Combustion Synthesis of Nanoparticulate LiMgxMn1-xPO4 (x=0, 0.1, 0.2) Carbon Composites Page: 4 of 31
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Such methods have been widely used to prepare nanoparticulate metal oxides,13 and
recently considered for preparation of LiFePO4.14 We present our preliminary results
as well as suggestions for further improvements.
LiMnPO4/C composites were prepared by combustion synthesis using citric acid
(ACS, 99.5+%, Alfa Aesar) or glycine (Aldrich), LiNO3 (lithium nitrate,
Mallinckrodt) Mn(NO3)2, 45-50 wt. % in dilute nitric acid (manganese nitrate
solution, Aldrich) and NH4H2PO4 (ammonium phosphate monobasic, Aldrich)
precursors. Several different fuel/nitrate ratios were used, ranging from 0.4-1.0. For
Mg-substituted materials, either a 9:1 or 8:2 molar mixture of Mn(NO3)2 and
Mg(NO3)2 6H20 (Aldrich) were used depending upon the desired stoichiometry.
Approximately 1M solutions of the nitrate and phosphate precursors were prepared
by dissolving them in water, and the desired amount of citric acid was then added.
This solution was then poured or sprayed into a stainless steel beaker used as a
reaction container, which was pre-heated on a hot plate. After evaporation of the
water, the solution became viscous and started to foam. Subsequent auto-ignition of
the precursors was accompanied by the evolution of a large volume of gaseous by-
products. The self-propagating combustion was completed in a few minutes. The
black powder obtained after combustion was collected, wet ball-milled with acetone
for one hour, and heat-treated at 500- 700 C under a nitrogen atmosphere for varying
lengths of time up to 5 hours. (Most materials were treated at 600 C for three hours.)
Some samples were then treated hydrothermally in a 125 mL Parr Teflon-lined
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Doeff, Marca M; Chen, Jiajun; Conry, Thomas E.; Wang, Ruigang; Wilcox, James & Aumentado, Albert. Combustion Synthesis of Nanoparticulate LiMgxMn1-xPO4 (x=0, 0.1, 0.2) Carbon Composites, article, December 14, 2009; Berkeley, California. (digital.library.unt.edu/ark:/67531/metadc1012800/m1/4/: accessed February 17, 2019), University of North Texas Libraries, Digital Library, digital.library.unt.edu; crediting UNT Libraries Government Documents Department.