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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Direct Observation of Plasma-Stimulated Activation of Surface Species Using Multimodal In Situ/Operando Spectroscopy Combining Polarization-Modulation Infrared Reflection-Absorption Spectroscopy, Optical Emission Spectroscopy, and Mass Spectrometry

Nonthermal plasmas (NTPs) produce reactive chemical environments, including electrons, ions, radicals, and vibrationally excited molecules, that can drive chemistry at temperatures at which such species are thermally inaccessible. There has been growing interest in the integration of conventional catalysis with reactive NTPs to promote novel chemical transformations. Unveiling the full potential of plasma-catalytic processes requires a comprehensive understanding of plasma-catalytic synergies, including characterization of plasma-catalytic surface interactions. In this work, we report on a newly designed multimodal spectroscopic instrument combining polarization-modulation infrared reflection-absorption spectroscopy (PM-IRAS), mass spectrometry, and optical emission spectroscopy (OES) for the investigation of plasma–surface interactions such as those found in plasma catalysis. In particular, this tool has been utilized to correlate plasma-phase chemistry with both surface chemistry and gas-phase products in situ (1) during the deposition of carbonaceous surface species via NTP-promoted nonoxidative coupling of methane and (2) during subsequent activation of surface deposits with an atmospheric pressure and temperature argon plasma jet on both nickel (Ni) and silicon dioxide (SiO 2 ) surfaces. For the first time, the activation of carbonaceous surface species by a NTP on Ni and SiO 2 surfaces to form hydrogen gas and C 2 hydrocarbons was directly observed, where both PM-IRAS and OES measurements suggest that they may form through different pathways. Furthermore, this unique tool for studying plasma–surface interactions could enable more rational design of plasma-stimulated catalytic processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Design and implementation of a portable diagnostic system for Thomson scattering and optical emission spectroscopy measurements

A diagnostic system, which has a design goal of high-portability, has been designed at Oak Ridge National Laboratory (ORNL). This project aims at providing measurements of key plasma parameters (ne, Te, ni, Ti) for fusion-relevant devices, utilizing Thomson scattering (TS) and optical emission spectroscopy (OES). The innovative design employs mostly commercial off-the-shelf instrumentation and a traveling team of researchers to conduct measurements at various magnetic-confinement plasma devices. The TS diagnostic uses a Quantel Q-smart 1500 Nd:YAG laser with a 2ω harmonic generator to produce up to 850 mJ of 532 nm laser pulses at 10 Hz. Collection optics placed at the detection port consists of an 11 × 3 optical fiber bundle, where the TS diagnostic uses an 11 × 1 subset array of the fibers, the OES diagnostic uses another 11 fibers, and the remaining fibers are available to the host institution. The detection system is comprised of two separate IsoPlane-320 spectrometers with triple-grating turrets of various line spacing and two PI-MAX 4 intensified CCD detectors, used simultaneously to measure a broad range of ion, impurity, and electron parameters. The self-contained diagnostic package also includes a data processing and storage system. The design and initial implementation of the TS-OES diagnostic system are described. The experiments from the proof-of-principle operation of the portable package on a high density (∼2.5 × 1022 m−3) and low-temperature (∼5 eV) electrothermal arc source at ORNL are also discussed.

Kafle, N. (ORCID:000000028144787X)↗
DOE OSTI2022

Portable diagnostic package for Thomson scattering and optical emission spectroscopy on Princeton field-reversed configuration 2 (PFRC 2)

An Advanced Research Projects Agency-Energy funded diagnostic system has been deployed to the Princeton field-reversed configuration 2 (PFRC-2) device, located at Princeton Plasma Physics Laboratory. The Portable Diagnostic Package (PDP), designed at Oak Ridge National Laboratory, allows for the measurement of Thomson Scattering (TS) for electron density and temperature and Optical Emission Spectroscopy (OES) for ion temperature, impurity density, and ion velocity. A tunable spectrometer on the PDP with three gratings provides the flexibility to measure low (1 eV) and high (1000 eV) electron temperature ranges from TS. Additionally, using a second spectrometer, the OES diagnostic can survey light emission from various ion excitation levels for wide wavelength ranges. The electron density (<2 × 10 19 m –3 ) of plasmas generated in PFRC-2 has been below the PDP TS discrimination threshold, which has made TS signal detection challenging against a high-background of laser stray light. The laser stray light was iteratively reduced by making modifications to the entrance and exit geometry on PFRC-2. Rayleigh scattering experiments on PFRC have yielded the TS discrimination sensitivity to be >1 × 10 20 m –3 for the PDP. A recently implemented narrow-band notch spectral filter that masks the second harmonic 532 nm Nd:YAG laser wavelength has increased the system’s TS light discrimination sensitivity 65 times compared to the instance when the notch filter was not implemented. The hardware implementation including design changes to the flight tubes and Brewster windows will be discussed, along with results from Rayleigh and rotational Raman scattering sensitivity analyses, which were used to establish a quantitative figure of merit on the system performance. Further, the Raman scattering calibration with the notch filter has improved the PDP electron density threshold to 1 ± 0.5 × 10 18 m –3 .

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Early- and late-time dynamics of laser-produced plasmas by combining emission and absorption spectroscopy

Optical emission spectroscopy and laser absorption spectroscopy are two highly complementary techniques for diagnosing plasmas, specifically in the determination of important parameters such as temperature and density. In this work, we characterized a laser-produced plasma by combining emission and tunable absorption spectroscopy. Plasmas are produced by focusing pulses from a frequency quadrupled Nd:YAG laser onto a glass target containing a minor concentration of aluminum in an ambient atmosphere of ~100 Torr N 2 . Here, emission spectroscopy is used to investigate the line behavior of Al and Ca, electron density, and excitation temperature at times = 5 μs, while absorption spectroscopy is used to investigate the line behavior of Al and Ca, species density, and kinetic temperature at times = 5-100 μs. A comparison is made between the excitation temperature measured from emission using the Boltzmann plot method and the kinetic temperature measured from absorption; the implications of this comparison on local thermodynamic equilibrium and line-of-sight averaging are discussed. By combining the two methods of optical emission and laser absorption spectroscopy, a comprehensive characterization of the plasma over the entire lifetime of its evolution is possible, leading to a greater understanding of the plasma behavior including particle condensation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2013

Phase-resolved optical emission spectroscopy for an electron cyclotron resonance etcher

Phase-resolved optical emission spectroscopy (PROES) is used for the measurement of plasma products in a typical industrial electron cyclotron resonance (ECR) plasma etcher. In this paper, the PROES of oxygen and argon atoms spectral lines are investigated over a wide range of process parameters. The PROES shows a discrimination between the plasma species from gas phase and those which come from the solid phase due to surface etching. The relationship between the micro-wave and radio-frequency generators for plasma creation in the ECR can be better understood by the use of PROES.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

Comparison endpoint study of process plasma and secondary electron beam exciter optical emission spectroscopy

Traditionally process plasmas are often studied and monitored by optical emission spectroscopy. Here, the authors compare experimental measurements from a secondary electron beam excitation and direct process plasma excitation to discuss and illustrate its distinctiveness in the study of process plasmas. They present results that show excitations of etch process effluents in a SF{sub 6} discharge and endpoint detection capabilities in dark plasma process conditions. In SF{sub 6} discharges, a band around 300 nm, not visible in process emission, is observed and it can serve as a good indicator of etch product emission during polysilicon etches. Based on prior work reported in literature the authors believe this band is due to SiF{sub 4} gas phase species.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2011

Comparison of Optical Emission Spectroscopy and Cavity Ring-Down Spectroscopy in Large-Scaled Negative-Ion Source

Optical emission spectroscopy (OES) and cavity ring-down spectroscopy (CRDS) systems are installed in a 1/3-scaled negative hydrogen-ion source at the National Institute for Fusion Science testbed to investigate the dynamics of H{sup -} ions in the extraction region near the plasma grid. The signal form of the H{sup -} ion density rapidly drops after beam extraction on applying a low-bias voltage. A similar signal drop appears in the intensity of the hydrogen Balmer-line emission measured by OES and is caused by decreasing atomic hydrogen produced by mutual neutralization effects between H{sup -} and H{sup +}. Shot trend of the beam currents are similar to the H{sup -} density and H{sub {alpha}}/H{sub {beta}} in the extraction region, which increases twice as large immediately after Cs seeding. We observe a linear correlation between the H{sup -} density and the inclination of H{sub {alpha}}/H{sub {beta}} which allows for experimentally benchmarking the OES measurement with that of CRDS. Thus, this approach is used for estimating the H{sup -} density by OES in negative-ion sources for high-energy neutral beam injector.

43 PARTICLE ACCELERATORS↗
DOE OSTI2023

Application of machine learning for optical emission spectroscopy data in NAGDIS-II

In this study, we applied machine learning to optical emission spectroscopy (OES) data and device parameters from the linear plasma device NAGDIS-II to explore the potential application of machine learning for predicting electron density, $n$ e , and temperature, $T$ e . The covered ranges of $n$ e and $T$ e , which were measured by an electrostatic probe, are 3.6 × 10 17 –2.4 × 10 19 m -3 and 0.3–7.1 eV, respectively. A three hidden layer neural network (NN) is introduced to model the relationship between $n$ e /$T$ e and the combination of line intensities, radial position, and device parameters. It is shown that the errors in $n$ e and $T$ e become 18.0 and 18.8%, respectively, which were almost the same level for the electrostatic probe, using all available data. Lasso regression and greedy algorithm are used to select the necessary line emissions. In conclusion, it is shown that four- or five-line intensities are sufficient to obtain almost the same quality as the one with all the other lines.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2011

Characterization of a low-pressure chlorine plasma column sustained by propagating surface waves using phase-sensitive microwave interferometry and trace-rare-gas optical emission spectroscopy

Phase-sensitive microwave interferometry and trace-rare-gas optical emission spectroscopy were used to measure the line-integrated electron density, n{sub e}, and electron temperature, T{sub e}, in a high-density chlorine plasma sustained in a quartz discharge tube (inner diameter = 6 mm) by an electromagnetic surface wave at 2.45 GHz. For pressures in the 0.1-1 Torr range, n{sub e} decreased nearly linearly along the tube's z-axis down to the critical density for surface wave propagation, where the plasma decayed abruptly. At lower pressures (< 50 mTorr), however, the plasma extended well beyond this critical point, after which n{sub e} decreased quasiexponentially toward the end of the plasma column. The length of this expansion region increased with decreasing pressure, going from {approx}8 cm at 5 mTorr to {approx}1 cm at 50 mTorr. T{sub e} was nearly independent of the axial position in the main plasma region and strongly decreased in the expansion region at lower pressures. The Cl{sub 2} percent dissociation, {tau}{sub D}, obtained from the calibrated Cl{sub 2} (306 nm)-to-Xe (828 nm) emission ratio, displayed behavior similar to that of n{sub e} and T{sub e}. For example, at 5 mTorr, {tau}{sub D} was close to 100% near the wave launcher and {approx}70% at 0.5 cm from the end of the plasma column.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2018

Note: Plasma optical emission spectroscopy for water vapor quantification and detection during vacuum drying process

In this work, a methodology involving plasma optical emission spectroscopy driven by a direct current (dc) plasma source is developed to quantify water vapor concentration in a gaseous stream. The experimental setup consists of a dc driven low-pressure plasma cell in which the emission from the plasma discharge is measured by using an optical emission spectrometer. The emission from Hα at 656.2 nm—the first transition in the Balmer series, was found to be the most sensitive to the water vapor concentration in the gas stream. Consistent linear trends of the emission signals with respect to variation in concentration of water are observed for multiple combinations of operating parameters. This method has been applied to a vacuum drying process of a mock nuclear fuel assembly to quantify the concentration of water vapor during the drying process.

47 OTHER INSTRUMENTATION↗
DOE OSTI2019

Evaluation and Specifications for In-Line Uranium Separations Using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) Detection for Trace Elemental Analysis

Automated introduction platforms integrated with inductively coupled plasma optical emission spectroscopy (ICP-OES) systems are continuously being improved. Expanding on the introduction systems, a newly developed automated ion chromatography system was explored for performing rapid in-line separations coupled to ICP-OES for the detection of trace elements in uranium. Trace elements are separated from a uranium material and the analytes are directed into the ICP-OES for subsequent detection. Detection parameters such as exposure time frequency, wavelength selection, and settling times were explored to gain insight on optimal detection schemes for in-line trace elemental analysis. The methodology was applied in the analysis of a uranium oxide (U3O8) certified reference material, CRM-124. It was found here that the sensitivity and uncertainty of the technique are greatly affected by how the ICP-OES is employed to collect data. Overall it was determined that faster exposure replicates can provide greater peak resolution with higher fidelity measurements but are limited with respect to the total analysis time (i.e., limited in detection timely separations). In conclusion zeta scores, which combine accuracy and uncertainty of certified values and experimental values, were used to validate the ICP-OES modes of operation.

47 OTHER INSTRUMENTATION↗
DOE OSTI2016

First hydrogen operation of NIO1: Characterization of the source plasma by means of an optical emission spectroscopy diagnostic

NIO1 (Negative Ion Optimization 1) is a compact and flexible radio frequency H{sup −} ion source, developed by Consorzio RFX and INFN-LNL. The aim of the experimentation on NIO1 is the optimization of both the production of negative ions and their extraction and beam optics. In the initial phase of its commissioning, NIO1 was operated with nitrogen, but now the source is regularly operated also with hydrogen. To evaluate the source performances, an optical emission spectroscopy diagnostic was installed. The system includes a low resolution spectrometer in the spectral range of 300-850 nm and a high resolution (50 pm) one, to study, respectively, the atomic and the molecular emissions in the visible range. The spectroscopic data have been interpreted also by means of a collisional-radiative model developed at IPP Garching. Besides the diagnostic hardware and the data analysis methods, the paper presents the first plasma measurements across a transition to the full H mode, in a hydrogen discharge. The characteristic signatures of this transition in the plasma parameters are described, in particular, the sudden increase of the light emitted from the plasma above a certain power threshold.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Trace Elemental Analysis of Bulk Thorium Using an Automated Separation–Inductively Coupled Plasma Optical Emission Spectroscopy Methodology

Presented here is a novel automated method for determining the trace element composition of bulk thorium by inductively coupled plasma–optical emission spectroscopy (ICP-OES). ICP-OES is a universal approach for measuring the trace elemental impurities present in actinide-rich materials; however, due to the emission rich spectrum of the actinide, a separation from the trace elements is warranted for spectrochemical analysis. Here, AG MP-1 ion exchange resin was utilized for retention of the Th matrix, while allowing the trace element impurities to be separated prior to subsequent analysis using ICP-OES. After demonstrating the separation on traditional gravity-driven columns, the methodology was transitioned to an automated platform for comparison. This automated platform utilizes syringe-driven sample and solvent flow and can collect the trace element and thorium fractions in separate locations. Finally, while reducing the sample size (500 µL, 1.5 mg of Th), maintaining the overall separation efficiency (recoveries >95%), and illustrating the sample throughput ability (n = 10+), this automated methodology could be readily adopted to nuclear facilities in which the determination of trace elemental impurities in Th samples is warranted.

47 OTHER INSTRUMENTATION↗
DOE OSTI2011

Langmuir probe diagnostics of electron energy distributions with optical emission spectroscopy in capacitively coupled rf discharge in nitrogen

Measurements with a rf compensated Langmuir probe and optical emission spectroscopy are carried out in capacitively coupled rf (13.56 MHz) pure nitrogen N{sub 2} discharges at fixed rf voltage over a wide range of pressure, 30 to 400 mTorr. The electron energy probability function (EEPF) measured below 100 mTorr resembles a bi-Maxwellian-type distribution. At pressure range of 100-200 mTorr, the EEPF has non-Maxwellian distribution with a ''dip'' near 4.5 eV. At the highest pressure of 400 mTorr, the EEPF evolves into a Druyvestein-like distribution and the ''dip'' disappears. The electron density significantly decreases with increase in the N{sub 2} pressure. On the other hand, the electron temperatures gradually decrease with an increase in N{sub 2} pressure, reaching minimum at 150 mTorr, beyond which it abruptly increases. Such evolution of the EEPFs shape with gas pressure has been discussed in terms of non-local electron kinetics and heating mode transition. The emission intensities of nitrogen (0-0) band of second positive system at 337.1 nm and (0-0) band of first negative systems at 391.4 nm are used to determine the dependence of their radiative states N{sub 2}(C{sup 3}{Pi}{sub u}) and N{sub 2}{sup +}(B{sup 2}{Sigma}{sub u}{sup +}) with nitrogen pressure. It is observed that the pressure influences the radiative states differently owing to their different populating mechanisms. The vibrational temperature T{sub {nu}ib} and rotational temperature T{sub rot} are measured for the sequence ({Delta}{nu}=-2) of N{sub 2} second positive system (C{sup 3}{Pi}{yields}B{sup 3}{Pi}{sub g}) using the method of comparing the measured and calculated spectra with a chi-squared minimization procedure. It was found that both T{sub {nu}ib} and T{sub rot} have similar dependences with N{sub 2} pressure; peaked at 100 mTorr beyond which it monotonically decreases with increase in the N{sub 2} pressure. The correlation between the observed maximum value of T{sub {nu}ib} around 100 mTorr and the detected ''dip'' in the EEPF in the same pressure range has been discussed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2012

Electron energy distribution functions measured by Langmuir probe with optical emission spectroscopy in very high frequency capacitive discharge in nitrogen

By using a rf compensated Langmuir probe and optical emission spectroscopy, the effects of driving frequency (13.56-50 MHz) on the electron energy probability function (EEPF), electron density, electron temperature, and the vibrational and rotational temperatures in capacitively coupled nitrogen discharge were investigated. Measurements were performed in the pressure range 60-200 mTorr, and at a fixed voltage of 140 V (peak-to-peak). With increasing the driving frequency, the dissipated power and electron density markedly increased along with the intensity of the optical emission lines belonging to the 2nd positive (337.1 nm) and 1st negative systems (391.4 nm) of N{sub 2}. The EEPF at low pressure 60 mTorr is two-temperature (bi-Maxwellian) distribution, irrespective of the driving frequency, in contrast with argon and helium discharges in the similar conditions. The mechanism forming such bi-Maxwellian shape was explained by two combined effects: one is the collisionless sheath-heating effect enhancing the tail electron population, and the other is the collision-induced reduction of electrons at the energy 2-4 eV where the collision cross-section for the vibrational excitation has a resonantly large peak. The two-temperature EEPF structure was basically retained at moderate pressure 120 mTorr and high pressure 200 mTorr. The vibrational temperature T{sub vib} and rotational temperature T{sub rot} are measured for the sequence ({Delta}{nu}=-2) of N{sub 2} second positive system (C{sup 3}{Pi}{sub u}{yields}B{sup 3}{Pi}{sub g}) using the method of comparing the measured and calculated spectra with a chi-squared minimization procedure. It was found that, both of T{sub vib} and T{sub rot} are a weakly dependent on driving frequency at low pressure 60 mTorr. At higher pressure (120 and 200 mTorr), T{sub vib} rises monotonically with the driving frequency, whereas the T{sub rot} slightly decreases with frequency below 37 MHz, beyond which it relatively increases or saturated.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2023

Tomographic optical emission spectroscopy of an atmospheric pressure plasma jet and surface ionization waves on planar and structured surfaces

Here in this paper, an approach for 3D plasma structure diagnostics using tomographic optical emission spectroscopy (Tomo-OES) of a nanosecond pulsed atmospheric pressure plasma jet (APPJ) is presented. In contrast to the well-known Abel inversion, Tomo-OES does not require cylindrical symmetry to recover 3D distributions of plasma light emission. Instead, many 2D angular projections are measured with intensified cameras and the multiplicative algebraic reconstruction technique is used to recover the 3D distribution of light emission. This approach solves the line-of-sight integration problem inherent to optical diagnostics, allowing recovery of localized OES information within the plasma that can be used to better infer plasma parameters within complex plasma structures. Here, Tomo-OES was applied to investigate an APPJ operated with helium in ambient air and impinging on planar and structured dielectric surfaces. Surface charging caused the guided streamer from the APPJ to transition to a surface ionization wave (SIW) that propagated along the surface. The SIW experienced variable geometrical and electrical material properties as it propagated, leading to 3D configurations that were non-symmetric and spatially complex. Light emission from He, N$_2^+$, and N2 were imaged at ten angular projections and the respective time-resolved 3D emission distributions in the plasma were then reconstructed. The spatial resolution of each tomographic reconstruction was 7.4 µm and the temporal resolution was 5 ns, sufficient to observe the guided streamer and the effects of the structured surface on the SIW. Emission from He showed the core of the jet and emission from N$_2^+$ and N2 indicated effects of entrainment of ambient air. Penning ionization of N2 created a ring or outer layer of N$_2^+$ that spatially converged to form the 'plasma bullet' or spatially diverged across a surface as part of a SIW. The SIW entered trenches of size 150 µm, leading to decreases in plasma light emission in regions above the trenches. The plasma light emission was higher in some regions with trenches, possibly due to effects of field enhancement.

plasma interactions with complex surfaces↗
DOE OSTI2013

Noninvasive, real-time measurements of plasma parameters via optical emission spectroscopy

Plasma process control applications require acquisition of diagnostic data at a rate faster than the characteristic timescale of perturbations to the plasma. Diagnostics based on optical emission spectroscopy of intense emission lines permit rapid noninvasive measurements with low-resolution ({approx}1 nm), fiber-coupled spectrographs, which are included on many plasma process tools for semiconductor processing. Here the authors report on rapid analysis of Ar emissions with such a system to obtain electron temperatures, electron densities, and metastable densities in argon and argon/mixed-gas (Ar/N{sub 2}, Ar/O{sub 2}, Ar/H{sub 2}) inductively coupled plasmas. Accuracy of the results (compared to measurements made by Langmuir probe and white-light absorption spectroscopy) are typically better than {+-}15% with a time resolution of 0.1 s, which is more than sufficient to capture the transient behavior of many processes, limited only by the time response of the spectrograph used.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2016

Investigation of local thermodynamic equilibrium of laser induced Al{sub 2}O{sub 3}–TiC plasma in argon by spatially resolved optical emission spectroscopy

Plasma plume of Al{sub 2}O{sub 3}–TiC is generated by third harmonic Q-switched Nd:YAG nanosecond laser. It is characterized using Optical Emission Spectroscopy (OES) at different argon background gas pressures 10, 10{sup 2}, 10{sup 3}, 10{sup 4} and 10{sup 5} Pa. Spatial evolution of excitation and ionic temperatures is deduced from spectral data analysis. Temporal evolution of Ti I emission originated from different energy states is probed. The correlation between the temporal behavior and the spatial temperature evolution are investigated under LTE condition for the possibility to use the temporal profile of Ti I emission as an indicator for LTE validity in the plasma.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗