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Diffusivity of Er3+ into LiNbO3 crystal has been studied as a function of Li2O content and crystal orientation. The Li2O content in single-crystal LiNbO3 plates was adjusted by Li-rich vapor transport equilibration (VTE) technique. Five X-cut and five Z-cut congruent substrates were VTE treated at first at 1100 °C for different durations ranging from 6 to 74 h, and then were subjected to a special post-VTE anneal procedure at the same temperature for 60 h to obtain homogeneous Li2O content. The Li2O content was determined from the measured fundamental optical absorption edge. Its homogeneity is verified by measuring the optical absorption edge as a function of the crystal thickness. After the composition characterization, the substrates were coated with 45 nm thick Er film and annealed at 1130 °C for 40 h in argon atmosphere. The Er3+ profile was analyzed by secondary ion mass spectrometry. The results show that the Er3+ diffusivity decreases monoexponentially with the increase in the Li2O content in both cases of X- and Z-cut. As the Li2O content is increased from the congruent point (48.4 mol %) to the near-stoichiometric composition (∼49.9 mol %), the diffusivity decreases from 0.107 (0.072) to 0.017 (0.018) μm2/h for the Z (X)-cut substrate. The diffusion shows considerable anisotropy for the lower Li2O content and the diffusivity in a Z-cut substrate is larger. The anisotropy weakens gradually with the increase in the Li2O content, and the diffusivities in the X- and Z-cut substrates ultimately tend to a same value (∼0.02 μm2/h) at the Li-rich phase boundary. After the Er diffusion procedure, endface coupling experiment was carried out to check if a planar waveguide layer was formed near the Er-diffused surface due to the Li outdiffusion. The results show that the Li outdiffusion did not accompany the Er diffusion procedure. [ABSTRACT FROM AUTHOR]

The thermal diffusion of Er3+ into X- and Z-cut congruent LiNbO3 crystal in Li-enriched atmosphere [i.e., vapor transport equilibration (VTE)], created by Li3NbO4–LiNbO3 two-phase powder at the temperature around 1130 °C, was attempted. Single-crystal x-ray diffraction, micro-Raman, photoluminescence spectroscopy, and secondary ion mass spectrometry (SIMS) were used to study the crystalline phase with respect to Er3+ ion and the Er3+ diffusivity. The results show that the thickness of the Er film coated should not be thicker than 10 nm for an X-cut plate and 15 nm for a Z-cut plate. In this case, the diffusion is complete if the duration is long enough (>150 h) and the Er3+ ions in the diffused layer still retain the LiNbO3 phase. On the other hand, if the initial thickness of the Er metal film is thicker than 10 nm for the X-cut plate and 15 nm for the Z-cut plate, the diffusion will be incomplete no matter how long the duration is. This is because the residual Er3+ ions form irremovable ErNbO4 grains on the surface of the crystal. SIMS analysis on an X-cut VTE (1130 °C/192 h) and a Z-cut VTE (1129 °C/158 h) crystal coated, respectively, with 10 and 15 nm thick Er film reveals that the Er diffusion shows obvious anisotropy with the mean diffusion coefficients of 0.0155 and 0.0957 μm2/h, respectively. The surface concentrations are 1.5×1020 and 1.0×1020 at./cm3, respectively. The diffused Er3+ ions follow the stretched-exponential decay profile with a stretching factor of 1.85 and 3.5, respectively. The Li/Nb ratio in the Er-diffused layer is similar to 99.4% for the X-cut sample coated with 10 nm thick Er film and 99.3% for the Z-cut crystal coated with 15 nm thick Er film. The rms roughness of the diffused surface is better than 6 and 4 nm for the X-cut and Z-cut samples, respectively. [ABSTRACT FROM AUTHOR]

Standard thermal diffusion of Er3+ into X-cut congruent LiNbO3 crystal with the MgO doping level close to the antiphotorefractive threshold concentration, 4.5 mol%, was attempted at the temperature close to Curie point of the crystal. Single-crystal x-ray diffraction, photoluminescence spectroscopy and secondary ion mass spectrometry (SIMS) were used to study the crystalline phase with respect to Er3+ ions and the depth profile of the diffused Er3+ ions. The results show that the thickness of the Er metal film coating should not be thicker than 4.6 nm. In this case, the diffusion is complete, the diffused surface is clean, and the Er3+ ions in the diffused layer still retain the LiNbO3 phase. On the other hand, the diffusion will be incomplete if the initial thickness of the Er metal film is thicker than 4.6 nm. The residual Er3+ ions form ErNbO4 grains on the surface of the crystal. SIMS analysis shows that the diffused Er3+ ions follow a monoexponential decay profile. The experimental results also show that the diffusivity of Er3+ in the X-cut congruent Mg(4.5 mol %):LiNbO3 is similar to 4.69×10-3 μm2/h at 1130 °C. Further vapor transport equilibration treatment following the standard diffusion procedure results in transformation of the diffused Er3+ ions from LiNbO3 into the ErNbO4 phase and, hence, substantial spectral change of the 1.5 μm emission. [ABSTRACT FROM AUTHOR]

Congruent LiNbO3 crystals doped with 5.5/1, 6/0.15, and 7/0.8 mol %/mol % of Zn/Er were thermally treated at 1120 °C over 101 h using vapor transport equilibration (VTE) technique. Unpolarized visible and infrared absorption spectra of the VTE-treated and corresponding as-grown crystals were recorded at room temperature. It is shown that VTE treatment has brought these crystals closer to stoichiometric composition. X-ray powder diffraction and optical absorption results show that the VTE treatment induces the crystalline phase transformation with respect to Er3+ from the original Er3+:LiNbO3 to the ErNbO4 in all crystals studied. The formation of the ErNbO4 phase results in substantial absorption changes that include the drop of the transparency in the visible region, the reduction of Er3+ absorption, and the Zn-doping-level-dependent changes in spectral shape and peaking position at 0.98 and 1.5 μm regions. Based upon the measured absorption spectra, the influences of Zn-doping level and VTE treatment on the Er3+ spectroscopic properties were studied by using the Judd-Ofelt (JO) theory. The results show that the VTE treatment has a little effect on the fluorescence branch ratio, while a large effect on the JO parameters, oscillator strength, and electron transition probability. The Zn doping level affects the JO parameters, oscillator strength, and transition probabilities of some individual manifolds. In addition, the VTE treatment leads to the increases of the theoretical radiative lifetimes of almost all manifolds considered. For the emission at 1.5 μm, the lifetime increase is as much as 30% and the theoretical results are in well agreement with the experimental data. The VTE-induced lifetime increase is qualitatively explained. [ABSTRACT FROM AUTHOR]

A model is proposed for describing two-dimensional diffusion of Ti into an initially congruent LiNbO3 crystal under a Li-enriched atmosphere created by a mixed two-phase (Li3NbO4 and LiNbO3) powder at elevated temperature [vapor transport equilibration (VTE)]. The influence of VTE treatment on Ti diffusivity is considered in the model. To solve the model, four key input parameters including Li-concentration-dependent Li and Ti diffusivities and two switching times t1 and t2 were determined. Prior to solve the Ti-diffusion model, a one-dimensional VTE model is solved at first to obtain the dynamic Li2O concentration depth profile. Both the Li-diffusion and Ti-diffusion models were solved by using finite difference method. Based on secondary-ion-mass spectrometry analysis, the validity of the VTE and Ti-diffusion models as well as the numerical method employed are confirmed. After that, diffusion at 1100 °C of an 8-μm-wide, 100-nm-thick Ti strip defined on the surface of a Z-cut or an X-cut substrate was simulated for the VTE duration up to 130 h. Based on the numerical results, the Ti-(Li-)diffusion characteristics are discussed in the aspects of (1) the relation of depth and width profile function of Ti concentration to the VTE duration, (2) the substrate cut effect on both the Ti and Li diffusions, (3) the relation of the 1/e Ti-concentration depth and half-width to the VTE duration, and (4) the VTE duration dependence of the mean [Li]/[Nb] ratio within the Ti-diffused layer. [ABSTRACT FROM AUTHOR]

A previous paper [D. K. Sardar et al., J. Appl. Phys. 93(5), 2602 (2003)] has reported Judd–Ofelt (J–O) spectroscopic properties of Er3+ in garnets Y3Al5O12, Y3(Sc2Ga3)O12, and Gd3Ga5O12. In that paper, the possible magnetic-dipole contribution to the oscillator strength, which is non-zero for the 4I13/2 ↔ 4I15/2 (1.5 μm) transition of Er3+, has been erroneously omitted in their J–O calculation, resulting in incorrect results of relevant spectroscopic parameters. In this Comment, we point out the error, perform correct J–O analysis, and report correct results. [ABSTRACT FROM AUTHOR]

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]

Refractive index of optical material of powder is measured not as easily as a bulk material. Here, the prism coupling technique in combination with the immersion method is proposed to measure the refractive index of an optical material of powder. First, the powder material to be measured was dispersed in α-bromonaphthalene (C10H7Br) liquid to form a suspension mixture. The refractive index of the mixture, together with that of pure C10H7Br, was then measured at the wavelengths of 632.8, 1311, and 1553 nm using a commercial prism coupler. From the measured index values of pure C10H7Br and powder-dispersed mixture, the refractive index of the powder material was obtained on the basis of the Maxwell-Garnett model. Microcrystal powder from a LiNbO3 single-crystal, which has the known refractive index values, has been exemplified to demonstrate the method. The results show that the method is feasible with an accuracy of ±0.05. [ABSTRACT FROM AUTHOR]

A letter to the editor is presented in response to the article "Demonstration of net gain at 1550nm in an erbium-doped polymer mode rib waveguide" that was published in a 2006 issue.

Near-stoichiometric planar and strip LiNbO3 optical waveguides were demonstrated using vapor transport equilibrium process and co-diffusion of titanium metal. Optical confinement is better in z-cut substrates than in x-cut substrates, and the waveguides were characterized optically. Spectral measurements, such as OH- absorption, optical absorption near the fundamental edge, and Raman scattering, were carried out to examine the Li-composition and crystalline phase inside and outside the guiding layer. The results have shown that the vapor transport equilibration process has brought these waveguides toward stoichiometric composition, the Li content inside and outside the waveguide layer is essentially identical, and the LiNbO3 phase is still retained within the waveguide layer. [ABSTRACT FROM AUTHOR]

A number of Li-deficient MgO-doped LiNbO 3 (LN) crystals with different Li 2 O contents ranging from 43.4 mol. % to 44.5 mol. % were prepared by carrying out the Li-poor vapor transport equilibration treatment on 5 mol. % (in growth melt) MgO-doped LN crystals. Unclamped electro-optic (EO) coefficients γ 13 and γ 33 of these crystals were measured by Mach-Zehnder interferometry. The results show that γ 13 (γ 33 ) increases linearly by ∼14% (11%) as the Li 2 O content decreases from 44.5 mol. % of the as-grown state to 43.4 mol. % of the Li-deficient state. This feature is desired for the EO application of the Li-deficient MgO:LN crystal.