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All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Mid-infrared luminescence properties of erbium and dysprosium doped lanthanum titanate glasses

Glasses of composition x RE 2 O 3 -(17− x ) La 2 O 3 -83 TiO 2 were prepared by levitation melting from x = 0.1 to 9 for RE=Er and at x =0.1 and 1 for RE=Dy. The glasses have high transition temperature, exhibit low OH, and 1 mm thick discs are transparent out to 6 μ m. Mid-infrared emission lineshapes and lifetimes are comparable to what is seen in tellurite glasses containing Er 3+ and Dy 3+ . For x fixed at 1, the Er 3+ : 4 I 11/2 → 4 I 13/2 transition at 2716 nm has a fluorescence lifetime of 254 μ s and the Dy 3+ : 6 H 13/2 → 6 H 15/2 transition at 2957 nm has a fluorescence lifetime of 9.09 μ s. The results indicate that doped lanthanum titanate glasses offer the thermal stability of a ’hard’ glass with the host properties typically associated with ’soft’ glasses. Problems with the measurement of spectral features in the mid-infrared that could erroneously be assigned as resulting from rare-earth ion emissions are presented and discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Impact of Erbium Doping in the Structural and Magnetic Properties of the Anisotropic and Frustrated SrYb 2 O 4 Antiferromagnet

We present a systematic study of the structural and magnetic properties of a series of powder samples of SrYb 2-x Er x O 4 with different Yb/Er concentrations. Magnetometry and neutron diffraction have been used to study the magnetic ground states of the compound series, while inelastic neutron scattering was used to investigate the crystal field excitations for a chosen concentration. These results show that the crystal structure remains the same for all compositions, while the lattice parameters increase linearly with the Er content. All compounds showed some type of magnetic transition below 1 K, however, both the magnetic structure and nature of the phase transition vary throughout the series. The samples present a non-collinear magnetic structure with the moments lying on the ab plane for low Er content. For high Er content, the magnetic structure is collinear with the moments aligned along the c-axis. A critical concentration is found where there is a bifurcation between zero-field and field-cooled magnetic susceptibility. This irreversible process could be due to the random mixture of single-ion magnetic anisotropies.

36 MATERIALS SCIENCE↗
NASA NTRS1982

Surface morphology of erbium silicide

The surface of rare-earth silicides (Er, Tb, etc.), formed by the reaction of thin-film metal layers with a silicon substrate, is typically dominated by deep penetrating, regularly shaped pits. These pits may have a detrimental effect on the electronic performance of low Schottky barrier height diodes utilizing such silicides on n-type Si. This study suggests that contamination at the metal-Si or silicide-Si interface is the primary cause of surface pitting. Surface pits may be reduced in density or eliminated entirely through either the use of Si substrate surfaces prepared under ultrahigh vacuum conditions prior to metal deposition and silicide formation or by means of ion irradiation techniques. Silicide layers formed by these techniques possess an almost planar morphology.

Lau, S. S.↗
NASA NTRS1990

A 980 nm pseudomorphic single quantum well laser for pumping erbium-doped optical fiber amplifiers

The authors have fabricated ridge waveguide pseudomorphic InGaAs/GaAs/AlGaAs GRIN-SCH SQW (graded-index separate-confinement-heterostructure single-quantum-well) lasers, emitting at 980 nm, with a maximum output power of 240 mW from one facet and a 22 percent coupling efficiency into a 1.55-micron single-mode optical fiber. These lasers satisfy the requirements on efficient and compact pump sources for Er3+-doped fiber amplifiers.

Larsson, A.↗
NASA NTRS2017

Experimental Observations of Nuclear Activity in Deuterated Materials Subjected to a Low-Energy Photon Beam

Exposure of highly deuterated materials to a low-energy (nom. 2 MeV) photon beam resulted in nuclear activity of both the parent metals of hafnium and erbium and a witness material (molybdenum) mixed with the reactants. Gamma spectral analysis of all deuterated materials, ErD2.8+C36D74+Mo and HfD2+C36D74+Mo, showed that nuclear processes had occurred as shown by unique gamma signatures. For the deuterated erbium specimens, posttest gamma spectra showed evidence of radioisotopes of erbium ((163)Er and (171)Er) and of molybdenum ((99)Mo and (101)Mo) and by beta decay, technetium (99mTc and 101Tc). For the deuterated hafnium specimens, posttest gamma spectra showed evidence of radioisotopes of hafnium (180mHf and 181Hf) and molybdenum ((99)Mo and (101)Mo), and by beta decay, technetium ((99m)Tc and (101)Tc). In contrast, when either the hydrogenated or non-gas-loaded erbium or hafnium materials were exposed to the gamma flux, the gamma spectra revealed no new isotopes. Neutron activation materials showed evidence of thermal and epithermal neutrons. CR-39 solid-state nuclear track detectors showed evidence of fast neutrons with energies between 1.4 and 2.5 MeV and several instances of triple tracks, indicating (is) greater than 10 MeV neutrons. Further study is required to determine the mechanism causing the nuclear activity.

Steinetz, Bruce M.↗
DOE OSTI2024

Optical and microstructural characterization of Er 3+ doped epitaxial cerium oxide on silicon

Rare-earth ion dopants in solid-state hosts are ideal candidates for quantum communication technologies, such as quantum memories, due to the intrinsic spin–photon interface of the rare-earth ion combined with the integration methods available in the solid state. Erbium-doped cerium oxide (Er:CeO 2 ) is a particularly promising host material platform for such a quantum memory, as it combines the telecom-wavelength (~ 1.5 μm) 4f–4f transition of erbium, a predicted long electron spin coherence time when embedded in CeO 2 , and a small lattice mismatch with silicon. In this work, we report on the epitaxial growth of Er:CeO 2 thin films on silicon using molecular beam epitaxy, with controlled erbium concentration between 2 and 130 parts per million (ppm). We carry out a detailed microstructural study to verify the CeO 2 host structure and characterize the spin and optical properties of the embedded Er 3+ ions as a function of doping density. In as-grown Er:CeO 2 in the 2–3 ppm regime, we identify an EPR linewidth of 245(1) MHz, an optical inhomogeneous linewidth of 9.5(2) GHz, an optical excited state lifetime of 3.5(1) ms, and a spectral diffusion-limited homogeneous linewidth as narrow as 4.8(3) MHz. We test the annealing of Er:CeO 2 films up to 900 °C, which yields narrowing of the inhomogeneous linewidth by 20% and extension of the excited state lifetime by 40%.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Photonic integration of Er 3+ :Y 2 SiO 5 with thin-film lithium niobate by flip chip bonding

Rare earth ions are known as promising candidates for building quantum light-matter interface. However, tunable photonic cavity access to rare earth ions in their desired host crystal remains challenging. Here, we demonstrate the integration of erbium doped yttrium orthosilicate (Er 3+ :Y 2 SiO 5 ) with thin-film lithium niobate photonic circuit by plasma-activated direct flip chip bonding. Resonant coupling to erbium ions is realized by on-chip electro-optically tuned high Q lithium niobate micro-ring resonators. Fluorescence and absorption of erbium ions at 1536.48 nm are measured in the waveguides, while the collective ion-cavity cooperativity with micro-ring resonators is assessed to be 0.36. This work presents a versatile scheme for future rare earth ion integrated quantum devices.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2020

Quantifying thermal barrier coating delamination through luminescence modeling

Thermal barrier coatings (TBCs) are widely used in the hot sections of gas turbine systems as they are remarkably efficient in insulating the underlying superalloys, leading to higher operating temperatures and therefore enhancing the performance of the engines. However, this benefit is only possible if the integrity of the TBC under aggressive thermo-mechanical environments is ensured. Delamination is a common but hard to detect failure mode. We present, in this work, supported by experimentation, the implementation of a modeling approach applying the Kubelka-Munk theory to provide numerical quantification of luminescence contrast and intensity due to top coat delamination in TBCs. The method relies on the drastic change in reflectivity when a delamination forms, exploiting it for high-contrast luminescence mapping. Two distinct TBC configurations containing an erbium-doped yttria-stabilized zirconia (YSZ:Er 3+ ) layer for delamination sensing were used to validate this model. A delamination zone induced by Rockwell indentation was successfully tracked by measuring an increase of the intensity of the erbium emission line at 562 nm. Luminescence-based methods for delamination detection can provide a revolutionary non-invasive technique, with potential for both off-line and on-line engine monitoring.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Spectroscopic study of GdVO{sub 4} : Yb + Er crystals

GdVO{sub 4} crystals doped with different erbium and ytterbium concentrations have been grown in order to study their spectroscopic and kinetic properties and identify the nature of active centres in them. Their polarised transmission and luminescence spectra have been used to construct energy level diagrams of the Er{sup 3+} ion. The lifetime of the lower level of the {sup 4}I{sub 11/2} excited-state multiplet has been shown to decrease markedly with increasing ytterbium concentration. Inequivalent erbium centres have been observed to form in the crystals with increasing ytterbium concentration. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2021

Microstructural Effects of High Dose Helium Implantation in ErD 2

Metal hydrides can store hydrogen isotopes with high volumetric density. In metal tritides, tritium beta decay can result in accumulation of helium within the solid, in some cases exceeding 10 at.% helium after only 4 years of aging. Helium is insoluble in most materials, but often does not readily escape, and instead coalesces to form nanoscale bubbles when helium concentrations are near 1 at.%. Blistering or spallation often occurs at higher concentrations. Radioactive particles shed during this process present a potential safety hazard. This study investigates the effects of high helium concentrations on erbium deuteride (ErD 2 ), a non-radioactive surrogate material for erbium tritide (ErT 2 ). To simulate tritium decay in the surrogate, high doses of 120 keV helium ions were implanted into ErD 2 films at room temperature. Scanning and transmission electron microscopy indicated spherical helium bubble formation at a critical concentration of 1.5 at.% and bubble linkage leading to nanoscale crack formation at a concentration of 7.5 at.%. Additionally, crack propagation occurred through the nanocrack region, resulting in spallation extending from the implantation peak to the surface. Electron energy loss spectroscopy was utilized to confirm the presence of high-pressure helium in the nanocracks, suggesting that helium gas plays a predominant role in deformation. This work improves the overall understanding of helium behavior in ErD 2 by using modern characterization techniques to determine: the critical helium concentration required for bubble formation, the material failure mechanism at high concentration, and the nanoscale mechanisms responsible for material failure in helium implanted ErD 2 .

36 MATERIALS SCIENCE↗
DOE OSTI2023

High-resolution laser system for the S 3 -Low Energy Branch

Here, in this paper we present the first high-resolution laser spectroscopy results obtained at the GISELE laser laboratory of the GANIL-SPIRAL2 facility, in preparation for the first experiments with the S 3 -Low Energy Branch. Studies of neutron-deficient radioactive isotopes of erbium and tin represent the first physics cases to be studied at S 3 . The measured isotope-shift and hyperfine structure data are presented for stable isotopes of these elements. The erbium isotopes were studied using the 4f 12 6s 2 3 H 6 → 4f 12 ( 3 H)6s6p J = 5 atomic transition (415 nm) and the tin isotopes were studied by the 5s 2 5p 2 ( 3 P 0 ) → 5s 2 5p6s( 3 P 1 ) atomic transition (286.4 nm), and are used as a benchmark of the laser setup. Additionally, the tin isotopes were studied by the 5s 2 5p6s( 3 P 1 ) → 5s 2 5p6p( 3 P 2 ) atomic transition (811.6 nm), for which new isotope-shift data was obtained and the corresponding field-shift F 812 and mass-shift M 812 factors are presented.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Comparing Pr 3+ and Nd 3+ for deactivating the Er 3+ : 4 I 13/2 level in lanthanum titanate glass

Erbium lanthanum titanate glasses were prepared by levitation melting for the spectroscopic study of ways to promote the mid-infrared fluorescence. Two series of heavily erbium doped glasses (15 wt%) were prepared with the addition of either Pr 3+ or Nd 3+ in amounts relative to Er 3+ of 0.05, 0.1, and 0.2. Both ions quench the lower Er 3+ laser level with the Pr 3+ doing so more rapidly. Although high co-dopant concentrations result in higher energy transfer, as clearly evidenced in upconversion and downconversion fluorescence measurements, the mid-infrared lifetime also suffers a reduction and, therefore, a balance must be struck in the co-dopant concentration. Lifetime and spectral measurements indicate that, at a fixed relative co-dopant amount, Pr 3+ is more effective than Nd 3+ at removing the bottleneck of the Er 3+ 4 I 13/2 level. Moreover, consideration of the lifetimes alongside the absorption data of the individual ions indicates that despite the large absorption cross-section of Nd 3+ at 808 nm, the concentration needed to yield more absorbed power than utilizing direct 976 nm excitation of Er 3+ results in unfavorable lifetimes of the mid-infrared transition. In the end, Pr 3+ prevails as the superior co-dopant in terms of the effects on fluorescence lifetimes as well as potential laser system design considerations. In a unique self-doping approach, a reducing melt atmosphere of Ar instead of O 2 creates a small fraction of Ti 3+ . In 5Er 2 O 3 -12La 2 O 3 -83TiO 2 glass, the presence of Ti 3+ quenches the 4 I 13/2 emission about 2.6 times more than the 4 I 11/2 when lifetimes are compared to an O 2 melt environment. As an additional means of increasing the mid-infrared emission, the effect of temperature on the mid- and near- infrared lifetimes of a lightly doped lanthanum titanate composition is investigated between 77-300 K. The mid-infrared lifetime increases by ∼30% while the near-infrared lifetime increases by ∼10%, which suggests in addition to co-doping, active cooling of the gain media will further enhance performance.

Materials Science↗
DOE OSTI2023

Direct Extraction of Lanthanide Oxides and Nitrates in Tributyl Phosphate

This work investigated the dissolution rate of lanthanide oxides and nitrates in a 30 vol % TBP-n-paraffin solvent (pre-equilibrated with various nitric acid concentrations) using visible (Vis) spectroscopy over time. Some dissolution mechanics were observed, such as an aqueous layer forming, considerably longer dissolution times for the heavier lanthanides (hours) vs. the lighter lanthanides (minutes), and the impacts of mixing lanthanide oxides or nitrates during dissolution. Neodymium, samarium, holmium, and erbium were selected due to their unique spectroscopic signatures and to represent the lighter (neodymium and samarium) and heavier (holmium and erbium) lanthanides. Even though europium does not have a strong absorbance in the range studied, europium was used in some instances to also represent the lighter lanthanides. Cerium oxide was used to representant dissolution of tetravalent lanthanides.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Quantum Transduction with Abundant Elements for Cleaner Energy

This three-year project established a new approach to calculating crystal field coefficients for rare-earth elements in solids, especially for quantum applications such as transduction. Crystal field values of erbium doping several oxide hosts were presented. In addition stoichiometric materials, erbium oxide and cerium vanadate and phosphate, were simulated to understand their properties for quantum information. A fundamental enhancement to transduction enabled by magnon interaction was presented, along with magnon calculations in several oxide hosts and 2D materials.

36 MATERIALS SCIENCE↗
NASA NTRS1995

Stress Tuning of Laser Crystals

The topic of stress tunable laser crystals is addressed in this study with the purpose of determining the piezo-optic coefficients of a new laser material. This data was collected using a quadruple pass birefringence technique because of its high degree of sensitivity relative to the other methods examined including fringe shift analysis using a Mach-Zender interferometer. A green He-Ne laser was passed through a light chopper and Glan-Thompson prism before entering a crystal of Erbium doped Yttrium Aluminum Garnet (Er:YAG) (used in order to validate the experimental technique). The Er:YAG crystal is mounted in a press mechanism and the laser is quadruple passed through test specimen before being returned through the prism and the orthogonally polarized portion of the beam measured with a optical sensor. At a later stage, the Er:YAG crystal was replaced with a new crystal in order to determine the piezo-optic coefficients of this uncharacterized material. The applied load was monitored with the use of a 50 lb. load cell placed in line with the press. Light transmission readings were taken using a lock-in amplifier while load cell measurements were taken with a voltmeter from a 5 volt, 0.5 amp power supply. Despite the fact that an effective crystal press damping system was developed, size limitations precluded the use of the complete system. For this reason, data points were taken only once per full turn so as to minimize the effect of non uniform load application on the collected data. Good correlation was found in the transmission data between the experimentally determined Er:YAG and the previously known peizo-optic constants of non-doped crystal with which it was compared. The variation which was found between the two could be accounted for by the aforementioned presence of Erbium in the experimental sample (for which exact empirical data was not known). The same test procedure was then carried out on a Yttrium Gallium Aluminum garnet (YGAG) for the purpose of establishing values of its unknown piezo-optic constant tensor using experimentally collected transmission data. Significant variation between the piezo-optic constants of YAG and YGAG crystals was found however, the excellent data correlation of separate experimental runs carried out on the YGAG sample demonstrates the validity of these results. The data collected during the stressing of the YGAG was of high quality, however the amount of data collected was somewhat limited by a fracture of YGAG specimen which undoubted altered the crystalline lattice structure and hence precluded any further testing.

Carty, Atherton A.↗
NASA NTRS1999

Rare Earth Doped High Temperature Ceramic Selective Emitters

As a result of their electron structure, rare earth ions in crystals at high temperature emit radiation in several narrow bands rather than in a continuous blackbody manner. This study develops a spectral emittance model for films of rare earth containing materials. Although there are several possible rare earth doped high temperature materials, this study was confined to rare earth aluminum garnets. Good agreement between experimental and theoretical spectral emittances was found for erbium, thulium and erbium-holmium aluminum garnets. Spectral emittances of these films are sensitive to temperature differences across the film. Emitter efficiency is also a sensitive function of temperature. For thulium aluminum garnet the efficiency is 0.38 at 1700 K but only 0.19 at 1262 K.

Chubb, Donald L.↗
NASA NTRS2008

Monitoring Delamination of Thermal Barrier Coatings by Near-Infrared and Upconversion Luminescence Imaging

Previous work has demonstrated that TBC delamination can be monitored by incorporating a thin luminescent sublayer that produces greatly increased luminescence intensity from delaminated regions of the TBC. Initial efforts utilized visible-wavelength luminescence from either europium or erbium doped sublayers. This approach exhibited good sensitivity to delamination of electron-beam physical-vapor-deposited (EB-PVD) TBCs, but limited sensitivity to delamination of the more highly scattering plasma-sprayed TBCs due to stronger optical scattering and to interference by luminescence from rare-earth impurities. These difficulties have now been overcome by new strategies employing near-infrared (NIR) and upconversion luminescence imaging. NIR luminescence at 1550 nm was produced in an erbium plus ytterbium co-doped yttria-stabilized zirconia (YSZ) luminescent sublayer using 980-nm excitation. Compared to visible-wavelength luminescence, these NIR emission and excitation wavelengths are much more weakly scattered by the TBC and therefore show much improved depth-probing capabilities. In addition, two-photon upconversion luminescence excitation at 980 nm wavelength produces luminescence emission at 562 nm with near-zero fluorescence background and exceptional contrast for delamination indication. The ability to detect TBC delamination produced by Rockwell indentation and by furnace cycling is demonstrated for both EB-PVD and plasma-sprayed TBCs. The relative strengths of the NIR and upconversion luminescence methods for monitoring TBC delamination are discussed.

Eldridge, J. I.↗