Nitriding is a surface hardening treatment used on steel components to improve their resistance to corrosion, fatigue, and wear. Iron nitrides at the nitrided steel surface form a compound layer known for its high hardness but also for its brittle nature. It is not uncommon for this layer to chip or break away during metallurgical sample preparation, making it difficult to accurately characterize the microstructure of the nitrided load. This paper presents the results of several studies that assess the effect of cutting and polishing operations along with polishing pressure, the use of foils, and Ni plating. A best practice procedure has been developed to prevent damage to nitrided samples and minimize uncertainty when evaluating part quality.

Microstructural examination of a nitrided part is the most commonly used method for evaluating nitriding material and process performance. Microstructural evaluation also helps to validate that the process ran as intended and produced the desired nitrided case characteristics. However, sample preparation is often complicated by the partial or complete breakaway of the compound layer and may affect the accuracy of the conclusions made. A set of experiments was performed to evaluate the effect of two saw cutting methods, the use of metal foil for sample mounting, and the use of Ni plating before cutting. Microstructures of 12 experimental conditions were analyzed. Recommendations were made for the nitrided sample preparation best practice to analyze compound layer uniformity and thickness.