Materials Science Forum Vols. 519-521

Abstract: By 3 dimensional X-ray diffraction (3DXRD) using high energy X-rays from synchrotron sources it is possible to study in-situ the nucleation and growth during recrystallization. In this paper it is described and discussed how 3DXRD can supplement EBSP measurements of nucleation and growth. Three types of studies are considered: i) orientation relationships between nuclei and parent deformed matrix, ii) recrystallization kinetics of individual bulk grains and iii) filming of growing grains in deformed single crystals.

Abstract: This study presents in situ observations of recrystallization texture formation in Al-3mass%Mg using SEM concurrent with electron back scattering pattern (EBSP) with hot stage. In the present discussion, the emphasis is on the characteristics of the preferred growth or the shrinkage of Cube and other oriented grains. The in-situ observations of recrystallization demonstrate clearly that the nucleation, growth and shrinkage of recrystallized grains occur simultaneously in each orientation in each region. The overall development of recrystallization texture depends on the balance of nucleation/growth and shrinkage/disappearance of each orientation during recrystallization. The preferential growth is determined by the grain boundary mobility between recrystallized grains or the clusters composed of several similar oriented grains, i.e. Cube clusters or S clusters, and neighboring deformed matrix, and the competitive growth with the surrounding grains. On the other hand, the isolated oriented grain and the strain-stored grains tend to shrink and disappear during recrystallization and grain growth.

Abstract: For 2195-T8 plate, design properties are based on the mechanical properties at the near surface location, corresponding to the load carrying thin membrane location in machined integrally stiffened structure. Mechanical properties at the near surface location are lower than those at the t/4 and t/2 locations. This work examined the effect of alternate temper and hot rolling practices on near surface strength levels. Results showed that alternate hot rolling practice were very effective in raising near surface strengths and improving property uniformity, and were well correlated with crystallographic texture measurements.

Abstract: The softening behaviour during annealing was investigated in cold and hot rolled AA3103 alloys after different heat treatments. It was found that the evolution of boundary spacing determined using gallium enhanced microscopy gives a very good representation of the softening behaviour. The results show that cold rolled Al-Mn alloys soften by continuous growth of the subgrain structure, “continuous recrystallisation”, provided the pre-treatment of the ingots has been made to avoid too high a density of dispersoids and the cold rolling reduction has been very large. The very high strain creates a microstructure with a large fraction of high angle boundaries that are mostly parallel to the sheet surface. A recently developed subgrain growth model which takes the effect of solute drag into account, gives a good description of the softening kinetics. The solute drag is controlled by bulk diffusion of Mn. The simultaneous precipitation of Mn from the solid solution takes place by grain boundary diffusion of the Mn atoms mainly to pre-existing particles. The solute concentration decreases as the inverse of the boundary spacing, which is due to the grain growth mainly in the thickness (normal) direction.

Abstract: This paper described new characterization methods and data to quantify the influence of solute atoms on grain boundary and sub-grain boundary mobilities in Al-Mn alloys with a view to their integration into recovery and recrystallization modelling. Detailed SEM measurements of grain boundary mobilities during recrystallization have been made by in-situ annealing experiments on cold deformed Al – 0.1 and 0.3wt.% Mn binary alloys. Stored energies are estimated from the sub-grain sizes and misorientations and the boundary velocities directly measured in the temperature range 200-450°C. It is shown that in many cases good agreement with the Cahn, Lücke, Stüwe model for solute drag is obtained, e.g. the activation energies are intermediate between those of boundary and volume solute diffusion. Some particular cases of rapid growth occur in Al-0.1%Mn indicating boundary breakaway from solute clouds. A complementary study of sub-grain boundary mobilities has started on the same alloys; in this case the average mobilities are estimated from FEG-SEM growth data for the average sub-grain size for temperatures in the range 150-300°C. The results are compared with some previous data on Al-Si and show similar rates.

Abstract: A simple model for recovery of a subgrain structure is used to distinguish and explain the respective influence of the deformed microstructure characteristics, annealing temperature and concurrent precipitation kinetics on the nucleation kinetics of recrystallisation. Simulation results demonstrate how the balance between recovery and precipitation kinetics controls nucleation.

Abstract: The starting material, the deformed state, as well as the recrystallised microstructure and texture have been analysed as a function of Zener-Hollomon parameter and strain for two differently heat-treated AlMgSi alloys, deformed in torsion. An interesting and somewhat surprising observation is that the grain size was always higher in the material heat treated to form large Mg2Si particles. Moreover, no indications of PSN effects were observed in any of the materials, even at the highest Zener-Hollomon parameters. This observation was quite unexpected as the highest Zener-Hollomon parameters were well above the typical critical level for which significant PSN effects have been observed in similar alloys. The results have been carefully analysed and possible explanations are discussed.

Abstract: Severe plastic straining is an established method for producing submicron grain (SMG) structures in alloys. However, the development of such a fine grained structure in single-phase alloys is usually futile if they are to be exposed or processed at elevated temperatures. This is a direct consequence of the natural tendency for rapid and substantial grain coarsening which completely removes the benefits obtained by grain refinement. This problem may be avoided by the introduction of nanosized, highly stable particles in the metal matrix. In this work, a SMG structure was generated in an Al-0.3 wt.% Sc alloy by Equal Channel Angular Pressing (ECAP). The alloy was prepared initially to produce a fine grained microstructure exhibiting a large fraction of high angle grain boundaries and a dispersion of nanosized Al3Sc particles. The evolution of microstructure during annealing at temperatures up to 550 °C was examined in detail and grain size distributions generated from the data. It was shown that grain coarsening is rapid at temperatures above 450 °C and the initial log-normal grain size distribution exhibiting low variance and skewness was altered considerably. The statistical information generated from the grain size distributions confirms that discontinuous grain coarsening occurs in this alloy only at temperatures greater than 500 °C.

Abstract: The Mesoalite alloy is formed using rapidly solidified powder metallurgy (RS-P/M) by hot extruding the RS powder produced by the atomization method. Meso20 is a Mesoalite alloy with a chemical composition of Al-9.5Zn3Mg-1.5Cu-4Mn-0.04Ag (mass%). Meso20 contains fine grains and precipitated intermetallic Mn compounds, and has a tensile strength of 910 MPa. During hot extrusion, dynamic recrystallization occurs and the fine grains develop. During heat treatment of Meso20, rod-like and granular Mn intermetallic compounds precipitate. The rod-like compounds are about 1 Ìm in length and the granular compounds are about 1 Ìm in diameter. X-ray diffraction measurement, transmission electron microscopy and energy dispersive X-ray (TEM/EDX) analysis and Rietveld analysis revealed the chemical composition of the granular and rod-like Mn intermetallic precipitates to be 86.5Al-10.9Mn-0.4Cu-0.9Zn-1.3Mg and 80.5Al - 10.3Mn-4.2Cu-2.5Zn-2.5Mg (mass%), respectively. The granular and rod-like compounds were identified as the Al6Mn and Q phases, respectively, with both belonging to the space group Cmcm. The lattice constants of Al6Mn were a=0.754 nm, b=0.648 nm c=0.855 nm and those of the Q phase were a=0.765 nm b=2.34 nm c=1.25 nm. Meso10, with a chemical composition of Al-9.5Zn-3Mg-1.5Cu-0.04Ag (mass%), contains no Mn and does not have fine grains, but rather coarse fibrous grains elongated along the extrusion direction. Thus the Mn intermetallic precipitates in Meso20 clearly affect the formation of fine grains. Microstructure development was studied during hot extrusion by observation using high resolution Electron Back Scattering Pattern method. Fine grains were found to develop in areas, which were relatively abundant in granular Mn intermetallic precipitates.

Abstract: This work describes the microstructure and properties of a range of Al-(4-6)Mg- (1.2-1.6)Li-(0.3-0.4)Zr-(0-0.2)Sc alloys produced at Oxford University by spraycasting. Follow- ing hot isostatic pressing of the as-spraycast billets to close any porosity and to precipitate a ¯ne, coherent dispersoid population, forging to a true strain of 1 at 250 and 400±C led to a substantial re¯nement of the microstructure with grain sizes in the range 0.8 to 5¹m. A large intra-granular orientation gradient with distance measured using EBSD showed that at 250±C, partial dynamic recrystallisation by progressive lattice rotation led to a `necklace' structure of very ¯ne grains surrounding larger deformed grains. At 400±C, dynamic recrystallisation oc- curred by nucleation of new grains at prior grain boundaries and triple points. The strength of as-forged alloys was 200-350MPa and the high ductilities of up to 30% rendered the alloys amenable to post-forging cold work. A proof strength of 460MPa with 9.5% elongation was achieved in a non-heat-treatable spraycast Al-6Mg-1.3Li-0.4Zr alloy, matching the best prop- erties of similar mechanically alloyed AA5091, and exceeding the properties of AA7010-T74. The as-forged alloys showed excellent thermal stability up to » 0.9Tm, with no abnormal grain growth and grain size stagnation due to Zener pinning. Finally, strain rate sensitivity testing revealed the potential for superplasticity at 400 and 500±C and strain rates of 0.001-0.05s¡1.