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DOE OSTI2025

Results of an interlaboratory study on the working curve in vat photopolymerization II: Towards a standardized method

The working curve measurement in photopolymer additive manufacturing is a ubiquitous measure of the cure depth of a printing resin as a function of radiant exposure of light. The fit parameters from this measurement (the depth of light penetration D p and the critical exposure E c ) are used to evaluate and report a resin’s printability, optimize processing parameters, and inform print and resin quality control. Despite its widespread use, the working curve lacks a standard measurement method. Here, following up on our paper “Results of an Interlaboratory Study on the Working Curve in Vat Photopolymerization” from last year, an interlaboratory study on the working curve was performed using calibrated, reproducible, bandpass filtered light sources. With these light sources, the variability between labs in measured working curves was dramatically reduced from the initial interlaboratory study. Aggregate data from this experiment produced reliable D p and E c measurements at 385 nm of 39.2 ± 3.7 µm and 12.3 ± 3.0 mJ cm −2 , respectively. At 405 nm the values of D p and E c are 69.3 ± 3.8 µm and 17.9 ± 2.3 mJ cm −2 , respectively. The results are agnostic to the thickness measurement tool utilized by participants, ensuring broad applicability across laboratories. We also tested the generalizability of the proposed method of using a filtered light source by filtering a commercial 405 nm light source and obtaining a working curve in agreement with the aggregate data from the interlaboratory study. This interlaboratory study provides a basis for a documentary standard for the working curve, so that the entire photopolymer additive manufacturing industry can share reproducible and interoperable working curve data.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Influence of fluorescent dopants on the vat photopolymerization of acrylate-based plastic scintillators for application in neutron/gamma pulse shape discrimination

Plastic scintillators, a class of solid-state materials used for radiation detection, were additively manufactured with vat photopolymerization. The photopolymer resins consisted of a primary dopant and a secondary dopant dissolved in a bisphenol A ethoxylate diacrylate-based matrix. The absorptive dopants significantly influence important print parameters, for example, secondary dopants decrease the light penetration depth by a factor > 12×. The primary dopant 2,5-diphenyloxazole had minimal impact on the printing process even when loaded at 25 % by mass of the resin. Working curve measurements, which relate energy dose to cure depth, were performed as a function of feature size to further assess the influence of dopants. Photopatterns smaller than 150 µm width had apparent increases in critical energy dose compared to larger photopatterns, while all resins maintained printed features in line gratings with 50 µm of separation. Printed scintillator monoliths were compared to scintillators cast by traditional molding, demonstrating that the layer-by-layer printing process does not decrease scintillation response. In conclusion, a maximum light output of 31 % of a benchmark plastic scintillator (EJ-200) and successful pulse shape discrimination were achieved with 20 % by mass 2,5-diphenyloxazole as the primary dopant and 0.1 % by mass 9,9-dimethyl-2,7-distyrylfluorene as the secondary dopant in printed scintillator samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1985

Sulfur transformations at the hydrogen sulfide/oxygen interface in stratified waters and in cyanobacterial mats

Stratified water bodies allow the development of several microbial plates along the water column. The microbial plates develop in relation to nutrient availability, light penetration, and the distribution of oxygen and sulfide. Sulfide is initially produced in the sediment by sulfate-reducing bacteria. It diffuses along the water column creating a zone of hydrogen sulfide/oxygen interface. In the chemocline of Solar Lake oxygen and sulfide coexist in a 0 to 10 cm layer that moves up and down during a diurnal cycle. The microbial plate at the chemocline is exposed to oxygen and hydrogen sulfide, alternating on a diurnal basis. The cyanobacteria occupying the interface switch from anoxygenic photosynthesis in the morning to oxygenic photosynthesis during the rest of the day which results in a temporal build up of elemental sulfur during the day and disappears at night due to both oxidation to thiosulfate and sulfate by thiobacilli, and reduction to hydrogen sulfide by Desulfuromonas sp. and anaerobically respiring cyanobacteria. Sulfate reduction was enhanced in the light at the surface of the cyanobacterial mats. Microsulfate reduction measurements showed enhanced activity of sulfate reduction even under high oxygen concentrations of 300 to 800 micrometer. Apparent aerobic SO sub 4 reduction activity is explained by the co-occurrence of H sub 2. The physiology of this apparent sulfate reduction activity is studied.

Cohen, Y.↗

NASA NTRS1993

Stable isotopic biogeochemistry of carbon and nitrogen in a perennially ice-covered Antarctic lake

Lake Hoare (77 degrees 38' S, 162 degrees 53' E) is an amictic, oligotrophic, 34-m-deep, closed-basin lake in Taylor Valley, Antarctica. Its perennial ice cover minimizes wind-generated currents and reduces light penetration, as well as restricts sediment deposition into the lake and the exchange of atmospheric gases between the water column and the atmosphere. The biological community of Lake Hoare consists solely of microorganisms -- both planktonic populations and benthic microbial mats. Lake Hoare is one of several perennially ice-covered lakes in the McMurdo Dry Valleys that represent the end-member conditions of cold desert and saline lakes. The dry valley lakes provide a unique opportunity to examine lacustrine processes that operate at all latitudes, but under an extreme set of environmental conditions. The dry valley lakes may also offer a valuable record of catchment and global changes in the past and present. Furthermore, these lakes are modern-day equivalents of periglacial lakes that are likely to have been common during periods of glacial maxima at temperate latitudes. We have analyzed the dissolved inorganic carbon (DIC) of Lake Hoare for delta 13C and the organic matter of the sediments and sediment-trap material for delta 13C and delta 15N. The delta 13C of the DIC indicates that 12C is differentially removed in the shallow, oxic portions of the lake via photosynthesis. In the anoxic portions of the lake (27-34 m) a net addition of 12C to the DIC pool occurs via organic matter decomposition. The dissolution of CaCO3 at depth also contributes to the DIC pool. Except near the Canada Glacier where a substantial amount of allochthonous organic matter enters the lake, the organic carbon being deposited on the lake bottom at different sites is isotopically similar, suggesting an autochthonous source for the organic carbon. Preliminary inorganic carbon flux calculations suggest that a high percentage of the organic carbon fixed in the water column is remineralized as it falls through the water column. At nearby Lake Fryxell, the substantial (relative to Lake Hoare) glacial meltstream input overprints Fryxell's shallow-water biological delta 13C signal with delta 13C-depleted DIC. In contrast, Lake Hoare is not significantly affected by surface-water input and mixing, and therefore the delta 13C patterns observed arise primarily from biological dynamics within the lake. Organic matter in Lake Hoare is depleted in 15N, which we suggest is partially the result of the addition of relatively light inorganic nitrogen into the lake system from terrestrial sources.

NASA Program Exobiology↗

DOE OSTI2025

Characterization of PuO 2 With Visible and UV Raman Spectroscopy: Discrimination Between the Bulk, Surface, and an Intermediate Disordered Layer

Raman spectroscopy is an ideal tool in the characterization of materials including PuO 2 . The wavelength-dependent absorptivity of the material defines the light penetration depth and the relative Raman scattering contribution from the bulk and the surface. Here, the surface contribution to the total Raman scattering was investigated for PuO 2 calcined at various temperatures and recorded with laser wavelengths of 355, 325, and 244 nm. These experiments provided the first glimpse of the wavelength-dependent disappearance and emergence of new phonons and electronic bands from the PuO 2 surface layers. The first indication of the wavelength transition in the Raman spectra was the loss of the 2LO2 (overtone, ~1155 cm -1 ) band and the weakening intensity of the Г 1 → Γ 5 electronic band (~2135 cm -1 ) with the 355-nm excitation laser. The Γ 5 electronic band was barely visible with the 244-nm excitation. The electronic band located at ~1050 cm -1 , corresponding to the Г 1 → Γ 4 electronic transition was observed to dramatically increase in intensity while the Г 1 → Γ 3 electronic band (2640 cm -1 ) sharpened as the UV wavelength was increased in energy from the near- to deep-UV (355–325–244 nm). The FWHM of the T 2g band was found to vary with calcination temperature (450°C and 900°C) with the 325-nm laser and the 244-nm laser. The T 2g band attributes, the strong emergence of the Г 1 → Γ 4 electronic band, and the disappearance of the 2LO2 overtone acquired with the 244-nm excitation for the different calcination temperatures suggest a shallow penetration depth.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2026

Monitoring the Stability of Porous Coordination Cages during the Photoreduction of Porous Salt Thin Films

This study investigates the photochemical properties and stability of zirconium-based porous salts composed of coordination cages and redox-active polyoxometalates (POMs). While bulk porous salts demonstrated photoreduction confined to surface regions due to lim-ited light penetration and scattering effects, thin films of cage-POM assemblies were fabricated to address these challenges. These optically transparent films allowed access to the catalyst core, enabling enhanced photochemical characterization. Comparative studies revealed that the thin films exhibited superior photochemical activity and maintained porosity under optimized conditions, whereas bulk powders suffered from surface-limited photoreduction and cage decomposition. Furthermore, this work highlights the utility of thin films as a platform for studying and advancing the photochemical applications of porous salts.

Hoq, Jahidul [Indiana University, Bloomington, IN ↗

DOE OSTI2021

Assessing Forest Level Response to the Death of a Dominant Tree within a Premontane Tropical Rainforest

Small-scale treefall gaps are among the most important forms of forest disturbance in tropical forests. These gaps expose surrounding trees to more light, promoting rapid growth of understory plants. However, the effects of such small-scale disturbances on the distribution of plant water use across tree canopy levels are less known. To address this, we explored plant transpiration response to the death of a large emergent tree, Mortoniodendron anisophyllum Standl. & Steyerm (DBH > 220 cm; height ~40 m). Three suppressed, four mid-story, and two subdominant trees were selected within a 50 × 44 m premontane tropical forest plot at the Texas A&M Soltis Center for Research and Education located in Costa Rica. We compared water use rates of the selected trees before (2015) and after (2019) the tree gap using thermal dissipation sap flow sensors. Hemispherical photography indicated a 40% increase in gap fraction as a result of changes in canopy structure after the treefall gap. Micrometeorological differences (e.g., air temperature, relative humidity, and vapor pressure deficit (VPD)) could not explain the observed trends. Rather, light penetration, as measured by sensors within the canopy, increased significantly in 2019. One year after the tree fell, the water usage of trees across all canopy levels increased modestly (15%). Moreover, average water usage by understory trees increased by 36%, possibly as a result of the treefall gap, exceeding even that of overstory trees. These observations suggest the possible reallocation of water use between overstory and understory trees in response to the emergent tree death. With increasing global temperatures and shifting rainfall patterns increasing the likelihood of tree mortality in tropical forests, there is a greater need to enhance our understanding of treefall disturbances that have the potential to redistribute resources within forests.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1969

Fraunhofer line-dept sensing applied to water

An experimental Fraunhofer line discriminator is basically an airborne fluorometer, capable of quantitatively measuring the concentration of fluorescent substances dissolved in water. It must be calibrated against standards and supplemented by ground-truth data on turbidity and on approximate vertical distribution of the fluorescent substance. Quantitative use requires that it be known in advance what substance is the source of the luminescence emission; qualitative sensing, or detection of luminescence is also possible. The two approaches are fundamentally different, having different purposes, different applications, and different instruments. When used for sensing of Rhodamine WT dye in coastal waters and estuaries, the FLD is sensing in the spectral region permitting nearly maximum depth of light penetration.

Stoertz, G. E.↗

NASA NTRS1972

Application of selected methods of remote sensing for detecting carbonaceous water pollution

The use of aerial photography to determine the nature and extent of water pollution from carbonaceous materials is discussed. Flights were conducted over the Galveston Bay estuarine complex. Ground truth data were developed from field sampling of the waters in a region near the Houston Ship Channel. Tests conducted in the field were those for the following physical and chemical factors: (1) ph, (2) dissolved oxygen, (3) temperature, and (4) light penetration. Laboratory analyses to determine various properties of the water are described and the types of instruments used are identified. Results of the analyses are presented as charts and graphs.

Davis, E. M.↗

NASA NTRS1973

Application of selected methods of remote sensing for detecting carbonaceous water pollution

A reach of the Houston Ship Channel was investigated during three separate overflights correlated with ground truth sampling on the Channel. Samples were analyzed for such conventional parameters as biochemical oxygen demand, chemical oxygen demand, total organic carbon, total inorganic carbon, turbidity, chlorophyll, pH, temperature, dissolved oxygen, and light penetration. Infrared analyses conducted on each sample included reflectance ATR analysis, carbon tetrachloride extraction of organics and subsequent scanning, and KBr evaporate analysis of CCl4 extract concentrate. Imagery which was correlated with field and laboratory data developed from ground truth sampling included that obtained from aerial KA62 hardware, RC-8 metric camera systems, and the RS-14 infrared scanner. The images were subjected to analysis by three film density gradient interpretation units. Data were then analyzed for correlations between imagery interpretation as derived from the three instruments and laboratory infrared signatures and other pertinent field and laboratory analyses.

Davis, E. M.↗

NASA NTRS1976

Soil, water, and vegetation conditions in South Texas

The author has identified the following significant results. Reflectance measurements with a field spectroradiometer on nine dates (between December 9 and April 8) during the growing season of two wheat varieties, Milam and Penjamo, showed that the reflectance curves had the characteristic shape of vegetated surfaces by 4 weeks after the emergence. Green light (0.55 micron) reflectance was maximal and between water absorption bands (1.65 and 2.2 microns) reflectance was minimal when green vegetation development was greatest. Computer classification was accomplished for 81,000 hectare coastal rangeland area for October 13 and December 10, 1975, overpass dates. A hard freeze occurred between these two dates and many of the deciduous woody species defoliated so that more light penetrated to the herbaceous understory in December than in October.

Wiegand, C. L.↗

NASA NTRS1978

Characterization of nonideal silicon in terms of lifetime and diffusion length

Experimental methods have been evaluated for the determination of lifetime and diffusion length in silicon intentionally doped with potentially lifetime-degrading impurities which may be present in low-cost silicon intended for use in terrestrial flat-plate arrays. Results obtained with these methods have been compared for mutual consistency. The effects of a number of impurities on bulk lifetime were determined from steady-state photoconductivity, and solar cells fabricated from this material were characterized in terms of diffusion length using a penetrating light technique. Comparison was made with results obtained by others using photoconductivity decay. General agreement was found in terms of the hierachy of impurities to which the lifetime is sensitive. The utility of the steady-state photoconductivity method is established even in the presence of considerable trapping.

Othmer, S.↗

NASA NTRS1991

The hemispherical asymmetry of the residual polar caps on Mars

A model of the polar caps of Mars was created which allows: (1) for light penetration into the cap; (2) ice albedo to vary with age, latitude, hemisphere, dust content, and solar zenith angle; and (3) for diurnal variability. The model includes the radiative effects of clouds and dust, and heat transport as represented by a thermal wind. The model reproduces polar cap regression data very well, including the survival of CO2 frost at the south pole and reproduces the general trend in the Viking Lander pressure data.

Lindner, Bernhard Lee↗

NASA NTRS1991

The effects of lunar dust accumulation on the performance of photovoltaic arrays

Lunar base activity, particularly rocket launch and landing, will suspend and transport lunar dust. From preliminary models, the resulting dust accumulation can be significant, even as far as 2 km from the source. For example, at 2 km approximately 0.28 mg/sq cm of dust is anticipated to accumulate after only 10 surface missions with a 26,800 N excursion vehicle. The possible associated penalties in photovoltaic array performance were therefore the subject of experimental as well as theoretical investigation. To evaluate effects of dust accumulation on relative power output, current-voltage characteristics of dust-covered silicon cells were determined under the illumination of a Spectrolab X-25L solar simulator. The dust material used in these experiments was a terrestrial basalt which approximated lunar soil in particle size and composition. Cell short circuit current, an indicator of the penetrating light intensity, was found to decrease exponentially with dust accumulation. This was predicted independently by modeling the light occlusion caused by a growing layer of dust particles. Moreover, the maximum power output of dust-covered cells, derived from the I-V curves, was also found to degrade exponentially. Experimental results are presented and potential implications discussed.

Katzan, Cynthia M.↗

NASA NTRS1992

Simulations of the seasonal polar caps on Mars

One of the most puzzling mysteries about the planet Mars is the hemispherical asymmetry in the polar caps. Every spring the seasonal polar cap of CO2 recedes until the end of the summer, when only a small part, the residual polar cap, remains. Scientists have sought to explain this asymmetry by modeling observations of the latitudinal recession of the polar cap and seasonal variations in atmospheric pressure (since the seasonal polar caps are primarily frozen atmosphere, they are directly related to changes in atmospheric mass). These models reproduce most aspects of the observed annual variations in atmospheric pressure fairly accurately. Furthermore, the predicted latitudinal recession of the northern polar cap in the spring agrees well with observations, including the fact that the CO2 ice is predicted to completely sublime away during the summer in the Southern Hemisphere, unlike what is observed. This power will show how the radiative effects of ozone, clouds, and airborne dust, light penetration into and through the polar caps, and the dependence of albedo on solar zenith angle affect CO2 ice formation and sublimation, and how they help explain the hemispherical asymmetry in the residual polar caps. These effects have not been studied with prior polar cap models.

Lindner, Bernhard Lee↗

NASA NTRS1992

Why is the north polar cap on Mars different than the south polar cap?

One of the most puzzling mysteries about the planet Mars is the hemispherical asymmetry in the polar caps. Every spring, the seasonal polar cap of CO2 recedes until the end of summer, when only a small part, the residual polar cap, remains. During the year that Viking observed Mars, the residual polar cap was composed of water ice in the Northern Hemisphere (Kieffer et al., Science, 194, 1341, 1976) but was primarily carbon dioxide ice in the Southern Hemisphere (Kieffer, J. Geophys. Res., 84, 8263, 1979). Scientists have sought to explain this asymmetry by modeling observations of the latitudinal recession of the polar cap and seasonal variations in atmospheric pressure (since the seasonal polar caps are primarily frozen atmosphere, they are directly related to changes in atmospheric mass). These models reproduce most aspects of the observed annual variation in atmospheric pressure fairly accurately. Furthermore, the predicted latitudinal recession of the northern polar cap in the spring agrees well with observations, including the fact that the CO2 ice is predicted to completely sublime away. However, these models all predict that the carbon dioxide ice will also sublime away during the summer in the Southern Hemisphere, unlike what is observed. This paper will show how the radiative effects of ozone, clouds, and airborne dust, light penetration into and through the polar cap, and the dependence of albedo on solar zenith angle affect CO2 ice formation and sublimation, and how they help explain the hemispherical asymmetry in the residual polar caps. These effects have not been studied with prior polar cap models.

Lindner, Bernhard Lee↗

NASA NTRS1992

Simulations of the seasonal polar caps on Mars

One of the most puzzling mysteries about the planet Mars is the hemispherical asymmetry in the polar caps. Every spring the seasonal polar cap of CO2 recedes until the end of summer, when only a small part, the residual polar cap, remains. During the year that Viking observed Mars, the residual polar cap was composed of water ice in the Northern Hemisphere (Kieffer et al., Science, 194, 1341, 1976), but was primarily carbon dioxide ice in the Southern Hemisphere (Kieffer, J. Geophys. Res., 84, 8263, 1979). Scientists have sought to explain this asymmetry by modeling observations of the latitudinal recession of the polar cap and seasonal variations in atmospheric pressure (since the seasonal polar caps are primarily frozen atmosphere, they are directly related to changes in atmospheric mass). These models reproduce most aspects of the observed annual variation in atmospheric pressure fairly accurately. Furthermore, the predicted latitudinal recession of the northern polar cap in the spring agrees well with observations, including the fact that CO2 ice is predicted to completely sublime away. However, these models all predict that the carbon dioxide ice will also sublime away during the summer in the Southern Hemisphere, unlike what is observed. It is shown here how the radiative effects of ozone, clouds, and airborne dust, light penetration into and through the polar cap, and the dependence of albedo on solar zenith angle affect CO2 ice formation and sublimation, and how they help explain the hemispherical asymmetry in the residual polar caps. These effects have not been studied with prior polar cap models. The combination of the effects of solar zenith angle on albedo and the radiative effects of clouds and dust act to extend the lifetime of CO2 ice on the south pole relatively more than on the north pole, possibly explaining the hemispherical asymmetry in the residual polar caps without the need of a hemispherical asymmetry in polar cap albedo. This does not imply that a hemispherical asymmetry in polar cap albedo does not exist, but that one is not necessary. Observations of the regression of the polar caps and the annual cycle in atmospheric pressure are reproduced fairly well by the model, as shown in the figures, although further improvement is needed. When CO2 ice is retained at the south pole, the model predictions of the annual cycle in atmospheric pressure have a phase shift relative to the data, no matter what model input parameters are used. We are investigating other processes not included in prior polar cap models.

Lindner, Bernhard Lee↗

NASA NTRS1994

Why is the north polar cap on Mars different than the south polar cap?

Lindner, Bernhard Lee↗