I have silicate mesoporous structure which is doped with boron and other elements. I have tried doing SEM/ EDAX but not that sensitive. Could anyone suggest a better technique? I am also thinking of performing Raman.
Electron energy loss spectroscopy (EELS) on the TEM will enable you to detect boron in the silica network. The technique will be sensitive to fairly low levels of boron. Also, if the signal is good enough, it is possible to determine if the boron is 4- or 3- coordinated as there is a distinctive change in the near edge structure. (see P.A. Bingham, et al. 2008. Boron environments and irradiation stability of iron borophosphate glasses analysed by EELS, Solid State Sciences, 10, 1194-1199.)
you can also think of X-ray photoelectron spectroscopy (XPS) to probe the amount of boron. This technique also benefits from the possibility that the observed binding energy can be related to the chemical bonding of the boron atoms (so-called chemical shifts), see, e.g., Figure 3 in
http://pubs.acs.org/doi/abs/10.1021/la400148h
In case that your department/university is not equipped with
an XPS setup, next location is Manchester (as far as I know).