氨气处理碳纤维 第I报 表面组成和反应机理Effect of Free Ammonia Treatment on the Surface Composition of Carbon Fiber and Reactions Mechanism
胡培贤,温月芳,杨永岗,刘朗
HU Pei-xian1,2, WEN Yue-fang1, YANG Yong-gang1
摘要(Abstract):
采用原位漫反射红外光谱(FT-IR)在线分析碳纤维表面谱图变化。结果发现,当温度升至500℃后,3260cm-1处吸收峰减弱,在3157cm-1、3048cm-1、2829cm-1和1405cm-1处新增吸收峰。用X-射线光电子能谱(XPS)对未处理与在氨气气氛中600℃处理30s后碳纤维的表面官能团组成进行分析对比发现,处理后的碳纤维表面氮元素显著增加,而氧含量降低。由FT-IR和XPS的谱图变化推测出在高温时,碳纤维表面的羟基和羧基与氨气发生反应,形成了氨基官能团。
The changes of infrared spectra for the surface of carbon fibers (CFs) were investigated on-line by FT-IR. When the reaction temperature exceeded 500 ℃, the strength of absorption peak at 3 260 cm-1 decreased and new characteristic peaks at 3 157 cm-1, 3 048 cm-1, 2 829 cm-1 and 1 405 cm-1 appeared. After been treated by free ammonia at 600 ℃ for 30 s, functional groups on the surface of the treated CFs and the untreated ones were contrasted by X-ray photoelectron spectroscopy(XPS). The nitrogen content on the surface was found to increase, while the oxygen content decreased. Concerning the changes in XPS and FT-IR spectra, it supposed that the hydroxyl and carboxyl on the surface of CFs had reacted with free ammonia at high temperature, which introduced amino groups to the surface of CFs.
关键词(KeyWords):
碳纤维;表面处理;氨气;氨基
carbon fiber, surface treatment, free ammonia, amino group
基金项目(Foundation): 973项目(编号:2006CB605304);; 国家自然科学基金项目(编号:50604025)
作者(Author):
胡培贤,温月芳,杨永岗,刘朗
HU Pei-xian1,2, WEN Yue-fang1, YANG Yong-gang1
参考文献(References):
- [1]Z R Yue,W Jiang,L Wang,et al.Surface characterization of elec-trochemically oxidized carbon fibers[J].Carbon,1999,37(11):1785-1796.
- [2]Y D Huang,L Liu,J H Qiu,et al.Influence of ultrasonic treatment on the characteristics of epoxy resin and the interfacial property of its carbon fiber composites[J].Composites Science and Technology,2002,62(16):2153-2159.
- [3]M A Montes-Mora′n,F W J van Hattum,J P Nunes,et al.A study of the effect of plasma treatment on the interfacial properties of carbon fi-bre-thermoplastic composites[J].Carbon,2005;43(8):1778-1814.
- [4]刘鸿鹏,吕春祥,李永红等.电化学表面处理PAN基碳纤维的表面性能研究[J].新型碳材料,2005,20(1):39-44.
- [5]Park S J,Seo M K,Lee Y S.Surface characteristics of fluorine-modified PAN-based carbon fibers[J].Carbon,2003;41(4):723-730.
- [6]Junqing Li,Yudong Huang,Zhiwei Xu,et al.High-energy radiation technique treat on the surface of carbon fiber[J].Materials Chemistry and Physics,2005,94:315-321.
- [7]T Ramanathan,A Bismark,E Schulz,et al.Investigation of the influ-ence of asidic and basic surface groups on carbon fibers on the interfacial shear strength in an epoxy matrix by means of single-fiber pull-out test[J].Composites Science and Technology,2001,61(4):599-605.
- [8]Buttry D A,Peng J C M,Donnet J B,et al.Immobilization of amines at carbon fiber surfaces[J].Carbon1999,37(12):1929-1940
- [9]Hiroto Fujimaki,Fumio Kodama,Reiho Takabe,et al.Process for the surface treatment of carbon fibers:US,4009305[P].1977.
- [10]Kawashima Keiko,Takahashi Hidefumi,el at.Adhesion characteris-tics of carbon fibers surface-modified with amino group[J].Tanso,2000,195:336.
- [11]余木火,赵世平,藤翠青等.碳纤维表面氨基化处理提高复合材料的界面粘合性[J].纤维复合材料,1999,20(4):20-22.
- [12]Stuart Mitchell.Multielectrolyte shear treatment of carbon fibers:US,4729820[P].1988.
- [13]Fujio N,Hirofumi U,Hiroshima.Surface treatment process for car-bon fibers:US,4839006[P].1989.
- [14]Seung-Kon Ryu,Byung-Jae Park,Soo-Jin Park.XPS analysis of carbon fiber surfaces-anodized and interfacial effects in fiber-epoxy com-posites[J].Journal Colloid and Interface Science.1999,215:169.
- [15]贺福.碳纤维及其应用技术[M].北京:化学工业出版社,2004:206.
- [16]Leea W H,Leea J G,Reucroft P J.XPS study of carbon fibers sur-faces treated by thermal oxidation in a gas mixture of O2/(O2+N2)[J].Appl Surf Sci,2001,171(2):136-142.