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At least 865 records · Page 48
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

In situ X-ray imaging of pore formation mechanisms and dynamics in laser powder-blown directed energy deposition additive manufacturing

Directed energy deposition (DED) additive manufacturing (AM) is receiving growing attention in many applications, such as repair, remanufacturing, and fabrication of functionally graded structures. However, the laser-matter interactions and melt pool dynamics in laser DED with powder flow are still unclear, particularly in how pores form and flow inside the melt pool during the process. Understanding the porosity formation mechanisms is critical in the qualification, certification, and overall properties of a DED AM part. Porosity is a common phenomenon and can significantly hinder the quality of DED fabricated parts, as the pores can act as sites of crack nucleation and propagation. Here in this paper, we reveal four types of pore formation mechanisms through in-situ and operando high-speed high-resolution X-ray imaging in the DED AM process. Our results confirm that porosity within the feedstock powder induces pores in the process. We also observed pore formation mechanisms unique to the laser-based, powder-blown DED process as a result of powder delivery, keyhole dynamics, melt pool dynamics, and shield gas. High-speed X-ray images provide direct evidence for pore formation mechanisms and show that the pores related to the interaction between the delivered powder and melt pool are the largest in size in laser-based powder-blown DED AM. These results will guide porosity mitigation, elimination, and control in DED AM.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Micro-cantilever beam experiments and modeling in porous polycrystalline UO 2

Understanding the impact of microstructure on the thermo-mechanical behavior of oxide nuclear fuels is vital to predicting their performance through multiscale models. Evaluating the mechanical properties at the sub-grain length scale is key to developing these multiscale models. In this work, 3D finite element (FE) models were constructed to simulate the micrometer-scale bending of micro-cantilever beams fabricated using porous polycrystalline uranium dioxide (UO 2 ) and tested at room temperature. Here, the results showed that the porosity and elastic anisotropy of individual grains can play a significant role in determining the effective mechanical properties of the material deduced from the tests. Specifically, the porosity had a non-negligible effect, given that the pore size was of the same order of magnitude as the dimensions of the micro-beams. Correlations between load-deflection data, pore location, and elastic properties (effective Young's modulus) were investigated using UO 2 micro-beam FE models, where pore clusters were included and placed at different locations along the length of the beam. Results indicated that the presence of pore clusters near the substrate, i.e., the clamp of the micro-cantilever beam, has the strongest effect on the load-deflection behavior, with the porosity leading to a reduction of stiffness that is the largest for any location of the pore clusters. Furthermore, it was also found that pore clusters located towards the middle of the span and close to the end of the beam have a comparatively small effect on the load-deflection behavior. Therefore, it is concluded that accurate estimates of Young's modulus can be obtained from micro-cantilever experiments after accounting for porosity on the one third of the beam length close to the clamp. This, in turn, provides an avenue to improve microscale experiments and their analysis in porous, anisotropic elastic materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Metal-organic frameworks for lithium ion batteries and supercapacitors

Porous materials have been widely used in batteries and supercapacitors attribute to their large internal surface area (usually 100–1000 m{sup 2} g{sup −1}) and porosity that can favor the electrochemical reaction, interfacial charge transport, and provide short diffusion paths for ions. As a new type of porous crystalline materials, metal-organic frameworks (MOFs) have received huge attention in the past decade due to their unique properties, i.e. huge surface area (up to 7000 m{sup 2} g{sup −1}), high porosity, low density, controllable structure and tunable pore size. A wide range of applications including gas separation, storage, catalysis, and drug delivery benefit from the recent fast development of MOFs. However, their potential in electrochemical energy storage has not been fully revealed. Herein, the present mini review appraises recent and significant development of MOFs and MOF-derived materials for rechargeable lithium ion batteries and supercapacitors, to give a glimpse into these potential applications of MOFs. - Graphical abstract: MOFs with large surface area and high porosity can offer more reaction sites and charge carriers diffusion path. Thus MOFs are used as cathode, anode, electrolyte, matrix and precursor materials for lithium ion battery, and also as electrode and precursor materials for supercapacitors. - Highlights: • MOFs have potential in electrochemical area due to their high porosity and diversity. • We summarized and compared works on MOFs for lithium ion battery and supercapacitor. • We pointed out critical challenges and provided possible solutions for future study.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Spatial heterogeneity analyses of pore structure and mineral composition of Barnett Shale using X-ray scattering techniques

The spatial heterogeneity of pore structure and mineral composition at mu m to mm scales in mm to cm-sized shale samples complicates the laboratory measurements of porosity & pore size distribution and consequently reservoir quality evaluation. Traditional fluid invasion characterization methods typically take hours to days to get data and can only test relatively small samples (usually 2.54 cm diameter core plugs and mm-sized rock chips). Furthermore, the Xray scattering techniques at the Advanced Photon Source of the Argonne National Laboratory have the capability to non-destructively determine the pore structure and mineral composition of mm x mm area in a short time of seconds and to hold several to hundreds of mm 2 sized sample to conduct large area heterogeneity analysis in the short duration of hours. With the use of ultra-small angle X-ray scattering (USAXS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS), the porosity, surface area and pore size distribution of two Barnett Shale samples have been mapped out and the mineral compositions are determined qualitatively. Overall, the porosity and pore surface area of the Barnett Shale Sample A over a 36 cm2 area ranges from 1.70 % to 8.13 % and 8.87 m 2 /g to 40.2 m 2 /g respectively. The porosity and surface area of Sample B over a 24 cm 2 area varies from 3.15 % to 11.7 % and 18.3 m 2 /g to 60.2 m 2 /g. In Sample A, the mineral composition shows a shift from carbonate-rich to siliciclastic-rich over a distance of several millimeters. For Sample B, the mineral compositions are mainly siliciclastic and do not show an obvious lithological change. The direct observations of high spatial heterogeneity of pore structure and mineral composition in shale illustrate the utility of integrated X-ray scattering techniques to provide valuable insights into shale studies and reservoir evaluation.

58 GEOSCIENCES↗
DOE OSTI2013

A study of the mechanism of laser welding defects in low thermal expansion superalloy GH909

In this paper, we describe experimental laser welding of low-thermal-expansion superalloy GH909. The main welding defects of GH909 by laser in the weld are liquation cracks and porosities, including hydrogen and carbon monoxide porosity. The forming mechanism of laser welding defects was investigated. This investigation was conducted using an optical microscope, scanning electron microscope, energy diffraction spectrum, X-ray diffractometer and other methodologies. The results demonstrated that porosities appearing in the central weld were related to incomplete removal of oxide film on the surface of the welding samples. The porosities produced by these bubbles were formed as a result of residual hydrogen or oxygenium in the weld. These elements failed to escape from the weld since laser welding has both a rapid welding speed and cooling rate. The emerging crack in the heat affected zone is a liquation crack and extends along the grain boundary as a result of composition segregation. Laves–Ni{sub 2}Ti phase with low melting point is a harmful phase, and the stress causes grain boundaries to liquefy, migrate and even crack. Removing the oxides on the surface of the samples before welding and carefully controlling technological parameters can reduce welding defects and improve formation of the GH909 alloy weld. - Highlights: ► It is a new process for the forming of GH909 alloy via laser welding. ► The forming mechanism of laser welding defects in GH909 has been studied. ► It may be a means to improve the efficiency of aircraft engine production.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Characterization of 430L porous supports obtained by powder extrusion moulding for their application in solid oxide fuel cells

The characterization of 430L stainless steel planar porous supports obtained by powder extrusion moulding was performed in this work. A thermoplastic multicomponent binder based on high density polyethylene and paraffin wax was selected for the process. Green supports were shaped by extrusion moulding, and subsequently the binder was removed by a thermal cycle previously optimized. Sintering was carried out at different temperatures in low vacuum. Density of sintered parts was measured by Archimedes' method and porosity was also evaluated through a microstructural analysis by optical microscopy. The porosity degree of samples sintered at low temperature was close to 35% which is a very suitable value for their application in SOFCs. Tensile tests were carried out in order to determine mechanical strength as a function of porosity degree. Based on these results, the best feedstock composition and processing parameters were selected. The oxidation behaviour in static air at high temperature was studied, and formed oxides were characterized in a scanning electron microscope equipped with energy dispersive analysis of X-rays. X-ray diffraction experiments were performed in order to identify the formed oxides based on formula Fe{sub 2−x}Cr{sub x}O{sub 3}. The results of these studies showed that this kind of ferritic stainless steel would be more suitable to be used as anodic supports where a rich hydrogen atmosphere is employed. Preliminary deposition tests allowed obtaining a homogeneous Ni–YSZ anode layer with a thickness of 10 μm on the porous metallic substrates. - Highlights: • 430L stainless steel porous supports were obtained by powder extrusion moulding. • Porosity degree was controlled sintering at different temperatures in low vacuum. • Tensile tests allowed determining mechanical strength of porous supports. • A study about its oxidation behaviour in static air at high temperature was realized. • After oxidation, formed oxides were characterized by EDS–SEM and XRD.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Interfacial characterization of alumina-to-alumina joints fabricated using silver–copper–titanium interlayers

Two Ag–Cu–Ti interlayers with different compositions (Ag–35.3Cu–1.75Ti and Ag–26.7Cu–4.5Ti) were used to join sintered polycrystalline Al{sub 2}O{sub 3} having different amounts of porosity to investigate the effect of titanium and porosity contents on evolution of interfacial chemistry and microstructures. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive spectroscopy (EDS) were used to characterize the interfacial microstructure. Two reaction layers, Ti{sub 2}O and Cu{sub 3}Ti{sub 3}O, were found at the interface of Ag–Cu–Ti interlayers and Al{sub 2}O{sub 3} using a series of simulated and experimental selected area diffraction patterns (SADP) of TEM and EDS. The total thickness of Ti{sub 2}O and Cu{sub 3}Ti{sub 3}O reaction layers at the interfaces increases with increasing amounts of Ti in the Ag–Cu–Ti interlayers but is independent of the porosity content in the Al{sub 2}O{sub 3}. Two possible formation mechanisms of Ti{sub 2}O and Cu{sub 3}Ti{sub 3}O reaction layers at the interface of Ag–Cu–Ti interlayers and Al{sub 2}O{sub 3} have been proposed based on the interfacial characterization performed in the present study. - Highlights: • Effect of alumina porosity and % Ti in interlayer on interface structure delineated • SEM, EDS, XRD, TEM with SADP used to delineate phases, compositions, crystallography • Ti{sub 2}O and Cu{sub 3}Ti{sub 3}O reaction layers identified and their formation mechanisms proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A complex approach to assessing porous structure of structured ceramics obtained by SPS technique

Highlights: • A complex approach to microstructural analysis of nanostructured SPS ceramics was presented. • A bunch of gas, intrusion and microscopic methods were applied for open/closed porosity determination in nanoceramics. • Kinetic TPR analysis for structural changes in nanoceramic was carried out. • 3D pore visualization for nanoceramics was provided via SEM/FIB tomography • Porosity calculations were performed via BET, BJH, t-plot, Washburn equation, FEI Avizo 9.1 software results. - Abstract: Spark plasma sintering (SPS) is a highly prospective technology providing rapid consolidation of nano-disperse compositions into structured ceramics with complex structural organization. Characterizing pore structure of such systems remains a challenge due to different types, size and shape of the pores as well as structural defects occurring in the material, thus requiring special methods to quantify certain porosity type. The paper presents a complex approach to studying structure of SPS hematite-based structured ceramics. The method involves a number of gas, intrusion and electron microscopy probing techniques to characterize open and closed pores in the ceramics bulk. Low temperature nitrogen sorption has been implemented to estimate open micro- and mesoporosity in the size range 0.7–50 nm using BET, BJH and t-plot methods to process experimental data. Additionally, structural peculiarities of consolidated structured ceramics have been studied using temperature-programmed reduction (TPR) with the kinetic analysis of the results being carried out. Volume of macropores sized above 50 nm has been measured with mercury intrusion. Closed pores and structural defects have been quantified with SEM and FIB/SEM tomography. By comparing experimental and estimated results we have shown that addressing all porosity types provides a highly precise structural characterization of the material.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Pore structure refinement of cement paste incorporating nanosilica: Study with dual beam scanning electron microscopy/focused ion beam (SEM/FIB)

Highlights: • The modifying effects of nanosilica on pore structure of cement-based composites are investigated. • Dual beam SEM/FIB is implemented to create the 3D pore structure model and calculate porosity and pore size distribution. • The porosity and pore diameter are found to decrease with the inclusion of nanosilica. - Abstract: Pozzolanic materials, micro- and nano-, have been found to improve the durability properties of cement-based materials by refining their pore structure. As a relatively newer material, the modifying effects of nanosilica on pore structure are still inconclusive in the literature. In this study, this was characterized by implementing dual beam SEM/FIB, which can generate 3D models of porous materials for quantitative analysis. The sample is milled by focused ion beam layer-by-layer, and each surface layer is 2D imaged via scanning electron microscopy. Three types of pores – large capillary pore, medium capillary pore and gel pore – can be observed. A 3D pore structure model is then reconstructed from 1000 of these 2D images, from which porosity and pore size distribution can be calculated. Cement pastes incorporating nanosilica and silica fume were compared. The porosity and pore diameter were found to decrease with the inclusion of nanosilica. Furthermore, reduction in capillary pores and subsequent increase in gel pores were also observed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Small-angle Neutron Scattering (SANS) Characterization of Clay- and Carbonate-rich Shale at Elevated Pressures

Unconventional oil and gas from shale formations have emerged as some of the fastest growing energy resources in the United States, providing both cleaner energy to consumers and reducing the nation’s reliance on energy imports. To properly harness these important natural resources, the nanopore structure of associated shales must be fully understood, particularly under hydraulic fracturing conditions, where they are exposed to both overburden compressive and hydrostatic fluid pressures. The current study uses small-angle neutron scattering (SANS) to characterize pore structure, including porosity, pore accessibility, and pore size distribution, in the 1–100 nm regime at elevated pressures for mineralogically distinct clay- and carbonate-rich shales from the Permian Basin. Unlike typical porosity measurement techniques, SANS is uniquely capable of characterizing both open and closed porosity, allowing measurement of how pore accessibility changes with pressure and determination of the size range of accessible versus inaccessible pores. The porosity of the clay-rich shale was 7.7%, compared to 0.51% for the carbonate-rich shale. However, only 2.6% of the nanopores in the carbonate-rich shale were inaccessible to water at 8 kPSI (55.1 MPa) compared to 7.8% for the clay-rich shale. Furthermore, our analyses indicated that the closed pores fall within distinct size ranges, likely corresponding with the chemical nature of the pore host material. These results provide valuable insight into the effects of shale petrophysical properties on hydrocarbon extraction from unconventional reservoirs.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Strain-Based Assessment of Shale Caprock during Cyclic Underground Hydrogen Storage

Successful large-scale underground hydrogen storage (UHS) in depleted gas reservoirs depends on the integrity of the overlying caprock to prevent hydrogen loss during cyclic injection and depletion. Prior studies on crushed Marcellus shale, a potential caprock, indicate that cyclic hydrogen injection and depletion induces microstructural changes, increasing porosity and permeability. However, the extent of these changes in intact shale remains unclear. This study presents a strain-based experimental approach to quantify volumetric strain evolution in intact Marcellus shale matrix under unconstrained stress conditions. A quadrant-shaped shale sample without visible fractures underwent eight hydrostatic pore-pressure cycles (injection to 1500 psi and depletion to 500 psi in 250 psi steps). Linear strain gauges measured strain in three orthogonal directions. Results indicate progressive plastic strain accumulation, leading to an ∼12% increase in matrix porosity after eight cycles, with an estimated 19% increase after 30 cycles. This porosity increase follows a logarithmic trend, suggesting a diminishing effect in later cycles. Additionally, permeability and diffusive mass flux are projected to rise by ∼70% over 30 cycles, enhancing hydrogen migration risk. The shale matrix also exhibited mechanical stiffening over successive cycles, limiting large-scale deformation but not preventing porosity enhancement. A new parameter, α, was introduced to characterize shale sensitivity to cyclic loading, aiding UHS caprock assessments. These findings underscore the necessity of incorporating cyclic loading effects in UHS site selection and operational strategies to ensure long-term storage integrity.

08 HYDROGEN↗
DOE OSTI2021

Surviving Under Pressure: The Role of Solvent, Crystal Size, and Morphology During Pelletization of Metal–Organic Frameworks

As metal–organic frameworks (MOFs) gain traction for applications, such as hydrogen storage, it is essential to form the as-synthesized powder materials into shaped bodies with high packing densities to maximize their volumetric performance. Mechanical compaction, which involves compressing the materials at high pressure, has been reported to yield high monolith density but often results in a significant loss in accessible porosity. Herein, we sought to systematically control (1) crystal size, (2) solvation, and (3) compacting pressure in the pelletization process to achieve high packing density without compromising the porosity that makes MOFs functional. It was determined that solvation is the most critical factor among the three factors examined. Solvation that exceeds the pore volume prevents the framework from collapsing, allowing for porosity to be maintained through pelletization. Higher pelletization pressure results in higher packing density, with extensive loss of porosity being observed at a higher pressure if the solvation is below the pore volume. Lastly, we observed that the morphology and size of the MOF particles result in variation in the highest achievable packing efficiency, but these numbers (75%) are still greater than many existing techniques used to form MOFs. Furthermore, we concluded that the application of pressure through pelletization is a suitable and widely applicable technique for forming high-density MOF-monoliths.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Molecular-Dynamics Analysis of the Mechanical Behavior of Plasma-Facing Tungsten

We report a systematic computational analysis of the mechanical behavior of plasma-facing component (PFC) tungsten focusing on the impact of void and helium (He) bubble defects on the mechanical response beyond the elastic regime. Specifically, we explore the effects of porosity and He atomic fraction on the mechanical properties and structural response of PFC tungsten, at varying temperature and bubble size. We find that the Young modulus of defective tungsten undergoes substantial softening that follows an exponential scaling relation as a function of matrix porosity and He atomic content. Beyond the elastic regime, our high strain rate simulations reveal that the presence of nanoscale spherical defects (empty voids and He bubbles) reduces the yield strength of tungsten in a monotonically decreasing fashion, obeying an exponential scaling relation as a function of tungsten matrix porosity and He concentration. Our detailed analysis of the structural response of PFC tungsten near the yield point reveals that yielding is initiated by emission of dislocation loops from bubble/matrix interfaces, mainly 1/2<111> shear loops, followed by gliding and growth of these loops and reactions to form <100> dislocations. Furthermore, dislocation gliding on the <111>{211} twin systems nucleates 1/6<111> twin regions in the tungsten matrix. These dynamical processes reduce the stress in the matrix substantially. Subsequent dislocation interactions and depletion of the twin phases via nucleation and propagation of detwinning partials lead the tungsten matrix to a next deformation stage characterized by stress increase during applied straining. Furthermore, our structural analysis reveals that the depletion of twin boundaries (areal defects) is strongly impacted by the density of He bubbles at higher porosities. After the initial stress relief upon yielding, increase in the dislocation density in conjunction with decrease in the areal defect density facilitates the initiation of dislocation-driven deformation mechanisms in the PFC crystal.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Controlling Mass Transport in Direct Carbon Dioxide Zero-Gap Electrolyzers via Cell Compression

The development of high-performance CO 2 electrolyzers is crucial for accelerating the sustainable production of fuels and chemicals integrated with renewable energy sources. Here, we introduce a methodology to actively control mass transport inside a realistic zero-gap membrane electrode assembly of a CO 2 electrolyzer by varying the gasket thickness, which consequently changes the cell compression. This allows control over the thickness and porosity of the gas diffusion electrodes, influencing the overall electrolyzer performance, as demonstrated using Ag-deposited electrodes. At low operating voltages (<2.9 V), both high- and low-compression electrolyzers exhibit similar faradaic efficiencies and partial current densities for CO formation. However, at high voltages, the low-compression electrolyzer with high electrode porosity demonstrates superior CO selectivity and activity with suppressed H 2 formation. These experimental results are validated by the computational membrane electrode assembly (MEA) model developed by using the measured in situ electrode thicknesses and electrode porosities. Additionally, liquid electrolyte saturation at the catalyst layer is found to play a dominant role in determining the mass transport, resulting in a decreased electrolyzer performance with low electrode porosity. Finally, the systematic investigation in this study improves the understanding of the transport dynamics in MEA-based devices and provides insights into optimizing device design parameters for industry-relevant CO 2 electrolysis.

30 DIRECT ENERGY CONVERSION↗
DOE OSTI2014

Shock compression behavior of bi-material powder composites with disparate melting temperatures

Laser driven experiments were used to investigate the shock compression behavior of powder processed Bismuth/Tungsten (Bi/W) composite samples. The constituents provide different functionality to the composite behavior as Bi could be shock melted at the pressures attained in this work, while the W could not. Samples were prepared by uniaxial pressing, and the relative density was measured as a function of particle size, applied pressure, and composition for both hot and cold pressing conditions. This resulted in sample densities between 73% and 99% of the theoretical maximum density, and also noticeable differences in microstructure in the hot and cold pressed samples. The compression waves were generated with a 1.3 × 1.3 mm square spot directly onto the surface of the sample, using irradiances between 10{sup 12} and 10{sup 13} W/cm{sup 2}, which resulted in calculated peak pressures between 50 and 150 GPa within a few micrometers. Sample recovery and post-mortem analysis revealed the formation of a crater on the laser drive surface, and the depth of this crater corresponded to the depth to which the Bi had been melted. The melt depth was found to be primarily a function of residual porosity and composition, and ranged from 167 to 528 μm. In general, a higher porosity led to a larger melt depth. Direct numerical simulations were performed, and indicated that the observed increase in melt depth for low-porosity samples could be largely attributed to increased heating associated with work done for pore collapse. However, the relative scaling was sensitive to composition, with low volume fraction Bi samples exhibiting a much stronger dependence on porosity than high Bi content samples. Select samples were repeated using an Al foil ablator, but there were no noticeable differences ensuring that the observed melting was indeed pressure-driven and was not a result of direct laser heating. The resultant microstructures and damage near the spall surface were also investigated qualitatively.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Dual mechanical behaviour of hydrogen in stressed silicon nitride thin films

In the present article, we report a study on the mechanical behaviour displayed by hydrogen atoms and pores in silicon nitride (SiN) films. A simple three-phase model is proposed to relate the physical properties (stiffness, film stress, mass density, etc.) of hydrogenated nanoporous SiN thin films to the volume fractions of hydrogen and pores. This model is then applied to experimental data extracted from films deposited by plasma enhanced chemical vapour deposition, where hydrogen content, stress, and mass densities range widely from 11% to 30%, −2.8 to 1.5 GPa, and 2.0 to 2.8 g/cm{sup 3}, respectively. Starting from the conventional plotting of film's Young's modulus against film porosity, we first propose to correct the conventional calculation of porosity volume fraction with the hydrogen content, thus taking into account both hydrogen mass and concentration. The weight of this hydrogen-correction is found to evolve linearly with hydrogen concentration in tensile films (in accordance with a simple “mass correction” of the film density calculation), but a clear discontinuity is observed toward compressive stresses. Then, the effective volume occupied by hydrogen atoms is calculated taking account of the bond type (N-H or Si-H bonds), thus allowing a precise extraction of the hydrogen volume fraction. These calculations applied to tensile films show that both volume fractions of hydrogen and porosity are similar in magnitude and randomly distributed against Young's modulus. However, the expected linear dependence of the Young's modulus is clearly observed when both volume fractions are added. Finally, we show that the stiffer behaviour of compressive films cannot be only explained on the basis of this (hydrogen + porosity) volume fraction. Indeed this stiffness difference relies on a dual mechanical behaviour displayed by hydrogen atoms against the film stress state: while they participate to the stiffness in compressive films, hydrogen atoms mainly behave like pores in tensile films where they do not participate to the film stiffness.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Structural and functional studies of bioobjects prepared from femoral heads

Results of examination of physicomechanical characteristics of samples of medial femoral head cuts are presented. The samples of medial femoral head cuts resected in 6 patients with coxarthrosis in primary endoprosthetic replacement of a coxofemoral joint have been tested for micro- and nanohardness. Young’s modulus and elemental composition of bone tissue have been investigated. To estimate the architectonics of cancellous tissue of the femoral head, adjacent cuts of the same patient have been analyzed. The porosity of bone tissue was estimated from macroscopic images obtained using macrophotography. The total porosity is calculated as the ratio of the total length of straight line segments overlapping pores to the total length of secants. A three-point bending test of the samples has shown that their strength changed from 0.187 to 1.650 MPa and their elasticity modulus changes from 1.69 to 8.15 MPa. The microhardness of the samples changes in the range 220–265 MPa and the average microhardness of medial femoral head cuts is 240 MPa. The elemental composition of medial femoral head cuts is represented by basic Ca, P, O, Na and Mg elements as well as by Sn, S, Fe, Cr, and C in microamounts. The atomic Ca to P ratio for bone tissue is 1.55. It is revealed that pores of the upper part of the femoral head have a more regular shape and in the lower part they are more elongated along the cut and occupy a larger volume. The lower part of the femoral head has a higher porosity (39 and 33%) than the upper part (34 and 30%). The total porosity of all samples does not exceed 37%.

62 RADIOLOGY AND NUCLEAR MEDICINE↗
DOE OSTI2016

Preparation and characterization of nanocomposite polymer electrolytes poly(vinylidone fluoride)/nanoclay

Polymer electrolytes are defined as semi solid electrolytes used as separator in lithium ion battery. Separator used as medium for transfer ions and to prevent electrical short circuits in battery cells. To obtain the optimal battery performance, separator with high porosity and electrolyte uptake is required. This can reduce the resistance in the transfer of ions between cathode and anode. The main objective of this work is to investigate the impact of different solvent (Dimethyl acetamide (DMAc), N-methyl-2-pyrrolidone (NMP) and dimethyl formamide (DMF)), pore forming agent poly(vinylpyrolidone) (PVP) and nanoclay as filler in addition of membrane using phase inversion method on the morphology, porosity, electrolyte uptake and degree of crystallinity. The membrane was prepared by the phase inversion method by adding PVP and Nanoclay using different solvents. The phase inversion method was prepared by dissolving Nanoclay and PVP in solvent for 1-2 hours, and then add the PVDF with stirring for 4 hours at 60°C. The membranes were characterized by porosity test, electrolyte uptake test, scanning electron microscope (SEM), and X-ray diffraction (XRD). The results showed that DMAc as solvent gives the highest value of porosity and electrolyte uptake. The addition of nanoclay and PVP enlarge the size of the pores and reduce the degree of crystallinity. So, the usage of DMAc as solvent is better than NMP or DMF.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗