MECHANICAL PROPERTIES OF SURFACTANT-COATING CARBON NANOFIBER/EPOXY COMPOSITE
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1 International Journal of Nanoscience, Vol. 1, Nos. 5 & 6 (2002) 1 6 c World Scientific Publishing Company MECHANICAL PROPERTIES OF SURFACTANT-COATING CARBON NANOFIBER/EPOXY COMPOSITE ZHE YING,, JIN-HONG DU, SHUO BAI, FENG LI, CHANG LIU, and HUI-MING CHENG Shenyang National Laboratory for Materials Science Institute of Metal Research, Chinese Academy of Sciences 72 Wenhua Road, Shenyang , China zying@imr.ac.cn Received 27 November 2002 Revised 24 December 2002 Carbon nanofibers (CNFs) were coated by surfactants of polyoxyetheylene alkyl ether (AEO 9, AEO 7 ) and polyvinyl alcohol (PVA 1799), respectively, after being mixed with surfactant aqueous solution and then treated with ultrasonication, high shear and magnetic stirring. The CNF/epoxy composites were prepared by mixing the surfactant coated CNFs with epoxy. Tensile strength, elastic modulus and ultimate strain of the composites were studied. The tensile strength and the ultimate strain of the composites were increased by 20% and 70%, respectively, after the CNFs were coated by surfactants. However, the elastic modulus of the composite will be lowered when the CNFs were treated by too high a concentration of surfactant solution. Keywords: Carbon nanofibers; composites; surfactant; mechanical property. 1. Introduction Due to their unique structure and extraordinary mechanical properties, carbon nanofibers (CNFs) are considered as a promising composite fillers and reinforcements. 1 4 CNF reinforced polymer composites have also attracted much research interest However, CNFs tend to agglomerate together and they are difficult to have it uniformly dispersed in the matrix, due to the strong interaction effect. Moreover, the interaction between the CNFs and the matrix is another important problem that need to be solved. Only when CNFs have strong interaction with polymer matrix, they can act as an effective reinforcing agent, which assures an effective transfer of the load from the polymer matrix to the CNFs when the composite is load-bearing. Presently, there are two main kinds of methods of surface treatment for CNFs employed to improve their interaction with the polymer matrix. One is surface functionalization 10 : some functional groups, which can improve the interaction between the CNF and the polymer matrix, are introduced into Corresponding author. 1
2 2 Z. Ying et al. the surface of the CNFs; another method is to have the CNFs physically coated by some surfactants with interaction-improving groups. These two methods have achieved good results in the preparation of CNF/polymer composites. However, organic solvents are not suitable for mass application due to their high cost and harm. In this paper, we chose several water-solvable surface-active resins and surfactants as the coating agents to prepare surfactant-coating CNFs. The CNF/epoxy composites were prepared, and their tensile properties were studied. The influence of surfactant-coating on the mechanical properties of the composites was investigated and discussed. 2. Experimental In our experiment, carbon nanofibers were prepared by a floating catalyst method. 12 An SEM observation revealed that the average diameter of the CNFs was about 200 nm, and the purity was about 80% Pre-treatment and surfactant coating of CNFs The CNFs were pulverized and annealed at 300 C under inert atmosphere for 2 h in order to remove organic materials introduced during preparation. The CNFs were then put into the aqueous solution of surfactants (AEO 7 and AEO 9 ), watersoluble resin (PVA 1799). A homogeneous suspension was obtained with magnetic stirring, ultrasonic and high shear stirring. Finally the coated CNFs were prepared by evaporating water in vacuum Preparation of CNF/epoxy composites The surfactant-coating CNFs were mixed with epoxy resin (Bisphenol A- epichlorhydrine, hydroxylated polyamide), and stirred at 300 rpm for 1 h. The composite fluid was poured into a mold and vacuum degassed. The CNF/epoxy composite was cured for 4 h at 100 C Tensile test The as-prepared composite with mold was cut into dumbbell-shaped samples. After the samples were annealed at 110 C for 10 h, the tensile test was performed with an Instron 127 Elongation Analyzer at 10 mm/min at room temperature SEM observations Surfactant-coating CNFs were observed by SEM and were analyzed by X-ray energy depressive spectroscopy (EDS). The fractural surface of CNF/epoxy composites and the interface between CNFs and epoxy matrix were also investigated.
3 Mechanical Properties of Surfactant-Coating Carbon Nanofiber/Epoxy Composite 3 a b Fig. 1. SEM images of (a) CNFs and (b) surfactant AEO 7 -coating CNFs. 3. Results and Discussion 3.1. Mechanical properties of surfactant-coating CNF/epoxy composite SEM images of AEO 7 -coating CNFs are shown in Fig. 1. We can see that the diameter of AEO 7 -coating CNFs is larger than that of as-prepared CNFs. The EDS spectrum showed that the oxygen content of the coated CNFs is higher than that of CNFs, which may have been introduced by AEO 7. According to these results, we conclude that the CNFs have been effectively coated by AEO 7. The results for AEO 9 and PVA 1799 are similar. Tensile properties of the surfactant-coating CNF/epoxy composite are shown in Fig. 2 and Table 1. Tensile strength of the composites can be improved up to about 20% by using the surfactant-coating CNFs, and the ultimate strain can be improved by as much as 60%. The functional mechanism of the surfactants may be these surfactants have hydrophilic segment as well as hydrophobic segment, the hydrophobic segment would wind around the surface of CNFs, while the hydrophilic ones stress(mpa) PVA AEO 30 9 EPOXY 20 no surfactant AEO strain(%) Fig. 2. Stress strain curves for different surfactant-coating CNF/epoxy composite.
4 4 Z. Ying et al. Table 1. Tensile properties of different surfactant-coating CNF/epoxy composite. CNF content Tensile strength Elastic modulus Ultimate strain (Wt %) Surfactant (MPa) (MPa) (%) PVA(1799) AEO AEO distribute outside of the CNFs and form hydrogen bonding with epoxy, 8 which is in favor of the dispersion of CNFs among epoxy matrix and improve the interfacial behavior. As a result, the load can be effectively transferred onto the CNFs when the composite is load-bearing. For AEO 7 and AEO 9, the hydrophobic segment is alkyl (mostly dodecyl), the hydrophilic segment is polyoxyethylene and hydroxy. The alkyl has strong interfacial bonding with CNFs, and the hydroxy and polyoxyethylene had strong interfacial bonding with epoxy. So AEO 7 and AEO 9 worked as reinforcement agent of the interfacial bonding of CNFs and epoxy. For PVA, the hydrophobic segment is polyethylene chain with hydroxy, and the hydrophilic is hydroxy. So PVA has an effect analogous to polyoxyethylene alkyl ether. However, there are many hydroxys on polyethylene chain, the hydrophobic properties of the polyethylene chain was weaker than that of the alkyl. So AEO 7 (or AEO 9 ) should have stronger interfacial bonding effect than for PVA Figure 3 shows the fractural surfaces of CNF (with and without surfactant-coating)/epoxy composites. In the case of the CNFs are not coated by surfactant, many CNFs were pulled out from epoxy matrix and slick ducks were left; when the CNFs are coated, the broken CNFs can be observed. These results indicate that the interfacial bonding between the coated CNFs and the epoxy is strong, while that between the uncoated CNFs and the epoxy is weak. a b Fig. 3. SEM images of fracture surface of (a) CNF/epoxy composite and (b) surfactant-coating CNF/epoxy composite.
5 Mechanical Properties of Surfactant-Coating Carbon Nanofiber/Epoxy Composite 5 Table 2. Tensile properties for CNF/epoxy composites with different ratio of surfactant to CNFs. Weight ratio of Tensile strength Elastic modulus Ultimate strain surfactant: CNF (MPa) (MPa) (%) 0: : : stress(mpa) no surfactant AEO 9 50% AEO 9 33% strain(%) Fig. 4. Stress strain curves of the composites with different surfactant contents Effect of the surfactant concentration on the tensile properties of the CNF/epoxy composite Two AEO 9 concentrations were employed to evaluate the surfactant concentration effect. The tensile results of the composites obtained are listed in Table 2 and Fig. 4. It is showed that with the increase in the AEO 9 concentration, the tensile strength does not increase, apart from the increase in the elongation. There is a noticeable decrease in elastic modulus due to the surplus surfactant acted as the plasticizer of the epoxy matrix. The plasticizers will dilute polymer matrix and the weaker interaction between polymer chains, so the elastic modulus of polymer matrix was decreased. Therefore, a suitable concentration of surfactants is important to improve the overall mechanical properties of CNF/epoxy composites. 4. Conclusion Three kinds of surfactants (PVA 1799, AEO 7 and AEO 9 ) were coated on the surface of CNFs, and then surfactant-coating CNF/epoxy composites were fabricated. The surfactants can be effectively coated on the CNFs thus enhance the interfacial bonding between the CNFs and the polymer matrix. The max increase of the tensile strength and the ultimate strain of the composites were increased by 20% and 70%, respectively, as compared with the composites reinforced by as-prepared CNFs. When the percentage of the added surfactants is too high, the surplus surfactant
6 6 Z. Ying et al. acted as plasticizer and lowered the elastic modulus of the composites. Moreover, AEO 9 seems to be the most effective surfactant to improve the tensile properties of CNF/epoxy composites. Acknowledgment This work was supported by the National Natural Science Foundation of China (Nos and ) and by Chinese Academy of Sciences. References 1. Z. Jin, W. Sun, G. Xu, S. H. Goh, and W. Ji, Chem. Phys. Lett. 318, 505 (2000). 2. D. Qian, E. C. Dickey, R. Andrews, and T. Rantell, Appl. Phys. Lett. 76(20), 2868 (2000). 3. A. Peigney, E. Flahart, C. H. Laurent, F. Chastel, and A. Rousset, Chem. Phys. Lett. 52, 20 (2002). 4. C. L. Xu, B. Q. Wei, R. Z. Ma, J. Liang, X. K. Ma, and D. H. Wu, Carbon 37, 855 (1999). 5. M. S. P. Shaffer and A. H. Windle, Adv. Mater. 11, 937 (1999). 6. L. Jin, C. Bower, and O. Zhou, Appl. Phys. Lett. 73, 1197 (1998). 7. C. Bower, R. Rosen, L. Jin, J. Han, and O. Zhou, Appl. Phys. Lett. 74, 3317 (1999). 8. X. G. Gong, J. Liu, S. Baskaran, R. D. Voise, and J. S. Young, Chem. Mater. 12, 1049 (2000). 9. R. Haggenmueller, H. H. Gommans, A. G. Rinzler, and J. E. Fischer, Chem. Phys. Lett. 330, 219 (2000). 10. K. Lozano and E. V. Barrera, J. Appl. Polym. Sci. 79, 125 (2001). 11. A. Rodney, J. David, M. Mickael, and R. Terry, Macromol. Mater. Eng. 287, 395 (2002). 12. Y. Y. Fan, H. M. Cheng, Y. L. Wei, G. Su, and Z. H. Shen, Carbon 38(6), 921 (2000).
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