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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 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Initial results from boron powder injection experiments in WEST lower single null L-mode plasmas

Using a recently installed impurity powder dropper (IPD), boron powder (<150 μm) was injected into lower single null (LSN) L-mode discharges in WEST. IPDs possibly enable real-time wall conditioning of the plasma-facing components and may help to facilitate H-mode access in the full-tungsten environment of WEST. The discharges in this experiment featured I p = 0.5 MA, B T = 3.7 T, q 95 = 4.3, t pulse = 12–30 s, n e,0 ~ 4 × 10 19 m –2 , and P LHCD ~ 4.5 MW. Estimates of the deuterium and impurity particle fluxes, derived from a combination of visible spectroscopy measurements and their corresponding S/XB coefficients, showed decreases of ~50% in O + , N + , and C + populations during powder injection and a moderate reduction of these low-Z impurities (~50%) and W (~10%) in the discharges that followed powder injection. Along with the improved wall conditions, WEST discharges with B powder injection observed improved confinement, as the stored energy W MHD , neutron rate, and electron temperature T e increased significantly (10%–25% for W MHD and 60%–200% for the neutron rate) at constant input power. Notably, these increases in confinement scale up with the powder drop rate and are likely due to the suppression of ion temperature gradient (ITG) turbulence from changes in Z eff and/or modifications to the electron density profile.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2025

Electromagnetic moments of 215,217 Bi: Probing shell evolution beyond N = 126

The nuclear properties of bismuth isotopes (Z = 83) , with just one valence proton above the closed spherical shell at (Z = 82) , are expected to be governed by a single unpaired proton. However, already in semimagic 209 Bi (Z = 83, N = 126) , , the magnetic moment (μ) strongly deviates from the single-particle Schmidt value. A near linear decrease in μ with the increase of N after the N = 126 magic number was observed up to N = 130 . In order to test whether this trend is kept at N > 130 and to reveal the underlying mechanisms, an investigation of 215,217 Bi (N = 132, 134) has been undertaken. The magnetic dipole and electric quadrupole moments of the I π = 9/2 - nuclear ground states in these isotopes have been measured for the first time using the in-source resonance-ionization spectroscopy technique at ISOLDE (CERN). It has been shown that the linearly decreasing trend of μ( 209,211,213 Bi g ) is broken in 215,217 Bi with a nearly constant value of μ observed. Experimental data have been compared to calculations in the framework of the configuration-interaction shell model with the monopole-based universal V MU +LS interaction. The peculiarities in the behavior of μ(Bi, 9/2 - ) with increasing neutron number are explained as being due to the shell evolution, change of the neutron orbitals occupancies and strong configuration mixing beyond N = 130 . Also, the difference in the μ trends for bismuth (Z = 83) and astatine (Z = 85) isotopes with N > 126 are reproduced by the shell-model calculations. It is shown that monopole interaction plays noticeable role in the description of the peculiarities of the μ behaviour. Additionally, the extension of the application of the V MU interaction to the μ isotopic trends for heavy nuclei is important for further study of the capabilities of this promising version of the shell-model calculations.

Dipole magnetic moments↗
DOE OSTI2020

Ni Nanoparticles on CeO 2 (111): Energetics, Electron Transfer, and Structure by Ni Adsorption Calorimetry, Spectroscopies, and Density Functional Theory

The morphology, interfacial bonding energetics and charge transfer of Ni clusters and nanoparticles on slightly-reduced CeO 2-x (111) surfaces at 100 to 300 K have been studied using single crystal adsorption calorimetry (SCAC), low-energy ion scattering spectroscopy (LEIS), Xray photoelectron spectroscopy (XPS), low energy electron diffraction (LEED) and density functional theory (DFT). The initial heat of adsorption of Ni vapor decreased with the extent of pre-reduction (x) of the CeO 2-x (111), showing that stoichiometric ceria adsorbs Ni more strongly than oxygen vacancies. On CeO 1.95 (111) at 300 K, the heat dropped quickly with coverage in the first 0.1 ML, attributed to nucleation of Ni clusters on stoichiometric steps, followed by the Ni particles spreading onto less favorable terrace sites. At 100 K, the clusters nucleate on terraces due to slower diffusion. Adsorbed Ni monomers are in the +2 oxidation state, and they bind by ~45 kJ/mol more strongly to step sites than terraces. The measured heat of adsorption versus average particle size on terraces is favorably compared to DFT calculations. The Ce 3d XPS lineshape showed an increase in Ce 3+ /Ce 4+ ratio with Ni coverage, providing the number of electrons donated to the ceria per Ni atom. The charge transferred per Ni is initially large but strongly decreases with increasing cluster size for both experiments and DFT, and shows large differences between clusters at steps versus terraces. This charge is localized on the interfacial Ni and Ce atoms in their atomic layers closest to the interface. This knowledge is crucial to understanding the nature of the active sites on the surface of Ni-CeO 2 catalysts for which metal-oxide interactions play a very important role in the activation of O-H and C-H bonds. In conclusion, the changes in these interactions with Ni particle size (metal loading) and the extent of reduction of the ceria help to explain how previously reported catalytic activity and selectivity change with these same structural details.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Vertical Gradient of Size-Resolved Aerosol Compositions over the Arctic Reveals Cloud Processed Aerosol in-Cloud and above Cloud

Arctic aerosols play a significant role in the aerosol-radiation and aerosol-cloud interactions, but ground-based measurements are insufficient to explain the interaction of aerosols and clouds in a vertically stratified Arctic atmosphere. This study shows the vertical variability of aerosol particle composition via tethered balloon system at Oliktok Point, Alaska, in August 2019, at different cloud layers for two case studies (background aerosol condition and polluted condition). Multi-modal micro-spectroscopy analysis of samples during the background case reveals a broadening of chemically specific size distribution above cloud top with a high abundance of sulfate and core-shell morphology, suggesting possible cloud processing of aerosols. The pollution case also indicates a broadening of size distribution at the upper cloud layer with the dominance of carbonaceous aerosol, which suggests the potential of carbonaceous aerosols for Arctic cloud formation. Here this study provides insights into the vertical profile of Arctic aerosols on cloud formation.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Ghost-imaging-enhanced noninvasive spectral characterization of stochastic x-ray free-electron-laser pulses

Abstract High-intensity ultrashort X-ray free-electron laser (XFEL) pulses are revolutionizing the study of fundamental nonlinear x-ray matter interactions and coupled electronic and nuclear dynamics. To fully exploit the potential of this powerful tool for advanced x-ray spectroscopies, a noninvasive spectral characterization of incident stochastic XFEL pulses with high resolution is a key requirement. Here we present a methodology that combines high-acceptance angle-resolved photoelectron time-of-flight spectroscopy and ghost imaging to enhance the quality of spectral characterization of x-ray free-electron laser pulses. Implementation of this noninvasive high-resolution x-ray diagnostic can greatly benefit the ultrafast x-ray spectroscopy community by functioning as a transparent beamsplitter for applications such as transient absorption spectroscopy in averaging mode as well as covariance-based x-ray nonlinear spectroscopies in single-shot mode where the shot-to-shot fluctuations inherent to a self-amplified spontaneous emission (SASE) XFEL pulse are a powerful asset.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
NASA NTRS1983

High throughput non-dispersive hard X-ray spectrograph with angular resolution for cosmic bursts, transients, and sources

An instrument concept which offers high throughput nondispersive spectroscopy in the 35-150 keV band for measuring line intensities and widths of faint supernovae is described. The design is based on existing xenon filled, two-dimensional, position sensitive, multiwired proportional counters. Effective detector areas of 1000 sq cm are readily achievable, and expansion to 10,000 sq cm per unit is feasible. Either single-unit or array operation to provide all-sky coverage with one arcmin resolution is possible. The instrument could be used to record gamma ray bursts and would have the capability of distinguishing particle events. Observations could also be made of X ray cyclotron lines and the Ti-44 lines expected to issue from a supernova explosion.

Gorenstein, P.↗
NASA NTRS2003

Nanocrystalline Chalcopyrite Materials (CuInS2 and CuInSe2) via Low-Temperature Pyrolysis of Molecular Single-Source Precursors

Nanometer sized particles of the chalcopyrite compounds CuInS2 and CuInSe2 were synthesized by thermal decomposition of molecular single-source precursors (PPh3)2CuIn(SEt)4 and (PPh3)2CuIn(SePh)4, respectively, in the non-coordinating solvent dioctyl phthalate at temperatures between 200 and 300 C. The nanoparticles range in size from 3 - 30 nm and are aggregated to form roughly spherical clusters of about 500 nm in diameter. X-ray diffraction of the nanoparticle powders shows greatly broadened lines indicative of very small particle sizes, which is confirmed by TEM. Peaks present in the XRD can be indexed to reference patterns for the respective chalcopyrite compounds. Optical spectroscopy and elemental analysis by energy dispersive spectroscopy support the identification of the nanoparticles as chalcopyrites.

Castro, Stephanie L.↗
DOE OSTI2021

Cadmium Magnesium Telluride for Next Generation X-Ray Free Electron Laser, Synchrotron and Many Other Applications

We developed a picosecond photodetector based on our Bridgman grown and specially engineered Cadmium Magnesium Telluride (Cd 1-x Mg x Te) single crystal that is sensitive to both optical and x-ray pulses for coarse timing in Free Electron Laser applications. Cd 1-x Mg x Te is a wide bandgap semiconductor material with potential applications, not only in optoelectronics, but also in particle physics as an intense pulse radiation detector for bremsstrahlung, X-ray/gamma ray radiation, thermal neutrons, and medical imaging. However, for femtosecond optical and x-ray cross correlation, the material has to have very short lifetime, a condition that is opposite to that required for nuclear spectroscopy applications. At the same time, the material also needs to have very low bulk leakage current, in the 0.10 pA range. Hence the ability to tailor or engineer the material is very crucial. In this paper, picosecond response and the crystal growth of this specially engineered cadmium magnesium telluride material will be presented. Other material characterization and transient measurements will also be discussed along with room temperature semiconductor detector performance for other nuclear radiation detection applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Clear as mud redefined: Tunable transparent mineral scaffolds for visualizing microbial processes below ground

Microbes inhabiting complex porous microenvironments in sediments and aquifers catalyze reactions that are critical to global biogeochemical cycles and ecosystem health. However, the opacity and complexity of porous sediment and rock matrices have considerably hindered the study of microbial processes occurring within these habitats. Here, we generated microbially compatible, optically transparent mineral scaffolds to visualize and investigate microbial colonization and activities occurring in these environments, in laboratory settings and in situ. Using inexpensive synthetic cryolite mineral, we produced optically transparent scaffolds mimicking the complex 3D structure of sediments and rocks by adapting a suspension-based, freeze-casting technique commonly used in materials science. Fine-tuning of parameters, such as freezing rate and choice of solvent, provided full control of pore size and architecture. The combined effects of scaffold porosity and structure on the movement of microbe-sized particles, tested using velocity tracking of fluorescent beads, showed diverse yet reproducible behaviors. The scaffolds we produced are compatible with epifluorescence microscopy, allowing the fluorescence-based identification of colonizing microbes by DNA-based staining and fluorescence in situ hybridization (FISH) to depths of 100 µm. Additionally, Raman spectroscopy analysis indicates minimal background signal in regions used for measuring deuterium and 13 C enrichment in microorganisms, highlighting the potential to directly couple D 2 O or 13 C stable isotope probing and Raman-FISH for quantifying microbial activity at the single-cell level. To demonstrate the relevance of cryolite scaffolds for environmental field studies, we visualized their colonization by diverse microorganisms within rhizosphere sediments of a coastal seagrass plant using epifluorescence microscopy. The tool presented here enables highly resolved, spatially explicit, and multimodal investigations into the distribution, activities, and interactions of underground microbes typically obscured within opaque geological materials until now.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Free Space Ramsey Spectroscopy in Rubidium with Noise below the Quantum Projection Limit

In this work, we demonstrate the utility of optical cavity generated spin-squeezed states in free space atomic fountain clocks in ensembles of 390 000 87 Rb atoms. Fluorescence imaging, correlated to an initial quantum nondemolition measurement, is used for population spectroscopy after the atoms are released from a confining lattice. For a free fall time of 4 milliseconds, we resolve a single-shot phase sensitivity of 814(61) microradians, which is 5.8(0.6) decibels (dB) below the quantum projection limit. We observe that this squeezing is preserved as the cloud expands to a roughly 200 μ m radius and falls roughly 300 μm in free space. Ramsey spectroscopy with 240 000 atoms at a 3.6 ms Ramsey time results in a single-shot fractional frequency stability of 8.4(0.2) × 10 –12 , 3.8(0.2) dB below the quantum projection limit. The sensitivity and stability are limited by the technical noise in the fluorescence detection protocol and the microwave system, respectively.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2020

Comparison of active interrogation methods for source location in a scattering and absorbing medium, consisting of PGNAA, and an AmBe quasi-forward biased directional source

Source location of Special Nuclear Material (SNM) encompassing 95% 235 U and 239 Pu is identified by utilizing a directional source from Patent No: US20190013109A1 using Prompt Gamma Neutron Activation Analysis (PGNAA) and neutron spectroscopy simulated with Monte-Carlo N-Particle transport 6.2 (MCNP). BC-408, HPGe, LaBr 3 detector arrays were used to identify the location of the SNM using total counts incident on each detector, and PGNAA photopeaks from HPGe and LaBr 3 detector arrays in a polyethylene shield. The conducted simulations varied the volume and location of the SNM in the MCNP input files to observe how the source location method behaved. PGNAA photopeaks used for source identification include 61 keV from fission, 2.223 MeV prompt gamma from hydrogen, 511 keV annihilation, and a single and double escape peaks from the prompt gamma interaction from hydrogen. The capabilities of each detector systems to acquire well resolved photopeaks with a 1% relative error or less, and total relative error for F4 and F8 tallies were less than 0.015% relative error. Source predictions of the SNM with uneven amounts of polyethylene shielding between the source and detectors was observed to overpredict and give invalid source location predictions. Source locations of the SNM with even amounts of polyethylene material between the source and each detector were found to be valid. With a 1 Ci 241 Am source activity, it was determined that 1630 s were needed to obtain the results for each detector system with the quasi-forward directional AmBe source. Coupling source and material identification together would increase acquisition time but would only require one system to determine.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Chemical Imaging of Atmospheric Biomass Burning Particles from North American Wildfires

The effects of biomass burning aerosols (BBA) on radiative forcing and cloud formation depend on chemical composition and the internal structures of individual particles within smoke plumes. To improve our understanding of the chemical and physical properties of BBA emitted at different times of the day and their evolution during atmospheric aging, we conducted a study as a part of the Fire Influence on Regional to Global Environments and Air Quality field campaign. Particle samples were collected onboard a research aircraft from smoke plumes from a wildfire in eastern Oregon during late afternoon and nighttime flights on August 28, 2019. A time-resolved aerosol collector was used to collect samples on substrates for offline spectromicroscopic imaging to investigate the single-particle characteristics of BBA particles. Approximately 20,400 individual particles from 10 selected samples were analyzed using computer-controlled scanning electron microscopy coupled with energy-dispersive X-ray microanalysis, revealing their elemental composition, morphology, and viscosity. Elemental microanalysis indicated that aged potassium is likely found in the form of K 2 SO 4 , KNO 3 , and possible K-organic salts. Further chemical speciation and carbon bonding mapping within individual particles were conducted using synchrotron-based scanning transmission X-ray microscopy (STXM) coupled with near edge X-ray absorption fine structure (NEXAFS) spectroscopy. Real-time, water-soluble light absorption measurements were acquired using a particle-into-liquid sampler instrument coupled to a liquid waveguide capillary cell and total organic analyzer. In the late afternoon samples, 65% of the total particle number population consisted entirely of organic components, compared to 46% in the nighttime particles. These differences were attributed to discrepancies in composition at the time of emission and to the daytime condensation and accumulation of photochemically formed secondary organic material on existing BBA particles, a process that halts at night. Microscopy images indicated that particle viscosity was lower in the nighttime particles (<10 1 Pa·s), likely due to increased relative humidity and a higher contribution from hygroscopic inorganic components. The chemical heterogeneity of individual particles was quantified using STXM-derived mixing state parameters. The nature of carbon bonding within individual particles was inferred from the extent of carbon sp 2 hybridization derived from NEXAFS spectra. Average percentages of sp 2 hybridization range between 40% and 60%, with no noticeable differences between late afternoon and nighttime flights. These findings were compared with the online optical properties of both late afternoon and nighttime smoke plumes, providing valuable insights into the complex relationship between chemical composition and optical properties of BBA particles at different times of the day.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Gamma-ray imaging of Np-237 metal using an organic glass imager

Neutron and gamma-ray imaging systems are deployed within the field of nuclear safeguards for the detection and localization of special nuclear materials and other materials of interest. 237 Np is one of these materials of interest due its presence in spent nuclear fuel and potential for use in nuclear weapons when purified. Here, for the first time, a 6 kg neptunium sphere (98.8 wt% 237 Np) was measured using a dual-particle imager, from the University of Michigan, consisting of organic glass and inorganic scintillators. The novel composition of organic glass scintillator was recently developed at Sandia National Labs and has been used in particle imaging systems due to its time resolution and particle discrimination capabilities. Gamma-ray energy spectra from single and coincident events were extracted and the sequencing of Compton scatter and photoelectric absorption gamma-ray events was used to generate images using simple backprojection. The emissions of interest in this work are the 312 keV and 416 keV gamma rays from 233 Pa, a daughter isotope from the neptunium decay series. The results of this work show that there is close agreement between the true source location in angular space and the converged location from the gamma ray images created using the system. The gamma spectroscopy from single and coincident events also identified the characteristic emission from the daughter isotope and could be used to assist with the identification of 237 Np. Furthermore, successful localization of the source with 5 s of data demonstrates the practical application of the imaging system for imaging and detection of material in weapons-useable quantities.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
NASA NTRS2026

Recommended Practices in Laser-Induced Fluorescence (LIF) Diagnostics for Electric Propulsion

Laser-induced fluorescence (LIF) spectroscopy uses Doppler-shifted laser photons to excite a bound electron transition in an atom or ion, with subsequent fluorescence emission detected in order to measure the local velocity distribution function (VDF) and/or particle density. Due to its non-invasive nature, high spatial resolution, and acceptable difficulty of implementation, LIF has become a favored diagnostic for electric propulsion (EP) plasmas, particularly in the study of Hall thrusters. This paper presents recommended best practices for LIF measurements in electric thrusters, drawn from over three decades of implementation heritage in the EP community. Focusing on both single-photon LIF (typically used to measure VDFs) and two-photon LIF (TALIF, typically used to determine densities), the paper covers selection of atomic transitions to target, experimental setups, and interpretation of data. A number of special topics and advanced applications are discussed, including uncertainty analysis, techniques for high-speed measurements, and applications to a variety of propellants.

plasma plume↗
DOE OSTI2024

A Comprehensive Experimental Study on Microstructure‐Graded Graphite Anodes for Enhancing Fast‐Charging Capability of Lithium‐Ion Batteries

Lithium‐ion batteries with high gravimetric capacity density and improved cycle life performance under fast‐charging conditions are crucial for widespread electric vehicle (EV) adoption. This study investigates how designing graphite anode microstructure, specifically porosity, and particle‐size gradients, improves lithium‐ion (Li + ) transport during fast‐charging conditions. Three‐layered graphite anodes with varying porosity (24%, 36%, 46%) and particle size gradients (3, 5, 10 μm) were compared to a conventional single‐layered electrode in half‐cell configurations. At room temperature and high discharge rate (2C), both gradient structures showed significantly enhanced capacity retention (80% and 67% vs. 50%) compared to the conventional electrode, highlighting the effectiveness of microstructure engineering for fast charging. The study also investigated the temperature's impact on cycle life. After 200 cycles at 2°C and 45°C, all gradient structures demonstrated superior capacity retention (≈80%) compared to the conventional electrode (35%), suggesting the gradients mitigate degradation rate at high temperatures. Electrochemical impedance spectroscopy confirmed superior Li+ diffusion and lower resistivity in gradient electrodes. Simulations explored the influence of gradient profiles on reaction kinetics across the electrode thickness. Overall, this research demonstrates that the fast‐charging capability of graphite electrodes can be greatly enhanced by engineering the electrode microstructure, thereby making EV technology more accessible and appealing.

Ahmadi, Soma↗
DOE OSTI2023

Make Selenium Reactive Again: Activating Elemental Selenium for Synthesis of Metal Selenides Ranging from Nanocrystals to Large Single Crystals

The inertness of elemental selenium is a significant obstacle in the synthesis of selenium-containing materials at low reaction temperatures. Over the years, several recipes have been developed to overcome this hurdle; however, most of the methods are associated with the use of highly toxic, expensive, and environmentally harmful reagents. As such, there is an increasing demand for the design of cheap, stable, and nontoxic reactive selenium precursors usable in the low-temperature synthesis of transition metal selenides with vast applications in nanotechnology, thermoelectrics, and superconductors. Herein, a novel synthetic route has been developed for activating elemental selenium by using a solvothermal approach. By comprehensive 77 Se NMR, Raman, and infrared spectroscopies and gas chromatography–mass spectrometry, we show that the activated Se solution contained HSe – , [Se–Se] 2– , and Se 2– ions, as well as dialkyl selenide (R 2 Se) and dialkyl diselenide (R–Se–Se–R) species in dynamic equilibrium. This also corresponded to the first observation of naked Se 2 2– in solution. The versatility of the developed Se precursor was demonstrated by the successful synthesis of (i) the polycrystalline room-temperature modification of the β-Ag 2 Se thermoelectric material; (ii) large single crystals of superconducting β-FeSe; (iii) CdSe nanocrystals with different particle sizes (3–10 nm); (iv) nanosheets of PtSe 2 ; and (v) mono- and dibenzyl selenides and diselenides at room temperature. In conclusion, The simplicity and diversity of the developed Se activation method holds promise for applied and fundamental research.

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

Time–connectivity superposition and the gel/glass duality of weak colloidal gels

Colloidal gels result from the aggregation of Brownian particles suspended in a solvent. Gelation is induced by attractive interactions between individual particles that drive the formation of clusters, which in turn aggregate to form a space-spanning structure. We study this process in aluminosilicate colloidal gels through time-resolved structural and mechanical spectroscopy. Using the time–connectivity superposition principle a series of rapidly acquired linear viscoelastic spectra, measured throughout the gelation process by applying an exponential chirp protocol, are rescaled onto a universal master curve that spans over eight orders of magnitude in reduced frequency. This analysis reveals that the underlying relaxation time spectrum of the colloidal gel is symmetric in time with power-law tails characterized by a single exponent that is set at the gel point. The microstructural mechanical network has a dual character; at short length scales and fast times it appears glassy, whereas at longer times and larger scales it is gel-like. These results can be captured by a simple three-parameter constitutive model and demonstrate that the microstructure of a mature colloidal gel bears the residual skeleton of the original sample-spanning network that is created at the gel point. Our conclusions are confirmed by applying the same technique to another well-known colloidal gel system composed of attractive silica nanoparticles. The results illustrate the power of the time–connectivity superposition principle for this class of soft glassy materials and provide a compact description for the dichotomous viscoelastic nature of weak colloidal gels.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Deriving the Infrared Complex Refractive Indices of Organic Powders for Optical Modeling: Comparison of Methods

Identification of solids via infrared reflection spectroscopy requires a spectral library of all solids likely to be encountered. A confounding factor in populating such a spectral library is that the reflectance spectra of solids vary with their form, including particle size, film thickness, and substrate. To reduce the efforts of experimentally constructing such a library, an alternate strategy is to use the wavelength-dependent optical constants, n and k, of a solid to calculate a series of reflectance spectra corresponding to each scenario or morphology. Because most n/k measurements are best performed on mm-sized crystals, however, the challenge of determining the optical constants increases when a solid is only readily available as a powder, as is often the case. Some organic solids, such as caffeine, are both unavailable in large crystals and difficult to press into pellets. In this study, the infrared optical constants, or complex refractive indices, of caffeine were determined using three different methods: single-angle reflectance, infrared spectroscopic ellipsometry, and quantitative absorbance measurements of KBr pellets. The n and k values derived through each method were used to model the hyperspectral imaging reflectance spectrum of a caffeine film on a steel planchet. Over 1,110 – 870 cm-1, the single-angle reflectance-derived n and k had the best correlation with the experimental spectrum. These results suggest different organic solids may require different methods to determine the most accurate infrared complex refractive indices for synthetic spectral libraries.

FTIR, hyperspectral imaging, infrared, infrared (I↗