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The key factors governing the single-phase or multi-phase structural changebehaviors during the intercalation/deintercalation of guest ions have not beenwell studied and understood yet. Through systematic studies of orthorhombicFe2(MoO4)3 electrode, two distinct guest ion occupation paths, namely discreteone for Li and pseudo-continuous one for Na, as well as their relationship withsingle-phase and two-phase modes for Na1 and Li1, respectively during theintercalation/deintercalation process have been demonstrated. For the firsttime, the direct atomic-scale observation of biphasic domains (discreteoccupation) in partially lithiated Fe2(MoO4)3 and the one by one Na occupation(pseudo-continuous occupation) at 8d sites in partially sodiated Fe2(MoO4)3 areobtained during the discharge processes of Li/Fe2(MoO4)3 and Na/Fe2(MoO4)3cells respectively. Our combined experimental and theoretical studies bring thenew insights for the research and development of intercalation compounds aselectrode materials for secondary batteries.

Discrete Li-occupation versus pseudo-continuous Na-occupation and their relationship with structural change behaviors in Fe2(MoO4)3