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PROGRESS ARTICLE RUSLAN VALIEV Institute of Physics of Advanced Materials,Ufa State Aviation Technical University,12 K.Marx str.,Ufa 450000,Russia e-mail: RZValiev@mail.rb.ru It has been over 20 years since Herbert Gleiter presented the first concepts for developing nanocrystalline materials (that is,ultrafine-grained materials with a grain size under 100 nm) with special properties1. Since then, the field of nanostructured materials has developed rapidly,owing to tremendous interest in this topic of scientific and technological importance. Gleiter’s original idea was that owing to a very small grain size,nanocrystalline materials contained an extremely large fraction of grain boundaries with a special atomic structure.As a result,nanomaterials should have unusual properties2.As regards mechanical properties,one could expect very high strength, toughness, fatigue life and wear resistance. Nanostructuring seemed likely to lead to a revolutionary use of nanomaterials for many functional and structural applications.But these interesting prospects were put in jeopardy. Numerous investigations3–5 showed that although nanocrystalline materials did demonstrate very high strength or hardness, they were of very low ductility or even brittle,producing insuperable problems for advanced structural applications.When addressing the reasons for the low ductility,many researchers point out drawbacks in their synthesis based on compacting of nanopowders,obtained using various methods4,5. Nanomaterials produced by compacting usually have residual porosity,contaminations and,as a rule, small geometric dimensions.All this may lead to a decline in their ductility.Another possible reason is of fundamental nature: the plastic deformation mechanism associated with generation and movement of dislocations may not be effective in ultrafine grains (see below).In this connection,recent findings of nature materials | VOL 3 | AUGUST 2004 | www.nature.com/naturematerials 511 Nanostructuring of metals by severe plastic deformation for advanced properties Despite rosy prospects, the use of nanostructured metals and alloys as advanced structural and functional materials has remained controversial until recently. Only in recent years has a breakthrough been outlined in this area, associated both with development of new routes for the fabrication of bulk nanostructured materials and with investigation of the fundamental mechanisms that lead to the new properties of these materials. Although a deep understanding of these mechanisms is still a topic of basic research, pilot commercial products for medicine and microdevices are coming within reach of the market. This progress article discusses new concepts and principles of using severe plastic deformation (SPD) to fabricate bulk nanostructured metals with advanced properties. Special emphasis is laid on the relationship between microstructural features and properties, as well as the first applications of SPD-produced nanomaterials. ××××××××××××××××× P P Plunger Work piece Plunger Support Sample Die ba Φ Figure 1 Principles of severe plastic deformation techniques.a,High-pressure torsion:a sample is held between anvils and strained in torsion under applied pressure (P ).b,Equal channel angular pressing: a work-piece is repeatedly pressed through a special die. nmat1180-FINAL 7/13/04 10:24 AM Page 511 © 2004 Nature Publishing Group PROGRESS ARTICLE extraordinarily high strength and ductility in several bulk ultrafine-grained metals are especially interesting6–9.However,various nanomaterials possess microstructural features closely linked to processing methods and regimes.Therefore we should first briefly address the principles of processing techniques and the structural features of processed materials. BULK NANOSTRUCTURED MATERIALS Earlier studies focused on fabricating nanostructured materials by inert gas condensation1,2.This technique makes it possible to produce ultrafine grains with a size refined down to 10 nm.On the other hand, it has well- known limitations — overall sample dimensions are small (only up to 10 mm in diameter and up to 1 mm in thickness for a typical disc-shaped sample) and some porosity remains.High residual porosity and contaminations are also inherent drawbacks in samples obtained by consolidation of nanopowders produced by ball-milling or mechanical alloying5. Recent years have therefore seen growing interest in a new approach to fabrication of bulk nanostructured metals and alloys, as an alternative to nanopowder compacting. This approach is based on microstructure refinement in bulk billets using severe plastic deformation (SPD): that is, heavy straining under high imposed pressure10. SPD-produced nanomaterials are fully dense and their large geometric dimensions make it possible to perform thorough mechanical tests. Fabrication of bulk nanostructured materials by severe plastic deformation is becoming one of the most actively developing areas in the field of nanomaterials11,12. Since the pioneering work on tailoring of ultrafine- grained structures by SPD processing13,14, two SPD techniques have attracted close attention and have lately experienced further development.These techniques are high-pressure torsion (HPT) and equal channel angular (ECA) pressing (Fig. 1). Samples processed under HPT are disc-shaped (Fig.1a). In this process, the sample,with a diameter ranging from 10 to 20 mm and thickness of 0.2–0.5 mm,is put between anvils and compressed under an applied pressure (P) of several GPa.The lower anvil turns,and friction forces result in shear straining of the sample.As a result of high imposed pressure, the deforming sample does not break even at high strains10. Essential structure refinement is observed after deformation through one-half or one complete (360°) turn.But to produce a homogeneous nanostructure, with a typical grain size of about 100 nm or less, deformation by several turns is necessary (Fig. 2). The important role of applied pressure in the formation of a more homogeneous nanostructured state during HPT is also shown in recent work on nickel15. During ECA pressing,the ingot is pressed in a special die through two channels with equal cross- section16,17, intersecting usually at an angle Φof 90° (Fig.1b).Here each pass imparts a supplementary strain of about 1.Among new trends in ECA pressing,there is processing of hard-to-deform materials which can be realized using back pressure or with increased channel intersection angles, that is,Φ> 90°.Experimental and theoretical modelling of the mechanics of ECA pressing, focusing on the stress-deformed state,contact stresses and friction conditions16,18,has made it possible to construct ECA pressing dies for processing of larger billets with uniform ultrafine grains out of various metals, including hard-to-deform titanium and its alloys19.Titanium billets up to 60 mm in diameter and 200 mm long have been successfully processed. Another new direction is the fabrication of long-length semi-products (rods,sheets) using continuous ECA pressing,or other SPD techniques such as accumulative roll bonding or repetitive corrugation and straightening11,12.This is an important step for successful commercialization of nanostructured metals. Strong refinement of microstructure by ECA pressing is fairly easy to achieve both in pure metals and in alloys,using straining with one pass or a few.But it remains a special problem to produce ultrafine-grained structures by this technique.For success,many more passes should be made (as a rule,eight or more; Fig.2b), and optimal processing routes and regimes should be determined.The final size of grains produced by ECA pressing depends on the material under investigation and on processing features,but for pure metals it is typically200–300 nm. The size and shape of ultrafine grains are important but not the only features of the structure of SPD- processed metals.As we demonstrate below,the structure of grain boundaries is an essential feature for attaining new properties.Early work on ultrafine- grained metals produced by SPD13 has aimed at formation of predominantly high-angle grain boundaries.This,however, is possible only at large accumulated strains ≥ 6–8.Modern diffraction methods,such as orientation imaging microscopy or back electron scattering diffraction,provide evidence of the presence of up to 70–80% of high-angle boundaries in the microstructure of samples subjected to multipass ECA pressing or HPT with five or more revolutions at relatively low temperatures (usually less than 0.3Tm; where Tm is the melting point in K)12,20. Among other important features of the microstructure of SPD metals, special emphasis should be laid on the appearance of a crystallographic texture21 and the presence of high internal stresses caused by high density of dislocations inside the grains and at their boundaries10.Formation of non-equilibrium grain boundaries containing numerous grain-boundary dislocations is an immediate consequence of severe straining,but it can be controlled by subsequent annealings or special thermomechanical treatments,or both.For instance,observations22 of HPT-processed titanium by transmission electron microscopy and 512 nature materials | VOL 3 | AUGUST 2004 | www.nature.com/naturematerials Figure 2TEM images of ultrafine-grained copper. a, Copper processed by HPT at room temperature (P = 6 GPa, five turns). b, Copper processed by ECA pressing (12 passes). a b 200 nm200 nm nmat1180-FINAL 7/13/04 10:24 AM Page 512 © 2004 Nature Publishing Group PROGRESS ARTICLE high-resolution electron microscopy revealed (Fig.3) that the grain boundaries are not well defined,but are wavy,curved or corrugated (Fig. 3c), indicating the presence of numerous atomic defects.Moreover, there is a variation in the misorientation angle along the same boundary by about 5°,probably as a result of the presence of disclinations. However,observations after annealing at 250–300 °C (this is below the temperature at which any grain growth can start) revealed a rearrangement of dislocations: they had moved from the grain interiors to the region near the grain boundaries.A schematic illustration of the defect rearrangement is presented in Fig.4.The figure emphasizes that although the total density of dislocations is decreased during low- temperature annealing, the local density of dislocations at grain boundaries can grow,thus increasing their non-equilibrium,and this may have a strong effect on grain-boundary processes such as sliding,diffusion or interaction with lattice dislocations23.Hence recent investigations show that ultrafine-grained metals produced by SPD possess a complex microstructure. Their microstructural features are conditioned by processing routes and regimes.These features should be taken into consideration when developing bulk nanostructured materials with improved properties. ENHANCED PROPERTIES IN SPD-PRODUCED NANOMATERIALS It is well known that grain refinement promotes mechanical strength, and thus one can expect ultrafine-grained materials to possess very high strength. Moreover, introduction of a high density of dislocations in SPD-processed nanometals may result in even greater hardening. However, all this normally decreases ductility. Strength and ductility are the key mechanical properties of any material, but they are typically opposing characteristics. Materials may be strong or ductile,but rarely both at once.Recent studies have shown that material nanostructuring may lead to a unique combination of exceptionally high strength and ductility (Fig. 5), but this task calls for original approaches6–9. One such new approach to the problem was suggested recently by Wang et al.8.They created a nanostructured copper by rolling the metal at low temperature — the temperature of liquid nitrogen — and then heating it to around 450 K.The result was a ‘bimodal’structure of micrometre-sized grains (at a volume fraction of around 25%) embedded in a matrix of nanocrystalline grains.The material showed extraordinarily high ductility,but also retained its high strength.The reason for this behaviour is that,while the nanocrystalline grains provide strength, the embedded larger grains stabilize the tensile deformation of the material.Other evidence for the importance of grain- size distribution comes from work on zinc24,copper25 and aluminium alloy26.What is more, the investigation of copper25 has shown that bimodal structures can increase ductility not only during tensile tests,but also during cyclic deformation.This observation is important for improving fatigue properties. Another approach suggested recently4 is based on formation of second-phase particles in the nanostructured metallic matrix,which are to modify shear-band propagation during straining, thereby increasing the ductility.A systematic study of both hard and soft second-phase particles with varying sizes and distributions is required here, to allow mechanical properties to be optimized. A third approach to the problem of strength and ductility is probably the most universal of the three, because it can be applied both for metals and for alloys.The approach is based on formation of ultrafine-grained structures with high-angle and non-equilibrium grain boundaries capable of grain- boundary sliding (GBS)6,10. It is well known that sliding, which increases ductility,normally cannot develop at low-angle boundaries.The importance of high-angle grain boundaries was verified in work6 on the nature materials | VOL 3 | AUGUST 2004 | www.nature.com/naturematerials 513 a b c 500 nm 0.295 nm A A B 5° 2 nm 200 nm Figure 3Typical images of microstructure of HPT-processed titanium.a,Bright-field transmission electron micrograph (with the selected- area diffraction pattern as an inset).b,Dark-field transmission electron micrograph.c,High- resolution electron micrograph demonstrating highly distorted grain boundaries in this as- processed metal.This is associated with the high distortion of the crystal lattice and a variation in the misorientation angle (see the region in the white rectangle and the position of the lines A,A and B). a b Figure 4 Arrangement of grain boundaries in nanostructured titanium. a,The dislocation structure after HPT processing. b,The dislocation structure after HPT and low-temperature annealing leading to formation of non-equilibrium grain boundaries. nmat1180-FINAL 7/13/04 10:24 AM Page 513 © 2004 Nature Publishing Group PROGRESS ARTICLE mechanical behaviour of metals subjected to different degrees of severe plastic deformation resulting in formation of various types of grain boundaries.As was noted above,sliding can be easier when non- equilibrium boundaries are present.Another example of this is the extraordinary influence of annealing temperature on mechanical behaviour found recently in nanostructured titanium produced by HPT22.Here a short annealing at 300 °C results in a noticeable increase in strength combined with greater ductility than in the HPT-produced state or after annealing at higher temperature.The growth of strength and ductility was associated with higher strain-rate sensitivity of flow stress.An increased strain-rate sensitivity has also been reported in other works investigating high strength and ductility in nanometals6,10,27.High strain-rate sensitivity indicates viscous flow and plays a key role in superplasticity in materials28,but on the other hand it is associated with the development of grain-boundary sliding,and therefore depends on grain-boundary structure.Thisfact is in agreement with the recent results of computer simulation and studies of deformation mechanisms active in nanostructured metals.Such molecular dynamics simulations have provided valuable insight into the deformation behaviour of nanometals29–31. For coarse-grained metals,dislocation movement and twinning are well-known primary deformation mechanisms.But the results of simulation show that ultrafine grains may also aid in specific deformation mechanisms such as grain-boundary sliding or nucleation of partial dislocations30–33.Moreover, the sliding may have a cooperative (grouped) character similar to that observed in earlier studies on superplastic materials34,35. It should be stressed that recent experiments investigating deformation mechanisms in nanostructured materials have confirmed a number of the results of computer simulation22,36,37. However, there is a question: why should grain- boundary sliding in nanostructured materials, in particular in those produced by SPD,take place at relatively low temperatures? GBS is a diffusion- controlled process and usually occurs at high temperatures.A possible explanation is that diffusion may be faster in SPD-produced ultrafine-grained materials with highly non-equilibrium grain boundaries.Experiments have shown that in SPD- produced metals the diffusion coefficient grows considerably (by two or three orders),and this is associated with non-equilibrium grain boundaries38,39. So perhaps grain-boundary sliding is easier in these ultrafine-grained metals and develops during straining even at lower temperatures,producing increased ductility. It is well known that enhanced sliding in nanostructured metals can lead even to superplasticity at relatively low temperatures40. Processing of nanomaterials to improve both strength and ductility is of primary importance for fatigue strength and fracture toughness25,41,42. An extraordinary increase in both low-cycle and high- cycle fatigue-strength may take place; there exists a theoretical explanation and the first experimental evidence of this interesting phenomenon41,42. It is interesting that the complex structure of SPD- processed materials can also result in multifunctional properties.For instance, the nanostructured TiNi alloy43 demonstrates an extraordinary combination of very high mechanical and functional properties: superelasticity and shape-memory effect.Such a combination makes the nanostructured TiNi alloy different in principle from its conventional (coarse- grained) counterpart.Engineering of multifunctional materials is becoming a new direction in the science of SPD nanomaterials. USING SPD-PRODUCED NANOSTRUCTURED METALS Markets for bulk nanostructured materials exist in virtually every product sector where superior mechanical properties (in particular, strength, strength-to-weight ratio and fatigue life) are critical. Formal market analyses, conducted by companies such as Metallicum that specialize in nanostructured metals, have identified over 100 specific markets for nanometals in aerospace, transportation, medical devices, sports products, food and chemical processing, electronics and conventional defence44. Among them we can single out the following directions: (1) development of extra-strong nanostructured light alloys (Al, Ti, Mg), for example Al-based commercial alloys with yield strength over 800–900 MPa, for the motor industry and aviation; (2) development of metals and alloys with ultrafine- grained structure for use at cryogenic temperatures45; (3) development of nanostructured ductile refractory metals and high-strength TiNi alloys with advanced shape-memory effect for space, medical and other applications. The applications of nanostructured materials in engineering of new-generation aviation engines46 or in high-strain-rate superplastic forming 514 nature materials | VOL 3 | AUGUST 2004 | www.nature.com/naturematerials Mo Mo Co Re Ti Cu Zr Ru Be 61% 37% 21% 11% 0 0 U Mg 75% 35% Al Pd Pt Th Ni V Ti Zr Ni Au Nb W Nanostructured Ti Nanostructured Cu FeTa 0 10 20 30 40 50 60 Elongaion to failure (%) 800 600 400 200 0 Yi el d st re ng th (M Pa ) Figure 5 Strength and ductility of the nanostructured metals compared with coarse-grained metals.Conventional cold rolling of copper and aluminium increases their yield strength but decreases their ductility.The two lines represent this tendency for Cu and Al and the % markings indicate a percentage on rolling. In contrast, the extraordinarily high strength and ductility of nanostructured Cu and Ti clearly set them apart from coarse- grained metals6. nmat1180-FINAL 7/13/04 10:24 AM Page 514 © 2004 Nature Publishing Group PROGRESS ARTICLE of complex-shaped parts for new automobiles and planes47 are worth a special mention. Out of the broad range of possible applications of advanced nanostructured metals,we focus here on one that is representative of the high-tech market: biomedical implants and devices.High mechanical and fatigue properties are the essential requirements for metallic biomedical materials, in particular titanium and its alloys48,which have excellent biological compatibility and high biomechanical properties. For example, in trauma cases,plates and screws made of new titanium materials are planned to be widely used for fixing bones.These plates need very high compressive and bending strength,and sufficient ductility.Different implant-plate constructions for osteosynthesis have been analysed,resulting in the design and processing of a series of nanostructured titanium plates (Fig. 6a,b). Figure 6c illustrates another application of nanostructured titanium for a special conic screw,which requires high fatigue strength as well. In this case all the advantages of nanostructured titanium are fully used49 — high static and fatigue strength (yield tensile strength ≥ 950 MPa at strain rate 10–3 s–1,endurance of more than 500 MPa at 2 × 107 cycles) and excellent biological compatibility. CONCLUSIONS Recent progress in fabricating bulk metallic materials using severe plastic deformation,and in understanding their fundamental mechanisms,probably brings us closer to the revolutionary use of nanomaterials for structural and functional applications.The atomic defect structure of SPD-processed metals is complex and is closely connected with the features of processing routes and regimes.Nevertheless, tailoring specific nanostructures (for example with bimodal grain-size distribution or ultrafine grains with high-angle and non-equilibrium grain boundaries) can produce unique combinations of properties, such as extraordinarily high strength and ductility,high fatigue life and toughness.These properties may be of great importance if nanostructured metals and alloys are to form the next generation of advanced structural and functional materials. doi:10.1038/nmat1180 Acknowledgements This work was supported partly by the Department of Energy NIS-IPP program at Los-Alamos National Laboratory, the Alexander von Humboldt Foundation research award and the Russian Foundation for Basic Research. 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