Study of the Method for the Accurate Determination of Gel Content in Cured Polyaluminocarbosilane Fibers

IF 2.8 3区 材料科学 Q3 CHEMISTRY, PHYSICAL Silicon Pub Date : 2025-02-07 DOI:10.1007/s12633-025-03237-3
Zhijing Li, Jing Huang, Zhanshuo Miao, Xiaoyu Wang, Qin Ouyang, Gaoming Mo, Qing Huang, Qiang Wei
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Abstract

The curing process is the key process for preparing SiC fibers. Currently, there are fewer reports on the measurement methods related to the curing degree, leading to a lack of effective guidance for controlling the curing degree. The gel content of cured fibers can be measured through Soxhlet extraction to reflect the curing degree, which can be utilized to guide the control of the curing process of fibers. However, there are limited reports on the key influencing factors for accurately determining the gel content through Soxhlet extraction, such as the selection of appropriate extractant, extraction temperature, extraction time, and the selection of wrapping materials for cured fibers with stable mass which require further investigation. In this work, cured polyaluminocarbosilane (PACS) fibers with air oxidation curing are utilized as the research subject, and provide a reference for an accurate method to determine the gel content in cured fibers based on Soxhlet extraction. A wrapping material with lower water absorption and lower cost is preferred, and the effects of key factors such as the extractant, extraction temperature, extraction time, and number of extraction experiments on the accurate determination of gel content are examined to establish the optimal testing conditions. The accuracy and reliability of the method are further verified. This method is anticipated to be expanded to determine the gel content in other types of cured fibers and the cured fibers crosslinked by different processes, providing an effective means of characterizing the control of curing degree in the preparation process of precursor-derived SiC fibers.

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固化过程是制备碳化硅纤维的关键过程。目前,有关固化度测量方法的报道较少,导致对固化度的控制缺乏有效的指导。通过索氏提取法测量固化纤维的凝胶含量可以反映固化度,从而指导纤维固化过程的控制。然而,关于通过索氏提取准确测定凝胶含量的关键影响因素,如选择合适的提取剂、提取温度、提取时间,以及选择质量稳定的固化纤维包覆材料等,目前报道有限,有待进一步研究。本研究以空气氧化固化的聚铝碳硅烷(PACS)纤维为研究对象,为基于索氏提取法精确测定固化纤维中的凝胶含量提供参考。优选吸水性较低、成本较低的包覆材料,考察萃取剂、萃取温度、萃取时间、萃取实验次数等关键因素对准确测定凝胶含量的影响,以确定最佳测试条件。进一步验证了该方法的准确性和可靠性。预计该方法将扩展到其他类型固化纤维和不同工艺交联的固化纤维的凝胶含量测定,为表征前驱体衍生碳化硅纤维制备过程中固化程度的控制提供有效手段。
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来源期刊
Silicon
Silicon CHEMISTRY, PHYSICAL-MATERIALS SCIENCE, MULTIDISCIPLINARY
CiteScore
5.90
自引率
20.60%
发文量
685
审稿时长
>12 weeks
期刊介绍: The journal Silicon is intended to serve all those involved in studying the role of silicon as an enabling element in materials science. There are no restrictions on disciplinary boundaries provided the focus is on silicon-based materials or adds significantly to the understanding of such materials. Accordingly, such contributions are welcome in the areas of inorganic and organic chemistry, physics, biology, engineering, nanoscience, environmental science, electronics and optoelectronics, and modeling and theory. Relevant silicon-based materials include, but are not limited to, semiconductors, polymers, composites, ceramics, glasses, coatings, resins, composites, small molecules, and thin films.
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