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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Role of Silica Support in Phosphoric Acid Catalyzed Production of p -Xylene from 2,5-Dimethylfuran and Ethylene

p-Xylene is a commodity chemical of industrial importance for terephthalic acid production, for which renewable sourcing from naturally abundant lignocellulosic biomass is highly desired. Previous work demonstrated that phosphoric acid stabilized on siliceous zeolite supports (e.g., P-BEA, P-SPP) exhibits high selectivity toward p-xylene (>97%) from 2,5-dimethylfuran (DMF) and ethylene. However, the effect of the support and the contribution of heterogeneous versus homogeneous phosphoric acid on the observed catalytic behavior in the solvated reaction system have not been addressed. Here, we determine the phosphoric acid catalytic activity for DMF conversion and its selectivity to p-xylene when it is supported on a silica support as well as in the absence of a support. Specifically, phosphoric acid catalysis was studied in three different scenarios: (1) phosphoric acid was added in the liquid reaction mixture in the absence of any solid support, (2) phosphoric acid was added in the liquid reaction mixture along with inert silica support including siliceous zeolite (i.e., allowing for phosphoric acid–support assembly to proceed in the reaction mixture), and (3) phosphoric acid was first impregnated on the siliceous zeolite support and then the preassembled supported phosphoric acid catalyst was added in the liquid reaction mixture. We found that the reaction rate and selectivity to p-xylene are different in the above scenarios reflecting the effect of the solid support on the catalytic performance of phosphoric acid. In scenario 1, a low concentration of phosphoric acid (1.7 mM) in the absence of any solid support exhibited high selectivity to p-xylene (80% selectivity to p-xylene at 60% conversion of DMF), which decreased with increasing acid concentration. The selectivity to p-xylene and activity of phosphoric acid significantly increased by adding a silica support into the reaction system (scenario 2). Furthermore, this improvement was attributed to phosphoric acid partial association with the surface of the silica support under the reaction conditions (in situ catalyst assembly). Phosphoric acid predeposited on siliceous zeolite supports (e.g., P-BEA, P-SPP) synthesized via impregnation prior to the reaction (scenario 3) catalyzed the reaction heterogeneously without noticeable leaching and exhibited the highest activity and selectivity to p-xylene, suggesting an important role of the silica support and the need to ensure that phosphoric acid acts as a heterogeneous catalyst in order to accomplish selective conversion of DMF to p-xylene.

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

Continuous recovery of phosphoric acid and Rare-Earths containing particles from phosphoric acid sludge using a decanter centrifuge

Recovery of rare earth elements (REEs) from various industrial and natural streams currently draws significant attention in efforts to meet the demands of the manufacturing industry. Among many industrial byproducts and waste streams, phosphoric acid sludge could be one of the most economically feasible resources for the recovery of REEs because solid particles in the sludge contain relatively concentrated REEs, up to 3,000 ppm, while the liquid component of the sludge is valuable phosphoric acid (P 2 O 5 ) that can be recovered and returned to the main product. Due to high viscosity and large solids content (e.g., 30–40 %), however, this byproduct stream requires multistep separation and purification processes. In this study, a single-step process involving a continuous-flow decanter centrifuge (CFDC) was employed to investigate its feasibility for continuous solid/liquid separation from real phosphoric acid sludge. High centrifugal forces generated from up to 1500 G gravity acceleration separate solid particles from the sludge, generating a liquid-rich stream and a solids-rich stream at the exit of the CFDC. A single pass of phosphoric-acid sludge through the CFDC yielded 95 % liquid recovery and 90 % recovery of REEs-containing solids from 20 to 34 wt% solids-containing sludge. Finally, a reduced order model developed for the CFDC operation showed good agreement with experimental data, and preliminary technoeconomic analysis revealed potential process feasibility.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
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↗
DOE OSTI2020

New red phosphor ceramic K 2 SiF 6 :Mn 4+

We report a new transparent ceramic phosphor for use in LED lighting has been fabricated. The previously reported and optimized narrow-emitting red phosphor, K 2 SiF 6 :Mn 4+ (KSF), has been consolidated into a transparent ceramic phosphor for the first time, accomplished via hot-pressing the feedstock phosphor powder in a die under vacuum. KSF ceramics were fabricated with varying doping concentrations of Mn 4+ and their properties studied. The absorption and emission spectra of the ceramics were identical to the feedstock phosphor powders and are ideal for LED lighting with strong absorption at 450 nm and narrow emission around 630 nm. The absorbance of the ceramics was directly proportional to the doping concentration. The ceramics were excited at various blue light fluxes and their emission intensities measured to study the effect of Mn 4+ concentration on intensity-driven “droop” in the emission output. The ceramics with a lower Mn 4+ doping were more efficient under higher light fluxes due to a decrease in Auger upconversion losses. KSF ceramics can allow a much longer path length of the diode light through the phosphor, as compared to phosphor-in-silicone, enabling the use of low optical absorption and the associated reduced activator concentration. The ceramics are measured to have a thermal conductivity of ~1.0 W/m-K, higher than that of phosphor-in-silicone or phosphor-in-glass. Several of these properties make KSF ceramics potentially desirable for use in white light LEDs. Greater thermal conductivity helps with heat dissipation, the lower surface area of the ceramic compared to the powder minimizes the environmental vulnerability of KSF, and the ability to lower the Mn 4+ concentration reduces Auger recombination losses and mitigates the temperature rise, particularly at higher light flux.

36 MATERIALS SCIENCE↗
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.↗
DOE OSTI2021

Visible emission spectra of thermographic phosphors under x-ray excitation

Thermographic phosphors have been employed for temperature sensing in challenging environments, such as on surfaces or within solid samples exposed to dynamic heating, because of the high temporal and spatial resolution that can be achieved using this approach. Typically, UV light sources are employed to induce temperature-sensitive spectral responses from the phosphors. However, it would be beneficial to explore x-rays as an alternate excitation source to facilitate simultaneous x-ray imaging of material deformation and temperature of heated samples and to reduce UV absorption within solid samples being investigated. Here, the phosphors BaMgAl 10 O 17 :Eu (BAM), Y 2 SiO 5 :Ce, YAG:Dy, La 2 O 2 S:Eu, ZnGa 2 O 4 :Mn, Mg 3 F 2 GeO 4 :Mn, Gd 2 O 2 S:Tb, and ZnO were excited using incident synchrotron x-ray radiation. These materials were chosen to include conventional thermographic phosphors as well as x-ray scintillators (with crossover between these two categories). X-ray-induced thermographic behavior was explored through the measurement of visible spectral response with varying temperature. The incident x-rays were observed to excite the same electronic energy level transitions in these phosphors as UV excitation. Similar shifts in the spectral response of BAM, Y 2 SiO 5 :Ce, YAG:Dy, La 2 O 2 S:Eu, ZnGa 2 O 4 :Mn, Mg 3 F 2 GeO 4 :Mn, and Gd 2 O 2 S:Tb were observed when compared to their response to UV excitation found in literature. Some phosphors were observed to thermally quench in the temperature ranges tested here, while the response from others did not rise above background noise levels. This may be attributed to the increased probability of non-radiative energy release from these phosphors due to the high energy of the incident x-rays. These results indicate that x-rays can serve as a viable excitation source for phosphor thermometry.

42 ENGINEERING↗
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↗
DOE OSTI2023

A flexible polymer-based luminescent ink for combined thermographic phosphors and digital image correlation (TP+DIC)

Recent work on the development of integrated thermographic phosphors and digital image correlation (TP+DIC) for combined thermal–mechanical measurements has revealed the need for a flexible, stretchable phosphor coating for metal surfaces. Herein, we coat stainless steel substrates with a polymer-based phosphor ink in a DIC speckle pattern and demonstrate that the ink remains well bonded under substrate deformation. In contrast, a binderless phosphor DIC coating produced via aerosol deposition (AD) partially debonded from the substrate. DIC calculations reveal that the strain on the ink coating matches the strain on the substrate within 4% error at the highest substrate loads (0.05 mm/mm applied substrate strain), while the strain on the AD coating remains near 0 mm/mm as the substrate deforms. Spectrally resolved emission from the phosphor is measured through the transparent binder throughout testing, and the ratio method is used to infer temperature with an uncertainty of 1.7 °C. In conclusion, this phosphor ink coating will allow for accurate, non-contact strain and temperature measurements of a deforming surface.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Europium-doped barium chloride storage phosphor plate synthesized by pulsed laser deposition

In computed radiography, scattering of the stimulation light by the storage phosphor crystals in the imaging plates negatively impacts spatial resolution. Storage phosphor plates with thinner phosphor layers have been developed to reduce scattering distance and increase spatial resolution, although at the expense of reduced x-ray absorption. The authors hypothesize that a transparent or translucent nanostructured film, containing a much higher percentage of storage phosphor crystals than achievable in bulk glass-ceramic materials made by conventional methods, may have acceptable photostimulated luminescence efficiency and imaging performance characteristics greater than commercial imaging plates. Films were produced via pulsed laser deposition by alternating target materials of the storage phosphor BaCl 2 :Eu 2+ and either silica or silicon. X-ray diffraction and photoluminescence characterization were conducted to confirm the presence of BaCl 2 :Eu 2+ crystallites. The films were able to store optical data and be read out to produce x-ray radiographs demonstrating 50-mu m spatial resolution. The performance of the experimental storage phosphor plates was compared to commercially available imaging plates. The authors demonstrate for the first time the synthesis of a glass-ceramic imaging plate for computed radiography by pulsed laser deposition.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Combined thermographic phosphor and digital image correlation (TP + DIC) for simultaneous temperature and strain measurements

We report thermographic phosphors (TP) are combined with stereo digital image correlation (DIC) in a novel diagnostic, TP + DIC, to measure full-field surface strains and temperatures simultaneously. The TP + DIC method is presented, including corrections for nonlinear CMOS camera detectors and generation of pixel-wise calibration curves to relate the known temperature to the ratio of pixel intensities between two distinct wavelength bands. Additionally, DIC is employed not only for strain measurements but also for accurate image registration between the two cameras for the two-colour ratio method approach of phosphoric thermography. TP + DIC is applied to characterize the thermo-mechanical response of 304L stainless steel dog bones during tensile testing at different strain rates. The dog bones are patterned for DIC with Mg 3 F 2 GeO 4 :Mn (MFG) via aerosol deposition through a shadow mask. Temperatures up to 425°K (150°C) and strains up to 1.0 mm/mm are measured in the localized necking region, with conservative noise levels of 10°K and 0.01 mm/mm or less. Finally, TP + DIC is compared to the more established method of combining infrared (IR) thermography with DIC (IR + DIC), with results agreeing favourably. Three topics of continued research are identified, including cracking of the aerosol-deposited phosphor DIC features, incomplete illumination for pixels on the border of the phosphor features, and phosphor emission evolution as a function of applied substrate strain. This work demonstrates the combination of phosphor thermography and DIC and lays the foundation for further development of TP + DIC for testing in combined thermo-mechancial environments.

304L stainless steel↗
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.↗