Hardness Measurements and Microstructure Analysis
Figure 4 shows the Vickers microhardness profile of niobium and OFE copper as a function of the distance from the weld. The hardness of niobium is nearly constant in the fusion zone, the HAZ, and the parent material (variations between 53 HV 0.2 and 58 HV 0.2). Similar values were obtained by Jiang et al. [29] who measured a higher hardness in the HAZ (55 HV 0.3 to 60 HV 0.3) compared with regions taken more than 80 mm away from the weld center (49 HV 0.3 to 55 HV 0.3). The nearly constant hardness is consistent with the high-purity of the material and the low contamination during EB welding, due to the vacuum in the chamber. A larger variation in hardness was measured in the OFE copper specimen. The hardness is highest in the fusion zone, with a maximum of 58.2 HV 0.2, lowest in the HAZ with an average of 41.5 HV 0.2, and intermediate in the parent material of the specimen, with an average of 47.1 HV 0.2. The higher hardness in the fusion zone could be due to a combination of multiple factors such as a recrystallized microstructure with smaller grains [43] and residual stresses induced by the welding process [44, 45] and not completely removed by the post-welding annealing heat treatment. Despite the heterogeneous hardness properties in the fusion zone, the measured tensile mechanical properties, i.e. the stress–strain curves up to necking, are similar to unwelded specimens (“Mechanical Properties” section) and fracture occurred in the region of the fusion zone (“Strain Heterogeneities and Necking” section).
Figure 5 shows the etched microstructure in the cross-section of welded OFE copper and niobium specimens revealing grains and annealing twins. The grains in the HAZ of the OFE copper specimen are larger than in the parent material and the fusion zone. Annealing twins are also visible in the HAZ and parent material, but not in the center of the weld, where the grains have smoother edges and often converge to a region where crystal nucleation likely started. The niobium specimen, shown in Fig. 5b, has much larger grains close to center of the weld and in the HAZ (500–1200 μm), compared to the parent material (20–200 μm). Similar grain dimensions were measured by Jiang et al. for EB butt welds of high-purity niobium [29].
Mechanical Properties
The engineering stress–strain curves of the short and long specimens are compared in Fig. 6 for quasi-static strain rates at the same order of magnitude (10−3 s−1 and 10−1 s−1) and similar mechanical properties are measured pre-necking, i.e. before the nominal stress reaches its maximum value. The strain of the small specimens was calculated using DIC by measuring the displacement between two points that were initially separated by about 5 mm and using the displacement of the cross-head of the tensile machine for the long specimens. The initial gage length of 5 mm was selected based on finite element modelling of the quasi-static tensile test of an unwelded OFE copper specimen using known material properties. The stress–strain curve was calculated using the output force and displacement of the specimen from the simulation for a given gage length and compared with the expected response. The similarities in mechanical properties for the long and short specimens confirm that the methodology using DIC and the short specimen geometry are appropriate to characterize the tensile mechanical properties (yield stress and ultimate tensile stress) of welded specimens.
Figure 7 shows the engineering stress–strain curves of OFE copper and niobium for the short specimen geometry at strain rates of 2.0 × 10−3 s−1 to ~ 1600 s−1. DIC was used for all tests to ensure consistent strain measurements between tests performed with the servo-hydraulic tensile machine (\(\dot{\varepsilon }\le 20\) s−1) and the split Hopkinson bars and to measure the strain in the gage length only.
The strain rate sensitivity of EB welded copper and niobium are typical of FCC and BCC metals, respectively. The 0.2% yield stress of OFE copper specimens is nearly constant at all strain rates and the flow stress slightly increases for increasing strain rate due to increases in strain hardening, as shown in Fig. 7a. Note that the 0.2% yield stress was calculated using the apparent elastic modulus in the linear section of the stress–strain curve. However, the end of the elastic domain is ill-defined for OFE copper since parabolic hardening gradually increases from a low stress. The yield stress of high-purity niobium strongly increases for increasing strain rates (Fig. 7b). The apparent hardening rate observed in the engineering stress–strain curve decreases and the ultimate tensile stress is reached at a lower strain for increasing strain rate. A similar increase in yield stress and reduction of the apparent hardening was obtained by Peroni and Scapin [46] for unwelded high-purity niobium specimens and by Croteau et al. [47] for niobium single crystals.
Tensile Strength Strain Rate Sensitivity
Figure 8 shows the yield stress (YS) and ultimate tensile stress (UTS) as function of strain rate (denoted by \(\dot{\varepsilon }\) hereafter) for OFE copper and high-purity niobium for the short (for 2.0 × 10−3 s−1 \(\le \dot{\varepsilon }\le\) ~1600 s−1) and long (for 10−3 s−1 ≤ \(\dot{\varepsilon }\le\)10−1 s−1) EB welded specimens. The same marker is used for both geometries since similar values are measured at strain rates of the same order of magnitude. The stresses of the welded specimens are compared with those of unwelded specimens from Peroni and Scapin [46] for niobium and from unpublished results obtained by the authors and collaborators from the Imperial College London for OFE copper. The UTS is very similar for the welded and unwelded specimens for both materials at strain rates between 10−3 s−1 and 20 s−1. The yield stress is, however, lower by approximately 10 MPa to 18 MPa for the welded OFE copper specimens and within the dispersion of the data for the niobium specimens, for the same strain rate range.
The tensile strength is likely preserved after EB welding due to the high-purity of the parent materials and the low contamination during the welding process. Recall that high-purity OFE copper and niobium have microstructures with a single phase and the welds are performed under vacuum. The welded microstructures are then still composed of a single phase, but with different grain sizes, as described in “Hardness Measurements and Microstructure Analysis” section. Thus, the conservation of mechanical properties is different from what is found for other materials, e.g. high strength low alloy (HSLA) steel, that can have lower and higher tensile strengths for different compositions, welding techniques, and welding parameters [48, 49].
The strain rate sensitivity at yield (\(m=\partial \mathrm{ln}{\sigma}_{y}/\partial \mathrm{ln}\dot{\varepsilon }\)) is approximately constant for both materials and equal to 0.045 for OFE copper and to 0.112 for niobium. A constant strain rate sensitivity at all strain rates in the range studied, shown with two light shaded straight lines in Fig. 8a and b, indicates that the same dominant deformation mechanism operates at all strain rates. Since the strain rate sensitivity \(m\) is derived from a power law relationship (\({\sigma }_{y}\propto {\dot{\varepsilon }}^{m}\)), the use of a log–log plot is more appropriate in the stress as function of strain rate plot to show the differences in m between different materials. A linear scale is often used in literature for the stress axis, but could lead to the false impression that a sudden increase in flow stress is measured at the highest strain rate. The apparent “upturn” in flow stress at strain rates between ~ 103 and 104 s−1 has been contradicted for few materials and reviewed by Rosenberg et al. [50]. While this upturn phenomenon is not happening in this study, mainly because the highest strain rate is too low, the authors still want to stress the importance of using a logarithmic scale to clearly see changes in strain rate sensitivity \(m\) and in activation volume (\({v}^{\ast}\propto {m}^{-1}\)), which are caused by a change in deformation mechanism [51], e.g. from thermal activation to dislocation drag.
A reduction in absolute difference in stress between the UTS and the YS (\(\Delta \sigma ={\sigma }_{\text{UTS}}-{\sigma }_{y}\)) is measured for niobium for increasing strain rates, from approximately 99.3 MPa at 10−3 s−1 to 28.8 MPa at ~ 1600 s−1. This is explained by the lower apparent strain hardening rate (in engineering stress–strain curves) for specimens tested at a higher strain rate. This behavior is typical for BCC metals, see for instance the analysis conducted by Zerilli and Armstrong [52] using dislocation mechanics arguments. For OFE copper, a small increase in \(\Delta \sigma\) from ~ 177.6 MPa at 10−3 s−1 to ~ 198.6 MPa at about 1600 s−1 is measured and due to an increasing strain hardening rate for increasing strain rates.
Ductility Strain Rate Sensitivity
As previously mentioned, and shown in Fig. 6, the post-necking behavior of the long and short specimens is different for similar strain rates. Higher elongation at break, measured with the crosshead displacement of the tensile machine, was found for short specimens deformed at strain rates in the order of 10−3 s−1 and 10−1 s−1. This is likely explained by the highest thickness-to-width ratio of the short specimens. While the different specimen geometries yield different absolute values of elongation at break, the change in strain to failure is similar for both geometries and materials between strain rates of 10−3 s−1 and 10−1 s−1. Therefore, the effect of strain rate on the ductility of the short specimens, from 2.0 × 10−3 to ~ 1600 s−1, can reasonably be extrapolated to the standardized geometry.
Due to the high ductility of the materials it is difficult to accurately measure the cross-sectional area of the broken specimens, so the area reduction at failure (A%) is not used to quantify the ductility of the materials [53]. Also, measuring the elongation at break by aligning the broken specimens, as specified in ASTM’s E8 standard [38], is difficult due to the non-standardized geometry and, again, the high ductility of both materials. The nominal strain to failure (\({\varepsilon }_{f}\)), defined as the elongation measured using DIC for the last frame before specimen failure (\(\Delta {y}_{DIC}\)) divided by the initial gage length (\({L}_{0}\)) of approximately 5 mm (\({\varepsilon }_{f}=\Delta {y}_{DIC}/{L}_{0}\)), is used. The last frame was selected based on a visual criterion. The specimen was considered to be broken when a translation of the specimen in the neck perpendicular to the loading direction was observed, even if both ends of the specimen still looked attached. The absolute values of nominal strain to failure are not intrinsic to each material, but the variation across approximately 7 orders of magnitude of strain rate provides valuable information for high-speed sheet forming of SRF cavities.
Figure 9 shows the nominal strain to failure as function of strain rate for short OFE copper and niobium welded specimens. Similar to the variation in yield and tensile strengths with strain rate (Fig. 8a and b), the nominal strain to failure is almost constant between 2.0 × 10−3 s−1 and ~ 1600 s−1 for EB welded OFE copper (the mean and standard deviation of \({\varepsilon }_{f}\) for all strain rates are equal to 0.75 and 0.01, respectively). The ductility of niobium is lower, less repeatable between tests performed at the same strain rate, and more strain rate sensitive than OFE copper. Average maximum and minimum nominal strain to failures of 0.74 ± 0.03 and 0.61 ± 0.03 were measured at strain rates of 2.0 × 10−2 s−1 and 400 s−1, respectively.
Peroni and Scapin [46] reported a relative reduction in strain to failure of about 20% between strain rates of 10−1 s−1 and 10 s−1 for unwelded high-purity niobium (calculated using the engineering strain at an engineering stress of zero at the end of the published stress–strain curves). EB welded specimens deformed at the same order of magnitude of strain rate showed a similar relative reduction in nominal strain to failure of approximately 15%. The increase in strain rate between quasi-static and intermediate rates is then reducing the ductility of welded and unwelded high-purity niobium. A reduction in ductility varying from 16 to 50% was also reported by Croteau et al. [47] for niobium single crystals with different crystallographic orientations deformed at strain rates of 10−2 s−1 and ~ 10 s−1.
The nominal strain to failure for the welded niobium specimens deformed at ~ 1600 s−1 is higher than for specimens deformed at 20 s−1 and ~ 400 s−1. The cause of the increase in ductility when the strain rate goes from ~ 400 to ~ 1600 s−1 is unknown, but it could be due to inertia effects that yield a stabilizing effect and enhance the ductility at very high strain rate [24]. However, the ductility remains lower than at quasi-static strain rates, which could be detrimental for high-speed sheet forming. Nevertheless, strain rates achieved in high-speed forming operations are generally larger than the maximal strain-rate considered in the present experiments. This can contribute to enhance inertia effects and the resulting formability improvement [54, 55]. Moreover, in high-speed sheet forming, part of the deformation takes place during the impact of the sheet on the die. This phenomenon also contributes to enhance formability [25, 56].
Strain Heterogeneities and Necking
Figure 10 shows the true (logarithmic) axial strain distribution in EB welded niobium specimens (short geometry) deformed at nominal strain rates of 2.0 × 10−3 s−1, 2.0 × 10−1 s−1, and ~ 1600 s−1. The axial true strain line scan in the gage section shown in Fig. 10a1, b1, and c1 reveal a region of lower strain close to the center of the specimen and surrounded by two peaks. This behavior is probably due to microstructural heterogeneity in the vicinity of the weld. The large strain heterogeneities, compared with OFE copper in Fig. 11, suggest that the anisotropic properties in the large niobium grains in the center of the specimen, as shown in Fig. 5b, affect the localization process. Moreover, Fig. 5b shows that the grain size is larger in the HAZ than in the fusion zone. These grain size heterogeneities may be responsible for the two peaks observed in the strain distribution (Fig. 10). In contrast, the more homogeneous strain distribution in OFE copper specimens are probably due to the more homogeneous grain size distribution. Note that plastic flow localization takes place near the center of the specimens for both materials and at all strain rates. It is believed that this phenomenon is due to the presence of the weld (and not to the rather short specimen length) as it also occurs with the long specimens. Figure 12 shows a comparison of the true strain distribution in the gage length between long and short specimens deformed at strain rates in the order of 10−3 s−1. The neck appears to be skewed to the right side of the gage length (corresponding to the upper-half of the specimen, which is closer to the moving end of the tensile machine) for the long specimens due to a reduced field of view to capture details in the fracture at a high resolution. However, fracture occurred at the center of the specimen at all strain rates for both materials. This suggests that the weld acts as an imperfection that promotes plastic flow localization in its vicinity.
The true strain peaks and valley around the center of the short niobium specimen (Fig. 10), which was attributed to grain size heterogeneities, is not as pronounced for the long niobium specimen (which has a larger width). The influence of the weld on the mechanical properties seems to be more important for the short niobium specimens. This is probably because size effects from the large grains in the fusion region begin to be apparent (at the scale of the short specimen). Based on the grain size measured in the fusion zone in “Hardness Measurements and Microstructure Analysis” section, there are approximately 3 to 6 grains across the width of the short specimens compared with about 10 to 100 grains for the long specimens.
Figure 13 shows long and short OFE copper and niobium specimens deformed at strain rates in the order of 10−3 s−1 during necking and after failure. Those pictures were acquired in-situ and used in the digital image correlation analyses. The long niobium specimen shows a more acute neck (the section reduction is more marked) and a narrower fracture surface than the long copper specimen. This indicates larger plastic strain in the neck of niobium specimens after the onset of localization, which suggests that niobium is intrinsically more ductile than OFE copper (the local strain to failure, at the center of the neck, is larger for niobium than for OFE copperFootnote 1). The difference in dimensions in the gage section of the short and long specimens (e.g. higher thickness-to-width ratio for the short specimen) resulted in different neck morphologies for both materials. The short OFE copper specimen has a narrower fracture surface than the long one and a non-symmetric neck is observed in the short niobium specimen. The latter is probably caused by material heterogeneities and anisotropic properties at the center of the specimen from the low amount of grains across the width and thickness of the specimens. During the manufacturing of SRF cavities, the size effects should be negligible due to the large sheet dimensions and a more uniform strain distribution (Fig. 12b) is expected.