GO涂层均匀。对GO预处理变量的研究表明,需要降低GO浓度以减少所得碳纤维的脆性,但代价是增加热稳定时间。