The fabrication of high strength Zr/Nb nanocomposites using high-pressure torsion
Introduction
In order to enhance the mechanical properties of metals, various elements may be mixed in a controllable way to form composite structures [[1], [2], [3]] and the mixture can then be tuned so that the required properties of the composite are enhanced and may even surpass the properties of the comprising elements [2,4]. In recent years, bimetallic composites have attracted considerable attention as they exhibit enhanced strength, hardness and plastic properties even under extreme conditions as well as resistance to shock and radiation damage compared to the constituent materials in bulk form. Examples of these composites include Al/Cu, Cu/Nb, V/Ag, etc. [[5], [6], [7], [8], [9], [10], [11], [12]].
To date, most of the research interest in metallic composites has focused on using combinations of crystal structures of bcc/fcc, fcc/fcc and bcc/bcc materials [[13], [14], [15], [16], [17], [18], [19]] but recently there has been an interest in developing cubic/hcp combinations [[20], [21], [22], [23], [24], [25]]. Considering the Zr/Nb system, it is well-known that zirconium and zircalloys are widely employed in the nuclear industry due to their small capture cross-section for thermal neutrons, their relatively good high temperature strength and their resistance to corrosion [26]. Therefore, it is reasonable to anticipate that Zr/Nb bimetallic nanoscale composites may be promising candidate materials for use in the nuclear industry due to the development of intrinsic highly efficient interfaces which will protect these materials against radiation damage [27,28].
Metallic composites of this type are generally obtained by using deposition methods such as magnetron sputtering [29] and already there is a report of the preparation of Zr/Nb nano-multilayers using this procedure [26]. Nevertheless, the relatively low deposition rate and the overall complexity of the equipment that is needed for this synthesis technique make this type of processing difficult for the fabrication of large volumes of material. Mechanical alloying (MA) is also a potential approach for preparing these composites [5] but a simpler and more direct procedure is through the use of a severe plastic deformation (SPD) technique such as high-pressure torsion (HPT) where this procedure is now routinely used to produce bulk nanostructured metallic materials [30]. Processing by HPT has been employed recently to produce nanostructured intermetallics and metal matrix composites and the results have shown that the procedure provides the potential for achieving true nanostructures [[31], [32], [33], [34], [35]]. Non-equilibrium phases, such as supersaturated solid solutions [36], may be formed using this procedure and the resultant mechanical properties are enhanced due both to the significant grain refinement and to the intensive introduction of point and line defects during processing [37].
An earlier report described the fabrication of a Zr/Nb composite using two semi-circular sections of a disk which were placed together to form a single whole disk within the HPT facility [5]. Processing by HPT produced an ultrafine-grained structure with grain sizes of less than 100 nm and a supersaturated solid solution with a hardness of up to 500 Hv at the disk edge after 100 turns of HPT [5]. In practice, most reports on the fabrication of bulk Zr/Nb composites have used the technique of accumulative roll bonding (ARB) [[38], [39], [40], [41]] and very limited information is at present available on the effect of heavy shear strains on the fabrication of bulk Zr/Nb composites when using the HPT technique. Furthermore, the early study using HPT produced a Zr/Nb composite by taking two semi-circular disks [5] and this is similar to early reports for other materials using two semi-circular disks [42] or four quarter disks [43], respectively. More recent experiments have been conducted differently by stacking whole disks in a sandwich-like configuration [31] where this procedure provides a better opportunity for evaluating the significance of mixing during the HPT process.
The only report on the HPT processing of a Zr/Nb composite available to date has limitations due to the necessity of cutting semi-circular Zr and Nb disks [5]. Accordingly, the present research was initiated to develop a novel and compact approach for making Zr/Nb composites by stacking Nb/Zr/Nb disks in a sandwich-like structure for the HPT processing. Therefore, a comprehensive investigation was conducted to examine the production, microstructure and the microhardness of a Zr/Nb composite after processing at room temperature. The results demonstrate the potential for using HPT for the fabrication of nanocomposites having exceptionally high levels of hardness.
Section snippets
Experimental material and procedures
The materials used in this study were commercial purity Zr and Nb rods purchased from Goodfellow (Cambridge, UK). Both the as-received Zr and Nb rods were in an annealed state. Disk-shaped samples with diameters of 9.9 mm and thicknesses of 0.85 mm were cut from the as-received Zr and Nb rods. A Zr disk was stacked on the lower anvil of the HPT facility contained between two Nb disks in a sandwich-like configuration where both the upper and lower anvils had central depressions with diameters of
Experimental results
Fig. 1 shows OM images of the cross-sectional areas of the Nb/Zr/Nb stacks after processing through 10, 20, 50, 80 and 100 turns, respectively. These images provide clear evidence for the gradual evolution of a nanocomposite. Initially there is a layered structure of Nb/Zr/Nb after 10 turns in Fig. 1(a) with the two elements well-defined in the image. As the numbers of turns increases to 20, as shown in Fig. 1(b), the initial layered structure becomes fragmented close to the disk edge but an
Discussion
In the HPT procedure, a disk is processed under a high compressive pressure with concurrent torsional straining and this is generally, but not always, conducted at room temperature. In practice, the large hydrostatic pressure which is an inherent feature of HPT processing is effective in leading to the successful processing of difficult-to-deform materials [48] that may be prone to segmentation and cracking when processing using other SPD techniques [49,50]. The physical and mechanical
Summary and conclusions
- 1.
By using a sandwich-like stacking of Nb/Zr/Nb disks, a Zr/Nb composite was successfully fabricated using processing by high-pressure torsion at ambient temperature. Processing through 100 turns of HPT gave a fully-mixed Zr/Nb composite with a large fraction of grains lying in the range of ~20–40 nm.
- 2.
The intermixing of the Zr/Nb layers increased with increasing numbers of imposed revolutions from 10 to 100 turns and with increasing radial position on the disks. After 100 turns, the material was
Data availability
The raw/processed data required to reproduce these findings cannot be shared at this time as the data also forms part of an ongoing study.
CRediT authorship contribution statement
Dan Luo: Investigation, Data curation, Formal analysis, Writing - original draft. Teodor Huminiuc: Investigation, Data curation, Formal analysis. Yi Huang: Data curation, Formal analysis, Supervision, Writing - review & editing. Tomas Polcar: Supervision, Writing - review & editing. Terence G. Langdon: Supervision, Writing - review & editing.
Declaration of competing interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgements
This work was supported by the European Research Council under ERC Grant Agreement No. 267464-SPDMETALS. The electron imaging was performed with the support of the South of England Analytical Electron Microscope (EP/K040375/1) within the David Cockayne Centre for Electron Microscopy, Department of Materials, University of Oxford. Additional support was provided by the Henry Royce Institute (EP/R010145/1) and CEITEC Nano Research Infrastructure (ID LM2015041, MEYS CR, 2016–2019) and CEITEC Brno
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