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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Indentation size effect in tungsten: Quantification of geometrically necessary dislocations underneath the indentations using HR-EBSD

Highlights: • Revealed the dislocation structure below nanoindentations via ECCI and HR-EBSD. • Experimentally quantification of GND densities, with higher GND densities at lower depths. • Qualitative validation of the Nix-Gao model on the indentation size effect. - Abstract: During indentation testing of the low defect density crystalline materials, higher hardness values are found at lower indentation depths, which is referred to as an indentation size effect. The depth-dependence of hardness can be described by the Nix-Gao model, which is based on the concept of Geometrically Necessary Dislocations (GNDs). The underlying dislocation mechanism remains, however, unclear and requires independent measurement of GND density below the indentation. In the present work, the depth-dependency of the GND density is quantified underneath the Berkovich indentations in tungsten via high-resolution electron backscatter diffraction. There a higher GND density is found for lower indentation depths, resulting in a higher Taylor hardness for measured GND density.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In situ indentation and high cycle tapping deformation responses in a nanolaminate crystalline/amorphous metal composite

The incorporation of nanostructured and amorphous metals into modern applications is reliant on the understanding of deformation and failure modes in constrained conditions. To study this, a 105 nm crystalline Cu/160 nm amorphous Cu 45 Zr 55 (at.%) multilayer structure was fabricated with the two crystalline layers sputter deposited between the top-middle-bottom amorphous layers and prepared to electron transparency. The multilayer was then in situ indented either under a single load to a depth of ~ 100 nm (max load of ~ 100 μN) or held at 20 μN and then repeatedly indented with an additional 5 μN up to 20,000 cycles in a transmission electron microscope to compare the deformation responses in the nanolaminate. For the single indentation test, the multilayer showed serrated load-displacement behavior upon initial indentation inductive of shear banding. Additionally, at an indentation depth of ~ 32 nm, the multilayer exhibited perfect plastic behavior and no strain hardening. Both indented and fatigue-indented films revealed diffraction contrast changes with deformation. Subsequent Automated Crystal Orientation Mapping (ACOM) measurements confirmed and quantified global texture changes in the crystalline layers with specifically identified grains revealing rotation. Using a finite element model, the in-plane displacement vectors under the indent mapped conditions where ACOM determined grain rotation was observed, indicating the stress flow induced grain rotation. Furthermore, the single indented Cu layers also exhibited evidence of deformation induced grain growth, which was not evident in the fatigue-indented Cu based multilayer. Finally, the single indented multilayer retained a significant plastic crater in the upper most amorphous layer that directly contacted the indenter; a negligible crater impression in the same region was observed in the fatigued tested multilayer. These differences are explained by the different loading methods, applied load, and deformation mechanisms experienced in the multilayers.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Lateral cracks during sliding indentation on various optical materials

A series of static and sliding indentation (ie, scratching) was performed and characterized on a wide range of optical workpiece materials [single crystals of Al 2 O 3 (sapphire), SiC, Y 3 Al 5 O 12 (YAG), CaF 2 , and LiB 3 O 5 (LBO); a SiO 2 –Al 2 O 3 –P 2 O 5 –Li 2 O glass ceramic (Zerodur); and glasses of SiO 2 :TiO 2 (ULE), SiO 2 (fused silica), and P 2 O 5 –Al 2 O 3 –K 2 O–BaO (Phosphate)] at various applied loads using various indenters (Vickers, 10 µm conical, and 200 µm conical). Despite having different load dependencies, the lateral crack depth formed during sliding indentation quantitatively scales with that formed during static indentation, explaining why static indentation has been historically effective in describing various grinding parameters. Depending on the indenter geometry, the amount of residual trench damage (plastic deformation and local fracturing) during sliding indentation was often enhanced by more than an order of magnitude compared with static indentation. A simple ploughing scratch model, which considers both tangential and normal stresses (where the tangential stress is amplified by relatively small tangential contact area), explains this enhancement and other observed trends. Accounting for the high correlation between residual trench depth and volumetric fracturing, the model is extended to estimate the amount of fracture damage as a function of the material properties of the workpiece, indenter geometry, and applied load. Such a model has utility in the design of optimized grinding processes, particularly the abrasive geometry. Finally, at higher loads (>1 N), lateral cracks were often observed to preferentially propagate in the forward scratching direction, as opposed to perpendicular to the scratch as typically observed. High-speed imaging of the scratch process confirms that these cracks propagate ahead of the sliding indenter during the scratching event. Finite element stress analysis suggests the ploughing frictional forces increase the mode I tensile stresses at the leading edge of the sliding indenter explaining the direction of crack propagation of such cracks.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Decoupling indentation size and strain rate effects during nanoindentation: A case study in tungsten

Materials indented at small scales may simultaneously exhibit indentation size and strain rate effects which complicate the identification of the mechanisms that control deformation and strength. Here, in this work, we explore the possibility that indentation size and rate effects in some materials can be decoupled in a simple way. Nanoindentation tests with various load-time histories were carried out to measure the hardness of a tungsten single crystal over a wide range of indentation depths (~500–3600 nm) and indentation strain rates (~5 ×10 –5 –2 ×10 –1 s –1 ). Under these conditions, this material exhibits significant indentation size and rate effects, but the size effect is, to a good approximation, independent of strain rate. It is shown that this behavior can be understood by the Nix-Gao model for the indentation size effect modified to include the effects of a strain rate dependent friction stress. As a consequence, the size and rate dependencies of the hardness can be expressed as the sum of two independent terms: H($\dot{ε}$ i , h c )=H f ($\dot{ε}$ i ) + (H 0 – H f ) $\sqrt{1+ \frac{h^*}{h_c}}$, where H($\dot{ε}$ i , h c ) is the hardness at given indentation strain rate ($\dot{ε}$ i ) and contact depth (h c ), H f ($\dot{ε}$ i ) is the hardness contributed by the rate dependent friction stress, and (H 0 – H f ) and h* are size and rate independent constants that follow from the Nix-Gao analysis. This formula, together with an expression for the rate dependence of H f , was successfully applied to decouple the indentation size and rate effects observed in tungsten. In addition, the physics underlying the rate independence of indentation size effect is discussed, which provides guidance for application of the proposed approach to other materials.

42 ENGINEERING↗
DOE OSTI2019

Å-Indentation for non-destructive elastic moduli measurements of supported ultra-hard ultra-thin films and nanostructures

During conventional nanoindentation measurements, the indentation depths are usually larger than 1–10 nm, which hinders the ability to study ultra-thin films (<10 nm) and supported atomically thin two-dimensional (2D) materials. Here, we discuss the development of modulated Å-indentation to achieve sub-Å indentations depths during force-indentation measurements while also imaging materials with nanoscale resolution. Modulated nanoindentation (MoNI) was originally invented to measure the radial elasticity of multi-walled nanotubes. Now, by using extremely small amplitude oscillations (<<1 Å) at high frequency, and stiff cantilevers, we show how modulated nano/Å-indentation (MoNI/ÅI) enables non-destructive measurements of the contact stiffness and indentation modulus of ultra-thin ultra-stiff films, including CVD diamond films (~1000 GPa stiffness), as well as the transverse modulus of 2D materials. Our analysis demonstrates that in presence of a standard laboratory noise floor, the signal to noise ratio of MoNI/ÅI implemented with a commercial atomic force microscope (AFM) is such that a dynamic range of 80 dB –– achievable with commercial Lock-in amplifiers –– is sufficient to observe superior indentation curves, having indentation depths as small as 0.3 Å, resolution in indentation <0.05 Å, and in normal load <0.5 nN. Being implemented on a standard AFM, this method has the potential for a broad applicability.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Crack nucleation and growth during dynamic indentation of chemically-strengthened glass

Dynamic point impact loading is a primary cause of fracture of glass screens on mobile devices. An improved understanding of crack initiation and evolution under high-speed indentation could contribute to the development of materials with better performance, but experimental observations are challenging due to the short timescales and limited depth-of-field of optical microscopy. To address this need, we have observed fracture of a chemically-strengthened glass during dynamic indentation using in situ x-ray phase-contrast imaging (XPCI). Median cracks initiate below the surface of the glass, at a depth approximately corresponding to the depth at which the surface residual compressive stress diminishes to zero. These cracks initially propagate at ~10ms –1 , rapidly accelerating to > 100ms –1 . We also observe some evidence for rate-dependent behavior, in that indentation at the lowest rates studied here (below about ~0.15ms –1 ) fails to initiate cracks regardless of the depth of the indentation (up to 18μm), while indentation at higher rates produces median cracks that either arrest or cause complete fracture, depending on the depth of indentation.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Use of indentation to study the degradation of photovoltaic backsheets

The ability of electrical insulating materials within a module to act as insulators is a key safety requirement for photovoltaic (PV) technology. Presently, however, the durability of backsheets may not be readily assessed. For example, the mechanical tensile test continues to be developed, and its use has not been validated such that a technically based pass/fail criteria may be established. This study examines the use of simple indentation methods, including durometer hardness and instrumented indentation, as a means to quantitively assess the degradation of PV backsheets. Characteristics including: hardness, modulus, load/displacement profile, creep hold response, and residual impression are explored in an empirical study. Glass/encapsulant/backsheet mini-modules constructed using backsheets including: polyamide (PA), poly(ethylene terephthalate) (PET), polyvinyl fluoride (PVF) laminate ('TPE'), and polyvinylidene fluoride (PVDF) were examined. An M-type durometer as well as Berkovich and cube-corner tips were used in the indentation experiments. Additional characterizations were performed to interpret the indentation measurements including: surface roughness measurements using atomic force microscopy (AFM), a chemical integrity study using Fourier-transform infrared spectroscopy (FTIR), and phase-transition measurements using differential scanning calorimetry (DSC). The results are analyzed in the context of the combined accelerated stress test (C-AST) also explored in this study. Instrumented indentation (i.e., using a Berkovich tip) was able to distinguish between backsheets and quantify the effects of accelerated testing (including up to 60%, 25%, and 20% change in hardness, modulus, and creep displacement, respectively). The embrittlement of the backsheets was not readily assessable using cube-corner indentation. Cracking of the known-bad polyamide backsheet was observed from the C-AST, which was not observed to result from steady state UV weathering.

14 SOLAR ENERGY↗
DOE OSTI2024

Spherical Indentation and Implementation of S 3 /P for yield stress determination of brittle materials

Here, a mathematically transparent and robust experimental method has been developed to estimate the yield stress of brittle materials through the analysis of depth-sensing spherical indentation. Employing Hertzian contact mechanics, an elastically invariant ratio based on the simple equation S 3 / P = 6RE r 2 , (where S and P are contact stiffness and indentation load, respectively) has been derived that enables more accurate and confident determination of the transition from elastic to inelastic deformation; a transition that the yield stress dictates and represents. Using two diamond spheres with radii of 3.2 and 8.6 μm, the indentation test method and analyses are applied to two vitreous silicates: Corning's HPFS 7980® fused silica and Vitro's Starphire® soda lime silicate. The estimated yield strengths are 8.15 GPa ± 2.5% for the fused silica and 6.1 GPa ± 3.3% for the soda-lime silicate, and both were independent of indenter radius. Verification of this new experimental method is demonstrated with an as-drawn titanium by showing equivalence of measured yield stress by its spherical indentation and that from uniaxial compression testing. This method will enable easier and more confident estimation of yield stress in brittle materials - a property that historically has been elusive to measure for these materials using common laboratory mechanical test methods.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Extraction of mechanical properties of materials through deep learning from instrumented indentation

Instrumented indentation has been developed and widely utilized as one of the most versatile and practical means of extracting mechanical properties of materials. This method is particularly desirable for those applications where it is difficult to experimentally determine the mechanical properties using stress–strain data obtained from coupon specimens. Such applications include material processing and manufacturing of small and large engineering components and structures involving the following: three-dimensional (3D) printing, thin-film and multilayered structures, and integrated manufacturing of materials for coupled mechanical and functional properties. Here, we utilize the latest developments in neural networks, including a multifidelity approach whereby deep-learning algorithms are trained to extract elastoplastic properties of metals and alloys from instrumented indentation results using multiple datasets for desired levels of improved accuracy. We have established algorithms for solving inverse problems by recourse to single, dual, and multiple indentation and demonstrate that these algorithms significantly outperform traditional brute force computations and function-fitting methods. Moreover, we present several multifidelity approaches specifically for solving the inverse indentation problem which 1) significantly reduce the number of high-fidelity datasets required to achieve a given level of accuracy, 2) utilize known physical and scaling laws to improve training efficiency and accuracy, and 3) integrate simulation and experimental data for training disparate datasets to learn and minimize systematic errors. The predictive capabilities and advantages of these multifidelity methods have been assessed by direct comparisons with experimental results for indentation for different commercial alloys, including two wrought aluminum alloys and several 3D printed titanium alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Extraction of mechanical properties of materials through deep learning from instrumented indentation

Instrumented indentation has been developed and widely utilized as one of the most versatile and practical means of extracting mechanical properties of materials. This method is particularly desirable for those applications where it is difficult to experimentally determine the mechanical properties using stress–strain data obtained from coupon specimens. Such applications include material processing and manufacturing of small and large engineering components and structures involving the following: three dimensional (3D) printing, thin-film and multilayered structures, and integrated manufacturing of materials for coupled mechanical and functional properties. Here, we utilize the latest developments in neural networks, including a multifidelity approach whereby deep-learning algorithms are trained to extract elastoplastic properties of metals an d alloys from instrumented indentation results using multiple datasets for desired levels of improved accuracy. We have established algorithms for solving inverse problems by recourse to single, dual, and multiple indentation and demonstrate that these algorithms significantly outperform traditional brute force computations and function-fitting methods. Moreover, we present several multifidelity approaches specifically for solving the inverse indentation problem which 1) significantly reduce the number of high-fidelity datasets required to achieve a given level of accuracy, 2) utilize known physical and scaling laws to improve training efficiency and accuracy, and 3) integrate simulation and experimental data for training disparate datasets to learn and minimize systematic errors. The predictive capabilities and advantages of these multifidelity methods have been assessed by direct comparisons with experimental results for indentation for different commercial alloys, including two wrought aluminum alloys and several 3D printed titanium alloys.

3D printed materials, stress-strain behavior, mult↗
DOE OSTI2020

Investigation on capacity loss mechanisms of lithium-ion pouch cells under mechanical indentation conditions

Capacity loss was observed in Li-ion cells after mechanical deformation approaching the onset of internal short circuit (ISCr). In this paper, a series of indentation tests were carried out on commercial Li-ion cells of three capacities (500, 1500 and 2000 mAh). Both in-situ and ex-situ methods were used to investigate the mechanisms of indentation-induced capacity loss. We note after indentation test, the cell capacity reduced by 0.5%–6% of its original value. The incremental capacity (IC) analysis results showed that IC curves generally shifted to lower voltage region, indicating the increase in cell internal resistance. In addition, the fitting results of electrochemical impedance spectroscopy (EIS) indicated that mechanical indentation can result in a reduction in ohmic resistance and the increase in polarization resistance. Scanning electron microscopy (SEM) and X-ray computed tomography (XCT) results showed crushing of graphite, mud cracking of copper current collectors and enlarged pores in separator, which is proposed to be the main reasons for the increase in polarization resistance and permanent capacity loss. The rapid capacity loss due to mechanical abuse was compared with the long-term capacity fading.

25 ENERGY STORAGE↗
DOE OSTI2018

Microstructural Characterization and High Strain Rate Plastic Flow Behavior of SMAW Armox500T Steel Joints from Spherical Indentation Experiments

Static indentation and uniaxial compression tests have been conducted on Armox500T steel and its weldments to predict the constraint factor (CF), i.e., ratio of Meyer’s hardness to uniaxial flow stress. Series of dynamic indentation experiments were carried out at impact velocities ranging from 5 to 300 m/s to estimate dynamic hardness as a function of average strain. Subsequently, dynamic indentation (DI) test data and CF determined under static indentation conditions have been used to study the high strain rate plastic flow behavior of Armox500T weldments in comparison with the base metal. It was observed that flow stress for Armox500T and its weldments under dynamic loading conditions (10{sup 4} s{sup −1}) are significantly higher than flow stress measured under static loading conditions (10{sup −3} s{sup −1}). The plastic flow behavior computed from DI is in good agreement with the data evaluated through conventional split Hopkinson pressure bar technique. Further, the study of the microstructure of base metal and weldments by optical microscopy and SEM revealed a considerable variation in the microstructure.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Macroscale property assessment and indentation characteristics of thick section friction stir welded AA 5083

The spatial gradients in microstructure have been proven to be effective in optimizing the performance of components, and several techniques have been developed to achieve this microstructure. Nevertheless, the local microstructural modification methods inevitably result in the formation of gradient microstructure leading to a variation in the property. Herein this work systematically investigates the effect of gradient microstructure formed during thick section friction stir weld Al5083 alloy on its mechanical properties. A novel macro-indentation technique, profilometer-based indentation plastometry (PIP), is utilized to capture the variation in the mechanical properties in the feedstock (rolled plate) and weld region. The feedstock exhibited a gradient microstructure owing to different stress states during rolling. Additionally, the stirring of the tool resulted in a complex material flow pattern producing a microstructure gradient in the weld region. The aspect ratio of the grains was identified as the primary factor causing variation in indentation response in the feedstock. In contrast, variation in the grain size in the weld region resulted in property variation. Overall, the stir zone has a lower yield strength (158±4MPa) than the base material (173±3MPa). In addition, microstructure heterogeneity in the stir zone resulted in lower elongation than the base material.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Coupling dynamic in situ X-ray micro-imaging and indentation: A novel approach to evaluate micromechanics applied to oil shale

Oil and gas shales are a system where understanding the mechanical properties at the microscale is of paramount importance, e.g. to better understand the behavior of proppant-shale contacts and their role in the evolution of propped fractures in unconventional reservoirs. Here we show for the first time an experiment coupling indentation testing with in situ X-ray imaging in a Green River shale sample. A full compliance curve has been measured with the sample in water, allowing to visualize the indentation of the sample in function of axial load, in a purpose-built system for combined in situ indentation and X-ray imaging. A series of 3D datasets were used for a digital volume correlation study to obtain local strain fields. This analysis has been complemented with the analysis of cracks. Finally, geomechanical modeling has been carried out to replicate and generalize the observed behavior in the shale. This study validated this experimental approach, providing a breakthrough in understanding micro-mechanics in shales, and demonstrates how this class of experiments can be important for studies involving the prediction of the evolution of propped fractures in shale reservoirs, with possible applications in a much larger number of application fields (geothermal, materials science, etc.)

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2022

Integrated simulation, machine learning, and experimental approach to characterizing fracture instability in indentation pillar-splitting of materials

Measuring fracture toughness of materials at small scales remains challenging due to limited experimental testing configurations. A recently developed indentation pillar-splitting method has shown promise of improved flexibility in fracture toughness measurements at the microscale, partly due to the occurrence of an unusual fracture instability, i.e., a transition from stable to unstable crack propagation. In spite of growing interest in this method, the underlying mechanism of this phenomenon is yet to be elucidated. Furthermore, we provide a comprehensive description of fracture instability in indentation pillar-splitting by combining in situ experiments with high-fidelity simulations based on cohesive zone and J-integral methods. In addition, a machine-learning-based solution for predicting the critical indentation load of fracture instability is established through Gaussian processes regression for broad use of this method by the community.

36 MATERIALS SCIENCE↗