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NASA NTRS1993

A method of making a single layer multi-color luminescent display

The invention is a method of forming a multi-color luminescent display including the steps of depositing on an insulator substrate a smooth single layer of host material which itself may be a phosphor with the properties to host varying quantities of different impurities and introducing one or more of said different impurities into selected areas of the single layer of host material via an appropriately positioned mask as by thermal diffusion or ion-implantation to form a pattern of phosphors of different colors in the single layer of host material such that the top surface of the host layer remains smooth. Red phosphors are formed by adding impurities selected from the group consisting of Sm, SmF3, Eu, EuF3, and ZnS:MnTbF3 to a ZnS host; green phosphors by adding impurities selected from the group consisting of Tb and TbF3 to a ZnS host; and blue phosphors by adding impurities selected from the group consisting of Tm, Al, Ag, and Mg to a ZnS host.

Robertson, James B.↗

NASA NTRS1994

Method development for compensating temperature effects in pressure sensitive paint measurements

Pressure sensitive luminescent paints (PSP) have recently emerged as a viable technique for aerodynamic pressure measurements. The technique uses a surface coating which contains probe molecules that luminesce when excited by light of an appropriate wavelength. The photoluminescence of these materials is known to be quenched by the presence of molecular oxygen. Since oxygen is a fixed mole fraction of the air, the coating's luminescence intensity varies inversely with air pressure. Digital imaging of the luminescence varying across a coated surface produces a pressure distribution map over that surface. One difficulty encountered with this technique is the temperature effect on the luminescence intensity. Present PSP formulations have significant sensitivity to temperature. At the moment, the most practical way of correcting for temperature effects is to calibrate the paint in place at the operating temperatures by using a few well-placed pressure taps. This study is looking at development of temperature indicating coatings that can be applied and measured concurrently with PSP, and use the temperature measurement to compute the correct pressure. Two methods for this dual paint formulation are proposed. One method will use a coating that consists of temperature sensitive phosphors in a polymer matrix. This is similar in construction to PSP, except that the probe molecules used are selected primarily for their temperature sensitivity. Both organic phosphors (e.g., europium thenoyltrifluoroacetonate, bioprobes) and inorganic phosphors (e.g., Mg4(F)GeO6:Mn, La2O2S:Eu, Radelin Type phosphors, Sylvania Type phosphors) will be evaluated for their temperature sensing potential. The next method will involve a novel coating composing of five membered heterocyclic conducting polymers which are known to show temperature dependent luminescence (e.g., poly(3-alkylthiopene), poly(3-alkylselenophene), poly(3-alkylfuran)). Both methods will involve applying a bottom layer of temperature sensitive coating followed by a top coating of PSP. An oxygen-impermeable polymer can be used as the temperature sensitive coating matrix, or it can be layered in between the coatings to prevent oxygen quenching of the bottom coating's luminescence. The probe molecules of the coatings will be excited by a broad band of light, with the different emissions detected and measured at their distinct wavelengths. Developmental research of these coatings is still in progress; however, preliminary results look very promising.

Demandante, Carlo Greg N.↗

NASA NTRS2012

Temperature Sensing Above 1000 C Using Cr-Doped GdAlO3 Spin-Allowed Broadband Luminescence

Cr-doped GdAlO3 (Cr:GdAlO3) is shown to produce remarkably high-intensity spin-allowed broadband luminescence with sufficiently long decay times to make effective luminescence-decay-time based temperature measurements above 1000 C. This phosphor is therefore an attractive alternative to the much lower luminescence intensity rare-earth-doped thermographic phosphors that are typically utilized at these elevated temperatures. In particular, Cr:GdAlO3 will be preferred over rare-earth-doped phosphors, such as Dy:YAG, at temperatures up to 1200 C for intensity-starved situations when the much lower emission intensity from rare-earth-doped phosphors is insufficient for accurate temperature measurements in the presence of significant radiation background. While transition-metal-doped phosphors such as Cr:Al2O3 (ruby) are known to exhibit high luminescence intensity at low dopant concentrations, quenching due to nonradiative decay pathways competing with the (sup 2)E to (sup 4)A(sub 2) radiative transition (R line) has typically restricted their use for temperature sensing to below 600 C. Thermal quenching of the broadband (sup 4)T(sub 2) to (sup 4)A(sub 2) radiative transition from Cr:GdAlO3, however, is delayed until much higher temperatures (above 1000 C). This spin-allowed broadband emission persists to high temperatures because the lower-lying (sup 2)E energy level acts as a reservoir to thermally populate the higher shorter-lived (sup 4)T(sub 2) energy level and because the activation energy for nonradiative crossover relaxation from the (sup 4)T(sub 2) level to the (sup 4)A(sub 2) ground state is high. The strong crystal field associated with the tight bonding of the AlO6 octahedra in the GdAlO3 perovskite structure is responsible for this behavior.

Eldridge, Jeffrey I.↗

DOE OSTI2020

Light source and method for making a light source

A light source fabrication process to fabricate a customized light source includes attaching a plurality of light emitting diodes to a circuit board, where each light emitting diode is configured to emit light within a same wavelength range. Further, the light source fabrication process includes applying a first phosphor layer to a first set of light emitting diodes of the plurality of light emitting diodes and applying a second phosphor layer to a second set of light emitting diodes of the plurality of light emitting diodes. The phosphor layers are applied to the light emitting diodes using one of a screen printing process and an inkjet printing process. The first phosphor layer is different from and has different optical properties from the second phosphor layer.

42 ENGINEERING↗

DOE OSTI2023

Intercalation And High-Pressure Effects On Structural Phase Transitions In Layered As x P 1-x Alloys

This project was aimed at understanding the role of composition, intercalation, and high pressure on the structural evolution of black phosphorous (BP) and layered arsenic phosphorous alloys, As y P 1-y . Under normal conditions, BP is the most stable phase of phosphorous, known as the α-phase, characterized by an orthorhombic honeycomb puckered crystal structure with the Cmca space group. On the other hand, the most stable phase of arsenic is its β-phase, known as gray arsenic (g-As), which has a rhombohedral buckled layered crystal structure with the R3m space group. In a wide range of compositions (y < 0.83), the arsenic phosphorous alloys form the α-phase, known as black arsenic phosphorous (b-As y P 1-y ) with a similar structure to BP. The project was aimed at the synthesis of BP and b-As y P 1-y with different compositions and at studying the structural evolution of these materials during intercalation with alkali metal (especially Li), and under high-pressure conditions. The main goals were to gain a better understanding of these processes and structural changes taking place under these conditions. In particular, the project was aimed at addressing whether such conditions could induce a structural transition between the α- and β-phases. For this, a series of systematic in-situ studies were conducted, including electrochemical lithium intercalation in an in-situ electrochemical cell, and high-pressure experiments in a diamond anvil cell (DAC). Overall, both types of experiments have shown that above a certain composition-dependent threshold level of intercalation or high pressure, the system undergoes phase segregation rather than phase transition. Specifically, the segregation of the excess arsenic was observed, and a single-phase system of b-As y P 1-y transformed into a two-phase system consisting of b-As y P 1-y and g-As, through the following process: 1∗(b-As y P 1-y ) → 1∗(b As y-δ P 1-y ) + δ∗(g-As). Also, the study showed that intercalation and high-pressure are two competing rather than synergistic processes causing at least a partial cancelation of these two factors

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microbial interactions with phosphorus containing glasses representative of vitrified radioactive waste

The presence of phosphorous in borosilicate glass (at 0.1 – 1.3 mol % P 2 O 5 ) and in iron-phosphate glass (at 53 mol % P 2 O 5 ) stimulated the growth and metabolic activity of anaerobic bacteria in model systems. Dissolution of these phosphorous containing glasses was either inhibited or accelerated by microbial metabolic activity, depending on the solution chemistry and the glass composition. The breakdown of organic carbon to volatile fatty acids increased glass dissolution. The interaction of microbially reduced Fe(II) with phosphorus-containing glass under anoxic conditions decreased dissolution rates, whereas the interaction of Fe(III) with phosphorous-containing glass under oxic conditions increased glass dissolution. Phosphorous addition to borosilicate glasses did not significantly affect the microbial species present, however, the diversity of the microbial community was enhanced on the surface of the iron phosphate glass. Results demonstrate the potential for microbes to influence the geochemistry of radioactive waste disposal environments with implication for wasteform durability.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Fluorescence-Based Aqueous Phosphate Sensing Using Eu(cpboda)(DMF) 2

Fluorescence-based phosphate sensing using phosphate-sensitive phosphors is a promising approach for in situ monitoring of phosphate pollution in waterways and reservoirs. To date, the most sensitive phosphor developed for this purpose is Tb(cpboda)(DMF) 2 , where cpboda = (3,3'-((5-Carboxy-1,3-phenylene)bis(oxy))dibenzoic acid). In this study, we further improve this sensitivity by replacing the Tb 3+ ions with Eu 3+ ions to make Eu(cpboda)(DMF) 2 and find concentration-independent phosphate-sensitivity of 1570 ± 120, which is ≈8× more sensitive than the Tb-version. This improvement is attributed to Eu 3+ having a hypersensitive transition, while Tb 3+ does not. Additionally, we characterize the phosphor’s optical properties, photodegradation, and water solubility. We find that the phosphor presents challenges with regards to both photodegradation and solubility, as it is found to be poorly soluble in water and is quickly photodegraded under UV radiation <360 nm. However, these obstacles can, in theory, be overcome with the use of direct excitation of the Eu 3+ ions at 394 nm and careful design of an analysis instrument to reduce concentration variations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Biobased Flame Retardants Towards Sustainable Building Materials with Low Embodied Carbon

Incorporation of fire retardants in different types of products is one of the essential steps in the material production process to minimize fire risk and meet fire safety requirements. A variety of commonly used flame retardants based on halogen, mineral, and other compounds has gained popularity due to their efficient flame-retardant behaviors. However, especially in the case of halides, there are numerous toxicity related issues and environmental pollution effects that have urged the building sector to deviate from their use and focus on the development of non-toxic alternatives. Therefore, to enhance the safety of flame retardants, the synthesis of flame retardants from waste feedstocks using phosphorous chemistry with a dual flame-retardant mechanism has been established. A range of waste feedstocks that include cardanol, vanillin, and gallic acids has been converted into a series of flame retardants using a one-step approach by incorporating phosphorous moieties into their structures. The established pathways allow to develop a range of flame-retardant materials by converting waste feedstocks into phosphorous-based materials with inherent flame retardancy. The introduction of abundant aromatic structures from biobased feedstocks enables high charring capabilities in materials in which these biobased flame retardants have been incorporated, increasing their char yields which significantly enhances the flame suppressing properties of the designed materials. Studies show that inclusion of phosphoric moieties into structures allows the displacement of flame enhancing radicals, by releasing non-flammable and non-toxic gases, therefore inhibiting the spread of fire in the gas phase. The resulting biobased flame retardants have been incorporated in wood substrates, foam insulation, and hemp fibers where the results show that only 1-5% of loading of biobased flame retardant suppressed the flame completely. This study represents a novel approach for the development of flame retardants with high performance while utilizing waste feedstocks as a source for their design.

Demchuk, Zoriana [ORNL] (ORCID:0000000326292235)↗

NASA NTRS1986

The chemical control of soluble phosphorus in the Amazon estuary

The role of sediments in controlling concentrations of soluble phosphorous in the Amazon estuary is examined. The efflux of phosphorous through the estuary is calculated using data collected on field excursions in December 1982 and May 1983, and laboratory mixing experiments. It is observed that soluble phosphorus was released from bottom sediments at a rate of 0.2 micro-M/day, when in seawater and deionizd water mixtures. The relation between release rates and salinity and sediment concentrations is studied. A one-dimensional dispersion model was developed to estimate phosphate inputs to the estuary. The model predicted total fluxes of soluble inorganic phosphorous of 15 x 10 to the 6th mole/day for December 1982 and 27 x 10 to the 6th mole/day for May 1983; the predictions correlate with field observations. It is noted that phosphorous removal is between 0 and 4 ppt at a rate of 0.044 + or - 0.01 micron-M/ppt per day and the annual mean input of phophorous from Amazon to outer-estuary is 23 x 10 to the 6th moles/day.

Fox, L. E.↗

NASA NTRS1991

Single layer multi-color luminescent display

The invention is a multi-color luminescent display comprising an insulator substrate and a single layer of host material which may be a phosphor deposited thereon that hosts one or more differential impurities, therein forming a pattern of selected and distinctly colored phosphors such as blue, green, and red phosphors in a single layer of host material. Transparent electrical conductor means may be provided for subjecting selected portions of the pattern of colored phosphors to an electric field thereby forming a multi-color, single layer electroluminescent display.

Robertson, James B.↗

NASA NTRS1990

Digital halftoning methods for selectively partitioning error into achromatic and chromatic channels

A method is described for reducing the visibility of artifacts arising in the display of quantized color images on CRT displays. The method is based on the differential spatial sensitivity of the human visual system to chromatic and achromatic modulations. Because the visual system has the highest spatial and temporal acuity for the luminance component of an image, a technique which will reduce luminance artifacts at the expense of introducing high-frequency chromatic errors is sought. A method based on controlling the correlations between the quantization errors in the individual phosphor images is explored. The luminance component is greatest when the phosphor errors are positively correlated, and is minimized when the phosphor errors are negatively correlated. The greatest effect of the correlation is obtained when the intensity quantization step sizes of the individual phosphors have equal luminances. For the ordered dither algorithm, a version of the method can be implemented by simply inverting the matrix of thresholds for one of the color components.

Mulligan, Jeffrey B.↗

NASA NTRS2004

Ionic Liquids and New Proton Exchange Membranes for Fuel Cells

There is currently a great surge of activity in fuel cell research as laboratories across the world seek to take advantage of the high energy capacity provided by &el cells relative to those of other portable electrochemical power systems. Much of this activity is aimed at high temperature fie1 cells, and a vital component of such &el cells must be the availability of a high temperature stable proton-permeable membrane. NASA Glenn Research Center is greatly involved in developing this technology. Other approaches to the high temperature fuel cell involve the use of single- component or almost-single-component electrolytes that provide a path for protons through the cell. A heavily researched case is the phosphoric acid fuel cell, in which the electrolyte is almost pure phosphoric acid and the cathode reaction produces water directly. The phosphoric acid fie1 cell delivers an open circuit voltage of 0.9 V falling to about 0.7 V under operating conditions at 170 C. The proton transport mechanism is mainly vehicular in character according to the viscosity/conductance relation. Here we describe some Proton Transfer Ionic Liquids (PTILs) with low vapor pressure and high temperature stability that have conductivities of unprecedented magnitude for non-aqueous systems. The first requirement of an ionic liquid is that, contrary to experience with most liquids consisting of ions, it must have a melting point that is not much above room temperature. The limit commonly suggested is 100 C. PTILs constitute an interesting class of non-corrosive proton-exchange electrolyte, which can serve well in high temperature (T = 100 - 250 C) fuel cell applications. We will present cell performance data showing that the open circuit voltage output, and the performance of a simple H2(g)Pt/PTIL/Pt/O2(g) fuel cell may be superior to those of the equivalent phosphoric acid electrolyte fuel cell both at ambient temperature and temperatures up to and above 200 C. My work at NASA Glenn Research Center during this summer is to develop and characterize proton exchange membranes doped with ionic liquids. The main techniques used to characterize these materials are: Impedance Spectroscopy, NMR, DSC, TGA, DMA, IR, and SEM ...

Belieres, Jean-Philippe↗

DOE OSTI2022

Ce:YAG/A12O3 composites for laser-excited solid-state white lighting

A method for fabricating a composite useful in a white light emitting device, includes mixing a phosphor and a filler to form a mixture; sintering the mixture (e.g., using spark plasma sintering) to form a composite; and annealing the composite to reduce oxygen vacancies and improve optical properties of the composite. Also disclosed is a white light emitting device including a laser diode or light emitting diode optically pumping the phosphor in the composite to produce white light. The composite fabricated using the method (and having. e.g., at most 50% phosphor by weight) can (1) reduce an operating temperature of the phosphor by 55 degrees, (2) increase an external quantum efficiency (e.g., by at least 15%) of the white light emitting device, and (3) result in color points and quality of the white light that is equal to or improved, as compared to without the filler.

Cozzan, Clayton J.↗

DOE OSTI2024

Mechanisms of proton transport in aqueous acid solutions

The fundamental understanding of proton transport, specifically the Grotthuss-like mechanism, is critical for many technological applications. The present study presents a comprehensive analysis of proton transport in aqueous solutions of sulfuric and phosphoric acids using quasielastic neutron and light scattering, broadband dielectric spectroscopy, rheology, pulsed-field gradient-NMR measurements, and ab initio molecular dynamic simulations. Results show that in all systems, proton transport occurs through short “jumps” of ~0.5 Å that are faster than structural relaxation. However, proton hopping appears to be coupled to structural relaxation in aqueous solutions of sulfuric acid, while these processes are decoupled in phosphoric acid. Neutron scattering indicates that all protons have the same fast mobility in phosphoric acid systems, while at least one proton per sulfuric molecule remains slower than other protons. Analysis reveals correlated proton jumps, but these correlations suppress conductivity, suggesting that expected Grotthuss-like enhancement of conductivity is unlikely in bulk liquids.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Sapphire advanced mitigation process: wet etch to expose sub-surface damage and increase laser damage resistance and mechanical strength

In this study, a novel, to the best of our knowledge, method of wet chemical etching of sapphire workpieces (such as optics, wafers, windows, and cones), called the sapphire advanced mitigation process (or sapphire AMP), has been developed that exposes sub-surface mechanical damage created during the optical fabrication process and significantly enhances the surface laser damage resistance (> 2×) and mechanical strength (up to ~ 2.6×). Sapphire AMP involves first treating the workpiece with a mixture of sulfuric and phosphoric acid ([H 2 SO 4 ]:[H 3 PO 4 ]= 1 : 3) at 220°C, followed with phosphoric acid at 160°C, then with sodium hydroxide base (NaOH) and surfactant at 40°C, and finally with a high-pressure deionized water spray rinse. Sapphire AMP has been demonstrated on both A- and C-plane sapphire workpieces. The mechanism of this etch process involves the reaction of the sapphire (Al 2 O 3 ) surface with sulfuric acid (H 2 SO 4 ) forming aluminum sulfate [Al2(SO4)3], which has low solubility. The high phosphoric acid content in the first and second steps of sapphire AMP results in the efficient conversion of Al 2 (SO 4 ) 3 to aluminum phosphate (AlPO 4 ), which is very soluble, greatly reducing reaction product redeposition on the workpiece surface. Sapphire AMP is shown to expose sub-surface mechanical damage on the sapphire surface created during the grinding and polishing processes, whose etched morphology has either isotropic or anisotropic evolution depending on the nature of the initial surface damage. Sapphire AMP was also designed to remove the key known surface, laser absorbing precursors (namely, foreign chemical impurities, the fracture surface layer of preexisting sub-surface damage, and reaction product or foreign species redeposition or precipitation). Static and sliding indention induced surface microfractures on sapphire are shown after sapphire AMP to have a significant decrease in the fast photoluminescence intensity (a known metric for measuring the degree of laser damaging absorbing precursors). In addition, the onset of laser damage (at 351 nm 3 ns) on sapphire AMP treated workpieces was shown to increase in fluence from ~ 4 to >9.5J/cm 2 . Finally, biaxial ball-on-ring mechanical tests on sapphire disks showed an increase in the failure stress from 340 MPa (with pre-existing 28 µm flaws) to ~ 900MPa after sapphire AMP, which is attributed to the blunting of the surface microfractures.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Entropy-defect synergy for dual luminescence mechanism in spinel: Time-resolved anti-counterfeiting and fingerprint visualization

Multimodal luminescent materials, while promising for anti-counterfeiting, often lack dynamic time-dependent responses and controllable spatial distribution, limiting their encryption capabilities in the spatiotemporal dimension. Here, this work presents a coordinated control strategy based on entropy and defect engineering, and uses a backpropagation (BP) neural network for material screening to successfully prepare spinel Mg 0.8 (Fe 0.04 Co 0.04 Ni 0.04 Cu 0.04 Zn 0.04 )Cr 2 O 4 (MgA 5 CO) phosphors with time-dependent dynamic luminescence behavior. This phosphor simultaneously activated the d-d transition luminescence (∼618 nm) derived from Co 2+ /Cr 3+ and the defect luminescence (∼398 nm) related to zinc vacancies (V Zn ) in a single-phase solid solution. The phosphor exhibits a time-dependent color evolution from pink to purple under fixed-wavelength excitation, due to the different excited-state dynamics and decay lifetimes associated with the d-d transition and defect luminescence. Structural characterization and spectral analysis confirmed the existence of V Zn and its significant role in defect luminescence process. The fluorescent and dynamic luminescent properties of entropy-based spinel oxide enable its use in advanced anti-counterfeiting applications like fingerprint recognition and color-changing dedicated anti-counterfeiting mark, showing promise in high-end and time-dynamic anti-counterfeiting fields. This research not only developed a new type of fluorescent dynamic anti-counterfeiting material, but also provided a new idea for constructing advanced optical functional materials with multiple luminescence mechanisms.

Defect project↗

DOE OSTI2022

Mechanical and tribological properties of anodic Al coatings as a function of anodizing conditions

Enhanced wear and corrosion resistance properties are vital for numerous functional and decorative applications. Anodizing is a process frequently used to generate stable oxide coatings on metal surfaces, including aluminium (Al). In this work, we present an evaluation of process variables for optimized anodized coating properties using existing methods and as a baseline for novel coating development. A representative relatively pure Al alloy was chosen as a model system with a goal of finding conditions to achieve high wear coatings with retained ductility. AA5052 alloy coupons were anodized in two different electrolytes (sulfuric and phosphoric acid) to study the effects of anodizing conditions on the mechanical and tribological properties of the anodic coatings. Porosity was evaluated with microscopy, coating hardness was determined via nanoindentation, and tribological properties were characterized using a pin-on-disk tribometer. These measurements were correlated and a loading evaluation was performed to assess the optimum nanoindentation parameters for the use of representative coupons without the need for special processing prior to anodizing. The porosity and coating thickness were found to depend on the anodizing time and the type of electrolyte. Thicker and harder anodic coatings were generated in sulfuric acid compared to phosphoric acid. Porosity studies of the anodic coatings generated in phosphoric acid revealed that coating porosity decreased as the anodizing time increased. Both electrolytes generated anodic coatings with improved tribological properties (friction coefficient and dimensional wear rate), and an optimum processing time was identified for best wear properties.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Lipid accumulation in nitrogen and phosphorus-limited yeast is caused by less growth-related dilution

Oleaginous yeasts are used commercially to produce oleochemicals and hold potential also for biodiesel production. In response to nitrogen or phosphorous limitation, oleaginous yeasts accumulate lipids in the form of triacylglycerols. Previous work has investigated potential mechanisms by which nutrient limitation induces lipid biosynthesis without verifying whether lipid biosynthesis flux is actually enhanced. Here, in this work, we show, using 13C-glucose tracing, that in nitrogen or phosphorous limitation, lipid accumulation occurs without consistent increases in biosynthetic flux. Instead, the main driver of increased lipid pools is decreased growth-related dilution. This conclusion holds across two divergent oleaginous yeasts: Rhodotorula toruloides and Yarrowia lipolytica . Quantitative proteomics shows a substantial proteome reallocation in response to nitrogen and phosphorous limitation, with ribosomal proteins strongly downregulated, while lipid enzymes are preserved but not consistently upregulated in absolute quantity. Thus, nutrient limitation, rather than triggering greatly enhanced lipid synthesis, results in roughly sustained lipid enzyme levels and biosynthetic flux. Due to slower lipid dilution by cell division, this suffices to drive marked lipid accumulation.

09 BIOMASS FUELS↗