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The mechanism of nanostructure formation during cryogenic and room-temperature milling of Cu and Cu–3wt%Zn was investigated using X-ray diffraction line profile analysis. For that, the whole powder pattern modeling approach (WPPM) was used to analyze the evolution of microstructural features including coherently scattering domain size, dislocation density, and density of planar faults. It was found that for all sets of experiments, structural decomposition is the dominant mechanism of nanostructure formation during cryomilling. During subsequent RT-milling, grain refinement still occurs by structural decomposition for pure copper. On the other hand, discontinuous dynamic recrystallization is responsible for nanostructure formation during RT-milling of Cu–3wt%Zn. This is attributed to lower stacking-fault energy of Cu–3wt%Zn compared to pure copper. Finally, room temperature milling reveals the occurrence of a detwinning phenomenon.

The thermal stability of nanocrystalline cartridge brass (Cu–30 at.% Zn) and brass–Zr alloys were investigated. The alloys were produced by cryogenic ball milling and subsequently heat treated to a maximum temperature of 800 °C. The grain size of pure brass was found to be relatively stable in comparison to pure copper, and a high hardness was retained up to 600 °C. When 1 at.% zirconium was alloyed with the brass, the grain size was stabilized near 100 nm even at 800 °C. At the highest temperature, hardness was retained above 2.5 GPa for 1 and 5 at.% zirconium alloys, but the pure brass softened significantly. The stabilization is believed to be dominated by Zn–Zr interactions as a second phase of these two was observed in X-ray diffraction and transmission electron microscopy. Thermodynamic modeling indicates a zero grain boundary energy may be achieved depending on the mixing enthalpy value used (i.e., calculated vs. experimental) under ideal conditions, but microstructural features such as twinning and second phase particles are thought to be the dominant stabilization mechanism. Zr worked well in stabilizing the brass in the nanocrystalline state to nearly 90 % of its melting temperature.

Nanocrystalline Cu–30% Zn samples were produced by high energy ball milling at 77 K and room temperature. Cryomilled flakes were further processed by ultrahigh strain high pressure torsion (HPT) or room temperature milling to produce bulk artifact-free samples. Deformation-induced grain growth and a reduction in twin probability were observed in HPT consolidated samples. Investigations of the mechanical properties by hardness measurements and tensile tests revealed that at small grain sizes of less than ∼35 nm Cu–30% Zn deviates from the classical Hall–Petch relation and the strength of nanocrsytalline Cu–30% Zn is comparable with that of nanocrystalline pure copper. High resolution transmission electron microscopy studies show a high density of finely spaced deformation nanotwins, formed due to the low stacking fault energy of 14 mJ m –2 and low temperature severe plastic deformation. Possible softening mechanisms proposed in the literature for nanotwin copper are addressed and the twin-related softening behavior in nanotwinned Cu is extended to the Cu–30% Zn alloy based on detwinning mechanisms.

The effect of low-temperature on the active deformation mechanism is studied in pure copper. For this purpose, cryogenic wire drawing at liquid nitrogen temperature (77 K) was performed using molybdenum disulfide lubrication. Microstructural investigation and texture analysis revealed severe twin formation in the cryogenically drawn copper, with a broad twin size distribution. The spacing of the observed deformation twins ranges from below 100 nm, as reported in previous investigations, up to several micrometers. The extent of twin formation, which is significantly higher when compared to other cryo-deformation techniques, is discussed with respect to the state of stress and the texture evolution during wire drawing. � 2011 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Pure copper and Cu–12.1 at.%Al–4.1 at.%Zn alloy were subjected to rolling in liquid nitrogen. TEM studies showed that dynamic recovery during the deformation process was effectively suppressed and hence microstructures with dislocation substructure and deformation twins were formed. Mechanical properties were assessed via microtensile testing that shows improved yield strength, 520 ± 20 MPa, and ductility, 22%, in the case of pure copper. Alloying with Al and Zn results in reduction in stacking fault energy (SFE) which can contribute to enhanced strength and good ductility. Physical activation volume obtained via stress relaxation tests is 26 b 3 , and 8 b 3 for pure copper, and Cu–12.1 at.%Al–4.1 at.%Zn, respectively. The effect of SFE on work hardening rate of samples is discussed. Although twinning is observed in the alloy, it is concluded that network dislocation strengthening plays the major role in determining the mechanical properties.

Copper alloys with different amounts of zinc were synthesized via high energy ball milling at liquid nitrogen and room temperature. Bulk samples were produced in situ by controlling the milling temperature. It is shown that temperature plays an important role in formation of artifact-free consolidated samples via its effect on defect formation and annihilation during the milling process. The mechanical behavior of Cu–Zn nanocrystalline alloys was examined using Vickers microhardness and tensile tests. The nanostructure of the alloys was investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The hardness results of processed alloys vary as a function of the alloying elements. Considering typical low ductility of nanocrystalline materials, the improved ductility with the high strength observed in these alloys suggests that they are artifact-free and may have several deformation mechanisms, which may include dislocation activity and nano-twinning.