Canada - Memorial University of Newfoundland

pattern is listed in Table A.LI3. Even though SNHPwas still present in the sample, the
JCPDS database identified different impurities than those in the product from the lower
temperature run. Sodium phosphate and sodium phosphate hydrates accounted for most
ofthe impurities present in the sample, but there were still peaks that could not be
assigned. The SEM images ofboth runs arc given in Figures 3.12a and b, respectively.
From SEM, it can be seen the crystals are large enough to perform single crystal XRD
analysis if they can be separated from the impurities. Again, as was the case with the
NiO reactions, the crystals were bundled together. The well-defined crystals are smaller
(5-15 pm) in size, too small for single crystal XRD. The elemental analysis canfinned
the presence ofsodium, nickel, and phosphorus in the reaction product.
In conclusion, using l·nNiNTA"] as a nickel source did not give a pure sample of
SNHP or large enough crystals to do a single crystal XRD analysis, as originally hoped.
Time constraints prevented further investigation into this area. However, a new synthesis
for SNHP has been developed. The use of NaNiNTA as a starting material could be
another possible route to synthesizing SNHP for any future work in this area.
88