ZrB2 coatings have been widely used in industrial fields due to their interesting intrinsic characteristics, such as high melting point, high hardness, excellent oxidation resistance and corrosion resistance, etc. However, they are still restricted to apply on the cutting tool surface owing to their high brittleness. The addition of nitrogen atoms is expected to cause a further improvement on the film toughness through forming nanocomposite microstructure, namely the nanocrystallines ZrN or ZrB2 are surrounded by amorphous BN phase. Usually, high purity nitrogen used as reactive gas is produced by physical liquid phase separation method. It is inevitable that small amount of oxygen impurity is remained in it. Because boron is easy to react with oxygen to form amorphous boron oxide. As a result, a large amount of amorphous boron oxide and boron nitride phases existing in the coatings severely affects their mechanical properties. To resolve the above problem, the oxygen impurities in the Zr-B-N coating must be removed. In this work, a new method to prepare high-purity, super-hard and highly wear-resistant Zr-B-N nanocomposite coatings was proposed. Namely, an appropriate amount of reducing hydrogen was mixed into the reactive gas during the coating deposition. Through reduction reaction, the combination of oxygen with elements other than hydrogen would be prohibited, and the oxygen impurities in the vacuum chamber could be removed. Therefore, the purity of the Zr-B-N coating and its related properties could also be improved. In addition, the use of reducing gas in the process of reactive deposition also lowered the technological requirements of coating equipment. A large amount of vacuum pumping time was saved. The coating efficiency was improved and the production cost is reduced.