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On the Cu-Nb Phase Diagram and Solidified Microstructures

Container and containerless processing was employed to determine liquidus temperatures and to examine microstructural development in the Cu-Nb system. The Cu-Nb phase diagram of an S-shaped, near-horizontal liquidus, has been confirmed by both the temperature-time profiles and resultant microstructures with only Nb dendrites in a Cu matrix, which were obtained from crucible experiments under clean conditions. However, the microstructural pathways of Cu-Nb alloys are particularly sensitive to processing variables. By the addition of oxygen impurities or rapid solidification, droplet-shaped morphology was observed for some compositions, implying occurrence of a liquid-phase separation. The effects of impurities and cooling rates are analyzed in connection with a stable and metastable liquid miscibility gap, respectively.

Li, D.↗

Microstructural evolution in Cu-Nb processed via friction consolidation

Immiscible alloys, whether in well-mixed or layered forms, are of increasing interest based on their novel structural and functional properties, such as enhanced thermal stability against grain growth or radiation-induced defect trapping at the interfaces. To address the need for new approaches to tailor microstructures, the microstructural development of an immiscible Cu-Nb alloy processed via friction consolidation of elemental powders is investigated. Friction consolidation is a solid-phase processing technique that imparts severe plastic strain into a deforming volume resulting in elevated temperatures below the melting temperature of the alloy. Two distinct processing pathways were chosen to understand the effect of thermomechanical conditions on the final microstructure. The microstructure was characterized using scanning electron microscopy, scanning transmission electron microscopy, and X-ray diffraction techniques. Path 1 exhibited larger strain, strain rate, and temperature as compared with path 2. In path 1, agglomerated Nb particles were present in the recrystallized ultrafine-grained Cu matrix, while in path 2 extremely fine and dispersed Nb particles were present in a highly deformed Cu matrix. In both pathways, supersaturation of Cu in Nb lattices was noted, but not vice-versa. The asymmetry in mixing is explained based on deformation-based, thermodynamic and kinetic factors. These findings provide a pathway for creation of novel tailored microstructures and improved properties in any number of binary immiscible alloy systems.

Cu-Nb alloys, Microstructural refinement, Friction↗

Modes of strain accommodation in Cu-Nb multilayered thin film on indentation and cyclic shear

Two-phase layered thin films with a high density of semi-coherent interfaces exhibit excellent mechanical properties and thermal stability. Here, in this study, a magnetron-sputtered Cu-Nb dual-layered thin film (~500 nm for Cu and ~150 nm for Nb) having an amorphous interface between Cu and Nb with a high density of aligned growth twins in Cu is subjected to severe surface deformation. The material is loaded using indentation and cyclic shear under tribological testing. The strain accommodation in the subsurface microstructure after deformation varies based on the local structure and deformation mode. Grain refinement and crack formations in the stressed region of the Nb layer and localized crystallization of the amorphous interface are observed after indentation and scratch testing. Pronounced detwinning of growth twins in the Cu layer under the cyclic shear strain leaves large dislocations sites and loops which are observed both by high-resolution transmission electron microscopy and experiment-guided molecular dynamic (MD) simulations. Our simulations provided insights into understanding the pathway for the detwinning process under cyclic shear loading.

36 MATERIALS SCIENCE↗

In-situ TEM observation of shear induced microstructure evolution in Cu-Nb alloy

Phase boundaries in multiphase alloys govern defect interaction and chemical intermixing across different phases during plastic deformation. Dynamic interaction of defects with phase boundaries in multiphase alloys, especially for immiscible alloys, has been topic of significant research interest in recent years. In this work, we describe a novel approach for carrying out in-situ TEM shear deformation to directly observe interfacial microstructural evolution of a Cu-Nb alloy. A unique double shear specimen geometry is microfabricated by a focused ion beam technique to apply shear deformation upon push loading inside the TEM. From the real-time observation, we discover that the phase boundary with a zigzag morphology effectively blocks stacking faults nucleated in a Cu grain from slipping into a Nb grain. Meanwhile, the Cu phase bears the most plastic deformation through slip or twinning mechanisms. This work sheds light on understanding the shear deformation and the behavior of phase boundaries in multiphase alloys during shear deformation.

36 MATERIALS SCIENCE↗

Decoupling of strain and temperature effects on microstructural evolution during high shear strain deformation

The interplay between defect generation by shear strain and defect annihilation by local heating is difficult to predict in shear-assisted processing techniques. In this study, we decoupled the effects of high shear strain and external heating in an immiscible Cu-Nb alloy using a pin-on-disk tribometer to mimic the microstructural evolution of material during solid-phase processing. The change in sub-surface deformation, strain distribution, and redistribution of the second phase as a function of temperature were examined using transmission electron microscopy and atom probe tomography. Zener-Hollomon parameter is used to semi-quantify the deformation of Cu-Nb alloys as a function of strain and temperature.

36 MATERIALS SCIENCE↗

The kinetics of composite particle formation during mechanical alloying

The kinetics of composite particle formation during attritor milling of insoluble binary elemental powders have been examined. The effects of processing conditions (i.e., mill power, temperature, and charge ratio) on these kinetics were studied. Particle size distributions and fractions of elemental and composite particles were determined as functions of milling time and processing conditions. This allowed the deduction of phenomenological rate constants describing the propensity for fracture and welding during processing. For the mill-operating conditions investigated, the number of particles in the mill generally decreased with milling time, indicating a greater tendency for particle welding than fracture. Moreover, a bimodal size distribution is often obtained as a result of preferential welding. Copper and chromium 'alloy' primarily by encapsulation of Cr particles within Cu. This form of alloying also occurs in Cu-Nb alloys processed at low mill power and/or for short milling times. For other conditions, however, Cu-Nb alloys develop a lamellar morphology characteristic of mechanically alloyed two-phase ductile metals. Increasing mill power or charge (ball-to-powder weight) ratio (CR) increases the rate of composite particle formation.

Aikin, B. J. M.↗

Liquidus Temperatures and Solidification Behavior in the Copper-Niobium System

The copper-niobium phase diagram has been under active debate; thus, a corroboratory experimental study is needed. In this investigation, the melts of Cu-Nb alloys at compositions ranging from 5 lo 86 wt% Nb were processed in different environments and solidified at relatively low rates of 50-75 C/s to determine liquidus temperatures and to study solidification behavior. For all samples processed under very clean conditions, only Nb dendrites in a Cu matrix were observed; while in the presents of oxygen impurities, the alloys containing 5-35 wt% Nb exhibited microstructure of Nb-rich spheroids and Nb dendrites in the Cu matrix. The results obtained from clean conditions are in fair agreement with the Cu-Nb phase diagram having an S-shaped, near-horizontal appearances of the liquidus. The formation of Nb-rich droplets at slow cooling rates is discussed in terms of a stable liquid miscibility gap induced by oxygen.

Li, D.↗

Liquidus Temperatures and Solidification Behavior in the Copper-Niobium System

The copper-niobium phase diagram has been under active debate; thus, a corroboratory experimental study is needed. In this investigation, the melts of Cu-Nb alloys at compositions ranging from 5 to 86 wt pct Nb were processed in different environments and solidified at relatively low cooling rates of 50 to 75 C/s to determine liquidus temperatures and to study solidification behavior. For all samples processed under very clean conditions, only Nb dendrites in a Cu matrix were observed; while in the presence of oxygen impurities the alloys containing 5 to 35 wt pct Nb exhibited microstructure of Nb-rich spheroids and Nb dendrites in the Cu matrix. The results obtained from clean conditions are in fair agreement with the Cu-Nb phase diagram having an S-shaped, near-horizontal appearance of the liquidus. The formation of Nb- rich droplets at slow cooling rates is discussed in terms of a stable liquid miscibility gap induced by oxygen.

Li, D.↗

The Impact of Rolling at Temperature on Conductivity and Texture in Nanolamellar Cu/Nb Bimetallic Composites

We report warm rolling is used to identify whether reductions in dislocation content would provide a significant impact on conductivity in accumulatively roll-bonded Cu-Nb nanolaminates. In addition, the impact of temperature on mechanical properties and interfacial texture is also quantified. Although temperature has a strong effect on dislocation content and mechanical properties, it is shown that length scale and volume fraction are most critical to defining the conductivity of the nanolaminate. Rolling at temperature reduced the flow stress of the material while maintaining the interfacial and layer structure, indicating that warm rolling can increase the ability to process the nanolaminates without reducing conductivity.

36 MATERIALS SCIENCE↗

Mechanical Property Evaluation of CuNb Composites Manufactured with High-Pressure Torsion

Copper is under consideration as the optimum material for both high heat flux applications and high pulsed magnets. One challenge is that copper has low strength which is problematic to deployment in these applications. One solution is to alloy copper with BCC elements to improve its mechanical properties. However, the limited solubility of the BCC elements in copper requires high deformation processes to be used in order to manufacture these 3D composites. Here, high energy ball milling combined with high pressure torsion was used to manufacture 3D Cu-Nb composites. After the consolidation the mechanical properties of the composites were measured using micro- and nanohardness testing at room and elevated temperature. The results indicated that after 10 turns during the high-pressure torsion consolidation, the mechanical properties of the composites were completely saturated displaying uniform properties across the manufactured disk. Performing the high pressure torsion at temperature further improved consolidation of the disk. The high temperature nanoindentation also indicated a change in the deformation mechanism between 200 and 500 ºC.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Heterogenous activation of dynamic recrystallization and twinning during friction stir processing of a Cu-4Nb alloy

An interplay between high degree of shear deformation and deformation-induced heating occurs during friction stir processing (FSP) of metals. In medium-to-low stacking fault energy Cu alloys, this can lead to a complex spatially heterogenous activation of dynamic recrystallization (DRX) and twinning mechanisms. Within the Cu-Nb system, the presence of Nb is further expected to influence the DRX mechanism of the Cu matrix. However, the microstructural changes induced by the co-deformation of Nb during FSP are still not well understood. So, this study uses a combination of multimodal microstructural characterization, solution thermodynamics-based predictions, and computational crystal plasticity simulation to reveal the various microstructural evolution mechanisms that can occur during FSP of a Cu-4at.%Nb binary model alloy. The formation of softer DRX zones, and harder shear localization regions are revealed using electron backscatter diffraction, transmission electron microscopy, atom probe tomography, and crystal plasticity modeling.

36 MATERIALS SCIENCE↗

Fragmentation of the edge of a terminated Cu nanolayer within a Nb matrix upon annealing

Here, we investigate the evolution of the tip of a terminated Cu nano-layer embedded within a Nb matrix upon annealing at 800°C. The tip of the terminated Cu layer fragments progressively into a series of single-crystal Cu particles upon continued annealing. This finding shows that layer fragmentation is the second step, after layer pinchoff, in the thermal coarsening of nanolayered metal composites. Comparison to prior phase-field modeling permits us to infer that the mobility at 800°C of Cu-Nb, as modeled by the Cahn-Hillard equation, is M(c)=(M 0 = 7.3 ± 3.6 nm 5 / s • eV) |1 – c 2 |, where the order parameter, c, is 1 for Cu and -1 for Nb.

36 MATERIALS SCIENCE↗

Electrical resistivity of composite superconductors

In addition to its superconducting properties, a superconductor is usually characterized by poor thermal conductivity and relatively high electrical resistivity in the normal state. To remedy this situation a study of superconducting properties of Cu-rich CU-Nb wires prepared by directionally solidified and cold-rolled technique was conducted. Some of the specimens were prepared by melting, directional solidification and diffusing in Tin. A total of 12 wire specimens was tested. Each specimen was analyzed by plotting experimental data into the following curves: the graph of the residual resistivity as a function of the specimen current at 4.3 K; and the graph of the electrical resistivity as a function of the temperature at a constant current.

Davis, J. H.↗

Materials Data on Nb3Cu by Materials Project

CuNb3 is alpha bismuth trifluoride structured and crystallizes in the cubic Fm-3m space group. The structure is three-dimensional. there are two inequivalent Nb sites. In the first Nb site, Nb is bonded in a distorted body-centered cubic geometry to four equivalent Nb and four equivalent Cu atoms. All Nb–Nb bond lengths are 2.80 Å. All Nb–Cu bond lengths are 2.80 Å. In the second Nb site, Nb is bonded in a 8-coordinate geometry to eight equivalent Nb and six equivalent Cu atoms. All Nb–Cu bond lengths are 3.24 Å. Cu is bonded in a distorted body-centered cubic geometry to fourteen Nb atoms.

36 MATERIALS SCIENCE↗