Journal of Electron Microscopy Advance Access originally published online on February 13, 2009
Journal of Electron Microscopy 2009 58(2):29-34; doi:10.1093/jmicro/dfp009
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Beam damage suppression of low-
porous Si–O–C films by cryo-electron-energy loss spectroscopy (EELS)
1 Toray Research Center, Inc., Sonoyama 3-3-7, Otsu-shi, Shiga 520-8567
2 Department of Materials Science and Engineering, Kyoto University, Yoshida, Sakyo, Kyoto 606-8501, Japan
* To whom correspondence should be addressed. E-mail: yuji_otsuka{at}trc.toray.co.jp
Porous Si–O–C films with lower dielectric constant (
) relative to silicon dioxide have been widely studied as inter-layer dielectrics in new-generation microelectronic devices. On the analysis of the film by transmission electron microscopy (TEM), it is susceptible of beam damage during both sample preparation by a focused ion beam (FIB) technique and TEM observation. We use electron energy loss spectroscopy (EELS) to quantify the magnitude of the beam damage during these processes. The intensity of the 285-eV peak in C-K electron energy loss near edge structures (ELNES) is enhanced by the damage, which can be ascribed to the formation of the C=C double bonds as a result of the decomposition of the methyl groups by the beam. The use of cryo-holder for TEM at 100 K is found to be essential to reduce the damage of the low-
layers. The lowering of the acceleration voltage of FIB down to 5 keV does not change the spectra. Since the FIB damage is localized at the surface, the use of thick regions in the TEM foil such as 130 nm is preferred to reduce the superposition of EELS of the damaged region on those from the sample of interest.
Keywords cryo-EELS, low-
film, VLSI, ELNES, FIB, irradiation damage
Received 27 December 2008, accepted 24 January 2009