J. Mater. Sci. Technol. ›› 2020, Vol. 52: 29-62.DOI: 10.1016/j.jmst.2020.02.046
• Research Article • Previous Articles Next Articles
T. Zhanga,*(), H.W. Dengb, Z.M. Xieb,*(), R. Liub, J.F. Yangb, C.S. Liub, X.P. Wangb, Q.F. Fangb, Y. Xiongc
Received:
2019-12-20
Revised:
2020-02-01
Accepted:
2020-02-04
Published:
2020-09-15
Online:
2020-09-18
Contact:
T. Zhang,Z.M. Xie
T. Zhang, H.W. Deng, Z.M. Xie, R. Liu, J.F. Yang, C.S. Liu, X.P. Wang, Q.F. Fang, Y. Xiong. Recent progresses on designing and manufacturing of bulk refractory alloys with high performances based on controlling interfaces[J]. J. Mater. Sci. Technol., 2020, 52: 29-62.
Fig. 2. a) Effects of oxygen and nitrogen impurity contents on DBTT measured by three-point bending at 5?×?10-3?mm?s-1 for TFGR W-1.1TiC/H with oxygen contents ranging from 160 to 870 wt. ppm [75]; b) APM-reconstruction of a measured atom probe sample with a GB of 45° rotation angle and detailed view on the GB [76]; c) Fracture surface of Whipped with an overlaying O mapping showing O covering most grain boundaries [71].
Fig. 3. Stress-strain curves (outer fibre) of pure Mo-1.5Si and Mo-1.5Si with Y2O3 and ZrH2 addition at (a) room temperature and at (b) 538 °C (c) 816 °C and (d) 1093 °C [39].
Fig. 4. (a) Model structure of the W ?27 < 110> {525} general twin GB as viewed from the <110> direction. The dashed line denotes the position of the GB cleavage plane. Different colors represent different coordinates along the <110> direction. (b) Cleavage energy as a function of substitutional elements at different positions [95].
Fig. 5. Plots of the strengthening energy ESEXversus segregation energy EsegX for the 29 dopants in the ? 5(310) tilt GB. (a) based on lowest energy dopant site in GB and free surface (l-to-l approach); (b) based on Site 0 (m-to-s approach). Dopants in the white region (positiveEsegX) prefer to stay in the bulk. For dopants that segregate, those with negativeESEX(blue region) tend to strengthen the GB [96].
Fig. 6. TEM micrographs of the specimens after two extrusion passes at 800 °C (a) and three extrusion passes at 950 °C (b); The load-displacement curves at different testing temperatures for the ECAP-strained specimens [107].
Fig. 7. SEM-BSE images showing the microstructure of the as-received polycrystalline tungsten (a) and ECAE processed (4A) polycrystalline tungsten (b); Flexural stress-strain curves of (c) the as-received and (d) the ECAE processed (4A) polycrystalline tungsten at various test temperatures [109].
Fig. 8. Back scattered electron SEM images taken on the flow plane of the wrought tantalum: a) as-received low magnification, b) as-received high magnification, c) 4A wrought low magnification, d) 4A wrought high magnification, e) 4E wrought low magnification, f) 4E wrought high magnification. 4A and 4E wrought material processed at room temperature [108].
Fig. 9. Bright-field (a), dark-field (b) images and SAED (c) from HPT-W. Notice the high density of defects in the grains, and break-ups in the elongated grains. The SAED shows nearly continuous rings, with no obvious intensity concentration along the rings, indicating large-angle GBs [105].
Fig. 10. Tensile specimens of (a) W-0.5TiC-H2 elongated to approximately 160% and (b) W-0.5TiC-Ar elongated to approximately 55% at 1973 K and at the initial strain rate of 5 × 10-4 s-1. For the W-0.5TiC-H2 the crosshead was arrested on the way of deformation. W-0.5TiC-Ar is elongated uniformly but fractures abruptly at the elongation of 55% without necking [120].
Fig. 11. TEM bright-field images showing grain structures for (a) W-0.5TiC-H2 and (b) W-0.5TiC-Ar, Size distribution of grains in W-0.5TiC-H2 and W-0.5TiC-Ar [120].
Fig. 12. (A) The nanostructure stability map for tungsten based alloys at 1100 °C. Pre- and post-annealing structures of tungsten powders after one week at 1100 °C. (B) The grain size histograms reveal only a minor change in the W-20 at.% Ti alloy after prolonged annealing and an almost two-orders-of-magnitude coarsening in unalloyed W. (C) The bright-field transmission electron microscopy (TEM) image shows a uniform distribution of nanometer-sized grains in the as-milled structure of the W-20 at.% Ti alloy, with the dark-field TEM image (inset) showing different diffracting crystallites. The post annealing structures vary with alloying: (D) a coarsened grain structure in unalloyed W, presented in a focused ion beam image, and (E) a retained nanocrystalline structure in W-20 at.% Ti, shown in a bright-field TEM image with a dark-field TEM (inset) [110].
Fig. 13. Chemical analysis of the annealed W-20 at.% Ti alloy. (A) Scanning TEM imaging shows the darker contrast from a heavier element and the brighter contrast from a lighter element. (B) The W-Ti elemental map confirms a nanoscale heterogeneous structure instead of a more homogeneous solute distribution expected from bulk thermodynamics. (C) The Ti compositional line scan across the three larger W-rich regions indicated by the yellow line in (A) further illustrates Ti atoms being depleted at the W-rich grain centers. The entire volume is apparently polycrystalline BCC structure, although with nanoscale composition gradients [110].
Fig. 14. (a) SEM in backscatter mode reveals a chromium-rich phase forming necks between the compact particles on heating up to 1200 °C (scale bar, 500 nm). (b) A direct visualization of a Cr-rich neck adjacent to W-rich particles is shown in the bright-field TEM image with W and Cr elemental maps (superimposed on the micrograph) using scanning TEM with energy dispersive spectroscopy (STEM-EDS) (scale bar, 200 nm), (c) SEM image of a bulk (6 × 4 mm right cylinder) nanocrystalline W-Ti-Cr alloy shows a grain size of about 100 nm at nearly full density (scale bar, 100 nm) [122].
Fig. 15. (a) SEM image showing the fracture surface of high dense bulk nano structured WYT, (b) the size distribution in this nano structured WYT, (c)-(d) TEM images showing the size and distribution of nano particles in this WYT, and (e)-(f) histograms showing the size distributions of intragranular and intergranular nano particles, respectively. (g) Hardness of the present nano structured WYT, and comparison with other reported W-based alloys; (h) High resolution TEM image showing the nanocrystalline in W5Y5T after high energy ball milling [124].
Fig. 16. (left) Bright-field TEM micrographs of UFG and NC tungsten irradiated with 2 keV helium ions (flux of 3.3 × 1016 ions m-2 s-1) at 1223 K demonstrating: (a) overview of sample with bubbles decorating GBs at a fluence of 3.6 × 1019 ions m-2; (b) nanocrystalline grain with large facetted bubbles/voids on GBs and few bubbles in the grain matrix at a fluence of 3.6 × 1019 ions m-2; and (c) GB and (d) GB triple-junction decorated by facetted bubbles with different sizes inside ultrafine grains at fluence of 4.0 × 1020 ions m-2. Bubble areal density (right columns) and average bubble size (left columns) versus grain size for 2 keV helium ions irradiation at 1223 K and a fluence of 3.6 × 1019 ions m-2. Bubbles located on GBs were not counted. A total of 18 neighboring grains were analyzed in order to ensure maximum consistency in ion fluence, sample thickness and irradiation temperature [132].
Fig. 17. TEM bright-field micrograph of as-deposited 40 nm Cu/40 nm Nb. Note selected area diffraction pattern showing {111}Cu//{110}Nb interface texture. Compression curves for 5 nm Cu/Nb multilayers. Note the high rate of work hardening up to a maximum flow stress of 2.4 GPa, followed by apparent work softening to failure at 26% true plastic strain [138].
Fig. 18. Cross section TEM (XTEM) images of as-deposited (a) Cu/V 50 nm, and (b) Cu/V 2.5 nm nanolayers. Films with smaller individual layer thickness (h) have a stronger Cu{111} and V{110} fiber texture. (c) and (d) Peak damage regions of irradiated Cu/V 50 nm and Cu/V 2.5 nm nanolayers, respectively. He bubbles are observed in both Cu and V. (e) Comparison of He bubble density distributions along film normal direction underneath the surface in ion irradiated Cu/V 2.5 nm and Cu/V 50 nm nanolayers. Peak He bubble density is reduced by a factor of ~3 in Cu/V 2.5 nm,compared to that in Cu/V 50 nm specimens. (f) Swelling vs. 1/h in ion irradiated Cu/V nanolayers, where h is individual layer thickness, shows a continuous swelling reduction with decreasing layer thickness [143].
Fig. 19. (a) Schematic for pure V and V-graphene nanolayers with repeat layer spacing (λ) of 110 nm and 300 nm. (b) Stress-strain curve determined from nanopillar compression testing of pure V, and V-graphene nanolayers with 110 nm and 300 nm repeated layer spacings. (c) SRIM ion trajectories of He+ irradiation on V thin film under condition of 120 keV [149].
Fig. 20. Transmission electron microcopy micrographs displaying the planar Cu-Nb interfaces after (A) extreme plastic strains of ~12, which produces an h = 20 nm composite, (B) elevated temperatures of 500 °C, which is 0.45 times the melting temperature of Cu (32), and (C) helium-ion irradiation, showing no voids in the layer or in the interfaces in an h = 20 nm composite, (D) the high-resolution transmission electron microscopy micrographs of the preferred Cu-Nb interface [150].
Fig. 22. Representative TEM images obtained for nanolamellar Cu/Ta multilayers prepared via CARB for different individual layer thicknesses h: (a) h =230 nm, (b) h = 110 nm, (c) h =50 nm [62].
Fig. 23. (a) Bulk tensile stress-strain curves for the CARB Cu/Ta nanolamellar multilayers; (b)Average nanohardness versus 1/h 1/2 for the CARB Cu/Ta nanolamellar multilayers; (c) Variation of the nanohardness after an annealing at elevated temperatures for the sample with a layer thickness h =50 nm [62].
Fig. 24. SEM cross-sectioning images of the CARB Cu/V multilayer composite with controlled individual layer thickness h: (a) h =38.0 μm, (b) h =19.0 μm, (c) h =9.0 μm, and (d) h =4.0 μm. EBSD-based inverse pole figure (IPF) maps (h =9.0 μm) for (d) Cu layers and (e) V layers, respectively. (g) EDS-mapping image of layer thickness h =4.0 μm nanocomposites after 3-6 rolling cycles, corresponding to an average layer thickness of 38.0, 19.0, 9.0, and 4.0 μm, respectively [141].
Fig. 25. A typical layer morphology and interface structure of Cu/V nanocomposite with individual layer thickness h =25 nm. (a) Typical bright field TEM image exhibiting single crystal layers with extremely high-aspect-ratio grains. (b) Representative HRTEM image of the predominant interface in the 25 nm CARB material, which is atomically ordered and sharp [141].
Fig. 26. High strength and thermal stability of the bulk Cu/V nanocomposite. (a) Average nanohardness versus h-1/2, showing that strength increases with decreasing layer thickness by the Hall-Petch scaling law. (b) Hardness reduction as a function of annealing temperature exhibiting outstanding thermal stability of CARB Cu/V nanolamellar nanocomposite [141].
Fig. 27. High magnification TEM images of an He implantation zone with depth ranging from surface to 600 nm: (a) microstructure with small size He bubbles and limited damage region after He implantation with fluence of 2 × 1021 ions/m2, (b) microstructure with large size He bubbles accompanied with grain boundary grooving after He implantation with fluence of 7 × 1022 ions/m2 [144].
Fig. 28. (a) Grain size in the pure Mo, Mo-0.5 wt. %La2O3, Mo-1.5 wt. %La2O3 and Mo-2.0 wt. %La2O3, and (b)-(e) Sketches illustrating the fracture process of the pure Mo, Mo-0.5 wt. %La2O3, Mo-1.5 wt. %La2O3 and Mo-2.0 wt. %La2O3 [161].
Fig. 29. (a) Comparison of room-temperature tensile behaviour for three different types of Mo alloys: tensile engineering stress-strain curves of CP-Mo with grain size D ~100 μm, ODS-Mo alloy with grain size D ~2.5 μm and oxide particle size d~1.2 μm, and NS-Mo alloy with grain size D ~0.5 μm and oxide particle size d ~80 nm Comparison of (L-L) mixing and liquid-solid (L-S) mixing processes and resulting microstructures: (b) Schematics showing the microstructural development in the L-S mixing/doping (c) and L-L mixing/doping processes that produced the ODS-Mo and NS-Mo alloys, respectively [166].
Fig. 30. SEM images and size distribution histograms for visible dark Y2O3 particles of (a) SPSed W-Y2O3, (b) sintered W-Y2O3 in flowing H2 and (c) deformed W-Y2O3 [178].
Fig. 32. Damage characteristics of the investigated materials after thermal loading with 100 pulses at 0.6 GW/m2 for 1 ms at RT. (a) the loaded surface of SPSed W-Y2O3, (b) the magnification of (a), (c) the loaded surface of deformed W-Y2O3, (d) the magnification of (c). The loaded areas are indicated by a red square (4 × 4 mm2) for the electron beam loading [178].
Fig. 34. Distribution of the grain/particle sizes and microstructures of the rolled W-Y2O3 (a-c) and W-Zr-Y2O3 (d-f) alloys: SEM images of rolled W-Y2O3 (a) and rolled W-Zr-Y2O3 (d) and insets of high magnification results; TEM images showing the fine tungsten grains in rolled W-Y2O3 (b) and rolled W-Zr-Y2O3 (e), second phase particles size distributions in rolled W-Y2O3 (c) and rolled W-Zr-Y2O3 (f). Tensile behaviors of the rolled W-Y2O3 and W-Zr-Y2O3 at different temperatures [27].
Fig. 35. Low magnification TEM image of the W-Y2O3 alloy prepared by wet chemical method and subsequent SPS, (b) high magnification TEM image showing the oxide particles within W grain, (c) HRTEM image of black square region in panel a, (d) HRTEM image of oxide particles within W grain [186].
Fig. 36. SEM images showing the representative fracture surfaces of (a) SPS W and (b) SPS W-0.5ZrC after tensile test at RT; (c) Comparison of tensile properties of SPS pure W, W-ZrC, W-Y2O3, W-Zr and W-Zr-Y2O3 materials tested at 700 °C [79,189].
Fig. 37. EBSD images of swaged W-0.5ZrC in the planes (a) parallel to and (b) perpendicular to the longitudinal direction; (c) Tensile engineering stress-strain curves of swaged W-0.5ZrC [190].
Fig. 38. SEM micrographs of the W-0.5 wt. %ZrC thin plate in normal direction (ND) and transverse direction (TD); Engineering stress-strain curves of W-0.5 wt. %ZrC thin plate specimens tested at different temperatures [50].
Fig. 40. Distribution of grain/particle sizes and microstructures of WZC05. (a) High magnification BSESEM image showing the tungsten grains possess equiaxed structure. The black contrast dots correspond to the second phase particles. (b) Grain size distribution. (c, d) ZrC and W-Zr-Cx-Oy particles size distribution [54].
Fig. 41. Detailed analysis of the interface structure between W matrix and second phase particlesin WZC. (a) HRTEM image of W matrix and ZrC phase (intragranular) as viewed along [001]. (b) The SAEDP revealing the particle with a face centered cubic structure. (c) Fast Fourier transform (FFT) pattern of selected red square area A on ZrC. (d) FFT pattern of selected red square area B at interface area between W and ZrC. It is clear that the particle-matrix PBs have coherent structure like showing in high magnification (e). (f) TEM image showing a deadbolt shaped ZrC particle (intergranular) tightly locking two tungsten grains (G1 represents the right one and G2 represents the left one). (g) Semi-coherent structure appears between the ZrC dispersoid and G2. (h) Some relatively large particles locating at GBs oftungsten contain W, Zr, C and O elements through (i) EDX analysis [54].
Fig. 42. Mechanical behaviors of WZC05. (a) Flexural stress-strain curves of WZC05 tested at different temperatures, note that values larger than a flexural strain of 15% are not accurate because of the limited bending angle of the machine. (b) Flexural strain of the tested samples versus temperature, DBTT is about 100 °C. (c) Temperature dependence of the yield strength (YS) of the WZC05 plate in comparison with available literature data. The YS of WZC05 is the highest among the all reported bulk W alloys. (d) Optical images of WZC05 samples after tests. (e) Tensile engineering stress-strain curves of WZC05 tested at various temperatures [54].
Fig. 43. SEM images showing the thermal shock resistance properties of WZC. (a) No cracks were detected on the samples with absorbed energy density (AED) ~ 3.3 MJ/m2. (b) There is still no crack with AED ~ 4.4 MJ/m2 despite the surface melting, which should benefit from the extraordinary plasticity and high strength. (c) Melting and cracks appear simultaneously with AED ~ 5.5 MJ/m2 and the wave-like stripes along with the crack illustrate the good ductility and plasticity of WZC alloy from other side [54].
Fig. 44. The mother grain structure (a); the state of H in columnar grain structure (sktech) (b); the thermal desorption spectrometry of deuterium in ITER grade W and W-0.5ZrC specimen (c). The irradiation temperature is 420 K [79].
Fig. 45. The surface morphologies of (a) pure W, (b) CVD-W, (c) W-1.0 % Y2O3 irradiated by 220 eV He+ at about 900 °C, and (d) pure W, (e) CVD W and (f) W-0.5ZrC irradiated by 620 eV He+ at 1000 °C to a same fluence of 1 × 1026 atoms/m2 [195].
Fig. 48. (a) Metallographic cross-sections of a single-fibre Wf/W composite consisting of a single coated tungsten wire which is embedded in a tungsten matrix formed by chemical vapour deposition. (b) Cross-section of the whole sample: a longitudinal section along the fibre axis showing the interface between fibre and matrix in detail [203]. (c) The fracture surface of the Wf/W composite (with the tungsten fibre array) [213].
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