Mesoporous lithium metal phosphates are an important class of materials for the development of lithium ion batteries. However, there is a limited success in producing mesoporous lithium metal phosphates in the literature. Here, a lyotropic liquid crystalline (LLC) templating method was employed to synthesize the first examples of LiMPO4 (LMP) of Mn(II), Co(II), and Ni(II). A homogeneous aqueous solution of lithium and transition metal nitrate salts, phosphoric acid (PA), and surfactant (P123) can be spin coated or drop‐cast coated over glass slides to form the LLC mesophases which can be calcined into mesoporous amorphous LMPs (MA‐LMPs). The metal salts of Mn(II), Co(II) and Ni(II) produce MA‐LMPs that crystallize into olivine structures by heat treatment of the LLC mesophase. The Fe(II) compound undergoes air oxidation. Therefore, both Fe(II) and Fe(III) precursors produce a crystalline Li3Fe2(PO4)3 phase at over 400 °C. The MA‐LMPs show no reactivity towards lithium, however the crystalline iron compound exhibits electrochemical reactivity with lithium and a good electrochemical energy storage ability using a lithium‐ion battery test.
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