CERAMICS 要 INTERNATIONAL ELSEVIER Ceramics International 32(2006)291-295 Influence of heat treatment on physical-chemical properties of PAN-based carbon fiber Song Wang", Zhao-Hui Chen, Wu-Jun Ma, Qing-Song Ma Key Laboratory of Advanced Ceramic Fibres and sites, College of Aerospace and Materials Engineering National University of Defense Technology, Changsha 410073, PR China b Shanghai Institute of Space Propulsion, Shanghai 200233, PR China Received 20 December 2004: received in revised form 21 December 2004; accepted 27 February 2005 Available online 13 May 2005 Abstract The influence of heat treatment at 1400C on physical-chemical properties of PAN-based high strength carbon fiber was investigated by means of TG, XRD, XPS as well as the tensile test. The results showed that heat treatment could improve the thermal stability and the degree of graphitization of carbon fiber and decrease the amount of functional groups on the surface. The tensile strength of carbon fiber was no found declined after heat treatment because the change of the microstructure caused by heat treatment was limited. C 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved. Keywords: Carbon fiber; Heat treatment; Physical-chemical properties 1. Introduction 5, 6]. Heat treatment is another treatment technique of carbon fibers and has been applied in the preparation of Carbon fibers offer numerous advantages, such as light arbon fiber reinforced ceramic matrix composites [7]. But it weight and excellent mechanical properties at room and is still not well clear which properties of the carbon fiber are elevated temperature. Carbon fiber reinforced composites affected by heat treatment and how the heat treatment on have been widely used in the fields of aerospace and high carbon fiber affected the load transfer mechanism and technical products. To realize the excellent mechanical energy dissipation in ceramic matrix composites properties of carbon fibers in composites, it is necessary to In this study, the t300 carbon fiber were heat treated at have a desirable fiber/matrix interface to ensure effective 00C in vacuum, and the physical and chemical load transfer from one fiber to another through the matrix properties of as-received and heat treated carbon fibers [1, 2]. The interfacial properties largely depend on the carbon were examined in order to understand the influence of heat fiber surface. As a result, many researches focus on the treatment on physical-chemical properties of carbon fiber surface treatment of carbon fibers to get a good interface and and gain an insight into how the heat treatment of carbon composites with perfect mechanical properties [3, 4]. Sur- fibers affected the mechanical properties of carbon fiber face oxidation of carbon fibers was the dominating surface reinforced ceramic matrix composites treatment technique. Surface oxidation can increase the quantity of functional groups on the fiber surface, and then strengthen the interfacial bonding. However, strong inter- 2. Experimental facial bonding is not always good for mechanical properties of composites, especially for ceramic PAN-based high strength carbon fiber with a trade name of T300 was used in this study. The physical properties of the fiber are listed in Table 1. The T300 fiber as received E-mailaddress:wangsong0731@163.com(S.Wang) commercially was named as sample T-0. T-4 indicated the 0272-8842/S30.00@ 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved doi: 10. 1016/1. ceramint 2005.02.014
Influence of heat treatment on physical–chemical properties of PAN-based carbon fiber Song Wang a, *, Zhao-Hui Chen a , Wu-Jun Ma b , Qing-Song Ma a a Key Laboratory of Advanced Ceramic Fibres and Composites, College of Aerospace and Materials Engineering, National University of Defense Technology, Changsha 410073, PR China b Shanghai Institute of Space Propulsion, Shanghai 200233, PR China Received 20 December 2004; received in revised form 21 December 2004; accepted 27 February 2005 Available online 13 May 2005 Abstract The influence of heat treatment at 1400 8C on physical–chemical properties of PAN-based high strength carbon fiber was investigated by means of TG, XRD, XPS as well as the tensile test. The results showed that heat treatment could improve the thermal stability and the degree of graphitization of carbon fiber and decrease the amount of functional groups on the surface. The tensile strength of carbon fiber was not found declined after heat treatment because the change of the microstructure caused by heat treatment was limited. # 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved. Keywords: Carbon fiber; Heat treatment; Physical–chemical properties 1. Introduction Carbon fibers offer numerous advantages, such as lightweight and excellent mechanical properties at room and elevated temperature. Carbon fiber reinforced composites have been widely used in the fields of aerospace and high technical products. To realize the excellent mechanical properties of carbon fibers in composites, it is necessary to have a desirable fiber/matrix interface to ensure effective load transfer from one fiber to another through the matrix [1,2]. The interfacial properties largely depend on the carbon fiber surface. As a result, many researches focus on the surface treatment of carbon fibers to get a good interface and composites with perfect mechanical properties [3,4]. Surface oxidation of carbon fibers was the dominating surface treatment technique. Surface oxidation can increase the quantity of functional groups on the fiber surface, and then strengthen the interfacial bonding. However, strong interfacial bonding is not always good for mechanical properties of composites, especially for ceramic matrix composites [5,6]. Heat treatment is another treatment technique of carbon fibers and has been applied in the preparation of carbon fiber reinforced ceramic matrix composites [7]. But it is still not well clear which properties of the carbon fiber are affected by heat treatment and how the heat treatment on carbon fiber affected the load transfer mechanism and energy dissipation in ceramic matrix composites. In this study, the T300 carbon fiber were heat treated at 1400 8C in vacuum, and the physical and chemical properties of as-received and heat treated carbon fibers were examined in order to understand the influence of heat treatment on physical–chemical properties of carbon fiber and gain an insight into how the heat treatment of carbon fibers affected the mechanical properties of carbon fiber reinforced ceramic matrix composites. 2. Experimental PAN-based high strength carbon fiber with a trade name of T300 was used in this study. The physical properties of the fiber are listed in Table 1. The T300 fiber as received commercially was named as sample T-0. T-4 indicated the www.elsevier.com/locate/ceramint Ceramics International 32 (2006) 291–295 * Corresponding author. E-mail address: wangsong0731@163.com (S. Wang). 0272-8842/$30.00 # 2005 Elsevier Ltd and Techna Group S.r.l. All rights reserved. doi:10.1016/j.ceramint.2005.02.014
S. Wang et al. /Ceramics International 32(2006) Table 1 Physicalproperties began to lose weight at450°C,550°C,and600°Cand of t300 carbon fiber remained 38%0, 44%, and 72% of original weight at 1200C, respectively, demonstrating that the thermal stability of carbon fibers can be improved by heat treatment At 450C, Density(g/cm) the weight loss of T-0 was due to the removal of organic 3.4 ng on fiber surface. With the increase of temperature, the Youngs modulus(GPa) removal of N, O atoms from the residual nitrogen and Elongation break(%) oxygen in the precursor fibers was partly responsible for the weight loss. Because sample T-14 suffered weight loss of less than 5 wt. during heat treatment at 1400C, its weight fibers after heat treating at 400C. T-14 was the fiber heat loss under N2(common purity) from 50C to 1200C was treated at 1400C in vacuum for 1 h mainly caused by the attack of impurity in N2 to fibers at The thermal stability of the samples from 50C to elevated temperature, such as Oz, CO2, and H2O. TGA 1200C was characterized by thermal gravimetric analysis suggested that T-14 have a better resistance to the attack of TGA)at a heating rate of 10C/min. A common purity impurity at elevated temperature (99%)nitrogen flow 50 cm" was used during test. X ray diffraction(XRD) was used to determine the crystallite 2C(s)+O2(g)→2COg) characteristics of specimens. XRD patterns of the samples were obtained from a dsadvance diffractometer using C(s)+CO2(g)→2CO(g) Cu Ka radiation(=0.15418 nm)as the source for C(s)+ H2O(g)-Co(g)+H2(g) measuring the interlayer spacing. X-ray photoelectron pectroscopy (XPs)was used to analyze the surface chemistry of samples. The data were obtained from an 3.2. Surface chemistry ESCALab220i-XL electron spectrometer using 300WA Ka radiation. The base pressure was about 3 x 10-mbar In Fig. 2, the XPS surveys of T-4 and T-14 exhibited The survey spectrum was collected from 0 eV to 1200 eV, onspicuous features due to carbon and oxygen. Minor and the binding energies were referenced to the C ls line at peaks due to nitrogen and silicon could also be discerned in 284.6eV from adventitious carbon. The tensile strength of T-4's spectrum, while undiscerned in T-14's spectrum fiber samples was measured by single fiber strength and Based on the survey spectrum results, the atom percents of C bundle strength. ls(≈285eV),Nls(≈400eV),Ols(≈533ev) and Si2p (a102 ev) in fiber surface were calculated fron peaks intensities, which were listed in Table 2. The 3. Results and discussion concentrations of O and n in T-4 were both nearly eight times higher than those in T-14. and the C concentration in 3.1. Thermal stability of carbon fibers T-4(86.0 at. %)was lower than that in T-14(98.0 at. %) The surface activity of carbon fiber is determined by Fig. 1 shows TG curves of carbon fibers under nitrogen many factors such as the concentration of oxygen atom, the from 50.C to 1200.C. It is clear that T-0, T-4, and T-14 O/C atomic ratio, C ls binding state and o ls binding state O1s 80 Nis T14 T-4 12001000
fibers after heat treating at 400 8C. T-14 was the fiber heat treated at 1400 8C in vacuum for 1 h. The thermal stability of the samples from 50 8C to 1200 8C was characterized by thermal gravimetric analysis (TGA) at a heating rate of 10 8C/min. A common purity (99%) nitrogen flow 50 cm3 min1 was used during test. Xray diffraction (XRD) was used to determine the crystallite characteristics of specimens. XRD patterns of the samples were obtained from a D8ADVANCE diffractometer using Cu Ka radiation (l = 0.15418 nm) as the source for measuring the interlayer spacing. X-ray photoelectron spectroscopy (XPS) was used to analyze the surface chemistry of samples. The data were obtained from an ESCALab220i-XL electron spectrometer using 300 W Al Ka radiation. The base pressure was about 3 109 mbar. The survey spectrum was collected from 0 eV to 1200 eV, and the binding energies were referenced to the C 1s line at 284.6 eV from adventitious carbon. The tensile strength of fiber samples was measured by single fiber strength and bundle strength. 3. Results and discussion 3.1. Thermal stability of carbon fibers Fig. 1 shows TG curves of carbon fibers under nitrogen from 50 8C to 1200 8C. It is clear that T-0, T-4, and T-14 began to lose weight at 450 8C, 550 8C, and 600 8C and remained 38%, 44%, and 72% of original weight at 1200 8C, respectively, demonstrating that the thermal stability of carbon fibers can be improved by heat treatment. At 450 8C, the weight loss of T-0 was due to the removal of organic sizing on fiber surface. With the increase of temperature, the removal of N, O atoms from the residual nitrogen and oxygen in the precursor fibers was partly responsible for the weight loss. Because sample T-14 suffered weight loss of less than 5 wt.% during heat treatment at 1400 8C, its weight loss under N2 (common purity) from 50 8C to 1200 8C was mainly caused by the attack of impurity in N2 to fibers at elevated temperature, such as O2, CO2, and H2O. TGA suggested that T-14 have a better resistance to the attack of impurity at elevated temperature. 2CðsÞ þ O2ðgÞ ! 2COðgÞ CðsÞ þ CO2ðgÞ ! 2COðgÞ CðsÞ þ H2OðgÞ ! COðgÞ þ H2ðgÞ 3.2. Surface chemistry In Fig. 2, the XPS surveys of T-4 and T-14 exhibited conspicuous features due to carbon and oxygen. Minor peaks due to nitrogen and silicon could also be discerned in T-4’s spectrum, while undiscerned in T-14’s spectrum. Based on the survey spectrum results, the atom percents of C 1s (285 eV), N 1s (400 eV), O 1s (533 eV) and Si 2p (102 eV) in fiber surface were calculated from peaks intensities, which were listed in Table 2. The concentrations of O and N in T-4 were both nearly eight times higher than those in T-14, and the C concentration in T-4 (86.0 at.%) was lower than that in T-14 (98.0 at.%). The surface activity of carbon fiber is determined by many factors such as the concentration of oxygen atom, the O/C atomic ratio, C 1s binding state and O 1s binding state. 292 S. Wang et al. / Ceramics International 32 (2006) 291–295 Table 1 Physical properties of T300 carbon fiber Species T300 Filament count 3000 Density (g/cm3 ) 1.75 Average diameter (mm) 7 Tensile strength (GPa) 3.45 Young’s modulus (GPa) 230 Elongation break (%) 1.5 Fig. 1. TG curves of samples. Fig. 2. XPS survey of samples.
Table 2 sharp peaks similar to the graphite fiber M40J. The average Fiber surface chemistry of different samples interlayer spacing door and the crystallite dimensions Lc(002 (at%) can be determined by XRD measurements [11-13, by using C Is O Is N Is Si 2p Bragg and Scherrer formulas, respectively, 0.114 1= 2d sin e Kλ The survey spectral features indicated that the O/C atomic ratio of T-14(0.013)was about 1/10 of that of T-4(0.11). where 8 is the scattering angle, d is the interlayer spacing, i The C ls spectrum was indicative of graphitic carbon is the wavelength of the X-rays, here was 0. 154 nm, B is the 284.6e V), carbon present as phenolic hydroxyl and/or half-maximum line width in radians. Jeffrey [14] determined ether groups(286.2 eV), carbonyl groups(287. 6eV), that the form factor K is 0.9 for L(o02. The average carboxyl and/or ester functions(288.8 eV) and possibly interlayer spacing dooz and the crystallite dimensions some carbonate species(290.6 eV)[8-10]. The O Is peaks Lc(oo2) of samples were calculated from the 002 diffraction were composed mainly of oxygen bonded in -OH groups peaks and listed in Table 3. The table showed that sample T-0 (533 e V)and inCO moieties(<531.5 eV). High relative had the biggest doo2(3.552 A)and the smallest Lc() fraction of carbon and low relative fraction of oxygen with (1.75 nm)of three samples. The data of doo2 and Lc(ooz low binding energy implied carbon fiber with low surface of T-14 were 3 490 A and 2.48 nm, and graphite fiber M40J activity. Figs. 3 and 4 shows XPS spectra of C ls and O ls of had the doo2(3.466 A)and Lcoo2)(3.00 nm).The results T-4 and T-14, respectively. It was found that relative fraction indicated that T-14 had higher graphitization degree than T- of carbon with low binding energy in T-4 was less than that 0, shortening of interlayer spacing and largening of crysta in T-14 and relative fraction of oxygen with low binding lite dimensions, but lower than M40J. The carbonization energy in T-4 was more than that in T-14. From the XPS temperature of T-0 was about 1400-1500C, but the time spectra, it maybe concluded that T-4 had high surface was very limited. As a result, after T-0 was heat-treated at activity,whereas T-14 possessed low surface activity. Heat 1400C for 1-2 h, the graphitization degree was improved. treatment at 1400C could decrease carbon fiber surface However heating to 1400C was not sufficient to obtain activity evidently similar graphitization form to the graphite fiber, conse- quently the crystallite characteristics of T-14 were between 3.3. Microstructure study hose of T-0 and M40J, even after extended treating time The average bulk structure of carbon materials can be 3. 4. Tensile strength study readily revealed using X-ray diffraction. The XRD patterns of T-0, T-14 and a kind of PAN-based high modulus type Table 4 shows the tensile strength of three sample carbon fiber M40J(Toray Co Japan)are shown in Fig. 5. As easured by single fiber means and fiber bundle mean a result, the diffraction angles 20 were around 25and 43 Different strength had been obtained by the two testing which were assigned to disordered graphitic 002 plane and means. Tensile strength of T-0 tested by single fiber me 0 I plane, respectively. The peaks of (00 2)reflections and was lower than that presented by manufacturer and that (10 1)reflections of T-0 sample were broad, while T-14 had tested by fiber bundle means, while the data gained by fiber O 1s 5000 3500 2500 2000 294292290288286284282280278276 540538536534532530528526 Fig 3. XPS spectra of C Is and O Is of sample T-4
The survey spectral features indicated that the O/C atomic ratio of T-14 (0.013) was about 1/10 of that of T-4 (0.11). The C 1s spectrum was indicative of graphitic carbon (284.6 eV), carbon present as phenolic hydroxyl and/or ether groups (286.2 eV), carbonyl groups (287.6 eV), carboxyl and/or ester functions (288.8 eV) and possibly some carbonate species (290.6 eV) [8–10]. The O 1s peaks were composed mainly of oxygen bonded in –OH groups (533 eV) and in C O moieties (531.5 eV). High relative fraction of carbon and low relative fraction of oxygen with low binding energy implied carbon fiber with low surface activity. Figs. 3 and 4 shows XPS spectra of C 1s and O 1s of T-4 and T-14, respectively. It was found that relative fraction of carbon with low binding energy in T-4 was less than that in T-14 and relative fraction of oxygen with low binding energy in T-4 was more than that in T-14. From the XPS spectra, it maybe concluded that T-4 had high surface activity, whereas T-14 possessed low surface activity. Heat treatment at 1400 8C could decrease carbon fiber surface activity evidently. 3.3. Microstructure study The average bulk structure of carbon materials can be readily revealed using X-ray diffraction. The XRD patterns of T-0, T-14 and a kind of PAN-based high modulus type carbon fiber M40J (Toray Co. Japan) are shown in Fig. 5. As a result, the diffraction angles 2u were around 258 and 438, which were assigned to disordered graphitic 0 0 2 plane and 1 0 1 plane, respectively. The peaks of (0 0 2) reflections and (1 0 1) reflections of T-0 sample were broad, while T-14 had sharp peaks similar to the graphite fiber M40J. The average interlayer spacing d002 and the crystallite dimensions Lc(002) can be determined by XRD measurements [11–13], by using Bragg and Scherrer formulas, respectively, nl ¼ 2d sin u L ¼ Kl b cos u where u is the scattering angle, d is the interlayer spacing, l is the wavelength of the X-rays, here was 0.154 nm, b is the half-maximum line width in radians. Jeffrey [14] determined that the form factor K is 0.9 for Lc(002). The average interlayer spacing d002 and the crystallite dimensions Lc(002) of samples were calculated from the 0 0 2 diffraction peaks and listed in Table 3. The table showed that sample T-0 had the biggest d002 (3.552 A˚ ´ ) and the smallest Lc(002) (1.75 nm) of three samples. The data of d002 and Lc(002) of T-14 were 3.490 A˚ ´ and 2.48 nm, and graphite fiber M40J had the d002 (3.466 A˚ ´ ) and Lc(002) (3.00 nm). The results indicated that T-14 had higher graphitization degree than T- 0, shortening of interlayer spacing and largening of crystallite dimensions, but lower than M40J. The carbonization temperature of T-0 was about 1400–1500 8C, but the time was very limited. As a result, after T-0 was heat-treated at 1400 8C for 1–2 h, the graphitization degree was improved. However, heating to 1400 8C was not sufficient to obtain similar grophitization form to the graphite fiber, consequently the crystallite characteristics of T-14 were between those of T-0 and M40J, even after extended treating time. 3.4. Tensile strength study Table 4 shows the tensile strength of three samples measured by single fiber means and fiber bundle mean. Different strength had been obtained by the two testing means. Tensile strength of T-0 tested by single fiber means was lower than that presented by manufacturer and that tested by fiber bundle means, while the data gained by fiber S. Wang et al. / Ceramics International 32 (2006) 291–295 293 Table 2 Fiber surface chemistry of different samples Samples O/C (at.%) C 1s O 1s N 1s Si 2p T-4 0.114 86.0 9.8 3.3 0.8 T-14 0.013 98.0 1.3 0.4 0.3 Fig. 3. XPS spectra of C 1s and O 1s of sample T-4.
S. Wang et al. /Ceramics International 32(2006) 10000 2200 C 1s 8000 2100 6000 4000 2000 40538536534532530528526 Binding Energy(ev) Binding energy (ev) Fig. 4.XPS spectra of C ls and O Is of sample T-14 Tensile strength of samples by two testing ways a,(GPa) a/oo(%) a,(GPa) 3.25 94 3.49 10l.2 82.6 T14 3.36 ao was the tensile strength of T300 carbon fiber presented by manufacturer (3.45GPa) be attributed to part monofilament. Therefore, the tested strength by fiber bundle means was lower than actual datum The strength of T-0 tested by fiber bundle means was credible because the fiber had sufficient surface activity and 203040506070 could be well solidified by resin. The surface activity of T-4 without surface sizing and T-14 heat treated at 1400C both Fig. 5. XRD of samples was weakened, so the strength data gained by fiber bundle means was incredible. The tensile strength of samples by single fiber means could be thought credible. There were not bundle means matched with that presented by manufacturer. obvious changes in the tensile strength of T-0, T-4, and T-14. The letter presented by manufacturer was obtained by fiber It could be concluded that heat treatment at 1400C did not bundle means [15]. The single fiber testing means was affect the strength of carbon fiber because the influence of insensitive to external factors compared with fiber bundle heat treatment at 1400C on the crystallite structure was testing means because the fiber bundle testing means had a relationship with carbon fiber surface state. The carbon fiber bundle should be resin-impregnated and cured before testing. If carbon fiber had low surface activity, resin could 4. Conclusions not solidify fibers well and fibers would slip in resin under stress. As a result, monofilament could not rupture The characterization of heat-treated carbon fiber has simultaneously and the ultimate destructive load can but demonstrated that physical and chemical the characteristics of the carbon fiber have changed. heat treatment can improve the thermal stability of carbon fiber and decrease Table 3 the surface activity due to the decrease of the amount of Crystallite characteristic of samples oxygen and nitrogen atoms and an increasing carbon △1n() 2e() doo(A) L(nm) fraction. Heat treatment can also improve the graphitization 2504 degree of carbon fiber, by decreasing the interlayer spacing 2549 and largening of crystallite dimensions. Heat treatment at 1400C does not damage the fiber' single tensile strength
bundle means matched with that presented by manufacturer. The letter presented by manufacturer was obtained by fiber bundle means [15]. The single fiber testing means was insensitive to external factors compared with fiber bundle testing means because the fiber bundle testing means had a relationship with carbon fiber surface state. The carbon fiber bundle should be resin-impregnated and cured before testing. If carbon fiber had low surface activity, resin could not solidify fibers well and fibers would slip in resin under stress. As a result, monofilament could not rupture simultaneously and the ultimate destructive load can but be attributed to part monofilament. Therefore, the tested strength by fiber bundle means was lower than actual datum. The strength of T-0 tested by fiber bundle means was credible because the fiber had sufficient surface activity and could be well solidified by resin. The surface activity of T-4 without surface sizing and T-14 heat treated at 1400 8C both was weakened, so the strength data gained by fiber bundle means was incredible. The tensile strength of samples by single fiber means could be thought credible. There were not obvious changes in the tensile strength of T-0, T-4, and T-14. It could be concluded that heat treatment at 1400 8C did not affect the strength of carbon fiber because the influence of heat treatment at 1400 8C on the crystallite structure was limited. 4. Conclusions The characterization of heat-treated carbon fiber has demonstrated that physical and chemical the characteristics of the carbon fiber have changed. Heat treatment can improve the thermal stability of carbon fiber and decrease the surface activity due to the decrease of the amount of oxygen and nitrogen atoms and an increasing carbon fraction. Heat treatment can also improve the graphitization degree of carbon fiber, by decreasing the interlayer spacing and largening of crystallite dimensions. Heat treatment at 1400 8C does not damage the fiber’ single tensile strength. 294 S. Wang et al. / Ceramics International 32 (2006) 291–295 Table 4 Tensile strength of samples by two testing ways Samples By single fiber means By fiber bundle means s1 (GPa) s1/s0 * (%) s2 (GPa) s2/s0 * (%) T-0 3.25 94.2 3.49 101.2 T-4 3.20 92.8 2.85 82.6 T-14 3.36 97.4 1.98 57.4 s0 * was the tensile strength of T300 carbon fiber presented by manufacturer (3.45 GPa). Table 3 Crystallite characteristic of samples Samples Du1/2 (8) 2u (8) d002 (A˚ ´ ) Lc (nm) T-0 4.65 25.04 3.552 1.75 T-14 3.28 25.49 3.490 2.48 M40J 2.72 25.67 3.466 3.00 Fig. 5. XRD of samples. Fig. 4. XPS spectra of C 1s and O 1s of sample T-14
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