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Two optimized methods for accurately measuring the 1.5 µm lifetime of Er[sup 3+] in LiNbO[sub 3] crystals and waveguides are proposed. The first method, suitable for measurement of bulk material, was suggested by forming an annealed proton exchanged sandwich structure and fluorescence was collected through an adjustable aperture. This excitation collection scheme was used to investigate bulk Er-doped LiNbO[sub 3] crystals with eight different Er[sup 3+] doping levels, three different crystal thicknesses, and three different cut orientations. The 1.5 µm lifetime was investigated in three configurations: with both a sandwich and an aperture, with a sandwich but without an aperture, and without not only a sandwich but also without an aperture. In addition, the effect of the aperture was also studied. The second method, suitable for a waveguide structure, was proposed on the basis of transversely gathering the fluorescence aided by an outcoupling fiber. It was optimized by comparing three different fluorescence collection schemes. Using this method, the lifetimes of some Ti: Er:LiNbO[sub 3] strip waveguides were measured. In addition, the effect of radiation trapping on the polarized fluorescence spectrum was also investigated. The experimental results are discussed and summarized. [ABSTRACT FROM AUTHOR]

(The origin of the formation of nanoprecipitates of ErNbO[SUB4] induced by vapor transport equilibration (VTE) in Er:LiNbO[SUB3] crystals was investigated by comparing x-ray powder diffraction patterns of VTE-treated, annealed and as-grown Er:LiNbO[SUB3] crystals. The results indicated that annealing an Er:LiNbO[SUB3] crystal in ambient atmosphere, whether the crystal is x or z cut, and whether it is highly or lower doped, does not influence its crystalline structure, and hence cannot cause the formation of the precipitate. The elevated temperature is not a sufficient requirement for the formation of this additional phase, but is only an essential prerequisite, together with the high-doping level of erbium. The incorporation of a certain amount of additional Li[SUP+] ions accompanying the VTE procedure is considered as the direct reason for the formation of the precipitate. The mechanism of the formation of the precipitates of ErNbO[SUB4] was tentatively suggested from both microscopic and macroscopic points of view. In addition, the origin of VTE-induced cracking, which occurs only in higher-doped x-cut crystals, was also considered based on the experimental results of annealed crystals. The incorporation of a certain amount of additional Li[SUP+] ions by the VTE procedure is again correlated with the cracking. [ABSTRACT FROM AUTHOR]

At room temperature, polarized visible and near infrared emission characteristics of 488 nm pumped vapor transport equilibration (VTE) treated Er:LiNbO[sub 3] crystals were investigated in comparison with the corresponding as-grown ones. The observed characteristics of the VTE crystal, whether it precipitates or not, include the retained polarization dependence, slight shift (less than 5 Å) of peak position, narrowing of some individual emission peaks, the appearance of additional emission peak near 1536.5 nm and the about 10% lengthening of 1.5 µm lifetime. In addition, in the case of lower Er doping level, the spectral shape are well reserved for the VTE crystals and no obvious changes in both visible and IR emission intensity. On the other hand, for those highly doped crystals, the VTE treatment not only results in a definite change of relative intensity between some emission peaks in IR region, but also causes the drop of both visible and IR emission intensity. Combining with the related absorption characteristic allow to conclude that the drop of the emission intensity results from the scattering of the nanocrystalline grains inside these crystals formed by VTE treatment. [ABSTRACT FROM AUTHOR]

The visible and infrared transmission spectra of vapor transport equilibration (VTE) treated Er:LiNbO[sub 3] crystals, which have different doping levels (0.2%, 0.4%, and 2.0% Er per cation site), different cut orientation (X and Z cut) and different VTE duration (80, 120, 150, and 180 h), were recorded at room temperature in the wavelength range of 250-3700 nm. All of 2.0 mol % doped VTE crystals have precipitated whether X cut or Z cut, while the others have not. Their absorption characteristics were summarized and discussed in contrast to those of corresponding as-grown crystals. The OH[sup -] absorption feature of VTE treated Er:LiNbO[sub 3] is found to be different from that of pure VTE LiNbO[sub 3] crystal. The significant reduction of OH[sup -] absorption band implies that the hydrogen content in the VTE crystals has been reduced substantially whether the crystal precipitates or not. The electron transition absorption characteristics of the lower-doped, not precipitated crystals mainly include the higher transmittance, slight shift of peak or band position, slight absorption intensity change, the appearance of some additional peaks or bands, the narrowing of the peak width (full width at half maximum), and the definite blueshift of the optical absorption edge. The spectral changes are associated with the redistribution of Er[sup 3+] spectroscopic sites induced by the VTE procedure. In comparison with those lower-doped VTE crystals, the highly doped VTE crystals display more significant absorption characteristics: the significant enhancement of 1480 nm pumping band and the obvious weakening of 1531 nm peak, the appearance of many additional peaks in the infrared region, and the interesting evolution of the transmittance with the wavelength. These substantial spectral changes are unambiguously conducted with the formation of a precipitate ErNbO[sub 4] induced by the VTE treatment in these crystals. The mechanism for the formation of the precipitate has... [ABSTRACT FROM AUTHOR]

Co-diffusion characteristics of Er3+ and Tm3+ ions in LiNbO3 crystal have been studied, together with two other properties: doping effect on refractive index of substrate, and Li out-diffusion. Er3+/ Tm3+-codoped LiNbO3 single-crystals were prepared by co-diffusion of stacked Er- and Tm-metal thin films, coated onto parts of the surfaces of X- and Z-cut congruent LiNbO3 crystal plates, at different temperatures and different durations in air. After diffusion, the surface refractive indices of the doped and undoped parts were measured by prism coupling technique, and the surface composition was evaluated from the measured indices. The results show that the dopings have negligible effect on the substrate index and the Li out-diffusion depends mainly on the diffusion temperature. The Er3+ and Tm3+ profiles were studied using secondary ion mass spectrometry, and a co-diffusion dynamical model is proposed and verified experimentally. From the measured profiles, the temperature-dependent Er3+/ Tm3+ diffusivity and solubility were obtained together with other relevant parameters, such as diffusion constant, activation energy, solubility constant and heat of solution. The Er3+ and Tm3+ co-diffusion exhibits similar temperature dependent diffusivity, and the dependence is similar to that of single-diffusion. In the co-diffusion case, the total solubility consists of two parts: Er3+ and Tm3+ parts, there is no anisotropy, and the value is equal to that of single-diffusion case, in which both ions have the similar solubility. The Er3+ and Tm3+ parts of solubility change relatively with the initial metal film thicknesses and hence have different temperature dependences. Nevertheless, their sum, i.e., the co-diffusion solubility, remains a constant at a given temperature. [ABSTRACT FROM AUTHOR]

Abstract: Influence of thermal reduction on intrinsic (bipolarons), extrinsic (Er3+) defects and OH− groups in Er:LiNbO3 crystals, which were as-grown and VTE-treated (VTE: vapor transport equilibration) before being reduced, was studied by measuring the polarised or unpolarised optical absorption in visible and near infrared regions. A wide and strong band extending from the optical absorption edge up to the infrared region and peaking around 500nm (∼2.5eV), resulting from the absorption of reduction-induced bipolarons, is observed. Meanwhile, the thermal reduction also induces an additional, relatively much narrow absorption band around 370nm in a crystal whether it is Er-doped or undoped and whether it is congruent or originally VTE-treated. Both the 500nm and the 370nm bands show similar polarisation dependence. The thermal reduction treatment hardly influences Er3+ spectroscopic properties such as absorption amplitude, linewidth, peaking position and polarisation dependence. The original VTE effects on the spectroscopic properties of Er:LiNbO3 crystal are essentially retained still. The thermal reduction has a similar effect on the OH− absorption to a strong VTE treatment: the removal of the OH− groups contained in the crystal. [Copyright &y& Elsevier]

Visible and near infrared absorption and emission (488 nm excitation) characteristics of ErNbO4 powder, which were prepared by calcining the Er2O3 (50 mol%) and Nb2O5 (50 mol%) powder mixture at 1100 and 1600 °C for different durations, have been investigated at room temperature. The absorption and emission characteristics of these calcined ErNbO4 powder were summarized and discussed in comparison with those of Er2O3. Weak emission of Er2O3 relative to the calcined ErNbO4 is mainly conducted with absorption difference at the excitation wavelength 488 nm. The obvious spectral changes from Er2O3 to calcined ErNbO4 samples are related to an elevated-temperature-assisted phase transformation according to the solid-state chemical reaction equation: Er2O3 + Nb2O5 ⇌ 2ErNbO4, which results in the changes of the ion environment of Er3+ and hence changes of the Stark levels of Er3+. The further spectral change as the strengthened calcination results from the improvement of ErNbO4 purity in the calcined mixture. The borders between two green transitions and between two near infrared transitions in the emission spectra of both calcined samples and Er2O3 were tentatively identified by referencing earlier reported emission spectra of the precipitated Z-cut VTE Er(2.0 mol%):LiNbO3 crystal and the match relation between absorption and emission spectra of the ErNbO4 powder. A comparison was performed on the spectra of calcined ErNbO4 powder and those of VTE Er(2.0 mol%):LiNbO3 crystals. The results allow to preliminarily deem the contribution of ErNbO4 precipitates, generated inside these crystals by the VTE procedure, to the spectra of these crystals. [Copyright &y& Elsevier]

Diffusion characteristics of Zr4+ in LiNbO3 single-crystal were studied. Zr4+-doped LiNbO3 crystal plates were prepared by in-diffusion of 100 nm thick ZrO2 film coated onto Z-cut congruent substrates in wet O2 at different temperatures. Zr4+-diffused profile was analyzed by secondary ion mass spectrometry. The results show that the Zr4+ diffusion follows the traditional diffusion theory. From the measured profiles, important diffusion parameters are obtained, such as diffusivity and its temperature dependence, diffusion constant, activation energy, surface concentration, and solubility. The Zr4+ has a diffusivity similar to that of Ti4+, implying that the Zr4+ doping and the Ti4+ diffusion can be performed simultaneously to simplify the fabrication process of a photorefractive-damage-resistant Zr4+-doped Ti-diffused LiNbO3 waveguide. [ABSTRACT FROM AUTHOR]

The influence of Li-rich vapor transport equilibration ( VTE) on surface Li2 O-content of 1-mm-thick, congruent X-, and Z-cut LiNbO3 crystal plates was studied against the VTE temperature. The VTE-induced surface Li2 O-content increase was evaluated from measured birefringence. The results show that the increase follows the traditional Arrhenius law with a surface Li2 O-content alteration constant (614 ± 136)/(91 ± 10) mol% and an activation energy (0.76 ± 0.05)/(0.53 ± 0.03) eV for the X/ Z-cut plate. An empirical expression that correlates the VTE-induced surface Li2 O-content alteration with both the VTE temperature and duration is presented. The expression is useful for producing a near-stoichiometric LiNbO3 plate with the desired surface Li2 O-content via balancing the VTE temperature and duration. [ABSTRACT FROM AUTHOR]

Diffusion-doping is an effective, practical method to improve material properties and widen material application. Here, we demonstrate a new physical phenomenon: diffusion control of an ion by another in LiNbO3 and LiTaO3 crystals. We exemplify Ti4+/Xn+ (Xn+ = Sc3+, Zr4+, Er3+) co-diffusion in the widely studied LiNbO3 and LiTaO3 crystals. Some Ti4+/Xn+-co-doped LiNbO3 and LiTaO3 plates were prepared by co-diffusion of stacked Ti-metal and Er-metal (Sc2O3 or ZrO2) films coated onto LiNbO3 or LiTaO3 substrates. The Ti4+/Xn+-co-diffusion characteristics were studied by secondary ion mass spectrometry. In the Xn+-only diffusion case, the Xn+ diffuses considerably slower than the Ti4+. In the Ti4+/Xn+ co-diffusion case, the faster Ti4+ controls the diffusion of the slower Xn+. The Xn+ diffusivity increases linearly with the initial Ti-metal thickness and the increase depends on the Xn+ species. The phenomenon is ascribed to the generation of additional defects induced by the diffusion of faster Ti4+ ions, which favors and assists the subsequent diffusion of slower Xn+ ion. For the diffusion system studied here, it can be utilized to substantially shorten device fabrication period, improve device performance and produce new materials. [ABSTRACT FROM AUTHOR]

Abstract An error in the previous paper "Electro-optic coefficients r 13 and r 33 of singly Er3+-doped and In3+/Er3+-codoped LiNbO 3 crystals" [J. Phys. Chem. Solids 100 (2017) 101–106] is corrected. The electro-optic coefficients γ 33 and γ 13 that were measured by applying a DC voltage to the crystal via the Al films coated onto the crystal surfaces are the unclamped instead of clamped coefficients. Highlights • An error in previous paper [J. Phys. Chem. Solids 100 (2017) 101] is corrected. • r 13 and r 33 were measured by two voltage-applying schemes, named A and B. • In Scheme B, a DC voltage is applied via Al films on sample surfaces. • r 13 and r 33 measured by Scheme B are unclamped instead of clamped. [ABSTRACT FROM AUTHOR]

Clamped and unclamped electro-optic coefficients γ 13 and γ 33 of In 3+ /Er 3+ -codoped LiNbO 3 crystals, which were grown by Czochralski method from the melts containing 0.5 mol% Er 2 O 3 while varied In 2 O 3 contents of 0.0, 0.5, 1.0 and 1.5 mol%, were measured by Mach-Zehnder interferometry. The results show that In 3+ /Er 3+ codoping does not cause change of γ 13 and γ 33 , and both γ 13 and γ 33 can be regarded as unchanged in the studied In 3+ concentration range of 0–2.6 mol% (in crystal) within the experimental error of 3%. The small doping effect is desired in light of the electro-optic application of the crystal. A qualitative, comprehensible explanation for the small effect is given on the basis of the EO coefficient model of LiNbO 3 and doping effect on the defect structure of LiNbO 3 . [ABSTRACT FROM AUTHOR]

A previous paper [J. Lumin. 177 (2016) 219] has studied Judd-Ofelt spectroscopic properties of Er3+ (0.5 at%)-doped Gd 3 (Al, Ga) 5 O 12 garnet single-crystal, and reported the Judd-Ofelt intensity parameters Ω 2 = 1.47 × 10−20 cm2, Ω 4 = 1.38 × 10−20 cm2 and Ω 6 = 1.19 × 10−20 cm2. We have performed a re-study on the Judd-Ofelt spectroscopic properties of a similar garnet single-crystal Er3+(20 at%)-doped Gd 3 (Al 0.4 Ga 0.6) 5 O 12 , and obtained quite different values of Judd-Ofelt intensity parameters Ω 2 = (0.34 ± 0.11) × 10−20 cm2, Ω 4 = (0.48 ± 0.16) × 10−20 cm2 and Ω 6 = (1.05 ± 0.17) × 10−20 cm2. The quite different Ω t values given by two studies are mainly due to remarkably different absorption characteristics of Er3+ in the crystals employed in two studies, and factors that lead to quite different absorption characteristics are discussed. Another reason is that the hypersensitive transition at 380 nm was excluded from the Judd-Ofelt calculation in that paper, resulting in deviation of their result. Instead, all of the Er3+ absorption bands were included in our calculation, allowing to obtain more accurate Ω t values. Quite different Ω t values lead to considerable differences of relevant spectroscopic parameters, such as radiative rates and lifetimes of typical Er3+ emissions, for which the difference from each other is as much as three times. In addition, visible, near-infrared and mid-infrared fluorescence spectra and lifetimes of Er3+ in the studied crystal were measured, and the emission characteristics are discussed. • Er:Gd 3 (Al,Ga) 5 O 12 crystal was grown and its spectroscopic properties are studied. • Judd-Ofelt analysis was done and the result is compared with previously reported. • The Judd-Ofelt data obtained show large differences from the previously reported. • Main reason is large difference of Er3+ absorption features in two studies. • Sellmeier equation, lattice constant and segregation coefficient are presented. [ABSTRACT FROM AUTHOR]

980-nm-upconverted 530 and 550 nm Er3+ green fluorescence spectra of Er3+/Yb3+-codoped NaGd(WO 4) 2 submicron crystals were measured in the temperature range of 298–383 K. A sextuple ratiometric thermometry is proposed. It is established on the basis of six schemes of fluorescence intensity ratio (FIR) that considers three component peaks of the 530 nm emission band and two component peaks of the 550 nm emission band, which involve electronic transitions between two Stark sublevels of Er3+. The study shows that the phosphor shows strong green fluorescence, which is verified by measured quantum yield, and thermally stable spectral structure desired for the sextuple ratiometric thermometry. All of the six FIR schemes display highly efficient sensing performances with slightly different thermal sensitivities. Each scheme gives a temperature value and the six schemes give an averaged result. In parallel, we have also carried out an ex vivo experimental study on the temperature characteristics of the green fluorescence of the phosphor. Almost same results have been obtained, verifying biological applicability of the phosphor. The ex vivo experimental results also show that the sextuple thermometry increases considerably the accuracy and reliability of temperature measurement in comparison with the conventional intensity integration method. We have demonstrated a sextuple ratiometric thermometry based on six schemes of fluorescence intensity ratio (FIR) that considers three component peaks of 530 nm emission band and two component peaks of 550 nm emission band of Er3+/Yb3+-codoped NaGd(WO 4) 2 (NGW) submicron crystals. Our study shows that the NGW phosphor shows strong fluorescence and thermally stable spectral structure, all of the six FIR schemes display highly efficient sensing performances, and the temperature can be overall determined by the six FIR schemes. Further ex vivo experimental results show that the NGW-dispersed suspension aqueous solution which was hypodermically injection into fresh chicken breast does not affect the spectral structure, strong fluorescence intensity, as well as highly efficient sensing performance, confirming the biological applicability of the NGW phosphor. The ex-vivo experimental results also show that the sextuple ratiometric thermometry considerably increases the accuracy and reliability of temperature detection in comparison with the conventional intensity-integration method. It is concluded that sextuple thermometry is promising for more accurate temperature detection of biological tissue. Unlabelled Image • A sextuple thermometry based on FIR of green emissions of Er3+ is proposed. • It considers electronic transitions between Stark sublevels of Er3+ ion. • Temperature is determined by six FIR schemes with efficient sensing performance. • The sextuple method is more accurate than the usual intensity-integration method. • Ex vivo experiments verify biological applicability of Er3+/Yb3+:NGW phosphor. [ABSTRACT FROM AUTHOR]