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At least 307 records · Page 17

An improved three-point bending test method for the investigation of nanosecond laser dicing of ultrathin Si dies with Cu stabilization layer

Highlights: • A selective chemical etching method has been developed for removal of metallization layers on ultrathin Si dies for three-point bending test. • The complex elastoplastic stress distribution in the die is simplified to an elastic stress distribution. • The die sidewall fracture strength can be determined using the standard three-point bending tensile stress equation. • The characteristic fracture strengths of ultrathin Si dies were correlated to the laser-induced microstructures of the die sidewall. - Abstract: The sidewall fracture strength of ultrathin Si dies with frontside and backside metallization layers cannot be determined directly from three-point bending (3PB) test. The complex 3PB elastoplastic stress distribution makes it difficult to determine the die sidewall fracture strength by analytical method or finite element analysis due to various theoretical and practical constraints. In this work, a selective chemical etching method has been developed for complete removal of the frontside and backside metallization layers on the ultrathin die without affecting the critical microstructure and strength of the die sidewall induced by laser dicing. By removing all the metallization layers on the die, the complex 3PB elastoplastic stress distribution is simplified to an elastic stress distribution. This enables a straightforward calculation of the die sidewall fracture strength using the standard 3PB tensile stress equation for a homogeneous linear elastic material with a rectangular cross section. Two chemical etchants were evaluated and found to be suitable but FeCl{sub 3} is preferred because of the much faster etching time. With this improved 3PB test method, the effect of nanosecond laser dicing on ultrathin Si dies with backside Cu layer was investigated. The die frontside and backside characteristic fracture strengths of ultrathin Si dies with varying backside Cu thickness were determined and correlated to TEM analyses of the compositions and microstructures at the fracture origins.

36 MATERIALS SCIENCE↗

Strengthening mechanisms for microstructures containing unimodal and bimodal γ' precipitates in ATI 718Plus

Here, the influence of γ' precipitate size distribution on the deformation mechanisms under tensile loading in ATI 718Plus was studied. A set of aging treatments within the temperature range of 720 °C–900 °C was performed on solution-treated samples to obtain various γ' precipitate size distributions. Unimodal and bimodal γ' precipitate size distributions were achieved through single-step and two-step aging sequences, respectively, and such microstructures were tensile tested to failure to assess their yield strength, ultimate tensile strength, and elongation-to-failure. Some of the tensile samples were interrupted after achieving 3–4 % plastic strain, and the deformed microstructures were examined using transmission electron microscopy to investigate the γ' precipitate-dislocation interactions. For the unimodal γ' precipitate size distribution samples with the smaller γ' precipitates (radius ~ 7 nm), dislocations sheared through the precipitates. Both dislocation loops and paired dislocations were observed for the microstructures containing larger γ' precipitates (radius ~ 24 nm). The microstructure containing a bimodal γ' precipitate size distribution, which included average γ' precipitate radii of ~6 nm and ~28 nm, exhibited shearing as the dominant deformation mechanism, and this microstructure exhibited the highest strength values. The experimental observations were rationalized based on the theoretically-calculated critical resolved shear stress values for shearing and looping and a modified model for predicting the yield strength for bimodal microstructures was introduced.

36 MATERIALS SCIENCE↗

Millimeter-Scale Exfoliation of hBN with Tunable Flake Thickness for Scalable Encapsulation

As a two-dimensional (2D) dielectric material, hexagonal boron nitride (hBN) is in high demand for applications in photonics, nonlinear optics, and nanoelectronics. Unfortunately, the high-throughput preparation of macroscopic-scale, high-quality hBN flakes with controlled thickness is an ongoing challenge, limiting device fabrication and technological integration. In this report we present a metal thin-film exfoliation method to prepare hBN flakes with millimeter-scale dimension, near-unity yields, and tunable flake thickness distribution from 1-7 layers, a substantial improvement over scotch tape exfoliation. The single crystallinity and high quality of the exfoliated hBN are demonstrated with optical microscopy, atomic force microscopy, Raman spectroscopy, and second harmonic generation. We further explore a possible mechanism for the effectiveness and selectivity based on thin-film residual stress measurements, density functional theory calculations, and transmission electron microscopy imaging of the deposited metal films. We find that the magnitude of the residual tensile stress induced by thin film deposition plays a key role in determining exfoliated flake thickness in a manner which closely resembles 3D semiconductor spalling. Lastly, we demonstrate that our exfoliated, large-area hBN flakes can be readily incorporated as encapsulating layers for other 2D monolayers. Altogether, this method brings us one step closer to the high throughput, mass production of hBN-based 2D photonic, optoelectronic, and quantum devices.

2D materials↗

3D Experimental Measurement of Lattice Strain and Fracture Behavior of Sand Particles Using Synchrotron X-Ray Diffraction and Tomography

3D synchrotron X-ray diffraction (3DXRD) and synchrotron micro-computed tomography (SMT) techniques were used to measure and monitor the lattice strain evolution and fracture behavior of natural Ottawa sand particles subjected to 1D compression loading. The particle-averaged lattice strain within sand particles was measured using 3DXRD and then was used to calculate the corresponding lattice stress tensor. In addition, the evolution and mode of fracture of sand particles was investigated using high-resolution 3D SMT images. The results of diffraction data analyses revealed that the major principal component of the lattice strain or stress tensor increased in most of the particles as the global applied compressive load increased until the onset of fracture. Particle fracture and subsequent rearrangements caused significant variation and fluctuations in measured lattice strain/stress values from one particle to another and from one load step to the next one. SMT image analysis at the particle-scale showed that cracks in fractured sand particles generally initiate and propagate along the plane that connects the two contact points. Fractured particles initially split into two or three major fragments followed by disintegration into multiple smaller fragments in some cases. In conclusion, microscale analysis of fractured particles showed that particle position, morphology, the number and location of contact points play a major role in the occurrence of particle fracture in confined comminution of the sand assembly.

47 OTHER INSTRUMENTATION↗

Initiation time of near-infrared laser-induced slip on the surface of silicon wafers

We have determined the initiation time of laser-induced slip on a silicon wafer surface subjected to a near-infrared continuous-wave laser by numerical simulations and experiments. First, numerical analysis was performed based on the heat transfer and thermoelasticity model to calculate the resolved shear stress and the temperature-dependent yield stress. Slip initiation time was predicted by finding the time at which the resolved shear stress reached the yield stress. Experimentally, the slip initiation time was measured by using a laser scattering technique that collects scattered light from the silicon wafer surface and detects strong scattering when the surface slip is initiated. The surface morphology of the silicon wafer surface after laser irradiation was also observed using an optical microscope to confirm the occurrence of slip. The measured slip initiation times agreed well with the numerical predictions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Grain orientation effects on dynamic strength of FCC multicrystals at low shock pressures: a hydrodynamic instability study

Variability in local dynamic plasticity due to material anisotropy in polycrystalline metals is likely to be important on damage nucleation and growth at low pressures. Hydrodynamic instabilities could be used to study these plasticity effects by correlating measured changes in perturbation amplitudes at free surfaces to local plastic behaviour and grain orientation, but amplitude changes are typically too small to be measured reliably at low pressures using conventional diagnostics. Correlations between strength at low shock pressures and grain orientation were studied in copper (grain size ≈ 800 μm) using the Richtmyer–Meshkov instability with a square-wave surface perturbation (wavelength = 150 μm, amplitude = 5 μm), shocked at 2.7 GPa using symmetric plate impacts. A Plexiglas window was pressed against the peaks of the perturbation, keeping valleys as free surfaces. This produced perturbation amplitude changes much larger than those predicted without the window. Amplitude reductions from 64 to 88% were measured in recovered samples and grains oriented close to $\langle$0 0 1$\rangle$ parallel to the shock had the largest final amplitude, whereas grains with shocks directions close to $\langle$1 0 1$\rangle$ had the lowest. Finite element simulations were performed with elastic-perfectly plastic models to estimate yield strengths leading lead to those final amplitudes. Anisotropic elasticity and these yield strengths were used to calculate the resolved shear stresses at yielding for the two orientations. In conclusion, results are compared with reports on orientation dependence of dynamic yielding in Cu single crystals and the higher values obtained suggest that strength estimations via hydrodynamic instabilities are sensitive to strain hardening and strain rate effects.

36 MATERIALS SCIENCE↗

Verification of experimental dynamic strength methods with atomistic ramp-release simulations

Material strength and moduli can be determined from dynamic high-pressure ramp-release experiments using an indirect method of Lagrangian wave profile analysis of surface velocities. This method, termed self-consistent Lagrangian analysis (SCLA), has been difficult to calibrate and corroborate with other experimental methods. Using nonequilibrium molecular dynamics, we validate the SCLA technique by demonstrating that it accurately predicts the same bulk modulus, shear modulus, and strength as those calculated from the full stress tensor data, especially where strain rate induced relaxation effects and wave attenuation are small. We show here that introducing a hold in the loading profile at peak pressure gives improved accuracy in the shear moduli and relaxation-adjusted strength by reducing the effect of wave attenuation. When rate-dependent effects coupled with wave attenuation are large, we find that Lagrangian analysis overpredicts the maximum unload wavespeed, leading to increased error in the measured dynamic shear modulus. Furthermore, these simulations provide insight into the definition of dynamic strength, as well as a plausible explanation for experimental disagreement in reported dynamic strength values.

36 MATERIALS SCIENCE↗

A Strength Model and Service Envelope for PBX 9501

An analytical method is proposed for making an assessment of the severity of the response of PBX 9501 in structural response simulations. The approach is based on the coherent use of a strength model and a failure criterion. The strength model is based on a creep rupture function and an associated cumulative damage model. The material's residual strength at any time during a simulation of structural response is determined by taking into account both the actual stress history up to that time, and a hypothetical continuation of the applied stresses that are assumed to grow until material failure results. The residual strength is used by the failure criterion to define the region of safe (non-failed) material response. The Mohr-Coulomb failure criterion is chosen for its general applicability to materials with both cohesive and frictional strength. The combined use of the residual strength model and the failure criterion provides a quantitative method of assessing the severity of the response of PBX 9501 material in structural simulations: the proximity of any evolving, general state of stress to the failure surface (which shrinks due to the cumulative damage caused by the past stress history) can be calculated and used as a measure of margin to failure. The strength model has been calibrated to a broad range of uniaxial tension and compression tests, and a small set of creep tests, and is applicable to a broad range of loading conditions.

42 ENGINEERING↗

An Investigation of the Applicability and Limitations of the ORNL Expanded Plug Test

The expanded plug test technique for measuring the circumferential tensile properties of irradiated nuclear fuel cladding was developed at Oak Ridge National Laboratory (ORNL) and has been used successfully in several applications. The primary advantage of this technique over other procedures is its simplicity for application in the complex hot cell environment. During the development stage, efforts were made to both qualify the technique as much as possible regarding its experimental application and to develop and validate the data reduction procedures. However, since this is a new technique, the technical community is cautious in adopting a procedure that has not been fully vetted. The purpose of this effort was to address several baseline issues regarding the applicability of the technique and the precision of the use of experimental expanded ring load-deformation data to calculate material circumferential stress-strain properties. The tests performed, in conjunction with the developed data reduction procedures, demonstrate good reliability in the prediction of ring material stress-strain behavior for several materials of widely different strengths.

tensile, nuclear fuel cladding↗

Report on the Integration of Experimental and Modeling Data for Initial Equivalence Study of Mechanical Performance in Irradiated LPBF 316 Stainless Steel

To ensure the rapid development, deployment, and use of advanced nuclear technologies, faster qualification approaches are needed. Typically, the primary pathway uses traditional data packages consistent with the American Society of Mechanical Engineers Boiler and Pressure Vessel Code, which does not consider the environmental effects the material will experience such as corrosion and radiation damage. Examining radiation effects requires a significant amount of space in US facilities at the Advanced Test Reactor and the High Flux Isotope Reactor (HFIR) and suffers from natural gradients in temperature and neutron flux profiles. Ion irradiation may enable rapid assessment of radiation-induced damage to a material and is proposed as part of an accelerated materials qualification framework through the Advanced Materials and Manufacturing Technologies program. To enhance the utility of ion irradiation as an examination tool, this report provides the initial assessment of engineering-relevant properties of microstructures produced from ion irradiation in the near-surface volume. Nanoindentation, Vickers hardness, and known tensile properties were brought together with simple mathematical models and experimental data for an initial equivalence study of the mechanical performance of irradiated laser powder bed fusion (LPBF) 316 stainless steels across length scales. Direct observation of the calculated ion irradiation yield stress and measured neutron irradiation yield stress at 2 dpa showed that both datasets exhibit the same trend with irradiation temperature and overlap within an acceptable band of stress values. Ion irradiations at 10 dpa serve as a prediction of properties to compare to postirradiation examination of HFIR-irradiated LPBF 316H further in the program. This work is a significant demonstration of the Licensing Approach with Ions and Neutrons, which uses ion irradiations to generate mechanical property information more rapidly than through neutron irradiations.

36 MATERIALS SCIENCE↗

Change in Limiting Channel Dimensions during Pneumatic Shaping of Multilayer Structures

A mathematical model is developed for determining the inert-gas pressure within rectangular channels in multilayer structures. The model permits calculation of the pressure, stress, and damage in the shaping of materials with different properties. The influence of the relative channel height on the relative limiting rounding radius of a corner element and the membrane thickness and also on the failure time for titanium (VT6S) and aluminum (AMg6) alloys is investigated. The deformation processes are described by the energetic and kinetic theories of creep and damage for viscous flow.

42 ENGINEERING↗

Determination of the mechanical properties of blisters by nanoindentation

In light-water reactors, a zirconium oxide layer will be formed at the outer surface of the fuel cladding as a consequence of the chemical reaction which takes place between zirconium and the cooling water. This zirconium oxide layer is a good thermal insulator, but at some point, it may spall-out. As a consequence, a cold spot will be formed at the outer surface of the cladding. In this situation, the hydrogen will quickly migrate to this spot to form a highly-enriched hydride zone, known as blister. In this work, an experimental procedure has been devised to produce blisters with a similar shape to the ones reported in the literature for irradiated cladding with severe hydriding. Nano-indentation tests were performed on blisters prepared in laboratory. A numerical simulation by the finite element method was developed to fit the load versus penetration depth data from the aforementioned nano-indentation tests. By means of an inverse process which combines experimental data and numerical simulations, the constitutive equation of the blister was determined. The process has been used to calculate the plastic stress-strain curve of the blister under study at room temperature. The results show an almost perfect numerical fitting of the experimental data.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Adhesion Capabilities of Permanent Foaming Fixatives

DOE-EM have identified an operational requirement for a fixative that can immobilize and/or encapsulate residual contamination in 3D void volumes (pipes, gloveboxes, waste containers, etc.) during D and D activities. Failure to safely and effectively immobilize residual contamination can: Put workers at risk; Contaminate the public and environment; Drive up costs. Commercial-off-the-shelf (COTS) polyurethane (PU) foams is one possible solution and is currently being investigated by Savannah River National Lab (SRNL). Adhesion testing will dictate how well PU foams will adhere and immobilize residual contamination onto a substrate. Results can provide a performance criteria for Section 5 of ASTM E3191: Standard Specification for Permanent Foaming Fixatives Used to Mitigate Spread of Radioactive Contamination. Initial mechanical testing showed intumescent rigid PU foams were best in class (tensile, compression, TGA/DSC) Application of intumescent rigid PU foam in pipe scenario with 'contamination' showed excellent adhesion capabilities as long as foam had contact with pipe. The foam, however, was not able to penetrate 'contamination' but created pockets where the contamination interacted with the substrate. Pretreatment options of pipe were considered to produce better immobilization capabilities. Pretreatment options included COTS products like baking spray, rubber cement, and soap. Foam was still able to immobilize on a global sense, but not a local sense. Essentially acted as a mechanical plug. A tensile tester (MTS Criterion Series 43) was utilized to evaluate the tensile adhesion strength of 6 COTS PU foams. ASTM D1623: Tensile and Tensile Adhesion Properties of Rigid Cellular Plastics. Procedures: PU foams were cured between two smooth 2'' x 2'' 304 stainless steel coupons with hinges glued on plates for gripping support. Parameters Used: Pull rate of 0.1 in/min. Calculations: Tensile adhesion strength, elongation, and ImageJ analysis of how PU foam is left on substrate. Outcome: The PU foam with the best adhesion capabilities would be downselected for further evaluation to be used as a permanent foaming fixative. The rigid PU foams had the best adhesion capabilities with the R1 foam having a max load of 236 N. One of the I-R2 samples reached almost 450 N and another sample reached 2500 N before slipping. The other intumescent foam, I-F4, had the most coverage on the stainless steel coupon's surface from the ImageJ results (61.43% surface coverage). The intumescent foam, I-R2, will be the foam of choice for future testing due its fire retardant and adhesion capabilities. Future directions: Conduct the following experiment in a pipe scenario with the down-selected PU foam. Procedures: PU foam will be cured between in a 304 stainless steel pipe (ID: 4'', OD: 4.5'', Height: 4''). Parameters Used: Compression testing results will be referenced to determine if foam's adhesion strength would be greater its compression strength as its being compressed. Calculations: Compression strength, shear stress, total time elapsed. Conduct further adhesion testing with the down-selected PU foam (I-R2) to be treated as a permanent foaming fixative (PFF). Determine the minimum contact the PFF should have with the substrate for adequate results. Evaluate if PFF's adhesion capabilities is time dependent (3.1.5 of ASTM E3911). Subject PFF to seismic stressors addressed in Safety Basis of Interim Operation documents (SBIO) to further evaluate adhesion capabilities.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Influence of Welding Strength Matching Coefficient and Cold Stretching on Welding Residual Stress in Austenitic Stainless Steel

Austenitic stainless steel is widely used in pressure vessels for the storage and transportation of liquid gases such as liquid nitrogen, liquid oxygen, and liquid hydrogen. Cryogenic pressure vessel manufacturing uses cold stretching technology, which relies heavily on welding joint performance, to construct lightweight and thin-walled vessels. Residual stress from welding is a primary factor in cases of austenitic stainless steel pressure vessel failure. In this paper, on the basis of Visual Environment 10.0 finite element simulation technology, the residual stress resulting from different welding strength matching coefficients (0.8, 1, 1.2, 1.4) for two S30408 plates welded with three-pass butt welds is calculated according to thermal elastoplastic theory. In addition, the stress field was calculated under a loading as high as 410 MPa and after the load was released. Path 1 was set to analyze stress along the welding line, and path 2 was set to analyze stress normal to the welding line. The welding strength matching coefficient strongly affected both the longitudinal residual stress (center of path 1) and the transverse residual stress (both ends of path 1) after the welding was completed. However, the coefficient had little effect on the longitudinal and transverse residual stress of path 2. Under the loading of 410 MPa, the longitudinal and transverse stress decreased and the stress distribution, with different welding strength matching coefficients, was less diverse. After the load was released, longitudinal and transverse stress distribution for both path 1 and path 2 decreased to a low level. Cold stretching could reduce the effect of residual stress to various degrees. Transverse strain along the stretching direction was also taken into consideration. The experimental results validated the reliability of the partial simulation.

36 MATERIALS SCIENCE↗

Phase field modeling of dislocations and obstacles in InSb

We present a phase-field dislocation dynamics (PFDD) model informed by first-principle calculations to elucidate the competitive dislocation nucleation and propagation between the glide and shuffle sets in InSb diamond cubic crystal. The calculations are directly informed with generalized stacking fault energy curves on the (111) slip plane for both the “glide set,” with the smaller interplanar spacing, and the “shuffle set,” with the larger interplanar spacing. The formulation also includes elastic anisotropy and the gradient term associated with the dislocation core. The PFDD calculations show that under no stress the equilibrium structure of screw glide set dislocations dissociates into Shockley partials, while those of the shuffle set dislocations do not dissociate, remaining compact. The calculated dislocation core widths of these InSb dislocations agree well with the measured values for other semiconductor materials, such as Si and GaN. We find that a shuffle set dislocation emits from a dislocation source at an applied stress about three times smaller than that needed to emit leading and trailing partials successively on the glide set plane. Once the partial dislocations in the glide set are emitted, they propagate faster than the shuffle set perfect dislocation at the same stress level.

36 MATERIALS SCIENCE↗

A kinetic model for stress generation in thin films grown from energetic vapor fluxes

We have developed a kinetic model for residual stress generation in thin films grown from energetic vapor fluxes, encountered, e.g., during sputter deposition. The new analytical model considers sub-surface point defects created by atomic peening, along with processes treated in already existing stress models for non-energetic deposition, i.e., thermally activated diffusion processes at the surface and the grain boundary. According to the new model, ballistically induced sub-surface defects can get incorporated as excess atoms at the grain boundary, remain trapped in the bulk, or annihilate at the free surface, resulting in a complex dependence of the steady-state stress on the grain size, the growth rate, as well as the energetics of the incoming particle flux. We compare calculations from the model with in situ stress measurements performed on a series of Mo films sputter-deposited at different conditions and having different grain sizes. The model is able to reproduce the observed increase of compressive stress with increasing growth rate, behavior that is the opposite of what is typically seen under non-energetic growth conditions. On a grander scale, this study is a step towards obtaining a comprehensive understanding of stress generation and evolution in vapor deposited polycrystalline thin films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Nudged Elastic Band Simulations of Kink Pairs in Tungsten

Atomistic techniques have been used to calculate energy barriers for dislocation motion that control the strength (yield stress and flow stress) of the material. In particular, the calculations focus on the change in enthalpy as a straight dislocation moves through the crystal lattice (the Peierls barrier) and kink pair formation enthalpy that controls the thermally activated double-kink mechanism important at low to moderate stresses. A novel means of assessing kink widths within atomistic simulations is introduced.

36 MATERIALS SCIENCE↗

ZPPR FUEL ELEMENT THERMAL STRESS-STRAIN ANALYSIS

The design temperature of high plutonium concentration ZPPR fuel assemblies is 600 degrees C. Cladding integrity of the 304L stainless steel cladding is a significant concern with this fuel since even small holes can lead to substantial fuel degradation. Since the fuel has a higher coefficient of thermal expansion than the cladding, an investigation of the stress induced in the cladding due to the differential thermal expansion of fuel and cladding up to the design temperature was conducted. Small holes in the cladding envelope would be expected to lead to the fuel hydriding and oxidizing into a powder over a long period of time. This is the same type of chemical reaction chain that exists in the degradion of the high uranium concentration ZPPR fuel. Unfortunately, the uranium fuel was designed with vents which allowed this degradation to occur. The Pu cladding is sealed so only fuel with damaged cladding would be subject to this damage. The thermal stresses that can be developed in the fuel cladding have been calculated in in this paper and compared to the ultimate tensile stress of the cladding. The conclusion is drawn that thermal stresses cannot induce holes in the cladding even for the highest storage temperatures predicted in calculations (292°C). In fact, thermal stress can not cause cladding failure as long as the fuel temperatures are below the design limit of 600 degrees C (1,112 degrees F).

99 GENERAL AND MISCELLANEOUS↗