For the
synthesis of LMS, MnSO4 anhydrous and Li2SO4 (5% excess) were used as precursors. Anhydrous MnSO4 and Li2SO4 were prepared by heating MnSO4·H2O and Li2SO4·H2O (Sigma-Aldrich) in a tube furnace under an argon gas flow
for approximately 1 h. MnSO4·H2O was treated
at 300 °C and Li2SO4·H2O at 200 °C. The anhydrous powders were then mixed in a ratio
of 1.3:1 by weight, respectively, and ball-milled in a SPEX 8000M
high-energy ball mill for 30 min in a stainless steel vial. The resulting
powder was pressed into a pellet of 20 mm diameter using a pelletizer
at a pressure of 8 MPa. The pellet was then annealed in a box furnace
for 12 h at 500 °C with a temperature ramp of 5 °C min–1. After annealing, the pellet was ground, pelletized,
and annealed under the same conditions. Finally, the pellet was ground
to a fine powder before carrying out the structural analysis. The
powder was stored in an Ar-filled glovebox to prevent moisture absorption
as the material is sensitive to degradation by moisture.
synthesis of LMS, MnSO4 anhydrous and Li2SO4 (5% excess) were used as precursors. Anhydrous MnSO4 and Li2SO4 were prepared by heating MnSO4·H2O and Li2SO4·H2O (Sigma-Aldrich) in a tube furnace under an argon gas flow
for approximately 1 h. MnSO4·H2O was treated
at 300 °C and Li2SO4·H2O at 200 °C. The anhydrous powders were then mixed in a ratio
of 1.3:1 by weight, respectively, and ball-milled in a SPEX 8000M
high-energy ball mill for 30 min in a stainless steel vial. The resulting
powder was pressed into a pellet of 20 mm diameter using a pelletizer
at a pressure of 8 MPa. The pellet was then annealed in a box furnace
for 12 h at 500 °C with a temperature ramp of 5 °C min–1. After annealing, the pellet was ground, pelletized,
and annealed under the same conditions. Finally, the pellet was ground
to a fine powder before carrying out the structural analysis. The
powder was stored in an Ar-filled glovebox to prevent moisture absorption
as the material is sensitive to degradation by moisture.