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NiO coated aluminum borate whiskers were prepared by a sol-gel process and an ultrasonic dispersion technique. The preparation process and characterizations of NiO coated aluminum borate whiskers were investigated. The results show that during the heating process of the xerogel coated aluminum borate whiskers, one endothermic peak appears at 100 °C and three exothermic peaks appear in the range of 150-350 °C according to the differential thermal analysis. And no weight loss occurs after 350 °C according to the thermogravimetry analysis. After the xerogel coated aluminum borate whiskers are calcined at 500 °C, the surface of each whisker is uniformly coated by a layer of NiO film and the NiO coated whiskers can be easily dispersed in water through an ultrasonic apparatus. Moreover, No phase transformation of NiO and interfacial reaction between NiO and aluminum borate whiskers occur when the xerogel coated aluminum borate whiskers are calcined in the range of 500 and 900 °C.