Jj. Bruckner et al., Cryogenic stabilization of high vapor pressure samples for surface analysis under ultrahigh vacuum conditions, J VAC SCI A, 17(5), 1999, pp. 2668-2675
A novel form of ultrahigh vacuum (UHV) cryogenic stabilization has been use
d to obtain high-resolution x-ray photoelectron - spectroscopy (XPS) data f
rom a complex amine, 1,8-bis(dimethylamino) naphthalene, whose solid phase
exhibited at room temperature an unacceptably high rate of sublimation. Pro
tonated versions of the amine exhibit hydrogen bonding. Electron spectrosco
py for chemical analysis chemical shifts can be used to describe the streng
th and asymmetry of hydrogen bonding formed in proton sponge complexes. Ana
lyzing the binding energy shifts of N (1s) induced by the presence of this
hydrogen bonding required obtaining corresponding XPS spectra from the nonp
rotonated (reference) sample, but the reference sample sublimes under even
moderate vacuum conditions. The combined results suggest that other high va
por pressure materials, particularly those that were previously considered
to be too corrosive for routine analysis, can be cryogenically stabilized f
or surface analysis under similar UHV conditions. (C) 1999 American Vacuum
Society. [S0734-2101(99)09605-0].