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DOE OSTI2025

Pulsed contact glow discharge electrification for online material quantification

Real-time elemental analysis of liquids in extreme environments remains a significant challenge for sensor development, particularly in applications such as advanced nuclear reactors. Plasma-based optical emission spectroscopy offers a promising solution. In this study, we investigate pulsed contact glow discharge electrolysis (CGDE) as an alternative plasma generation method for emission-based material quantification. Using aqueous NaCl solutions, we examine the role of discharge polarity on plasma behavior, emission characteristics, and spectral output. Our results demonstrate that cathodic discharges generate more energetic plasmas, enabling the detection of ionic species such as cerium, while anodic discharges favor atomic emission. These findings reveal a potential dual-mode sensing capability controlled by circuit configuration rather than hardware changes. Through synchronized measurements of emission, current, bubble, and spectral dynamics, we present a model in which electron emission and ohmic heating drive plasma formation. This model enhances our understanding of pulsed-CGDE and supports its potential as a versatile, adaptable platform for future deployment in high-temperature liquids such as molten salts.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

DOE OSTI2021

Improved Glow Discharge Polymer Removal from Beryllium Capsules Using Ozone

Copper-doped beryllium spheres are an attractive ablator for inertial confinement fusion experiments. Beryllium spheres are made by sputtering beryllium onto spherical plastic mandrels which must then be removed through a hole that is laser drilled through the shell wall. The currently used mandrel material is glow discharge polymer. This material cannot be removed by solvent and must be “burned” out. The burnout process was originally performed by etching with dry air at 425°C, but this process can substantially roughen the inner surface, which can seed instabilities and increase mix during implosion experiments. In this paper, we explore the use of pure oxygen and ozone to reduce process temperature and improve inner and outer surface quality.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2000

Inception of Snapover and Gas Induced Glow Discharges

Ground based experiments of the snapover phenomenon were conducted in the large vertical simulation chamber at the Glenn Research Center (GRC) Plasma Interaction Facility (PIF). Two Penning sources provided both argon and xenon plasmas for the experiments. The sources were used to simulate a variety of ionospheric densities pertaining to a spacecraft in a Low Earth Orbital (LEO) environment. Secondary electron emission is believed responsible for dielectric surface charging, and all subsequent snapover phenomena observed. Voltage sweeps of conductor potentials versus collected current were recorded in order to examine the specific charging history of each sample. The average time constant for sample charging was estimated between 25 and 50 seconds for all samples. It appears that current drops off by approximately a factor of 3 over the charging time of the sample. All samples charged in the forward and reverse bias directions, demonstrated hysteresis. Current jumps were only observed in the forward or positive swept voltage direction. There is large dispersion in tile critical snapover potential when repeating sweeps on any one sample. The current ratio for the first snapover region jumps between 2 and 4.6 times, with a standard deviation less than 1.6. Two of the samples showed even larger current ratios. It is believed the second large snapover region is due to sample outgassing. Under certain preset conditions, namely at the higher neutral gas background pressures, a perceptible blue-green glow was observed around the conductor. The glow is believed to be a result of secondary electrons undergoing collisions with an expelled tenuous cloud of gas, that is outgassed from the sample. Spectroscopic measurements of the glow discharge were made in an attempt to identify specific lines contributing to the observed glow.

Galofaro, J. T.↗

DOE OSTI2023

HCOO - aq Degradation in Droplets by OH aq in an Atmospheric Pressure Glow Discharge

Plasmas in contact with liquids can degrade organic molecules in solution, as reactive oxygen and nitrogen species produced in the plasma solvate into the liquid. Immersing small droplets (tens of microns in diameter) in the plasma can more rapidly activate the liquid compared to treating a large volume of liquid with a smaller surface-to-volume ratio. The interactions between a radio frequency glow discharge sustained in He/H 2 O and a water droplet containing formate (HCOO - aq ) immersed in and flowing through the plasma were modeled using a 0-dimensional global plasma chemistry model to investigate these activation processes. HCOO - aq interacts with OH aq , produced from solvation of OH from the gas phase. HCOO - aq concentrations were benchmarked with previously reported experimental measurements. The diameter of the droplet, initial HCOO - aq concentration, and gas flow rate affect only the HCOO - aq concentration and OH aq density, leaving the OH density in the gas phase unaffected. Power deposition and gas mixture (e.g., percentage of H 2 O) change both the gas and liquid phase chemistry. A general trend was observed – during the first portion of droplet exposure to the plasma, OH aq primarily consumes HCOO - aq . However, O2 - aq , a byproduct of HCOO - aq consumption, consumes OH aq once O2 - aq reaches a critically large density. Using HCOO - aq as a surrogate for OH aq sensitive contaminants, combinations of residence time, droplet diameter, water vapor density, and power will determine the optimum remediation strategy.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Complete resolution across the neodymium/samarium isotopic envelope with a liquid sampling‐atmospheric pressure glow discharge — Orbitrap mass spectrometer

Rationale Nd and Sm isotope ratios play an important role in geological dating and as nuclear forensic signatures; however, the overlap of the respective 144, 148, 150 Nd/Sm isobars requires prior separations to be performed before analysis on typical MS platforms. The work presented here overcomes these isobaric interferences using ultrahigh‐mass resolution to alleviate interference without prior chemical separations. Methods A liquid sampling‐atmospheric pressure glow discharge ion source was coupled to a standard, QExactive Focus Orbitrap mass spectrometer, providing a mass resolution of ~80 k. A Spectroswiss FTMS booster X2 data acquisition package was used to collect extended transients, providing much higher mass resolution; ~230 k and ~600 k are employed here for Nd and Sm isotopes. Results While the standard Orbitrap resolution is far greater than typical “atomic” MS platforms, it was insufficient to alleviate all isobars. The use of a resolution of ~230 k resulted in baseline separation across the entire isotopic envelope for both Nd and Sm. Isotope ratios obtained from Nd:Sm mixtures using high‐resolution were equivalent to those found for individual‐element solutions, while isotope ratios obtained at a resolution of ~80 k (standard for the OEM data system) showed large deviations. Conclusions Use of ultrahigh‐resolution is an attractive alternative to extensive chemical separations to alleviate severe isobaric interferences. Sufficient mass resolution greatly reduces/eliminates the need for sample manipulations (separations) before analysis while reducing costs and total analysis times.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Parametric optimization of the liquid sampling-atmospheric pressure glow discharge ionization source coupled to an Orbitrap mass spectrometer for neodymium isotope ratio determinations

Isotope ratio determinations are a valuable tool in several application areas. In nuclear forensics, the isotope ratios of uranium and plutonium are commonly used as a signature for the nuclear material's provenance and processing history. However, signatures from other coexisting elements, such as neodymium and samarium, can offer additional insights. Here, the liquid sampling-atmospheric pressure glow discharge (LS-APGD) ionization source coupled to an Orbitrap mass spectrometer (MS) has demonstrated its utility for actinide measurements. This instrumental platform can leverage the high resolution offered by the Orbitrap MS to overcome potential isobaric interferences, such as 144 Nd- 144 Sm, 148 Nd- 148 Sm, and 150 Nd- 150 Sm pairs. The work presented herein demonstrates the rapid, accurate, and precise determination of the isotope ratios for neodymium using the LS-APGD/Orbitrap MS. Both the LS-APGD and Orbitrap MS parameters were optimized systematically, with NdO + found to be the most abundant, most reduced species after applying the optimal collision-induced dissociation modalities. A limit of detection of 3 pg of 142 Nd was achieved when data was acquired and processed using the FTMS Booster, an external data acquisition and processing system offered by Spectroswiss. Excellent accuracy of better than 99 % and precision of <1 % RSD were achieved when a solution of the well-characterized neodymium standard (JNdi-1 standard) was analyzed under the optimized condition, indicating the LS-APGD/Orbitrap's great potential for isotope ratio analysis of Nd and other REEs for diverse applications.

47 OTHER INSTRUMENTATION↗

NASA NTRS2005

Impurity Studies of Cd(0.8)Zn(0.2)Te Crystals Using Photoluminescence and Glow Discharge Mass Spectroscopy

Cd(1-x)Zn(x)Te semiconductor crystal is a highly promising material for room temperature x- and gamma-ray detector applications because of its high resistivity, long carrier lifetime, and relatively high hole and electron mobilities. This paper reports the investigation of the impurities in several Cd(1-x)Zn(x)Te (x = 0.20) crystals grown using the vertical Bridgman method under a Cd overpressure. The impurity concentrations were measured using glow discharge mass spectroscopy (GDMS). The energy states of the impurities were studied using photoluminescence (PL) spectroscopy at liquid helium temperature. The PL spectra showed a series of sharp high energy lines which are associated with free excitons and excitons bound to impurities as donors and acceptors in the crystals. The impurities also contributed to donor-acceptor pair recombination. The correlation between the GDMS and PL results will be reported.

Su, Ching-Hua↗

NASA NTRS2005

Application of Glow Discharge Plasma to Alter Surface Properties of Materials

Some polymer materials that are considered important for spaceport operations are rendered noncompliant when subjected to the Kennedy Space Center (KSC) Standard electrostatic testing. These materials operate in stringent environmental conditions, such as high humidity. Treating materials that fail electrostatic testing and altering their surface properties so that they become compliant would result in considerable cost savings. Significant improvement in electrostatic dissipation of Saf-T-Vu PVC after treatment with air Atmospheric Plasma Glow Discharge (APGD) was observed and the material now passed the KSC electrostatic test. The O:C ratio on the surface, as monitored by X-ray Photoelectron Spectroscopy, increased from 0.165 tO 0.275 indicating enhanced oxidation, and surface contact angle measurements decreased from 107.5 to 72.6 showing increased hydrophilicity that accounted for the increased conductivity. Monitoring of the aging showed that the materials hydrophobic recovery resulted in it failing the electrostatic test 30 hours after treatment. This was probably due to the out-diffusion of the added Zn, Ba, and Cd salt stabilizers detected on the surface and/or diffusion of low molecular weight oligomers. On going work includes improving the long term hydrophilicity by optimizing the APGD process with different gas mixtures. Treatment of other spaceport materials is also presented.

Trigwell, Steve↗

DOE OSTI2023

Coupling of the Liquid Sampling–Atmospheric Pressure Glow Discharge to Orbitrap Mass Analyzers for Uranium Isotope Ratio Analysis: Evolution of the Methodology and Implications to the Field

Just over a decade ago, a truly outside-of-the-box approach to isotope ratio mass spectrometry (IRMS) was undertaken between research groups at Clemson University and the Pacific Northwest National Laboratory. The original motivation dealt with projections as to whether or not microplasmas could be developed into practical elemental ionization sources, perhaps for transportable analysis applications. In particular, the use of the liquid sampling–atmospheric pressure glow discharge (LS-APGD) was pursued. Its interfacing to an ultra-high resolution Orbitrap platform, proved not only facile, but opened up a wealth of potential applications. Here, we lay out a historical, tutorial description of the interfacing and the evolution of the methodology regarding IRMS of uranium. Practical challenges and opportunities are described, which hopefully provide guidance to further applications in high resolution IRMS. It is hoped that, while detailed and lengthy, the didactic nature of the presentation provides experimental insights and tips, and also serves as an homage to our very good friend, Professor Gary M. Hieftje, whose scientific inspiration and comradery have been immeasurably important in our own careers.

Koppenaal, David W.↗

NASA NTRS2004

Glow Discharge Plasma Demonstrated for Separation Control in the Low-Pressure Turbine

Flow separation in the low-pressure turbine (LPT) is a major barrier that limits further improvements of aerodynamic designs of turbine airfoils. The separation is responsible for performance degradation, and it prevents the design of highly loaded airfoils. The separation can be delayed, reduced, or eliminated completely if flow control techniques are used. Successful flow control technology will enable breakthrough improvements in gas turbine performance and design. The focus of this research project was the development and experimental demonstration of active separation control using glow discharge plasma (GDP) actuators in flow conditions simulating the LPT. The separation delay was shown to be successful, laying the foundation for further development of the technologies to practical application in the LPT. In a fluid mechanics context, the term "flow control" means a technology by which a very small input results in a very large effect on the flow. In this project, the interest is to eliminate or delay flow separation on LPT airfoils by using an active flow control approach, in which disturbances are dynamically inserted into the flow, they interact with the flow, and they delay separation. The disturbances can be inserted using a localized, externally powered, actuating device, examples are acoustic, pneumatic, or mechanical devices that generate vibrations, flow oscillations, or pulses. A variety of flow control devices have been demonstrated in recent years in the context of the external aerodynamics of aircraft wings and airframes, where the incoming flow is quiescent or of a very low turbulence level. However, the flow conditions in the LPT are significantly different because there are high levels of disturbances in the incoming flow that are characterized by high free-stream turbulence intensity. In addition, the Reynolds number, which characterizes the viscous forces in the flow and is related to the flow speed, is very low in the LPT passages.

Ashpis, David e.↗

DOE OSTI2023

The transport dynamics of tens of micrometer-sized water droplets in RF atmospheric pressure glow discharges

Abstract Charging of particles having diameters of tens of microns has been extensively studied at atmospheric pressure in the context of, for example, electrostatic precipitators where the focus was on unipolar charging. The ambipolar charging of particles in atmospheric pressure plasmas, and of droplets in particular, has received less attention. The plasma activation of droplets is of interest for water purification, fertilizer production and materials synthesis, all of which depend on the transport of the droplets through the plasma, which in turn depends on their charging. In this paper, we report on the transport dynamics of water droplets, tens of microns in diameter, carried by the gas flow through an atmospheric pressure radiofrequency glow discharge sustained in helium. The droplets pass through the plasma with minimal evaporation and without reaching the Rayleigh limit. The droplet trajectory in the presence and absence of the plasma provides insights on the forces acting on the droplet. The measurements were analyzed using results from a three-dimensional fluid model and a two-dimensional plasma hydrodynamics model. We found that the transport dynamics as the droplet enters and leaves the plasma are due to differential charging of the droplet in the plasma gradients of the bounding sheaths to the plasma.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1998

Enhanced Glow Discharge Production of Oxygen

Studies starting in late seventies have shown Mars atmosphere can be used as a feedstock for oxygen production using simple chemical processing systems during early phases of the Mars exploration program. This approach has been recognized as one of the most important in-situ resource utilization (ISRU) concepts for enabling future round trip Mars missions. It was determined a decade ago that separation of oxygen can be accomplished efficiently by permeation through a silver membrane at temperatures well below 1000 K. This process involves adsorption of atomic oxygen on the surface and its subsequent diffusion through a silver lattice via an oxygen concentration gradient. We have determined recently that glow discharge can be used to liberate atomic oxygen from Mars atmosphere and that the oxygen can be collected through a silver permeation membrane. Recently, we demonstrated a substantial increase in energy efficiency of the process by applying a radio frequency discharge in combination with a silver permeation membrane. The experiments were performed using pure carbon dioxide in the pressure range equal to Mars surface conditions. Energy efficiency was defined as the ratio of the energy required to dissociate a unit mass of oxygen from carbon dioxide to the (electrical) energy consumed by the overall system during the dissociation and collection process. The research effort, started at NASA Langley Research Center, continued with this project. Oxygen production apparatus, built and operated under the research grant NAG1-1140 was relocated to the Atomic Beams Laboratory at ODU in July 1996, being since then in fall operation.

Ash, Robert↗

NASA NTRS2006

Use of Atmospheric Glow Discharge Plasma to Modify Spaceport Materials

Numerous materials used in spaceport operations require stringent evaluation before they can be utilized. It is critical for insulative polymeric materials that any surface charge be dissipated as rapidly as possible to avoid Electrostatic Discharges (ESD) that could present a danger. All materials must pass the Kennedy Space Center (KSC) standard electrostatic test [1]; however several materials that are considered favorable for Space Shuttle and International Space Station use have failed. Moreover, to minimize contamination of Mars spacecraft, spacecraft are assembled under cleanroom conditions and specific cleaning and sterilizing procedures are required for all materials. However, surface characteristics of these materials may allow microbes to survive by protecting them from sterilization and cleaning techniques. In this study, an Atmospheric Pressure Glow Discharge Plasma (APGD) [2] was used to modify the surface of several materials. This allowed the materials surface to be modified in terms of hydrophilicity, roughness, and conductivity without affecting the bulk properties. The objectives of this study were to alter the surface properties of polymers for improved electrostatic dissipation characteristics, and to determine whether the consequent surface modification on spaceport materials enhanced or diminished microbial survival.

Trigwell, S.↗

DOE OSTI2026

Single-Particle Isotopic Analysis Using the Liquid Sampling-Atmospheric Pressure Glow Discharge Microplasma Coupled to an Orbitrap Mass Spectrometer

Isotope ratio (IR) determinations on individual particles can provide valuable information relative to the sample, including processing and dating, which could be valuable to geological and nuclear material analysis communities. In comparison to “bulk” measurements, in which all particle information is lost and homogenized within a sample, “particle” measurements allow for fingerprinting and can provide unique insights related to the sample’s nano- and micro- compositions. Furthermore, the complex nature of particles, with potential isobaric interferences from either the matrix or other elements within the same particle, poses a significant analytical challenge for conventional mass spectrometry platforms employed for elemental analysis due to their limited mass resolution. Presented here is the first demonstration of an ultrahigh resolution method for single particle (SP) isotopic analysis using the liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma ionization source coupled to an Orbitrap mass spectrometer and FTMS Booster X2T acquisition/processing system. For proof of concept, well-characterized CeO 2 microparticles with a nominal diameter of 1.0 μm were analyzed at a mass resolution of ∼330,000. Important instrumental parameters were optimized to enable the detection of single particles. The 142 Ce/ 140 Ce ratio of individual particles and the population average were determined and compared to an SP inductively coupled plasma time-of-flight mass spectrometry (ICP-TOF-MS) analysis. The isotopic accuracy and precision were determined by two methods and found to be in good agreement with the SP-ICP-TOF-MS method, with the linear regression slope method providing a more accurate ratio, showing a ∼1.4% relative difference from the ratio determined from a particle digest. The encouraging performance of the method was further supported by a determined detection limit of 2.9 fg ( 142 Ce). The developed method is anticipated to overcome many of the challenges posed by isobaric interferences encountered in conventional mass spectrometry techniques when analyzing real-world samples for particle isotopic composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Striations in moderate pressure dc driven nitrogen glow discharge

Plasma stratification has been studied for more than a century. Despite the many experimental studies reported on this topic, theoretical analyses and numerical modeling of this phenomenon have been mostly limited to rare gases. In this work, a one-dimensional fluid model with detailed kinetics of electrons and vibrationally excited molecules is employed to simulate moderate-pressure (i.e. a few Torrs) dc discharge in nitrogen in a 15.5 cm long tube of radius 0.55 cm. The model also considers ambipolar diffusion to account for the radial loss of ions and electrons to the wall. The proposed model predicts self-excited standing striations in nitrogen for a range of discharge currents. The impact of electron transport parameters and reaction rates obtained from a solution of local two-term and a multi-term Boltzmann equation on the predictions are assessed. In-depth kinetic analysis indicates that the striations result from the undulations in electron temperature caused due to the interaction between ionization and vibrational reactions. Furthermore, the vibrationally excited molecules associated with the lower energy levels are found to influence nitrogen plasma stratification and the striation pattern strongly. A balance between ionization processes and electron energy transport allows the formation of the observed standing striations. Simulations were conducted for a range of discharge current densities from ~0.018 to 0.080 mA cm –2 , for an operating pressure of 0.7 Torr. Parametric studies show that the striation length decreases with increasing discharge current. Furthermore, the predictions from the model are compared against experimental measurements and are found to agree favorably.

42 ENGINEERING↗

DOE OSTI2022

Self-organized patterns at the plasma–liquid anode interface in a helium glow discharge: temporal development and mechanisms

Self-organization at the plasma–liquid anode interface is a commonly observed phenomenon for atmospheric pressure glow plasmas, resulting in patterns with distinctive shapes such as circular ring, star-shaped, and gear-like structures, depending primarily on the discharge current and solution conductivity. Recent studies have shown that the electrode gap distance, solute used for liquid anode solution, and gas composition can also significantly impact pattern formation. Nonetheless, an overarching model or explanation of the key underlying mechanisms consistent with all experimentally observed trends is not yet reported. We propose a key underlying mechanism enabling pattern formation motivated by a detailed parametric study of pattern formation complemented by the temporal development of patterns and consistent with all observed trends. Pattern formation was observed to be on a time scale of 100 μs, similar to the time scales of gas heating and evaporation. It was found that a minimum water evaporation rate of (3.5 ± 0.5) × 10 –6 kg s –1 and reduced electric field in the positive column of 16.6 ± 0.4 Td is required for pattern formation in the investigated cases irrespective of solution conductivity and gas composition for NaCl solutions. Nonetheless, the presence of cations for which the corresponding metal atom has a low ionization energy was identified as a necessary condition for pattern formation. Furthermore, the reported results suggest that the presence of a small amount of metal atoms in the gas phase with low ionization energy enhances the overall ionization rate in the near anode region which triggers pattern formation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Liquid-to-gas transfer of sodium in a liquid cathode glow discharge

Abstract Plasma-liquid interactions have been extensively studied with a focus on the transport of reactive species from the plasma to the liquid phase and their induced liquid phase chemistry and resulting applications. While solute transfer from the liquid to the gas phase in plasmas has been widely used in analytical chemistry, the underlying processes remain relatively unexplored. We report spatially and temporally resolved absolute density measurements of sodium in a plasma with a NaCl solution cathode using two-photon absorption laser induced fluorescence (TaLIF). The observed non-linear increase in sodium density with solution conductivity is shown to correlate with droplet generation as visualized by Mie scattering. The findings are explained by droplet generation by electrospray induced by Taylor cone formation as underpinning mechanism for the introduction of sodium in the plasma. An analytical sheath model combined with a scaling law shows an increase in electric field force with solution conductivity that is consistent with the observed non-linear increase in sodium density in the plasma with solution conductivity.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

Townsend to glow discharge transition for a nanosecond pulse plasma in helium: space charge formation and resulting electric field dynamics

Stark polarization spectroscopy is used to investigate the temporal evolution of the electric field distribution in the cathode region of a nanosecond pulsed discharge in helium at 120 Torr. The measurements are performed on the He I transition at 492.19 nm, during the early stages of the discharge formation. The experimental results are compared with the predictions of a 1D fluid model. Time-resolved ICCD images show that the discharge develops as a diffuse, cathode-directed ionization wave with a Townsend-like feature before transitioning into a glow-like structure. Near anode instabilities characterized by filament formation were observed near the high voltage electrode. Within 30 ns, a reduction of the sheath thickness to about 250 μm is observed, coinciding with a gradual increase of the discharge current and proportional increase in electric field at the cathode. Additionally, the cathode electric field corresponding to this sheath with a thickness of 250 μm is about 40 kV cm -1 . A subsequent steep increase of the discharge current leads to a further reduction of the sheath width. The electric field evolution as obtained by the fluid model is in excellent agreement with the measurements and shows that an enhanced ionization near the cathode is causing the space charge formation responsible for the increase in electric field.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗