A nanohybrid C-LiMnPO
4 is important to tailor its electrochemical properties useful for Li
+-ion batteries and photo-catalysis. In this article, we report a simple in situ C-LiMnPO
4 synthesis, wherein the LiMnPO
4 grows from a supersaturated solution LiOH·H
2O, MnSO
4·H
2O, and H
3PO
4 in water at 200 °C in an autoclave in a hydrothermal reaction and bonds in situ to nascent carbon of a surface layer on a surface reaction with a long chain hydrocarbon used during the reaction. A phase pure C-LiMnPO
4 is formed in a shape of nanorods (Pnma orthorhombic crystal structure), with 100–150 nm diameters, 150–800 nm lengths, and 2–3 nm thickness of a co-bonded C-sp
2 surface layer. The LiMnPO
4 rigidly co-bonds to C-sp
2 via O
2? in the PO
4 3? polygons in a joint surface layer that a single molecular bonding extends well up to 600 °C, with a due mass loss on an extended heating in air. The sample contains fine pores with an average 3.0 nm diameter and a 9.0 m
2/g surface area. At room temperature, it develops a huge dielectric permittivity
ε r~1.9 × 10
5 near 1 Hz frequencies, which on raising the frequency decays progressively to a fairly steady
ε r~1.5 × 10
3 at ≥1 kHz. Bare LiMnPO
4 is a low dielectric phase,
ε r < 10. A non-Debye type of dielectric relaxation is shown in the modulus plots. As frequency approaches to 10
5 Hz, nearly three orders of larger ac conductivity, 2.5 × 10
?5 Scm
?1 at 10
6 Hz, develop over a carbon-free LiMnPO
4 value useful for the applications.
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