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At least 127 records · Page 7

A Progress Report for a 44-month Aging Study on Nitroplasticizer (NP) Stability - Summary of DFT and FTIR Results

In the past few years, a 44-month long aging experiment was conducted under various aging conditions. The properties of aged nitroplasticizer (NP) samples were analyzed using Fourier transform infrared spectroscopy, Karl Fischer (KF) titration, thermogravimetric analysis (TGA), liquid chromatography tandem quadrupole time of flight mass spectrometry (LC/QTOF), and ion chromatography (IC). In this progress report, some FTIR results are documented and discussed. On the theoretical front, density functional theory (DFT) calculations were carried out. Some DFT results are discussed as well.

36 MATERIALS SCIENCE↗

Molten Salt Loop Testing of Sensors and Off-Gas Components: FY23 progress

The Liquid Salt Test Loop (LSTL) at the US Department of Energy’s (DOE’s) Oak Ridge National Laboratory (ORNL) was developed to demonstrate technology for high-temperature fluoride salt systems (Figure 1). The LSTL is primarily constructed using Inconel 600 alloy and operates at temperatures of up to 700°C. The facility is loaded with 165 kg of LiF-NaF-KF salt (FLiNaK). This salt provides a relevant test environment for de-risking technology while avoiding the costs and hazards associated with beryllium-based or uranium-bearing salts. FLiNaK is also an advantageous salt for the secondary side of molten salt reactors. The facility’s major components include a centrifugal pump for salt circulation, an air-based heat exchanger to reject heat, a suite of instrumentation, and trace heating to prevent salt freezing. Additional heating is available through an induction heater rated at 200 kW. The relatively large heating and cooling capability enables the formation of a temperature gradient across the loop (i.e., a hot and a cold side), which is important for chemistry and corrosion studies. The LSTL is a unique US capability for high-temperature molten halide salt testing. Although some efforts are underway at universities, the LSTL’s scale, co-located purification system, and relatively large power differentiates it from other testing systems. Furthermore, unlike efforts within industry, access to the DOE-supported facility and communication of results, which are generally disseminated publicly, result in a broad significance in the molten salt reactor community.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Molten Salt Loop Operational Experience and Test Campaigns in FY24

The Facility to Alleviate Salt Technology Risks (FASTR) at the US Department of Energy (DOE) Oak Ridge National Laboratory (ORNL) was developed to demonstrate technology for high-temperature chloride salt systems (Figure 1). FASTR is primarily constructed using alloy C-276 and is designed to operate at temperatures of up to 725°C. The facility is loaded with 250 kg of NaCl-KCl-MgCl 2 salt. This salt provides a relevant test environment for de-risking technology while avoiding the costs and hazards associated with beryllium-based or uranium-bearing salts. The facility’s major components include a centrifugal pump for salt circulation, an air-based heat exchanger to reject heat, a suite of instrumentation, and trace heating to prevent salt freezing. The salt was purified in 2020 and 2022, and the pumped loop first operated in December 2022. FASTR is a unique US capability for high-temperature molten halide salt testing. FASTR’s scale, co located purification system, and relatively large power (465 kW) differentiates it from other testing systems. Furthermore, access to the DOE-supported facility and efficient communication of results— which are generally disseminated publicly—distinguish FASTR as being broadly significant throughout the molten salt reactor community. FASTR is similar to ORNL’s Liquid Salt Test Loop (LSTL), although FASTR contains chloride-based salt instead of the fluoride-based salt (LiF-NaF-KF) found in LSTL. Furthermore, FASTR is approximately 2× larger than LSTL in terms of pipe size and length, power, salt volume, flow rate, and number of thermocouples. The LSTL first operated in 2016. At the end of FY23, there was a suspected gas leak in the LSTL that halted operation. At the start of FY24, a leak in the LSTL pump’s tank gas space was confirmed. Because the gas-space leak prevented operation of LSTL, FY24 efforts were focused on operation of FASTR. This report summarizes the progress made during FY24 in support of the DOE Office of Nuclear Energy (DOE-NE) work package, AT-24OR070202 Salt Loop and Capability for Testing Sensors and Off Gas Components.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Fluoride Analysis by Ion Chromatography in Support of Fast Critical Assembly (FCA) Spent Nuclear Fuel Processing

INTRODUCTION The Savannah River Site (SRS) is currently processing Fast Critical Assembly (FCA) fuel received from the Japan Atomic Energy Agency (JAEA) for disposition. Stainless steel-clad plate and rods in stainless steel containers are dissolved using electrolysis with a solution mixture of nitric acid (HNO3), potassium fluoride (KF), and gadolinium (Gd). An ion chromatography (IC) was developed and vetted to monitor fluoride at various sampling points of the process. To finalize the method, FCA test solution was analyzed to qualify the analytical method followed by real FCA process solution analysis using two different analytical columns. This presentation summarizes the development and vetting of the IC method.

White, Thomas L. [Savannah River National Laborato↗

Friction and wear of nuclear graphite exposed to molten FLiNaK salt environment

This report formally documents the completion of the Advanced Reactor Technologies Level 3 Milestone (M3TG-25OR0501104), “Initiate graphite wear studies of graphite samples exposed to molten salt environment,” due August 1, 2025. The report summarizes the ongoing activities aimed at characterizing the friction and wear behavior of graphite in molten LiF–NaF–KF (FLiNaK) salt environment. The wear and friction behavior of self-mated ET-10 nuclear graphite were tested at varying temperatures (550°C and 650°C), contact loads (40 and 80 N) and sliding speeds (1 and 10 mm/s) in a controlled argon environment. The results were compared to the wear and friction behavior of the same graphite material in a dry argon environment. This report presents initial studies on the friction and wear behavior of graphite in sliding contact mode, with future work focused on investigating the graphite matrix materials, as well as rolling and impact contact modes. The outcomes of this report could provide insights into assessing the integrity of the graphitic components of pebble-bed fluoride salt–cooled high-temperature reactors (PB-FHRs) to enhance their safe operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Fundamental ignition study for material fire safety improvement, part 2

The autoignition behavior of polymeric compositions in oxidizing media was investigated as well as the nature and relative concentration of the volatiles produced during oxidative decomposition culminating in combustion. The materials investigated were Teflon, Fluorel KF-2140 raw gum and its compounded versions Refset and Ladicote, 45B3 intumenscent paint, and Ames isocyanurate foam. The majority of the tests were conducted using a stagnation burner arrangement which provided a laminar gas flow and allowed the sample block and gas temperatures to be varied independently. The oxidizing atmospheres were essentially air and oxygen, although in the case of the Fluorel family of materials, due to partial blockage of the gas inlet system, some tests were performed unintentionally in enriched air (not oxygen). The 45B3 paint was not amenable to sampling in a dynamic system, due to its highly intumescent nature. Consequently, selected experiments were conducted using a sealed tube technique both in air and oxygen media.

Paciorek, K. L.↗

High energy density capacitors for vacuum operation with a pulsed plasma load

Results of the effort of designing, fabricating, and testing of a 40 joules/lb (88.2 joules/Kg) high voltage energy storage capacitor suitable for operating a pulsed plasma thruster in a vacuum environment for millions of pulses are presented. Using vacuum brazing and heli-arc welding techniques followed by vacuum and high pressure helium leak tests it was possible to produce a hermetically sealed relatively light weight enclosure for the dielectric system. An energy density of 40 joules/lb was realized with a KF-polyvinylidene fluoride dielectric system. One capacitor was D.C. life tested at 4 KV (107.8 joules/lb) for 2,000 hours before it failed. Another exceeded 2,670 hours without failure at 38.3 joules/lb. Pulse life testing in a vacuum exceeded 300,000 discharges with testing still in progress. The D.C. life test data shows a small decrease in capacitance and an increase in dissipation factor with time. Heat transfer from the load to the capacitor must also be considered besides the self-heat generated by the capacitor.

Guman, W. J.↗

A joint fracture toughness evaluation of hot-pressed beryllium

Fracture toughness tests at room temperature were made on three-point bend specimens cut from hot-pressed beryllium obtained from two suppliers. The test specimens had dimensions conforming to ASTM fracture toughness standard E399-72. A total of 42 specimens were machined from each batch of material. Six specimens from each batch were then distributed to seven independent laboratories for testing. The test data from the laboratories were collected and analyzed for differences between the laboratories and the two batches of material. It is concluded that ASTM 399-72 can be used as a valid test procedure for determining the fracture toughness of beryllium, providing that Kf(max) in fatigue cracking could be up to 80 percent of the K(0) value.

Conrad, H.↗

Electrochemical fluorination of trichloroethylene and N, N-dimethyltrifluoroacetamide

Fluorination of trichloroethylene and N, N-dimethyltrifluoroacetamide was carried out on a laboratory scale in an advanced Simons type electrochemical apparatus which could be operated automatically from ambient to 50 psi pressure. A variety of fluorine-substituted products are formed, depending upon electrolysis conditions and concentrations of reactant relative to the NaF, KF, HF electrolyte. A new reaction mechanism of electrochemical fluorination of trichloroethylene is proposed. The solvency-to-fluorine content relationship of fluorinated N, N-dimethyltrifluoroacetamide is described.

Hsu, L. C.↗

Electrochemical fluorination of trichloroethylene and N, N-dimethyltrifluoroacetamide

The paper presents the results of experiments concerning the fluorination of trichloroethylene and N, N-dimethyltrifluoroacetamide carried out on a laboratory scale in an advanced 'Simons' type electrochemical apparatus which could be operated automatically from ambient to 50 psi pressure. It is shown that a variety of fluorine-substituted products are formed, depending upon electrolysis conditions and concentrations of reactant relative to the NaF, KF, HF electrolyte. A new reaction mechanism of electrochemical fluorination of trichloroethylene is proposed. Finally, the solvency-to-fluorine content relationship of fluorinated N, N-dimethyltrifluoroacetamide is described.

Hsu, L.-C.↗

Development of high-speed balancing technology

An investigation into laser material removal showed that laser burns act in a manner typical of mechanical stress raisers causing a reduction in fatigue strength; the fatigue strength is lowered relative to the smooth specimen fatigue strength. Laser-burn zones were studied for four materials: Alloy Steel 4340, Stainless Steel 17-4 PH, Inconel 718, and Aluminum Alloy 6061-T6. Calculations were made of stress concentration factors K, for laser-burn grooves of each material type. A comparison was then made to experimentally determine the fatigue strength reduction factor. These calculations and comparisons indicated that, except for the 17-4 PH material, good agreement (a ratio of close to 1.0) existed between Kt and Kf. The performance of the 17-4 PH material has been attributed to early crack initiation due to the lower fatigue resistance of the soft, unaged laser-affected zone. Also covered in this report is the development, implementation, and testing of an influence coefficient approach to balancing a long, slender shaft under applied-torque conditions. Excellent correlation existed between the analytically predicted results and those data obtained from testing.

Demuth, R.↗

An adaptive tracking observer for failure-detection systems

The design problem of adaptive observers applied to linear, constant and variable parameters, multi-input, multi-output systems, is considered. It is shown that, in order to keep the observer's (or Kalman filter) false-alarm rate (FAR) under a certain specified value, it is necessary to have an acceptable proper matching between the observer (or KF) model and the system parameters. An adaptive observer algorithm is introduced in order to maintain desired system-observer model matching, despite initial mismatching and/or system parameter variations. Only a properly designed adaptive observer is able to detect abrupt changes in the system (actuator, sensor failures, etc.) with adequate reliability and FAR. Conditions for convergence for the adaptive process were obtained, leading to a simple adaptive law (algorithm) with the possibility of an a priori choice of fixed adaptive gains. Simulation results show good tracking performance with small observer output errors and accurate and fast parameter identification, in both deterministic and stochastic cases.

Sidar, M.↗

The application of LQR synthesis techniques to the turboshaft engine control problem

A power turbine governor was designed for a recent-technology turboshaft engine coupled to a modern, articulated rotor system using Linear Quadratic Regulator (LQR) and Kalman Filter (KF) techniques. A linear, state-space model of the engine and rotor system was derived for six engine power settings from flight idle to maximum continuous. An integrator was appended to the fuel flow input to reduce the steady-state governor error to zero. Feedback gains were calculated for the system states at each power setting using the LQR technique. The main rotor tip speed state is not measurable, so a Kalman Filter of the rotor was used to estimate this state. The crossover of the system was increased to 10 rad/s compared to 2 rad/sec for a current governor. Initial computer simulations with a nonlinear engine model indicate a significant decrease in power turbine speed variation with the LQR governor compared to a conventional governor.

Pfeil, W. H.↗

The application of LQR synthesis techniques to the turboshaft engine control problem

A power turbine governor was designed for a recent-technology turboshaft engine coupled to a modern, articulated rotor system using Linear Quadratic Regulator (LQR) and Kalman Filter (KF) techniques. A linear, state-space model of the engine and rotor system was derived for six engine power settings from flight idle to maximum continuous. An integrator was appended to the fuel flow input to reduce the steady-state governor error to zero. Feedback gains were calculated for the system states at each power setting using the LQR technique. The main rotor tip speed state is not measurable, so a Kalman Filter of the rotor was used to estimate this state. The crossover of the system was increased to 10 rad/s compared to 2 rad/sec for a current governor. Initial computer simulations with a nonlinear engine model indicate a significant decrease in power turbine speed variation with the LQR governor compared to a conventional governor.

Pfeil, W. H.↗

Lunar mining of oxygen using fluorine

Experiments during the first year of the project were directed towards generating elemental fluorine via the electrolysis of anhydrous molten fluorides. Na2SiF6 was dissolved in either molten NaBF4 or a eutectic (minimum-melting) mixture of KF-LiF-NaF and electrolyzed between 450 and 600 C to Si metal at the cathode and F2 gas at the anode. Ar gas was continuously passed through the system and F2 was trapped in a KBr furnace. Various anode and cathode materials were investigated. Despite many experimental difficulties, the capability of the process to produce elemental fluorine was demonstrated.

Burt, Donald M.↗

Relativistic Corrections to the Properties of the Alkali Fluorides

Relativistic corrections to the bond lengths, dissociation energies and harmonic frequencies of KF, RbF and CsF have been obtained at the self-consistent field level by dissociating to ions. The relativistic corrections to the bond lengths, harmonic frequencies and dissociation energies to the ions are very small, due to the ionic nature of these molecules and the similarity of the relativistic and nonrelativistic ionic radii.

Dyall, Kenneth G.↗

A Comparison of Cumulus Parameterizations in Idealized Sea-Breeze Simulations

Four cumulus parameterizations in the Penn State-NCAR model MM5 are compared in idealized sea-breeze simulations, with the aim of discovering why they work as they do. The most realistic results appear to be those using the Kain-Fritsch scheme. Rainfall is significantly delayed with the Betts-Miller-Janjic scheme, due to the method of computing the reference sounding. This method can be corrected, but downdrafts should be added in a physically realistic manner. Even without downdrafts, a corrected version of the BMJ scheme produces nearly the same timing and location of deep convection as the KF scheme, despite the very different physics. In order to simulate the correct timing of the rainfall, a minimum amount of mass is required in the layer that is the source of a parameterized updraft. The Grell parameterization, in the present simulation, always derives the updraft from the top of the mixed layer, where vertical advection predominates over horizontal advection in increasing the moist static energy. This makes the application of the quasi-equilibrium closure more correct than it would be if the updrafts were always derived from the most unstable layer, but it evades the question of whether or not horizontal advection generates instability. Using different physics, the parameterizations produce significantly different cloud-top heights.

Cohen, Charles↗

Kinetics of antigen binding to arrays of antibodies in different sized spots

A fluorescence-based array biosensor has been developed which can measure the binding kinetics of an antigen to an immobilized antibody in real time. A patterned array of antibodies immobilized on the surface of a planar waveguide was used to capture a Cy5-labeled antigen present in a solution that was continuously flowed over the surface. The CCD image of the waveguide was monitored continuously for 25 min. The resulting exponential rise in fluorescence signal was determined by image analysis software and fitted to a reaction-limited kinetics model, giving a kf of 3.6 x 10(5) M(-1) s(-1). Different spot sizes were then patterned on the surface of the waveguide using either a PDMS flow cell or laser exposure, producing width sizes ranging from 80 to 1145 microm. It was demonstrated that under flow conditions, the reduction of spot size did not alter the association rate of the antigen with immobilized antibody; however, as the spot width decreased to < 200 nm, the signal intensity also decreased.

Non-NASA Center↗