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This paper reports a template-free method to synthesize a series of inorganic hollow spheres (IHSs) including Cu-1,Cu-2,Ni-1,Ni-2 based on mineralization reactions at water/water-brother interfaces.Water-brother was defined as a solvent which is miscible with water,such as ethanol and acetone.The water/water-brother interfaces are very different from water/oil interfaces.The water-brother solvent will usually form a homogenous phase with water.Interestingly,in our method,these interfaces can be formed,observed and utilized to synthesize hollow spheres.Utilizing the unique porous properties of the spheres,their potential application in water treatment was demonstrated by using Cu-1 IHSs as Fenton-like reagents for adsorption and decomposition of Congo Red from aqueous solution.The final adsorption equilibrium was achieved after 30 min with the maximum adsorption capacity of 86.1 mg/g,and 97.3% removal of the dye in 80 min after adsorption equilibrium.The IHSs can be reused as least 5 times after treatment by NaOH.This method is facile and suitable for large-scale production,and shows great potential for watertreatment.