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First experimental evidence of alluaudite-like phosphates with high Li-content

¹ Laboratoire de Minéralogie, Université de Liège, 4000 Liège, Belgium
² Institut für Mineralogie und Kristallchemie, Universität Stuttgart, 70550 Stuttgart, Germany
³ Institut für Anorganische Chemie, Universität Stuttgart, 70550 Stuttgart, Germany
⁴ Institut Scientifique de Service Public, 4000 Liège, Belgium

e-mail: fhatert{at}ulg.ac.be

Members of the Na_1-xLi_xMnFe₂(PO₄)₃ series, with the alluaudite structure type, were synthesized by solid-state reaction in air. The crystal structure refinement of the NaMnFe₂(PO₄)₃ end-member (space group C2/c, Z = 4, a = 12.018(2), b = 12.565(3), c = 6.415(1) Å, ß = 114.33(3)°), a synthetic compound with a chemical composition corresponding to the idealized composition of the Buranga alluaudite, was carried out to R₁ = 0.026. The following cationic distribution was observed: Na⁺ + in A(1) and A(2)' ( denotes lattice vacancies), Mn²⁺ in M(1), Fe³⁺ + Fe²⁺ in M(2). The A(2)' site exhibits a distorted gable disphenoid morphology and is found at the (0, y, ) (y 0) position in channel 2 of the alluaudite structure. The crystal structure of Na_0.5Li_0.5MnFe₂(PO₄)₃ (space group C2/c, Z = 4, a = 11.988(2), b = 12.500(3), c = 6.392(1) Å, ß = 114.67(3)°), refined to R₁ = 0.034, leads to the cationic distribution: Li⁺ + Na⁺ + in A(2)', Na⁺ + in A(1), Mn²⁺ in M(1), Fe³⁺ + Fe²⁺ in M(2). Thus, the substitution mechanism involved in the replacement of Na by Li in the Na_1-xLi_xMnFe₂(PO₄)₃ alluaudite-like compounds corresponds to + Na Li + , with x ranging from 0.00 to 0.90.

Key-words: Na_1-xLi_xMnFe₂(PO₄)₃, alluaudite structure type, solid-state reaction synthesis, crystal structure refinement, lithium crystal chemistry.

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