The novel carbonate sorbents of Mg–Al–CO3 and (Mg3−x, Cux)–Al–CO3, were synthesized by co-precipitation method with individual nitrate salt of metal ions under alkaline conditions. The synthetic sorbent was characterized by analysis techniques such as BET surface area analysis, X-ray diffraction (XRD), and scanning electron microscopy (SEM). Elemental mercury capture experiments were carried out in a fixed-bed reactor including Hg permeation source, furnace, and Hg analyzer, which was conducted at temperature ranging from 30 to 300 o C. Mercury removal tests demonstrated that the breakthrough time increased with temperature by adding transition metals to Mg–Al–CO3 as (Mg3−x, Cux)–Al–CO3. Hg uptake by the (Mg3−x, Cux)–Al–CO3 sorbent rapidly increased with elevated temperature up to 200 o C and reached the maximum capacity of 12.93 µg/g, and then gradually decreased after 300 o C. Surface area and unique properties of transition metals are the reason toward improving Hg capture sorbent. These results represent the feasibility of using such Hg sorbents for elemental mercury removal under elevated temperature conditions, and the detail mechanism is needed to be further studied.