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DOE OSTI2024

Science challenges and research opportunities for plasma applications in microelectronics

Low-temperature plasmas (LTPs) are essential to manufacturing devices in the semiconductor industry, from creating extreme ultraviolet photons used in the most advanced lithography to thin film etching, deposition, and surface modifications. It is estimated that 40%–45% of all process steps needed to manufacture semiconductor devices use LTPs in one form or another. LTPs have been an enabling technology in the multidecade progression of the shrinking of device dimensions, often referred to as Moore’s law. New challenges in circuit and device design, novel materials, and increasing demands to achieve environmentally benign processing technologies require advances in plasma technology beyond the current state-of-the-art. The Department of Energy Office of Science Fusion Energy Sciences held a workshop titled Plasma Science for Microelectronics Nanofabrication in August 2022 to discuss the plasma science challenges and technical barriers that need to be overcome to continue to develop the innovative plasma technologies required to support and advance the semiconductor industry. One of the key outcomes of the workshop was identifying a set of priority research opportunities (PROs) to focus attention on the most strategic plasma science challenges to address to benefit the semiconductor industry. For each PRO, scientific challenges and recommended strategies to address those challenges were identified. Furthermore, this article summarizes the PROs identified by the workshop participants.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Simultaneous Imaging of Molecular Rovibrational Nonequilibrium, Reactive Species, and Electric Field for Plasma-Assisted Chemistry

The Sandia-PRF has built a new capability for the low-temperature plasma community for the simultaneous imaging of molecular rotation/vibration nonequilibrium, electric field, and the distribution of OH radical and formaldehyde in reactive low temperature plasma systems. The system is currently investigating the plasma-assisted deflagration to detonation transition in a micro-combustor channel.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2008

Characterizing ISS Charging Environments with On-Board Ionospheric Plasma Measurements

Charging of the International Space Station (ISS) is dominated by interactions of the biased United States (US) 160 volt solar arrays with the relatively high density, low temperature plasma environment in low Earth orbit. Conducting surfaces on the vehicle structure charge negative relative to the ambient plasma environment because ISS structure is grounded to the negative end of the US solar arrays. Transient charging peaks reaching potentials of some tens of volts negative controlled by photovoltaic array current collection typically occur at orbital sunrise and sunset as well as near orbital noon. In addition, surface potentials across the vehicle structure vary due to an induced v x B (dot) L voltage generated by the high speed motion of the conducting structure across the Earth's magnetic field. Induced voltages in low Earth orbit are typically only approx.0.4 volts/meter but the approx.100 meter scale dimensions of the ISS yield maximum induced potential variations ofapprox.40 volts across the vehicle. Induced voltages are variable due to the orientation of the vehicle structure and orbital velocity vector with respect to the orientation of the Earth's magnetic field along the ISS orbit. In order to address the need to better understand the ISS spacecraft potential and plasma environments, NASA funded development and construction of the Floating Potential Measurement Unit (FPMU) which was deployed on an ISS starboard truss arm in August 2006. The suite of FPMU instruments includes two Langmuir probes, a plasma impedance probe, and a potential probe for use in in-situ monitoring of electron temperatures and densities and the vehicle potential relative to the plasma environment. This presentation will describe the use of the FPMU to better characterize interactions of the ISS with the space environment, changes in ISS charging as the vehicle configuration is modified during ISS construction, and contributions of FPMU vehicle potential and plasma environment measurements to investigations of on-orbit anomalies in ISS systems.

Minow, Jospeh I.↗

DOE OSTI2023

Nonthermal plasma synthesis of silicon carbonitride

Abstract The use of a low‐temperature plasma for the synthesis of amorphous silicon carbonitride (SiCN) nanoparticles enables the realization of sintered bulk samples with high thermal stability. Amorphous SiCN nanoparticles are produced from a mixture of silane, methane, and ammonia utilizing a mid‐pressure, radio‐frequency, continuous flow reactor. Particle characterization shows that the nanoparticles are largely amorphous with some crystalline silicon and silicon carbide domains <10 nm in size. Compositional tuning, controlled by varying the precursor flow rates, coupled with the uniform mixing of elements at the nanoscale, results in samples that resist crystallization even when sintered at temperatures as high as 2000°C. This study suggests that the low‐temperature plasma synthesis of nanoparticles has great potential to produce bulk structural materials for application in harsh environments.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2020

Expansion dynamics and chemistry evolution in ultrafast laser filament produced plasmas

Laser ablation in conjunction with optical emission spectroscopy is a potential non-contact, standoff detection method for all elements in the periodic table and certain isotopes such as radionuclides. Currently, significant development efforts are on-going to use ultrafast laser filaments for remote sensing. The application of filaments is of particular interest in extending the range of stand-off capability associated with elemental and isotopic detection via laser-induced breakdown spectroscopy. In this study, we characterize the expansion dynamics and chemical evolution of filament-produced uranium (U) plasmas. Laser filaments are generated in the laboratory by loosely focusing 35 femtosecond (fs), 6 milli Joule (mJ) pulses in air. Two-dimensional spectrally-integrated and time-resolved imaging was performed to study hydrodynamics and evolution of U atomic and UO molecular emission in filament-produced U plasmas. Our results highlight that filament ablation of U plasmas gives a cylindrical plasma plume morphology with an appearance of plume splitting into slow and fast moving components at later times of its evolution. Emission from the slow-moving region shows no distinct spectral features (i.e. broadband-like) and is contributed in part by nanoparticles generated during ultrafast laser ablation. Additionally, we find U atoms and U oxide molecules (i.e. UO, UxOy) co-exist in the filament produced plasma, which can be attributed to the generation of low-temperature plasma conditions during filament ablation

(140.3440) Laser-induced breakdown, (280.5395) Pla↗

DOE OSTI2023

Low temperature hydrogen plasma permeation in palladium and its alloys for fuel recycling in fusion systems

Superpermeation of hydrogen isotopes through metal foils is a critical component for efficient fuel recycling in fusion power systems. In that context hydrogen permeation through foils of palladium and its alloys with silver and copper was studied at low temperature (60 - 200°C) under plasma exposure. These alloys differ significantly in both bulk and surface properties, and comparisons can provide mechanistic insights. Here, permeation was observed only during plasma operation, confirming the negligible contribution of molecular hydrogen to the observed flux. As-received foils required surface treatment to achieve top performance. For Pd and Pd75Ag25 an oxidation treatment increased permeation an order of magnitude, but proved unstable as this desirable surface was reduced under hydrogen plasma exposure. In contrast, an Ar plasma cleaning step provided both high and stable flux. As-received FCC phase Pd60Cu40 foils required annealing to transform it into the high permeability BCC phase that delivered top performance. All foils displayed similar temperature dependence with flux declining with temperature, suggesting that the primary rate-limiting step is absorption of superthermal hydrogen. Among these foils the hydrogen flux through PdCu was 3 - 5X greater than that of Pd or PdAg, which were similar. The superiority of BCC PdCu is attributed to its superior hydrogen desorption kinetics. Using PdCu 100% permeation of supplied hydrogen was achieved, and the flux saturated with increasing plasma power at values >10 –2 mol H•m –2 •s– 1 , and under these conditions permeation rates are equivalent with or without the membrane present. The fluxes achieved are the highest reported to date at these conditions, and the results highlight the important roles of both surface and bulk properties.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2021

DOE Plasma Science Center - Predictive Control of Plasma Kinetics: Multi-Phase and Bounded Systems (Final Report DE-SC0001939)

Low temperature plasmas (LTPs) are the plasmas of electron-volt (eV) physics and eV technologies. LTPs have characteristic electron temperatures of a few eV and fractional ionizations that are typically small. Since LTPs have electron temperatures commensurate with the threshold energies of excited states in neutral atoms and molecules, power transfer from electrons to these atoms and molecules efficiently produces activated species (e.g., radicals, excited states, photons). Acceleration of ions in the sheaths of LTPs to energies of tens to hundreds of eV enable activation of surface modifying processes – sputtering, etching, deposition. With such properties, LTPs are often and beneficially used in technological devices, ranging from etching and deposition in microelectronics and solar cell fabrication, to hardening of surgical instruments. LTPs harbor fundamental science issues that are intellectually challenging and rewarding. At the same time, there are enormous societal benefits that are enabled by LTPs. The entire present-day and future information technology infrastructure owes its very existence to LTPs. Renewable energy sources, such as solar cell arrays, could not be economically produced in the absence of deposition and etching by LTPs. In acknowledgment of the importance of LTPs, the DOE Office of Fusion Energy Sciences supported the Plasma Science Center for Predictive Control of Plasma Kinetics: Multi-Phase and Bounded Systems from August 2009 to July 2021, consisting of an initial 5-year grant, 3 funded extensions and 2 no-cost extensions. This is the final report of the Center in which the productivity of the Center is discussed in terms of publications, impact and personnel. High-lights of the research performed in the Center are provided.

36 MATERIALS SCIENCE↗

NASA NTRSDate not supplied

Plasma for Crewed Transit and Planetary Habitation

As human exploration moves beyond low Earth orbit, innovative life support and resource production systems become forerunners for human colonization. Plasma systems allow for complex chemical processes while mitigating consumable needs. Plasma technology and applications can redefine the space environment. With this, scientists at NASA are looking to close known space technology gaps and create a paradigm shift in space-based applications. NASA’s Kennedy Space Center is exploring the use of low-temperature plasma for applications in agriculture, sanitation ,regolith reduction, waste gasification, water activation, and nutrient recovery techniques. Using low temperature plasmas, we report on the success criteria and experimental results for plasma applications for crewed transit and planetary habitation.

Plasma↗

NASA NTRSDate not supplied

Plasma for Crewed Transit and Planetary Habitation

As human exploration moves beyond low Earth orbit, innovative life support and resource production systems become forerunners for human colonization. Plasma systems allow for complex chemical processes while mitigating consumable needs. Plasma technology and applications can redefine the space environment. With this, scientists at NASA are looking to close known space technology gaps and create a paradigm shift in space-based applications. NASA’s Kennedy Space Center is exploring the use of low-temperature plasma for applications in agriculture, sanitation, regolith reduction, waste gasification, water activation, and nutrient recovery techniques. Using low temperature plasmas, we report on the success criteria and experimental results for plasma applications for crewed transit and planetary habitation.

Waste management↗

DOE OSTI2023

Pretreatment of Bituminous Coal By-Products for the Hydrometallurgical Extraction of Rare Earth Elements

Low-temperature plasma (LTP) oxidation has been widely used to study the mineralogy of the mineral matter existing in coal sources. The current study investigated the potential of LTP oxidation as a pre-treatment method to improve rare earth element (REE) leachability from coal and its by-products. Representative density-fractionated samples of Baker and Fire Clay coarse refuse seam materials were ground to a top size of 180 µm and subjected to low-temperature plasma oxidation. Subsequently, the treated samples were leached at 1% w/v solids concentration and 75 °C for 5 h using (i) de-ionized (DI) water, (ii) 0.1 mol/L of ammonium sulfate, and (iii) 1.2 mol/L of sulfuric acid. It was determined that LTP treatment improved REE leaching characteristics, especially the leaching of heavy REEs (HREE), existing in the lighter density fractions of the Baker seam coarse refuse material. For instance, the HREE recovery for the 1.6 specific gravity (SG) float fraction increased from 8% to 33% using 0.1 mol/L of ammonium sulfate solution after 32 h of LTP treatment. This finding indicated that HREEs associated with the organic matter were released by the LTP treatment and adsorbed onto the surfaces of highly negative charged mineral matter and was exchanged with ammonium to allow their recovery. Similarly, when using 1.2 mol/L of sulfuric acid, the HREE recovery increased from 23% to 53% for the 1.6 SG float fraction. Interestingly, LTP oxidation did not provide significant improvement in REE recovery from the 2.2 sink density fractions, which was likely due to its lower organic content. No significant benefits were observed when treating the Fire Clay coarse refuse material, which was likely due to the lack of organic affinity and the difficult-to-leach REE minerals associated with the coal source such as monazite, xenotime, and zircon. Conversely, high-temperature oxidation within a temperature range of 600–750 °C significantly improved REE leaching characteristics for both coal sources. Improvement in REE recovery was due to decarbonization of the material, clay dehydroxylation and subsequent conversion of liberated REE-bearing minerals into a more leachable form. However, increasing the temperature above 800 °C decreased REE recovery due to the conversion of meta-kaolinite into mullite, which is chemically stable.

58 GEOSCIENCES↗

NASA NTRS2016

Discovery of X-Ray Emission from the Galactic Supernova Remnant G32.8-0.1 with Suzaku

We present the first dedicated X-ray study of the supernova remnant (SNR) G32.8-0.1 (Kes 78) with Suzaku. X-ray emission from the whole SNR shell has been detected for the first time. The X-ray morphology is well correlated with the emission from the radio shell, while anti-correlated with the molecular cloud found in the SNR field. The X-ray spectrum shows not only conventional low-temperature (kT approximately 0.6 kiloelectronvolts) thermal emission in a nonequilibrium ionization state, but also a very high-temperature (approximately 3.4 kiloelectronvolts) component with a very low ionization timescale (approximately 2.7 times 10 (sup 9) per cubic centimeter per second), or a hard nonthermal component with a photon index Gamma approximately equal to 2.3. The average density of the low-temperature plasma is rather low, of the order of 10 (sup -3) - 10 (sup -2) per cubic centimeter, implying that this SNR is expanding into a low-density cavity. We discuss the X-ray emission of the SNR, also detected in teraelectronvolts with H.E.S.S. (High Energy Stereoscopic System), together with multi-wavelength studies of the remnant and other gamma-ray emitting SNRs, such as W28 and RCW 86. Analysis of a time-variable source, 2XMM J185114.3-000004, found in the northern part of the SNR, is also reported for the first time. Rapid time variability and a heavily absorbed hard-X-ray spectrum suggest that this source could be a new supergiant fast X-ray transient.

Petre, Robert↗

DOE OSTI2023

In Situ Infrared Spectroscopy of a Plasma Jet and Data-Driven Solution of Multi-Scale Plasma Chemistry Problems

Multi-scale problems are commonly known in many scientific and engineering fields where microscopic behaviors are coupled with macroscopic processes. This is also an unsolved problem in low-temperature plasma chemistry where hundreds of chemical species are involved in thousands of chemical reactions. To address this problem, a physics-informed data-driven modeling is developed to solve such a multi-scale problem using the experimental Fourier-transform infrared spectroscopy (FTIR) measurements of several species’ concentrations. The modeling based on modern machine learning techniques provides concentrations of other relevant species along with the electron temperature and gas temperature at the location of FTIR measurements. For example, the concentrations O, OH, and H 2 O 2 play key roles in plasma-based cancer therapy. This approach overcomes the multi-scale difficulties of microscopic low-temperature plasma chemistry coupling with macroscopic gas flow and allows the acquisition of a full picture of output species concentrations. Presented here for the helium-air jet at atmospheric pressure, the ML-based modeling can be used to describe and possibly control multiscale systems using partial experimental data sets.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS1998

Measurements of the Plasma Parameters and Low Frequency Oscillations in the Fisk Plasma Source

A new plasma device, the Fisk Plasma Source (FPS), has been developed at Fisk University. This plasma device is used to study the physics of low temperature plasmas and plasma-material interactions. The FPS device is a stainless steel vacuum 6-way cross vacuum vessel with at 10-inch inner diameter. Low temperature argon plasmas are generated using DC glow discharge and thermionic filament techniques. Spatial profiles of the plasma density, plasma potential, and electron temperature are measured using Langmuir probes. We present initial experimental measurements of density and temperature profiles in the FPS device. Experimental and theoretical studies of low frequency oscillations observed in the FPS device are also presented.

Thomas, Edward, Jr.↗

DOE OSTI2024

Process Intensification by One-Step, Plasma-Assisted Catalytic Synthesis of Liquid Chemicals from Light Hydrocarbons

In this project, we present a plasma-assisted, catalytic process that can handle variations in production rates and gas compositions of producing wells and reliably converts the hydrocarbons to gas phase olefins, high molecular weight alkanes, and liquid chemicals. The low-temperature plasma serves as a reactive chemical environment that activates and converts the light hydrocarbons to these valuable products. We present results from the integration of a catalyst into the low-temperature plasma zone to improve reaction efficiency and product selectivity. We show that the gas composition, bulk gas temperature, and input power of the plasma, with and without catalysts, influence the production rates of liquids from natural gas feeds.

03 NATURAL GAS↗

DOE OSTI2021

Observation of fully detached divertor integrated with improved core confinement for tokamak fusion plasmas

Integration of divertor detachment with a high-performance (β N ~ 3, β p > 2, H 98 ~ 1.5) core plasma has been demonstrated in DIII-D high-β p (poloidal beta) plasmas associated with a sustained core internal transport barrier (ITB) and an H-mode edge transport barrier (ETB). Such good core-edge integration has been achieved for both neon and nitrogen seeding, for both favorable and unfavorable B-field directions, independently from the impurity puffing locations, though these variations play important roles on divertor characteristics. Compared to the standard H-mode plasmas, the high-β p plasma exhibits a much wider window of detachment compatible with high confinement core. Fully detached divertor plasmas with low plasma temperature (Te < 5 eV), low particle flux, and low heat flux across the entire divertor target plate were obtained by using nitrogen seeding. This detached high-β p plasma is compatible with a newly developed detachment control system which can help optimize the nitrogen gas flow rate. Several features, i.e., the high edge safety factor in the high-β p scenario, impurity injection, closed divertor and reduced heating power requirement due to the high confinement, facilitate the achievement of full divertor detachment at lower density. Instead of degrading global performance, the divertor detachment facilitates the access to an even stronger ITB at large radius with a relatively weak ETB through self-organized synergy between ITB and ETB, leading to sustained high confinement. The strengthening of the large-radius ITB compensates for the ETB degradation associated with divertor detachment. In addition, a weak ETB naturally has smaller edge localized modes (ELMs). In particular, with neon injection, a long-period no-ELM H-mode phase has been achieved simultaneously with high-performance core and partially detached divertor plasmas. Furthermore, these results demonstrate the possibility of integrating excellent core plasma performance with an effective divertor solution, an essential step toward steady-state operation of reactor-grade plasmas.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

NASA NTRS2010

Titanium Hydroxide - a Volatile Species at High Temperature

Nguyen, QuynhGiao N.↗

NASA NTRS2010

Selective Functionalization of Carbon Nanotubes: Part II

An alternative method of low-temperature plasma functionalization of carbon nanotubes provides for the simultaneous attachment of molecular groups of multiple (typically two or three) different species or different mixtures of species to carbon nanotubes at different locations within the same apparatus. This method is based on similar principles, and involves the use of mostly the same basic apparatus, as those of the methods described in "Low-Temperature Plasma Functionalization of Carbon Nanotubes" (ARC-14661-1), NASA Tech Briefs, Vol. 28, No. 5 (May 2004), page 45. The figure schematically depicts the basic apparatus used in the aforementioned method, with emphasis on features that distinguish the present alternative method from the other. In this method, one exploits the fact that the composition of the deposition plasma changes as the plasma flows from its source in the precursor chamber toward the nanotubes in the target chamber. As a result, carbon nanotubes mounted in the target chamber at different flow distances (d1, d2, d3 . . .) from the precursor chamber become functionalized with different species or different mixtures of species. In one series of experiments to demonstrate this method, N2 was used as the precursor gas. After the functionalization process, the carbon nanotubes from three different positions in the target chamber were examined by Fourier-transform infrared spectroscopy to identify the molecular groups that had become attached. On carbon nanotubes from d1 = 1 cm, the attached molecular groups were found to be predominantly C-N and C=N. On carbon nanotubes from d2 = 2.5 cm, the attached molecular groups were found to be predominantly C-(NH)2 and/or C=NH2. (The H2 was believed to originate as residual hydrogen present in the nanotubes.) On carbon nanotubes from d3 = 7 cm no functionalization could be detected - perhaps, it was conjectured, because this distance is downstream of the plasma source, all of the free ions and free radicals of the plasma had recombined into molecules.

Meyyappan, Meyya↗

DOE OSTI2026

Dielectric Resonator Design for Low Power and Low Temperature Microwave Plasma

Waveguide-based microwave plasmas generally operate at high temperatures (2000 - 6000K)[1], making it difficult to directly interface solid materials with the plasma without significant thermal damage. Dielectric microwave resonators (DMRs), long studied for wave-based manipulation of electromagnetic radiation for telecom and optics, can focus radiation to extremely small mode volumes, creating intense localized fields with low-power input.[2] This phenomenon can be used for applications ranging from efficient plasma electronics to near-ambient plasma-materials interactions. Such DMR-based plasmas have been demonstrated a handful of times in the literature, but the majority of research towards this utilize the lowest frequency resonance mode.[3], [4], [5] By carefully controlling the geometry of cylindrical resonators, a variety of electromagnetic modes can be excited. In this work, COMSOL Multiphysics simulations are used to study the electric field enhancement and absorption properties of CaTiO3 DMRs as a function of geometry and excitation frequency. Whereas previous studies have utilized the HEM111 resonance frequency to drive low power plasma excitation, we find that higher order resonance frequencies are more effective at field enhancement and result in less power loss within the dielectric material, hence less wasted heating. The effectiveness of these modes is also geometry dependent and can be computationally optimized for plasma generation. Complementing these computational efforts, we demonstrate a new closed-system reactor design built in a WR-650 waveguide and experimentally demonstrate the formation of atmospheric argon microwave plasma using < 30 W input power on DMR dimers. We observe a shifting resonance frequency as the DMRs heat in response to microwave excitation and develop a Python-based lock-in mechanism to effectively track the DMR resonance over time, leading to stable plasma operation. We use infrared thermal imaging to monitor the temperature of the DMR dimers and surrounding quartz chamber, demonstrating thermal temperatures < 60 degreesC. Finally, we utilize optical emission spectroscopy (OES) to probe the plasma properties as a function of the resonance mode.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗