Properties of powder ground in ultrahigh vacuum Final technical report, 24 Aug. 1965 - 23 Aug. 1966
Lunar soil properties determination through simulation of rock grinding in ultrahigh vacuum
ROCK↗
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REMOTE REFURBISHMENT OF THE METALLOGRAPHY PREPARATION BOX AT THE INL
One of the most utilized hot cell capabilities at the Idaho National Laboratory is referred to as the containment box. This is where all destructive examination samples are prepared for analysis. This one window box is contained within the much larger Hot Fuels Examination Facility which consists of a 21x10x8 meter hot cell with an inert argon atmosphere. The refurbishment of this box entailed removing of all sample preparation equipment and support systems, as well as the design and installation of new preparation equipment. The new equipment consists of low and high speed saws, grinding and polishing equipment, water recirculation systems, and sample storage units. This paper includes the details of this refurbishment.
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
Status of Process Development for Pyrolysis of Biomass for Liquid Fuels and Chemicals Production.
Pyrolysis is one of several thermochemical conversion strategies to produce useful fuels from biomass material . The goal of fast pyrolysis is to maximize liquid product yield. Fast pyrolysis is accomplished by the thermal treatment of the biomass in an air-free environment. Very short heat up and cool-down is a requirement for fast pyrolysis. The typical residence time in the pyrolysis reactor is 1 second. In order to accomplish the fast heatup, grinding the biomass to a small particle size in the range of 1 mm is typical and pre-drying of the biomass to less than 10 weight percent moisture is considered the standard. Recovery of the product liquid, called bio-oil, is accomplished by a variety of methods all of which require a quick quench of the product vapor. A definition of fast pyrolysis bio-oil is provided for the CAS # RN 1207435-39-9 recently issued by ChemAbstracts Services.
09 BIOMASS FUELS↗
Plasma Sprayed Pour Tubes and Other Melt Handling Components for Use in Gas Atomization
Ames Laboratory has successfully used plasma sprayed ceramic components made from yttria stabilized zirconia as melt pouring tubes for gas atomization for many years. These tubes have proven to be strong, thermal shock resistant and versatile. Various configurations are possible both internally and externally. Accurate dimensions are achieved internally with a machined fugitive graphite mandrel and externally by diamond grinding. The previous study of the effect of spray parameters on density was extended to determine the effect of the resulting density on the thermal shock characteristics on down-quenching and up-quenching. Encouraging results also prompted investigation of the use of plasma spraying as a method to construct a melt pour exit stopper that is mechanically robust, thermal shock resistant, and not susceptible to attack by reactive melt additions. The Ames Laboratory operates two close-coupled high pressure gas atomizers. These two atomizers are designed to produce fine and coarse spherical metal powders (5{mu} to 500{mu} diameter) of many different metals and alloys. The systems vary in size, but generally the smaller atomizer can produce up to 5 kg of powder whereas the larger can produce up to 25 kg depending on the charge form and density. In order to make powders of such varying compositions, it is necessary to have melt systems capable of heating and containing the liquid charge to the desired superheat temperature prior to pouring through the atomization nozzle. For some metals and alloys this is not a problem; however for some more reactive and/or high melting materials this can pose unique challenges. Figure 1 is a schematic that illustrates the atomization system and its components.
36 MATERIALS SCIENCE↗
A Novel Mobile Examination and Remediation Facility for On-Site Remediation of Dry Storage Systems - 18389
Most of the spent nuclear fuel (SNF) in dry storage in the United States is safely and securely stored in dual-purpose (i.e., storage and transportation) canisters [1]. However, some of the SNF is stored in storage-only (i.e., non-transportable) packages, or packages that may become nonconforming for continued storage or transportation for a variety of reasons. Currently, the capability to remediate dry storage systems (DSSs) for SNF that are not transportable or that need to be repaired to maintain confinement boundary integrity during storage service does not exist without on-site access to a spent fuel pool. Hence, there is a potential future need for a mobile facility with remediation capabilities that can be used at multiple storage installations. These capabilities would permit needed repairs to an existing DSS to support continued storage or for the dry transfer of fuel to a new conveyance suitable for transport, if necessary. This is a technical paper that does not take into account the contractual limitations under the Standard Contract for Disposal of Spent Nuclear Fuel and/or High-Level Radioactive Waste (Standard Contract) (10 CFR Part 961). Under the provisions of the Standard Contract, DOE does not consider spent nuclear fuel in canisters to be an acceptable waste form, absent a mutually agreed to contract amendment. To the extent discussions or recommendations in this paper conflict with the provisions of the Standard Contract, the Standard Contract provisions prevail. A novel design concept for a Mobile Examination and Remediation Facility (MERF) is proposed with functions and capabilities to remediate a DSS. The proposed MERF would be a multi-purpose facility, remotely operated and computer-controlled with semi-automated equipment to allow trained operators to safely perform remediation activities while keeping worker radiation dose as low as reasonably achievable. It would include a shielded rotating platform with support towers and would use commercial off- the-shelf examination and repair equipment. A slip ring arrangement underneath the rotating platform would allow for the power supply without impeding the continuous rotation and would simplify cable management. The support towers would be mounted on the rotating platform, and each tower would have vertical and horizontal positioning capability for axial and radial tool location. The rotating platform would be attached to the main MERF structure. Capabilities would include visual, surface, and volumetric examinations to fully characterize physical conditions on canister surface before and after a repair; repair techniques, e.g., laser beam welding, friction stir welding, or cold spray, to perform needed remediation activities; and associated equipment for surface preparation such as cutting and grinding equipment. The proposed design would be simple, modular, robust, economically viable, and easily transportable and would have a small footprint. The modular design would present several advantages including compatibility with a variety of different DSSs, on-site assembly, and transportability; it also would be built in interchangeable sections to facilitate decontamination. Further, shielding would be supplemented through interface with the existing transfer cask and storage overpack. Robustness and canister stability would be achieved using pneumatic holders and steel support structures designed with vibration absorbers to reduce impacts and/or a 'pendulum' effect during a seismic event. Thus, the proposed MERF would be designed to: (i) minimize handling of an affected DSS to the extent practicable, (ii) provide radiation shielding and minimize dose to operators and the public during remediation activities, and (iii) enable examination, repair, and repackaging. This paper describes the proposed MERF design concept and capabilities, main components, equipment, different modes of operation, and operating procedures. Structural and safety assessments would need to be performed before final design, licensing, and deployment. The MERF is evaluated with respect to regulatory impact (first of a kind, prior experience), operational impact (safety, security, staffing, ongoing operations, constraints), worker dose (low, medium, high), cost (low, medium, high), schedule (duration, time sequence), and technology readiness level. (authors)
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Stimuli‐Responsive Emission from Hybrid Metal Halides
Abstract Stimuli‐responsive photoluminescent (PL) materials have attracted considerable attention in recent years owing to their potential applications in anti‐counterfeiting, information encryption, and sensing. Further investigations of the transformation mechanism and potential applications of stimulus‐responsive PL materials are considerably important. In the current study, an organic–inorganic metal halide, C 9 H 15 N 3 SbCl 5 ([C 9 H 13 N 3 ] 2+ is a 1‐(2‐pyridyl) piperazine cation) is obtained, which exhibits a 0D structure withP‐1 space group. At room temperature, when excited by UV light, the C 9 H 15 N 3 SbCl 5 single crystals exhibit unimodal blue light emission at 405 nm, and grinding or hydrostatic pressure induces double‐peak emissions at 405 and 650 nm. Interestingly, double‐emission samples can be restored to single‐emission samples by short annealing or storage in air for 2 weeks, and this process is reversible. Luminescence response to mechanical stimuli can also be achieved in the presence of hydrochloric acid and water. Spectral analysis and the analysis of the microstructural changes revealed that the structural modifications of the inorganic group play a pivotal role in the response to the stimulus. Finally, a composite film device based on C 9 H 15 N 3 SbCl 5 is prepared to demonstrate the potential of these smart materials in anti‐counterfeiting and sensing applications.
Chemistry↗
The Anode Challenge for Lithium‐Ion Batteries: A Mechanochemically Synthesized Sn–Fe–C Composite Anode Surpasses Graphitic Carbon
Carbon‐based anodes are the key limiting factor in increasing the volumetric capacity of lithium‐ion batteries. Tin‐based composites are one alternative approach. Nanosized Sn–Fe–C anode materials are mechanochemically synthesized by reducing SnO with Ti in the presence of carbon. The optimum synthesis conditions are found to be 1:0.25:10 for initial ratio of SnO, Ti, and graphite with a total grinding time of 8 h. This optimized composite shows excellent extended cycling at the C/10 rate, delivering a first charge capacity as high as 740 mAh g −1 and 60% of which still remained after 170 cycles. The calculated volumetric capacity significantly exceeds that of carbon. It also exhibits excellent rate capability, delivering volumetric capacity higher than 1.6 Ah cc −1 over 140 cycles at the 1 C rate.
25 ENERGY STORAGE↗
Solvent‐Free Self‐Assembly for Scalable Preparation of Highly Crystalline Mesoporous Metal Oxides
Abstract Mesoporous metal oxides (MMOs) have been demonstrated great potential in various applications. Up to now, the direct synthesis of MMOs is still limited to the solvent induced inorganic‐organic self‐assembly process. Here, we develop a facile, general, and high throughput solvent‐free self‐assembly strategy to synthesize a series of MMOs including single‐component MMOs and multi‐component MMOs (e.g., doped MMOs, composite MMOs, and polymetallic oxide) with high crystallinity and remarkable porous properties by grinding and heating raw materials. Compared with the traditional solution self‐assembly process, the avoidance of solvents in this method not only greatly increases the yield of target products and synthesis efficiency, but also reduces the environmental pollution and the consumption of cost and energy. We believe the presented approach will pave a new avenue for scalable production of advanced mesoporous materials for various applications.
Xiong, Hailong↗
Solvent-Free Self-Assembly for Scalable Preparation of Highly Crystalline Mesoporous Metal Oxides
Mesoporous metal oxides (MMOs) have been demonstrated great potential in various applications. Up to now, the direct synthesis of MMOs is still limited to the solvent induced inorganic-organic self-assembly process. In this work, we develop a facile, general, and high throughput solvent-free self-assembly strategy to synthesize a series of MMOs including single-component MMOs and multi-component MMOs (e.g., doped MMOs, composite MMOs, and polymetallic oxide) with high crystallinity and remarkable porous properties by grinding and heating raw materials. Compared with the traditional solution self-assembly process, the avoidance of solvents in this method not only greatly increases the yield of target products and synthesis efficiency, but also reduces the environmental pollution and the consumption of cost and energy. We believe the presented approach will pave a new avenue for scalable production of advanced mesoporous materials for various applications.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Intercalation-Activated Layered MoO 3 Nanobelts as Biodegradable Nanozymes for Tumor-Specific Photo-Enhanced Catalytic Therapy
The existence of natural van der Waals gaps in layered materials allows them to be easily intercalated with varying guest species, offering an appealing strategy to optimize their physicochemical properties and application performance. Herein, we report the activation of layered MoO 3 nanobelts via aqueous intercalation as an efficient biodegradable nanozyme for tumor-specific photo-enhanced catalytic therapy. In this work, the long MoO 3 nanobelts are grinded and then intercalated with Na + and H 2 O to obtain the short Na + /H 2 O co-intercalated MoO 3–x (NH–MoO 3–x ) nanobelts. In contrast to the inert MoO 3 nanobelts, the NH–MoO 3–x nanobelts exhibit excellent enzyme-mimicking catalytic activity for generation of reactive oxygen species, which can be further enhanced by the photothermal effect under a 1064 nm laser irradiation. Thus, after bovine serum albumin modification, the NH–MoO 3–x nanobelts can efficiently kill cancer cells in vitro and eliminate tumors in vivo facilitating with 1064 nm laser irradiation.
36 MATERIALS SCIENCE↗
SnO 2 Transparent Printing Pastes from Powders for Photon Conversion in SnO 2 -Based Dye-Sensitized Solar Cells
Tin oxide (SnO 2 ) is the most enticing alternative to titanium oxide (TiO 2 ) with the aim of identifying a more positive conduction band material for dye-sensitized solar cells (DSCs). We put forward a protocol based on grinding, sonication, and centrifuge to generate transparent SnO 2 pastes to minimize light reflectance losses from the metal oxide. Under optimized conditions, a highly transparent film with substantially enhanced light penetration depth through active layer SnO 2 is realized for efficient light harvesting from two different commercially available powders (18 and 35 nm nanoparticle sizes). A ruthenium sensitizer ( B11 ) and two organic sensitizers ( NL3 and MK2 ) are shown to achieve higher or comparable photocurrent densities with SnO 2 relative to standard TiO 2 -based DSCs. SnO 2 -based DSCs show minimum recombination losses, comparable charge collection efficiencies, and minimal photovoltage losses relative to TiO 2 DSCs. Thus, the option of a transparent metal oxide, which can facilitate high photocurrents (>16 mA cm -2 observed) and lower recombination rates than TiO 2 is an attractive material for DSC applications.
14 SOLAR ENERGY↗
Effect of bimetallic modification on blast furnace slag and its application in low‐temperature selective catalytic reduction
Abstract Objective In order to control NO x in low‐temperature flue gases emitted from non‐power industries and to reduce the preparation cost of denitration catalysts, this study uses inexpensive blast furnace slag as raw material to prepare denitration catalysts. Methods After cooling, drying and grinding, the blast furnace slag becomes a powder with considerable fineness and meets the requirements of activity index, which is called GGBS (ground granulated blast furnace slag). Using GGBS as denitration catalyst carrier, the active components M (M = Fe, Co, Ni, Cu and Ce) are loaded on Mn‐based GGBS catalyst using an impregnation method. Conclusions The effect of different active components on the denitration performance and sulfur resistance of Mn‐based GGBS catalysts is investigated. The results show that the Mn‐Ce/GGBS catalyst has better denitration performance and sulfur resistance. The Mn‐Ce/GGBS catalyst has a significant denitration performance when load ratio is 2:1. The active component Ce improves the denitration performance of the catalyst, reduces sulfur poisoning and extends the life of the catalyst. The SO 2 in the flue gas increases the acid sites on the catalyst surface and improves catalyst activity. The larger the ratios of Mn 4+ /Mn 3+ , Ce 4+ /Ce 3+ and O α /O β , the stronger the catalyst activity and the better the denitration performance. © 2022 Society of Chemical Industry (SCI).
Zhang, Lei↗
Ball Milling Modified SAPO‐11 Based Catalysts for n ‐Decane Hydroisomerization
Abstract Bifunctional Pt/SAPO‐11 catalysts were prepared using as acid matrix the microporous silico‐aluminophosphate, SAPO‐11, synthesized under microwave radiation. After synthesis, the material was physically modified using a ball mill, changing the grinding time but keeping frequency constant. The metal function (0.5 wt.% Pt) was introduced through mechanical mixture with commercial Pt loaded alumina. The catalysts were characterized by several techniques: powder X‐Ray Diffraction, pyridine adsorption followed by infrared spectroscopy, low temperature N 2 adsorption, Hg intrusion porosimetry and electronic microscopy (SEM). The characterization data show modifications of structural and textural properties of the samples as the milling time increases. The catalytic behaviour of Pt/SAPO‐11 materials was studied for hydroisomerization of long chain n ‐alkanes, using n ‐decane as model molecule, aiming to increase the production of mono‐branched isomers. The catalytic results show that, under optimized milling conditions (60 min; 50 Hz) the selectivity into mono‐branched isomers increased when compared with parent catalyst.
Ferreira, Luisa↗
Isolation and characterization of lignocellulosic nanofibers from four kinds of organosolv-fractionated lignocellulosic materials
The objective of this research was to investigate the presence of residual lignin in cellulose fibers on the efficiency and energy consumption during nanofibers processing. Four kinds of lignin-containing cellulose nanofibers (LCNFs) from switchgrass, yellow poplar, hybrid poplar, and pine, respectively, were isolated via organosolv fractionation coupling mechanical grinding. Nanofibrils were observed after organosolv fractionation. The details of their morphological features, chemical structures, water retention value (WRV), and thermal degradation characteristics were revealed and compared. Mean diameters of nanofibers separated from switchgrass, yellow poplar, hybrid poplar, and pine were 27.9 nm, 25.4 nm, 24.6 nm, and 21.5 nm, respectively. The presence of lignin for the four types of LCNFs led to a decrease in energy consumption and an increase in WRV, among which pine nanofibers show the best with an average energy consumption of 0.511 kWh/kg and a WRV of 537%. It was also demonstrated that increasing lignin content for LCNFs could contribute to the sample’s thermal stability. In conclusion, exact benefits of residual lignin for nanofiber will facilitate its preparation process and extend its application.
36 MATERIALS SCIENCE↗
Effect of Surface Treatment on High-Temperature Oxidation Behavior of IN 713C
The effects of surface preparations on oxidation kinetics and oxide scale morphology for the commercially available Ni-based superalloy IN 713C have been investigated. The ground and polished samples were exposed in air at 800-1100 °C. The ground specimens were found to demonstrate lower oxidation kinetics compared to those after polishing. The grinding also affected the oxide scale morphology, resulting in a protective alumina scale, while the polished samples developed Ni-/Cr-rich mixed oxides on the surface. Better oxidation resistance of the ground surfaces is related to a higher concentration of defects in the near-surface region introduced by cold working. These defects facilitate the outward transport of the scale-forming element Al and thus are beneficial for protective oxidation. The oxidation mechanism at lower temperatures was introduced. The model based on the generalized Darken method and multiphase approximation was proposed.
36 MATERIALS SCIENCE↗
High Wear-Resistant Aluminum Matrix Composite Layer Fabricated by MIG Welding with Lateral B{sub 4}C Powder Injection
In this work, a low-cost technique combining MIG welding and lateral powder injection was developed to fabricate B{sub 4}C particles-reinforced aluminum matrix composite (AMC) layer on a T6 heat-treated 7075 aluminum alloy (AA7075-T6) substrate. The AMC layer was 6-7 mm thick and well bonded to the substrate. The B{sub 4}C particles were dispersed throughout the AMC layer with an average content of approximately 7 vol.%. No significant reaction products existed either at the particle–matrix interface or in the Al-matrix. In pin-on-disk dry sliding wear tests against Al{sub 2}O{sub 3} grinding wheels, the AMC layer exhibited excellent wear resistance with volume wear rate approximately 1/10-3/10 that of the quenched AISI 1045 steel and only approximately 2-7% that of the AA7075-T6 alloy under the same wear conditions. A small addition of ceramic particles can greatly improve wear resistance, suggesting that this technique has good prospects for a wide variety of applications.
36 MATERIALS SCIENCE↗
Role of Si in the Surface Damage Mechanism of RB-SiC/Si Under Mechanical Loading
Indentation test (Nanoindentation and Vickers indentation), diamond scratching and high spindle speed grinding are conducted to investigate the role of silicon (Si) in the surface damage behavior of reaction-bonded SiC/Si composites (RB-SiC/Si). Even though the addition of Si contributes to densifying the bulk materials and improving the toughness, the indentation and diamond scratching results firstly indicate that the cracks initiate at the SiC/Si interfaces due to the non-uniform deformation caused by the existence of Si, and the phase transformation of Si also leads to the pop-out effect during the nanoindentation and the diamond scratching test. The ground surface of RB-SiC/Si is characterized by scratching grooves and brittle fracture, indicating the ductile material removal mode and brittle material removal mode for RB-SiC/Si, respectively, and the surface reliefs form on the ground surface due to the different hardness between Si and SiC phases. Moreover, the phase transformation of Si contributes to the easy fracture of phase boundaries under the mechanical loading, and the accompanied volume change also results in the dislodgement of hard particles and the generation of surface burs on the ground surface.
36 MATERIALS SCIENCE↗
Grain-Refined Microstructure and Hard Surface Layer Produced by SMRGT Process for Improved Corrosion Behavior of Mg-3Al-1Zn Alloy
To improve the surface properties and performance, a grain-refined surface layer was produced on AZ31B Mg alloy by a newly developed surface nano-crystallization and hardening process called surface mechanical rolling grinding treatment (SMRGT). The grain size refinement and minimal surface hardening were confirmed by the microstructure observations, XRD results and microhardness tests and were attributed to the multipass small strain-induced plastic deformation of the material during the SMRGT process. A nano-grain surface layer (average grain size of ~ 100 nm) and a graded microhardness variation (average ~ 113 HV adjacent to surface) along the thickness direction were generated. The E{sub corr} values of the as-SMRGTed samples were − 1.43 ± 0.03 and − 1.42 ± 0.02 V, increasing by ~ 30-40 mV compared with the values of the as-received (AR) sample (− 1.46 ± 0.02 V), corresponding to i{sub corr} ranging from 3.0 × 10{sup −5} to 1.0 × 10{sup −5} and 5.0 × 10{sup −6} A/cm{sup 2}, respectively. Charge transfer resistance (R{sub ct}) increased from 93.4 to 292.4 and 578.3 Ω (~ 3-6 times) with the increasing number of SMRGT passes. The corrosion resistance improvement was attributed mainly to the dramatic strain-induced surface grain refinement and minimal surface hardening that give rise to a more smooth and densely packed surface state.
36 MATERIALS SCIENCE↗