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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Experimental investigation into coal wettability changes caused by reactions with scCO 2 -H 2 O

Geological CO 2 sequestration (GCS) can help mitigate global warming and enhance methane recovery from coal beds. However, few studies have linked the effects of CO 2 to surface chemistry changes controlling wetting behavior in deep coal beds. Contact angles (CAs) of CO 2 /N 2 -high volatile bituminous coal-water systems were measured under different temperatures and pressures. The surface chemistry and physical structure of coals were characterized to investigate changes in physicochemical properties and their relations with wettability after reactions. For N 2 treatment, the time-dependence of static and dynamic CAs were insignificant, ranging within 4°. For gaseous CO 2 treatment, the static CAs and the average advancing angles increased slightly. With supercritical (sc) CO 2 , both the static and dynamic CAs increased significantly, and θ adv changed to intermediate-wet (92°). Reactions with minerals exposed to scCO 2 resulted in greater surface roughness and heterogeneity, greater contact angle hysteresis and more surface sites occupied by scCO 2 rather than H 2 O. Increases in hydrophobic functional groups and decreases in hydrophilicity were shown by FTIR spectra, reflecting the shedding of polar oxygen-containing functional groups, reduction of hydrogen bonds, and increasing percentage of hydrocarbons. XRD patterns obtained following scCO 2 -treatment showed that crystallite growth and molecular polymerization were higher toward graphite-like. The calculated structural parameters of functional groups and crystallites both showed elevated coal rank. Changes in crystallite structure, notably higher carbon content and decreased negative surface charge, are unfavorable for water-wetting. Finally, this study contributes to understanding surface chemistry changes responsible for decreased wettability during CO 2 -enhanced coal bed methane recovery and GCS in coal reservoirs.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2026

Characterization of runaway electron impact on instrumented sacrificial limiters on DIII-D

Instrumented sacrificial limiter heads, both domed (proud) and flat (flush) are used in DIII-D runaway electron (RE) wall strikes to study the wall impact dynamics with high spatial and time resolution. The approximate structure of the RE wetted area and heating depth on the domed limiter heads were predicted qualitatively using orbit-tracking simulations, although a strong left–right asymmetry (about the magnetic field direction) was not captured well by the simulations. It is hypothesized that this difference is perhaps due to the local 3D magnetic field perturbation of the dome limiter head. The average kinetic energy K and pitch angle θ of REs striking the limiter head were estimated from the spatial distribution of local HXR emission and were estimated to be roughly K ≈ 4 MeV and θ ≈ 0.2 rad. These values are roughly consistent with in-plasma values estimated before the loss event, indicating that RE kinetic energy and pitch angle are not drastically altered when transporting to the wall. Large shot–shot variations (1–10 kJ) in energy deposition into the limiter head were observed and were explained by shot–shot variations in locked magneto-hydrodynamics mode toroidal phase. For the largest deposited energies (10 kJ), graphite material failure and explosive dust release was observed, and the depth of material failure at higher energy deposition was successfully reproduced using modelling of volumetric energy deposition and brittle failure. The presence of energetic (keV) level ion impact during the RE wall strike was confirmed by three different surface analysis techniques. The ratio of energetic ion to RE flux appears to be larger on flat surfaces within the RE wetted area, although the energetic ion flux and total energy flux due to energetic ions have not yet been quantified.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2013

Scaling Analysis for the Direct Reactor Auxillary Cooling System For AHTRS

The Direct Reactor Auxiliary Cooling System (DRACS) is a passive heat removal system proposed for the Advanced High-Temperature Reactor (AHTR) that combines the coated particle fuel and graphite moderator with a liquid fluoride salt as the coolant. The DRACS features three coupled natural circulation/convection loops relying completely on buoyancy as the driving force. In the DRACS, two heat exchangers, namely, the DRACS Heat Exchanger (DHX) and the Natural Draft Heat Exchanger (NDHX) are used to couple these loops. In addition, a fluidic diode is employed to minimize the parasitic flow during normal operation of the reactor and to activate the DRACS in accidents. While the DRACS concept has been proposed, there are no actual prototypic DRACS systems for AHTRs built and tested in the literature. In this paper, a detailed scaling analysis for the DRACS is performed, which will provide guidance for the design of the scaled-down DRACS test facilities. Based on the Boussinesq assumption and one-dimensional flow formulation, the governing equations are non-dimensionalized by introducing appropriate dimensionless parameters. The key dimensionless numbers that characterize the DRACS system are obtained straightforwardly from the non-dimensional governing equations. Based on the dimensionless numbers and non-dimensional governing equations, similarity laws are proposed. In addition, a scaling methodology has also been developed, which consists of the core scaling and loop scaling. The consistence between the core and loop scaling is examined through the reference volume ratio, which can be obtained from the core and loop scaling processes. The scaling methodology and similarity laws have been applied to obtain a design of the scaled-down high-temperature DRACS test facility (HTDF).

Scaling auxiliary AHTRS DRACS liquid salt molten r↗
DOE OSTI2018

Multiscale characterization of irradiation behaviour of ion-irradiated SiC/SiC composites

Here, the irradiation tolerance of SiC/SiC composites was studied using 10 MeV Au ion irradiations at 350 °C, for surface doses between 1 and 50 displacements per atom (dpa). Atomic force microscopy and optical profilometry revealed irradiation-induced axial and radial shrinkage of SiC-fibers. At 50 dpa, net fiber shrinkage reached 2.8 ± 0.3%. We conclude that the primary cause of SiC-fiber shrinkage in SiC/SiC composites is the irradiation-induced loss of pre-existing carbon packets, which had occupied 2–3% fiber volume in unirradiated state. A compelling evidence of the carbon packet loss was revealed using a combination of state-of-art conventional transmission electron microscopy (TEM), high resolution TEM, energy-filtered TEM and electron energy loss spectroscopy. Additionally, the carbon packet volume fraction decreased with increasing dose, reaching near-complete loss after 50 dpa. Carbon packet loss was further confirmed using Raman spectroscopy where the carbon D and G peaks disappeared after irradiation. In contrast, irradiation-induced swelling of 1 ± 0.5% was observed in the matrix after 50 dpa. The study also shows that up to 50 dpa, the multilayer pyrolytic-carbon (PyC) interface in the composite is highly irradiation tolerant as it maintained its morphology, graphitic nature and showed no signs of amorphization. Additionally, Raman spectroscopy revealed a saturation of TEM invisible disorder at 1 dpa for both ultra-fine grains of the fiber and the larger SiC-matrix grains. However, TEM visible extended defect formation such as dislocation loops were only detected in the larger matrix grains, thereby revealing a potential role of grain size on defect accumulation in SiC.

36 MATERIALS SCIENCE↗
NASA NTRS2012

First Keck Nulling Observations of a Young Stellar Object: Probing the Circumstellar Environment of the Herbig Ae Star MWC325

We present the first N-band nulling plus K- and L-band V(sup 2) observations of a young stellar object, MWC 325, taken with the 85 m baseline Keck Interferometer. The Keck nuller was designed for the study of faint dust signatures associated with debris disks, but it also has a unique capability for studying the temperature and density distribution of denser disks found around young stellar objects. Interferometric observations of MWC 325 at K, L, and N encompass a factor of five in spectral range and thus, especially when spectrally dispersed within each band, enable characterization of the structure of the inner disk regions where planets form. Fitting our observations with . geometric models such as a uniform disk or a Gaussian disk show that the apparent size increases 'monotonically with wavelength in the 2-12/Lm wavelength region, confirming the widely held assumption based on radiative transfer models, now with spatially resolved measurements over a broad wavelength range, that disks are extended with a temperature gradient. The effective size is a factor of about 1.4 and 2.2 larger in the L band and N band, respectively, compared to that in the K band. The existing interferometric measurements and the spectral energy distribution can be reproduced by a flat disk or a weakly shadowed nearly flat disk model, with only slight flaring in the outer regions of the disk, consisting of representative "sub-micron" (0.1 micron) and "micron" (2 micron) grains of a 50:50 ratio of silicate and graphite. This is in marked contrast io the disks previously found in other Herbig Ae/Be stars, suggesting a wide variety in the disk properties among Herbig Ae/Be stars.

Ragland, S.↗
NASA NTRS2012

First Keck Nulling Observations of a Young Stellar Object: Probing the Circumstellar Environment of the Herbig Ae star MWC 325

We present the first N-band nulling plus K- and L-band V(sup 2) observations of a young stellar object, MWC325, taken with the 85 m baseline Keck Interferometer. The Keck nuller was designed for the study of faint dust signatures associated with debris disks, but it also has a unique capability for studying the temperature and density distribution of denser disks found around young stellar objects. Interferometric observations of MWC 325 at K, L and N encompass a factor of five in spectral range and thus, especially when spectrally dispersed within each band, enable characterization of the structure of the inner disk regions where planets form. Fitting our observations with geometric models such as a uniform disk or a Gaussian disk show that the apparent size increases monotonically with wavelength in the 2-12 micrometer wavelength region, confirming the widely held assumption based on radiative transfer models, now with spatially resolved measurements over broad wavelength range, that disks are extended with a temperature gradient. The effective size is a factor of about 1.3 and 2 larger in the Lband and N-band, respectively, compared to that in the K-band. The existing interferometric measurements and the spectral energy distribution can be reproduced by a flat disk or a weakly shadowed nearly flat-disk model, with only slight flaring in the outer regions of the disk, consisting of representative "sub-micron" (0.1 micron) and "micron" (2 micron) grains of a 50:50 ratio of silicate and graphite. This is marked contrast with the disks previously found in other Herbig Ae/Be stars suggesting a wide variety in the disk properties among Herbig Ae/Be stars.

Ragland, S.↗
DOE OSTI2019

Long-Term Stewardship Optimization for a Decommissioned Nuclear Reactor - 19579

The decommissioned Hallam Nuclear Power Facility (Hallam), located in Lancaster County, Nebraska, approximately 19 miles south of Lincoln, was developed as a prototype to investigate the technical and economic feasibility of a sodium-cooled, graphite-moderated nuclear reactor. As part of its Power Demonstration Program, the US Atomic Energy Commission (US AEC), a predecessor agency of the US Department of Energy (US DOE), operated the Hallam reactor from 1962 to 1964. The radiological surveillance of the Hallam site was established when the operating agreement between AEC and the Nebraska Public Power District was terminated. The US DOE Chicago Operations Office and the Nebraska Department of Health (NDH) agreed to install a shallow groundwater monitoring system as part of the environmental surveillance program. Surveillance at the site was scheduled to end in fiscal year 2005, with no further activities planned after that. At that time, the plan was to transition the site to the Nebraska Public Power District with future use of the facility to remain restricted. US DOE has title to and responsibility for the entombed radioactive materials. A surveillance and monitoring program was initiated in 1970 by NDH and was funded by US AEC. It included the analysis of samples from deep production wells (groundwater from the regional aquifer at depths greater than 55 meters [180 feet]) at the Sheldon Station. NDH was concerned in 1990 about the possibility of shallow groundwater coming in contact with the buried radiological materials along the buried walls of the reactor. Subsequently, DOE and NDH agreed to further characterize hydrologic conditions and establish a monitoring program in the shallow, perched groundwater zones. The current monitoring program focuses on the shallow, perched groundwater. Today, decades since facility decommissioning, site inspections and groundwater monitoring continue at this Cold War-era legacy site. The US DOE Office of Legacy Management (LM) monitors groundwater as a best management practice in response to a request from the Nebraska Department of Health and Human Services (DHHS). In 2006, LM recommended discontinuing groundwater monitoring because analytical results since 1970 demonstrated there had been no impact to shallow, perched groundwater and no current or anticipated unacceptable risk to human health and the environment. The State of Nebraska did not concur with the recommendation to stop monitoring but did agree to a reduction in sampling and analysis from once a year to once every 2 years--a schedule that began in 2008. An updated assessment of the groundwater monitoring effort was issued in 2016. The entire body of water-quality data continues to demonstrate that there have been no negative impacts to the shallow, perched groundwater from radioactive materials entombed at the site 46 years ago. LM, with concurrence from Nebraska DHHS, changed the sampling frequency, effective in 2018, as follows: once every 5 years from 2021 to 2041 and once every 10 years from 2041 to 2071. In summary, LM remains committed to its primary mission to protect human health and the environment at each of its 92 legacy sites. With results from groundwater sampling events demonstrating compliance for 48 years, the Hallam site was able to set an LM benchmark to optimize long-term stewardship and define an end-state strategy for other decommissioned reactor facilities across the DOE complex. Continued collaboration with local communities, stakeholder, and regulators often leads to outcomes of sound protectiveness without compromise to safety or compliance, as demonstrated by the optimization of the long-term stewardship at the Hallam site. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Graphitic Carbon Nitride Quantum Dots (g‐C 3 N 4 QDs): From Chemistry to Applications

Since their emergence in 2014, graphitic carbon nitride quantum dots (g-C 3 N 4 QDs) have attracted much interest from the scientific community due to their distinctive physicochemical features, including structural, morphological, electrochemical, and optoelectronic properties. Owing to their desirable characteristics, such as non-zero band gap, ability to be chemically functionalized or doped, possessing tunable properties, outstanding dispersibility in different media, and biocompatibility, g-C 3 N 4 QDs have shown promise for photocatalysis, energy devices, sensing, bioimaging, solar cells, optoelectronics, among other applications. As these fields are rapidly evolving, it is very strenuous to pinpoint the emerging challenges of the g-C 3 N 4 QDs development and application during the last decade, mainly due to the lack of critical reviews of the innovations in the g-C 3 N 4 QDs synthesis pathways and domains of application. Herein, an extensive survey is conducted on the g-C 3 N 4 QDs synthesis, characterization, and applications. Scenarios for the future development of g-C 3 N 4 QDs and their potential applications are highlighted and discussed in detail. In conclusion, the provided critical section suggests a myriad of opportunities for g-C 3 N 4 QDs, especially for their synthesis and functionalization, where a combination of eco-friendly/single step synthesis and chemical modification may be used to prepare g-C 3 N 4 QDs with, for example, enhanced photoluminescence and production yields.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

FIRST KECK NULLING OBSERVATIONS OF A YOUNG STELLAR OBJECT: PROBING THE CIRCUMSTELLAR ENVIRONMENT OF THE HERBIG Ae STAR MWC 325

We present the first N-band nulling plus K- and L-band V{sup 2} observations of a young stellar object, MWC 325, taken with the 85 m baseline Keck Interferometer. The Keck nuller was designed for the study of faint dust signatures associated with debris disks, but it also has a unique capability for studying the temperature and density distribution of denser disks found around young stellar objects. Interferometric observations of MWC 325 at K, L, and N encompass a factor of five in spectral range and thus, especially when spectrally dispersed within each band, enable characterization of the structure of the inner disk regions where planets form. Fitting our observations with geometric models such as a uniform disk or a Gaussian disk show that the apparent size increases monotonically with wavelength in the 2-12 {mu}m wavelength region, confirming the widely held assumption based on radiative transfer models, now with spatially resolved measurements over a broad wavelength range, that disks are extended with a temperature gradient. The effective size is a factor of about 1.4 and 2.2 larger in the L band and N band, respectively, compared to that in the K band. The existing interferometric measurements and the spectral energy distribution can be reproduced by a flat disk or a weakly shadowed nearly flat disk model, with only slight flaring in the outer regions of the disk, consisting of representative 'sub-micron' (0.1 {mu}m) and 'micron' (2 {mu}m) grains of a 50:50 ratio of silicate and graphite. This is in marked contrast to the disks previously found in other Herbig Ae/Be stars, suggesting a wide variety in the disk properties among Herbig Ae/Be stars.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2025

Interpretation of wide-angle x-ray diffraction patterns from mesophase pitch-based carbon fibers – a simulation and experimental study

Carbon fiber is a critical material in a wide range of industries, where it is highly valued for its high specific strength/stiffness, excellent wear resistance, efficient electrical and thermal transport properties, chemical resistance, and low coefficient of thermal expansion. The properties of a specific carbon fiber are closely tied to its structural characteristics at all length scales. Here, in this work, we applied wide-angle x-ray diffraction to a set of heat-treated mesophase pitch-based carbon fibers, with the goal of elucidating the crystalline structures as a function of fiber orientation. To assist with analysis and interpretation of the experimental data, we employed diffraction pattern simulations using the scalar and vector forms of the Debye scattering equation to determine the influence of basal plane orientation, crystalline ordering (turbostratic-graphitic), and basal plane asymmetry on the diffraction patterns. The results presented here suggest that growth of the transverse crystallites in mesophase pitch-based carbon fiber is fixed until graphitization temperatures are reached. The work completed here provides a framework for the analysis of carbon fiber and other oriented carbon-based materials via diffraction.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Cost-effective carbon fiber precursor selections of polyacrylonitrile-derived blend polymers: carbonization chemistry and structural characterizations

Blending polyacrylonitrile (PAN) with plastic wastes and bio-based polymers provides a convenient and inexpensive method to realize cost-effective carbon fiber (CF) precursors. In this work, PAN-based blend precursors are investigated using ReaxFF reactive molecular dynamics simulations with respect to the formation of all-carbon rings, the evolutions of oxygen-containing and nitrogen-containing species, and the migration of carbon atoms to form turbostratic graphene. From these simulations, we identify that PAN/cellulose (CL) blend manifests the highest carbon yield and the most substantial all-carbon ring formation. This ReaxFF-based finding is confirmed by Raman and TEM experiments indicating high crystallinity for PAN/CL-derived blend CFs. We trace the pathway of gasification and carbonization of PAN/CL to elaborate the mechanism of the formation of all-carbon ring networks. We discover that the acetals of CL can catalyze the cyclization of the blend precursor, allowing for the search for CL derivatives or the other kinds of bio-based polymers with similar functionalities as alternative blends. In addition, we examine the structural characteristics using the carbon–carbon (C–C) radial distribution functions, C–C bond length distributions, and sp2 C atom ratios for the four representative precursors, i.e., PAN, oxidized PAN, PAN/nylon 6,6, and PAN/CL. Our simulation results show the most extensive all-carbon ring cluster and graphitic structure growths for PAN/CL. Here, we propose PAN/CL as a cost-effective alternative CF precursor, since (a) CL is naturally abundant and eco-friendly for production, (b) the blend precursor PAN/CL does not require oxidation treatment, (c) PAN/CL has a high carbon yield with substantial all-carbon ring formation, and (d) PAN/CL based CFs potentially provide a mechanical property enhancement.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Management of the decommissioning of the Thetis reactor

The Thetis research reactor on the site of the Nuclear Sciences Institute of the Ghent University has been in operation from 1967 until December 2003. This light-water moderated graphite-reflected low-enriched uranium pool-type reactor has been used for various purposes e.g. the production of radioisotopes and activation analyses. During the first years its core power was 15 kW. In the early '70, a core enlargement allowed for operation at typically 150 kW, while the maximum was allowed to be 250 kW In September 2007, Ghent University entrusted to SCK-CEN the management of the back-end of the spent fuel and the decommissioning of the reactor. In 2010, the spent fuel was removed from the reactor and transported to Belgoprocess for cementation in 400 l drums and interim storage awaiting final disposal. This activity allows tackling the decommissioning of the reactor. The objective is to complete its decommissioning by the end of 2014. In the framework of the decommissioning of the Thetis reactor, SCK-CEN set-up the final decommissioning plan and the decommissioning licensing file. These documents include among others a radiological inventory of the reactor. The graphite moderator blocks, the control and the safety pates, the liner of the pool were modeled to assess the activation products (isotopic vector and intensity). At the end of the unloading of the reactor in 2010 a brief mapping of the equipment's and internals of the reactor pool was performed. In 2012, we realized a more detailed mapping. These results confirmed those performed earlier and allowed to confirm the assumptions made in the final decommissioning plan. We set-up the terms of reference for the first decommissioning phase of the reactor namely the dismantling of the reactor i.e. reactor pool, circuits and rabbit system, equipment's and ventilation ducts. The removal of asbestos is also included into this phase. We conducted the selection process and the awarding of this decommissioning job. We gained the decommissioning license in May 2012. We also prepared the software tool allowing managing the decommissioning project by updating the inventory and recording the progress, the characterization measurements and the material and waste production. This software allows also to trace all the material streams and to report to the Authorities. This software is a simplified release of the ones developed by SCK-CEN in the framework of other decommissioning projects like BR3 and Belgonucleaire. The dismantling of the reactor i.e. reactor pool, circuits and rabbit system, will be performed in 2013. In 2014, it is planned to map all the surfaces of the infrastructure to highlight residual contamination of floor, walls and ceiling. The contaminated surfaces will be decontaminated and controlled. The objective is to reach the free release of the reactor building and laboratories by the end of 2014. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1997

Interstellar and Cometary Dust

'Interstellar dust' forms a continuum of materials with differing properties which I divide into three classes on the basis of observations: (a) diffuse dust, in the low-density interstellar medium; (b) outer-cloud dust, observed in stars close enough to the outer edges of molecular clouds to be observed in the optical and ultraviolet regions of the spectrum, and (c) inner-cloud dust, deep within the cores of molecular clouds, and observed only in the infrared by means of absorption bands of C-H, C=O, 0-H, C(triple bond)N, etc. There is a surprising regularity of the extinction laws between diffuse- and outer-cloud dust. The entire mean extinction law from infrared through the observable ultraviolet spectrum can be characterized by a single parameter. There are real deviations from this mean law, larger than observational uncertainties, but they are much smaller than differences of the mean laws in diffuse- and outer-cloud dust. This fact shows that there are processes which operate over the entire distribution of grain sizes, and which change size distributions extremely efficiently. There is no evidence for mantles on grains in local diffuse and outer-cloud dust. The only published spectra of the star VI Cyg 12, the best candidate for showing mantles, does not show the 3.4 micro-m band which appreciable mantles would produce. Grains are larger in outer-cloud dust than diffuse dust because of coagulation, not accretion of extensive mantles. Core-mantle grains favored by J. M. Greenberg and collaborators, and composite grains of Mathis and Whiffen (1989), are discussed more extensively (naturally, I prefer the latter). The composite grains are fluffy and consist of silicates, amorphous carbon, and some graphite in the same grain. Grains deep within molecular clouds but before any processing within the solar system are presumably formed from the accretion of icy mantles on and within the coagulated outer-cloud grains. They should contain a mineral/carbonaceous matrix, without organic refractory mantles, in between the ices. Unfortunately, they may be significantly processed by chemical processes accompanying the warming (over the 10 K of the dark cloud cores) which occurs in the outer solar system. Evidence of this processing is the chemical anomalies present in interplanetary dust particles collected in the stratosphere, which may be the most primitive materials we have obtained to date. The comet return mission would greatly clarify the situation, and probably provide samples of genuine interstellar grains.

Mathis, John S.↗
NASA NTRS2004

Interstellar Dust Models

A viable interstellar dust model - characterized by the composition, morphology, and size distribution of the dust grains and by the abundance of the different elements locked up in the dust - should fit all observational constraints arising primarily from the interactions of the dust with incident radiation or the ambient gas. As a minimum, these should include the average interstellar extinction, the infrared emission from the diffuse interstellar medium (ISM), and the observed interstellar abundances of the various refractory elements. The last constraint has been largely ignored, resulting in dust models that require more elements to be in the dust phase than available in the ISM. In this talk I will describe the most recent advances towards the construction of a comprehensive dust model made by Zubko, Dwek, and Arendt, who, for the first time, included the interstellar abundances as explicit constraints in the construction of interstellar dust models. The results showed the existence of many distinct models that satisfy the basic set of observational constraints, including bare spherical silicate and graphite particles, PAHs, as well as spherical composite particles containing silicate, organic refractories, water ice, and voids. Recently, a new interstellar dust constituent has emerged, consisting of metallic needles. These needles constitute a very small fraction of the interstellar dust abundance, and their existence is primarily manifested in the 4 to 8 micron wavelength region, where they dominate the interstellar extinction. Preliminary studies show that these models may be distinguished by their X-ray halos, which are produced primarily by small angle scattering off large dust particles along the line of sight to bright X-ray sources, and probe dust properties largely inaccessible at other wavelengths.

Dwek, Eli↗
DOE OSTI2018

High catalytic performance of Fe-Ni/Palygorskite in the steam reforming of toluene for hydrogen production

The inexpensive and abundant material, palygorskite, was used as a promising catalyst support to prepare Fe-Ni/Pal catalysts. Catalytic steam reforming of toluene as a biomass tar model compound over these catalysts was investigated in a fixed-bed reactor under different parameters, including reaction temperatures and S/C molar ratios. The stability and lifetime of Fe 3 Ni 8 /Palygorskite catalyst was evaluated under optimal conditions and its kinetic parameters were determined as well. The fresh and used catalysts were characterized using X-ray diffraction (XRD), H 2 temperature-programmed reduction (H 2 -TPR), transmission electron microscopy (TEM), and Raman spectra. The results showed that the Fe 3 Ni 8 /Palygorskite catalyst with high dispersion was successfully prepared and exhibited superior catalytic performance compared with those of the monometallic catalysts (Fe 3 /Palygorskite and Ni 8 /Palygorskite) and the bare Palygorskite. Increasing the reaction temperature from 500 °C to 700 °C was beneficial for the toluene conversion and gaseous yields. The catalytic activity of Fe 3 Ni 8 /Palygorskite varied distinctly with the increase of S/C molar ratio and reached maximum at the the S/C molar ratio of 1.0. The apparent activation energy of 41.55 kJ mol -1 and the pre-exponential factor of 1.35 × 10 3 m 3 kg -1 h -1 were obtained for Fe 3 Ni 8 /Palygorskite in kinetic studies under optimal reaction conditions, respectively. Here, the carbon deposition analysis of the used catalysts revealed that the formation of graphitic carbon rather than amorphous carbon was the main reason for the deactivation of Fe 3 Ni 8 /Palygorskite catalysts. When ceased the injection of steam into the reaction system, the graphitic carbon would be accelerating formed on the surface of the Fe 3 Ni 8 /Palygorskite and decreased its catalytic activity for toluene conversion. But owing to the water gas shift reaction, the catalytic activity of Fe 3 Ni 8 /Palygorskite seemed to recover gradually to its optimum.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

TH-C-19A-01: Analytic Design Method to Make a 2D Planar, Segmented Ion Chamber Water-Equivalent for Proton Dose Measurements

Purpose: Quality Assurance (QA) measurements of proton therapy fields must accurately measure steep longitudinal dose gradients as well as characterize the dose distribution laterally. Currently, available devices for two-dimensional field measurements perturb the dose distribution such that routine QA measurements performed at multiple depths require multiple field deliveries and are time consuming. Methods: A design procedure for a two-dimensional detector array is introduced whereby the proton energy loss and scatter are adjusted so that the downstream dose distribution is maintained to be equivalent to that which would occur in uniform water. Starting with the design for an existing, functional two-dimensional segmented ion chamber prototype, a compensating material is introduced downstream of the detector to simultaneously equate the energy loss and lateral scatter in the detector assembly to the values in water. An analytic formalism and procedure is demonstrated to calculate the properties of the compensating material in the general case of multiple layers of arbitrary material. The resulting design is validated with Monte Carlo simulations. Results: With respect to the specific prototype design considered, the results indicate that a graphite compensating layer of the proper dimensions can yield proton beam range perturbation less than 0.1mm and beam sigma perturbation less than 2% across the energy range of therapeutic proton beams. Conclusion: We have shown that, for a 2D gas-filled detector array, a graphite-compensating layer can balance the energy loss and multiple Coulomb scattering relative to uniform water. We have demonstrated an analytic formalism and procedure to determine a compensating material in the general case of multiple layers of arbitrary material. This work was supported by the US Army Medical Research and Materiel Command under Contract Agreement No. DAMD17-W81XWH-04-2-0022. Opinions, interpretations, conclusions and recommendations are those of the author and are not necessarily endorsed by the US Army.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2010

Correlation between grain orientation and the shade of color etching

Color etching is an extremely effective metallographic technique not only for making grains well visible, but also for making them distinguishable for automated image analyzers. During color etching, a thin film is formed on the surface of the specimen. The thickness of this layer is in the order of magnitude of the visible light and since both the metal-film boundary and the film surface reflect light, an interference occurs. A wavelength-component of the white line is eliminated and its complementary color will be seen on the surface. As the thickness changes, the colors also change grain by grain. The thickness of the film is dependent on several factors, mostly on the type of the phase. However, different color shades can be observed on the surfaces of single phase materials, which phenomenon is caused by the different crystallographic orientations of the grains. This paper shows a combined color etching electron backscatter diffraction (EBSD) investigation of cast iron. An area of the surface of a gray cast iron specimen was etched. Colors were characterized by their luminescence and their red, green and blue intensity. An EBSD orientation map was taken from the same area and the orientations of the individual grains were determined. Results showed that a strong correlation was found between the luminescence and the R, G, B intensity of the color and the angle between the specimen normal and the < 100> direction, while such correlation was not observed between the color parameters and the < 110 > and < 111> directions, respectively. This indicates that film thickness is sensitive to the < 100> direction of the crystal.

36 MATERIALS SCIENCE↗