I'm trying to synthesize Li2FeSiO4 using sol-gel method. The substrates are lithium acetate, iron nitrate, TEOS and citric acid. Lithium acetate and iron nitrate are mixed in water solution with citric acid, while the TEOS is added dropwise from ethanol solution. In the resulting gel, after drying, I can observe peaks from LiNO3 phase in the XRD. After calcination of gel, I obtain the lithium-depleted phase of Fe2SiO4, which I suspect is due to the presence of crystalline LiNO3 in gel.
Shouldn't the gel be amorphous after drying? I guess that LiNO3 comes from reaction of lithium acetate with iron nitrate - is it correct? How can I prevent the formation of crystalline LiNO3 in gel?
Thank you in advance.
As a result of the reaction in water of lithium acetate with iron nitrate, a precipitate of iron acetate is obtained. Crystalline lithium nitrate remains in the gel after drying. After calcination, lithium nitrate decomposes and goes into the atmosphere. The boiling point of lithium metal is 1340 ° C. It may be less in your mixture.
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