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At least 1,063 records · Page 59
All sourcesNASA NTRSDOE OSTI
NASA NTRS2000

Phase Shift Interferometer and Growth Set Up to Step Pattern Formation During Growth From Solutions. Influence of the Oscillatory solution Flow on Stability

We have assembled an experimental setup based on Michelson interferometry with the growing crystal surface as one of the reflective surfaces. The crystallization part of the device allows optical monitoring of a face of a crystal growing at temperature stable within 0.05 C in a flow of solution of controlled direction and speed. The reference arm of the interferometer contains a liquid crystal element that allows controlled shifts of the phase of the interferograms. We employ an image-processing algorithm, which combines five images with a pi/2 phase difference between each pair of images. The images are transferred to a computer by a camera capable of capturing 60 frames per second. The device allows data collection on surface morphology and kinetics during the face layers growth over a relatively large area (approximately 4 sq. mm) in situ and in real time during growth. The estimated depth resolution of the phase shifting interferometry is approximately 50 Angstroms. The data will be analyzed in order to reveal and monitor step bunching during the growth process. The crystal chosen as a model for study in this work is KH2PO4 (KDP). This optically non-linear material is widely used in frequency doubling applications. There have been a number of studies of the kinetics of KDP crystallization that can serve as a benchmark for our investigations. However, so far, systematic quantitative characteristics of step interaction and bunching are missing. We intend to present our first quantitative results on the onset, initial stages and development of instabilities in moving step trains on vicinal crystal surfaces at varying supersaturation, flow rate, and flow direction. Behavior of a vicinal face growing from solution flowing normal to the steps and periodically changing its direction in time was considered theoretically. It was found that this oscillating flow reduces both stabilization and destabilization effects resulted from the unidirectional solution flow directed up the step stream and down the step stream. This reduction of stabilization and destabilization comes from effective mixing which entangles the phase shifts between the spatially periodic interface perturbation and the concentration wave induced by this perturbation. Numerical results and simplified mixing criterion will be discussed.

Chernov, Alex A.↗
NASA NTRS2001

Abiotic Versus Biotic Weathering Of Olivine As Possible Biosignatures

We are investigating the weathering of silicate minerals by both purely inorganic, and biologically mediated processes using field-emission scanning electron microscopy (FESEM) and energy dispersive x-ray spectroscopy (EDS). By resolving surface textures and chemical compositions of weathered surfaces at the sub-micron scale we hope to be able to distinguish abiotic from biotic weathering processes and so establish a new biosignature applicable to the study of astromaterials including but not limited to the Martian meteorites. Sterilized olivine grains (San Carlos, Arizona) no more than 1-2 mm in their longest dimension were optically assayed to be uniform in color and free of inclusions were selected as weathering subjects. Prior to all experiments surface morphologies and Fe/Mg ratios were determined for each grain using FE-SEM and EDS. Experiments were divided into two categories abiotic and biotic and were compared with "naturally" weathered samples. For the preliminary experiments, two trials (open and closed to the ambient laboratory environment) were performed under abiotic conditions, and three trials under biotic conditions (control, day 1 and day 2). The open system abiotic trials used sterile grains heated at 98 C and 200 C for both 24 and 48 hours in 1L double distilled de-ionized water. The closed system abiotic trials were conducted under the same conditions but in a sealed two layer steel/Teflon "bomb" apparatus. The biotic trials used sterile grains mounted in a flow-through device attached to a wellhead on the Columbia River aquifer. Several discolored, altered, grains were selected to document "natural" weathering surface textures for comparison with the experimental samples. Preliminary results indicate there are qualitative differences in weathered surface textures among all the designed experiments. The olivine grains in abiotic trials displayed etching, pitting, denticulate margins, dissolution and clay formation. The scale of the features ranged from tens to a few microns with textures that remained relatively sharp and were crystallographically controlled. These results were comparable to that observed in the "naturally" weathered comparison/reference grains. Chemical analysis by EDS indicates these textures correlated with the relative loss of Mg and Fe cations by diffusional processes. In contrast the biotic results indicated changes in the etching patterns on the scale of hundreds of nm, which are neither sharp nor crystallographically controlled (nanoetching). Organisms, organic debris and/or extracellular polymeric substances (biofilm) were often in close proximity or direct contact with the nanoetching. While there are many poorly constrained variables in natural weathering experiments to contend with, such as the time scale, the chemistry of the fluids and degree of biologic participation, some preliminary observations can be made: (1) certain distinct surface textures appear correlated with the specific processes giving rise to these textures; (2) the process of diffusing cations can produce many similar styles of surface textural changes; and (3) the main difference between abiotic and biotically produced weathering is the scale (microns versus nanometers) and the style (crystallographically versus noncrystallographically controlled) of the textural features. Further investigation into nanosize scale surface textures should attempt to quantify both textures and chemical changes of the role of microorganisms in the weathering of silicates. Additional experiments addressing nanoscale textures of shock features for comparison with the current data set.

Longazo, Teresa G.↗
DOE OSTI2017

Influence of MAO Treatment on the Galvanic Corrosion Between Aluminum Alloy and 316L Steel

To slow down the galvanic corrosion of aluminum alloy and 316L stainless steel in subsea water, a micro-arc oxidation (MAO) coating was prepared on the surface of the Al alloy, and no treatment was performed on the surface of the 316L. The surface morphology of MAO-coated Al alloy was evaluated using a scanning electron microscope (SEM) before and after corrosion. A micro-hardness tester was used to measure the micro-hardness. Corrosion behaviors were evaluated by open-circuit potential (OCP), potentiodynamic polarization (PDP) and electrode impedance spectroscopy (EIS) tests in a 3.5 g/L NaCl solution. The results of PDP testing show that the corrosion potential of the MAO-coated galvanic pair was more positive than that of the uncoated galvanic pair and that the corrosion current density was smaller than that of the uncoated galvanic pair. EIS results show that the impedance of the galvanic pair increased after MAO coating. SEM images show that the corrosion damage of the uncoated Al alloy was more severe than that of the MAO-coated one, and the post-corrosion images of the surface of the 316L connected with MAO-coated Al alloy were more compact than those of the 316L connected with uncoated Al alloy. A physical model was developed to discuss the influence of MAO treatment on the galvanic corrosion process and corrosion mechanism.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Improvement of the thermal stability of nickel silicide using a ruthenium interlayer deposited via remote plasma atomic layer deposition

In this study, the effects of a thin Ru interlayer on the thermal and morphological stability of NiSi have been investigated. Ru and Ni thin films were deposited sequentially to form a Ni/Ru/Si bilayered structure, without breaking the vacuum, by remote plasma atomic layer deposition (RPALD) on a p-type Si wafer. After annealing at various temperatures, the thermal stabilities of the Ni/Ru/Si and Ni/Si structures were investigated by various analysis techniques. The results showed that the sheet resistance of the Ni/Ru/Si sample was consistently lower compared to the Ni/Si sample over the entire temperature range. Although both samples exhibited the formation of NiSi{sub 2} phases at an annealing temperature of 800 °C, as seen with glancing angle x-ray diffraction, the peaks of the Ni/Ru/Si sample were observed to have much weaker intensities than those obtained for the Ni/Si sample. Moreover, the NiSi film with a Ru interlayer exhibited a better interface and improved surface morphologies compared to the NiSi film without a Ru interlayer. These results show that the phase transformation of NiSi to NiSi{sub 2} was retarded and that the smooth NiSi/Si interface was retained due to the activation energy increment for NiSi{sub 2} nucleation that is caused by adding a Ru interlayer. Hence, it can be said that the Ru interlayer deposited by RPALD can be used to control the phase transformation and physical properties of nickel silicide phases.

36 MATERIALS SCIENCE↗
NASA NTRS1988

Constraints on Mars sampling based on models of basaltic flow surfaces and interiors

Recent field observation and numerical modelling of the pattern and origin of vesicle zones and joints in terrestrial basaltic flows has resulted in increased understanding of the processes which affect flow surface morphology. This work has documented the ubiquitous occurrence of three vertical zones in basalt flows: (1) an upper vesicular zone; (2) a middle vesicle-free zone; and (3) a lower vesicular zone. The upper vesicular zone is generally about one-half of the total flow thickness. Computer modeling of the development of these zones confirms that vesicle zonation is a result of the nucleation, growth and rise of bubbles in solidifying lava and can be expected to occur in all basaltic flows. Degradation of basaltic flows, therefore, will produce vesicular blocks until the erosional level reaches the central vesicle-free zone. In addition, observation of terrestrial basaltic flows has shown that most thin (less than 10 m thick) flows have a regular pattern of orthogonal joints in vertical section in which the spacing of joints increases with depth beneath the flow surface. Using these studies we have performed a preliminary analysis of the Viking lander sites.

Aubele, J. C.↗
DOE OSTI2015

Kinetics and Mechanisms of Calcite Reactions with Saline Waters

Project Description: The general objective of the proposed research is to determine the kinetics and mechanisms of calcite reactions with saline waters over a wide range of saline water composition, pCO 2 , and modest ranges in T and P. This will be accomplished by studying both reaction rates and solubility from changes in solution chemistry, and making nanoscale observations of calcite precipitate surface morphology and composition at the micro-to-nano-scale to provide an understanding of controlling reaction mechanisms and pathways. The specific objectives necessary to reach the general objective are: a) determination of how pCO 2 , Ca 2+ , ionic strength and “foreign” ions influence reaction rates; and b) investigate the influence of these parameters on apparent kinetic solubility from dissolution and precipitation reactions. This information will clearly be central to the construction of reliable reaction-transport models to predict reservoir and formation response to increased CO 2 in saline waters. This program was initially collaborative with John Morse at Texas A&M, however his passing shortly after the beginning of this program resulted in abbreviated research time and effort. Summary of Results: Early studies using electron microscopy and spectroscopy indicated that carbonate precipitation from natural seawater (NSW) conditions onto aragonite substrates was mediated by a surface amorphous calcium carbonate layer. It was hypothesized that this ACC layer (observed after < 5days reaction time) was responsible for the abnormal reaction kinetics and also served as a metastable seed layer for growth of epitaxial aragonite. Further studies of the ACC formation mechanism indicated a strong dependence on the Mg concentration in solution. Subsequent studies at shorter times (10 hrs) on calcite substrates and in a wide range of supersaturation conditions did not indicate any ACC layer. Instead, an epitaxial layer by layer growth mechanism was confirmed by grazing incidence X-ray diffraction, µ-Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and electron diffraction. Extended time studies out to 45 days confirmed the epitaxial relationship of the overgrowth layer with the substrate. Under NSW conditions, overgrowths were found to have ~0.4 to 0.8 nm / hr growth rates and accommodating 4 at% Mg, resulting in a highly strained overgrowth layer. Following the initial layer by layer growth mechanism, the growth changes to Stranski-Krastanov type after a critical thickness of approximately 100 nm.

58 GEOSCIENCES↗
DOE OSTI2014

Structural anisotropic properties of a-plane GaN epilayers grown on r-plane sapphire by molecular beam epitaxy

Heteroepitaxial non-polar III-Nitride layers may exhibit extensive anisotropy in the surface morphology and the epilayer microstructure along distinct in-plane directions. The structural anisotropy, evidenced by the “M”-shape dependence of the (112{sup ¯}0) x-ray rocking curve widths on the beam azimuth angle, was studied by combining transmission electron microscopy observations, Raman spectroscopy, high resolution x-ray diffraction, and atomic force microscopy in a-plane GaN epilayers grown on r-plane sapphire substrates by plasma-assisted molecular beam epitaxy (PAMBE). The structural anisotropic behavior was attributed quantitatively to the high dislocation densities, particularly the Frank-Shockley partial dislocations that delimit the I{sub 1} intrinsic basal stacking faults, and to the concomitant plastic strain relaxation. On the other hand, isotropic samples exhibited lower dislocation densities and a biaxial residual stress state. For PAMBE growth, the anisotropy was correlated to N-rich (or Ga-poor) conditions on the surface during growth, that result in formation of asymmetric a-plane GaN grains elongated along the c-axis. Such conditions enhance the anisotropy of gallium diffusion on the surface and reduce the GaN nucleation rate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Extreme sensitivity of magnetic properties on the synthesis routes in La{sub 0.7}Sr{sub 0.3}MnO{sub 3}

La{sub 0.7}Sr{sub 0.3}MnO{sub 3} polycrystalline samples have been prepared using different synthesis routes. X-ray Diffraction (XRD) confirms that the samples are of single phase with R-3c space group. The surface morphology and particle size has been observed using Field Emission Scanning Electron Microscopy (FESEM). Magnetic measurement shows that the magnetization in the materials are affected by low crystallite size which destroys the spin ordering due to strain at grain boundaries and this also leads to reduction in magnetization as well as high coercivity in the material.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Superabsorbent hydrogel composite based on copolymer cellulose/poly (vinyl alcohol)/CNT

Superabsorbent hydrogels are cross-linked hydrophilic polymers that can absorb and retain a large volume of water, saline solution, or physiological fluids. A distinctive superabsorbent hydrogel composite based on cellulose/ poly (vinyl alcohol)/ carbon nanotubes was successfully synthesized via the graft bio-copolymerization in an aqueous medium with glutaraldehide as a crosslinking agent. The effect of carbon nanotubes (CNT) on water absorption capacity and mechanical properties of superabsorbent composite were particularly investigated. The Fourier transform infrared spectra showed the evidence of copolymerization of hydrogel precursors as well as the interaction of CNT filler with the hydrogel matrices, as indicated by the shifting of peak intensity and position of several functional groups (O-H, C-H sp{sup 3}, C=O, C-N, C-O). The modification of hydrogel surface morphology and porosity owing to CNT insertion was also confirmed by scanning electron microscopy images. The CNT insertion improved the mechanical strength of superabsorbent hydrogel composites. Moreover, insertion of CNT into hydrogel matrix remarkably increased the swelling capacity of superabsorbent composites up to 840%. This huge water absorption capacity of hydrogel composites offers promising applications in development of superabsorbent polymers.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Thermoluminescence property of nano scale Al{sub 2}O{sub 3}: C by combustion method

In this study, thermoluminescence dosimetry material of carbon doped aluminium oxide by combustion method using Aluminium nitrate and Glycine. The Structure of the prepared Sample was carried out by XRD. The sample was nano crystalline in nature. Having hexagonal structure with unit cell parameters a=4.75Å, C=12.99Å. The surface morphology of the prepared nanopowder was carried out through (SEM). The morphology of the prepared sample is platelet structure and functional group analysis carried out through FT-IR Spectrum. The prepared sample was irradiated through γ-ray CO{sup 60} (100 Gy) was used as γ-ray source. The thermoluminescence glow curve of the irradiated sample showed an isolated peak at around 200°C. The result suggest the prepared nanopowder is suitable for medical radiation dosimetry.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2023

Laboratory-Scale Coal-Derived Graphene Process (Final Report)

The Energy & Environmental Research Center (EERC) conducted a laboratory-scale coal-derived graphene (CDG) project focused on developing a technological process for making graphene from four U.S. domestic coal or coal wastes, including lignite from North Dakota, subbituminous coal from Wyoming, bituminous coal from Utah, and anthracite from Pennsylvania. The project was divided into two performance or budget periods (BPs), with BP1 comprising the up-front laboratory experiments to make graphene materials from coal beginning on May 1, 2020, to April 30, 2022. BP2 was conducted from May 1, 2022, to April 30, 2023, and was focused on analyzing the CDG process economic feasibility and the technical gaps for technological scale-up and commercialization. During this project, a few different coal-derived high-value products have been demonstrated, including graphite, graphene oxide (GO), reduced graphene oxide (rGO), and graphene quantum dots (GQDs). A new graphite microstructure was discovered and named “croissant graphite” because of the exterior morphological and textural resemblance to croissant food items sold in commercial groceries stores. The new graphite structure and the associated preparation from coal or coal waste feedstocks has been the subject of a U.S. patent application. The systematic experimental processes involving coal cleaning, upgrading, and conversion to high-value carbon products culminated into a developed upgraded coal-to-products (UCP) technology that is being pursued for potential fast-track commercialization, if funding is available. It is envisioned that commercialization of the UCP technology would increase consumption of U.S. domestic coals or coal wastes to make environmentally sustainable high-value products for the electronics industry, high-energy-storage applications, and clean energy technologies such as electric vehicle (EV) lithium-ion batteries (LIBs), for which graphite has become a critical mineral commodity. Croissant graphite microstructures, when observed by field emission scanning electron microscopy (FESEM), display wavy surface morphology and often grow from a base that is made of graphitized particles with honeycomb-like layers, which are believed to be graphene layers. While more studies are needed to fully ascertain the mechanisms of the croissant graphite microstructure formation, it is postulated that their growth may begin from curling of the graphene sheets into ribbon-like structures, and continuous growth and densification of the ribbon-like structures forms croissant microstructures. Additional studies are ongoing to evaluate the electrochemical performance of croissant graphite for LIB applications and to determine the experimental conditions necessary to tune on/off croissant formation so that it can be either optimized or suppressed depending on performance evaluation results. In addition to the discovery of croissant graphite, the graphitization process from the four coal ranks in general was successful. X-ray diffraction (XRD) analysis showed that the degree of graphitization (DoG) ranged from 12% to 80% in an early sample set, and further optimization on lignite coal produces a DoG of about 92%, which was spectacular to see as lignite is the lowest-rank coal. Thus, it is expected that the graphitization performance for higher-rank coals will be similar or better when optimized as well. The coal-derived graphite was used to make GO and rGO. Analytical characterization, e.g., by methods such as Raman spectroscopy, XRD, Fourier transform infrared (FTIR) spectroscopy and FESEM, showed that the sequence of converting the coal to graphite, exfoliating it to GO, and then chemically reducing the GO to rGO was successful. Although coal naturally contains aromatic compounds and some relatively small-sized condensed aromatic units, it does not contain graphene sheets. In the UCP process, the aromatic domains in the coals, particularly low-rank coals, are concentrated and condensed further into graphene sheets, which are ordered into a 3D stack during graphitization. The synthesized graphite is then unpacked by methods such as exfoliation to various graphene products. GQDs were synthesized from all four coal types, and their optical properties were demonstrated to be tunable by the coal precursor preprocessing treatments. In all four coal types, enhanced optical properties were observed for the produced GDQs with incremental improvements made to the coal precursors. GQDs produced from raw coal samples displayed lower ultraviolet–visible (UV–Vis) spectroscopy absorbance intensity compared to those obtained from cleaned and upgraded coal residues. The photoluminescence (PL) intensities also varied with pretreatment conditions and with the concentration of GQDs in aqueous solutions. GQDs obtained from anthracite show longer emission wavelengths and can be excited by visible light as opposed to GQDs derived from the other coal ranks. UV fluorescence 3D maps and spectra revealed that the emission wavelength at which the GQDs solutions display the highest intensity was slightly redshifted based on the coal precursor pretreatments. In low-rank coal (lignite and subbituminous) samples, two clusters were observed in the maps for GQDs, which may suggest that there are potentially two types of fluorophores in solution or two main size populations. The ability to tune the properties of GQDs based on processing methods can be exploited to make GQDs for various optical display or optoelectronics applications. The results also highlight the importance of removing coal-borne impurities to improve the quality of the coal precursor for preparation of graphene products. Coal and/or coal wastes preprocessing methods were developed and applied to clean and upgrade the coal precursors prior to graphitization and subsequent conversion to graphene products. The preprocessing methods involve high specific-gravity separations, mineral acid cleaning (no hydrofluoric acid), and subsequent upgrading by reducing the coal-borne heteroatom (nitrogen, sulfur, and oxygen) content using proprietary chemical agents. Analytical characterization revealed that the preprocessing steps were successful, with ash reductions that range from 38% to 80% and residual ash content that was below the 5 wt% initial target. Based on proximate and ultimate analysis, the heteroatom reduction reactions produced upgraded coal residues with the oxygen content reduced by 8% to 24%, with additional reductions in the nitrogen and sulfur contents. An initial assessment of the waste streams from the UCP process shows very small to negligible environmental impact due to CO 2 , NO x , and SO x because most process steps are performed under inert atmosphere with argon. Consequently, reactive oxygen environments that tend to create these species are avoided. The inorganic and potentially hazardous species are released into aqueous waste streams that are easy to handle for proper disposal. The liquid waste streams were found to contain low-level concentrations of rare-earth elements (REEs), which could be concentrated and recovered as value-added by-products. Additionally, the volatile and gaseous fractions from carbonization and heat treatment contain useful organic compounds that can also be recovered as potential valuable by-products. Thus, the UCP technology is considered an environmentally sustainable and promising emerging technology for making high-value products from coal and coal wastes, with potential additional value-added by-products. Analysis of potential markets for the coal-derived carbon products shows a strong demand in both niche market sectors and across a wide variety of other industrial sectors. Graphite is currently considered a critical mineral commodity that has a large and growing demand in the LIB industry for EV applications. Based on data from Fortune Business Insights (2022) and Marketwatch (2023) reports, the average global graphite market is projected to reach about 33 billion by 2028, growing at a compound annual growth rate (CAGR) of about 7%, with much of this growth expected to be in the LIB industry. GO and rGO have strong market potentials in various application areas, such as coatings for anticorrosion, anti-icing, and antimicrobial protection, thermal barriers, wear resistance, sensors, additive manufacturing such as 3D inks, and others. GQDs are the emerging key player in the bioimaging, photovoltaics, and light-emitting diodes (LEDs) applications, with the potential to replace traditional semiconductor quantum dots (SQDs), which are based on metallic systems that are more toxic and more expensive. Biomedical applications of GQDs are becoming more attractive because of low to no toxicity and extremely low cost compared to SQDs. The major challenges for scale-up and commercialization of coal-derived carbon products such as graphene vary from the inherent attributes of graphene itself to reluctance to accept graphene in new manufacturing processes because of the uncertainty of the unknown. The 2D nature of graphene materials with a thickness of one atom presents significant challenges to proper handling/processing, and process scale-up becomes difficult because it requires high-end, expensive equipment, even for routine handling and analysis for quality assurance and control. Pristine graphene can also be extremely difficult to work into other matrices, thus hindering downstream processibility, especially at large scale. Currently, the cost of graphene and graphene products is still high and presents an economic risk that tends to slow down investment in scaling up emerging technologies. The lack of a standard for graphene materials for quality assurance and quality control poses a great challenge not only for the markets but also for commercialization efforts. A first-look economic feasibility analysis of the UCP technology provided valuable information that suggests the UCP process would be feasible, especially when it is scaled to a pilot scale and could be more competitive at the full scale. Graphitization was found to be the most energy-consuming and most capital-intensive step in the overall process. In small laboratory- and bench-scale experiments, labor is a significant contributor to the total process costs. Although these energy, capital, and labor constraints contribute to a higher selling price for the product, a preliminary economic model suggests that the process would be feasible at large scale when the process is fully integrated, optimized, and automated.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2025

Additively manufactured and cast high-temperature aluminum alloys for electric vehicle brake rotor application

Electric vehicle brake rotors demand lightweight, high thermal conductivity materials with good resistance to wear, creep, salt corrosion, and thermal fade, all of which present challenges to the traditionally used cast iron. In this work, we investigated the braking performance of recently developed high-temperature aluminum alloys in both cast and 3D printed forms, that possess excellent microstructural and mechanical stability at elevated temperatures. Three aluminum alloys, Al-6Cu-Mn-Zr, Al-9Cu-Mn-Zr, and Al-Ce-Ni-Mn-Zr and a reference cast iron were tested on a sub-scale brake tester against a commercial brake pad material over a range of sliding speeds between 2 and 15 m/s. The performance of these alloys was evaluated for wear resistance, friction behavior, temperature elevation, and surface morphological change. Although all three candidate alloys had lower wear-resistance than cast iron, Al-Ce-Ni-Mn-Zr showed a significantly reduced wear rate in comparison to the Al-Cu-Mn-Zr alloys. Moreover, Al-Ce-Ni-Mn-Zr alloy had the most consistent friction behavior at all sliding speeds and good fade resistance, as the coefficient of friction did not dramatically decrease with temperature rise but stayed within a desirable range of 0.35–0.50 instead. The superior wear resistance and braking performance of the Al-Ce-Ni-Mn-Zr alloy were attributed to its higher hardness, and high temperature yield strength and creep resistance compared with the Al-Cu-Mn-Zr alloys. In conclusion, the results suggest that the braking performance of these aluminum alloys could be further enhanced by increasing the hardness and forming a more stable transfer layer on the sliding surface.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Fabrication of ZnO nanorod using spray-pyrolysis and chemical bath deposition method

ZnO thin films with nanorod structure were deposited using Ultrasonic Spray Pyrolysis method for seed growth, and Chemical Bath Deposition (CBD) for nanorod growth. High purity Zn-hydrate and Urea are used to control Ph were dissolved in ethanol and aqua bidest in Ultrasonic Spray Pyrolysis process. Glass substrate was placed above the heater plate of reaction chamber, and subsequently sprayed with the range duration of 5, 10 and 20 minutes at the temperatures of 3500 C. As for the Chemical Bath Deposition, the glass substrate with ZnO seed on the surface was immerse to Zn-hydrate, HMTA (Hexa Methylene Tetra Amine) and deionized water solution for duration of 3, 5 and 7 hour and temperatures of 600 C, washed in distilled water, dried, and annealed at 3500 C for an hour. The characterization of samples was carried out to reveal the surface morphology using Scanning Electron Microscopy (SEM). From the data, the combination of 5 minutes of Ultrasonic Spray Pyrolysis process and 3 hour of CBD has showed the best structure of nanorod. Meanwhile the longer Spraying process and CBD yield the bigger nanorod structure that have been made, and it makes the films more dense which make the nanorod collide each other and as a result produce unsymetric nanorod structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Characteristics of TiO{sub 2}/ZnO bilayer film towards pH sensitivity prepared by different spin coating deposition process

In this study, titanium dioxide (TiO{sub 2}) and zinc oxide (ZnO) bilayer film for pH sensing application will be presented. TiO{sub 2}/ZnO bilayer film with different speed of spin-coating process was deposited on Indium Tin Oxide (ITO), prepared by sol-gel method. This fabricated bilayer film was used as sensing membrane for Extended Gate Field-Effect Transistor (EGFET) for pH sensing application. Experimental results indicated that the sensor is able to detect the sensitivity towards pH buffer solution. In order to obtained the result, sensitivity measurement was done by using the EGFET setup equipment with constant-current (100 µA) and constant-voltage (0.3 V) biasing interfacing circuit. TiO{sub 2}/ZnO bilayer film which the working electrode, act as the pH-sensitive membrane was connected to a commercial metal-oxide semiconductor FET (MOSFET). This MOSFET then was connected to the interfacing circuit. The sensitivity of the TiO2 thin film towards pH buffer solution was measured by dipping the sensing membrane in pH4, pH7 and pH10 buffer solution. These thin films were characterized by using Field Emission Scanning Electron Microscope (FESEM) to obtain the surface morphology of the composite bilayer films. In addition, I-V measurement was done in order to determine the electrical properties of the bilayer films. According to the result obtained in this experiment, bilayer film that spin at 4000 rpm, gave highest sensitivity which is 52.1 mV/pH. Relating the I-V characteristic of the thin films and sensitivity, the sensing membrane with higher conductivity gave better sensitivity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

Atmospheric-pressure plasma-enhanced chemical vapor deposition of a-SiCN:H films: Role of precursors on the film growth and properties

Atmospheric pressure plasma enhanced chemical vapor deposition (AP-PECVD) using Surfx Atomflow TM 250D APPJ was utilized to synthesize amorphous silicon carbonitride coatings using tetramethyldisilizane (TMDZ) and hexamethyldisilizane (HMDZ) as the single source precursors. The effect of precursor chemistry and the substrate temperature (T s ) on the properties of a-SiCN:H films were evaluated, while nitrogen was used as the reactive gas. Surface morphology of the films was evaluated using atomic force microscopy (AFM); chemical properties were determined using Fourier transform infrared spectroscopy (FTIR); thickness and optical properties were determined using spectroscopic ellipsometry and mechanical properties were determined using nano-indentation. In general films deposited at substrate temperature (T s ) <200 °C contained organic moieties, while the films deposited at T s >200 oC depicted strong Si-N and Si-CN absorption. Refractive indices (n) of the thin films showed values between 1.5 -2.0 depending on the deposition parameters. Mechanical properties of the films determined using nano-indentation revealed that these films have hardness between 0.5 GPa to 15 GPa depending on the Ts. AFM evaluation of the films showed high roughness (R a ) values of 2-3 nm for the films grown at low T s (< 250 °C), while the films grown at T s ≥ 300 °C exhibited atomically smooth surface with R a of ~ 0.5 nm. Furthermore, based on the gas phase (plasma) chemistry, precursor chemistry and the other experimental observations, a possible growth model that prevails in the AP-PECVD of a-SiCN:H thin films is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Protecting the properties of monolayer MoS 2 on silicon based substrates with an atomically thin buffer

Semiconducting 2D materials, like transition metal dichalcogenides (TMDs), have gained much attention for their potential in opto-electronic devices, valleytronic schemes, and semi-conducting to metallic phase engineering. However, like graphene and other atomically thin materials, they lose key properties when placed on a substrate like silicon, including quenching of photoluminescence, distorted crystalline structure, and rough surface morphology. The ability to protect these properties of monolayer TMDs, such as molybdenum disulfide (MoS 2 ), on standard Si-based substrates, will enable their use in opto-electronic devices and scientific investigations. Here we show that an atomically thin buffer layer of hexagonal-boron nitride (hBN) protects the range of key opto-electronic, structural, and morphological properties of monolayer MoS 2 on Si-based substrates. The hBN buffer restores sharp diffraction patterns, improves monolayer flatness by nearly two-orders of magnitude, and causes over an order of magnitude enhancement in photoluminescence, compared to bare Si and SiO 2 substrates. Lastly, our demonstration provides a way of integrating MoS 2 and other 2D monolayers onto standard Si-substrates, thus furthering their technological applications and scientific investigations.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Investigation of the effect of low energy ion beam irradiation on mono-layer graphene

In this paper, the effect of low energy irradiation on mono-layer graphene was studied. Mono-layer graphene films were irradiated with B, N and F ions at different energy and fluence. X-ray photoelectron spectroscopy indicates that foreign ions implanted at ion energies below 35 eV could dope into the graphene lattice and form new chemical bonds with carbon atoms. The results of Raman measurement indicate that ion beam irradiation causes defects and disorder to the graphene crystal structure, and the level of defects increases with increasing of ion energy and fluence. Surface morphology images also prove that ion beam irradiation creates damages to graphene film. The experiment results suggest that low-energy irradiation with energies of about 30 eV and fluences up to 5·10{sup 14} cm{sup −2} could realize small amount of doping, while introducing weak damage to graphene. Low energy ion beam irradiation, provides a promising approach for controlled doping of graphene.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Characterization of diamond-like nanocomposite thin films grown by plasma enhanced chemical vapor deposition

Diamond-like nanocomposite (DLN) thin films, comprising the networks of a-C:H and a-Si:O were deposited on pyrex glass or silicon substrate using gas precursors (e.g., hexamethyldisilane, hexamethyldisiloxane, hexamethyldisilazane, or their different combinations) mixed with argon gas, by plasma enhanced chemical vapor deposition technique. Surface morphology of DLN films was analyzed by atomic force microscopy. High-resolution transmission electron microscopic result shows that the films contain nanoparticles within the amorphous structure. Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and x-ray photoelectron spectroscopy (XPS) were used to determine the structural change within the DLN films. The hardness and friction coefficient of the films were measured by nanoindentation and scratch test techniques, respectively. FTIR and XPS studies show the presence of C-C, C-H, Si-C, and Si-H bonds in the a-C:H and a-Si:O networks. Using Raman spectroscopy, we also found that the hardness of the DLN films varies with the intensity ratio I{sub D}/I{sub G}. Finally, we observed that the DLN films has a better performance compared to DLC, when it comes to properties like high hardness, high modulus of elasticity, low surface roughness and low friction coefficient. These characteristics are the critical components in microelectromechanical systems (MEMS) and emerging nanoelectromechanical systems (NEMS).

36 MATERIALS SCIENCE↗