PII: SOOll-2275(96)OOlOS-7

Cryogenics 37 (1997) 135-138 0 1997 Elsevier Science Limited Printed in Great Britain. All rights reserved 001 l-2275/97/$17.00

Mechanical properties of carbon fiber reinforced plastics and their response to a radiation environment
S.M. SpieRberger, and Y. lwasakit K. Humer, E.K. Tschegg*, H.W. Weber, K. Nomat

Atominstitut der ijsterreichischen Universitsten, A-1020 Wien, Austria Institut f. Angewandte u. Technische Physik, TU, A-1040 Wien, Austria tshikibo Ltd, Osaka 541, Japan Received 31 July 1996 TORAYCA T300 3K is a two and a half dimensional woven carbon fiber reinforced epoxy which was developed for various applications including cryogenics. Scaling experiments in tension, in the shear-mode (mode II) and in the crack-opening-mode (mode I) were made at room and low temperature, in order to establish suitable sample geometries for irradiation experiments. Moreover, the interlaminar and the intralaminar shear strength as well as the ultimate tensile strength were investigated after irradiation at 340 K with a reactor spectrum up to a fast neutron fluence of 5 x IO** m-* (E>O.l MeV). The irradiated material was measured at 77 K and acoustic emission (AE) investigations were made for the tensile and the mode II samples. 0 1997 Elsevier Science Limited Keywords: intralaminar shear plastics; acoustic emission strength; radiation effects; carbon fibre reinforced

Carbon fiber reinforced plastics (CFRPs) offer applications especially to cryogenic technology such as superconductivity, aeronautics, and wherever low electrical and thermal conductivity, sufficient radiation resistance and a high stiffness need to be correlated with light weight, good fatigue behavior and a low axial negative coefficient of thermal expansion. Carbon/epoxy composites were tested previously by Egusa et al.* who investigated the influence of 6oCo yrays and 2 MeV electrons on the ultimate flexural strength and the shear modulus at room temperature and 77 K. It was found that the ultimate strength shows no decrease at a dose of 20 MGy at 293 K and falls to about 90% at 77 K, and that both properties had a much better resistance at 140 MGy when tested at room temperature3. A comparison of the fiber matrix interface between carbon and glass fiber reinforced plastics (GFRPs)~ indicates that the friction force (mechanical bond) mode in CFRPs may dominate, whereas the chemical bond mode does not make any contribution to the total bond mode, in contrast to the glass fibers. The ultimate shear strength of carbon composites shows a better radiation resistance at 140 MGy than that of GFRPs at both test temperatures. Sasuga et ~1.~investigated the interlaminar shear (ILSS) and flexural strength of PEEK/CF composites after electron beam irradiation. At 293 K, both keep their properties unchanged up to a dose of 180 MGy. At 77 K, the flexural

strength decreases slightly with some scatter at higher doses. In addition, Garg6 investigated graphite/epoxy laminates in mode I and the inter- and intralaminar fracture in mode II. Furthermore, Ahlbom et aL7 tested unidirectional and cross-ply lay-ups of CFR-thermoplastics by tensile and short beam shear tests. Hartwig et cd.* and Schwartz et ~1.~ dealt with the thermal expansion of CFRPs.

Experimental
Firstly, scaling experiments on small geometries were made, which are necessary because of the restricted spatial situation in present radiation facilities. The specimens were cut from plates with three different thicknesses, all with a warp to weft ratio of about 9:l. The samples for the ultimate tensile tests (scaled down from the DIN 53455 standardlO) had thicknesses of 1.2, 1.6 and 2 mm. Furthermore, three different widths (3, 6 and 8 mm) were chosen. The 2 mm specimens with a tensile width of 3 mm were also exposed to three fluences; samples of all thicknesses were exposed to a fluence of 10z2 m-. Mode I samples with a thickness of 2 mm and ligament lengths of 14, 17 and 20 mm were measured (the geometry is shown in reference 11). The unirradiated samples were tested at 293 and 77 K. The mode II samples were investigated with thicknesses

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Results and discussion

Acoustic emission Together with the tensile and the mode II measurements, acoustic emission investigations were made for the unirradiated material and for each of the three fluences. This kind of investigation enables the detection of beginning material damage before it becomes macroscopically evident. Every single crack releases a mechanical tension wave, which is reflected at the sample surface and can therefore be detected by a piezoelectric sensor*. Figure 2 represents the recorded AE count rates (AE events per second) and the total number of AE events versus displacement on the one hand and the distribution of the AE peak amplitude (PA) on the other hand. Events in the low dB range are caused by matrix cracking, followed by damage of the fiber-matrix interface and fiber pull out, and finally by fiber cracking in the high dB range. The curves show the AE activity of the unirradiated specimens in comparison with those irradiated to 5 x lo** m-*. Concerning the tensile investigations (Figures 2a, b), the maximum of the total amount of the AE events is 5.59 times higher in the irradiated specimen than in the unirradiated state, the maximum number of PA is 5.36 times higher. In the irradiated mode II samples (Figures 2c, d), the maximum number of PA as well as the maximum of the total amount of events is 1.25 times higher. Scaling results

x ona
Figure 1 Schematic load-displacement curve in the intralaminar shear mode. G$ is the specific fracture energy, C& is the specific crack initiation energy

of 1.6 and 2 mm and shear heights of 4,6 and 8 mm (details of their geometry and a description of the fracture energy concept can be found in reference 12). 2 mm thick specimens with a shear height of 6 mm were irradiated with three fluences, samples of both thicknesses were only exposed to a fluence of lo** m-*. Important material parameters in the intralaminar shear mode are the specific crack initiation energy GL and the specific fracture energy GF , which can be obtained as described in Figure 1. For the specific crack initiation energy Gh, the tangent to the initial linear elastic slope of the curve is tilted by lo%, which results in a certain point of intersection on the load-displacement curve. A line through this point, which is parallel to the original tangent, defines the shaded area in Figure 1. If this area is divided by the shear area, GL is obtained. This method was used by Schwalbe13, who applied it to metals with similar loaddisplacement behavior, but tilted the tangent only by 5%. For reinforced plastics, the empirical tilting percentage of 10% proved to be useful throughout many investigations. The other parameter, namely the specific fracture energy QFr is represented by the area under the recorded loaddisplacement curve divided by the shear area. This requires a load-displacement curve, which decreases to zero at high displacements, a behavior that was not observed in the present investigations. The short beam shear (ASTM D2344 standard), the tensile and the mode II samples were exposed to irradiation in the TRIGA reactor Vienna at 340 K to neutron fluences of 102, lo** and 5 x lo** mm2 (E>O.lMeV). The total absorbed doses amount to the values listed in Table 1 according to calculations discussed in reference 14. All irradiated samples were measured at 77 K. The crosshead speed of the testing machine was kept constant at 1.3 mm min- during the short beam shear test and at 0.5 mm min- throughout the other experiments. The applied load and the crosshead displacement were recorded.
Table 1

Scaling experiments in mode I show decreasing crack initiation energy with increasing ligament length. At room temperature, where the values are about 10% higher, most of the specimens do not split at all, but show elastic behavior. This can also be observed at 77 K, where all specimens split along one horizontal direction between two fiber bundles. The elastic effect becomes smaller with decreasing starter notch length at both temperatures. Concerning the variation of the shear height and the material thickness in mode II, no influence is found neither in the unirradiated state nor after irradiation, where specimens with 1.6 and 2 mm thickness were exposed to a dose of 4.64 x lo7 Gy. Both findings are related to the inhomogeneous structure of the reinforcement (rough distribution

ld

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(a) 0.5 1.0 displacement

.*
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L1
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m
-. 40 50 60 70 80 90 (b) peak amplitude (dB) 40 (d) 50 60 70 80 90 100 peak amplitude (dB)

4000 3000 2000

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100 O

I@0 1 2 3 (mm) 4 (c) displacement

Total absorbed dose for three neutron fluences

IO 4.64 x IO6 10*2 4.64 x lo7 5 x 1022 2.32 x lo8

Neutron fluence (m-?, E>O.lMeV Total absorbed energy (Gy)

Figure2 AE activity of the tensile (top) and of the mode II samples (bottom). In (a) and (c), the AE events and the total AE events (monotonously ascending lines) are plotted versus displacement; (b) and (d) show the distribution of the peak amplitude. The solid (dotted) line refers to measurements on the irradiated (unirradiated) specimen

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of fibre bundles) and the fact that the scaling parameters cover only a range of a few millimeters. The temperature dependence shows that the specific crack initiation energy Cr (30 N/mm) is three times higher at 77 K than at room temperature (Figure AZ). The material thickness has also no systematic influence on the ultimate tensile strength (UTS), neither in the unirradiated state nor after exposure to a fluence of 1O22 mm2, whereas the UTS increases linearly with the tensile width, by ~200 MPa from 3 to 8 mm. The room temperature strength lies about 10% below the value at low temperature (Figure 3b). In summary, the scaling experiments on the tensile and the mode II samples of Torayca T300 3K demonstrate, that the test geometries, which had been developed for several glass fiber reinforced plasticsz2, are not as successful as in the latter case. However, it should be pointed out, that this might be due to the inhomogeneous structure of the investigated composites and the corresponding large standard deviations of the experimentally obtained material parameters. Irradiation Regarding effects irradiation effects in the intralaminar shear mode

Figure4 Normalized specific fracture energy (a), ultimate tensile strength (b) and interlaminar shear strength (c) as a function of total absorbed dose. The data are normalized to those orior to irradiation, i.e. 30 Nmm-, 106 MPa and 466 MPa for &,, lLSSO and UTS,,, respectively for a thickness of 2 mm. Triangle symbols refer to a thickness of 1.6 mm (UT!%, = 734 MPa, GFO= 34 Nmm-), square symbols to 1.2 mm (UTS,, = 576 MPa)

(Figure 4a), the values of Gb fall to only 90% at the first

fluence, to 70% at the second and finally to 30%. For the majority of the specimens, it was not possible to reach complete material separation during the shear test. Especially at higher dose levels, the load does not fall to zero, which would be necessary to calculate the specific fracture energy, GE! as mentioned above. Under irradiation (Figure 4b), the ultimate tensile strength keeps its value until the first fluence and then falls to 60-70% at higher dose levels. The interlaminar shear strength (ILSS) which is only defined for a pure 2 dimensional laminate has to be con40 35 30 t $ #

125-1

2mm

10

(a) *l=ight(-) l n . 0 0 0 1.2mm 1.6mm 2mm 1.2mm 1.6mm 2mm

sidered as a qualitative indication for the influence of the third reinforcement direction in this material. The specimens show no bending, they simply break upon loading at lower dose levels. The ILSS of 110 MPa keeps its value up to the first fluence and decreases to 80% at the second and to 30% at the highest dose as shown in Figure 4c. In order to obtain a more complete description of the mechanical properties, further investigations especially with regard to other irradiation conditions (e.g. irradiation at 5 K) are necessary. This is taken into account in our current program, where tensile and short beam shear samples are irradiated in the FRM Garching, Munich, at 5 K and measured with and without a warm-up cycle to room temperture. A comparison of the mechanical properties of the CFRP and GFRPs at 77 K shows the following trends. The ultimate tensile strength of unirradiated glass fiber reinforced resins lies between 400 and 1000 MPa at 77 K14 and deteriorates at a fluence of 5 x 1O22 mW2(E>O.l MeV) to between 60 and 80%, Toraycas UTS (with a thickness of 2 mm) is around 500 MPa and falls to 70%. The interlaminar shear strength of GFRPs is between 65 and 107 MPai6, the CFRP shows 110 MPa, and both groups of composites fall to 20-30% at the highest dose. The specific crack initiation energy of unirradiated GFRPs is between 40 and 50 Nmm- and lower (30 Nmm-) in the CFRP. Under irradiation, the decrease is in general 25-40%, the CFRP is found in the lower range.

Conclusions
The two and a half dimensional carbon fiber reinforced epoxy Torayca T300 3K was investigated by scaling experiments in the crack opening mode (mode I), in the intralaminar shear mode (mode II) and under tensile load at 293 and 77 K. The material was exposed to three fluences of neutron- and gamma-radiation and tested in these modes as well as in the interlaminar shear mode at 77 K. The main results are the following: 1. The material shows no systematic change in its intralaminar shear properties, neither by varying the thick-

200'

, 2

I 8 10

(b)4tii*ewidZ(mm)

Figure3 Scaling experiments in the intralaminar shear mode and in the tensile test. (a) Shows the specific crack initiation energy G; as a function of the shear height and the thickness of the material. (b) Represents the ultimate tensile strength as a function of the tensile width and the thickness of the material. The open symbols are values measured at room temperature, the filled symbols at 77 K

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nesses nor the shear heights. This is probably a consequence of the inhomogeneous structure of the reinforcement (fiber bundles). The crack initiation energy at low temperature is about three times higher than at 293 K. In the tensile tests, the thickness has no influence as well, but with increasing width a linear increase by 2030% takes place. Room temperature conditions show an ultimate tensile strength that is on average 10% smaller. Mode I tests, especially at room temperature, show an elastic behavior of the material and a splitting of the specimen in the horizontal (ill defined) direction. Therefore, the specific crack initiation energy has to be considered to be a qualitative parameter. The short beam shear test that can be correctly applied according to the ASTM D2344 standard only for 2 dimensional laminates, indicates good radiation resistance at the second dose, i.e. the ILSS falls to only 80%, but at the highest dose it decreases to 30%. The ultimate tensile strength also shows good radiation resistance and decreases to 70% at 2.32 x lo8 Gy. Radiation has the worst effect on the specific crack initiation energy under shear as it drops to 25% of its unit-radiated value. Acoustic emission investigations recorded together with the tensile and the mode II measurements show more activity of all parameters (AE count rate, total number of AE events and distribution of peak amplitude) in the irradiated state, especially in the tensile mode.

References
1 Egusa, S., Kirk, M.A., Birtcher, R.C. and Hagiwara, M. Neutron and y-ray irradiation effects in composite organic insulators, J. Nucl. Mar. (1985) 133-134 795-799 Egusa, S. and Hagiwara, M. Mechanical Properties of polymer matrix composites at 77 K and room temperature after irradiation with @%Zo y-rays, Cryogenics (1986) 26 417-422 Egusa, S. Mechanism of radiation-induced degradation in mechanical properties of polymer matrix composites, J. Mat. Sci. (1988) 23 2753-2760 Egusa, S. Anisotropy of radiation-induced degradation in mechanical properties of fabric-reinforced polymer-matrix composites, J. Mar. Sci. (1990) 25 1863-1871 Sasuga, T., Seguchi, T., Sakai, H., Nakakura, T. and Masutani, M. Electron beam irradiation effects on mechanical properties of PEEK/CF composite, J. Mat. Sci. ( 1989) 24 1570-1574 Garg, A.C. Intralaminar and interlaminar fracture in graphite/epoxy laminates, Engineering Fracture Mechanics (1986) 23 7 19-733 Ahlborn, K. Cryogenic mechanical response of carbon fiber reinforced plastics with thermoplastic matrices to quasi-static loads, Cryogenics (1991) 31 252-256 Hartwig, G. and Knaak, S. Fiber-epoxy composites at low temperatures, Cryogenics ( 1984) 639-647 Schwartz, G. and Hartwig, G. Thermal expansion of polymers and fiber composites at low temperatures, Adv. Cryog. Eng. (1990) 36 1007-1010 Tschegg, E.K., Humer, K. and Weber, H.W. Influence of test geometry on tensile strength in fibre reinforced plastics at cryogenic temperatures, Cryogenics (1991) 31 3 12-3 18 Tschegg, E.K., Humer, K. and Weber, H.W. Fracture tests in Mode I on tibre reinforced plastics, J. Mar. Sci. ( 1993) 28 2471-2480 Tschegg, E.K., Humer, K. and Weber, H.W. Mode II fracture tests on fibre-reinforced plastics, J. Mar. Sci. (1995) 30 1251- 1258 Schwalbe, K.-H. Bruchmechanik metallischer Werkstoffe, Carl Hanser Vet-lag, Mtlnchen Wien (1980) Humer, K., Weber, H.W. and Tschegg, E.K. Radiation effects on insulators for superconducting fusion magnets, Cryogenics (1995) 35 871-882 Walters, J. Anwendung der Schallemissionstechnik zum Beschreiben von Schadensmechanismen in partikelgeftillten Thermoplasten, VDI Berichte ( 1989) 5 163 SpieRberger, S.M., Humer, K. Tschegg, E.K., Weber, H.W. and Gerstenberg, H. Interlaminar shear and flexural strength of fiber reinforced plastics at 77 K after room and low temperature reactor irradiation, Adv. Cryog. Eng. (1997) 42 105-l 12

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Acknowledgements
Technical help by Mr is acknowledged. This Federal Ministry of Vienna, under contract E. Tischler and Mr H. Niedermaier work was supported in part by the Science, Transport and the Arts, No. 77.859/2-R/5/95.

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