Mechano‐Hydrothermal Synthesis of Tetraborate Pillared Li–Al Layered Double Hydroxides

Tetraborate pillared Li–Al layered double hydroxide was synthesized for the first time by a mechano‐hydrothermal process in which gibbsite (Al( OH ) 3 ) sample was first activated by a ball milling, followed by hydrothermal treatment with Li 2 B 4 O 7 in water at 95°C. Activation of gibbsite Al( OH ) 3 induced by mechanochemical process was essential for the formation of thin disk‐like Li–Al LDH intercalated with borate anion. When in excess the activated Al( OH ) 3 was transformed into bayerite phase during the hydrothermal process.