Tungsten Strongly Inhibits Sintering of Porous Iron During High-Temperature Redox Cycling.

Freeze-cast Fe-25 W (at%) lamellar foams show excellent resistance to degradation at 800 °C during steam-hydrogen redox cycling between the metallic and oxide states, with fast reaction kinetics maintained up to at least 100 redox cycles with full Fe utilization. This very high stability stems from the sintering inhibition of W combined with the freeze-cast architecture and the chemical vapor transport (CVT) mechanism of reduction. These three factors create a hierarchical porosity in the foam, consisting of i) macroscopic elongated channels, ii) micro-scale sintering inhibition pores, and iii) submicron CVT pores. Microstructural characterization via SEM and EDS is combined with in situ XRD to fully explore the phase evolution and microstructural impact of W on Fe during redox cycling. Comparison with tapped Fe-25 W (at%) powder beds reveals that the freeze-cast channels and lamellae are not critical to the performance of the material.

Ink-Extrusion 3D Printing and Silicide Coating of HfNbTaTiZr Refractory High-Entropy Alloy for Extreme Temperature Applications.

An oxygen-resistant refractory high-entropy alloy is synthesized in microlattice or bulk form by 3D ink-extrusion printing, interdiffusion, and silicide coating. Additive manufacturing of equiatomic HfNbTaTiZr is implemented by extruding inks containing hydride powders, de-binding under H2, and sintering under vacuum. The sequential decomposition of hydride powders (HfH2+NbH+TaH0.5+TiH2+ZrH2) is followed by in situ X-ray diffraction. Upon sintering at 1400 °C for 18 h, a nearly fully densified, equiatomic HfNbTaTiZr alloy is synthesized; on slow cooling, both α-HCP and ß-BCC phases are formed, but on quenching, a metastable single ß-BCC phase is obtained. Printed and sintered HfNbTaTiZr alloys with ≈1 wt.% O shows excellent mechanical properties at high temperatures. Oxidation resistance is achieved by silicide coating via pack cementation. A small-size lattice-core sandwich is fabricated and tested with high-temperature flames to demonstrate the versatility of this sequential approach (printing, sintering, and siliconizing) for high-temperature, high-stress applications of refractory high-entropy alloys.

Cavitation-resistant intergranular precipitates enhance creep performance of θ'-strengthened Al-Cu based alloys.

Tensile and compressive creep properties of a quaternary Al-Cu-Mn-Zr (ACMZ) alloy and its commercial counterpart (Al-Cu-Mn-Zr with Ni, Co and Sb additions, RR350) are investigated at 300° C. At low stresses up to 30 MPa where diffusional creep dominates, creep resistance is the same in tension and compression and RR350 deforms more slowly than ACMZ, consistent with RR350 alloy's larger linear fraction of intergranular precipitates (Al7 Cu2 (NiFe) and Al9 FeNi for RR350 vs. θ-Al2 Cu for ACMZ) and a reduced fraction of precipitate-free zones near grain boundaries. At stresses between 30 and 80 MPa, dislocation creep with a stress exponent n ~ 3 becomes rate-limiting in compression, which is expected to be controlled by θ'precipitates within the grain bulk. By contrast, in tension, enhanced creep rate and higher apparent stress exponents are measured, consistent with cavitation at intergranular precipitates becoming increasingly dominant as the stress increases. In the dislocation creep regime, RR350 alloy is again more creep resistant than ACMZ alloy, which is related to three mechanisms (i) a reduced fraction of softer precipitate-free zones, (ii) more effective load transfer to intergranular precipitates, and (iii) reduced cavitation. A model for cavitation is applied to calculate tensile creep rates from compressive creep rates and the model successfully predicts the improved tensile creep resistance of the RR350 alloy. The present investigation underscores the importance of intergranular grain boundary precipitates, in addition to strengthening θ' precipitates, in enhancing the creep resistance of Al-Cu alloys.

Comparing evolution of precipitates and strength upon aging of cast and laser-remelted Al-8Ce-0.2Sc-0.1Zr (wt.%).

The microstructural evolutions, upon solidification and subsequent aging, and associated hardening effects for both cast and laser-surface-remelted Al-8Ce-0.2Sc-0.1Zr (wt.%) hypo-eutectic alloy are investigated with focus on precipitation and coarsening behavior of their Al11Ce3 and L12-Al3(Sc,Zr) precipitates. Laser surface remelting, which produces solidification conditions typical of additive manufacturing (AM) processes, suppresses formation of undesirable primary Al11Ce3 and Al3(Sc,Zr) precipitates on solidification. It also greatly refines the interlamellar spacing of the eutectic Al11Ce3 phase, thus enhancing the Orowan strengthening effect as compared to the cast alloy, beyond the load-transfer effect from the Al11Ce3 phase. Subsequent aging at 325 °C leads to further hardening of both alloys due to secondary Al3(Sc,Zr) nanoprecipitation, with much more pronounced hardness increases in the laser-remelted alloy, owing to a higher number density of finer Al3(Sc,Zr) nano-precipitates, as compared to the cast alloy. This improvement is rationalized by an enhancement of Al3(Sc,Zr) nucleation rate upon aging of laser-remelted alloy, as compared to the cast alloy, considering differences in elemental supersaturation within the α-Al regions of these alloys. Prolonged aging, up to 1000 h, at 325 °C causes the hardness of both alloys to decline relatively slowly, implying that this alloy is suitable for AM processes and subsequent applications where high strength and good heat resistance are needed.

Enhanced age-hardening response and creep resistance of an Al-0.5Mn-0.3Si (at.%) alloy by Sn inoculation.

Precipitation-strengthening at ambient and high temperatures is examined in Al-0.5Mn-0.3Si (at.%) alloys with and without 0.02 at.% Sn micro-additions. Isochronal aging experiments reveal that Sn inoculation results in a pronounced age-hardening response: a hardening increment of 125 MPa is achieved at peak-aging (475 °C), which is five times greater than that of a Sn-free alloy. Scanning electron microscopy and synchrotron x-ray diffraction analyses demonstrate that, while the structure of the α-Al(Mn,Fe)Si precipitates formed in the peak-aged alloys is identical, their mean radius is smaller (R ~ 25 vs. 100-500 nm) and their number density is greater (~1021 vs. ~1019-20 m -3) in the Sn-modified alloy. Atom-probe tomography analyses reveal that the enhanced dispersion of the α-precipitates is related primarily to the formation of Sn-rich nanoprecipitates at intermediate temperatures, which act as nucleation sites for Mn-Si-rich nanoprecipitates. High-resolution transmission electron microscopy analyses demonstrate that these Mn-Si-rich nanoprecipitates exhibit icosahedral quasicrystal ordering (I-phase), which transform into the cubic-approximant α-phase upon peak aging. Significant Sn segregation at the semi-coherent interfaces of the α-precipitates in the peak-aged Sn-modified alloy is observed via APT, which promotes homogeneous nucleation of the I/α-precipitates at aging temperatures > 400 °C. At 300 °C, creep threshold stresses are observed in both alloys in the peak-aged state, which increases from ~30 MPa in the Sn-free alloy to ~52 MPa in the Sn-modified alloy. This boost in creep resistance is consistent with the enhanced aging response (higher Orowan stress).

Bulk Nanostructured Metal from Multiply-Twinned Nanowires.

Using chemically synthesized silver nanowires with 5-fold twinning planes as a model system, a bottom-up process to generate a bulk nanostructured metal has been demonstrated. Although the nanowires would be shortened and deformed during densification, they are chosen as a model system because they are currently the most scalable and convenient way to obtain Ag particles with high twinning densities. Direct cold pressing of a silver nanowire filter cake did not generate a sufficiently cohesive sample, while hot pressing at 190 °C for 8 h resulted in extensive sintering, eliminating the nanowire morphology. Copper was then electroplated on the silver nanowires as a binder and filler to increase the densification upon hot pressing; despite nonuniform plating across the thickness of the filter cake, the thermal stability of the nanowires was increased, allowing hot pressing at 390 °C. Finally, a uniform copper coating on silver nanowires was achieved by electroless plating, leading to cohesive bulk metal after hot pressing.

Solute-induced strengthening during creep of an aged-hardened Al-Mn-Zr alloy.

We examine the precipitation and creep behavior of Al-0.5Mn-0.02Si (at.%) alloys, with and without the L12-forming elements Zr and Er (0.09 and 0.05 at.%, respectively), utilizing isochronal aging experiments as well as compressive and tensile creep tests performed between 275 and 400 °C. The Al-0.5Mn-0.09Zr-0.05Er-0.05Si alloy exhibits an unusually high creep resistance in the peak-aged state, which is significantly better than that observed generally in its Mn-free L12-strengthened counterparts; for example, the creep threshold stresses at 300 °C are 34-37 MPa, about three times higher than those in a Mn-free Al-0.11Zr-0.005Er-0.02Si alloy. Scanning transmission electron microscopy illustrates that nanoscale Al 3 (Zr,Er) L1 2 -precipitates are formed in the dendritic cores and micron-sized Al(Mn,Fe)Si α-precipitates in the inter-dendritic channels. Moreover, the Al(f.c.c.)-matrix remains supersaturated with randomly distributed Mn solute atoms, as determined by atom-probe tomography and electrical conductivity measurements, for months at creep temperatures. Creep experiments on the Zr- and Er-free Al-0.5Mn-0.02Si solid-solution alloy reveal a small primary creep strain, a high apparent stress exponent, na ~9-7, and a threshold-stress-type behavior. After ruling out other possible mechanisms, we provide evidence that the threshold stress in this precipitate-free alloy originates from dislocation/solute elastic interactions leading to a strong drag force exerted on edge dislocations, hindering their ability to climb. The relatively high creep resistance of Al-0.5Mn-0.09Zr-0.05Er-0.05Si is interpreted in terms of the synergy between this solute-induced threshold stress (SITS, from Mn in solid-solution) and the known precipitate-bypass threshold stress (from the L12-nanoprecipitates).

Hierarchical Structural Changes During Redox Cycling of Fe-Based Lamellar Foams Containing YSZ, CeO2, or ZrO2.

Several high-temperature energy conversion and storage technologies rely on redox cycling of Fe-based materials, including storage materials in solid-oxide Fe-air batteries and oxygen carriers in chemical-looping combustion. The materials' macroporosity necessary for gas flow is, however, irreversibly diminished during redox cycling due to (i) large volume changes during the redox transformations, (ii) foam sintering at elevated operating temperature (550-900 °C), and (iii) formation and growth of Kirkendall microporosity. To address these challenges, we use directional freeze-casting to create highly porous, lamellar, Fe-composite foams containing uniformly distributed sintering inhibitor (SI) particles-either Y2O3-stabilized ZrO2 (YSZ), CeO2, or ZrO2-at 0, 5, 10, or 15% of the solid volume. We characterize these foams before, during, and after redox cycling (Fe/FeO/Fe3O4, via H2O and H2) at 800 °C using operando synchrotron X-ray microtomography, metallography, and scanning electron microscopy. Shrinkage of the foam volume and formation of a gas-blocking shell surrounding the foam are reduced as the SI fraction increases. Volumetric shrinkage after the first five redox cycles is decreased from 66% (for pure-Fe foams) to 45% (for all Fe-composites containing 5 vol % SI). Foams containing 15 vol % YSZ show no volumetric shrinkage after five cycles, although, after 20 cycles, they have shrunk 53%. Post-cycling analysis reveals segregation of the SI particles to the cores of individual lamellae, surrounded by thick layers of sintered Fe on the lamellae surfaces. This segregation occurs due to Fe diffusion through FeO to the lamellae surfaces during oxidation, leaving behind the SI particles, which are then pushed into clusters by FeO/Fe3O4 contraction during reduction. The SI is thus rendered ineffective, which explains why foam densification is delayed (compared with pure-Fe foams), rather than fully prevented, after repeated cycling.

3D ink-extrusion additive manufacturing of CoCrFeNi high-entropy alloy micro-lattices.

Additive manufacturing of high-entropy alloys combines the mechanical properties of this novel family of alloys with the geometrical freedom and complexity required by modern designs. Here, a non-beam approach to additive manufacturing of high-entropy alloys is developed based on 3D extrusion of inks containing a blend of oxide nanopowders (Co3O4 + Cr2O3 + Fe2O3 + NiO), followed by co-reduction to metals, inter-diffusion and sintering to near-full density CoCrFeNi in H2. A complex phase evolution path is observed by in-situ X-ray diffraction in extruded filaments when the oxide phases undergo reduction and the resulting metals inter-diffuse, ultimately forming face-centered-cubic equiatomic CoCrFeNi alloy. Linked to the phase evolution is a complex structural evolution, from loosely packed oxide particles in the green body to fully-annealed, metallic CoCrFeNi with 99.6 ± 0.1% relative density. CoCrFeNi micro-lattices are created with strut diameters as low as 100 µm and excellent mechanical properties at ambient and cryogenic temperatures.

Ice-Templated W-Cu Composites with High Anisotropy.

Controlling anisotropy in self-assembled structures enables engineering of materials with highly directional response. Here, we harness the anisotropic growth of ice walls in a thermal gradient to assemble an anisotropic refractory metal structure, which is then infiltrated with Cu to make a composite. Using experiments and simulations, we demonstrate on the specific example of tungsten-copper composites the effect of anisotropy on the electrical and mechanical properties. The measured strength and resistivity are compared to isotropic tungsten-copper composites fabricated by standard powder metallurgical methods. Our results have the potential to fuel the development of more efficient materials, used in electrical power grids and solar-thermal energy conversion systems. The method presented here can be used with a variety of refractory metals and ceramics, which fosters the opportunity to design and functionalize a vast class of new anisotropic load-bearing hybrid metal composites with highly directional properties.

NiTi-Nb micro-trusses fabricated via extrusion-based 3D-printing of powders and transient-liquid-phase sintering.

We present a novel additive manufacturing method for NiTi-Nb micro-trusses combining (i) extrusion-based 3D-printing of liquid inks containing NiTi and Nb powders, solvents, and a polymer binder into micro-trusses with 0/90° ABAB layers of parallel, ∼600 µm struts spaced 1 mm apart and (ii) subsequent heat-treatment to remove the binder and solvents, and then bond the NiTi powders using liquid phase sintering via the formation of a transient NiTi-Nb eutectic phase. We investigate the effects of Nb concentration (0, 1.5, 3.1, 6.7 at.% Nb) on the porosity, microstructure, and phase transformations of the printed NiTi-Nb micro-trusses. Micro-trusses with the highest Nb content exhibit long channels (from 3D-printing) and struts with smaller interconnected porosity (from partial sintering), resulting in overall porosities of ∼75% and low compressive stiffnesses of 1-1.6 GPa, similar to those of trabecular bone and in agreement with analytical and finite element modeling predictions. Diffusion of Nb into the NiTi particles from the bond regions results in a Ni-rich composition as the Nb replaces Ti atoms, leading to decreased martensite/austenite transformation temperatures. Adult human mesenchymal stem cells seeded on these micro-trusses showed excellent viability, proliferation, and extracellular matrix deposition over 14 days in culture. STATEMENT OF SIGNIFICANCE: Near-equiatomic NiTi micro-trusses are attractive for biomedical applications such as stents, actuators, and bone implants because of their combination of biocompatibility, low compressive stiffness, high surface area, and shape-memory or superelasticity. Extrusion-based 3D-printing of NiTi powder-based inks into micro-trusses is feasible, but the subsequent sintering of the powders into dense struts is unachievable due to low diffusivity, large particle size, and low packing density of the NiTi powders. We present a solution, whereby Nb powders are added to the NiTi inks, thus forming during sintering a eutectic NiTi-Nb liquid phase which bonds the solid NiTi powders and improves densification of the struts. This study investigates the microstructure, porosity, phase transformation behavior, compressive stiffness, and cytocompatibility of these printed NiTi-Nb micro-trusses.

Multidimensional Anodized Titanium Foam Photoelectrode for Efficient Utilization of Photons in Mesoscopic Solar Cells.

Mesoscopic solar cells based on nanostructured oxide semiconductors are considered as a promising candidates to replace conventional photovoltaics employing costly materials. However, their overall performances are below the sufficient level required for practical usages. Herein, this study proposes an anodized Ti foam (ATF) with multidimensional and hierarchical architecture as a highly efficient photoelectrode for the generation of a large photocurrent. ATF photoelectrodes prepared by electrochemical anodization of freeze-cast Ti foams have three favorable characteristics: (i) large surface area for enhanced light harvesting, (ii) 1D semiconductor structure for facilitated charge collection, and (iii) 3D highly conductive metallic current collector that enables exclusion of transparent conducting oxide substrate. Based on these advantages, when ATF is utilized in dye-sensitized solar cells, short-circuit photocurrent density up to 22.0 mA cm-2 is achieved in the conventional N719 dye-I3- /I- redox electrolyte system even with an intrinsically inferior quasi-solid electrolyte.

Iron Oxide Photoelectrode with Multidimensional Architecture for Highly Efficient Photoelectrochemical Water Splitting.

Nanostructured metal oxide semiconductors have shown outstanding performances in photoelectrochemical (PEC) water splitting, but limitations in light harvesting and charge collection have necessitated further advances in photoelectrode design. Herein, we propose anodized Fe foams (AFFs) with multidimensional nano/micro-architectures as a highly efficient photoelectrode for PEC water splitting. Fe foams fabricated by freeze-casting and sintering were electrochemically anodized and directly used as photoanodes. We verified the superiority of our design concept by achieving an unprecedented photocurrent density in PEC water splitting over 5 mA cm-2 before the dark current onset, which originated from the large surface area and low electrical resistance of the AFFs. A photocurrent of over 6.8 mA cm-2 and an accordingly high incident photon-to-current efficiency of over 50 % at 400 nm were achieved with incorporation of Co oxygen evolution catalysts. In addition, research opportunities for further advances by structual and compositional modifications are discussed, which can resolve the low fill factoring behavior and improve the overall performance.

Evolution of dealloying induced strain in nanoporous gold crystals.

We studied the evolution of dealloying-induced strain along the {111} in a Ag-Au nano-crystal in situ, during formation of nanoporous gold at the initial stage of dealloying using Bragg coherent X-ray diffractive imaging. The strain magnitude with maximum probability in the crystal doubled in 10 s of dealloying. Although formation of nano-pores just began at the surface, the greatest strain is located 60-80 nm deep within the crystal. Dealloying induced a compressive strain in this region, indicating volume shrinkage occurred during pore formation. The crystal interior showed a small tensile strain, which can be explained by tensile stresses induced by the non-dealloyed region upon the dealloyed region during volume reduction. A surface strain relaxation developed, attributed to atomic rearrangement during dealloying. This clearer understanding of the role of strain in the initial stages of formation of nanoporous gold by dealloying can be exploited for development of new sensors, battery electrodes, and materials for catalysis.

Modeling of Stresses and Strains during (De)Lithiation of Ni3Sn2-Coated Nickel Inverse-Opal Anodes.

Tin alloy-based anodes supported by inverse-opal nanoscaffolds undergo large volume changes from (de)lithiation during cyclic battery (dis)charging, affecting their mechanical stability. We perform continuum mechanics-based simulation to study the evolution of internal stresses and strains as a function of the geometry of the active layer(s): (i) thickness of Ni3Sn2 single layer (30 and 60 nm) and (ii) stacking sequence of Ni3Sn2 and amorphous Si in bilayers (60 nm thick). For single Ni3Sn2 active layers, a thinner layer displays higher strains and stresses, which are relevant to mechanical stability, but causes lower strains and stresses in the Ni scaffold. For Ni3Sn2-Si bilayers, the stacking sequence significantly affects the deformation of the active layers and thus its mechanical stability due to different lithiation behaviors and volume changes.

3D macroporous electrode and high-performance in lithium-ion batteries using SnO2 coated on Cu foam.

A three-dimensional porous architecture makes an attractive electrode structure, as it has an intrinsic structural integrity and an ability to buffer stress in lithium-ion batteries caused by the large volume changes in high-capacity anode materials during cycling. Here we report the first demonstration of a SnO2-coated macroporous Cu foam anode by employing a facile and scalable combination of directional freeze-casting and sol-gel coating processes. The three-dimensional interconnected anode is composed of aligned microscale channels separated by SnO2-coated Cu walls and much finer micrometer pores, adding to surface area and providing space for volume expansion of SnO2 coating layer. With this anode, we achieve a high reversible capacity of 750 mAh g(-1) at current rate of 0.5 C after 50 cycles and an excellent rate capability of 590 mAh g(-1) at 2 C, which is close to the best performance of Sn-based nanoscale material so far.

Microstructure and Creep Properties of Boron- and Zirconium-Containing Cobalt-based Superalloys.

The effects of micro-additions of boron and zirconium on grain-boundary (GB) structure and strength in polycrystalline γ(f.c.c.) plus γ'(L12) strengthened Co-9.5Al-7.5W-X at. % alloys (X = 0-Temary, 0.05B, 0.01B, 0.05Zr, and 0.005B-0.05Zr at. %) are studied. Creep tests performed at 850 °C demonstrate that GB strength and cohesion limit the creep resistance and ductility of the ternary B- and Zr-free alloy due to intergranular fracture. Alloys with 0.05B and 0.005B-0.05Zr both exhibit improved creep strength due to enhanced GB cohesion, compared to the baseline ternary Co-9.5Al-7.5W alloy, but alloys containing 0.01B or 0.05Zr additions displayed no benefit. Atom-probe tomography is utilized to measure GB segregation, where B and Zr are demonstrated to segregate at GBs. A Gibbsian interfacial excess of 5.57 ± 1.04 atoms nm-2 was found for B at a GB in the 0.01B alloy and 2.88 ± 0.81 and 2.40 ± 0.84 atoms nm-2 for B and Zr, respectively, for the 0.005B-0.05Zr alloy. The GBs in the highest B-containing (0.05B) alloy exhibit micrometer-sized boride precipitates with adjacent precipitate denuded-zones (PDZs), whereas secondary precipitation at the GBs is not present in the other four alloys. The 0.05B alloy has the smallest room temperature yield strength, by 6 %, which is attributed to the PDZs, but it exhibits the largest increase in creep strength (with an ~2.5 order of magnitude decrease in the minimum strain rate for a given stress at 850 °C) over the baseline Co-9.5Al-7.5W alloy.

Ferritic Alloys with Extreme Creep Resistance via Coherent Hierarchical Precipitates.

There have been numerous efforts to develop creep-resistant materials strengthened by incoherent particles at high temperatures and stresses in response to future energy needs for steam turbines in thermal-power plants. However, the microstructural instability of the incoherent-particle-strengthened ferritic steels limits their application to temperatures below 900 K. Here, we report a novel ferritic alloy with the excellent creep resistance enhanced by coherent hierarchical precipitates, using the integrated experimental (transmission-electron microscopy/scanning-transmission-electron microscopy, in-situ neutron diffraction, and atom-probe tomography) and theoretical (crystal-plasticity finite-element modeling) approaches. This alloy is strengthened by nano-scaled L21-Ni2TiAl (Heusler phase)-based precipitates, which themselves contain coherent nano-scaled B2 zones. These coherent hierarchical precipitates are uniformly distributed within the Fe matrix. Our hierarchical structure material exhibits the superior creep resistance at 973 K in terms of the minimal creep rate, which is four orders of magnitude lower than that of conventional ferritic steels. These results provide a new alloy-design strategy using the novel concept of hierarchical precipitates and the fundamental science for developing creep-resistant ferritic alloys. The present research will broaden the applications of ferritic alloys to higher temperatures.

Effect of cyclic loading on the nanoscale deformation of hydroxyapatite and collagen fibrils in bovine bone.

Cyclic compressive loading tests were carried out on bovine femoral bones at body temperature (37 °C), with varying mean stresses (-55 to -80 MPa) and loading frequencies (0.5-5 Hz). At various times, the cyclic loading was interrupted to carry out high-energy X-ray scattering measurements of the internal strains developing in the hydroxyapatite (HAP) platelets and the collagen fibrils. The residual strains upon unloading were always tensile in the HAP and compressive in the fibrils, and each increases in magnitude with loading cycles, which can be explained from damage at the HAP­collagen interface and accumulation of plastic deformation within the collagen phase. The samples tested at a higher mean stress and stress amplitude, and at lower loading frequencies exhibit greater plastic deformation and damage accumulation, which is attributed to greater contribution of creep. Synchrotron microcomputed tomography of some of the specimens showed that cracks are produced during cyclic loading and that they mostly occur concentric with Haversian canals.

Effect of stress and temperature on the micromechanics of creep in highly irradiated bone and dentin.

Synchrotron X-ray diffraction is used to study in situ the evolution of phase strains during compressive creep deformation in bovine bone and dentin for a range of compressive stresses and irradiation rates, at ambient and body temperatures. In all cases, compressive strains in the collagen phase increase with increasing creep time (and concomitant irradiation), reflecting macroscopic deformation of the sample. By contrast, compressive elastic strains in the hydroxyapatite (HAP) phase, created upon initial application of compressive load on the sample, decrease with increasing time (and irradiation) for all conditions; this load shedding behavior is consistent with damage at the HAP-collagen interface due to the high irradiation doses (from ~100 to ~9,000 kGy). Both the HAP and fibril strain rates increase with applied compressive stress, temperature and irradiation rate, which is indicative of greater collagen molecular sliding at the HAP-collagen interface and greater intermolecular sliding (i.e., plastic deformation) within the collagen network. The temperature sensitivity confirms that testing at body temperature, rather than ambient temperature, is necessary to assess the in vivo behavior of bone and teeth. The characteristic pattern of HAP strain evolution with time differs quantitatively between bone and dentin, and may reflect their different structural organization.