Structural and chemical bonding changes in nuclear graphite have been investigated during in-situ electron irradiation in a transmission electron microscope (TEM); electron beam irradiation has been employed as a surrogate for neutron irradiation of nuclear grade graphite in nuclear reactors. This paper aims to set out a methodology for analysing the microstructure of electron-irradiated graphite which can then be extended to the analysis of neutron-irradiated graphites. The damage produced by exposure to 200 keV electrons was examined up to a total dose of approximately 0.5 dpa (equivalent to an electron fluence of 5.6x 10 21 electrons cm -2 ). During electron exposure, high resolution TEM images and electron energy loss spectra (EELS) were acquired periodically in order to record changes in structural (dis)order and chemical bonding, by quantitatively analysing the variation in phase contrast images and EEL spectra.

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a b s t r a c tThe neutron irradiation-induced structural changes in nuclear grade graphites PCEA and PCIB were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED) and electron energy loss spectroscopy (EELS). The graphite samples were irradiated at the Advanced Test Reactor at the Idaho National Laboratory. Received doses ranged from 1.5 to 6.8 displacements per atom and irradiation temperatures varied between 350 C and 670 C.XRD and Raman measurements provided evidence for irradiation induced crystallite fragmentation, with crystallite sizes reduced by 39e55%. Analysis of TEM images was used to quantify fringe length, tortuosity, and relative misorientation of planes, and indicated that neutron irradiation induced basal plane fragmentation and curvature. EELS was used to quantify the proportion of sp 2 bonding and specimen density; a slight reduction in planar-sp 2 content (due to the buckling basal planes and the introduction of non-six-membered rings) agreed with the observations from TEM.

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