LiCoPO
4 (LCP) exists in three different structural modifications: LCP-
Pnma (olivine structure), LCP-
Pn2
1a (KNiPO
4 structure type), and LCP-
Cmcm (Na
2CrO
4 structure type). The synthesis of the LCP-C
mcm polymorph has been reported via high
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LiCoPO
4 (LCP) exists in three different structural modifications: LCP-
Pnma (olivine structure), LCP-
Pn2
1a (KNiPO
4 structure type), and LCP-
Cmcm (Na
2CrO
4 structure type). The synthesis of the LCP-C
mcm polymorph has been reported via high pressure/temperature solid-state methods and by microwave-assisted solvothermal synthesis. Phase transitions from both LCP-
Pn2
1a and LCP-C
mcm to LCP-
Pnma upon heating indicates a metastable behavior. However, a precise study of the structural changes during the heating process and the magnetic properties of LCP-C
mcm are hitherto unknown. Herein, we present the synthesis and characterization of LCP-
Cmcm via a rapid and facile soft-chemistry approach using two different kinetically controlled pathways, solvothermal and polyol syntheses, both of which only require relatively low temperatures (~200 °C). Additionally, by polyol, method a dumbbell-like morphology is obtained without the use of any additional surfactant or template. A temperature-dependent in situ powder XRD shows a transition from LCP-C
mcm at room temperature to LCP-
Pnma and finally to LCP-
Pn21a at 575 and 725 °C, respectively. In addition to that, the determination of the magnetic susceptibility as a function of temperature indicates a long-range antiferromagnetic order below
TN = 11 K at 10 kOe and 9.1 K at 25 kOe. The magnetization curves suggests the presence of a metamagnetic transition.
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