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DOE OSTI2024

Technoeconomic Assessment of Phosphoric Acid and Rare Earth Element Recovery from Phosphoric Acid Sludge

Sustainability faces many challenges, including the availability of materials necessary for technological advancement. Rare earth elements (REEs), for example, are key materials for several manufacturing industries that can unlock renewable energy and sustainable development. In this study, a decanter centrifuge has been employed to successfully separated phosphoric acid and REE-containing particles from phosphoric acid sludge with concentrations ranging from 1000 to 2200 ppm REEs. Operating efficiently with up to 35 wt.% solids, the centrifuge was demonstrated to achieve approximately 95% phosphoric acid recovery and 90% REE recovery in a single pass, eliminating the need for additional processing steps. This breakthrough supports a proposed rare earth oxide (REO) recovery process integrating phosphoric acid (PA), elemental phosphorus (P4), and REO into two potential pathways: PA-REO and PA-P4-REO. These processes aim to reintroduce recovered phosphoric acid into the main product to significantly increase output and revenue. Post-separation, phosphorus-rich particles can be converted to P4, while REE-containing solids undergo further treatment including acid leaching, extraction/stripping, precipitation, and calcination to produce a marketable REO material. Technoeconomic analysis indicates promising profitability, with the PA-REO process showing a delta net present value (ΔNPV) of USD 441.8 million over a 12-year period and expected return within a year of construction, while the PA-P4-REO process yields a ΔNPV of USD 178.7 million over a 12-year return period. Both pathways offer robust financial prospects and demonstrate the feasibility of commercial-scale REO recovery from phosphoric acid sludge, offering an economically feasible approach to produce REEs for future sustainable development challenges related to sustainability.

36 MATERIALS SCIENCE↗

NASA NTRS2004

Depth-Penetrating Measurements Developed for Thermal Barrier Coatings Incorporating Thermographic Phosphors

The insulating properties of thermal barrier coatings (TBCs) provide highly beneficial thermal protection to turbine engine components by reducing the temperature sustained by those components. Therefore, measuring the temperature beneath the TBC is critical for determining whether the TBC is performing its insulating function. Currently, noncontact temperature measurements are performed by infrared pyrometry, which unfortunately measures the TBC surface temperature rather than the temperature of the underlying component. To remedy this problem, the NASA Glenn Research Center, under the Information Rich Test Instrumentation Project, developed a technique to measure the temperature beneath the TBC by incorporating a thin phosphor layer beneath the TBC. By performing fluorescence decay-time measurements on light emission from this phosphor layer, Glenn successfully measured temperatures from the phosphor layer up to 1100 C. This is the first successful demonstration of temperature measurements that penetrate beneath the TBC. Thermographic phosphors have a history of providing noncontact surface temperature measurements. Conventionally, a thermographic phosphor is applied to the material surface and temperature measurements are performed by exciting the phosphor with ultraviolet light and then measuring the temperature-dependent decay time of the phosphor emission at a longer wavelength. The innovative feature of the new approach is to take advantage of the relative transparency of the TBC (composed of yttria-stabilized zirconia) in order to excite and measure the phosphor emission beneath the TBC. The primary obstacle to achieving depth-penetrating temperature measurements is that the TBCs are completely opaque to the ultraviolet light usually employed to excite the phosphor. The strategy that Glenn pursued was to select a thermographic phosphor that could be excited and emit at wavelengths that could be transmitted through the TBC. The phosphor that was selected was yttria doped with europia (Y2O3:Eu), which has a minor excitation peak at 532 nm (green) and an emission peak at 611 nm (red)--both are wavelengths that exhibit significant transmission through the TBC. The measurements were performed on specimens consisting of a 25- m-thick phosphor layer beneath a 100- m-thick TBC. The 532-nm (green) excitation light was provided by a frequency-doubled YAG:Nd (yttrium-aluminum-garnet:neodymium) laser, and the fluorescence decay time measurements were acquired with a modified Raman microscope. The preceding graph compares the intensity of the phosphor emission of the phosphor layer above the TBC versus that of the phosphor layer beneath the TBC. Although there was considerable attenuation of the phosphor signal (a factor of 30), the phosphor emission at the reduced intensity was more than sufficient to perform fluorescence decay time measurements. The following graph shows the fluorescence lifetime temperature dependency for the Y2O3:Eu phosphor layers both above and below the TBC. These curves show an excellent match and indicate that, despite the attenuation due to the overlying TBC, the phosphor layer beneath the TBC still functions as an effective temperature indicator.

Eldridge, Jeffrey I.↗

NASA NTRS1998

Reduction and Analysis of Phosphor Thermography Data With the IHEAT Software Package

Detailed aeroheating information is critical to the successful design of a thermal protection system (TPS) for an aerospace vehicle. This report describes NASA Langley Research Center's (LaRC) two-color relative-intensity phosphor thermography method and the IHEAT software package which is used for the efficient data reduction and analysis of the phosphor image data. Development of theory is provided for a new weighted two-color relative-intensity fluorescence theory for quantitatively determining surface temperatures on hypersonic wind tunnel models; an improved application of the one-dimensional conduction theory for use in determining global heating mappings; and extrapolation of wind tunnel data to flight surface temperatures. The phosphor methodology at LaRC is presented including descriptions of phosphor model fabrication, test facilities and phosphor video acquisition systems. A discussion of the calibration procedures, data reduction and data analysis is given. Estimates of the total uncertainties (with a 95% confidence level) associated with the phosphor technique are shown to be approximately 8 to 10 percent in the Langley's 31-Inch Mach 10 Tunnel and 7 to 10 percent in the 20-Inch Mach 6 Tunnel. A comparison with thin-film measurements using two-inch radius hemispheres shows the phosphor data to be within 7 percent of thin-film measurements and to agree even better with predictions via a LATCH computational fluid dynamics solution (CFD). Good agreement between phosphor data and LAURA CFD computations on the forebody of a vertical takeoff/vertical lander configuration at four angles of attack is also shown. In addition, a comparison is given between Mach 6 phosphor data and laminar and turbulent solutions generated using the LAURA, GASP and LATCH CFD codes. Finally, the extrapolation method developed in this report is applied to the X-34 configuration with good agreement between the phosphor extrapolation and LAURA flight surface temperature predictions. The phosphor process outlined in the paper is believed to provide the aerothermodynamic community with a valuable capability for rapidly obtaining (4 to 5 weeks) detailed heating information needed in TPS design.

Merski, N. Ronald↗

NASA NTRS2003

High-Temperature Sprayable Phosphor Coating Developed for Measuring Surface Temperatures

The use of phosphor thermography for noncontact temperature measurements in harsh environments has been proven over the last decade, but it has suffered from difficult application procedures such as vapor deposition or sputtering techniques. We have developed a high-temperature-sensitive paint that is easily applied with commercially available paint-spraying equipment and have successfully demonstrated it to temperatures up to 1500 C. Selected phosphors have also shown measurable signals to 1700 C, thus allowing a combination of phosphors to be used in high-temperature binders to make surface temperature measurements from ambient to over 1500 C. Phosphor thermography is an optical technique that measures the time response of fluorescence light, which is a function of the phosphor temperature. The phosphors are excited with short wavelength light (ultraviolet or blue), and they emit light at a longer wavelength. This technique has a benefit over other temperature measurements, such as thermocouples and infrared thermography, in difficult environments such as high blackbody backgrounds, vibration, flames, high electromagnetic noise, or where special windows may be needed. In addition, the sprayable phosphor paints easily cover large or complicated structures, providing full-surface information with a single measurement. Oak Ridge National Laboratories developed and tested the high-temperature binders and phosphors under the direction of the NASA Glenn Research Center. Refractory materials doped with rare earth metals were selected for their performance at high temperature. Survivability, adhesion, and material compatibility tests were conducted at high temperatures in a small furnace while the fluorescent response from the phosphors was being measured. A painted sample in a furnace with a clearly visible fluorescing dot excited by a pulsed laser is shown. Measuring the decay time of this fluorescence yields the surface temperature. One new paint was recently tested in a rocket test stand at Glenn. The floor of a square duct nozzle was painted, and full-field lifetime decay measurements were acquired for multiple firings of the rocket. Good agreement with predicted results was obtained, matching temperature gradients along the length of the nozzle and clearly showing shock structures. These good results were very satisfactory given that the measurements were made looking through the combustion plume. Infrared pyrometry was incapable of making the surface measurements because of the interference from the rocket exhaust, which contaminated the infrared signature.

Bencic, Timothy J.↗

NASA NTRS1991

A relative-intensity two-color phosphor thermography system

The NASA LaRC has developed a relative-intensity two-color phosphor thermography system. This system has become a standard technique for acquiring aerothermodynamic data in LaRC Hypersonic Facilities Complex (HFC). The relative intensity theory and its application to the LaRC phosphor thermography system is discussed along with the investment casting technique which is critical to the utilization of the phosphor method for aerothermodynamic studies. Various approaches to obtaining quantitative heat transfer data using thermographic phosphors are addressed and comparisons between thin-film data and thermographic phosphor data on an orbiter-like configuration are presented. In general, data from these two techniques are in good agreement. A discussion is given on the application of phosphors to integration heat transfer data reduction techniques (the thin film method) and preliminary heat transfer data obtained on a calibration sphere using thin-film equations are presented. Finally, plans for a new phosphor system which uses target recognition software are discussed.

Merski, N. Ronald↗

NASA NTRS2003

Depth-Selective Diagnostics of Thermal Barrier Coatings Incorporating Thermographic Phosphors

Thermographic phosphors have been previously demonstrated to provide effective non-contact, emissivity-independent surface temperature measurements. Because of the translucent nature of thermal barrier coatings (TBCs), thermographic-phosphor-based temperature measurements can be extended beyond the surface to provide depth-selective temperature measurements by incorporating the thermographic phosphor layer at the depth where the temperature measurement is desired. In this paper, thermographic phosphor (Y2O3:Eu) fluorescence decay time measurements are demonstrated for the first time to provide through-the-coating-thickness temperature readings up to 1000 C with the phosphor layer residing beneath a 100-Fm-thick TBC (plasma-sprayed 8wt% yttria-stabilized zirconia). With an appropriately chosen excitation wavelength and detection configuration, it is shown that sufficient phosphor emission is generated to provide effective temperature measurements, despite the attenuation of both the excitation and emission intensities by the overlying TBC. This depth-selective temperature measurement capability should prove particularly useful for TBC diagnostics, where a large thermal gradient is typically present across the TBC thickness.

Eldridge, Jeffrey I.↗

NASA NTRS2003

Depth-Selective Diagnostics of Thermal Barrier Coatings Incorporating Thermographic Phosphors

Thermographic phosphors have been previously demonstrated to provide effective non- contact, emissivity-independent surface temperature measurements. Because of the translucent nature of thermal barrier coatings (TBCs), thermographic-phosphor-based temperature measurements can be extended beyond the surface to provide depth-selective temperature measurements by incorporating the thermographic phosphor layer at the depth where the temperature measurement is desired. In this paper, the use of thermographic phosphor (Y2O3:Eu) luminescence decay time measurements is demonstrated for the first time for through-the-thickness temperature readings up to 1000 C with the phosphor placed beneath a 100-micron-thick TBC (plasma-sprayed 8wt% yttria-stabilized zirconia). With an appropriately chosen excitation wavelength and detection configuration, it is shown that sufficient phosphor emission is generated to provide effective temperature measurements, despite the attenuation of both the excitation and emission intensities by the overlying TBC. This depth-selective temperature measurement capability should prove particularly useful for TBC diagnostics, where a large thermal gradient is typically present across the TBC thickness.

Eldridge, J. I.↗

NASA NTRS2003

Depth-Penetrating Temperature Measurements of Thermal Barrier Coatings Incorporating Thermographic Phosphors

Thermographic phosphors have been previously demonstrated to provide effective non-contact, emissivity-independent surface temperature measurements. Because of the translucent nature of thermal barrier coatings (TBCs), thermographic phosphor-based temperature measurements can be extended beyond the surface to provide depth-selective temperature measurements by incorporating the thermographic phosphor layer at the depth where the temperature measurement is desired. In this paper, thermographic phosphor (Y2O3:Eu) fluorescence decay time measurements are demonstrated to provide through-the-coating thickness temperature readings up to 1100 C with the phosphor layer residing beneath a 100 micron thick TBC (plasma-sprayed 8wt% yttria-stabilized zirconia). With an appropriately chosen excitation wavelength and detection configuration, it is shown that sufficient phosphor emission is generated to provide effective temperature measurements, despite the attenuation of both the excitation and emission intensities by the overlying TBC. This depth-penetrating temperature measurement capability should prove particularly useful for TBC diagnostics where a large thermal gradient is typically present across the TBC thickness. The fluorescence decay from the Y2O3:Eu layer exhibited both an initial short-term exponential rise and a longer-term exponential decay. The rise time constant was demonstrated to provide better temperature indication below 500 C while the decay time constant was a better indicator at higher temperatures.

Eldridge, Jeffrey I.↗

NASA NTRS2000

Long-persistence blue phosphors

This invention relates to phosphors including long-persistence blue phosphors. Phosphors of the invention are represented by the general formula: MO . mAl.sub.2 O.sub.3 :Eu.sup.2+,R.sup.3+ wherein m is a number ranging from about 1.6 to about 2.2, M is Sr or a combination of Sr with Ca and Ba or both, R.sup.3+ is a trivalent metal ion or trivalent Bi or a mixture of these trivalent ions, Eu.sup.2+ is present at a level up to about 5 mol % of M, and R.sup.3+ is present at a level up to about 5 mol % of M. Phosphors of this invention include powders, ceramics, single crystals and single crystal fibers. A method of manufacturing improved phosphors and a method of manufacturing single crystal phosphors are also provided.

Yen, William M.↗

NASA NTRS2001

Phosphors with long-persistent green phosphorescence

This invention relates to phosphors including long-persistence green phosphors. Phosphors of the invention are represented by the general formula: M.sub.k Al.sub.2 O.sub.4 :2xEu.sup.2+,2yR.sup.3+ wherein k-1-2x-2y, x is a number ranging from about 0.0001 to about 0.05, y is a number ranging from about x to about 3x, M is an alkaline earth metal, and R.sup.3+ is one or more trivalent metal ions. Phosphors of this invention include powders, ceramics, single crystals and single crystal fibers. A method of manufacturing improved phosphors and a method of manufacturing single crystal phosphors are also provided.

Yen, William M↗

DOE OSTI2025

Cryogenic Vibrational Spectroscopy of the Deprotonated Dimer of Phosphoric Acid

Phosphate-containing molecules are ubiquitous in nature, where they play crucial roles in biochemical processes. Further, they are of technical importance, for example, in certain batteries and in fuel cells, where a unique property of phosphoric acid is exploited its exceptionally high proton conductivity. Proton transport in phosphoric acid is known to involve proton shuttling; however, the elementary steps involved are not clear. To elucidate the hydrogen bonding preferences of phosphoric acid, we investigate the dihydrogen phosphate anion as well as the deprotonated dimer of phosphoric acid (H 3 PO 4 ·H 2 PO 4 − ) in the gas phase using infrared action spectroscopy in helium nanodroplets and infrared D 2 -tagging photodissociation spectroscopy, and the experimental spectra are compared to theoretical ones. Theory finds for H 3 PO 4 ·H 2 PO 4 − two different structures that are predicted to be nearly isoenergetic. The comparison to the experimental spectra, however, allows for a clear assignment and structure identification. The resulting structure has an interesting binding motif, which might be of relevance to interactions of phosphoric acid in the condensed phase and which can serve as a benchmark for quantum chemical calculations.

Chemical structure↗

NASA NTRS1991

Laser discrimination by stimulated emission of a phosphor

A method for discriminating sources of UV, near infrared, and far infrared laser radiation was discovered. This technology is based on the use of a single magnesium sulfide phosphor doubly doped with rare earth ions, which is thermally/optically stimulated to generate colors correlatable to the incident laser radiation. The phosphor, after initial charging by visible light, exhibits green stimulated luminescence when exposed to a near infrared source (Nd: YAG laser). On exposure to far infrared sources (CO2 laser) the phosphor emission changes to orange color. A UV laser produces both an orange red as well as green color. A device using this phosphor is useful for detecting the laser and for discriminating between the near infrared, far infrared, and UV lasers. The technology is also capable of infrared laser diode beam profiling since the radiation source leaves an imprint on the phosphor that can be photographed. Continued development of the technology offers potential for discrimination between even smaller bandwidths within the infrared spectrum, a possible aid to communication or wavemixing devices that need to rapidly identify and process optical signals.

Mathur, V. K.↗

NASA NTRS2009

Thermal and Electrical Conductivity Measurements of CDA 510 Phosphor Bronze

Many cryogenic systems use electrical cables containing phosphor bronze wire. While phosphor bronze's electrical and thermal conductivity values have been published, there is significant variation among different phosphor bronze formulations. The James Webb Space Telescope (JWST) will use several phosphor bronze wire harnesses containing a specific formulation (CDA 510, annealed temper). The heat conducted into the JWST instrument stage is dominated by these harnesses, and approximately half of the harness conductance is due to the phosphor bronze wires. Since the JWST radiators are expected to just keep the instruments at their operating temperature with limited cooling margin, it is important to know the thermal conductivity of the actual alloy being used. We describe an experiment which measured the electrical and thermal conductivity of this material between 4 and 295 Kelvin.

Tuttle, James E.↗

DOE OSTI2024

Phosphor Ceramic Composite for Tunable Warm White Light

Composite phosphor ceramics for warm white LED lighting were fabricated with K 2 SiF 6 :Mn 4+ (KSF) as both a narrowband red phosphor and a translucent matrix in which yellow-emitting Y 3 Al 5 O 12 :Ce 3+ (YAG) particles were dispersed. The emission spectra of these composites under blue LED excitation were studied as a function of YAG loading and thickness. Warm white light with a color temperature of 2716 K, a high CRI of 92.6, and an R9 of 77.6 was achieved. A modest improvement in the thermal conductivity of the KSF ceramic of up to 9% was observed with the addition of YAG particles. In addition, a simple model was developed for predicting the emission spectra based on several parameters of the composite ceramics and validated with the experimental results. The emission spectrum can be tuned by varying the dopant concentrations, thickness, YAG loading, and YAG particle size. This work demonstrates the utility of KSF/YAG composite phosphor ceramics as a means of producing warm white light, which are potentially suitable for higher-drive applications due to their increased thermal conductivity and reduced droop compared with silicone-dispersed phosphor powders.

36 MATERIALS SCIENCE↗

NASA NTRS2015

Surface Temperature Measurements from a Stator Vane Doublet in a Turbine Engine Afterburner Flame Using a YAG:Tm Thermographic Phosphor

Luminescence-based surface temperature measurements were obtained from a YAG:Tm-coated stator vane doublet exposed to the afterburner flame of a J85 test engine at University of Tennessee Space Institute (UTSI). The objective of the testing was to demonstrate that reliable surface temperatures based on luminescence decay of a thermographic phosphor producing short-wavelength emission could be obtained from the surface of an actual engine component in a high gas velocity, highly radiative afterburner flame environment. YAG:Tm was selected as the thermographic phosphor for its blue emission at 456 nm (1D23F4 transition) and UV emission at 365 nm (1D23H6 transition) because background thermal radiation is lower at these wavelengths, which are shorter than those of many previously used thermographic phosphors. Luminescence decay measurements were acquired using a probe designed to operate in the afterburner flame environment. The probe was mounted on the sidewall of a high-pressure turbine vane doublet from a Honeywell TECH7000 turbine engine coated with a standard electron-beam physical vapor deposited (EB-PVD) 200-m-thick TBC composed of yttria-stabilized zirconia (YSZ) onto which a 25-m-thick YAG:Tm thermographic phosphor layer was deposited by solution precursor plasma spray (SPPS). Spot temperature measurements were obtained by measuring luminescence decay times at different afterburner power settings and then converting decay time to temperature via calibration curves. Temperature measurements using the decays of the 456 and 365 nm emissions are compared. While successful afterburner environment measurements were obtained to about 1300C with the 456 nm emission, successful temperature measurements using the 365 nm emission were limited to about 1100C due to interference by autofluorescence of probe optics at short decay times.

thermographic phosphor↗

DOE OSTI2025

Increasing the Stability of Deep Blue Phosphor‐Sensitized OLEDs Using the Polariton‐Enhanced Purcell Effect

Abstract The stability of efficient, deep blue organic light‐emitting diodes (OLEDs) remains a major challenge in the field of organic electronics. Poor device stability originates from the high probability for destructive non‐radiative triplet exciton annihilation events. Phosphor‐sensitized fluorescence (PSF) is proposed to achieve an efficient, deep blue color by energy transfer from phosphors to fluorophores. Recently, the polariton‐enhanced Purcell (PEP) effect is introduced to decrease the triplet radiative lifetime and density, resulting in an increase in blue phosphorescent OLED lifetime. Here, the PEP effect is introduced to enhance the stability of the PSF‐OLEDs. It is shown that the PEP effect increases all radiative decay rates of the phosphors and fluorophores, leading to a reduction in the triplet annihilation events. Using a Pt‐complex phosphor sensitizer and a so‐called multi‐resonance fluorescent emitter in a PEP cavity, a 3.1‐fold lifetime increase is observed at a current density ofJ= 10 mA cm −2 , reduced EQE roll‐off and deep blue color with Commission Internationale de l'Eclairage coordinates of (0.13, 0.09). The PEP effect maximally extends PSF‐OLED lifetimes in devices with the highest triplet‐to‐singlet energy transfer rates. Moreover, this work suggests that the benefits of PEPs apply to all triplet‐based OLEDs.

Chemistry↗

NASA NTRS1985

Persistence of phosphor glow in microchannel plate image intensifiers

Image intensifier tubes using microchannel plate amplification stages and phosphor output stages are being increasingly used in various detection applications. In this paper, measurements of the decay times of what are attributed to be the P20 phosphors in various image intensifiers are reported. It is found that the long tail on the decay curve of the phosphor following illumination can be a limitation for certain observations. In addition, the background level of phosphor glow (which is seen by the subsequent detection system as a light signal) continues to build with continuing illumination.

Torr, M. R.↗

NASA NTRS1988

Single-Layer, Multicolor Electroluminescent Phosphors

Etching eliminated in producing phosphor layers for displays. New process enables production of single-layer, two-color phosphor layer without etching. Method of construction, beginning with glass substrate with electrode and insulator layers, involves deposition of green phosphor masking with metal mask or photoresist; diffusion or ion implantation of manganese through mask to produce red phosphor and removal of mask.

Robertson, James B.↗