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A novel multi-electrode glow discharge provides increased sensitivity and analytical flexibility for both atomic and molecular MS determinations.
The Atmospheric Pressure Glow Discharge (APGD) is a relatively simple and versatile plasma source used in a wide range of applications. Active cooling of the cathode can effectively mitigate instabilities, leading to glow-to-arc transitions. This study investigates the effect of varying the degree of cathode cooling in APGD with a planar cathode in helium. The plasma flow model incorporates mass conservation, chemical species transport, momentum conservation, conservation of thermal energy of heavy species and of electrons, and electrostatics. The model is applied to time-dependent simulations through a three-dimensional computational domain describing the whole discharge, without geometric symmetry or steady-state assumptions. Simulations of an experimentally characterized APGD explore the effects of electric current and cathode cooling—ranging from thermally insulated to extreme convective cooling. Results show the formation of an annular region with high electric field over the cathode surface under conditions of high current and low cooling.
The atmospheric pressure glow discharge (APGD) is a relatively simple and versatile plasma source used in diverse applications. Stable APGD operation at high currents, generally a challenge due to instabilities leading to glow-to-arc transition, has been demonstrated using actively-controlled cathodic cooling. This article presents the computational modelling and simulation of a self-sustained direct-current APGD in helium within a 10 mm pin-to-plate inter-electrode gap for currents ranging from 4 to 40 mA. The APGD model is comprised of the conservation equations for total mass, chemical species, momentum, thermal energy of heavy-species and of free electrons, and electric charge. The model equations are discretized using a nonlinear variational multi-scale finite element method that has demonstrated superior accuracy in other plasma flow problems, on a temporal and three-dimensional computational domain suitable to unveil the potential occurrence of instabilities. Modelling results show good agreement with experimental measurements of voltage drop and the same trend but higher values of temperature. The higher temperatures obtained by the simulations appear to be due to the absence of a near-cathode heat dissipation model. Here, the results also reveal that the distribution of electron density and of the ratio of atomic helium ions to total ions transitions from monotonically increasing away from the cathode to presenting a minimum near the centre of the gap with increasing current.
In the Large Helical Device (LHD), boronization is utilized for wall conditioning, employing two distinct methods: glow discharge using diborane gas and the injection of boron powder into the plasma via an impurity powder dropper (IPD). Glow discharge boronization is conducted after maintenance when the vacuum vessel is exposed to air and just before the start of an experimental campaign. In contrast, real-time boronization using the IPD is performed during discharges. The distribution of boron on plasma-facing components was assessed through long-term material probes in the case of glow discharge and through numerical simulations for the IPD method. Results indicated non-uniform boron distributions in both cases. The impact of these boronization techniques on impurity levels and the lifetime of their effects were also examined. Both methods effectively reduced oxygen and iron in the plasma, with the iron impurities originating from the first wall. For glow discharge boronization, the reduction in oxygen levels persisted until the end of the experimental campaign, whereas the reduction in iron levels only lasted a few days. In the case of boron injection during long pulse discharges exceeding 200 s, the suppression of oxygen and iron was observed. The effect on iron quickly diminished within several seconds after the injection ended, whereas the effect on oxygen lasted more than 100 s. The difference in the lifetimes of the boronization effects is further discussed.
Apparatus include an atmospheric pressure glow discharge (APGD) analyte electrode defining an analyte discharge axis into an APGD volume, and a plurality of APGD counter electrodes having respective electrical discharge ends directed to the APGD volume, wherein the APGD analyte electrode and the APGD counter electrodes are configured to produce an APGD plasma in the APGD volume with a voltage difference between the APGD analyte electrode and one or more of the AGPD counter electrodes. An electrode can be integrated into an ion inlet. Apparatus can be configured to perform auto-ignition and/or provide multi-modal operation through selectively powering electrodes. Electrode holder devices are disclosed. Related methods are disclosed.
The liquid sampling-atmospheric pressure glow discharge (LS-APGD) ionization source has proven to be an effective analysis tool for making uranium isotope ratio measurements when coupled to high-resolution mass spectrometers, such as the Orbitrap. While previous studies have shown the capabilities of the LS-APGD for isotope ratio determination, a systematic evaluation of the measurement uncertainty of the technique has not been conducted. To this end, the International Standards Organizations (ISO) guidelines to the expression of uncertainty in measurement (GUM analysis) have been applied to generate an uncertainty budget. For this work, a preliminary assessment derived from the GUM analysis was performed. The uncertainty in the instrument blank determination has been identified as a primary factor contributing to measurement uncertainty for the LS-APGD-Orbitrap method. These findings for the specific test case of uranium isotopic analysis will be invaluable in applications across the breadth of isotope ratio mass spectrometry performed on this unique instrumental platform.
Solute transfer from the liquid to the gas phase in plasmas has been widely used in analytical chemistry often focused on liquid cathode discharges. In this study, we report on time-resolved absolute density measurements of sodium in a glow discharge plasma with a NaCl solution anode using two-photon absorption laser induced fluorescence. The averaged maximum sodium density is found to be similar to the electron density in the discharge consistent with plasma-induced vapor generation. Random sodium flashes were also observed extending into the plasma afterglow and are attributed to sodium particles falling back on the liquid surface. Cataphoresis can explain the location of the maximum sodium density near the cathode side of the electrode gap rather than near the liquid anode region.
Abstract Plasma self-organization on anode surfaces in 1 atm DC glow discharges remains poorly understood. This effort aims to elucidate the nature of self-organization through the experimental study of resulting patterns on liquid anode surfaces with 13 different electrolytes and thus improves our understanding of the underlying physical processes that give rise to self-organization by investigating electrolyte sensitivity. Self-organization pattern formation and behavior were studied as a function of discharge current, solution ionic strength, and their chemical property evaluation. The response of the patterns to variation in these parameters was measured using an imaging camera and optical emission spectroscopy. Observed pattern characteristic length scales for all of the electrolytes were ranged from 2 to 13 mm and typically increased with current over the investigated range of 20–80 mA. Complex self-organized pattern structures not reported to date were also observed. The parameters associated with pattern formation and morphology complexity are discussed and summarized.
Using a uniquely configured glow discharge-based Shivalik Plasma Device-I, we demonstrate a variety of collective phenomena in dusty plasma away from the glow discharge region. The cylindrical glass device produces plasma using parallel disc-shaped electrodes with a smaller anode size than the cathode. The dust microparticles are initially sprinkled over the grounded cathode. These particles acquire a significant negative charge upon plasma formation, resulting in their levitation due to the balance between the Coulomb force and gravity. The new device supports the levitation of a big-sized (10 × 8 × 5 cm 3 ) three-dimensional dust cloud over the glass surface. It contrasts the dusty plasma formations in-between electrodes reported earlier. As the discharge voltage varies from high to low, the dust cloud travels from over the glass surface to between the electrodes. A complex interplay of dust void over the cathode, a sharp density gradient, and gravity lead to self-excitation of collective dust phenomena. It includes dust density waves (phase velocity, v ph ~4 cm/s), dust cloud oscillation (frequency, f = 5 Hz), sheared flow (flow velocity, v f ~ 1 cm/s), and multiple-sized dust vortices. These dust vortices provided an excellent platform for studying turbulent mixing phenomena. The power spectrum analysis agreed with two-dimensional Kolmogorov power-law scaling. This is an ideal dusty plasma apparatus where we can create or move the dust cloud to a location of choice from the glass surface to in-between the electrodes and excite one among many collective dust dynamics.
The liquid sampling-atmospheric pressure glow discharge (LS-APGD) is a versatile combined atomic and molecular (CAM) ionization source capable of ionizing elemental species, small polar compounds, low-polarity polycyclic aromatic hydrocarbons, and proteins. While the LS-APGD has been proven capable of determining the 235U/238U isotope ratio in enriched and natural uranium, recent efforts have strived to reduce the analysis time of individual measurements by employing higher-order data processing techniques, specifically, moving average methods. Additionally, the use of a moving average (of data windows of various widths) improves the precision of the ratio measurements and reduces the number of scans needed to be collected to generate high-precision results. Additionally, use of the moving average minimizes the quantity of sample that needs to be analyzed while reducing the measurement time. These reductions have allowed isotope ratio (IR) determinations to be made using injections instead of direct infusion of the analyte. For example, employing a 40-point window width in the moving average to direct infusion data reduced the percent relative standard deviation (% RSD) of the 235U/238U values from 3.4% to 0.5%. For the injection of a 100 μL aliquot, the % RSD was reduced from 5.3% to 0.7%.
Intricate, self-organized plasma structures observed above the surface of a liquid anode of atmospheric DC glow discharge were found to give rise to coherent, organized surface deformation and mechanical wave formation at the plasma–liquid interface. This new phenomenon indicates that the liquid is closely coupled to the plasma by the anode sheath’s electrohydrodynamic (EHD) force. A scientific question then arises: Do surface perturbations, coupled with the nonuniform surface charge distribution, enhance the electric field and induce self-organization? Using the reflective background-oriented schlieren technique, the liquid surface profile under the plasma pattern was measured for the first time. The results show that surface distortions are driven by the repulsive Coulomb force of nonuniform net-negative surface charge acted by the anode sheath field. The impacts of various operating parameters on the patterns and surface waves were examined, revealing the significance of gas heating and liquid charge relaxation time in the pattern formation mechanism. Time-resolved dynamics of a pulsed DC discharge indicated that the surface deformation only appeared after the establishment of plasma patterns. Statistically, the surface wave under the plasma has high wave numbers (8000–16000 m −1 ) and small amplitudes ($<$ 10 µm), generally found in the capillary wave regime. Yet the motion of surface deformations is in tandem with the plasma pattern and exhibits a nondispersive nature of constant phase velocity (0.1–0.4 m s −1 ), suggesting the dominant role of EHD force over the surface tension in the observed surface wave. These results indicate that the deformed liquid surface is driven by the EHD force of the plasma sheath. Although they share a similar geometry, the deformation and wave dynamics of the liquid surface do not stimulate a plasma pattern. Importantly, the complex EHD coupling in the plasma–liquid system raises awareness and new challenges for plasma control engineering, and the quantitative characteristics of the nondispersive surface wave are informative for advancing relevant theory and modeling.
In inertial confinement fusion target design, the shape discrepancy between the cylindrical hohlraum and the spherical capsule creates a low mode asymmetry in the implosion. One way to correct such asymmetry is to shim the target capsule surface with extra mass in specific locations following a 3D P4 Legendre mode. Previously, the desired surface pattern was precision machined out of the capsule. The resulting 2DConA experiments that investigated the implosion’s shape demonstrated the shimming method’s success. However, machining leaves large defects on the capsule surface which will degrade neutron yield in a DT implosion. An alternative shimming approach is to grow the pattern on the capsule surface using a glow discharge polymerization coating process in a stencil lithography application. In this study, we discuss the fabrication, characterization and challenges of making shimmed target capsules with this new method.
This paper demonstrates that tungsten (W) based powder reconstituted Plasma Facing Components (PFCs) can be treated in situ in a fusion reactor to remove W oxide and carbon (C) contamination. Doing so should ease the challenge of using these materials in a Capillary Porous System (CPS) with lithium (Li) by enabling better wetting and less contamination of the Li by the underlying CPS. Most powder reconstituted materials including 3D printed and sintered PFCs suffer from a high surface contamination from oxides and surface C, which complicates their use with liquid Li, a primary PFC candidate. Spark plasma sintered porous W samples were fabricated to be used as a CPS with liquid Li. The samples were characterized in terms of morphology and surface chemistry. Analysis confirms a high C and oxygen (O) contamination. We present the results of exposing this type of CPS to Glow Discharge Cleaning (GDC) cycles in the Lithium Tokamak Experiment-β (LTX-β). The sample was exposed to neon (Ne) GDC in the midplane of the low-field side of LTX-β and analyzed in vacuo with Temperature Programmed Desorption (TPD) and Secondary Ion Mass Spectrometry (SIMS) to investigate the effects the Ne GDC had on the chemical composition of the sample. The combination of Ne GDC with rapid heating as done in TPD was successful in reducing the W oxides and removing the C contamination.
In this work, we investigated non-equilibrium plasma produced by nanosecond repetitively pulsed glow discharges applied across a lean premixed methane-air flame. The flame is stationary, axisymmetric, and laminar. The discharges are applied on the symmetry axis crossing the reactant gases, flame front, and product gases, allowing phase-locked averaged measurements and comparisons with axisymmetric numerical simulations. The thermal effect and methyl radical production are quantified in the discharge in the reactant gas region. One-dimensional, two-beam, hybrid, femtosecond-picosecond, coherent anti-Stokes Raman scattering is used to acquire spatial and temporal profiles of temperature and oxygen-to-nitrogen concentration ratio. Photo-fragmentation laser-induced fluorescence is used to acquire quantitative two-dimensional profiles of methyl radicals in the discharge providing the first quantitative imaging of methyl produced ahead of a flame by plasma-induced methane dissociation. The spatial profiles of temperature and oxygen-to-nitrogen concentration ratio are in steady state, indicating that individual discharges have an insignificant heating effect. Upper and lower bounds of the produced mole fraction of methyl radicals in the plasma are obtained due to uncertainties in the collisional quenching rates of excited state methylidyne radicals in the plasma. The discharges produce a maximum of 600–1100 ppm of methyl radicals upstream of the flame front within 25 ns. This amount is similar to the predicted methyl mole fraction for the flame without plasma and thus represents a significant chemical perturbation to the reactants upstream of the flame front. The produced methyl follows an exponential decay in the first microsecond after the discharge with a decay constant of 8 µs close to the flame, and 0.8 µs further from the flame. The decay then deviates from the exponential curve and the methyl persists for tens of microseconds. The results suggest that for the tested configuration, the thermal effect of individual discharges through fast gas heating is negligible, while active chemical species are produced in large quantities in the reactant gases, upstream of the flame front.
Plutonium measurements are essential to the nuclear forensics and safeguards community. The liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma ionization source coupled with an Orbitrap mass spectrometer is a proven platform for uranium isotope ratio determinations. Here, this work expands the LS-APGD-Orbitrap platform capabilities by reporting the first-ever analysis of plutonium with the LS-APGD and the first-ever measurement of elemental plutonium with an Orbitrap mass spectrometer. This coupling has the potential to dramatically reduce the complex sample manipulations required for traditional analysis techniques employed for actinide isotope ratio determinations. As a first step toward the goal of simultaneous uranium and plutonium isotope ratio determinations, the initial characterization and optimization of the platform for the detection of plutonium are reported. Collision-induced dissociation modality settings were optimized to reduce water-related and other molecular clusters containing plutonium, maximizing 242 Pu 16 O 2 + responses. A design of experiments study was conducted to optimize the discharge conditions of the dual-electrode LS-APGD toward the responsivity of 242 Pu 16 O 2 +. The measurement sensitivity was determined from a Pu response curve, yielding a limit of detection of 10 fg (absolute) of total analyte when data was collected and processed with a Spectroswiss FTMS Booster X2 data acquisition system. Additionally, plutonium and uranium were measured in a simultaneous acquisition, and each analyte remained unaffected by the other. It is believed that the LS-APGD-Orbitrap platform could be a valuable addition to the nuclear forensics’ toolbox and, indeed, other scientific disciplines and regulatory communities in which rapid, high-resolution plutonium determinations are paramount.
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.
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.
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.