Delubrication of Chromium Prealloyed Powder Metallurgy Steels

Licentiate thesis, 2013

Consolidation of steel components produced by means of powder metallurgy (PM) is achieved typically through compaction and sintering. During consolidation, final dimensions of the part are already achieved after compaction, while sintering imparts strength to the components. Prior to the compaction stage, lubricants are added to the metal powder to reduce the inter-particle and die-wall friction during pressing and hence improve powder compressibility and ejection of the component from the compaction tool. These lubricants have to be safely removed after compaction since they are source of oxygen and carbon that can negatively affect further sintering process as well as final performance of the sintered components. Lubricants commonly used for PM steels are based on ethylene bis-stearamide (EBS) and their removal is achieved through thermolysis in the initial zone of the sintering furnace. With increasing demands on the achievable densities and performance of PM components, lubricants and possible risks of improper delubrication have received interest. Among the problems encountered during sintering, those concerning delubrication are frequent but difficult to detect. Hence previous studies have aimed at improving the efficiency of lubricant removal and predicting the same. Delubrication being a complex process still poses problems in practice and its proper control requires a system which monitors the delubrication sequence and can be incorporated into a closed loop control. In the present work, a reliable approach for in-situ monitoring of delubrication of PM steel compacts is presented. The method is based on continuous monitoring of the processing atmosphere using sensors commonly used in the industry (CO2 and O2). It was demonstrated that the initial stages of lubricant removal can be monitored using the oxygen sensor based on zirconia ceramics and the later stages can be detected utilizing CO2 sensor based on infrared cell technology. Based on the established methodology, a systematic study on the effect of various process parameters on lubricant removal in the processing of chromium prealloyed PM steels has been conducted. Effect of temperature, holding time, heating rate, process gas composition (inert, reducing and oxygen containing atmospheres) and purity (wet and dry gases), flow rate and graphite addition was evaluated. Additionally, change in surface chemistry of the base powder occurring during delubrication and its effect on sintering have been studied using X-ray photoelectron spectroscopy and scanning electron microscopy combined with the energy dispersive X-ray analysis. Based on the experimental results it is recommended to perform delubrication at ~ 450 °C applying low heating rates in dry-nitrogen atmosphere with flow sufficient enough to provide dynamic gas conditions around the component surface. This is especially important in the case of powder prealloyed with oxygen sensitive elements like chromium.