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DOE OSTI2020

Preparation, mechanical properties, and toughening mechanisms of SiCw/SiCp‐reinforced zirconia‐toughened alumina ceramics

ABSTRACT Zirconia‐toughened alumina (ZTA) ceramics with high mechanical properties were sintered by hot‐pressing method using SiC particles (SiCp) and SiC whiskers (SiCw) as the reinforcing agents simultaneously. The influences of sintering temperature, SiCp, and SiCw contents on the microstructure and mechanical properties of ZTA ceramics were investigated. It was found that both SiCp and SiCw could contribute to grain refinement significantly and promote the mechanical properties of the ceramics. However, the excess addition of SiCp or SiCw led to the formation of pores with large sizes and degraded the mechanical properties instead. When 13 wt% SiCp was introduced, the maximum flexural strength of 1180.0 MPa and fracture toughness of 15.9 MPa·m 1/2 were obtained, whereas the maximum flexural strength of 1314.0 MPa and fracture toughness of 14.7 MPa·m 1/2 were achieved at 20 wt% SiCw. Interestingly, the simultaneous addition of SiCp and SiCw could further improve the mechanical properties, and the highest flexural strength of 1334.0 MPa and fracture toughness of 16.0 MPa·m 1/2 were achieved at a SiCw/SiCp ratio of 16/4. The reinforcement mechanisms in the ceramics mainly included the phase transformation toughening of ZrO 2 , the crack deflection and bridging of SiCp and SiCw, and the pull‐out of SiCw.

Liu, Longyang↗

NASA NTRS1984

Fracture temperature and flaw growth in nitronic 40 at cryogenic temperatures

The fracture resistance and fatigue response of Armco Nitronic 40 austenitic stainless steel were evaluated under cryogenic conditions. Tensile, fracture toughness and fatigue crack growth properties were measured at -275 F. The tensile yield strength was approximately 120 ksi and the fracture toughness was estimated to be 350 ksi-in /2 on the basis of fracture toughness measurements. Testing was conducted to evaluate the behavior of a simulated section of the wing of the Pathfinder 1 model subject to a load and temperature history typical of that for testing in the National Transonic Facility. The wing section model incorporated a proposed brazing technique for pressure-transducer attachment. The simulated wing section performed satisfactorily at stress levels of nearly 60 percent of the material yield strength. The brazing technique proved to be an effective method of transducer attachment under conditions of high stress levels and large temperature excursions.

Domack, M. S.↗

NASA NTRS1986

Effect of laminate thickness and specimen configuration on the fracture of laminated composites

Attention is given to the effect of laminate thickness on graphite/epoxy laminates in the present measurements of fracture toughness in center cracked tension specimens, compact tension specimens, and three-point bend specimens. Crack tip damage development prior to fracture is also studied. The results obtained show fracture toughness to be a function of laminate thickness, being in all cases independent of crack size. The fracture surface of all thick laminates was uniform in the interior and self-similar with the starter notch. With only one exception, the fracture toughness of the thicker laminates was relatively independent of specimen configuration.

Harris, C. E.↗

DOE OSTI2020

J-integral measured from experimental torque load versus torque-ends rotation angle obtained from a spiral notch torsion test

In this work, Spiral Notch Torsion Test (SNTT) was developed to measure the intrinsic fracture toughness of structural materials using small specimens. The SNTT system operates by applying pure torsion to cylindrical specimens with a notch line that spirals around the specimen at a 45° pitch. 3-D finite-element analysis has been used to estimate the fracture toughness obtained from SNTT test specimen with 3-D non-coplanar crack front. Furthermore, here a newly developed SNTT protocol to estimate J-integral directly from the experimental torque load versus torque-ends rotation angle trend curve without the aid of 3-D finite element analyses is presented and its applicability is illustrated by applying it for the evaluation of fracture toughness of SS304/308 weldment. The estimated JQ’ for the SS304/308 weld is 144.2 kJ/m2, which is consistent with that obtained from CT specimen.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Thermomechanical Processing for Improved Mechanical Properties of HT9 Steels

Thermomechanical processing (TMP) of ferritic–martensitic (FM) steels, such as HT9 (Fe–12Cr–1MoWV) steels, involves normalizing, quenching, and tempering to create a microstructure of fine ferritic/martensitic laths with carbide precipitates. HT9 steels are used in fast reactor core components due to their high-temperature strength and resistance to irradiation damage. However, traditional TMP methods for these steels often result in performance limitations under irradiation, including embrittlement at low temperatures (<~430 °C), insufficient strength and toughness at higher temperatures (>500 °C), and void swelling after high-dose irradiation (>200 dpa). This research aimed to enhance both fracture toughness and strength at high temperatures by creating a quenched and tempered martensitic structure with ultrafine laths and precipitates through rapid quenching and unconventional tempering. Mechanical testing revealed significant variations in strength and fracture toughness depending on the processing route, particularly the tempering conditions. Tailored TMP approaches, combining rapid quenching with limited tempering, elevated strength to levels comparable to nano-oxide strengthened ferritic alloys while preserving fracture toughness. For optimal properties in high-Cr steels for future reactor applications, this study recommends a modified tempering treatment, i.e., post-quench annealing at 500 °C or 600 °C for 1 h, possibly followed by a brief tempering at a slightly higher temperature.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Mechanical testing of PH13-8Mo H950 Steel for Xue-Wierzbicki Fracture Criterion Determination at 20° C and -40° C

Mechanical testing was conducted to collect the data needed to build a Xue-Wierzbicki (XW) fracture model for PH13-8 Mo H950 stainless steel (PH 13-8 SS). This model is intended for use in structural analysis of this material between room temperature and -40° C. Tests were performed on four different specimen geometries such that a range of stress states were characterized at room temperature and -40° C. Tensile tests on R5 tensile specimens were also performed to assess material anisotropy. Fracture toughness test were also conducted. The fracture toughness of this material at -40° C was 68% of the room-temperature value. Material strength generally increased with decreasing temperature while the opposite trend was observed for ductility. These trends were most pronounced for specimens with the largest stress triaxialities.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Effects of secondary void-initiating particles on the steady-state crack growth resistance of high-strength steel

In this investigation, we focus on the dependence of stable crack growth resistance, as measured by the short-rod fracture toughness test, on secondary void-initiating particles such as AlN and Ti-based grain-refining precipitates in a variety of high-strength steels with tempered martensitic microstructures. The model developed by Ritchie and Thompson is modified to illustrate the significant amounts of toughening that can result from the refinement of secondary particles. Analysis of the data suggests that material strength is a predominant factor in increasing the short-rod fracture toughness relative to linear-elastic measures of initiation fracture toughness, but the extent of toughening is limited by the size and number density of secondary particles in the microstructure. The variation in estimates of secondary microvoid initiation and growth strains with precipitate size reinforce the notion that primary fracture at non-metallic inclusions and secondary fracture at smaller particles occur as sequential processes with a degree of concurrence that is dependent on the state of precipitation in both particle dispersions. Toughening in this connection is maximized by increases in microvoid growth strain that result from decreases in the size and areal number density of secondary void-initiating particles. Finally, the occurrence of transient instabilities during crack extension in short-rod specimens is explained with a phenomenological model that relates crack growth stability to natural variations in the dispersion of secondary void-initiating particles in the microstructure.

42 ENGINEERING↗

NASA NTRS1987

Interfacial strength development in thermoplastic resins and fiber-reinforced thermoplastic composites

An experimental program to develop test methods to be used to characterize interfacial (autohesive) strength development in polysulfone thermoplastic resin and graphite-polysulfone prepreg during processing is reported. Two test methods were used to examine interfacial strength development in neat resin samples. These included an interfacial tension test and a compact tension (CT) fracture toughness test. The interfacial tensile test proved to be very difficult to perform with a considerable amount of data scatter. Thus, the interfacial test was discarded in favor of the fracture toughness test. Interfacial strength development was observed by measuring the refracture toughness of precracked compact tension specimens that were rehealed at a given temperature and contact time. The measured refracture toughness was correlated with temperature and contact time. Interfacial strength development in graphite-polysulfone unidirectional composites was measured using a double cantilever beam (DCB) interlaminar fracture toughness test. The critical strain energy release rate of refractured composite specimens was measured as a function of healing temperature and contact time.

Howes, Jeremy C.↗

NASA NTRS1983

A unifying strain criterion for fracture of fibrous composite laminates

Fibrous composite materials, such as graphite/epoxy, are light, stiff, and strong. They have great potential for reducing weight in aircraft structures. However, for a realization of this potential, designers will have to know the fracture toughness of composite laminates in order to design damage tolerant structures. In connection with the development of an economical testing procedure, there is a great need for a single fracture toughness parameter which can be used to predict the stress-intensity factor (K(Q)) for all laminates of interest to the designer. Poe and Sova (1980) have derived a general fracture toughness parameter (Qc), which is a material constant. It defines the critical level of strains in the principal load-carryng plies. The present investigation is concerned with the calculation of values for the ratio of Qc and the ultimate tensile strain of the fibers. The obtained data indicate that this ratio is reasonably constant for layups which fail largely by self-similar crack extension.

Poe, C. C., Jr.↗

NASA NTRS2016

Slow Crack Growth of Germanium

The fracture toughness and slow crack growth parameters of germanium supplied as single crystal beams and coarse grain disks were measured. Although germanium is anisotropic (A=1.7), it is not as anisotropic as SiC, NiAl, or Cu, as evidence by consistent fracture toughness on the 100, 110, and 111 planes. Germanium does not exhibit significant slow crack growth in distilled water. (n=100). Practical values for engineering design are a fracture toughness of 0.7 MPam and a Weibull modulus of m=6+/-2. For well ground and reasonable handled coupons, fracture strength should be greater than 30 MPa.

Stress Corrosion Susceptibility↗

DOE OSTI2024

Reactive flash sintering and characterization of bulk high entropy nitrides

Over the past decade, numerous high-entropy ceramics have been synthesized, often displaying attractive properties. However, the study on facile preparation of bulk high entropy nitrides (HEN) are limited, despite its broad potential applications. This research demonstrates for the first time rapid fabrication (within ∼6 min) of bulk high-entropy nitrides, especially (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N, from binary nitride powder mixtures using a highly efficient reactive flash sintering (RFS) technique. X-ray diffraction (XRD) shows the HENs from RFS are near single-phase solid solutions with a rock salt crystal structure, while in situ synchrotron study carried out during RFS captured in real time the formation of HEN, which was preserved upon cooling, suggesting thermodynamic stability of the HEN phase, even up to extreme pressure (∼35.6 GPa). Microscopic analyses using SEM, STEM, and EDS reveal decent uniformity for HEN with no obvious segregation of elements, even to submicron scale. Some properties of the obtained bulk HENs are consistent with expectations. For example, their hardness and bulk modulus are close to estimates based on rule-of-mixture (ROM) values from the constituent binary nitrides. Meanwhile, some other measured properties seem to show surprises. For example, the fracture toughness for the HENs (e.g., 7.81 ± 1.40 MPa•m 1/2 or higher) turns out to be more than double of the expected ROM estimates. The significantly improved fracture toughness is attributed to the observed nano-layered structure of the HENs, despite the HEN’s cubic crystal structure and high hardness. In addition, the oxidation resistance shows improvement up till ∼800°C, possibly due to Ta doping that suppress oxygen vacancy formation in the oxide shell, while the 5-metal HEN of (Al 0.17 Nb 0.17 Ta 0.17 Ti 0.32 Zr 0.17 )N displays superconductivity (T c of ∼5–7 K from magnetism and resistivity measurements, slightly lower than ROM estimate), despite insulating property of starting AlN. Furthermore, future study combining experimental investigation using larger samples to confirm the observed increase in fracture toughness and oxidation resistance, theoretical modeling at different length scale, and more detailed structural/chemical characterization, especially at the atomic scale, are all needed to fully understand the inter-relationships between composition, processing, structure, and novel properties for these HENs and the development of related new materials for different applications.

Flash sintering↗

NASA NTRS1974

Fracture mechanics data for 2024-T861 and 2124-T851 aluminum

The fracture toughness and fatigue flaw growth characteristics of 2024-T861 and 2124-T851 aluminum were evaluated under plane stress conditions. Center cracked tension specimens were employed to evaluate these properties under a number of different test conditions which included variations in specimen thickness, specimen orientation, test environment, and initial flaw size. The effect of buckling was also investigated for all tests of thin gage specimens, and the effect of frequency and stress ratio was evaluated for the cyclic tests. Fracture toughness test results were analyzed and presented in terms of fracture resistance curves; fatigue flaw growth data was analyzed using empirical rate models. The results of the study indicate that both fracture toughness and resistance to fatigue crack growth improve with increasing temperature and decreasing thickness. The presence of buckling during testing of thin gage panels was found to degrade the resistance to fatigue flaw growth only at elevated temperatures.

Pionke, L. J.↗

NASA NTRS2022

Fracture Mechanics Properties of Fused Silicas Used for International Space Station Windowpanes

The fracture toughness and slow crack growth (SCG) parameters of a quartz-based silica and a high-purity fused silica were measured as part of a program to review the reliability of the International Space Station windows. The materials exhibit the same fracture toughness (.75 MPa m^(1/2) in N2) and very similar SCG parameters. The literature on fused silica indicates excellent agreement of fracture toughness, but a very wide range of SCG parameters, even from the same institution, with strength-based methods usually yielding a lower power law exponent than direct crack velocity measurements. Use of the exponential function is shown to provide better agreement between test methods, with velocity curves derived from strength tests of bare fiber and polished or ground test specimens paralleling those from wide-range, direct crack velocity observations, implying that constant stress rate tests can predict long lifetime via the exponential function. However, much variation still exists. SCG parameters for soda–lime silicate are much less sensitive to the test method than fused silica. Static load tests and stress intensity measurements resulted in a fatigue threshold of .3 MPa m^(1/2) for fused silica.

Silica, toughness, impact, crack growth, windows, ↗

NASA NTRS1986

Effect of adherend thickness and mixed mode loading on debond growth in adhesively bonded composite joints

Symmetric and unsymmetric double cantilever beam (DCB) specimens were tested and analyzed to assess the effect of: (1) adherend thickness, and (2) a predominantly mode I mixed mode loading on cyclic debond growth and static fracture toughness. The specimens were made of unidirectional composite (T300/5208) adherends bonded together with EC3445 structural adhesive. The thickness was 8, 16, or 24 plies. The experimental results indicated that the static fracture toughness increases and the cyclic debond growth rate decreases with increasing adherend thickness. This behavior was related to the length of the plastic zone ahead of the debond tip. For the symmetric DCB specimens, it was further found that displacement control tests resulted in higher debond growth rates than did load control tests. While the symmetric DCB tests always resulted in cohesive failures in the bondline, the unsymmetric DCB tests resulted in the debond growing into the thinner adherend and the damage progressing as delamination in that adherend. This behavior resulted in much lower fracture toughness and damage growth rates than found in the symmetric DCB tests.

Mangalgiri, P. D.↗

NASA NTRS1986

The effects of biaxial loading on the fracture characteristics of several engineering materials

Using the George Washington University biaxial test system, a static fracture toughness study of two polymers (PMMA and PVC) and three aluminum alloys was performed for several variations in specimen geometry. Photoelastic experiments indicate that the applied load biaxiality has a very strong influence on the size and shape of the crack-tip stress field, and fracture toughness values for both polymers were seen to decrease with increasing load biaxiality. The load biaxiality was also found to have a strong influence on the crack growth direction in PMMA and a negligible influence on the PVC. The 7075-T6 aluminum toughness values increased with biaxiality, while intermediate peak toughness values were noted at a 0.5 biaxiality ratio for the more ductile 2024-T3 and 6061-T4 alloys. Fracture toughnesses at the highest biaxiality ratios were found to be equal to the uniaxial results.

Jones, D. L.↗

DOE OSTI2021

Multifunctional application of nanoscratch technique to characterize cementitious materials

This study aims to further explore the multifunctional applicability of nanoscratch technique to cementitious materials for comprehensive characterization. Based on the investigation of deformation, applied force, and fracture toughness of hardened cement paste during scratching, the methods of phase identification, fracture toughness of individual phase, and the interfacial transition zone (ITZ) thickness quantification were proposed and discussed. After redefining the vertical loading rate of scratching, the slope of the square scratching depth vs. scratching length is recognized as a reliable parameter to distinguish the individual phases for the first time. A fracture toughness-based method is proposed to quantify the thickness of ITZ between clinker and hydrates. Meanwhile, the applicability of phase identification by the scratch method is discussed for different transverse scratching speeds and the vertical loading rates. The findings will benefit the investigation and mechanism understanding of cementitious materials at the microscale by utilizing nanoscratch technique.

36 MATERIALS SCIENCE↗

NASA NTRS1989

Evaluation of the split cantilever beam for Mode 3 delamination testing

A test rig for testing a thick split cantilever beam for scissoring delamination (mode 3) fracture toughness was developed. A 3-D finite element analysis was conducted on the test specimen to determine the strain energy release rate, G, distribution along the delamination front. The virtual crack closure technique was used to calculate the G components resulting from interlaminar tension, GI, interlaminar sliding shear, GII, and interlaminar tearing shear, GIII. The finite element analysis showed that at the delamination front no GI component existed, but a GII component was present in addition to a GIII component. Furthermore, near the free edges, the GII component was significantly higher than the GIII component. The GII/GIII ratio was found to increase with delamination length but was insensitive to the beam depth. The presence of GII at the delamination front was verified experimentally by examination of the failure surfaces. At the center of the beam, where the failure was in mode 3, there was significant fiber bridging. However, at the edges of the beam where the failure was in mode 3, there was no fiber bridging and mode 2 shear hackles were observed. Therefore, it was concluded that the split cantilever beam configuration does not represent a pure mode 3 test. The experimental work showed that the mode 2 fracture toughness, GIIc, must be less than the mode 3 fracture toughness, GIIIc. Therefore, a conservative approach to characterizing mode 3 delamination is to equate GIIIc to GIIc.

Martin, Roderick H.↗

NASA NTRS1991

Evaluation of the split cantilever beam for mode III delamination testing

Martin, Roderick, H.↗