The DC plasma chemical vapor deposition (DC-PCVD) method was a promising technique to fabricate CVD diamond coatings in industry, because it has many good properties, such as high grown rate of diamond films, big grown area, high qualities, and cost effective. In the present work, we synthesized diamond films on cemented carbide (YG6) substrates, and studied the different nitric acid aqueous solution treatment durations influence on diamond nucleation stage. The results indicated that well-chosen nitric acid aqueous solution treatment durations should be selected. For too short treatment times, the residual Co will promote the carbon transform from diamond metastable phase into graphite stable phase. On the other side, too long treatment times will consume too much Co, which will lead to the shortage of cohesive body, and finally the crackers in the bulk propagated and peeled off with the diamond films well grown on WC grains.