Anisotropic conductive adhesive (ACA) is an advanced packaging material with lots of merits, but its manufacture is of high tech upon multiple branches of knowledge. In this letter, a step of preparing the conductive particles of ACA was investigated, that is, electroless nickel plating on polymer microshperes. The process of the coating formation consists of four steps: chemical etching, sensitization, activation, and electroless plating. 0.23 pim in thickness uniform and smooth Ni-P coating on 3.7 pim in diameter polystyrene microspheres was formed upon 25 min plating. The advantage of this plating process is to ensure an easy and accurate control on the thickness and the quality of the plating coat.