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DOE OSTI2020

Interfacial toughness: dependence on surface roughness and test temperature

Interfacial toughness quantifies resistance to crack growth along an interface and in this investigation the toughness of an aluminum/epoxy interface was measured as a function of surface roughness and test temperature. The large strain response of the relatively ductile epoxy adhesive used in this study was also characterized. This epoxy adhesive exhibits intrinsic strain-softening after initial compressive yield and then deforms plastically at a roughly constant flow stress until it rapidly hardens at large compressive strains. Here, we find that interface toughness scales as the product of the temperature dependent epoxy yield strength and a length scale that characterizes surface roughness. The proposed scaling is based upon dimensional considerations of a model problem that assumes that the characteristic length scale of both the roughness and the crack-tip yield zone is small relative to the region dominated by the linear elastic asymptotic crack-tip stress field. Furthermore, the model assumes that interfacial failure occurs only after the epoxy begins to harden at large strains. The proposed relationship is validated by our interfacial toughness measurements.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Strong tough hydrogels via the synergy of freeze-casting and salting out

Natural load-bearing materials like tendons possess high water content of ~70% but14 are still strong and tough even when used for over 1 million cycles per year, which is owed to the hierarchical assembly of anisotropic structures across multi-length-scales . In imitation of natural systems, various hydrogels have been created via methods like electro-spinning, extrusion, compositing, freeze casting, self-assembly, and mechanical stretching for improved mechanical performance. However, in contrast to tendons, many hydrogels with the same high water content do not show high strength, large toughness or high fatigue resistance. In this work, we present a strategy to produce strong, tough and fatigue resistant hydrogels with multi-length-scale hierarchical architecture using a freezing-assisted salting-out treatment. The produced exemplary poly(vinyl alcohol) hydrogels are highly anisotropic, comprising micrometer-scale honeycomb-like pore walls, which in turn comprise interconnected nanofibrils meshes, entirely physically assembled from polymer chains. These hydrogels are made of 70-95% water but can exhibit ultra-high ultimate stress (23.5 ± 2.7 MPa) and strain (2900 ± 450%), giant 32226 toughness (210 ± 13 MJ/m , 175 ± 8 kJ/m) and remarkable fatigue threshold (10.5 ± 1.3 kJ/m), which are 10 times tougher than natural tendon. The presented strategy could expand the applicability of weak polymeric material, like hydrogels, in practical applications that requires long-term services with high-loads and abrupt-impacts and extend the development of structural hydrogels.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Exceptional fracture toughness of CrCoNi-based medium- and high-entropy alloys at 20 kelvin

Medium- and high-entropy alloys based on the CrCoNi-system have been shown to display outstanding strength, tensile ductility and fracture toughness (damage-tolerance properties), especially at cryogenic temperatures. Here we examine the J Ic and (back-calculated) K JIc fracture toughness values of the face-centered cubic, equiatomic CrCoNi and CrMnFeCoNi alloys at 20 K. At flow stress values of ~1.5 GPa, crack-initiation K JIc toughnesses were found to be exceptionally high, respectively 235 and 415 MPa√m for CrMnFeCoNi and CrCoNi, with the latter displaying a crack-growth toughness K ss exceeding 540 MPa√m after 2.25 mm of stable cracking, which to our knowledge is the highest such value ever reported. Characterization of the crack-tip regions in CrCoNi by scanning electron and transmission electron microscopy reveal deformation structures at 20 K that are quite distinct from those at higher temperatures and involve heterogeneous nucleation, but restricted growth, of stacking faults and fine nanotwins, together with transformation to the hexagonal closed-packed phase. The coherent interfaces of these features can promote both the arrest and transmission of dislocations to generate respectively strength and ductility which strongly contributes to sustained strain hardening. Indeed, we believe that these nominally single-phase, concentrated solid-solution alloys develop their fracture resistance through a progressive synergy of deformation mechanisms, including dislocation glide, stacking-fault formation, nano-twinning and eventually in situ phase transformation, all of which serve to extend continuous strain hardening which simultaneously elevates strength and ductility (by delaying plastic instability), leading to truly exceptional resistance to fracture.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Fracture Toughness Characterization of Generation II FeCrAl Alloys after ~18 dpa Irradiation

FeCrAl alloys are promising candidate materials for the accident tolerant fuel (ATF) cladding applications due to their excellent corrosion resistance to the elevated temperature steam environment. Currently, the handbook on FeCrAl material properties contains only limited data regarding the fracture toughness properties of any FeCrAl alloy. This includes alloys currently under investigation within the Advanced Fuels Campaign (AFC) at Oak Ridge National Laboratory (ORNL). In this project, a series of irradiation capsules have been irradiated in the High Flux Isotope Reactor (HFIR) at ORNL with two Generation II FeCrAl candidate alloys, i.e., C06M and C36M, to assess the fracture response of these alloys after neutron irradiation. These alloys represent the “book-end” compositions for C26M, the alloy currently being developed as the leading candidate for LWR cladding. A total of six irradiation capsules were irradiated in HFIR at target temperatures of 200°C, 330°C, and 500°C up to target damage doses of 8 displacements per atom (dpa) and 16 dpa. These damage doses represent the expected middle and end of life damage levels for typical LWR cladding while the irradiation temperature regimes will provide insight into the role of varying microstructural features on the fracture toughness properties of neutron irradiated FeCrAl alloys. To date, irradiation of all capsules has been completed in HFIR. This report summarizes the latest results of microhardness and fracture toughness PIE for the 16 dpa capsules (FCAB2, FCAB4, and FCAB6), for which the measured irradiation conditions were: 204°C/17.6dpa, 343°C/18.3dpa, and 507°C/18.6dpa. The main conclusions of this study can be summarized as follows: 1) After the 204°C/17.6dpa irradiation, both C06M and C36M exhibited significant irradiation hardening and embrittlement 2) After the 343°C/18.3dpa irradiation, both C06M and C36M exhibited small irradiation hardening without irradiation embrittlement 3) After the 507°C/18.6dpa irradiation, both C06M and C36M exhibited irradiation softening without irradiation embrittlement 4) Comparing the microhardness and Master Curve reference temperature T 0q before and after neutron irradiation, we did not observe a linear correlation between the two parameters for both C06M and C36M. This should be mainly due to a flat response of the Master Curve reference temperature T 0q to the irradiations at 166-204°C and 315-343°C ranges 5) C06M showed a lower T 0q , meaning better toughness, than C36M at the unirradiated condition and such trend was kept even after neutron irradiation except for the 166-204°C irradiation where both materials had similar T 0q . 6) In terms of hardening and embrittlement, the irradiation effect on both C06M and C36M appeared to saturate after an irradiation dose of 7 dpa.

36 MATERIALS SCIENCE↗

NASA NTRS1972

An Experimental Investigation of the Effects of Vacuum Environment on the Fatigue Life, Fatigue-Crack-Growth Behavior, and Fracture Toughness of 7075-T6 Aluminum Alloy

Axial load fatigue life, fatigue-crack propagation, and fracture toughness tests were conducted on 0.090-inch thick specimens made of 7075-T6 aluminum alloy. The fatigue life and fatigue-crack propagation experiments were conducted at a stress ratio of 0.02. Maximum stresses ranged from 33 to 60 ksi in the fatigue life experiments, and from 10 to 40 ksi in the fatigue-crack propagation experiments, and fatigue life experiments were conducted at gas pressures of 760, 0.5, 0.05, and 0.00000005 torr. Fatigue-crack-growth and fracture toughness experiments were conducted at gas pressures of 760 and 5 x 10 to the minus 8th power torr. Residual stress measurements were made on selected fatigue life specimens to determine the effect of such stresses on fatigue life. Analysis of the results from the fatigue life experiments indicated that fatigue life progressively increased as the gas pressure decreased. Analysis of the results from the fatigue-crack-growth experiments indicates that at low values of stress-intensity range, the fatigue crack growth rates were approximately twice as high in air as in vacuum. Fracture toughness data showed there was essentially no difference in the fracture toughness of 7075-T6 in vacuum and in air.

Hudson, C. M.↗

NASA NTRS1973

Effect of specimen thickness of fatigue-crack-growth behavior and fracture toughness of 7075-T6 and 7178-T6 aluminum alloys

A study was made to determine the effects of specimen thickness on fatigue crack growth and fracture behavior of 7075-T6 and 7178-T6 aluminum alloy sheet and plate. Specimen thicknesses ranged from 5.1 to 12.7 mm (0.20 to 0.50 in.) for 7075-T6 and from 1.3 to 6.4 mm (0.05 to 0.25 in.) for 7178-T6. The stress ratios R used in the crack growth experiments were 0.02 and 0.50. For 7075-T6, specimen thickness had relatively little effect on fatigue-crack growth. However, the fracture toughness of the thickness of the thickest gage of 7075-T6 was about two-thirds of the fracture toughness of the thinner gages of 7075-T6. For 7178-T6, fatigue cracks generally grew somewhat faster in the thicker gages than in the thinnest gage. The fracture toughness of the thickest gage of 7178-T6 was about two-thirds of the fracture toughness of the thinner gages of 7178-T6. Stress intensity methods were used to analyze the experimental results. For a given thickness and value of R, the rate of fatigue crack growth was essentially a single-valued function of the stress intensity range for 7075-T6 and 7178-T6. An empirical equation developed by Forman, Kearney, and Engle fit the 7075-T6 and 7178-T6 crack growth data reasonably well.

Hudson, C. M.↗

NASA NTRS1973

The effect of microstructure on the fracture toughness of titanium alloys

The high-strength titanium alloys are widely used in aircraft and aerospace structures due to their high strength to density ratios. In such applications, the fracture toughness rather than the strength is often the factor which requires larger size sections and lower useful payloads. The response of the strength and toughness of titanium alloys was analyzed generally without regard to the fracture mode or the effect of microstructure on the fracture mechanisms. Research on the fracture mechanisms in aluminum alloys and steels showed that the toughness may be improved by decreasing the sizes of inclusions and sub-micron precipitates. An investigation was conducted to study the fracture mechanisms in titanium alloys which may lead to suggestions for the improvement of the fracture toughness without a corresponding loss in strength.

Vanstone, R. H.↗

NASA NTRS1976

Effect of water and ice on strength and fracture toughness of intermittently bonded boron-epoxy composites

The effects of water and ice on the strength and fracture toughness of boron-epoxy composites with polyurethane intermittent bonding have been investigated. Neither simple soaking in water nor soaking followed by freezing and thawing have marked effects on the strength of the fully-coated composites, but they have disastrous effects on the uncoated composites. Toughness is affected only marginally, with some small reductions in the fully-coated samples, and with essentially no effect on the uncoated composites. An analysis is presented which explains adequately the experimental strength and toughness results obtained, and which is based on an argument that water absorption reduces the interfacial shear strength only of the uncoated areas and not those regions coated by the polyurethane varnish. The results indicate that the advantages of appropriate intermittent bonding (i.e., high strength combined with high toughness) are retained in wet conditions so that such composites may be favorably used in such adverse environmental conditions.

Atkins, A. G.↗

NASA NTRS1987

Interlaminar shear fracture toughness and fatigue thresholds for composite materials

Static and cyclic end notched flexure tests were conducted on a graphite epoxy, a glass epoxy, and graphite thermoplastic to determine their interlaminar shear fracture toughness and fatigue thresholds for delamination in terms of limiting values of the mode II strain energy release rate, G-II, for delamination growth. The influence of precracking and data reduction schemes are discussed. Finite element analysis indicated that the beam theory calculation for G-II with the transverse shear contribution included was reasonably accurate over the entire range of crack lengths. Cyclic loading significantly reduced the critical G-II for delamination. A threshold value of the maximum cyclic G-II below which no delamination occurred after one million cycles was identified for each material. Also, residual static toughness tests were conducted on glass epoxy specimens that had undergone one million cycles without delamination. A linear mixed-mode delamination criteria was used to characterize the static toughness of several composite materials; however, a total G threshold criterion appears to characterize the fatigue delamination durability of composite materials with a wide range of static toughness.

Obrien, T. Kevin↗

NASA NTRS1989

Interlaminar shear fracture toughness and fatigue thresholds for composite materials

O'Brien, T. Kevin↗

NASA NTRS1992

Strength, toughness and R-curve behaviour of SiC whisker-reinforced composite Si3N4 with reference to monolithic Si3N4

The flexural strength and fracture toughness of 30 vol pct SiC whisker-reinforced Si3N4 material were determined as a function of temperature from 25 to 1400 C in an air environment. It was found that both strength and toughness of the composite material were almost the same as those of the monolithic counterpart. The room-temperature strength was retained up to 1100 C; however, appreciable strength degradation started at 1200 C and reached a maximum at 1400 C due to stable crack growth. In contrast, the fracture toughness of the two materials was independent of temperature with an average value of 5.66 MPa sq rt m. It was also observed that the composite material exhibited no rising R-curve behavior at room temperature, as was the case for the monolithic material. These results indicate that SiC whisker addition to the Si3N4 matrix did not provide any favorable effects on strength, toughness and R-curve behavior.

Choi, S. R.↗

NASA NTRS1990

A laboratory means to produce tough aluminum sheet from powder

The rapid solidification of aluminum alloys as powder and the subsequent fabrication processes can be used to develop and tailor alloys to satisfy specific aerospace design requirements, including high strength and toughness. Laboratory procedures to produce aluminum powder-metallurgy (PM) materials are efficient but require evidence that the laboratory methods used can produce a product with superior properties. This paper describes laboratory equipment and procedures which can be used to produce tough aluminum PM sheet. The processing of a 2124 + 0.9 percent Zr aluminum alloy powder is used as an example. The fully hardened sheet product is evaluated in terms of properties and microstructure. The key features of the vacuum hot press pressing operation used to consolidate the powder are described. The 2124 + 0.9 percent Zr - T8 temper aluminum sheet produced was both strong (460-490 MPa yield strength) and tough (Kahn Tear unit-propagation- energy values over three times those typical for ingot metallurgy 2024-T81). Both the longitudinal and longitudinal-transverse directions of the sheet were tested. The microstructure was well refined with subgrains of one or two micrometers. Fine dispersoids of Al3Zr in the precipitate free regions adjacent to boundaries are believed to contribute to the improved toughness.

Singleton, O. R.↗

NASA NTRS1995

Effects of stitching on fracture toughness of uniweave textile graphite/epoxy laminates

The effects of through-the-thickness stitching on impact damage resistance, impact damage tolerance, and Mode 1 and Mode 2 fracture toughness of textile graphite/epoxy laminates were studied experimentally. Graphite/epoxy laminates were fabricated from AS4 graphite uniweave textiles and 3501-6 epoxy using Resin Transfer Molding. The cloths were stitched with Kevlar(tm) and glass yarns before resin infusion. Delamination was implanted during processing to simulate impact damage. Sublaminate buckling tests were performed in a novel fixture to measure Compression After Impact (CAI) strength of stitched laminates. The results show that CAI strength can be improved up to 400% by through-the-thickness stitching. Double Cantilever Beam tests were performed to study the effect of stitching on Mode 1 fracture toughness G(sub 1c). It was found that G(sub 1c) increased 30 times for a low stitching density of 16 stitches/sq in. Mode 2 fracture toughness was measured by testing the stitched beams in End Notch Flexure tests. Unlike in the unstitiched beams, crack propagation in the stitched beams was steady. The current formulas for ENF tests were not found suitable for determining G(sub 2C) for stitched beams. Hence two new methods were developed - one based on crack area measured from ultrasonic C-scanning and the other based on equivalent crack area measured from the residual stiffness of the specimen. The G(sub 2c) was found to be at least 5-15 times higher for the stitched laminates. The mechanisms by which stitching increases the CAI strength and fracture toughness are discussed.

Sankar, Bhavani V.↗

NASA NTRS1996

A New Aging Treatment for Improving Cryogenic Toughness of the Main Structural Alloy of the Super Lightweight Tank

Marshall Space Flight Center (MSFC) has developed a new technique that can enhance cryogenic fracture toughness and reduce the statistical spread of toughness values in alloy 2195. This aging treatment can control the location and size of strengthening precipitate T1, making improvements possible in cryogenic fracture toughness (CFT) and fracture toughness ratio (FTR). At the start of this program, design of experiments (DOE) ingot No. 10 was used as a baseline for aging process development and optimization. The new aging treatment was found to be very effective, improving CFT by approximately 15 to 20 percent for DOE ingot No. 10. To further evaluate the repeatability and effectiveness of this new treatment, the investigators selected and tested three more lots of alloy 2195, using 1.75-in-thick gauge plates with FTR values ranging from 0.85 to 1.07. The new aging treatment effectively enhanced CFT and FTR values for all three lots. In one instance, the material was considered rejectable because it did not meet the minimum FTR value (1.0) of the super lightweight tank (SLWT). The new aging treatment improved its FTR from 0.85 to 1.01, making this material acceptable for use in the SLWT.

Chen, P. S.↗

NASA NTRS1997

Strong, Tough, and Pest Resistant MoSi2-Base Hybrid Composite for Structural Applications

Addition of about 30 to 50 vol % of Si3N4 particulate to MoSi2 improved resistance to low temperature accelerated oxidation by forming a Si2ON2 protective scale and thereby eliminating catastrophic 'pest failure'. The Si3N4 addition also improved the high temperature creep strength by nearly five orders of magnitude, doubled the room temperature toughness and significantly lowered the CTE of the MoSi2 and eliminated matrix cracking in SCS-6 reinforced composites even after thermal cycling. The SCS-6 fiber reinforcement improved the room temperature fracture toughness by seven times and impact resistance by five times. The composite exhibited excellent strength and toughness improvement up to 1400 C. More recently, tape casting was adopted as the preferred processing of MoSi2-base composites for improved fiber spacing, ability to use small diameter fibers, and for lower cost. Good strength and toughness values were also obtained with fine diameter Hi-Nicalon tow fibers. This hybrid composite remains competitive with ceramic matrix composites as a replacement for Ni-base superalloys in aircraft engine applications.

Hebsur, M. G.↗

NASA NTRS2003

Effect of Elevated Temperature and Loading Rate on Delamination Fracture Toughness

The effects of temperature and loading rate on delamination growth were studied. The delamination fracture toughness of IM7/K3B was measured at 149 C, 177 C, and 204 C. At each temperature the tests were performed with a variety of loading rates so that the delamination initiated over the range of time from 0.5 sec to 24 hrs. The double cantilever beam (DCB) test was used to measure fracture toughness. The results showed that the delamination resistance is a complicated function of both time and temperature with the effect of temperature either increasing or decreasing the fracture toughness depending on the time scale. The results also showed that the fracture toughness changed by as much as a factor of three as the time scale changed over the five orders of magnitude tested.

Reeder, J. R.↗

NASA NTRS2006

Effect of Embedded Piezoelectric Sensors on Fracture Toughness and Fatigue Resistance of Composite Laminates Under Mode I Loading

Double-cantilevered beam (DCB) specimens of a glass/epoxy composite material with embedded piezoelectric sensors were tested both statically and under fatigue loading to determine the effect of the embedded material on the Mode I fracture toughness and fatigue resistance compared to baseline data without the embedded elements. A material known as LaRC-Macrofiber Composite (LaRC-MFC (TradeMark)), or MFC, was embedded at the midplane of the specimen during the layup. Specimens were manufactured with the embedded MFC material either at the loaded end of the specimen to simulate an initial delamination; or with the MFC material located at the delaminating interface, with a Teflon film at the loaded end to simulate an initial delamination. There were three types of specimens with the embedded material at the delaminating interface: co-cured with no added adhesive; cured with a paste adhesive applied to the embedded element; or cured with a film adhesive added to the embedded material. Tests were conducted with the sensors in both the passive and active states. Results were compared to baseline data for the same material without embedded elements. Interlaminar fracture toughness values (G(sub Ic)) for the passive condition showed little change when the MFC was at the insert end. Passive results varied when the MFC was at the delaminating interface. For the co-cured case and with the paste adhesive, G(sub Ic) decreased compared to the baseline toughness, whereas, for the film adhesive case, G(sub Ic) was significantly greater than the baseline toughness, but the failure was always catastrophic. When the MFC was in the active state, G(sub Ic) was generally lower compared to the passive results. Fatigue tests showed little effect of the embedded material whether it was active or passive compared to baseline values.

Murri, Gretchen B.↗

NASA NTRS2006

Dynamic Fracture Initiation Toughness at Elevated Temperatures With Application to the New Generation of Titanium Aluminide Alloys

Recently, a new generation of titanium aluminide alloy, named Gamma-Met PX, has been developed with better rolling and post-rolling characteristics. I'revious work on this alloy has shown the material to have higher strengths at room and elevated temperatures when compared with other gamma titanium aluminides. In particular, this new alloy has shown increased ductility at elevated temperatures under both quasi-static and high strain rate uniaxial compressive loading. However, its high strain rate tensile ductility at room and elevated temperatures is limited to approx. 1%. In the present chapter, results of a study to investigate the effects of loading rate and test temperature on the dynamic fracture initiation toughness in Gamma-Met PX are presented. Modified split Hopkinson pressure bar was used along with high-speed photography to determine the crack initiation time. Three-point bend dynamic fracture experiments were conducted at impact speeds of approx. 1 m/s and tests temperatures of up-to 1200 C. The results show that thc dynamic fracture initiation toughness decreases with increasing test temperatures beyond 600 C. Furthermore, thc effect of long time high temperature air exposure on the fracture toughness was investigated. The dynamic fracture initiation toughness was found to decrease with increasing exposure time. The reasons behind this drop are analyzed and discussed.

Shazly, Mostafa↗