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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]