油剂对聚丙烯腈原丝预氧化与低温碳化的影响Effect of Finishes on the Structural Transformation of PAN Precursor Fiber during the Pre-Oxidation and Low-Temperature Carbonization Process
邹瑞芬,欧阳琴,王雪飞,陈友汜
ZOU Rui-fen,OUYANG Qin,WANG Xue-fei,CHEN You-si(National Engineering Laboratory for Carbon Fiber Preparation Technology
摘要(Abstract):
在相同聚合、纺丝工艺条件下制得两种分别上有不同油剂(No.1、No.2)的聚丙烯腈(PAN)原丝,然后在相同工艺条件下依次进行预氧化、低温碳化处理。采用红外光谱和X-射线衍射表征了两种原丝的预氧化结构,采用差示扫描量热仪研究了预氧丝除油前后在低温碳化阶段的热行为,结果表明:采用No.1油剂的PAN原丝预氧化程度较高,表面除油后在低温碳化阶段时质量损失较小,表现出较好的耐热性;但在不除油的情况下,采用耐热性好的No.2油剂的PAN原丝尽管预氧化程度较低,但在低温碳化阶段时质量损失较小,表现出更好的耐热性。与预氧化程度相比,油剂的耐热性对预氧化纤维在低温碳化阶段的热行为影响更大。
Two different finishes named No.1 and No.2 were separately applied to PAN precursor fibers prepared under the same conditions of polymerization,spinning,and then the the fibers were treated in pre-oxidation and carbonization.The structure of the pre-oxidized fibers was characterized by FTIR and XRD.A comparative study on the thermal properties was made by using DSC/TG regarding both the untreated pre-oxidized fibers and the treated pre-oxidized fibers from which the finish was extracted by using the organic solvent.The results showed that the No.1 finish-applied PAN precursor fiber had a higher pre-oxidization degree resulting in a better heat-resistance and less weight-lose after removing finishes during the low-temperature carbonization.Referring to the pristine oxidized fibers,although No.2 finish-applied fiber had a lower oxidization degree,it had a better heat-resistance and less weight-lose because the No.2 finish had much excellent heat-resistance than No.1 finish.
关键词(KeyWords):
油剂;聚丙烯腈原丝;碳纤维;预氧化;低温碳化
finish,PAN precursor,carbon fiber,pre-oxidation,low-temperature carbonization
基金项目(Foundation): 国家重点基础研究发展计划项目(2011CB605602);; 浙江省重点科技创新团队项目(2011R50013)
作者(Author):
邹瑞芬,欧阳琴,王雪飞,陈友汜
ZOU Rui-fen,OUYANG Qin,WANG Xue-fei,CHEN You-si(National Engineering Laboratory for Carbon Fiber Preparation Technology
DOI: 10.16090/j.cnki.hcxw.2013.06.006
参考文献(References):
- [1]Yoshinobu Okabe,Yoshiaki Tanaka,Yoshio Hashimoto,et al.Finishfor acrylic fiber processed into carbon fiber,and carbon fiber manufac-turing method therewith:US,0263576[P].2009-10-22.
- [2]Hiromi Aso,Naoki Sugiura.Oil agent composition for acrylic precur-sor fibers for carbon fibers,acrylic precursor fiber bundle for producingthe same:US,0247911[P].2010-09-30.
- [3]Kunio Maruyama,Ryuichi Koide.Finishing oil for precursor for highperformance carbon fibers and precursor:US,5726241[P].1998-03-10.
- [4]Takao Masaki,Tomoo Komatsubara,Yoshiaki Tanaka.Finish for car-bon fiber precursors:US,5783305[P].1998-07-21.
- [5]贺福.高性能碳纤维原丝与油剂[J].高科技纤维与应用,2004,29(5):1-5.
- [6]张淑斌,王浩静.氨改性硅油的合成、表征及其在PAN基碳纤维原丝预氧化过程中的作用[J].合成纤维,2010,38(1):17-19.
- [7]郭雅明,李常清,马晓娜,等.硅系油剂对PAN纤维预氧化的影响[J].材料科学与工程学报,2011,29(4):555-558.
- [8]Jin DB,Huang Y,Liu XL,et al.The influence of silicone finishes onthermooxidative stabilization of PAN precursor fibers[J].J Mater Sci,2004,39:3 365-3 368.
- [9]张淑斌,王浩静.油剂处理对原丝热性能的影响[J].高科技纤维与应用,2009,34(5):26-29.
- [10]Mittal J,Bahl O P,Mathur R B,et al.IR studies of PAN fibres ther-mally stabilized[J].Carbon,1994,32(6):1 133-1 136.
- [11]Shimada I,Takahagi T,Fukuhara M,et al.FT-IR study of the stabi-lization reaction of polyacrylonitrile in the production of carbon fibers[J].JPolym Sic,Part A:Polym Chem,1986,24(8):1 989-1 995.
- [12]Jiang H,Wu C,Zhang A,et al.Structural characteristics of polyacry-lonitrile(PAN)fibers during oxidative stabilization[J].Compos Sci Tech-nol,1987,29(1):33-44.
- [13]Zhang WX,Liu J,Wu G.Evolution of structure and properties ofPAN precursors during their conversion to carbon fibers[J].Carbon,2003,41:2 805-2 812.
- [14]贺福.碳纤维及石墨纤维[M].北京:化学工业出版社,2010.
- 邹瑞芬
- 欧阳琴
- 王雪飞
- 陈友汜
ZOU Rui-fen - OUYANG Qin
- WANG Xue-fei
- CHEN You-si(National Engineering Laboratory for Carbon Fiber Preparation Technology
- 邹瑞芬
- 欧阳琴
- 王雪飞
- 陈友汜
ZOU Rui-fen - OUYANG Qin
- WANG Xue-fei
- CHEN You-si(National Engineering Laboratory for Carbon Fiber Preparation Technology