Effect of high-pressure torsion processing on the microstructure evolution and mechanical properties of consolidated micro size Cu and Cu-SiC powders

In this paper, micro size Cu and Cu-SiC composites powders were consolidated by powder metallurgy (PM) followed by sintering or high-pressure torsion (HPT) to study the effect of the different processing methods on microstructure evolution and mechanical properties. HPT contributes in producing fully dense samples with a relative density higher than those processed by PM followed by sintering. Bimodal and trimodal microstructures with a mixture of ultrafine grain (UFG) and micro or nano grain sizes were noted in the case of Cu and Cu-SiC HPTed samples, respectively. The increase of the SiC volume fraction (SiC%) produces smaller grain size with higher fractions of high angle grain boundaries (HAGBs) in the HPTed Cu-SiC samples than that in the case of HPTed Cu sample. The HPT under a pressure of 10 GPa and 15 revolutions was effective to achieve a complete fragmentation of SiC particles down to ultrafine particle size. HPT processing of Cu and Cu-SiC composites enhanced the mechanical properties (hardness and tensile strength) with conserving a reasonable degree of ductility (elongation%). The yield strength of the samples was estimated based on the microstructure observations and processing parameters by different models correctly with an error range of 5.1–1% from the experiential results.     

Consolidation of Cu-based amorphous alloy powders by high-pressure torsion

We applied high-pressure torsion (HPT) for consolidation of gas-atomized metallic glass Cu₅₄Zr₂₂Ti₁₈Ni₆ powders into high-density bulk disks. The effects of the number of revolutions (N = 1–5 turns), applied pressure (2.5–10 GPa), and temperature (298–473 K) on densification and structural changes were investigated. The consolidated glassy disks showed an excellent hardness of ~5.2 GPa although a mechanical softening effect along with fragmentation in the center of HPT disks occurred at N > 3 by a couple of branching cracks. The HPT process at higher applied pressures improved the bulk density and inter-particulate bonding, resulting in higher hardness. Increasing the temperature of HPT processing enhanced the densification and deep drawability of the consolidated metallic glass. Although the HPT process did not change the crystallization temperature of the metallic glass powders, it increased the crystallization enthalpy, suggesting the free volume increase and inhibition of a significant nanocrystallization during the HPT process.     

Mechanical properties and thermal stability of a Cu-based bulk metallic glass microalloyed with silicon

(Cu₄₂Zr₄₂Al₈Ag₈)_{100? x} Si _x (x?=?0?～?1) amorphous alloy rods of 2–6?mm diameter were prepared by Cu-mold drop casting. The thermal properties, microstructure evolution, and mechanical properties were studied by differential scanning calorimetry (DSC), X-ray diffractometry (XRD), transmission electron microscopy (TEM), hardness test, and compression test. The XRD result revealed that all as-quenched (Cu₄₂Zr₄₂Al₈Ag₈)_100?x Si _x alloy rods exhibited a broad diffraction pattern in the amorphous phase. The (Cu₄₂Zr₄₂Al₈Ag₈)_99.5Si_0.5 alloy was found to possess the highest glass forming ability (GFA) as well as the best thermal stability among all tested samples. In addition, both its hardness and yield strength were increased by the microalloyed Si content. The fracture strength and the plastic strain of (Cu₄₂Zr₄₂Al₈Ag₈)_99.5Si_0.5 amorphous alloy can reach 2000?MPa and 3.5 %.     

Mechanical properties and microstructure evolution in an aluminum 6082 alloy processed by high-pressure torsion

A commercial aluminum 6082 alloy was used to investigate the effect of the initial condition on subsequent processing by high-pressure torsion (HPT). The alloy was prepared in two different initial conditions: (i) in a T651 annealed condition and (ii) after a solution treatment followed by over-aging and subsequent processing by equal-channel angular pressing (ECAP). All samples were processed by HPT through 1/2, 1, 2, 5, and 10 turns and then the microstructures were examined using electron backscattered diffraction (EBSD). Significant grain refinement was achieved after processing by HPT through 5 turns with measured grain sizes of ~0.5 μm in both types of alloy. Microhardness measurements were conducted to evaluate the evolution of hardness after HPT for the two initial conditions. It is demonstrated that there is a difference in the hardness values between these two initial conditions, and this difference remains almost constant after processing by HPT.     

W-35%Cu粉末形变强化复合材料组织及性能研究

为了提高W-Cu复合材料的致密度,采用机械球磨-冷压制坯-液相烧结-热静液挤压-热处理工艺,制备出微观组织弥散分布、性能优异的W-35%Cu复合材料.采用扫描电镜、电子探针等测试手段分别对烧结及挤压后材料的组织及性能进行了分析.实验结果表明,采用机械球磨技术制备的W-35%Cu复合粉,经液相活化烧结后,再经热静液挤压进一步形变和致密,材料的硬度以及导电性能都有较大提高.在800℃真空热处理2 h后,获得了硬度高于200HB,电导率高于40m/Ω·mm2的W-35%Cu形变复合材料.     

Mechanical alloying of Co–Cu powders

The aim of this work was to investigate two cobalt alloys, namely, the Co–20Cu and the Co–30Cr (atomic percentage), prepared by mechanical alloying, by using balls and Szegvari mills. The samples obtained were characterized by X-ray diffraction, differential scanning calorimetry, and chemical microanalysis. The main results for the Co–20Cu show a good agreement with previous work in terms of the corresponding lattice parameters values which are function of milling times, the milled mixtures show a nodular morphology. For the Co–30Cr, difference in X-ray patterns from the final samples were found as compared to other works. The particle size of the powders plays an important role in the alloys preparation. Received: 31 March 2000 / Reviewed and accepted: 8 June 2000     

Mechanical properties and thermal stability of nitrogen incorporated diamond-like carbon films

The nitrogen incorporated diamond-like carbon films were deposited on Si (100) substrates by arc ion plating (AIP) under different N₂ content in the gas mixture of Ar and N₂. The influence of N₂ content on the film microstructure and mechanical properties was studied by atomic force microscopy, transmission electron microscopy, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and nanoindentation. It was found that the hardness (H), elastic modulus (E), elastic recovery (R) and plastic resistance parameter (H/E) decrease with increasing the nitrogen content. The decrease of mechanical properties of DLC films resulted from nitrogen incorporation was associated with total sp³ carbon bond content and N-sp³C bond content. The structural modification as well as mechanical properties of the annealed nitrogen incorporated diamond-like carbon films was investigated as a function of annealing temperature. Raman spectra indicate that the I_D/I_G ratio starts to increase and G peak position shifts upward at the annealing temperature over 500 °C. The hardness and elastic modulus of thermally annealed nitrogen incorporated DLC films decreased slightly at lower annealing temperature and then significantly decreased at higher annealing temperature. The strong covalent bonding between C and N atoms is expected to be effective on their thermal stability enhancement.     

Fabrication of nanograined silicon by high-pressure torsion

This paper describes fabrication of Si nanograins through allotropic phase transformation by concurrent application of high pressure and intense straining using high-pressure torsion (HPT). Single-crystalline Si(100) wafers were processed by HPT under a pressure of 24 GPa at room temperature. X-ray diffraction and Raman analysis revealed that the HPT-processed samples were composed of metastable Si-III and Si-XII phases and amorphous phases in addition to the original diamond-cubic Si-I phase. It was found that nanograins formed because the Si-I diamond phase had transformed to high-pressure phases (Si-II, Si-XI, and Si-V) having metallic nature, and it then became easier to generate a high density of dislocations to form grain boundaries. The high-pressure phases were further transformed to the Si-XII and Si-III phases via the Si-II phase upon unloading and they existed as metastable phases at ambient pressure. Subsequent annealing at 873 K gave rise to reverse transformation to Si-I but with nanograin sizes. Although no appreciable photoluminescence (PL) peak was observed from the HPT-processed sample, a broad PL peak centered around 600 nm was detected from the annealed sample due to quantum confinement in the Si-I nanograins.     

Microstructural evolution and the mechanical properties of an aluminum alloy processed by high-pressure torsion

Processing by high-pressure torsion (HPT) was performed on disks of an Al-7075 alloy at room temperature. The alloy was initially annealed at 753 K and then processed by HPT under a pressure of 6.0 GPa up to a maximum of ten turns. Measurements of the Vickers microhardness showed lower values at the centers of the disks after small numbers of turns but higher numbers of turns led to a reasonable hardness homogeneity across each disk. After five turns, the grain size at the edge of the disk was ~250 nm. It is demonstrated that results from mechanical testing are consistent with the hardness and microstructural data.     

Mechanical properties of bulk metallic glasses

The mechanical properties of bulk metallic glasses, including their superior strength and hardness, and excellent corrosion and wear resistance, combined with their general inability to undergo homogeneous plastic deformation have been a subject of fascination for scientists and engineers. The scientific interest stems from the unconventional deformation and failure initiation mechanisms in this class of materials in which the typical carriers of plastic flow (dislocations) are absent. Metallic glasses undergo highly localized, heterogeneous deformation by formation of shear bands, a particular mode of deformation of interest for certain applications, but which also causes them to fail catastrophically due to uninhibited shear band propagation. Varying degrees of brittle and plastic failure creating intricate fracture patterns are observed in metallic glasses, quite different from those observed in crystalline solids. The tension–compression anisotropy, strain-rate sensitivity, thermal stability, stress-induced crystallization and polyamorphism transformations, are some of the attributes that have sparked engineering studies on bulk metallic glasses. Understanding of the glass-forming ability and the deformation and failure mechanisms of bulk metallic glasses, has given insight into alloy compositions and intrinsically-forming or extrinsically-added reinforcement phases for creating composite structures, to attain the combination of high strength, tensile ductility, and fracture toughness needed for use in advanced structural applications. The relative ease of fabricating metallic glasses into bulk forms, combined with their unique mechanical properties, has made these materials attractive options for possible applications in aerospace, naval, sports equipment, luxury goods, armor and anti-armor systems, electronic packaging, and biomedical devices.     

Long-term self-annealing of copper and aluminium processed by high-pressure torsion

High-pressure torsion (HPT) is recognized as the most effective method for producing ultrafine-grained and even nanocrystalline structures in metallic systems. Although there are many reports on microstructural refinement of pure metals and metallic alloys, several important problems remain unresolved. For example, more information is needed on the homogeneity of the processed microstructure and on the heat release and temperature rise during HPT processing. Recently, there were reports of hardening in HPT-processed pure metals under conditions of self-annealing. This report presents new experimental data on the relaxation processes in HPT copper and aluminium processed at room temperature under loads of 6.0 and 1.0 GPa for zero and one turn. The experimental results were obtained using X-ray diffraction and by measuring the average Vickers microhardness after ageing.     

Significance of temperature increase in processing by high-pressure torsion

Experiments and finite element simulations were conducted to measure the temperature increase in processing disc samples by high-pressure torsion. Aluminum, copper, iron and molybdenum were selected as model materials. The temperature increases at the early stages of straining but saturates to steady-state levels at large strains. The increase of temperature is proportional to the hardness and rotation speed and is higher at higher imposed pressures and is somewhat higher at larger distances from the disc center.     

Mechanical and thermal properties of physical vapour deposited alumina films Part I Thermal stability

Thermal stability of non-reactive physical vapour deposited alumina films of varying thickness on Al₂O₃-TiC and Si substrates, deposited at two different substrate biases, is examined. Substrate curvature measurements were used to determine the deposition stress and stress development during thermal cycling and annealing. Thermal cycling experiments revealed that the films deposited on Al₂O₃-TiC substrates become irreversibly more compressive on heating and annealing while films deposited on Si substrates become irreversibly more tensile. The deposition stress was found to be independent of film thickness, substrate material, and substrate bias during deposition. The thermal stability was independent of film thickness and substrate bias during deposition.     

Allotropic phase transformation of pure zirconium by high-pressure torsion

Pure Zr is processed by high-pressure torsion (HPT) at pressures in the range of 1–40 GPa. A phase transformation occurs from α to ω phase during HPT at pressures above 4 GPa while the total fraction of ω phase increases with straining and saturates to a constant level at higher strain. This phase transformation leads to microstructural refinement, hardness and strength enhancement and ductility reduction. Lattice parameter measurements confirm that c for α phase is expanded about 0.6% by the presence of ω phase. The temperature for reverse transformation from ω to α phase increases with straining and thus, straining under high pressure increases thermal stability of ω phase. The ω phase obtained by HPT is stable for more than 400 days at room temperature.     

Microstructure evolution of CuZr polycrystals processed by high-pressure torsion

The microstructure evolution of extruded Cu–0.18 wt% Zr polycrystals processed by high-pressure torsion (HPT) at room temperature at the pressure of 4 GPa and the different number of the HPT revolutions (i.e. different strain) was investigated using the combination of the electron back-scatter diffraction, microhardness measurements and the X-ray diffraction. A significant transition from the inhomogeneous microstructure after few HPT revolutions into the homogeneous equiaxed microstructure with increasing number of HPT rotations was observed. HPT straining leads to the grain size refinement by a factor more than 100 after the 25 HPT revolutions. Moreover, the EBSD revealed an increase in the fraction of high-angle grain boundaries (HAGBs) with increasing HPT straining reaching the value of 70% after 25 revolutions. Additionally, a slight increase of the twin-related CSL Σ3 grain boundaries occurred during the microstructure refinement. The microhardness measurements confirmed the billet radial inhomogeneity at early stages of the HPT straining, whereas with increasing number of the HPT rotations, causing the specimen fragmentation and homogenization, the microhardness values increased. The average crystallite size and the average dislocation density in individual specimens determined by the XRD diffraction were in the range of approximately 100–200 nm and 2 × 10¹⁵ m⁻², respectively. Moreover, XRD measurements confirmed the absence of residual stresses in all specimens.     

Microstructure and microtexture in pure copper processed by high-pressure torsion

The evolution of microstructure and microtexture in high purity copper was examined after processing by high-pressure torsion (HPT). Copper disks were annealed for 1 h at 800 °C and later processed monotonously in HPT at ambient temperature for 1/4, 1/2, 1, and 5 turns under a pressure of 6.0 GPa. Electron backscattered diffraction (EBSD) measurements were taken for each disk at three positions: center, mid-radius, and near-edge. Results from EBSD for samples processed between 1/4 and 1 turn indicate the formation of Σ3 twin boundaries by recrystallization before complete microstructural refinement. The results show a gradual increase in the homogeneity of the microstructure with increasing numbers of turns, reaching a stabilized ultrafine-grained structure at 5 turns with a bimodal distribution of fine and coarse grains of 0.15 and 0.5 μm in diameter, respectively. The occurrence of recrystallization in the early straining stages was further supported by examining microtexture development with increasing numbers of turns, where this shows a gradual transition from a shear texture to a mixture of shear and recrystallization and later to a shear texture at high HPT strains. The promotion of recrystallization during HPT is probably related to the high purity of the copper.     

Degassing and surface analysis of gas atomized aluminium alloy powders

The degassing behaviour and surface characterization of Al-Mg base alloys has been investigated using quadrupole mass spectrometry (QMS) and X-ray photoelectron spectroscopy (XPS). The alloy composition, particle size and the nature of the atomizing gas have been studied in terms of gas evolution and surface composition. XPS has been used both to measure oxide thicknesses and magnesium enrichment ratios. XPS results show that magnesium segregation increases for larger particle sizes and this is supported by QMS, with a correspondingly higher hydrogen evolution on heating being observed for the larger size fractions. High-resolution XPS of the carbon 1s photoelectron peak (C1s) indicates the presence of carbonate component on the as-received magnesium-containing powders. This component is less pronounced on degassed powders indicating the evolution of CO₂ on heating. This observation is supported by thermodynamic calculations.     

Interfacial microstructures and properties of aluminum alloys/galvanized low-carbon steel under high-pressure torsion

A new composite processing technology characterized by hot-dip Zn–Al alloy process was developed to achieve a sound metallurgical bonding between Al–7 wt% Si alloy (or pure Al) castings and low-carbon steel inserts, and the variations of microstructure and property of the bonding zone were investigated under high-pressure torsion (HPT). During hot-dipping in a Zn–2.2 wt% Al alloy bath, a thick Al₅Fe₂Zn_x phase layer was formed on the steel surface and retarded the formation of Fe–Zn compound layers, resulting in the formation of a dispersed Al₃FeZn_x phase in zinc coating. During the composite casting process, complex interface reactions were observed for the Al–Fe–Si–Zn (or Al–Fe–Zn) phases formation in the interfacial bonding zone of Al–Si alloy (or Al)/galvanized steel reaction couple. In addition, the results show that the HPT process generates a number of cracks in the Al–Fe phase layers (consisting of Al₅Fe₂ and Al₃Fe phases) of the Al/aluminized steel interface. Unexpectedly, the Al/galvanized steel interface zone shows a good plastic property. Beside the Al/galvanized steel interface zone, the microhardnesses of both the interface zone and substrates increased after the HPT process.     

The thermal stability of high-energy ball-milled nanostructured Cu

The thermal stability of nanostructured (NS) Cu prepared by high-energy ball milling was investigated. The as-prepared samples were isothermal annealed for 1 h in the temperature range of 200–1000 °C. Effects of annealing on NS Cu samples were studied by means of Vickers hardness test, differential scanning calorimetry (DSC) and stress relaxation test. The exceptional high microhardness of as-prepared Cu sample of 1.7 GPa was not detected to decrease after annealing at 500 °C for 1 h with corresponding small value of activation volumes V^* of 22.6b³ and high value of strain rate sensitivity m of 0.0176. A prominent decrease of microhardness was detected after higher temperature annealing with a rapidly increase of activation volume and decrease of strain rate sensitivity. The present investigation demonstrates that the thermal stability of NS Cu prepared by high-energy ball milling is determined by not only the grain size but also the microstructure of grain boundaries, and during annealing process, the strain release process occurred prior to the grain growth process, therefore, the NS Cu has a relatively high thermal stability.