大尺寸高浓度掺杂Nd:GGG和Nd:YAG晶体的光谱性质

由于Nd3 离子半径0.112nm和Y3 离子半径0.101nm相差10.9%,使得Nd3 离子非常难于进入YAG晶体中。我们用温度梯度法生长了大尺寸高浓度(2.8 at%)的Nd:YAG晶体,同时与用提拉法Nd:GGG晶体进行了比较。分析了高浓度掺杂Nd:GGG和Nd:YAG晶体浓度猝灭问题。研究了不同浓度掺杂的猝灭效应。在同样的掺杂浓度下,我们发现它们的猝灭程度不同,其原因是两种晶体中ΔE(m is-)m和ΔE(m i s )m不同。     

激光晶体Nd3+:Gd3Ga5O12中的核心和小面生长

Nd3+:Gd3Ga5O12(Nd:GGG)晶体是热容固体激光器的一种重要的工作介质.采用提拉法沿〈111〉方向生长出了Nd:GGG单晶,利用激光器、应力仪和偏光显微镜等仪器和方法,对晶体的小面生长及核心等缺陷进行了观察,分析了小面生长的机理,并提出了消除这些缺陷的办法.通过研究,为改善生长工艺、生长大尺寸优质Nd:GGG晶体提供参考.     

Modification of the crystal structure of gadolinium gallium garnet by helium ion irradiation

The structure of gadolinium gallium garnet (GGG) single crystals before and after implantation by He⁺ ions has been investigated using high-resolution X-ray diffraction methods and the generalized dynamic theory of X-ray scattering. The main types of growth defects in GGG single crystals and radiation-induced defects in the ion-implanted layer have been determined. It is established that the concentration of dislocation loops in the GGG surface layer modified by ion implantation increases and their radius decreases with an increase in the implantation dose.     

5英寸Nd:GGG激光晶体的生长

本文介绍采用提拉法,运用上称重自等径技术(ADC)生长5inch的掺钕钆镓石榴石(Nd:GGG)晶体.通过调整生长工艺参数,优化温场结构,我们成功生长了5inch的Nd:GGG晶体.晶体外观完整,无宏观缺陷,有望作为激光工作物质用于强固体热容激光器中.此外,我们对晶体的外形和生长界面作了讨论.     

An X-ray double-crystal method utilizing non-parallel setting for measuring local lattice mismatches between epitaxial films and substrates

An X-ray topographic method utilizing non-parallel (+,-) setting for measuring lattice mismatches between epitaxial films and substrates is reported. This method gives quantitative as well as topographical information on lattice distortions in a distorted crystal and allows us to study any reflection from various crystals, in which the fractional variation of lattice spacing, δd/d, is of the order of 10^-4?10^-5. Examples of applications are lattice mismatches between epitaxial magnetic garnet films and (111) gadolinium garnet (GGG) substrates. The spacing of the epitaxial film was slightly larger along the [111] direction than that of the substrate and the apparent crystal symmetry of the epitaxial film is rhombohedral.     

Nd(III) and Yb(III) ions incorporated in Y4Al2O9 obtained by sol‐gel method: synthesis,structure, crystals and luminescence

The nanocrystalline powders of Y₄Al₂O₉ (YAM) pure and doped by Nd, Yb and codoped by Nd and Yb were obtained via modified sol‐gel method. These powders were characterized by X‐ray diffraction method, scanning electron microscopy and high resolution scanning electron microscopy, luminescence spectroscopy and differential thermal analysis (DTA). We obtained single phase powders of crystalline structure with average size 70 nm exhibiting interesting luminescent properties. Efficient non‐radiative energy transfer between Nd and Yb was found. DTA confirmed the phase transition at about 1400 °C. From these nanocrystalline powders, the crystals YAM:Yb, YAM:Yb,Nd were grown by micro‐pulling down technique. They were cracking during cooling owing to the phase transition. Luminescent properties of YAM:Nd,Yb crystals were identical with properties of corresponding nanopowders within experimental incertitude. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The effect of crucible bottom deformation on the quality of Nd:GGG crystals grown by Czochralski method

In this paper, we report the growth of neodymium doped Gadolinium Gallium Garnet (Nd: GGG) crystal using Czochralski (CZ) method, and study the effects of crucible bottom deformation and thermal insulator thickness on the growth process and crystal quality. Garnet structure and <111> crystallography orientation of the crystal were confirmed by the X‐Ray diffraction (XRD) analysis. Macroscopic defects, residual stresses, quality, and homogeneity of the crystals were investigated by means of parallel plane polariscope and laser fizeau interferometer respectively and the results compared together. Experimental observations show that the crucible bottom deformation from flat to convex, and decreasing the thickness of zirconia insulator under the crucible result in the formation of lateral cores and increasing the crystal inhomogeneity and tensions, leading to the decrease of the crystal quality. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and properties of Nd:Lu3Ga5O12 laser crystal by floating-zone method

Neodymium (Nd) doped lutetium gallium garnet (Nd:Lu₃Ga₅O₁₂, Nd:LuGG) single crystal was successfully grown by the optical floating-zone method for the first time to our knowledge. Its absorption and luminescence spectra at room temperature were measured. By using the J–O theory, the spectral parameters of Nd:LuGG were calculated, which indicated that Nd:LuGG should possess comparable and even better laser properties than Nd:YAG. The maximum output power of 855 mW at 1062 nm was achieved with slope efficiency of 23.4% under a pump power of 5.2 W, and optical conversion efficiency of 16.4%. All the results show that Nd:LuGG is a potential laser material.     

Optimization of the Growth Technology for Crystals with Garnet Structure Based on X-Ray Diffraction Data

High efficiency of the methods of double-crystal X-ray diffractometry (DCXRD) and topography for improving the growth technology of highly homogeneous crystals has been demonstrated on the example of gadolinium gallium garnet (GGG) single crystals. The main types of structural defects observed in Czochralski-grown GGG crystals are found to be macroscopic inhomogeneity of composition distribution, caused by the facet effect manifestation; microinhomogeneous distribution of impurity and main components of the composition in striations; dislocations; and second-phase inclusions. The relationship between the type and density of newly formed defects and the technological conditions for crystal growth are considered. Optimization of the composition of crystals and their growth technology made it possible to obtain high-quality dislocation-free crystals of GGG and complex-substituted garnets on its basis for magneto-optical and microwave devices, elements of solid-state lasers, and other applications.     

Concentration distribution of Nd3+ In Nd:Gd3Ga5O12 crystals studied by optical absorption method

Nd:Gd₃Ga₅O₁₂ crystals with different concentrations of Nd³⁺ were grown by Czochralski method, their absorption spectra were measured at room temperature. By using the optical absorption method, the effective distribution coefficient k_eff for Nd³⁺ in GGG was fitted to be 0.40±0.01, which is higher than that of Nd³⁺ in YAG. The 808nm absorption cross‐section was calculated to be 4.0±0.2×10^‐20cm^‐2. The lengthways and radial concentration distribution of Nd³⁺ in the crystals were also analyzed and discussed. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of Nd,Yb – yttrium oxide nanopowders obtained by sol‐gel method

Nanopowders of Y₂O₃ pure, doped and codoped by Nd³⁺, Yb³⁺ were obtained by sol‐gel method. Solution with ethylene glycol was choosed as the proper solution where crystallites of powder with Nd and Yb dopants had the same size. Finally the one‐phased compounds of Y₂O₃ doped 0.5 at% Nd and 1, 2 or 4 at% Yb were obtained. Grain growth and their morphology were investigated in various temperature and time of heating. The changes of crystallite sizes and lattice constants in relation to the heating time and temperature for the composition Y₂O₃ doped 0.5 at% Nd and 2 at% Yb are presented. Y₂O₃ containing 0,5 at% of Nd exhibits intense luminescence bands centered at 920 nm, 1100 nm and 1360 nm whereas a single band at about 1020 nm appears in samples co‐doped with neodymium and ytterbium. Luminescence spectra recorded did not depend on the sample preparation procedure and size of grains. OH impurity affects critically the relaxation dynamics of luminescent ion in nanopowders. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and magneto‐optical characteristics of cerium‐doped terbium gallium garnet by the floating zone method

Cerium‐doped terbium gallium garnet single crystal having a large Verdet constant was grown by floating zone (FZ) method, which was suitable for the use in optical devices. The lattice parameters and the X‐ray rocking curve measurement of the crystal was determined by X‐ray diffraction analysis. The Verdet constant of the crystal (B = 0.55 T) at the wavelength of 632.8 nm was −165.8 rad m⁻¹ T⁻¹ at room temperature, 23.7% larger than that of pure TGG (−134.0 rad m⁻¹ T⁻¹). The performance of the high optical quality and excellent magneto‐optical properties of the crystal shows the great potential of using this new method to meet the increasing demand of VI‐NIR Faraday rotators.     

Luminescence characteristics of undoped and Eu‐doped GdCa4O(BO3)3 single crystals and nanopowders

Single crystals of GdCa₄O(BO₃)₃ (GdCOB) pure and doped with Eu concentration of 1 and 4 at% were grown by the Czochralski and micropulling‐down methods. The distribution of Eu ions in GdCOB crystals was uniform. The substitutions of Eu³⁺ in Gd, Ca(1) and Ca(2) cation sites and eventually formation Eu²⁺ have been investigated. The spectroscopic properties of crystals are compared with the properties of nanopowders obtained by sol‐gel method. Radioluminescence spectra of undoped GdCOB crystal show the characteristic emission of Gd³⁺ at about 312 nm, whereas this emission dramatically decreases in Eu‐doped crystals upon X‐ray excitation, as well as in Eu‐doped nanopowders excited in vacuum ultraviolet (VUV) region. The VUV excitation in the range 125‐333 nm for Eu‐doped samples leads to strong emission in red coming from the ⁵D₀ multiplet of Eu³⁺, only. In the photoluminescence decay kinetics of 312 nm emissions substantial shortening and departure for single exponential decay in Eu‐doped samples is clearly observed. Higher Eu doping results in further acceleration of the decay. In undoped GdCOB crystal, the lifetime of the Gd^{3+ 6}P_7/2 multiplet is 2.79 ms. The Eu^{3+ 5}D₀ decay kinetics monitored at 613 nm are rather constant. Numerical fitting of fully exponential curves, reveals lifetimes 2.7 ms for nanopowder and 2.5 ms for single crystal. The results suggest that this material may be used as a red phosphor in plasma display panels in nanopowder form because of strong excitation band of Eu³⁺ luminescence in the 160‐200 nm regions. Contrary to nanopowder sample, such an excitation band, attributed to the Gd³⁺–O^2– charge transfer was not observed in crystal obtained by the micropulling‐down method. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structural,thermal and optical characterizations of a NLO material: L‐alaninium oxalate

An organic electro‐optic and nonlinear optical (NLO) material, L‐alaninium oxalate, was synthesized by the standard method. The synthesized material was purified by repeated recrystallization. Single crystals were grown by the slow evaporation technique. The grown crystals were transparent and had optimum dimensions (20 × 3 × 2 mm³) and were characterized by single crystal XRD, FT‐NMR, FT‐IR, TGA‐DTA and UV‐Vis‐NIR techniques. The second harmonic generation (SHG) from the material was confirmed using Nd:YAG laser. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of Nd:Y3Al5O12 nanocrystals by low temperature glycol route

Y₃Al₅O₁₂, yttrium aluminum garnet (YAG) single crystals are extensively used as host materials for solid‐state lasers. The materials in nano sizes are of immense importance due to their fascinating physical and chemical properties. Nanocrystals of Nd doped YAG were synthesized by low temperature glycol route. This method consists of a mixing of nitrates in an aqueous media at reasonably low temperatures. The Nd doping concentration was optimized and kept at 2 mol%. The prepared material was annealed at different temperatures. Single phase Nd:YAG nanocrystals were obtained at 850 °C. The prepared nanocrystals were characterized by XRD, SEM and TEM techniques for the crystalline phase, crystalline size and structure. The crystalline sizes were obtained in the range of ∼20–30 nm. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth of Nd:GdVO4 Single Crystal and its Laser Output at 1062 nm,1342 nm

A new liquid‐phase method synthesizing Nd:GdVO₄ polycrystalline materials was introduced. High optical quality Nd:GdVO₄ single crystals have been successfully grown by the Czochralski method. The effective segregation coefficients of Nd ion in Nd:GdVO₄ crystal have been measured and discussed. Laser outputs at 1.06 μm and at 1.34 μm were achieved when Nd:GdVO₄ crystal samples of 0.52 at% Nd concentration were pumped by a high‐power LD. A maximum output of 14.5 W at 1.06 μm has been obtained when the pump power is to 26 W, giving the slope efficiency of 63%. It is reported the first time that up to 4.64 W power laser at 1.34 μm has been achieved with optical conversion efficiency of 31.4% and slope efficiency of 32.9%.     

Thermal conductivity and refractive indices of Nd:GdVO4 crystals

The thermal conductivities of Nd:YAG, M(Y,Gd)VO₄ crystals were measured at 298 K. The value of Nd:GdVO₄ crystal along <001> direction was 11.4 W/mK, which was higher than that of YAG crystal measured to be 10.7 W/mK. The principal refractive indices of Nd:GdVO₄ crystal in the temperature range from 20 °C to 170 °C were determined by auto‐collimation method. Based on the measured values of refractive indices, the Sellmeier equation and expression of temperature dependence of refractive indices have been obtained. The measured results show that the birefringence Δn is 0.22007 at 20 °C and temperature coefficient of birefringence is 4.33 × 10⁻⁶/°C for 1.064 μm. These results prove that the GdVO₄ crystal is a laser crystal with excellent thermal and birefringence properties. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and spectroscopic investigation of Yb/Nd co‐doped KLu(WO4)2 laser crystals

Single crystals of Yb, Nd: KLu(WO₄)₂ (Yb, Nd: KLW) of dimensions up to 40mm× 40mm×5mm have been grown by top‐seeded solution growth (TSSG) method. X‐ray powder diffraction pattern was measured and compared with that of Nd: KLuW and Yb: KLuW. Absorption and fluorescence spectra were measured at room temperature. The Judd‐Ofelt theory was applied to analyze the spectrum of Nd, Yb: KLuW crystal. The intensity parameters Ω_t (t=2, 4 and 6) were calculated as Ω₂=20.68×10^‐20cm², Ω₄=11.04×10^‐20cm², Ω₆=6.74×10^‐20cm² respectively, with a root mean square deviation of 0.58×10^‐20 cm². (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

吸收光谱测量晶体折射率的简易方法

折射率是晶体的基本参数,本文提出了利用透过光谱来测量晶体折射率的简易方法,此种方法具有对样品的尺寸要求低、测量范围无限制、操作简单、易获得一定光谱范围晶体折射率的优点.用吸收光谱法和自准直法测量了Nd:GGG的折射率,二者给出的折射率测量结果符合得很好,表明用晶体透射光谱来测量折射率是一种有效的简易测量方法.     

Broad near‐infrared fluorescence properties of Nd‐doped PbClF crystals

Nd‐doped PbClF crystals were grown with modified Bridgman method. Broad and flat emission band at 1.0 μm was observed. The FWHM value of 0.0091 wt.% Nd³⁺‐doped PbClF crystal at 1064 nm reached up to 30 nm with the peak emission cross‐section of 1.05×10^‐19 cm². All the results indicated that Nd‐doped PbClF crystal should be a promising tunable and ultrafast laser material. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)