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Microstructure and fracture toughness characterization of three 9Cr ODS EUROFER steels with different thermo-mechanical treatments

Ferritic martensitic ODS steels are one of the candidate structural materials for future Gen-IV nuclear fission and fusion reactors. Here, the dependence of fracture toughness on microstructure was investigated by comparing three 9Cr ODS EUROFER steels manufactured through different thermo-mechanical processing routes. Quasi-static fracture toughness testing was performed with sub-sized C(T) specimens and microstructural characterization was carried out using scanning electron microscopy, electron backscatter diffraction, and transmission electron microscopy. It was found that at lower test temperatures (-100 – 22 °C), the fracture toughness was primarily controlled by crack initiation at sub-micron particles and by production of secondary cracks during fracture. At higher temperatures (above 100 °C), fracture toughness was predominantly controlled by the matrix ductility and the grain boundary strength with a relatively ductile coarse-grained alloy demonstrating higher fracture toughness compared to high-strength fine-grained alloys. These results and discussion show that variations in thermomechanical treatments can produce significant differences in microstructure and fracture toughness behavior of ferritic martensitic ODS steels.

36 MATERIALS SCIENCE↗

Effects of HFIR neutron irradiation on fracture toughness properties of standard and Ni-doped F82H

F82H is the Japanese reference reduced-activation ferritic-martensitic (RAFM) steel for fusion blanket applications. The harsh environment of a fusion reactor, such as neutron irradiation and He/H damage, can result in significant degradation of F82H fracture toughness. Therefore, understanding the fracture toughness behavior of F82H in the fusion environment is critical to ensure the long-term safe operation of the fusion reactor. Here, we summarize seven irradiation campaigns of the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) covering five variants of F82H steels, including F82H IEA, F82H Mod3, F82H doped with 1.4% natural Ni, F82H doped with 1.4% 58 Ni, and F82H doped with 1.4% 60 Ni. The irradiation temperatures covered the range from 220 °C to 530 °C and the neutron irradiation dose spanned 4 dpa to 70 dpa. The effects of neutron irradiation temperature, dose, materials composition, Ni doping, and He production on F82H fracture toughness are discussed. Our results showed that irradiation embrittlement monotonically decreased with increasing irradiation temperature until 400 °C for F82H IEA and F82H Mod3. F82H Mod3 showed better fracture toughness than F82H IEA both before and after neutron irradiation. We determined that 1.4% Ni alloying can be applied to F82H for simulating He effect in a fission reactor without jeopardizing the fracture toughness of the material. However, more studies are needed to understand the effect of high dose (>20 dpa) and He production on F82H fracture toughness.

36 MATERIALS SCIENCE↗

Influence of microstructure and temperature on impact toughness of H13 steel produced by binder jet additive manufacturing

Binder Jet Additive Manufacturing (BJAM) is a promising manufacturing pathway to produce H13 steel dies and tooling with complex geometries for applications in high pressure aluminum die casting, hot stamping, and injection molding. While fully dense H13 coupons produced using BJAM have been subjected to detailed microstructure characterization, properties which are critical and relevant to the aforementioned applications, such as impact toughness, have not been reported. Here, this work evaluated the influence of microstructural characteristics and test temperature on the impact toughness of H13 produced by BJAM. Coupons were produced from three different powder size distributions (PSDs), with nominal powder size ranges of −22 μm, 10-32 μm, and 15-53 μm. Coupons were printed, sintered, hot isostatically pressed (HIPed), and heat treated by quenching and tempering. After HIPing, the measured porosities of the different PSDs were all less than 0.015 vol%. The −22 μm PSD BJAM material exhibited the best impact toughness of all three PSDs across the entire test temperature range from 25 to 400 °C, and also exhibited an ambient temperature impact toughness of 10.9 J at a hardness of 46 HRC, equivalent to minimum threshold requirements for premium grade H13. However, all three BJAM PSDs exhibited moderately lower impact toughness than premium grade wrought H13 from RT to 400 °C. We attribute this in part due to the very large prior-austenite grain (PAG) sizes near 400 μm and segregation from former liquid channels leading to greater amounts of carbide precipitation on PAG boundaries. Technical pathways for optimizing processing and chemistry of BJAM H13 to further improve impact toughness are discussed.

Binder jet additive manufacturing↗

Fracture toughness evaluations for spent nuclear fuel dry storage canister welds and spent nuclear fuel clad-pellet structures

Integrity of spent nuclear fuel (SNF) interim storage canisters is very important to the safety of the back-end nuclear fuel cycle. Stress corrosion cracking (SCC) potential of interim storage canister has been considered as a high priority. Because no post-weld heat treatment was required for forming these canisters, the high tensile residual stress existed within these canister welds. This can change the fracture resistance capacity significantly as well as increase SCC potential. Due to relative thin shell thickness of a canister weldment, the spiral notch torsion test (SNTT) method was used to estimate the canister weldment fracture toughness. SNTT was developed to measure the intrinsic fracture toughness of structural materials using small specimens. The SNTT method has been applied to a wide variety of structural materials, such as low-alloy steels, stainless steel, aluminum alloy, ceramics, concrete, and composites. The SNTT system operates by applying pure torsion to cylindrical specimens with a notch line that spirals around the specimen at a 45° pitch. In order to carry out pure torsion load mode, biaxial tension/torsion tester was developed accordingly to perform SNTT protocol. Moreover, applying fracture mechanics approach to SNF system reliability investigation is warranted due to the inherent flaws and hydride structures existed in a SNF system after nuclear reactor operation. However, none of the existing fracture toughness data deal with fuel cladding specific geometry or spent fuel material conditions, such as cladding structure with the pellet-inserts and the associated pellet clad mechanical interactions induced mixed-mode damage mechanisms. Thus, the development of an intrinsic fracture mechanics approach that is suitable for SNF materials is needed. Furthermore, due to thin wall and small dimension of clad tubing structure, the SNTT method was used to estimate the clad tubing structure fracture toughness. Fracture testing were performed on the received stainless steel canister weldment, most SNTT weld samples fracture initiation sites are at heat-affected zone (HAZ) regions. The estimated fracture toughness J Q ’ for the baseline SS304 steel is at 283 kJ/m². The estimated JQ’ for the SS304/308 weld and baseline metals are 148 kJ/m 2 and 459 kJ/m 2 , respectively. Out of cell fracture testing for spent fuel structure were carried out on the surrogate rods made of Zr-4 clad and alumina inserts, the estimated fracture toughness values for baseline Zr-4 cladding with alumina-pellet inserts are: (1) For SNTT samples with a short or medium crack length, between 5.4-mm and 8-mm, the estimate J IQ upon fracture initiation for the baseline Zr-4 cladding is at 50 kJ/m 2 with 2-sigma uncertainty of 3.26 kJ/m 2 , and the associated K IQ is at 67.46 MPa$\sqrt{m}$; and (2) For SNTT samples with a long crack length, around 13-mm, the crack initialization is deviated from that of the Mode-I tensile fracture and appears to be a mixed-mode fracture of Mode I - tensile stress and Mode III - out of plane shear stress; the estimated J MQ is at 18.9 kJ/m 2 , the associated K MQ is at 41.4 MPa$\sqrt{m}$.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A study of the effect of subcritical crack growth on the geometry dependence on nonlinear fracture toughness parameters

The effect of subcritical crack growth on the geometry dependence of nonlinear fracture toughness parameters was studied by comparing the toughness values for different specimen geometries at the onset of subcritical crack growth and at the initiation of unstable crack propagation. Center-cracked thin sheet specimens of 2024-T3 and 7075-T6 aluminum alloys were tested by varying the specimen length L, width w, and crack length-to-width ratio c/w. When the onset of unstable crack propagation was selected as the critical point, the nonlinear energy toughness and the R curve toughness increased with increasing w and decreasing L and c/w. However, when the onset of subcritical crack growth was taken as the critical point, energy toughness and the linear toughness values were independent of these geometrical variables.

Jones, D. L.↗

On the feasibility of quantitative ultrasonic determination of fracture toughness: A literature review

The three main topics covered are: (1) fracture toughness and microstructure, (2) quantitative ultrasonic and microstructure; and (3) scattering and related mathematical methods. Literature in these areas is reviewed to give insight to the search of a theoretical foundation for quantitative ultrasonic measurement of fracture toughness. The literature review shows that fracture toughness is inherently related to the microstructure and in particular, it depends upon the spacing of inclusions or second particles and the aspect ratio of second phase particles. There are indications that ultrasonic velocity attenuation measurements can be used to determine fracture toughness. The leads to a review of the mathematical models available in solving boundary value problems related to microstructural factors that govern facture toughness and wave motion. A framework towards the theoretical study for the quantitative determination of fracture toughness is described and suggestions for future research are proposed.

Fu, L. S.↗

Development of tough, strong, iron-base alloy for cryogenic applications

The development of an iron-base alloy that combines the normally divergent properties of high toughness and high strength at cryogenic temperatures is discussed. Specifically, alloy properties were sought which at -196 C would exhibit a fracture toughness of 220 MPa-m(1/2) with a corresponding yield strength of 1.4 GPa (200 ksi). Early work showed that high toughness could be achieved in Fe-12Ni alloys containing reactive metal additions such as Al, Nb, Ti, and V. Further research emphasized strengthening of these tough alloys by thermomechanical processing and the addition of Cu. Results showed that high strength and high toughness could be achieved in a single alloy at temperatures as low as -196 C. An alloy with composition Fe-12Ni-9.5Al-2Cu exhibited a yield strength of 1.65 GPa with a corresponding fracture toughness of 220 MPa-m(1/2) at -196 C. Strengthening due to Cu additions to the Fe-12Ni base alloys results primarily from precipitation of Cu-rich epsilon particles approximately 20 nm in diameter. Strengthening mechanisms are discussed in terms of an elastic modulus hardening model and are supported by transimission electron microscopy examinations of selected test specimens.

Stephens, J. R.↗

A parametric study of fracture toughness of fibrous composite materials

Impacts to fibrous composite laminates by objects with low velocities can break fibers giving crack-like damage. The damage may not extend completely through a thick laminate. The tension strength of these damage laminates is reduced much like that of cracked metals. The fracture toughness depends on fiber and matrix properties, fiber orientations, and stacking sequence. Accordingly, a parametric study was made to determine how fiber and matrix properties and fiber orientations affect fracture toughness and notch sensitivity. The values of fracture toughness were predicted from the elastic constants of the laminate and the failing strain of the fibers using a general fracture toughness parameter developed previously. For a variety of laminates, values of fracture toughness from tests of center-cracked specimens and values of residual strength from tests of thick laminates with surface cracks were compared to the predictions to give credibility to the study. In contrast to the usual behavior of metals, it is shown that both ultimate tensile strength and fracture toughness of composites can be increased without increasing notch sensitivity.

Poe, C. C., Jr.↗

A parametric study of fracture toughness of fibrous composite materials

Impacts to fibrous composite laminates by objects with low velocities can break fibers giving crack-like damage. The damage may not extend completely through a thick laminate. The tension strength of these damage laminates is reduced much like that of cracked metals. The fracture toughness depends on fiber and matrix properties, fiber orientations, and stacking sequence. Accordingly, a parametric study was made to determine how fiber and matrix properties and fiber orientations affect fracture toughness and notch sensitivity. The values of fracture toughness were predicted from the elastic constants of the laminate and the failing strain of the fibers using a general fracture toughness parameter developed previously. For a variety of laminates, values of fracture toughness from tests of center-cracked specimens and values of residual strength from tests of thick laminates with surface cracks were compared to the predictions to give credibility to the study. In contrast to the usual behavior of metals, it is shown that both ultimate tensile strength and fracture toughness of composites can be increased without increasing notch sensitivity.

Poe, C. C., Jr.↗

Fracture toughness testing of polymer matrix composites

A review of the interlaminar fracture indicates that a standard specimen geometry is needed to obtain consistent fracture toughness measurements in polymer matrix composites. In general, the variability of measured toughness values increases as the toughness of the material increases. This variability could be caused by incorrect sizing of test specimens and/or inconsistent data reduction procedures. A standard data reduction procedure is therefore needed as well, particularly for the tougher materials. Little work has been reported on the effects of fiber orientation, fiber architecture, fiber surface treatment or interlaminar fracture toughness, and the mechanisms by which the fibers increase fracture toughness are not well understood. The little data that is available indicates that woven fiber reinforcement and fiber sizings can significantly increase interlaminar fracture toughness.

Grady, Joseph E.↗

Simplified data reduction methods for the ECT test for mode 3 interlaminar fracture toughness

Simplified expressions for the parameter controlling the load point compliance and strain energy release rate were obtained for the Edge Crack Torsion (ECT) specimen for mode 3 interlaminar fracture toughness. Data reduction methods for mode 3 toughness based on the present analysis are proposed. The effect of the transverse shear modulus, G(sub 23), on mode 3 interlaminar fracture toughness characterization was evaluated. Parameters influenced by the transverse shear modulus were identified. Analytical results indicate that a higher value of G(sub 23) results in a low load point compliance and lower mode 3 toughness estimation. The effect of G(sub 23) on the mode 3 toughness using the ECT specimen is negligible when an appropriate initial delamination length is chosen. A conservative estimation of mode 3 toughness can be obtained by assuming G(sub 23) = G(sub 12) for any initial delamination length.

Li, Jian↗

Evaluation of the Edge Crack Torsion (ECT) Test for Mode 3 Interlaminar Fracture Toughness of Laminated Composites

An analytical and experimental investigation was carried out on G40-800/R6376 graphite epoxy laminates to evaluate the Edge Crack Torsion (ECT) test as a candidate for a standard Mode 3 interlaminar fracture toughness test for laminated composites. The ECT test consists of a (90/(+/- 45)(sub 3)/(+/- 45)(sub 3)/90))(sub s) laminate with a delamination introduced by a non-adhesive film at the mid-plane along one edge and loaded in a special fixture to create torsion along the length of the laminate. Dye penetrate enhanced X-radiograph of failed specimens revealed that the delamination initiated at the middle of the specimen length and propagated in a self similar manner along the laminate mid-plane. A three-dimensional finite element analysis was performed that indicated that a pure Mode 3 delamination exists at the middle of specimen length away from both ends. At the ends near the loading point a small Mode 2 component exists. However, the magnitude of this Mode 2 strain energy release rate at the loading point is small compared to the magnitude of Mode 3 component in the mid-section of the specimen. Hence, the ECT test yielded the desired Mode 3 delamination. The Mode 3 fracture toughness was obtained from a compliance calibration method and was in good agreement with the finite element results. Mode 2 End-Notched Flexure (ENF) tests and Mode 1 Double Cantilever Beam (DCB) tests were also performed for the same composite material. The Mode 1 fracture toughness was much smaller than both the Mode 2 and Mode 3 fracture toughness. The Mode 2 fracture toughness was found to be 75% of the Mode 3 fracture toughness.

Li, Jian↗

Strength and Fracture Toughness of Solid Oxide Fuel Cell Electrolyte Material Improved

Solid oxide fuel cells (SOFC) are being developed for various applications in the automobile, power-generation, and aeronautics industries. Recently, the NASA Glenn Research Center has been exploring the possibility of using SOFC's for aeropropulsion under its Zero Carbon Dioxide Emission Technology (ZCET) Program. 10-mol% yttriastabilized zirconia (10YSZ) is a very good anionic conductor at high temperatures and is, therefore, used as an oxygen solid electrolyte in SOFC. However, it has a high thermal expansion coefficient, low thermal shock resistance, low fracture toughness, and poor mechanical strength. For aeronautic applications, the thin ceramic electrolyte membrane of the SOFC needs to be strong and tough. Therefore, we have been investigating the possibility of enhancing the strength and fracture toughness of the 10YSZ electrolyte without degrading its electrical conductivity to an appreciable extent. We recently demonstrated that the addition of alumina to zirconia electrolyte increases its strength as well as its fracture toughness. Zirconia-alumina composites containing 0 to 30 mol% of alumina were fabricated by hot pressing. The hot pressing procedure was developed and various hot pressing parameters were optimized, resulting in dense, crackfree panels of composite materials. Cubic zirconia and a-alumina were the only phases detected, indicating that there was no chemical reaction between the constituents during hot pressing at elevated temperatures. Flexure strength sf and fracture toughness K(sub IC) of the various zirconia-alumina composites were measured at room temperature as well as at 1000 C in air. Both properties showed systematic improvement with increased alumina addition at room temperature and at 1000 C. Use of these modified electrolytes with improved strength and fracture toughness should prolong the life and enhance the performance of SOFC in aeronautics and other applications.

Bansal, Narottam P.↗

On plasticity-enhanced interfacial toughness in bonded joints

Here, the performance and reliability of many structures and components depend on the integrity of interfaces between dissimilar materials. Interfacial toughness Γ is the key material parameter that characterizes resistance to interfacial crack growth, and Γ is known to depend on many factors including temperature. For example, previous work showed that the toughness of an epoxy/aluminum interface decreased 40 % as the test temperature was increased from -60 °C to room temperature (RT). Interfacial integrity at elevated temperatures is of considerable practical importance. Recent measurements show that instead of continuing to decrease with increasing temperature, Γ increases when test temperature is above RT. Cohesive zone finite element calculations of an adhesively bonded, asymmetric double cantilever beam specimen of the type used to measure Γ suggest that this increase in toughness may be a result of R-curve behavior generated by plasticity-enhanced toughening during stable subcritical crack growth with interfacial toughness defined as the critical steady-state limit value. In these calculations, which used an elastic-perfectly plastic epoxy model with a temperature-dependent yield strength, the plasticity-enhanced increase in Γ above its intrinsic value Γ o depended on the ratio of interfacial strength σ* to the yield strength σyb of the bond material. There is a nonlinear relationship between Γ/Γ o and σ*/σ yb with the value Γ/Γ o increasing rapidly above a threshold value of σ*/σ yb . The predicted increase in toughness can be significant. For example, there is nearly a factor of two predicted increase in Γ/Γ o during micrometer-scale crack-growth when σ*/σ yb = 2 (a reasonable choice for σ*/σ yb ). Furthermore, contrary to other reported results, plasticity-enhanced toughening can occur prior to crack advance as the cohesive zone forms and the peak stress at the tip of the original crack tip translates to the tip of the fully formed cohesive zone. These results suggest that plasticity-enhanced toughening should be considered when modeling interfaces at elevated temperatures.

36 MATERIALS SCIENCE↗

High temperature fracture toughness of single-layer CrAlN and CrAlSiN hard coatings

Hardness and toughness are among of the most important physical properties of hard coatings and it is important to analyze them at temperatures present during coating applications. CrAlN and CrAlSiN are hard coating materials frequently used in high temperature applications. Here, while both possess high oxidation resistance and thermal stability, they differ in their microstructure. In this work, the fracture toughness of magnetron-sputtered single-layer CrAlN and CrAlSiN hard coatings was determined up to 700 °C by in-situ scanning electron microscopy micro-cantilever deflection tests. The results show a decreasing trend of the fracture toughness with increasing temperature. While both coatings' fracture toughness trends are similar up to 400 °C, they diverge at higher temperatures. In general, the evolution of the fracture toughness with increasing temperature shows similarities to the observed changes in hardness in the same temperature range.

36 MATERIALS SCIENCE↗

Grain Boundary and Lattice Fracture Toughness of UO 2 Measured Using Small-Scale Mechanics

Small-scale mechanical testing has been used to isolate the properties of individual grain boundaries and regions of the lattice in undoped UO 2 polycrystals. Notched microcantilever specimens were prepared by focused ion beam milling and tested in bending. Fracture toughness values were calculated from finite element analysis of the sample geometry at fracture load using the J-integral method. Lattice and grain boundary fracture toughness values of 1.17 ± 0.16 MPa m 1/2 and 1.08 ± 0.08 MPa m 1/2 , respectively, were obtained. The similarity between the lattice and grain boundary fracture toughness values is consistent with the preference for transgranular room-temperature fracture in UO 2 . The grain boundary and lattice fracture toughness values also agree well with the toughness of dense polycrystals, which suggests that microstructural-scale toughening mechanisms are limited in such samples.

36 MATERIALS SCIENCE↗

Fracture toughness of schist, amphibolite, and rhyolite from the Sanford Underground Research Facility (SURF), Lead, South Dakota

The Cracked Chevron Notched Brazilian Disc (CCNBD) method was selected for Mode I fracture toughness tests on Poorman schist, Yates amphibolite, and rhyolite dikes from the EGS Collab site at the SURF in Lead, South Dakota. The effects of lithology, anisotropy, and loading rate were investigated. Fracture toughness was greatest in amphibolite, with schist and rhyolite having similar toughness values ($K$ amphibolite > $K$ rhyolite ≈ $K$ schist ). The effects of anisotropy on fracture toughness were investigated in the foliated schist samples. Schist samples were prepared in three geometries (divider, arrester, and short transverse) which controlled how the fracture would propagate relative to foliations. The divider geometry was strongest and short transverse geometry was the weakest ($K$ divider > $K$ arrester > $K$ shorttransverse ). Fracture toughness was observed to decrease with decreasing loading rate. Optical and SEM microscopy revealed that for the short transverse geometry, fractures tended to propagate along grain boundaries, whereas in arrester and divider geometries fractures tended to propagate through grains. In foliated samples, the tortuosity of the fracture observed in thin section was greater in arrester and divider geometries than in short transverse geometries.

58 GEOSCIENCES↗

Tritium Aging Effects on Fracture Toughness of Stainless Steel Weldments

The long-term embrittlement effects of tritium and decay helium on the structural properties of stainless steels have been studied for years at Savannah River to provide required data for establishing safe operating conditions and lifetimes of pressure vessels used to contain tritium gas. In this study, the fracture toughness properties of the longest-aged tritium-precharged stainless-steel base metals and weldments tested at Savannah River were measured and compared to earlier results. The fracture toughness values were the lowest recorded here for tritium-exposed stainless steel. As-forged and as-welded specimens were thermally precharging with tritium gas at 34.5 MPa and 623 K, then aged for up to 17 years to buildin decay helium prior to testing. ASTM J-Integral fracture mechanics analyses, transmission electron microscopy (TEM), and small angle neutron scattering (SANS) examinations were conducted to characterize the effects of tritium and its radioactive decay product, helium-3. Results show that the fracture toughness values were reduced to less than 2-4% of the as-forged values for specimens with more than 1300 appm helium from tritium decay. The trend of decreasing fracture toughness values with increasing helium content was consistent with earlier observations, and the data show that Type 304L stainless steel is more resistant to tritium-induced cracking than Type 21-6-9 stainless at similar decay helium levels. The fracture toughness properties of long-aged weldments were also affected, but the reductions were not as severe over time because weldments did not retain as much tritium as did the base metals. TEM observations were used to characterize the effects of decay helium bubbles on the deformation substructures, but nanometer-sized helium bubbles were not easily resolved because of high dislocation densities within the forged microstructures. SANS results are presented that suggest the technique can provide information on decay helium bubble size, spacing, and distribution in these steels.

36 MATERIALS SCIENCE↗