|dc.description.abstract||Development of sustainable manufacturing and conservation of primary materials are the key challenges to environmental degradation and climate change. Recycling of primary materials is one of the approaches suggested for sustainable green manufacturing. In the present study, an attempt has been made to encompass both these concepts, i.e. recycling of waste machined chips of magnesium and development of sustainable manufacturing process.
Chips generated during machining operations are of significant importance; they dissipate the heat from the work-piece and control the quality of the finished products. In recent years researchers have shown that by controlled machining it is possible to tailor size, shape and microstructure of chips and this has added new dimensions to the utility of these machined chips. Chips in the form of thin strips, rods, very fine powders with varying aspect ratio have been successfully machined with grain structure having nano size (~80nm) to submicron size. Consolidation of such machined chips and subsequent fabrication of products is of great interest from the point of view of sustainable manufacturing. Consolidation of machined chips by cold compaction followed by hot extrusion was proposed and has been termed as solid state recycling (SSR). This alternative method of manufacturing using machined chips circumvents melting and casting. Although several materials have been tried by this route, magnesium appears to be the most investigated material. Being lightest among the structural materials, magnesium and its alloys have wide ranging applications especially in automotive industry. Further, magnesium melting is cumbersome and environmentally hazardous which necessitates researchers to explore methods of overcoming the melting route. In this pursuit, SSR appears to be a choice for a soft material like magnesium whose products are fabricated by conventional processing techniques which include cold compaction followed by hot extrusion.
Most of the work in literature with regard to SSR of magnesium has been centered around development of new alloys and their characterisation at room and elevated temperatures. Effect of oxide contaminants has also been widely studied. However, studies on microstructural evolution during processing (i.e. microstructure prior to and after extrusion) have not been reported. Further, such studies with pure metal is important since it is possible to separate the effect of secondary phases including precipitates which are otherwise present in alloys of Mg.
Hence, commercial grade pure magnesium is the material of interest in the present work. Process of consolidation includes room temperature compaction followed by hot extrusion. The aim of the present work includes:
Consolidation of machined chips of magnesium into billets by cold compaction at room temperature followed by hot extrusion,
Microstructural characterisation of these cold compacted billets prior to and after extrusion,
Evaluation of mechanical properties after extrusion at different temperatures.
Correlating the mechanical properties with microstructure.
In the present study mechanical properties evaluated include:
strength properties (hardness, tensile and compressive properties), and
As-cast billet of pure magnesium was turned in a lathe to produce chips at ambient conditions. The chips were cold compacted into billets of 28 mm diameter at a pressure of 350 MPa and held for 30 minutes. The billets of compacted chips (referred here as CC) were later extruded at four different temperatures, viz. 250, 300, 350 and 400°C, with an extrusion ratio of 49:1. Prior to extrusion, the CC was soaked at the desired extrusion temperature for 1 hour. Here, extrusions of compacted chips are designated as CCE (chip compacted and extruded). For comparison, the as-cast billet was extruded under similar conditions and is designated as AE (as-cast and extruded). The extruded rods had a diameter of 4 mm. Microstructural characterisation was done prior to and after extrusion, which forms the first part of the thesis. The extruded rods were characterised for their room temperature strength properties in the second part of the thesis. In the third and last part, damping properties were characterised as a function of time and temperature. Microstructural changes at the end of temperature sweep tests were also examined. Optical microscopy did not reveal the grain structure of CC due to the intense strains associated with chip formation and subsequent cold compaction. However, chip boundaries were found randomly oriented and tri-junctions were found to be porous. The CC showed a relative density of 95.4% and this happens to be the highest amongst the values reported in literature for SSR machined chips. TEM images of CC revealed an average grain size of 0.75µm.
CCs were soaked at extrusion temperature and quenched to unravel the microstructure that exists prior to extrusion. Grain size and hardness measurements indicate that the material was recrystallised prior to extrusion. Bulk texture estimated from X-ray diffraction, showed weak crystallographic textures. The CC had a typical texture with c-axis aligned along the compaction direction which subsequently got randomised during soaking (pre-heating at extrusion temperature).
After extrusion, the 250°C extruded AE had slightly stronger texture than CCE: with clear preference for < 1010 > and < 1120 > plane normals. High working temperatures removed such preference and made the textures randomised for both AE and CCE. In-grain misorientations and the relative presence of the twins, estimated from EBSD scans show a clear pattern for higher in-grain misorientations in CCE compared to AE. The values for AE at higher extrusion temperatures approached that of fully recrystallised magnesium. Higher twin fraction in AE was attributed to its relatively larger grain size compared to CCE. The chip boundaries that were randomly oriented before extrusion appeared aligned along the extrusion direction after extrusion. On the contrary AE had an equiaxed structure. Both longitudinal and transverse section micrographs showed pronounced chip boundaries in the 250°C extruded CCE while it was no so pronounced in the case of 400°C extruded material. Density measurements showed 98.6% relative density for 250°C extruded CCE as compared to 99.9% densification achieved in 400°C extruded CCE. Dislocation density estimated using Variance method from the peaks of the X-ray diffraction data showed higher values for CCE compared to AE. Dislocation density reduced with increase in extrusion temperature. For comparison extruded rods were annealed at 250°C for 2 hours and their dislocation density was estimated.
Vickers hardness indentations were done at low load (25g) and higher load (200g). Both showed decreasing values with increase in extrusion temperature. Grain size dependent hardness variation followed the Hall-Petch relationship. CCE showed higher hardness compared to AE.
Room temperature tensile test showed higher 0.2% tensile proof stress (TPS) in CCE material and obeyed the grain size dependent Hall-Petch relationship, though the strain to failure was poor. CCE extruded at 250°C showed fibrous fracture surface and was different from the rest of the CCEs with evidence of shearing at chip boundaries before fracture.
The rest of the CCEs had a typical fracture surface which was similar to AE material. Strain hardening behaviour, measured in terms of hardening exponent (n), hardening capacity (Hc) and hardening rate (θ) was quiet different for CCE compared to AE.
Room temperature compression test showed different kind of failure for 250°C extruded CCE with longitudinal splitting (de-bonding at chip boundaries) and shearing at an angle to loading direction. The rest of the CCEs failed in a typical manner similar to AE material. The 0.2% compressive proof stress (CPS) as a function of grain size obeyed the Hall-Petch relationship for AE while the fit was not so good for CCE. Moreover, except 400°C extruded CCE (CPS was higher by ~22%) the rest of the CCEs had lower CPS compared to AE despite having finer grain size. This was contrary to the TPS and hardness findings wherein CCE was consistently higher compared to AE owing to grain refinement. Density measurements showed presence of 1.4%, 0.8% and 0.5% porosity in 250°, 300° and 350°C extruded CCE samples respectively. Prompted by density, hardness and TPS findings, the CPS values were back-calculated using the Hall-Petch relationship of AE. The back-calculated CPS values of CCE were higher than corresponding AE. Strength asymmetry, measured as a ratio of compressive proof stress to tensile proof stress was higher in CCE compared to AE.
Damping capacity (tanφ) and dynamic modulus were determined as a function of time (tested upto 30 minutes) and temperature (from RT to 300°C) at a constant frequency (5 Hz). CCE material displayed higher tanφ during time and temperature sweep tests (by 10-15%) with CCE extruded at 250° showing the highest values. Dynamic modulus was comparable for both the materials (with less than 5% difference) though, modulus was higher in materials extruded at higher temperature. Microstructural changes were examined at the end of temperature sweep test, both at the point of loading and away from the point of loading. A significant grain growth was observed in region under the loading point (in a 3-point bending set-up) and was insignificant at regions away from the loading point. Coarsening was low in CCE material on account of suppression at chip boundaries. Microstructure of CCE and AE specimens subjected to similar heating conditions but without loading showed no such coarsening.||en_US