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At least 1,207 records · Page 67

All sources NASA NTRS DOE OSTI

DOE OSTI2018

Direct AFM-based nanoscale mapping and tomography of open-circuit voltages for photovoltaics

The nanoscale optoelectronic properties of materials can be especially important for polycrystalline photovoltaics including many sensor and solar cell designs. For thin film solar cells such as CdTe, the open-circuit voltage and short-circuit current are especially critical performance indicators, often varying between and even within individual grains. A new method for directly mapping the open-circuit voltage leverages photo-conducting AFM, along with an additional proportional-integral-derivative feedback loop configured to maintain open-circuit conditions while scanning. Alternating with short-circuit current mapping efficiently provides complementary insight into the highly microstructurally sensitive local and ensemble photovoltaic performance. Furthermore, direct open-circuit voltage mapping is compatible with tomographic AFM, which additionally leverages gradual nanoscale milling by the AFM probe essentially for serial sectioning. The two-dimensional and three-dimensional results for CdTe solar cells during in situ illumination reveal local to mesoscale contributions to PV performance based on the order of magnitude variations in photovoltaic properties with distinct grains, at grain boundaries, and for sub-granular planar defects.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS1985

Sputtered W-N diffusion barriers

The thermal stability of reactively sputtered tungsten-nitrogen alloy thin films is investigated for the application as diffusion barriers in silicon contact metallizations. The composition of W-N barriers is varied over a wide range including pure W. Aluminum, gold, and silver are used as low resistivity overlayers. Metallurgical interactions at temperatures ranging from 500 to 900 C are studied. Incorporating nitrogen into tungsten advantageously stabilizes all three systems. The overall failure takes place rapidly above critical temperatures that depend on both the metal overlayer and the microstructure of the barrier. In some cases, W-N alloys can effectively prevent interdiffusion at temperatures as high as 800 C for 30 min.

Kattelus, H. P.↗

DOE OSTI2020

Corrosion behavior of ferritic FeCrAl alloys in simulated BWR normal water chemistry

Ferritic iron-chromium-aluminum (FeCrAl) alloys with varying Cr content were subjected to in-situ irradiation-corrosion with energetic protons or electron beams in pure water with various oxygen concentrations. Oxide microstructure and composition were characterized to compare the corrosion under irradiation with the thermal corrosion in the same water conditions. The dominant effect seems to be the production of H 2 O 2 at the surface by the intense proton and electron beams. The corrosion potential of FeCrAl under BWR-NWC condition is somewhat above the Cr 2 O 3 /CrO 4 2- phase boundary, oxidizing the Cr(III) to Cr(VI) in the outer part of the film, but with some Cr(III) remaining in the interior of the oxide. The beam increases the corrosion potential, significantly reducing Cr(III) content throughout the oxide. Finally, the crystallites on the surface, which form by re-precipitation from solution, do not contain Cr because at low potential Cr(III) is not soluble, and at high potential Cr(VI) is quite soluble.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Improved Understanding of Zircaloy Hydrogen Pickup Mechanisms in BWRs. NSUF Report (Final Report)

Using an instrumented autoclave operating at 288°C and 1100 psi, electrical impedance spectroscopy (EIS) measurements were taken from three neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). The three high priority fuel channel samples were tested at 288°C using a simulated PWR water with the AC frequency range extending down through 10 -4 Hz, with corresponding DC measurements to validate the resistance measurements. EIS measurements were also taken at room temperature using a simulated PWR water from four neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). and four water rod samples (Zircaloy-2). EIS measurements were also performed on unirradiated Zircaloy-2 tubes that were previously oxidized in autoclaves at various temperatures for different time durations to obtain oxide layers of different thicknesses. These experiments proved to be more challenging than anticipated because of the small size of the samples, which required development of fixtures to allow valid testing of the materials, some of which are radioactive, under pressure and temperature. Equivalent circuits were used to model the data. Some samples resulted in Nyquist plots where the arcs were too close to each other resulting in the inability to separate the different oxide morphological thicknesses. Microstructural characterization in the form of optical microscopy, scanning electron microscopy and (scanning) transmission electron microscopy was performed to document the microstructural features of the oxidized Zr-2 and Zr-4 samples (oxide and metal/oxide interface) and to interpret the EIS results. At the start of this work, it was assumed that despite the laminar cracks and porosity visible in both optical and SEM, the oxide scale is dense near the metal, effectively preventing the water from contacting the metal directly. While it is generally accepted that the large laminar cracks pores allow the water to percolate into the oxide film, it is unknown just how deep it can go, and how interconnected is the porosity, which will dictate how much the porosity is connected electrically to the water within the oxide scale. The EIS results demonstrated that there is in fact a distribution of oxide thicknesses over the various samples, and within each material condition, that are communicating to the liquid. This is derived from the fact that Nyquist plots have an arc radius whose center point is often below the Z’ axis, implying that instead of a single oxide thickness, these oxides have a distribution of thicknesses. This distribution of thicknesses produces arcs that are not clearly separable in most of the samples.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1987

Mechanical properties and morphology of poly(etheretherKetone)

Mechanical properties and morphology of poly(etheretherketone) (PEEK) were studied for samples having different thermal histories. Isothermal and rate-dependent crystallization were studied to ascertain the relationship between crystallinity/morphology and processing condition. Degree of crystallinity and microstructure were controlled by cooling the melt at different rates, ranging from quenching to slowly cooling, and by annealing amorphous material above the glass transition temperature Tg. It is found that degree of crystallinity was not as important as processing history in determining the room temperature mechanical properties. Samples with the same degree of crystallinity had very different tensile properties, depending on rate of cooling from the melt. All samples yielded by shear band formation and necked down. Quenched films had the largest breaking strains, drawing to 270 percent. Slowly cooled films exhibited ductile failure at relatively low strains. Best combined mechanical properties were obtained from semicrystalline films cooled at intermediate rates from the melt.

Cebe, Peggy↗

DOE OSTI2021

Unraveling the Unconventional Order of a High-Mobility Indacenodithiophene-Benzothiadiazole Copolymer

We report a new class of donor–acceptor (D-A) copolymers found to produce high charge carrier mobilities competitive with amorphous silicon (>1 cm 2 V –1 s –1 ) exhibit the puzzling microstructure of substantial local order, however lacking long-range order and crystallinity previously deemed necessary for achieving high mobility. Here, we demonstrate the application of low-dose transmission electron microscopy to image and quantify the nanoscale and mesoscale organization of an archetypal D-A copolymer across areas comparable to electronic devices (≈9 μm 2 ). The local structure is spatially resolved by mapping the backbone (001) spacing reflection, revealing nanocrystallites of aligned polymer chains throughout nearly the entire film. Analysis of the nanoscale structure of its ordered domains suggests significant short- and medium-range order and preferential grain boundary orientations. Moreover, we provide insights into the rich, interconnected mesoscale organization of this new family of D-A copolymers by analysis of the local orientational spatial autocorrelations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1982

Durability of spacecraft materials

Research efforts are reviewed on the space durability of materials, including radiation effects on polymer matrix composites and films, dimensional stability of polymer matrix composites and tension-stabilized cables, and thermal control coatings. Research to date has concentrated on establishing a fundamental understanding of space environmental effects on current graphite-reinforced composites and polymer systems, and development of analytical models to explain observed changes in mechanical, physical, and optical properties. As a result of these research efforts, new experimental facilities have been developed to simulate the space environment and measure the observed property changes. Chemical and microstructural analyses have also been performed to establish damage mechanisms and the limits for accelerated testing. The implications of these results on material selection and system performance are discussed and additional research needs and opportunities in the area of tougher resin/matrix and metal/matrix composites are identified.

Darrel R. Tenney↗

DOE OSTI2017

Ion-damage-free planarization or shallow angle sectioning of solar cells for mapping grain orientation and nanoscale photovoltaic properties

Ion beam milling is the most common modern method for preparing specific features for microscopic analysis, even though concomitant ion implantation and amorphization remain persistent challenges, particularly as they often modify materials properties of interest. Atomic force microscopy (AFM), on the other hand, can mechanically mill specific nanoscale regions in plan-view without chemical or high energy ion damage, due to its resolution, directionality, and fine load control. As an example, AFM-nanomilling (AFM-NM) is implemented for top-down planarization of polycrystalline CdTe thin film solar cells, with a resulting decrease in the root mean square (RMS) roughness by an order of magnitude, even better than for a low incidence FIB polished surface. Subsequently AFM-based property maps reveal a substantially stronger contrast, in this case of the short-circuit current or open circuit voltage during light exposure. Furthermore, electron back scattering diffraction (EBSD) imaging also becomes possible upon AFM-NM, enabling direct correlations between the local materials properties and the polycrystalline microstructure. Smooth shallow-angle cross-sections are demonstrated as well, based on targeted oblique milling. As expected, this reveals a gradual decrease in the average short-circuit current and maximum power as the underlying CdS and electrode layers are approached, but a relatively consistent open-circuit voltage through the diminishing thickness of the CdTe absorber. AFM-based nanomilling is therefore a powerful tool for material characterization, uniquely providing ion-damage free, selective area, planar smoothing or low-angle sectioning of specimens while preserving their functionality. This then enables novel, co-located advanced AFM measurements, EBSD analysis, and investigations by related techniques that are otherwise hindered by surface morphology or surface damage.

33 ADVANCED PROPULSION SYSTEMS↗

DOE OSTI2018

Origin of dielectric relaxor behavior in PVDF-based copolymer and terpolymer films

Relaxor ferroelectrics exhibit frequency-dispersion of their dielectric permittivity peak as a function of temperature, the origin of which has been widely debated. Microscopic understanding of such behavior for polymeric ferroelectrics has presented new challenges since unlike traditional ceramic ferroelectrics, dielectric relaxation in polymers is a consequence of short-range molecular dynamics that are difficult to measure directly. Here, through careful analysis of atomic-level H-atom dynamics as determined by Quasi-elastic Neutron Scattering (QENS), we show that short-range molecular dynamics within crystalline domains cannot explain the macroscopic frequency-dispersion of dielectric properties observed in prototypical polyvinylidene-fluoride (PVDF)-based relaxor ferroelectrics. Instead, from multiscale quantitative microstructural characterization, a clear correlation between the amount of crystalline-amorphous interfaces and dielectric relaxation is observed, which indicates that such interfaces play a central role. These results provide critical insights into the role of atomic and microscopic structures towards relaxor behavior in ferroelectric polymers, which will be important for their future design.

42 ENGINEERING↗

DOE OSTI2021

A pathway to desired functionalities in vertically aligned nanocomposites and related architectures

Epitaxial vertically aligned nanocomposites (VANs) and their related architectures have shown many intriguing features that are not available from conventional two-dimensional planar multilayers and heterostructures. The ability to control constituent, interface, microstructure, strain, and defects based on VANs has enabled the multiple degrees of freedom to manipulate the optical, magnetic, electrochemical, electronic, ionic, and superconducting properties for specific applications. This field has rapidly expanded from the interest in oxide:oxide to oxide:metal, metal:nitride and nitride:nitride systems. To achieve unparalleled properties of the materials, three-dimensional super-nanocomposites based on a hybrid of VAN and multilayer architectures have been recently explored as well. The challenges and opportunities of VAN films are also discussed in this article.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Microstructural characterization of SiO2/Ni nanocomposites electrodeposited from a sulphate bath modified by PEI

Highlights: • SiO{sub 2}/Ni + PEI nanocomposites are deposited from the sulphate bath containing PEI. • PEI allows incorporation of higher SiO{sub 2} vol% in SiO{sub 2}/Ni + PEI nanocomposites. • PEI in the form of a thin layer surrounds spherical Ni nanograins and SiO{sub 2} clusters. • PEI action ensures high hardness, tribological properties and corrosion resistance. - Abstract: SiO{sub 2}/Ni nanocomposite coatings containing well-dispersed SiO{sub 2} nanoparticles were electrodeposited from a sulphate bath with and without the addition of polyethylenimine (PEI) as a cationic surfactant. The surface morphology and microstructure in the cross-sections of the deposited nanocomposites were examined by scanning electron microscopy. More detailed microstructure characterization was performed using transmission, scanning-transmission and high resolution transmission electron microscopy. It was determined that the addition of 0.05 g/L and 0.1 g/L of PEI allows the incorporation of SiO{sub 2} nanoparticles in the nickel matrix to be increased in comparison with the nanocomposite deposited without a surfactant. Based on high spatial resolution microanalysis, performed using high count rate energy dispersive spectroscopy of characteristic X-rays in the scanning-transmission mode, the distribution of SiO{sub 2} nanoparticles in the nanocomposite was visualized on elemental maps. Image analysis of the electron microscopy images enabled the mean equivalent circle diameters of grains in the nickel matrix to be determined, together with the volume fraction of SiO{sub 2} nanoparticles in the nanocomposites. The volume fraction of SiO{sub 2} clusters in the SiO{sub 2}/Ni + PEI nanocomposites with the addition of 0.05 g/L and 0.1 g/L of PEI is equal to 18.4% and 13.3%, respectively. Furthermore, the PEI addition allows the nickel grain size in the matrix to be reduced. The combination of different imaging techniques confirmed that PEI is not only present as a surfactant in the electrolytic bath, but also incorporates into the microstructure of the nanocomposite. Nanocomposites electrodeposited in the presence of 0.05 g/L of PEI exhibit higher hardness, good tribological properties and improved corrosion resistance. Although increasing the PEI concentration in the bath up to 0.1 g/L strongly promotes grain size reduction and increase of the SiO{sub 2} volume fraction, it also causes an increase in the PEI fraction embedded in the microstructure, which results in deterioration of the properties of the SiO{sub 2}/Ni + PEI nanocomposites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2016

Orientation dependence of indentation behavior in Al–SiC nanolaminate composites

Al and SiC nanolaminate films were characterized in the perpendicular, inclined and parallel orientations using nanoindentation. The deformation was dominated by buckling of the layers when the layers were parallel to the indenter and by compression of the ductile Al layers when the layers were perpendicular to the indenter, while indentation in inclined orientations showed an intermediate behavior. Finite element modeling (FEM) of indentation deformation using wavy layers showed much more compliant behavior and prominent layer buckling than the idealized flat structure, highlighting the large effect these microstructural details can have on the deformation behavior.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Pitting behavior of friction stir repair-welded 304L stainless steel in 3.5% NaCl solution at room temperature: role of grain and defect structures

Stainless steel (SS) canisters used for storing spent nuclear waste are prone to chloride-induced stress corrosion cracking. Friction stir welding (FSW), being a low heat input process, can be used for repair welding of these canisters. In this study, an artificial crack was introduced on the 304L SS coupons by an electric discharge machining process. The artificial crack was repair-welded by FSW by maintaining the tool temperature a constant at two levels (725 and 825 °C). Friction stirring significantly reduced the grain size of the stirred zone (SZ) from about 47 to 2–4 μm. The fraction of low-angle grain boundaries increased in the SZ from 2 to 37–43%. Here, on the other hand, the fraction of special grain boundaries (Σ3 and Σ9) that was ~ 50% in the base metal reduced to < 10% in the SZ. During friction stirring, the oxide layer of artificial crack was broken and aligned to form a spiral defect called lazy-S structure. All these microstructural changes affected the corrosion behavior of the FSW specimens when tested in 3.5% NaCl at room temperature using cyclic polarization, chronoamperometry, and electrochemical impedance spectroscopy. The FSW specimens showed lower polarization resistance and lower transpassive potential than those of the base metal specimens. However, the pitting protection potentials of the FSW specimens were higher than that of the base metal. The pitting behavior of the FSW specimens was influenced more by the preferential attack on the lazy-S region than by passive film breakdown. The flat band potentials of the passive film formed on the FSW specimens were more positive than that of base metal. The charge carrier density of passive film formed on the FSW specimens was higher than that of the base metal. The higher fraction of low-angle grain boundaries present in the FSW specimens could supply more number of misorientation dislocations at the metal/film interface which could form anion vacancies by a climb process leading to formation of oxide at these locations without stressing the substrate. Therefore, low-angle boundaries are considered helpful for formation of stress-free passive films that will be highly stable and enhance both pitting and stress corrosion cracking resistance.

Dry storage canister↗

DOE OSTI2023

Microstructure and corrosion of CrFeMnV multi-principal element alloy

In this study, a multi-principal element alloy consisting of equiatomic concentrations of Cr, Fe, Mn, and V was produced by arc melting. The combination of X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy indicated that the CrFeMnV MPEA was comprised of a BCC matrix with a dispersion of a secondary phase. Cyclic potentiodynamic polarization tests in 0.6M NaCl revealed high corrosion resistance – superior to that of stainless steel 304L, as evident from high breakdown and repassivation potentials. X-ray photoelectron spectroscopy and time-of-flight secondary ion mass spectrometry provided insight into the formed multi-layer surface film after constant immersion and potentiostatic conditioning.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Three-dimensional structure investigation of Waterborne Paint by Electron Microscopic Imaging

In this paper, the three-dimensional (3D) spatial structure of a TiO 2 coated waterborne paint film has been successfully investigated by serial block-face scanning electron microscopy (SBFSEM). The investigation clearly shows the spatial distribution of the TiO2 particles in the paint film and illustrates the degree of dispersion of the particles in the composite material. More than 58% of the volume of the TiO 2 particles are between 1.0 × 10 6 nm 3 to 1.0 × 10 7 nm 3 and the minimum distance between different particles can be detected is 124 nm. Different types of voids can be found in the 3D image of the cured water-borne paint film: voids that exist in the paint itself, voids produced by particle shedding, water evaporating and particles stacking. Among these voids, the ones produced by particle shedding is a cutting artefact. The research provides a different approach to clearly present the 3D spatial structure of paints and can clearly illustrate different kinds of voids inside the water-borne paint. While the resulting 3D structure of the paint, especially the different voids are important for further systematic research on the relationships between the spatial microstructure and the physical and chemical properties of the water-borne paint.

36 MATERIALS SCIENCE↗

DOE OSTI2022

High Seebeck Coefficient from Screen-Printed Colloidal PbSe Nanocrystals Thin Film

Thin-film thermoelectrics (TEs) with a thickness of a few microns present an attractive opportunity to power the internet of things (IoT). Here, we propose screen printing as an industry-relevant technology to fabricate TE thin films from colloidal PbSe quantum dots (QDs). Monodisperse 13 nm-sized PbSe QDs with spherical morphology were synthesized through a straightforward heating-up method. The cubic-phase PbSe QDs with homogeneous chemical composition allowed the formulation of a novel ink to fabricate 2 μm-thick thin films through robust screen printing followed by rapid annealing. A maximum Seebeck coefficient of 561 μV K -1 was obtained at 143 °C and the highest electrical conductivity of 123 S m -1 was reached at 197 °C. Power factor calculations resulted in a maximum value of 2.47 × 10 -5 W m -1 K -2 at 143 °C. To the best of our knowledge, the observed Seebeck coefficient value is the highest reported for TE thin films fabricated by screen printing. Thus, this study highlights that increased Seebeck coefficients can be obtained by using QD building blocks owing to quantum confinement.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Enhanced van der Waals epitaxy of germanium by out-of-plane dipole moment induced from transferred graphene on TiN/AlN multilayers

We report recent advances in 3D/2D heterostructures have opened up tremendous opportunities in building highly flexible and durable optoelectronic devices. However, the inherit lack of interfacial bonding and low surface energy of van der Waals surfaces limit the nucleation and growth of 3D materials. Enhancing wettability by providing a porous buffer is effective in growing compound semiconductors on graphene while van der Waals epitaxy of Ge remains challenging. Here, the nucleation of Ge has been significantly improved from an islanded mode to granular modes by using a TiN/AlN multilayered buffer prior to Ge/graphene integration. Highly textured Ge growth with dominating (111), (220), and (311) peaks are identified by x-ray diffraction. The microstructure of the buffer TiN/AlN demonstrates a polycrystalline quality with clean interfaces between each interlayer and the substrate. Kelvin probe force microscopy measurements along the lateral TiN/AlN interface identify a potential drop corresponding to the AlN phase. This contact potential difference between TiN and AlN is the key in generating the out-of-plane dipole moment that modifies the surface energy of the monolayer graphene, resulting in enhanced wettability of the Ge adatoms nucleated on top. Surface dipole induced nucleation of 3D semiconductor thin films on 2D materials via the proper design of buffer layer is fundamentally important to enhance the 3D/2D growth toward flexible optoelectronic applications.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Probing Fundamental Mechanisms of Plastic Deformation with High Energy X-rays (Final Progress Report)

Overall, substantial progress was made on developing BCDI techniques in the direction of imaging defects in multi-crystal samples. Section 2.1 describes a new method to reconstruct the 3D atomic displacement field within a grain from multiple coherently resolved diffraction peaks. The key development is the ability to recover a best fit to the grain shape at the same time as the internal displacement (strain) variation with no prior knowledge of the microstructure. This is complemented by the development of a method, Sec. 2.2, to separate out sets of Laue reflections that belong to a single grain (and thus be able to index its orientation) in the commonly encountered situation in which the beam illuminates several grains in a given location. This is essential for enabling collection of coherent diffraction data (at APS 34-ID-C) from neighboring grains. All experiments depend on the quality of samples used. Although good progress has been made with thin film samples, we are working with a broader range of geometries. A new sample design uses a high-Z metal (e.g., Pt) deposited in a sub-micron trench in a low-Z metal (e.g., Al) so that the grain size is prevented from exceeding the current limit for BCDI. We also report in section 3.1 on successfully applying NF-HEDM to a fine-grain Mg sample that would normally be considered out of scope for the method. This represents progress towards being able to map out polycrystalline samples in 3D before performing BCDI on individual grains. We further report in section 3.2 on preliminary NF-HEDM characterization of a sample of UO2 that has sub-micron grains; the data imply the capability of mapping fine-grain polycrystals at 1-ID-E, again for the purposes of BCDI in the bulk. Lastly, our plan is to load grains in polycrystalline samples by inducing thermal stress. We also report the experimental measurements of the Ti- 6Al-4V alloy obtained at the European Synchrotron Radiation Facility (ESRF), which had been indexed and mapped via HEDM at APS in section 9. As discussed below, however, technique development pre-occupied the team throughout the project which meant that we did not make any significant progress towards answering the original hypotheses as stated in the proposal. In summary, we assert that we have made good progress in methods and samples and future work taking advantage of this progress is likely to obtain and analyze BCDI data from multiple adjacent grains in 3D polycrystals. Obtaining such data depends on re-gaining access to the Advanced Photon Source, which is anticipated in late summer or the Fall. In all cases, work has involved close collaboration with faculty, staff, postdocs and students from Brigham Young University (BYU), the Los Alamos National Laboratory and APS beamlines 1-ID and 34-ID.

36 MATERIALS SCIENCE↗