I use Ca(NO3)2.4H2O and P2O5 as precursors and Sol-gel method to synthesis my powder but the CA/P ratio is more than stochiometric (167) and my powder is dark. Does anyone know why this happens?
You have to be very cautious with the sol-gel conditions. Especially regarding the N2 atmosfera under the synthesis surely has to be made. I find curious that you chose a nitrate as a precursor of calcium and probably the oxidant anion nitrate could be responsible of the observed derives, you´d better chose other soluble salt for calcium other than a nitrate. The stoichiometric deviation probablý could be attributed to that salt again since I have a reasonable doubt concerning the hidration rate, that .4H2O does not seem to be that credible as seen in another nitrate salts (I found this problem critic using zirconyl nitrates). So, probably you have to rethink the precursors and condition for your experiment and that will lead you to success. Have luck with all that good chemistry of yours. Greets from Mendoza, Argentina. Gustavo.