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We report the sputter deposition of Cu-7V and Cu-27V (at.%) alloy films in an attempt to yield a “clean” alloy to investigate nanocrystalline stability. Films grown in high vacuum chambers can mitigate processing contaminates which convolute the identification of nanocrystalline stability mechanism(s). The initial films were very clean with carbon and oxygen contents ranging between ~0.01 and 0.38 at.%. Annealing at 400 °C/1 h facilitated the clustering of vanadium at high-angle grain boundary triple junctions. At 800 °C/1 h annealing, the Cu-7V film lost its nanocrystalline grain sizes with the vanadium partitioned to the free surface; the Cu-27V retained its nanocrystalline grains with vanadium clusters in the matrix, but surface solute segregation was present. Though the initial alloy and vacuum annealing retained the low contamination levels sought, the high surface area-to-volume ratio of the film, coupled with high segregation tendencies, enabled this system to phase separate in such a manner that the stability mechanisms that were to be studied were lost at high temperatures. This illustrates obstacles in using thin films to address nanocrystalline stability. 

Abstract Atom probe tomography (APT) of a nanocrystalline Cu–7 at.% V thin film annealed at 400°C for 1 h revealed chemical partitioning in the form of solute segregation. The vanadium precipitated along high angle grain boundaries and at triple junctions, determined by cross-correlative precession electron diffraction of the APT specimen. Upon field evaporation, the V 2+ /(V 1+ + VH 1+ ) ratio from the decomposed ions was ~3 within the matrix grains and ~16 within the vanadium precipitates. It was found that the VH 1+ complex was prevalent in the matrix, with its presence explained in terms of hydrogen's ability to assist in field evaporation. The change in the V 2+ /(V 1+ + VH 1+ ) charge-state ratio (CSR) was studied as a function of base temperature (25–90 K), laser pulse energy (50–200 pJ), and grain orientation. The strongest influence on changing the CSR was with the varied pulse laser, which made the CSR between the precipitates and the matrix equivalent at the higher laser pulse energies. However, at these conditions, the precipitates began to coarsen. The collective results of the CSRs are discussed in terms of field strengths related to the chemical coordination. 

The microstructures of materials typically undergo significant changes during shock loading, causing failure when higher shock pressures are reached. However, preservation of microstructural and mechanical integrity during shock loading are essential in situations such as space travel, nuclear energy, protection systems, extreme geological events, and transportation. Here, we report ex situ shock behavior of a chemically optimized and microstructurally stable, bulk nanocrystalline copper–tantalum alloy that shows a relatively unchanged microstructure or properties when shock compressed up to 15 GPa. The absence of shock-hardening indicates that the grains and grain boundaries that make up the stabilized nanocrystalline microstructure act as stable sinks, thereby annihilating deformation-induced defects during shock loading. This study helps to advance the possibility of developing advanced structural materials for extreme applications where shock loading occurs.