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At least 523 records · Page 29

Nonlinear spectral analysis of ion acoustic solitons arising from a streaming charged object using the numerical inverse scattering transform

Observations of nonlinear coherent plasma phenomena in spacecraft and terrestrial experiments often rely on visual identification of solitary modes because nonlinear coherent modes are broadband in a Fourier transform based analysis. We implement an alternative spectral decomposition known as the inverse scattering transform and demonstrate its ability to successfully isolate nonlinear modes on the homogeneous and forced Korteweg–De Vries equation which models these nonlinear modes. We also demonstrate for the first time that this decomposition is useful when forcing is applied. This is because the stable modes generated by localized forcing are similar to the homogeneous solutions where the inverse scattering transform is a rigorous decomposition. This spectral technique is then applied to simulations of ion acoustic waves generated by a 10 mm spherical debris object interacting with the ionospheric plasma orbiting at 2000 km altitude. The algorithm is found to successfully detect the resultant solitons. This demonstrates the feasibility of using this spectral technique as a real time analysis tool for screening spacecraft data for nonlinear solitary modes.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Towards a heat- and mass-balanced kinetic model of TATB decomposition

We report TATB (1,3,5-triamino-2,4,6-trinitrobenzene) was thermally degraded by two small-scale analytical methods – simultaneous differential scanning calorimetry and thermogravimetric analysis (SDT) and a hot-stage microscope with Fourier Transform Infrared (FTIR) analysis capabilities. SDT used ramped heating, isothermal soaking, and thermal pretreatment at various conditions. The heat flow and mass loss were monitored during various treatment conditions to derive chemical decomposition kinetics and Arrhenius parameters. FTIR experiments used isothermal heating, and changes were monitored spectroscopically. Solid samples generated at specific conditions were collected from both methods and were analyzed by DMSO extraction followed by chemical speciation by optical and mass spectrometric methods. Characterization provided the following reaction insights: TATB decreases in a sigmoidal pattern in isothermally heated samples. Other soluble products gradually increase in concentration and then abruptly decline in concentration during the second exotherm, such as diamino-dinitro-benzofurazan and amino-nitro-benzodifurazan. FTIR showed gradual changes in the amino and nitro functionality, shifting positions and decreasing intensity for the first 40 min. Then the solid gradually appeared more like an amorphous C with N incorporated, similar to previous studies on thermally degraded TATB-type materials. Extracted residues (DMSO-soluble components removed) examined by FTIR showed an abrupt change in chemical composition between 40- and 45-min isothermal treatment, indicating early forming solids are different than later forming residues. A reliable mass- and energy-balanced global reaction network must include at least two autocatalytic reactions, either in parallel or series, and at least one must have an explicit initiation reaction having a low activation energy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Reactivity of CO 2 with Utica, Marcellus, Barnett, and Eagle Ford Shales and Impact on Permeability

We report that in order to reduce greenhouse gas emissions while recovering hydrocarbons from unconventional shale formations, processes that make use of carbon dioxide to enhance oil recovery while storing carbon dioxide (CO 2 ) should be considered. Here, we examine samples from three shale basins across the United States (Utica and Marcellus Shales in the Appalachian Basin, Barnett Shale in the Bend Arch-Ft. Worth Basin, and Eagle Ford in the Western Gulf Basin) to address the following questions: (1) do changes from reaction with CO 2 and fluids at the micrometer and nanometer scale alter flow pathways and, in turn, impact hydrocarbon production, CO 2 storage, and seal integrity and (2) can CO 2 or fluid reactivity be predicted based on physical or chemical properties of shale formations? Experiments were conducted at 40 °C and 10.3 MPa to characterize the interaction between CO 2 and shale using X-ray diffraction (XRD), carbon and sulfur analysis, in situ Fourier transform infrared spectroscopy (FT-IR), feature relocation scanning electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS), mercury (Hg) intrusion porosimetry, and Brunauer-Emmett-Teller (BET) surface area and pore size analysis coupled with density functional theory (DFT) methods. Changes in mechanical, physical, and flow properties of shale cores due to CO 2 exposure were addressed using a New England Research Autolab 1500 and Xenon X-ray computed tomography (CT) scanning. Results showed that CO 2 did not promote significant reactivity with the shale if water was not present; only shales with swelling clays or residual interstitial pore water reacted with dry CO 2 to promote reactivity in shale. When water was added as a reactant, CO 2 formed carbonic acid and reacted with the shale to dissolve carbonate pockets, etched and pitted the shale matrix surfaces, and increased the microporosity and decreased nanoporosity. Porosity and permeability increased appreciably in core shale samples after exposure to CO 2 saturated fluid due to dissolution of carbonate. Shale mechanical properties were not altered. Trends were not observed that could tie CO 2 or fluid reactivity to physical or chemical properties of the shale formations at the basin scale from the samples we examined. However, if the shale contained significant amounts of carbonate and water was available to react with the CO 2 , pore sizes were altered in the matrix and permeability and porosity increased.

04 OIL SHALES AND TAR SANDS↗

Acousto-ultrasonic measurements to monitor damage during fatigue of composites

An acousto-ultrasonic nondestructive testing method used to monitor damage during static and fatigue loading of thin graphite epoxy laminates is described. The experimental procedure, the signal analysis by the Fast Fourier Transform (FFT) algorithm, and the results of this analysis are discussed. Quasi-static tension tests showed a sharp decrease in the quantitative parameters when transverse cracks developed in the 90 degrees plies of a (0, 90/2/)s laminate. When internal micro-delaminations unite to form macro-delaminations, a sharp decrease in the parameters is also observed. The parameters are found to correlate well with other indications of damage development such as stiffness and degradation. The root mean square value of the moment is found to be more sensitive to damage than stiffness. Various signals and spectrums of graphite epoxy systems are presented.

Govada, A.↗

Use of kaolinite clays in development of a low carbon MgO-clay binder system

Magnesium oxide based cements may provide a promising alternative to the conventional Portland cement in many applications. This study investigates the feasibility of using calcined kaolinitic clay to produce an MgO binder. The MgO-based binder were prepared using a low kaolinite content clay and metakaolin and were compared with a silica fume system. Implications of the addition of magnesium carbonate in the binder were also investigated. Isothermal calorimetry, X-ray diffraction (XRD), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) were used to study the hydration characteristics of the binder system whereas compressive strength and porosity were measured to determine mechanical and durability attributes. The economic and environmental aspects of the binder system is also discussed. Hydrotalcite like phases were clearly produced on hydration in the clay mixes containing carbonate additions. The compressive strength of clay mixes was at par or better compared to systems containing silica fume, and the clay systems had significantly lower porosity levels. The presence of magnesium carbonate further enhanced the physical properties of the clay mixes.

36 MATERIALS SCIENCE↗

Analysis of a thioether lubricant by infrared Fourier microemission spectrophotometry

An infrared Fourier microemission spectrophotometer is used to obtain spectra (wavenumber range, 630 to 1230 0.1 cm) from microgram quantities of thioether lubricant samples deposited on aluminum foil. Infrared bands in the spectra are reproducible and could be identified as originating from aromatic species (1,3-disubstituted benzenes). Spectra from all samples (neat and formulated, used and unused) are very similar. Additives (an acid and a phosphinate) present in low concentration (0.10 percent) in the formulated fluid are not detected. This instrument appears to be a viable tool in helping to identify lubricant components separated by liquid chromatography.

Jones, W. R., Jr.↗

Relaxation factors for supercritical flows.

Relaxation procedures for solution of steady supercritical transonic flows are investigated. Von Neumann (Fourier-mode) stability analysis is used to find bounds of relaxation factors. The bounds depend on local Mach number and local mesh aspect ratio. Long wave instability of Murman-Cole implicit method is indicated. Two new relaxation procedures are introduced. Both employ central differencing exclusively. Group velocities of Fourier modes are used to study signal propagation. It was found necessary to avoid or to damp out signals propagating upstream in supersonic zones in order to obtain physically meaningful transonic solutions. It appears that requirements of high rate of convergence, of stability and accuracy, are in conflict, and that a combination of relaxation methods must be used in order not to compromise the requirements.

Kentzer, C. P.↗

Refraction of coastal ocean waves

Refraction of gravity waves in the coastal area off Cape Hatteras, NC as documented by synthetic aperture radar (SAR) imagery from Seasat orbit 974 (collected on September 3, 1978) is discussed. An analysis of optical Fourier transforms (OFTs) from more than 70 geographical positions yields estimates of wavelength and wave direction for each position. In addition, independent estimates of the same two quantities are calculated using two simple theoretical wave-refraction models. The OFT results are then compared with the theoretical results. A statistical analysis shows a significant degree of linear correlation between the data sets. This is considered to indicate that the Seasat SAR produces imagery whose clarity is sufficient to show the refraction of gravity waves in shallow water.

Shuchman, R. A.↗

Welch Method and Bootstrapping Applied to Subcritical Gamma Noise

We measured the prompt neutron decay constant 𝛼 of the CROCUS zero-power reactor at the Swiss Federal Institute of Technology Lausanne using cross-power spectral density (CPSD) analysis of gamma-gamma correlations from two trans-stilbene organic scintillators positioned near the reactor core. We measured critical and subcritical states, with water levels ranging from 960 mm (critical) to 800 mm (𝜌=−1.4 $ subcritical). Our analysis used the Welch method, dividing signal segments for fast Fourier transform (FFT) frequency analysis and applying bootstrapping uncertainty quantification that uses Welch-defined segments. Results demonstrated a clear increase in the measured 𝛼 as reactor reactivity decreased, distinguishing critical from subcritical conditions. At the 960-mm critical level, 𝛼 was estimated at 155.9 ± 0.7 s −1 , and for the 800-mm subcritical level, 𝛼 increased significantly to 367.3 ± 6.9 s –1 . A linear regression of subcritical states yielded a critical estimate of 154.0 ± 3.1 s –1 , aligning with the static 𝛼 estimate at critical. The bootstrapping method produced normally distributed 𝛼 estimates, confirming data consistency. The gamma CPSD 𝛼 estimates clearly distinguish reactor states and improve monitoring of zero-power reactors. The future deployment of modular and microreactors as potential candidates for noise analysis is demonstrated in CROCUS, particularly zero-power mock-ups of new designs. The improvement of noise analysis in the subcritical domain from this work will support experimental data for reactor deployment and procedure.

CROCUS↗

Influence of plasticizers on thermal and mechanical properties of biocomposite filaments made from lignin and polylactic acid for 3D printing

Polylactic acid (PLA) and organosolv lignin were mixed at different ratios and extruded to obtain PLA-lignin composite filaments. PLA was replaced with lignin up to 20 wt%. Two plasticizers (polyethylene glycol (PEG) 2000 and struktol TR451) were added in varying concentrations to enhance the properties of PLA_L20 (20% lignin in PLA) composite filaments. Furthermore, the effect of lignin in PLA, and PEG, and struktol in PLA_L20 composites was investigated via tensile test, differential scanning calorimetry, thermogravimetric analysis, scanning electron microscopy, Fourier transform infrared spectroscopy of the filaments, and dynamic mechanical analysis of 3D printed samples. A 2 wt% PEG was able to enhance both tensile stress and elongation at maximum load of PLA_L20 composite by 19% and 35%, respectively, whereas struktol TR451 was able to improve elongation at maximum load by 24%.

3D printing↗

On the Hilbert-Huang Transform Theoretical Developments

One of the main heritage tools used in scientific and engineering data spectrum analysis is the Fourier Integral Transform and its high performance digital equivalent - the Fast Fourier Transform (FFT). Both carry strong a-priori assumptions about the source data, such as linearity, of being stationary, and of satisfying the Dirichlet conditions. A recent development at the National Aeronautics and Space Administration (NASA) Goddard Space Flight Center (GSFC), known as the Hilbert-Huang Transform (HHT), proposes a novel approach to the solution for the nonlinear class of spectrum analysis problems. Using a-posteriori data processing based on the Empirical Mode Decomposition (EMD) sifting process (algorithm), followed by the normalized Hilbert Transform of the decomposition data, the HHT allows spectrum analysis of nonlinear and nonstationary data. The EMD sifting process results in a non-constrained decomposition of a source real value data vector into a finite set of Intrinsic Mode Functions (IMF). These functions form a near orthogonal adaptive basis, a basis that is derived from the data. The IMFs can be further analyzed for spectrum interpretation by the classical Hilbert Transform. A new engineering spectrum analysis tool using HHT has been developed at NASA GSFC, the HHT Data Processing System (HHT-DPS). As the HHT-DPS has been successfully used and commercialized, new applications post additional questions about the theoretical basis behind the HHT and EMD algorithms. Why is the fastest changing component of a composite signal being sifted out first in the EMD sifting process? Why does the EMD sifting process seemingly converge and why does it converge rapidly? Does an IMF have a distinctive structure? Why are the IMFs near orthogonal? We address these questions and develop the initial theoretical background for the HHT. This will contribute to the developments of new HHT processing options, such as real-time and 2-D processing using Field Programmable Array (FPGA) computational resources, enhanced HHT synthesis, and broaden the scope of HHT applications for signal processing.

Kizhner, Semion↗

On Certain Theoretical Developments Underlying the Hilbert-Huang Transform

One of the main traditional tools used in scientific and engineering data spectral analysis is the Fourier Integral Transform and its high performance digital equivalent - the Fast Fourier Transform (FFT). Both carry strong a-priori assumptions about the source data, such as being linear and stationary, and of satisfying the Dirichlet conditions. A recent development at the National Aeronautics and Space Administration (NASA) Goddard Space Flight Center (GSFC), known as the Hilbert-Huang Transform (HHT), proposes a novel approach to the solution for the nonlinear class of spectral analysis problems. Using a-posteriori data processing based on the Empirical Mode Decomposition (EMD) sifting process (algorithm), followed by the normalized Hilbert Transform of the decomposed data, the HHT allows spectral analysis of nonlinear and nonstationary data. The EMD sifting process results in a non-constrained decomposition of a source real-value data vector into a finite set of Intrinsic Mode Functions (IMF). These functions form a nearly orthogonal derived from the data (adaptive) basis. The IMFs can be further analyzed for spectrum content by using the classical Hilbert Transform. A new engineering spectral analysis tool using HHT has been developed at NASA GSFC, the HHT Data Processing System (HHT-DPS). As the HHT-DPS has been successfully used and commercialized, new applications pose additional questions about the theoretical basis behind the HHT and EMD algorithms. Why is the fastest changing component of a composite signal being sifted out first in the EMD sifting process? Why does the EMD sifting process seemingly converge and why does it converge rapidly? Does an IMF have a distinctive structure? Why are the IMFs nearly orthogonal? We address these questions and develop the initial theoretical background for the HHT. This will contribute to the development of new HHT processing options, such as real-time and 2-D processing using Field Programmable Gate Array (FPGA) computational resources,

Kizhner, Semion↗

On the Hilbert-Huang Transform Data Processing System Development

One of the main heritage tools used in scientific and engineering data spectrum analysis is the Fourier Integral Transform and its high performance digital equivalent - the Fast Fourier Transform (FFT). The Fourier view of nonlinear mechanics that had existed for a long time, and the associated FFT (fairly recent development), carry strong a-priori assumptions about the source data, such as linearity and of being stationary. Natural phenomena measurements are essentially nonlinear and nonstationary. A very recent development at the National Aeronautics and Space Administration (NASA) Goddard Space Flight Center (GSFC), known as the Hilbert-Huang Transform (HHT) proposes a novel approach to the solution for the nonlinear class of spectrum analysis problems. Using the Empirical Mode Decomposition (EMD) followed by the Hilbert Transform of the empirical decomposition data (HT), the HHT allows spectrum analysis of nonlinear and nonstationary data by using an engineering a-posteriori data processing, based on the EMD algorithm. This results in a non-constrained decomposition of a source real value data vector into a finite set of Intrinsic Mode Functions (IMF) that can be further analyzed for spectrum interpretation by the classical Hilbert Transform. This paper describes phase one of the development of a new engineering tool, the HHT Data Processing System (HHTDPS). The HHTDPS allows applying the "T to a data vector in a fashion similar to the heritage FFT. It is a generic, low cost, high performance personal computer (PC) based system that implements the HHT computational algorithms in a user friendly, file driven environment. This paper also presents a quantitative analysis for a complex waveform data sample, a summary of technology commercialization efforts and the lessons learned from this new technology development.

Kizhner, Semion↗

Buoyancy Effects on Flow Structure and Instability of Low-Density Gas Jets

A low-density gas jet injected into a high-density ambient gas is known to exhibit self-excited global oscillations accompanied by large vortical structures interacting with the flow field. The primary objective of the proposed research is to study buoyancy effects on the origin and nature of the flow instability and structure in the near-field of low-density gas jets. Quantitative rainbow schlieren deflectometry, Computational fluid dynamics (CFD) and Linear stability analysis were the techniques employed to scale the buoyancy effects. The formation and evolution of vortices and scalar structure of the flow field are investigated in buoyant helium jets discharged from a vertical tube into quiescent air. Oscillations at identical frequency were observed throughout the flow field. The evolving flow structure is described by helium mole percentage contours during an oscillation cycle. Instantaneous, mean, and RMS concentration profiles are presented to describe interactions of the vortex with the jet flow. Oscillations in a narrow wake region near the jet exit are shown to spread through the jet core near the downstream location of the vortex formation. The effects of jet Richardson number on characteristics of vortex and flow field are investigated and discussed. The laminar, axisymmetric, unsteady jet flow of helium injected into air was simulated using CFD. Global oscillations were observed in the flow field. The computed oscillation frequency agreed qualitatively with the experimentally measured frequency. Contours of helium concentration, vorticity and velocity provided information about the evolution and propagation of vortices in the oscillating flow field. Buoyancy effects on the instability mode were evaluated by rainbow schlieren flow visualization and concentration measurements in the near-field of self-excited helium jets undergoing gravitational change in the microgravity environment of 2.2s drop tower at NASA John H. Glenn Research Center. The jet Reynolds number was varied from 200 to 1500 and jet Richardson number was varied from 0.72 to 0.002. Power spectra plots generated from Fast Fourier Transform (FFT) analysis of angular deflection data acquired at a temporal resolution of 1000Hz reveal substantial damping of the oscillation amplitude in microgravity at low Richardson numbers (~0.002). Quantitative concentration data in the form of spatial and temporal evolutions of the instability data in Earth gravity and microgravity reveal significant variations in the jet flow structure upon removal of buoyancy forces. Radial variation of the frequency spectra and time traces of helium concentration revealed the importance of gravitational effects in the jet shear layer region. Linear temporal and spatio-temporal stability analyses of a low-density round gas jet injected into a high-density ambient gas were performed by assuming hyper-tan mean velocity and density profiles. The flow was assumed to be non parallel. Viscous and diffusive effects were ignored. The mean flow parameters were represented as the sum of the mean value and a small normal-mode fluctuation. A second order differential equation governing the pressure disturbance amplitude was derived from the basic conservation equations. The effects of the inhomogeneous shear layer and the Froude number (signifying the effects of gravity) on the temporal and spatio-temporal results were delineated. A decrease in the density ratio (ratio of the density of the jet to the density of the ambient gas) resulted in an increase in the temporal amplification rate of the disturbances. The temporal growth rate of the disturbances increased as the Froude number was reduced. The spatio-temporal analysis performed to determine the absolute instability characteristics of the jet yield positive absolute temporal growth rates at all Fr and different axial locations. As buoyancy was removed (Fr . 8), the previously existing absolute instability disappeared at all locations establhing buoyancy as the primary instability mechanism in self-excited low-density jets.

Pasumarthi, Kasyap Sriramachandra↗

Chemically Recyclable Polyester Thermosets from Activated Adipic Acid and Renewable Polyols

This study outlines a method for producing chemically recyclable crosslinked polyesters using renewable polyols-glycerol and sorbitol-combined with adipic acid (AA), which is transformed/activated into a polyanhydride mixture prior to use. A three-step procedure has been designed: 1) an acid-catalyzed reaction of AA with nontoxic isopropenyl acetate or acetic anhydride to form a crosslinking mixture (CLM) made of adipic-acetic mixed polyanhydrides; 2) a solvent- and additive-free process where glycerol or sorbitol, or a combination thereof, is reacted with the CLM to achieve a prepolymer, and 3) a casting/molding of the liquid viscous prepolymer to yield a thermoset as the end product. Different thermosets (eight examples) are prepared by changing the reagents ratio. These solids are thoroughly characterized by tensile tests, DMA, high-resolution magic angle spinning and solid-state NMR, thermal gravimetric analysis, DSC, and fourier transformed infra red (FT-IR) spectroscopy. The formation of cross-linked polyesters is confirmed in all cases, but mechanical properties varied significantly from one specimen to another. Interestingly, a tensile strength up to 18 MPa-approximately an order of magnitude higher than similar polymers-is achieved when sorbitol and the CLM are used in a 1:1 wt% ratio. The chemical recycle of the resulting polymers is achieved via methanolysis with quantitative recovery of the monomeric units.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermo-mechanical deterioration and molecular degradation of 3D-printed methacrylate-based polymer in various chemical environments

The advancement of additive manufacturing (AM) has accelerated the development of stereolithographic (SLA) photo-curable resins, particularly methacrylate-based polymers, due to the ability to their high-resolution, robust mechanical properties, and suitability. However, their long-term performance in chemical environments remains poorly understood. This study investigates the extent and mechanisms of degradation on an SLA-printed methacrylate-based polymer subjected to various chemicals, including polar and non-polar solvents, as well as strongly acidic aqueous solutions over a 12-week accelerated aging period. A comprehensive analytical approach incorporating swelling kinetics, surface morphology, tensile and dynamic mechanical analysis (DMA), Fourier-transform infrared (FTIR) spectroscopy, and mass spectrometry (MS) was employed to characterize chemical absorption, structural integrity, and leached products. Results reveal that degradation severity is governed by both the polarity and reactivity of the chemical environment. Notably, exposure to 6 mol L -1 HNO₃ induced the most severe deterioration, with over threefold higher swelling compared to other media, and significant reductions in tensile strength, tensile modulus, and glass transition temperature (T g ). In contrast, specimens aged in non-polar solvents (xylene and dodecane) exhibited negligible chemical interaction and retained mechanical performance. FTIR and MS analyses identified acid-catalyzed hydrolysis of ester groups as prominent degradation pathways in acidic media, while diffusion-controlled plasticization prevailed in polar solvents. Furthermore, this study provides valuable insights into the chemical stability of SLA-printed polymers and develops predictive degradation profiles that are crucial for designing durable polymer systems for advanced industrial use.

36 MATERIALS SCIENCE↗

Determination of the regeneration energy of direct air capture solvents/sorbents using calorimetric methods

Regeneration energy and recyclability are important parameters that dictate the viability of a CO 2 direct air capture (DAC) process. In this study, differential scanning calorimetry (DSC) is used in conjunction with thermogravimetric analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR) to evaluate the regeneration energy required for CO 2 -loaded 3 M aqueous potassium sarcosinate (K-SAR) solvent and crystalline methyl-glyoxal-bisiminoguanidine (MGBIG) sorbent. Based on calorimetric measurements, for aqueous K-SAR, the sensible heat amounts to 1.5 GJ/tCO 2 and the enthalpy of desorption is estimated at 3.68 GJ/tCO 2 . The total energy of regeneration will also include the enthalpy of solvent vaporization, which will depend on the thermodynamic conditions and the level of regeneration. For MGBIG, the total regeneration energy required was measured at approximately 7.0 GJ/tCO 2 . Further, FTIR measurements were used to observe CO 2 and H 2 O release during the thermal regeneration process. For K-SAR, CO 2 release is seen to take place at temperatures greater than 80 °C and, for MGBIG, the CO 2 release takes place at temperatures greater than 100 °C. The moderate temperatures required for K-SAR and MGBIG regenerations compared to other DAC solvents/sorbents suggest that low-cost sources of heat, such as geothermal heat, could potentially be used for regeneration to drive down the cost of direct air capture.

42 ENGINEERING↗

Design, Synthesis, and Characterization of Polymer Precursors to Li x PON and Li x SiPON Glasses: Materials That Enable All-Solid-State Batteries (ASBs)

LiPON-like glasses that form lithium dendrite impenetrable interfaces between lithium battery components are enabling materials that may replace liquid electrolytes permitting production of all-solid-state batteries (ASBs). Unfortunately, to date, such materials are introduced only via gas-phase deposition. Furthermore, we demonstrate the design and synthesis of easily scaled, lowtemperature, low-cost, solution-processable inorganic polymers containing LiPON/LiSiPON elements. OPCl 3 and hexachlorophosphazene [Cl 2 P=N] 3 provide starting points for elaboration using MNH 2 (M = Li/Na) or (Me 3 Si)NH followed by reaction with controlled amounts of LiNH 2 to produce oligomers/polymers with molecular weights (MWs) ≈1–2 kDa characterized by multinuclear NMR, gel permeation chromatography (GPC), thermogravimetric analysis (TGA), Fourier-transform infrared (FTIR), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and matrix-assisted laser desorption/ ionization (MALDI)-time-of-flight (ToF) offering stabilities to 150–200 °C and ceramic yields (800 °C) of 50–60%. 7 Li NMR suggests that precursor-bound Li + dissociates easily, beneficial for electrochemical applications. XPS shows higher N/P ratios (1–3) than via gas-phase methods (<1) correlating N/P ratios, 7 Li shifts, and Li + conductivities. Li 2 SiPHN offers the highest ambient conductivity of 3 × 10 –1 mS cm –1 at 400 °C/2 h/N 2 .

36 MATERIALS SCIENCE↗