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At least 37 records · Page 2

Improvements in Production of Single-Walled Carbon Nanotubes

A continuing program of research and development has been directed toward improvement of a prior batch process in which single-walled carbon nanotubes are formed by catalytic disproportionation of carbon monoxide in a fluidized-bed reactor. The overall effect of the improvements has been to make progress toward converting the process from a batch mode to a continuous mode and to scaling of production to larger quantities. Efforts have also been made to optimize associated purification and dispersion post processes to make them effective at large scales and to investigate means of incorporating the purified products into composite materials. The ultimate purpose of the program is to enable the production of high-quality single-walled carbon nanotubes in quantities large enough and at costs low enough to foster the further development of practical applications. The fluidized bed used in this process contains mixed-metal catalyst particles. The choice of the catalyst and the operating conditions is such that the yield of single-walled carbon nanotubes, relative to all forms of carbon (including carbon fibers, multi-walled carbon nanotubes, and graphite) produced in the disproportionation reaction is more than 90 weight percent. After the reaction, the nanotubes are dispersed in various solvents in preparation for end use, which typically involves blending into a plastic, ceramic, or other matrix to form a composite material. Notwithstanding the batch nature of the unmodified prior fluidized-bed process, the fluidized-bed reactor operates in a continuous mode during the process. The operation is almost entirely automated, utilizing mass flow controllers, a control computer running software specific to the process, and other equipment. Moreover, an important inherent advantage of fluidized- bed reactors in general is that solid particles can be added to and removed from fluidized beds during operation. For these reasons, the process and equipment were amenable to modification for conversion from batch to continuous production.

Balzano, Leandro↗

Development of a Solvent-Free Process to Prepare DNAN

Objectives: Additive-free, solvent-free chemical reactions are generally more environmentally benign than alternative processes that involve these reaction components. 2,4-Dinitroanisole (DNAN) is of interest to the military and to industry as a replacement for trinitrotoluene (TNT) in melt-cast explosives. As anisole is a widely used feedstock chemical, the development of an efficient, additive-free, solvent-free method for its dinitration could lead to adoption of a new “green” synthetic route for DNAN manufacture. Technical Approach: Our goal is the scale-up (from the previously demonstrated one gram scale to a 500 gram scale) of the additive-free, solvent-free dinitration of anisole using the equipment and facilities available at the Los Alamos National Laboratory. Results: Through a series of simple optimization process, we have been successful at scaling demonstrating the development of a solvent-free process for the synthesis of 2,4-dinitroanisole using a batch process. The overall method involves the use of a mixture of propionic anhydride and 98% nitric acid to form the reactive nitrating species, proprionyl nitrate. This nitrating reagent is then added to a highly concentrated solution mixture of anisole and proprionic anhydride slowly over time to produce the desired 2,4-dinitroanisole product. This batch process could be scaled-up to the 270g scale. Flow-reaction methods should allow for larger scale production of DNAN. Benefits: This work has addressed the SERDP SEED Statement Of Need regarding environmentally benign methods for the synthesis of DNAN. Having achieved our goal, the next step will be to partner with a commercial manufacturer of explosive materials to scale the synthesis up to production levels.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Time-Domain Terahertz Computed Axial Tomography NDE System

NASA has identified the need for advanced non-destructive evaluation (NDE) methods to characterize aging and durability in aircraft materials to improve the safety of the nation's airline fleet. 3D THz tomography can play a major role in detection and characterization of flaws and degradation in aircraft materials, including Kevlar-based composites and Kevlar and Zylon fabric covers for soft-shell fan containment where aging and durability issues are critical. A prototype computed tomography (CT) time-domain (TD) THz imaging system has been used to generate 3D images of several test objects including a TUFI tile (a thermal protection system tile used on the Space Shuttle and possibly the Orion or similar capsules). This TUFI tile had simulated impact damage that was located and the depth of damage determined. The CT motion control gan try was designed and constructed, and then integrated with a T-Ray 4000 control unit and motion controller to create a complete CT TD-THz imaging system prototype. A data collection software script was developed that takes multiple z-axis slices in sequence and saves the data for batch processing. The data collection software was integrated with the ability to batch process the slice data with the CT TD-THz image reconstruction software. The time required to take a single CT slice was decreased from six minutes to approximately one minute by replacing the 320 ps, 100-Hz waveform acquisition system with an 80 ps, 1,000-Hz waveform acquisition system. The TD-THZ computed tomography system was built from pre-existing commercial off-the-shelf subsystems. A CT motion control gantry was constructed from COTS components that can handle larger samples. The motion control gantry allows inspection of sample sizes of up to approximately one cubic foot (.0.03 cubic meters). The system reduced to practice a CT-TDTHz system incorporating a COTS 80- ps/l-kHz waveform scanner. The incorporation of this scanner in the system allows acquisition of 3D slice data with better signal-to-noise using a COTS scanner rather than the gchirped h scanner. The system also reduced to practice a prototype for commercial CT systems for insulating materials where safety concerns cannot accommodate x-ray. A software script was written to automate the COTS software to collect and process TD-THz CT data.

Zimdars, David↗

Analysis of Operating Strategies Using Different Target Designs For 238Pu Production

An engineering effort is underway to re-establish capability to produce 238Pu oxide at the kilogram scale in the United States. A multi-step batch process is being developed to produce this important material. Recently, a portion of this process was studied using discrete-event simulation tools to determine whether the conceptual process might achieve its yearly production goal. The study showed the conceptual process can meet the yearly production goal under some circumstances, but process improvements would be needed to ensure greater likelihood of success. This study extends the work performed previously by examining the effects of changing the reactor target design on the yearly process output. Two new reactor target configurations are considered an aluminum-clad reactor target containing 50% greater 237Np oxide content than the original target, and a zirconium alloy-clad target using no aluminum. The results indicate that use of the new aluminum-clad target configuration may allow the process to achieve the same yearly production goal in less time using fewer targets. If the zirconium alloy-clad target is used, then even fewer targets would be needed to reach the production goal, but some process changes would be required to handle the zirconium cladding. The number of days needed to process a target batch to completion, and the steady state 238Pu oxide production rate, for each configuration are compared to the results from the initial simulation study.

campaign↗

Development of a Batch Fabrication Process for Chemical Nanosensors: Recent Advancements at NASA Glenn Research Center

A major objective in aerospace sensor development is to produce sensors that are small in size, easy to batch fabricate and low in cost, and have low power consumption. Chemical sensors involving nanostructured materials can provide these characteristics as well as the potential for the development of sensor systems with unique properties and improved performance. However, the fabrication and processing of nanostructures for sensor applications currently is limited by the ability to control their location on the sensor platform, which in turn hinders the progress for batch fabrication. This presentation will discuss the following: the development of a novel room temperature methane (CH4) sensor fabricated using porous tin oxide (SnO2) nanorods as the sensing material, the advantages of using nanomaterials in sensor designs, the challenges encountered with the integration of nanostructures into microsensordevices, and the different methods that have been attempted to address these challenges. An approach for the mass production of sensors with nanostructures using a method developed by our group at the NASA Glenn Research Center to control the alignment of nanostructures onto a sensor platform will also be described.

Nanotechnology↗

B827 Chemical Synthhesis Project - Industrial Control System Integration - Statement of Work & Specification with Attachments 1-14

The Chemical Synthesis Pilot Process at the Lawrence Livermore National Laboratory (LLNL) Site 300 827 Complex will be used to synthesize small quantities of material to support research and development. The project will modernize and increase current capabilities for chemical synthesis at LLNL. The primary objective of this project is the conversion of a non-automated hands-on process to a remoteoperation process, while providing enhanced batch process step control, stored recipe-specific parameter sets, process variable visibility, monitoring, alarm and warning handling, and comprehensive batch record data logging. This Statement of Work and Specification provides the industrial-grade process control requirements for the chemical synthesis batching control system, hereafter referred to as the “Control System” to be delivered by the System Integrator.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A novel defoamer for processing nuclear waste: Testing and performance

Abstract Legacy radioactive waste from nuclear weapons material processing is the biggest environmental challenge in the state of South Carolina, and one of the biggest in the United States. Although substantial progress has been made in processing and vitrifying high‐level radioactive waste at the Savannah River site, approximately 35 million gallons remains to be treated and dispositioned. In this article, we show the development of a new defoamer for use in the processing of high‐level radioactive waste. The application of the new defoamer is not only more effective at controlling foam but will shorten the batch processing time leading to safer and more efficient processing. This has the potential to help shorten the overall site mission lifetime, saving the federal government hundreds of millions of dollars. The novel aspect of the new defoamer is its effectiveness and stability in the harsh conditions needed for processing high‐level radioactive waste: high temperatures, pH 4–13, strong oxidizing and reducing agents, and numerous metal catalysts. The defoamer will replace an existing antifoam agent that decomposes to form multiple flammable gases. Because the existing antifoam agent decomposes quickly, processing changes increased processing time. Statement of novelty We demonstrate that a new defoamer has been developed for use in processing high‐level radioactive waste. This novel defoamer is effective and stable in the harsh processing conditions with no detectable flammable by‐products. Because the existing antifoam agent decomposes quickly, processing changes, including lowering acid addition rates and evaporation rates, increased processing time. The new defoamer is not only more effective at controlling foam but will shorten the batch processing time and lead to safer and more efficient processing by eliminating the production of flammable gases. Statement of industrial relevance Foaming is of great concern in many industrial processes involving three‐phase gas/liquid/fine‐solids systems, like in water evaporation, mineral floatation, air sparging in situ remediation techniques, and in those found in the paper industry.

Lambert, Dan P.↗

Stochastic growth logistic model with aftereffect for batch fermentation process

In this paper, the stochastic growth logistic model with aftereffect for the cell growth of C. acetobutylicum P262 and Luedeking-Piret equations for solvent production in batch fermentation system is introduced. The parameters values of the mathematical models are estimated via Levenberg-Marquardt optimization method of non-linear least squares. We apply Milstein scheme for solving the stochastic models numerically. The effciency of mathematical models is measured by comparing the simulated result and the experimental data of the microbial growth and solvent production in batch system. Low values of Root Mean-Square Error (RMSE) of stochastic models with aftereffect indicate good fits.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Evaluation of no-MST operations in the SRS ARP for Hanford LAWPS

The Savannah River Site (SRS) Actinide Removal Process has been processing salt waste since 2008. This process includes a filtration step in the 512-S facility. Initial operations included the addition, or strike, of monosodium titanate (MST) to remove soluble actinides and strontium. The added MST and any entrained sludge solids were then separated from the supernate by cross flow filtration. During this time, the filter operations have, on many occasions, been the bottleneck process limiting the rate of salt processing. Recently, 512-S- has started operations utilizing “No-MST” where the MST actinide removal strike was not performed and the supernate was simply pre-filtered prior to Cs removal processing. Direct filtration of decanted tank supernate, as demonstrated in 512-S, is the proposed method of operation for the Hanford Low Activity Waste Pretreatment System (LAWPS) facility. Processing decanted supernate without MST solids has been demonstrated for cross flow filtration to provide a significant improvement in production with the SRS Salt Batches 8 and 9 feed chemistries. The average filtration rate for the first 512-S batch processing cycle using No-MST has increased filtrate production by over 35% of the historical average. The increase was sustained for more than double the amount of filtrate batches processed before cleaning of the filter was necessary. While there are differences in the design of the 512-S and Hanford filter systems, the 512-S system should provide a reasonable indication of LAWPS filter performance with similar feed properties. Based on the data from the 512-S facility and with favorable feed properties, the LAWPS filter, as currently sized at over twice the size of the 512-S filter (532 square feet filtration area versus 235 square feet), has the potential to provide sustained filtrate production at the upper range of the planned LAWPS production rate of 17 gpm.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of tank 51 sludge samples (HTF-51-17-44/ HTF-51-17-48) in support of sludge batch 10 processing

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The two Tank 51 sludge samples were sampled and delivered to SRNL in May of 2017. These two tank 51 sludge samples were combined into one composite sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids and aluminum hydroxides (gibbsite and boehmite) by x-ray diffraction.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of Tank 51 Sludge Slurry Samples (HTF-51-17-67, -68, -69, -74, -75, and -76) in Support of Sludge Batch 10 Processing

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The six Tank 51 sludge samples were sampled and delivered to SRNL in August of 2017. These six Tank 51 sludge samples, after undergoing physical characterizations which included rheology, weight percent total solid, dissolved solids and density measurements, were combined into one composite Tank 51 sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of Tank 51 Sludge Slurry Samples (HTF-51-17-44/ HTF-51-17-48) in Support of Sludge Batch 10 Processing

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The two Tank 51 sludge samples were sampled and delivered to SRNL in May of 2017. These two Tank 51 sludge samples were combined into one composite sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids and aluminum hydroxides (gibbsite and boehmite) by x-ray diffraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Low-cost polycrystalline process for solar cells

Economical batch process includes resolidification step to improve conversion efficiency. Experimental models made by process vary in conversion efficiency from 1.4 to more than 6 percent.

Chu, T. L.↗

Towards Automating Spacecraft Attitude Sensor Calibration

With a view towards reducing cost and complexity for spacecraft early mission support at the NASA Goddard Space Flight Center (GSFC), efforts are being made to automate the attitude sensor calibration process. This paper addresses one of the major components needed by such a system. The beneficiaries of an improved calibration process are missions that demand moderate to high precision attitude knowledge or that need to perform accurate attitude slews. Improved slew accuracy reduces the time needed for re-acquisition of fine-pointing after each attitude maneuver, Rapid target acquisition can be very important for astronomical targeting or for off-nadir surface feature targeting by Earth-oriented spacecraft. The normal sequence of on-orbit calibration starts with alignment calibration of the star trackers and possibly the Sun sensor. Their relative alignment needs to be determined using a sufficiently large data set so their fields of view are adequately sampled. Next, the inertial reference unit (IRU) is calibrated for corrections to its alignment and scale factors. The IRU biases are estimated continuously by the onboard attitude control system, but the IRU alignment and scale factors are usually determined on the ground using a batch-processing method on a data set that includes several slews sufficient to give full observability of all the IRU calibration parameters. Finally, magnetometer biases, alignment, and its coupling to the magnetic torquers are determined in order io improve momentum management and occasionally for use in the attitude determination system. The detailed approach used for automating calibrations will depend on whether the automated system resides on the ground or on the spacecraft with an ultimate goal of autonomous calibration. Current efforts focus on a ground-based system driving subsystems that could run either on the ground or onboard. The distinction is that onboard calibration should process the data sequentially rather than in a single large batch since onboard computer data storage is limited. Very good batch- processing calibration utilities have been developed and used extensively at NASA/GSFC for mission support but no sequential calibration utilities are available. To meet this need, this paper presents the mathematical description of a sequential IRU calibration system. The system has been tested using flight data from the Rossi X-ray Timing Explorer (RXTE) during a series of attitude slews. The paper also discusses the current state of the overall automated system and describes plans for adding sequential alignment calibration and other additions that will reduce the amount of analyst time and input.

Sedlak, Joseph↗

Using the scanning electron microscope on the production line to assure quality semiconductors

The use of the scanning electron microscope to detect metallization defects introduced during batch processing of semiconductor devices is discussed. A method of determining metallization integrity was developed which culminates in a procurement specification using the scanning microscope on the production line as a quality control tool. Batch process control of the metallization operation is monitored early in the manufacturing cycle.

Adolphsen, J. W.↗

Microfluidic, One-Batch Synthesis of Pd Nanocrystals on N-Doped Carbon in Surfactant-Free Deep Eutectic Solvents for Formic Acid Electrochemical Oxidation

One of the grand challenges that impedes practical applications of nanomaterials is the lack of robust manufacturing methods that are scalable, cheap, and environmentally friendly. In this work, we address this challenge by developing a microfluidic approach that produces surfactant-free Pd nanocrystals (NCs) uniformly loaded on N-doped porous carbon in a one-batch process. The deep eutectic solvent (DES) prepared from choline chloride and ethylene glycol was employed as a novel synthesis solvent, and its extended hydrogen networks and abundant ionic species effectively stabilize Pd facets and confine nanocrystal sizes without using surfactants. The microreactors provide faster heat exchange and more uniform mass transport, which in combination with DES produced Pd NCs with better-defined shape and predominately exposed Pd (100) facet. Furthermore, we describe that the N-doped functional groups in porous carbon direct dense and uniform heterogeneous growth of Pd NCs in a one-batch process, thereby eliminating a separate catalyst deposition step that is often involved in conventional synthesis. The Pd NCs in the one-batch-produced Pd/C catalysts exhibited a size distribution of similar to ~13 ± 3.5 nm and a high ESCA of 46.0 m 2 /g and delivered 362 mA/mg for formic acid electrochemical oxidation with improved stability, demonstrating the unique potentials of microfluidic reactors and DES for the controllable and scalable synthesis of electrocatalyst materials for practical applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Scalable continuous flow synthesis of ZnO nanorod arrays in 3-D ceramic honeycomb substrates for low-temperature desulfurization

Scalable and cost-effective synthesis and assembly of technologically important nanostructures in three-dimensional (3D) substrates hold keys to bridge the demonstrated nanotechnologies in academia with industrially relevant scalable manufacturing. In this paper, using ZnO nanorod arrays as an example, a hydrothermal-based continuous flow synthesis (CFS) method is successfully used to integrate the nano-arrays in multi-channeled monolithic cordierite. Compared to the batch process, CFS enhances the average growth rate of nano-arrays by 125%, with the average length increasing from 2 μm to 4.5 μm within the same growth time of 4 hours. The precursor utilization efficiency of CFS is enhanced by 9 times compared to that of batch process by preserving the majority of precursors in recyclable solution. Computational fluid dynamic simulation suggests a steady-state solution flow and mass transport inside the channels of honeycomb substrates, giving rise to steady and consecutive growth of ZnO nano-arrays with an average length of 10 μm in 12 h. The monolithic ZnO nano-array-integrated cordierite obtained through CFS shows enhanced low-temperature (200 °C) desulfurization capacity and recyclability in comparison to ZnO powder wash-coated cordierite. This can be attributed to exposed ZnO {101¯0} planes, better dispersion and stronger interactions between sorbent and reactant in the ZnO nanorod arrays, as well as the sintering-resistance of nano-array configurations during sulfidation–regeneration cycles. Finally, with the demonstrated scalable synthesis and desulfurization performance of ZnO nano-arrays, a promising, industrially relevant integration strategy is provided to fabricate metal oxide nano-array-based monolithic devices for various environmental and energy applications.

36 MATERIALS SCIENCE↗

Continuous Water Quality Sensing for FGD Wastewater

The coal fired plant power industry requires new solutions for on-line monitoring of flue gas desulfurization (FGD) wastewaters for regulated trace metals to reduce recurring operating and off-site laboratory analysis costs and provide a high level of confidence of compliance with state and federal discharge guidelines. The University of Alabama at Birmingham (UAB) developed an integrated water sensor package for continuous water quality monitoring of flue gas desulfurization (FGD) wastewaters for concentration measurements of Selenium (Se). UAB utilized a diverse team of University Professors/Staff Members/Student(s) (Engineering and Innovative Technology Development Group), a University Affiliated Research Institution from the local area (Southern Research), and a cost sharing Industry Partner (Metrohm). The team developed and validated a proprietary wet chemistry batch process for water sample preparation; and implemented this process as a fully automated on-line monitor prototype system. This prototype system’s performance was evaluated in both the laboratory and during in-field deployment to a coal fired power plant. In both environments it was found that the prototype system was unable to recreate the batch process’s success at preparing FGD water samples for total Se measurements with a commercial-off-the-shelf (COTS) cyclic anodic stripping voltammetry (CSV) system. Through this experience, UAB has provided insight into a number of specific areas where improvements can be made with respect to the COTS systems used in this project to yield a more complete and competitive industry solution for on-line monitoring of total Se in industrial wastewater.

20 FOSSIL-FUELED POWER PLANTS↗