The pH effect upon the sample phase components of Mg/Al-LDH nanocrystalline prepared by the one-step reaction liquid phase method and the nanocrystalline particle sizes is studied.In order to obtain Nano-LDH crystallines with the small aggregate-free and particle sizes,the effects of 3 kinds of drying methods——vacuum drying,common oven drying and solvent replacement drying upon the formation of hardening aggregation of Nano-LDH crystallines are discussed.The physical phase,morphology,and particle sizes of the samples are characterized using XRD and TEM respectively.The results from experiments indicate that when Nano-LDH is prepared,the 11~13 should be the suitable pH value,and the solvent replacement drying method should be adopted to prevent the nanometer powder from froming hardening aggregation.The samples are good in dispersity and appear to be in needle morphology being 50 nm in length and 5 nm or so in width.