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DOE OSTI2014

Co-localised Raman and force spectroscopy reveal the roles of hydrogen bonds and π-π interactions in defining the mechanical properties of diphenylalanine nano- and micro-tubes

An integrated atomic force and polarized Raman microscope were used to measure the elastic properties of individual diphenylalanine (FF) nano- and micro-tubes and to obtain quantitative information regarding the inter-molecular interactions that define their mechanical properties. For individual tubes, co-localised force spectroscopy and Raman spectroscopy measurements allowed the calculation of the Young's and shear moduli (25 ± 5 GPa and 0.28 ± 0.05 GPa, respectively) and the contribution of hydrogen bonding network to the Young's modulus (∼17.6 GPa). The π-π interactions between the phenyl rings, dominated by T-type arrangements, were estimated based on previously published X-ray data to only 0.20 GPa. These results provide experimental evidence obtained from individual FF tubes that the network of H-bonds dominates the elastic properties of the FF tubes.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Zirconium dioxide nanofilled poly(vinylidene fluoride-hexafluoropropylene) complexed with lithium trifluoromethanesulfonate as composite polymer electrolyte for electrochromic devices

Highlights: • Successful synthesis of electrolyte by blending PVdF-HFP, ZrO{sub 2} and LiCF{sub 3}SO{sub 3}. • ZrO{sub 2} increased electrolyte conductivity by two orders of magnitude. • ZrO{sub 2} doubled bulk mechanical strength of electrolyte in terms of Young’s modulus. • Electrolytes gave a optimum optical transmittance of 52.6%. - Abstract: Poly(vinylidene fluoride-hexafluoropropylene) (PVdF-HFP) polymer electrolyte containing zirconium dioxide nanocrystals (ZrO{sub 2}-NC) and lithium trifluoromethanesulfonate (LiCF{sub 3}SO{sub 3}) has been synthesized using the conventional solution casting method. The addition of ZrO2-NC into the polymeric substrate gave remarkable properties in terms of the electrolyte’s ionic conductivity as well as its bulk mechanical strength. The enhanced amorphicity of the polymeric substrate due to ZrO{sub 2} and the nanofiller’s high dielectric constant make an excellent combination to increase the ionic conductivity (above 10{sup −4} S cm{sup −1}). Increasing the nanofiller content raises the ionic conductivity of the electrolyte by two orders of magnitude of which the optimum is 2.65 × 10{sup −4} S cm{sup −1} at 13.04 wt% ZrO{sub 2}-NC loading. Also, the Young’s modulus, an indicator of electrolyte’s mechanical stability, dramatically increased to 207 MPa upon loading 13.04 wt% ZrO{sub 2}-NC. Using UV–vis spectroscopy, the electrolytes with 13.04% ZrO{sub 2}-NC scanned from 200–800 nm wavelengths exhibited a maximum optical transmittance of 52.6% at 10 μm film thickness. The enhanced conductivity, high mechanical strength and reasonable optical transmittance shown by our composite polymer electrolyte make an excellent electrolyte for future energy saving smart windows such as electrochromic devices.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Dissimilar Tendencies of Innovative Green Clay Organo-Modifier on the Final Properties of Poly(ε-caprolactone) Based Nanocomposites

Composites based on poly(ε-caprolactone) (PCL) were prepared by melt blending the polymer with natural and modified bentonite. Soy lecithin (SL), a natural and nontoxic biosurfactant, was used as modifier agent. Three organoclays with different SL contents were employed as fillers and composites containing 1 and 2 wt% of each clay, were prepared. Thermal (by thermogravimetric analysis, and differential scanning calorimetry), morphological (by X-ray diffraction (XRD) and melt rheology), mechanical (by tensile tests) and barrier properties (by means of water vapor permeability tests) of matrix and composites were studied as a function of clay type and content. Morphological analysis by XRD showed nanocomposites with intercalated-exfoliated structures while melt rheology suggests thermal degradation of PCL matrix catalyzed by SL bentonite modifier. Thermal and mechanical properties were consistent with this assumption, due to the slight increment in crystallinity percentage and detriment in the Young’s modulus of the nanocomposites in comparison with the neat matrix. On the other hand, water vapor permeability of PCL significantly decreased in composites, as is expected for polymer/clay nanocomposites, favoring its potential application as food packaging. Thus, dissimilar tendencies were found in the final properties of the nanocomposites that were attributed to the matrix molecular weight degradation catalyzed by the novel green clay organo-modifier.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Temperature effect of elastic anisotropy and internal strain development in advanced nanostructured alloys: An in-situ synchrotron X-ray investigation

Nanostructured ferritic alloys (NFAs) are a promising structural material for advanced nuclear systems due to their exceptional radiation tolerance and high-temperature mechanical properties. Their remarkable properties result from the ultrafine ultrahigh density Y-Ti-O nanoclusters dispersed within the ferritic matrix. In this work, we performed in-situ synchrotron X-ray diffraction tests to study the tensile deformation process of the three types of NFAs: 9YWTV, 14YWT-sm13, and 14YWT-sm170 at both room temperature and elevated temperatures. A technique was developed, combining Kroner’s model and X-ray measurement, to determine the intrinsic monocrystal elastic-stiffness constants, and polycrystal Young’s modulus and Poisson’s ratio of the NFAs. Temperature dependence of elastic anisotropy was observed in the NFAs. An analysis of intergranular strain and strengthening factors determined that 14YWT-sm13 had a higher resistance to temperature softening compared to 9YWTV, attributed to the more effective nanoparticle strengthening during high-temperature mechanical loading.

Gan, Yingye↗

DOE OSTI2019

Investigation of Stress Field and Fracture Development During Shale Maturation Using Analog Rock Systems

The emergence of hydrocarbons within shale as a major recoverable resource has sparked interest in fluid transport through these tight mudstones. Recent studies suggest the importance to recovery of microfracture networks that connect localized zones with large organic content to the inorganic matrix. This paper presents a joint modeling and experimental study to examine the onset, formation, and evolution of microfracture networks as shale matures. Both the stress field and fractures are simulated and imaged. A novel laboratory-scale, phase-field fracture propagation model was developed to characterize the material failure mechanisms that play a significant role during the shale maturation process. The numerical model developed consists of coupled solid deformation, pore pressure, and fracture propagation mechanisms. Benchmark tests were conducted to validate model accuracy. Laboratory-grade gelatins with varying Young’s modulus were used as scaled-rock analogs in two dimensional Hele-Shaw cell apparatus. Yeast within the gelatin generates gas in a fashion analogous to hydrocarbon formation as shale matures. These setups allow study and visualization of host rock elastic-brittle fracture and fracture network propagation mechanisms. The experimental setup was fitted to utilize photoelasticity principles coupled with birefringence properties of gelatin to explore visually the stress field of the gelatin as the fracture network developed. Stress optics image analysis and Linear Elastic Fracture Mechanics (LEFM) principles for crack propagation were used to monitor fracture growth for each gelatin type. Observed and simulated responses suggest gas diffusion within and deformation of the gelatin matrix as predominant mechanisms for energy dissipation depending on gelatin strength. LEFM, an experimental estimation of principal stress development with fracture growth, at different stages was determined for each gelatin rheology. Here, the interplay of gas diffusion and material deformation determines the resulting frequency and pattern of fractures. Results correlate with Young’s modulus. Experimental and computed stress fields reveal that fractures resulting from internal gas generation are similar to, but not identical to, type 1 opening mode.

58 GEOSCIENCES↗

DOE OSTI2014

Pressure-assisted fabrication of organic light emitting diodes with MoO{sub 3} hole-injection layer materials

In this study, pressures of ∼5 to ∼8 MPa were applied to organic light emitting diodes containing either evaporated molybdenum trioxide (MoO{sub 3}) or spin-coated poly(3,4-ethylene dioxythiophene) doped with poly(styrene sulphonate) (PEDOT:PSS) hole-injection layers (HILs). The threshold voltages for both devices were reduced by about half, after the application of pressure. Furthermore, in an effort to understand the effects of pressure treatment, finite element simulations were used to study the evolution of surface contact between the HIL and emissive layer (EML) under pressure. The blister area due to interfacial impurities was also calculated. This was shown to reduce by about half, when the applied pressures were between ∼5 and 8 MPa. The finite element simulations used Young's modulus measurements of MoO{sub 3} that were measured using the nanoindentation technique. They also incorporated measurements of the adhesion energy between the HIL and EML (measured by force microscopy during atomic force microscopy). Within a fracture mechanics framework, the implications of the results are then discussed for the pressure-assisted fabrication of robust organic electronic devices.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Physicochemical, Antimicrobial and Cytotoxic Characteristics of Corn Starch Film Containing Propolis for Wound Dressing

Modern dressings increase the rate of wound healing rather than just covering them. Dressing can protect the injured skin and keep it appropriately moist to speed up the healing process. In this study, the ethanolic extract of propolis loaded with corn starch was successfully prepared using solvent casting. Characterizations of the samples performed in respect to their mechanical properties were examined by scanning electron microscopy, contact angle, and attenuated total reflectance—fourier transform infrared spectroscopy, as well as antimicrobial capacities. The MTT assay using fibroblast cells showed the cell viability of corn starch in the ethanolic extract of propolis wound dressing. The results showed that by increasing the amount of ethanolic propolis extract from 0.25 to 1%, the tensile strength and the Young’s modulus of the samples were decreased, the elongation at the break increased about 15% as compared to the control films, and the contact angle properties were detected by a slightly hydrophobic character of the films in the antibacterial activity against Escherichia coli and Staphylococcus aureus even at low ethanolic extract of propolis concentrations (1%), mainly due to its phenolic compounds. Therefore, ethanolic extract of propolis loaded with corn starch film will be a potential candidate for wound dressing and skin tissue engineering.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Flux Pinning-Induced Stress in a Long Hollow Cylindrical Superconductor Restricted by a Metal Tube

The tensile stress in a hollow cylindrical superconductor completely restricted by a metal tube in a parallel magnetic field is investigated. Using the plane strain approach, analytical expressions for the stress distribution of the superconductor and the contact stress between the metal tube and the superconductor are obtained and show that both the ratio of Young’s modulus and thickness ratio of the high-temperature superconductors and the metal tube significantly affect the stress distribution in the superconductor explicitly. In addition, the flux pinning-induced stress in the above-mentioned superconductor is systematically studied by the exponential critical state model during the field cooling process. The results indicate that the metal tube can reduce effectively the tensile stress in the hollow cylindrical superconductor during the magnetization process. The findings suggest that the appropriate selection of material parameters and size of the metal tube can improve superconductor performance efficiently.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Mechanical deformations of boron nitride nanotubes in crossed junctions

We present a study of the mechanical deformations of boron nitride nanotubes (BNNTs) in crossed junctions. The structure and deformation of the crossed tubes in the junction are characterized by using atomic force microscopy. Our results show that the total tube heights are reduced by 20%–33% at the crossed junctions formed by double-walled BNNTs with outer diameters in the range of 2.21–4.67 nm. The measured tube height reduction is found to be in a nearly linear relationship with the summation of the outer diameters of the two tubes forming the junction. The contact force between the two tubes in the junction is estimated based on contact mechanics theories and found to be within the range of 4.2–7.6 nN. The Young's modulus of BNNTs and their binding strengths with the substrate are quantified, based on the deformation profile of the upper tube in the junction, and are found to be 1.07 ± 0.11 TPa and 0.18–0.29 nJ/m, respectively. Finally, we perform finite element simulations on the mechanical deformations of the crossed BNNT junctions. The numerical simulation results are consistent with both the experimental measurements and the analytical analysis. The results reported in this paper contribute to a better understanding of the structural and mechanical properties of BNNTs and to the pursuit of their applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Note: A component-level frequency tunable isolator for vibration-sensitive chips using SMA beams

This note presents a component-level frequency tunable isolator for vibration-sensitive chips. The isolator employed 8 U-shaped shape memory alloy (SMA) beams to support an isolation island (used for mounting chips). Due to the temperature-induced Young’s modulus variation of SMA, the system stiffness of the isolator can be controlled through heating the SMA beams. In such a way, the natural frequency of the isolator can be tuned. A prototype was fabricated to evaluate the concept. The test results show that the natural frequency of the isolator can be tuned in the range of 64 Hz–97 Hz by applying different heating strategies. Moreover, resonant vibration can be suppressed significantly (the transmissibility decreases about 65% near the resonant frequency) using a real-time tuning method.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Microstructure and mechanical properties of bulk highly faulted fcc/hcp nanostructured cobalt microstructures

Nanostructured cobalt powders with an average particle size of 50 nm were synthesized using a polyol method and subsequently consolidated by spark plasma sintering (SPS). SPS experiments performed at 650 °C with sintering times ranging from 5 to 45 min under a pressure of 100 MPa, yielded to dense bulk nanostructured cobalt (relative density greater than 97%). X-ray diffraction patterns of the as-prepared powders showed only a face centered cubic (fcc) crystalline phase, whereas the consolidated samples exhibited a mixture of both fcc and hexagonal close packed (hcp) phases. Transmission electron microscopy observations revealed a lamellar substructure with a high density of nanotwins and stacking faults in every grain of the sintered samples. Room temperature compression tests, carried out at a strain rate of 10{sup −3} s{sup −1}, yielded to highest strain to fracture values of up to 5% for sample of holding time of 15 min, which exhibited a yield strength of 1440 MPa, an ultimate strength as high as 1740 MPa and a Young's modulus of 205 GPa. The modulus of elasticity obtained from the nanoindentation tests, ranges from 181 to 218 GPa. The lowest modulus value of 181 GPa was obtained for the sample with the highest sintering time (45 min), which could be related to mass density loss as a consequence of trapped gases releasing. - Highlights: • Co nanopowder (50 nm) was prepared by reduction in polyol medium. • SPS was used to process bulk nanostructured Co specimens. • Microstructures were made of intricate fcc/hcp, along with nanotwins and SFs. • High strengths and moderate compressive ductility were obtained. • Deformation mechanisms related to complex interplay of different length scales.

36 MATERIALS SCIENCE↗

DOE OSTI2019

A two-set order parameters phase-field modeling of crack deflection/penetration in a heterogeneous microstructure

Modeling of crack deflection/penetration or manifested as intergranular/transgranular fracture in polycrystals has long been a challenge in both fracture mechanics and materials science. A phase-field model formulated with two-set order parameters describing the crack field and the microstructure field respectively, is herein established to investigate the competition between crack penetration and deflection at an interface. The advantages of the proposed model are three-fold: (1) the fracture toughness of grain boundaries and/or interfaces, besides single crystal properties (e.g., Young’s modulus, Poisson ratio, and fracture toughness), can be automatically incorporated, (2) cohesive interfaces are treated in one phase-field framework in comparison with the integrated phase-field and cohesive zone model in which cohesive elements have to be manually placed at the interface, and (3) two-set order parameters enable to describe the concurrent crack propagation and microstructure evolution. The proposed model is validated by comparing the simulated critical deflection angles with the results from theoretical analysis of the linear elastic fracture mechanics and the experiments. The model is then applied to a heterogeneous Silicon Nitride polycrystal to determine the effect of interface fracture toughness on the intergranular/transgranular fracture transition and the effective toughness of the materials.

Chen, Hu↗

NASA NTRS1974

High modulus invert analog glass compositions containing beryllia

Glass compositions having a Young's modulus of at least 15 million psi and a specific modulus of at least 110 million inches consisting essentially of, in mols, 10-45% SiO2, 2-15% Li2O, 3-34% BeO, 12-36% of at least one bivalent oxide selected from the group consisting of CaO, ZnO, MgO and CuO, 10-39% of at least one trivalent oxide selected from the group consisting of Al2O3, B2O3, La2O3, Y2O3 and the mixed rare earth oxides, the total number of said bivalent and trivalent oxides being at least three, and up to 10% of a tetravalent oxide selected from the group consisting of ZrO2, TiO2 and CeO2.

Bacon, J. F.↗

DOE OSTI2014

Mechanically induced self-propagating reaction and consequent consolidation for the production of fully dense nanocrystalline Ti{sub 55}C{sub 45} bulk material

We employed a high-energy ball mill for the synthesis of nanograined Ti{sub 55}C{sub 45} powders starting from elemental Ti and C powders. The mechanically induced self-propagating reaction that occurred between the reactant materials was monitored via a gas atmosphere gas-temperature-monitoring system. A single phase of NaCl-type TiC was obtained after 5 h of ball milling. To decrease the powder and grain sizes, the material was subjected to further ball milling time. The powders obtained after 200 h of milling possessed spherical-like morphology with average particle and grain sizes of 45 μm and 4.2 nm, respectively. The end-products obtained after 200 h of ball milling time, were then consolidated into full dense compacts, using hot pressing and spark plasma sintering at 1500 and 34.5 MPa, with heating rates of 20 °C/min and 500 °C/min, respectively. Whereas hot pressing of the powders led to severe grain growth (∼ 436 nm in diameter), the as-spark plasma sintered powders maintained their nanograined characteristics (∼ 28 nm in diameter). The as-synthesized and as-consolidated powders were characterized, using X-ray diffraction, high-resolution electron microscopy, and scanning electron microscopy. The mechanical properties of the consolidated samples obtained via the hot pressing and spark plasma sintering techniques were characterized, using Vickers microhardness and non-destructive testing techniques. The Vickers hardness, Young's modulus, shear modulus and fracture toughness of as-spark plasma sintered samples were 32 GPa, 358 GPa, 151 GPa and 6.4 MPa·m{sup 1/2}, respectively. The effects of the consolidation approach on the grain size and mechanical properties were investigated and are discussed. - Highlights: • Room-temperature synthesizing of NaCl-type TiC • Dependence on the grain size on the ball milling time • Fabrication of equiaxed nanocrystalline grains with a diameter of 4.2 nm • Fabrication of nanocrystalline bulk TiC material by SPS with minimal grain growth • Dependence of improved mechanical properties on the consolidation techniques.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Microstructural and bulk property changes in hardened cement paste during the first drying process

This paper reports the microstructural changes and resultant bulk physical property changes in hardened cement paste (hcp) during the first desorption process. The microstructural changes and solid-phase changes were evaluated by water vapor sorption, nitrogen sorption, ultrasonic velocity, and {sup 29}Si and {sup 27}Al nuclear magnetic resonance. Strength, Young's modulus, and drying shrinkage were also examined. The first drying process increased the volume of macropores and decreased the volume of mesopores and interlayer spaces. Furthermore, in the first drying process globule clusters were interconnected. During the first desorption, the strength increased for samples cured at 100% to 90% RH, decreased for 90% to 40% RH, and increased again for 40% to 11% RH. This behavior is explained by both microstructural changes in hcp and C–S–H globule densification. The drying shrinkage strains during rapid drying and slow drying were compared and the effects of the microstructural changes and evaporation were separated.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Elastic-properties measurement at high temperatures through contact resonance atomic force microscopy

Miniaturization of products and need for further improvement of machines performance introduce new serious challenges in materials characterization. In particular non-destructive mechanical testing in the sub-micrometer scale is needed to better understand and improve micro-manufacturing operations. To this regard, some open issues are of particular interest: low depth of penetration, high lateral resolution and measurements at elevated temperatures. An interesting solution is given by acoustic microscopy techniques, which can be successfully implemented for advanced research in surface elasticity, allowing fast direct and non-destructive measurement of Young’s modulus and related surface parameters. In this work an instrument set up for Contact Resonance Atomic Force Microscopy is proposed, where the sample with is coupled to a heating stage and a piezoelectric transducer directly vibrate the cantilever during scanning, in order to allow exploitation of high resolution measurements at relatively high temperatures. Such instrument set up was undergone a set of calibration experiments in order to allow not only qualitative but also quantitative characterization of surfaces. The work was completed with a feasibility study with mechanical and topography measurements at temperatures as high as 150°C, with lateral resolution lower than 100 nm.

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 OSTI2014

Fluoroethylenepropylene ferroelectret films with cross-tunnel structure for piezoelectric transducers and micro energy harvesters

Layered fluoroethylenepropylene (FEP) ferroelectret films with cross-tunnel structure were fabricated from sheets of FEP films by template-patterning followed by a fusion-bonding process and contact charging. The typical piezoelectric d{sub 33} coefficients, measured by a quasi-static method of samples not annealed, are in the range of 1000–3700 pC/N. The resonance behavior of the samples is analyzed by dielectric spectroscopy which also yields Young's modulus. Microphones built with such films exhibit a somewhat decreasing frequency response up to 1 kHz, an increase of the responses due to diffraction effects at higher frequencies, and eventually a peak probably due to a thickness resonance at about 40 kHz. Annealing at 125 °C indicates that the sensitivity stabilizes at about 40% of the original value. From this data, stable dynamic d{sub 33} coefficients of up to 300 pC/N can be calculated. A micro energy harvesting generator utilizing these films and based on the excitation of thickness vibrations is also described. With an active area of 4.3 cm{sup 2} and a seismic mass of 69.5 g, power up to 0.5 μW referred to an acceleration of 1 g can be generated at a frequency of 120 Hz.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗