Melt Flow and Species Transport in μg‐Gradient‐Freeze Growth of Germanium

The result of a μg‐experiment on the Gradient‐Freeze growth of Ge:Zn with doping from the vapour phase shows a homogeneous distribution of the zinc in the melt, indicating the dominating role of a gravity‐independent transport mechanism. This effect is investigated numerically on the basis of a global model of the growth setup. The numerical simulation includes the melt flow and the transport of the dopant taking into account buoyant and thermocapillary forces. The results confirm the minor influence of gravity on the species transport. The complete mixing of the melt can be explained by thermocapillary (Marangoni) convection only.     

Synthesis of Zn‐doped talc in hydrothermal atmosphere

Zn‐doped talc were synthesized under hydrothermal conditions at constant reaction time and pressure of 160 hours and 2 kbar respectively, at three different temperatures (300, 500 and 650 °C) with pH‐values of 5 and 7. The starting materials and run products were characterized by X‐ray powder diffraction (XRPD), scanning electron microscopy with annexed energy‐dispersive spectrometry (SEM‐EDS), differential scanning calorimetry thermogravimetric analysis (DSC‐TG) and Fourier transform infrared (FT‐IR). The results showed that the temperature, pH‐value of the reaction mixture and amount of zinc in the starting mixture affected the growth of the Zn‐doped talc. When synthesized at low temperature talc presents low crystallinity, flawed morphology but higher content in zinc in its lattice. A thermal treatment at, or above 500 °C allowed a significant flaw reduction in talc morphology, a higher crystallinity and a lower content in dopant. When large amounts of Zn were present in the starting mixtures, Zn‐doped talc grew small in size and poorly shaped. The effect of Zn doping on some chemical/physical characteristics of the synthesized talc was also discussed.     

Second Harmonic Generation in Zn‐doped Li‐rich LiNbO3 Crystals

6.0 mol. % ZnO doped LiNbO₃ crystals were grown by Czochralski technique. Various Li/Nb mole ratios of 0.942, 0.970, 1.000, and 1.020 were used to prepare the starting materials. Second harmonic generation (SHG) experimental results show that the phase matching temperature increases near linearly with the increasing of Li/Nb ratio, and the SHG efficiency is enhanced by the Zn doping and the increasing of Li/Nb ratio. The intrinsic and extrinsic defects are discussed in this paper to explain the SHG behavior and photo‐damage resistance in the Zn doped Li‐rich LiNbO₃ crystals.     

Contribution to the tin‐rich region of the Sn‐Zn‐Ti system

The tin‐rich region of the system Sn‐Zn‐Ti system has been studied by diffusion couples, differential scanning calorimetry and electron microprobe analyses. Ternary eutectic reaction occurs at 193.7°C near to the binary tin‐zinc eutectic point and titanium content less than 0.9 at.% Ti. Three ternary compounds with approximate formulae: Ti₈Sn₅Zn₂ to Ti₅Sn₃Zn, TiSn₄Zn₅ and Ti₂Sn₄Zn₃ have been observed. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization of Silver — Germanium Alloys under Microgravity II. Primary Crystallization

Results of a study on primary crystallization in hypoeutectic and hypereutectic alloys under different convection conditions during solidification are presented. The conditions of suppressed buoyancy driven convection are assumed in the microgravity samples. The intensity of convection was shown to affect the resulting microstructures significantly. The number and the size of primary dendrites in both hypoeutectic samples was found to be comparable. In the microgravity processed hypoeutectic sample the primary dendrites exhibit a greater tendency to branch compared with the ground-based sample. In eutectic samples, a small amount of primary solid solution, due to the existence of an asymmetric coupled zone, was observed. In hypereutectic samples the number of primary germanium crystals is higher in the space sample. The influence of convection on the nucleation of primary crystals thus depends on the composition of such samples. In the case of the primary solid solution the effect of convection on the growth stage of crystallization appears. On the other hand, in the case of primary germanium the intensity of convection affects mainly the nucleation stage of crystallization. The influence of convection on the growth is only secondary. The reasons for such a difference are based on the transport requirements during the nucleation stage.     

Electroluminescence studies of chemically deposited (Zn‐Cd)S:Cu,F films

Electroluminescence (EL) emission has been observed under AC field excitation in chemically deposited (dipping technique) films of (Zn‐Cd)S:Cu,F using substrates of conducting glass plates. Results of XRD, SEM, absorption spectra, transmission spectra, EL emission spectra, voltage, frequency and temperature dependence and brightness waves of EL brightness are presented and discussed. SEM studies show better growth condition in presence of F. X‐ray diffraction studies show diffraction lines due to CdS and ZnS. Both the studies represent average particle sizes of the order of 1Å. Absorption studies show change in band gap due to increasing concentration of ZnS. The observed EL emission (blue‐green region) may be due to Cu, F combination. Results of transmission spectra give band gap similar to those given by absorption spectra. From voltage dependence of EL brightness acceleration‐collision mechanism is found to be effective. Frequency dependence of EL brightness shows first an increase in brightness in the lower frequency range followed by saturation at higher frequencies. Temperature dependence of EL emission shows a maximum at 40°C. Brightness waves consist of primary and secondary waves, which depend on voltage and frequency of excitation & the ambient temperature. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Dewetted growth of CdTe in microgravity (STS‐95)

Two CdTe crystals had been grown in microgravity during the STS‐95 mission. The growth configuration was dedicated to obtain dewetting of the crystals and to achieve high quality material. Background for the performed experiments was based on the theory of the dewetting and previous experience. The after flight characterization of the crystals has demonstrated existance of the dewetting areas of the crystals and their improved quality regarding the earth grown reference sample. The samples had been characterized by EDAX, Synchrotron X‐ray topography, Photoluminescence and Optical and IR microscopy. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Physical properties of Zn‐ 22 wt.% Al‐ x wt.% Ce melt spun eutectoid alloy

Zn‐ 22 wt.% Al (Zn ‐ 40 Al in atomic%) eutectoid alloys with different Cerium (Ce) contents of 0, 1, 2, and 6 (in wt.%), 0.35, 0.70 and 2.1 (in atomic%) were rapidly solidified by melt spun technique. The effects of high cooling rate and alloying element (Ce) on microstructure of the studied alloys were analyzed by X‐ray diffractometry (XRD), scanning electron microscopy (SEM) and electrical resistance measurements. The results showed that the dendrites as well as grains size were refined by the additions of Ce. The main phases in melt spun alloys were α‐Al and η‐Zn, in addition to intermetallic CeZn₅ and Al₄Ce. Additional metastable intermetallic Al_0.71Zn_0.29 phase has been observed only for melt spun alloy of 6 wt.% Ce content. XRD peaks of melt spun alloys demonstrated a considerable broadening with percentage of Ce due to the grain refinement and lattice distortion. Moreover, increase of Ce content results in a decrease of Al lattice constant which could be related to formation of supersaturated solid solution of Zn and/or Ce in α‐Al. Crystallite size of all phases were in the range of nanometer scale which reflects the role of the high cooling rate and the existence of Ce as alloying element for producing nanocrystalline structure. Resistance measurements of melt spun alloys show that the relative resistance rate for the alloys of higher Ce content relaxed faster to lower value than that of lower Ce content. Electrical resistance and microstructure exhibit strongly Ce content dependence.     

Growth and properties of Ba‐doped KDP crystals

KDP crystals were rapidly grown from solution doped with different Ba²⁺ concentrations. The effects of Ba²⁺ on the growth rate, morphology and quality of KDP crystals were discussed. Significant changes in shapes and volume of the grown crystals have been observed. During the growth process, defect region expands gradually with the increasing Ba²⁺ concentration. Samples were cut from different parts of the as‐grown crystals for investigating the optical quality, including transmission spectrum, scattering centers. Through comparison, it is found that the nonuniform distribution of Ba²⁺ ions causes remarkable difference in optical quality between prismatic and pyramidal sectors. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Three‐dimensional unsteady thermocapillary flow under rotating magnetic field

Under a rotating magnetic filed (RMF), the instability of thermocapillary flow and its evolution with increasing Marangoni number (Ma) for semiconductor melt (Pr = 0.01) in a floating liquid bridge model (As = 1) are investigated numerically. Under 5 mT RMF, the thermocapillary flow is steady and axisymmetric with Ma < Ma_c, and the critical Marangoni number Ma_c for convection instability is 29.5, which is obtained by the direct numerical simulation. When the Ma is a little bit beyond the Ma_c, the thermocapillary flow loses stability to become a three‐dimensional rotating oscillatory convection, and a periodic oscillation is confirmed by the fast Fourier transform analysis, the oscillatory main frequency decays with increasing Ma. Under 1 mT–6 mT RMF, the Ma_c increases roughly with the magnetic strength except the Ma_c at 4 mT, where the corresponding change of flow mode after the instability is observed. The oscillatory convection occurs with a smaller Ma in the RMF than that without magnetic field. In addition, no instability toward a three‐dimensional steady convection, which is the state of thermocapillary flow without magnetic field after the first instability, is observed under the RMF.     

Growth and characterization of L‐alanine doped KDP crystals

Potassium Dihydrogen Phosphate (KDP) is an excellent inorganic nonlinear optical (NLO) material with different device applications. Most of amino acids possess NLO property; therefore, it is of interest to dope them in KDP crystals. In the present study, amino acid L‐alanine doped KDP crystals were grown by slow aqueous solvent evaporation technique. The doping of L‐alanine was confirmed by the paper chromatography, the CHN analysis and the FT‐IR spectroscopy. The powder XRD was carried out to assess the single phase nature of the samples. The effect of doping on thermal stability of the crystals was studied by TGA and the kinetic and thermodynamic parameters of dehydration were evaluated. As the amount of doping increased the thermal stability of crystals decreased. However, the second harmonic generation (SHG) efficiency and the UV‐Vis spectroscopy studies indicated that as the L‐alanine doping increased the SHG efficiency and optical transmission percentage increased. The dielectric behavior of the samples has been studied. The variation of dielectric constant, dielectric loss (tanδ), a.c.resistivity and a.c.conductivity with frequency of applied field in the range from 100 Hz to 100 kHz was studied. The dielectric constant and dielectric loss decreased with increase the value of frequency of applied field. The dielectric constant and the dielectric loss values of L‐alanine doped KDP crystals were lower than the pure KDP crystals. The results are discussed. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

On the morphology of <100>-textured Germanium Crystallites in Zn—Ge Eutectic Alloy

Different geometry parameters for the cross-like germanium crystallites (eutectic dendrites) of the Zn-Ge eutectic alloys unidirectionally solidified have been related to the growth rate R and liquid temperature gradient G using linear regression analysis. It has been found that for eutectic dendrite spacing λ, balk length d and balk thickness b follow the relationship of the type w = C_wR^−rwG^−gw; C_w is a constant. The spacing relationship of eutectic dendrites (r_λ = 0.21; g_λ = 0.48) shows a similarity with published experimental and theoretical results on primary dendrite arm spacing (r_λ = 0.25; g_λ = 0.5). It has been shown in terms of a profile ration λ/d that for geometrical similar morphologies the relationship λ²R = const. is valid.     

Work‐hardening characteristics of Zn‐Ti alloy single crystals

Shear stress – shear strain curves of 0.14 at.%Ti alloyed Zn single crystals were measured in compression at different temperatures and shear strain rates. The work‐hardening coefficient for basal slip increases with decreasing temperature and increasing shear strain rate. The work‐hardening characteristics are compared with those reported for Zn single crystals with different constituents and purities. It is discussed with respect to the interaction of dislocations with dislocations, vacancies, vacancy agglomerates and solute atoms. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Long-term Crystal Growth under Microgravity during the EURECA-1 Mission (I) THM Growth of AlxGa1−xSb

Long-term crystal growth experiments were successfully performed under microgravity conditions during the first flight of the unmanned mission EURECA-1 in the automatic mirror furnace (AMF). Two crystals of Al_xGa_1−xSb with [001] and [111] orientation respectively were grown from gallium solution by the travelling heater method. The grown length of the single crystals is 4.0 mm and 4.2 mm respectively. The space-grown samples show a high microscopic homogeneity which indicates the absence of time dependent convection. From pulse markers a constant growth rate of 0.6 ± 0.1 μm/min is measured which is lower than 0.8 ± 0.1 μm/min obtained in earth grown reference samples. Details about the experiment performance and the growth results are given.     

微重力下静态磁场对浮区法硅单晶生长的影响

考虑晶体生长界面的变形,利用有限体积方法对侧面加热的空间全浮区法硅单晶生长中熔区内的热质传输、流场及晶体生长界面位置和形态特征进行了数值研究.应用不同中等强度的轴向磁场和勾型磁场对硅熔体内的热毛细对流进行抑制.分析了静态磁场不同强度下熔区中的对流模式,研究表明,轴向和勾型磁场均能有效抑制熔体内的对流,并将热毛细对流挤压到自由表面附近.轴向磁场可有效抑制熔体的径向流动,但难以有效抑制轴向对流;勾型磁场则可以达到更好的控制熔体对流的效果.对不同强度下的固液面形态及位置分析发现:轴向磁场下固液面基本和无磁场时的重合,但磁场强度较小时固液面在自由表面边缘处向单晶侧有个凸起;勾型磁场作用下的固液面比较平滑,其中心区域较无磁场时整体向z轴正向偏移.研究结果可对浮区法晶体生长中获得高质量晶体提供帮助.     

Growth and characterization of Mn2+ doped calcium l‐tartrate crystals

Single crystals of Mn²⁺ doped calcium levo‐ tartrate tetrahydrate (CLTT) were grown by single diffusion gel growth technique in silica hydro‐gel media. The doping of Mn²⁺ was varied by mixing 0.001M, 0.005M, 0.01M, 0.05M, and 0.1M solutions of MnCl₂ with 1M CaCl₂ solution in equal volumes in the supernatant solutions. The actual amount of Mn²⁺ doping in CLTT crystals was estimated by ICP (Inductively Coupled Plasma) technique. The powder XRD of the samples suggested no significant change in the unit cell dimensions and the presence of any extra phase. The FT‐IR spectra indicated the presence of water molecule, O‐H bond, C‐O bond and carbonyl C=O bond. The EPR spectra confirmed the presence of Mn²⁺ ions in the crystals. The variation of the dielectric constant with temperature confirmed the earlier results of pure calcium tartrate crystals and indicated the ferroelectric nature of the doped crystals. As the amount of doping of Mn²⁺ increased the value of dielectric constant increased. The results are discussed. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Long-term Crystal Growth under Microgravity during the EURECA-1 Mission (II) THM Growth of Sulphur-doped InP

Long-term crystal growth experiments were successfully performed under microgravity conditions during the first flight of the unmanned EURECA-1 mission in the automatic mirror furnace (AMF). Two crystals of sulphur-doped InP with [001] and [111] orientation respectively were grown from indium solution by the travelling heater method (THM). The absence of time dependent buoyancy-driven convection is documented by the lack of type I striations in the space-grown crystals. The sulphur concentration is measured by spatially resolved photoluminescence. As expected, the macrosegregation can be described by a pure diffusion-controlled model which is in good agreement with the findings from the first German spacelab mission D1. Compared to the earth-grown reference samples, both of the space-grown InP crystals show strong disturbances such as inclusions and type II striations. The morphological instabilities are similar to growth disturbances already known from the space-grown MD-ELI-01 from the D1 mission.     

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.     

锗晶体放电切割中钝化物形成机理及防范方法

在利用电火花线切割(WEDM)加工锗晶体时,会出现回路放电电流逐渐减少,并伴随着进电材料与锗晶体间有钝化物的生成,最终导致放电切割无法延续.本实验对放电切割状态进行了实验模拟并生成了钝化物,运用XRD技术对钝化物进行了分析,提出了一种防范钝化物产生的方法,最后采用这种方法利用改进的线切割机床对N型锗进行了放电切割,高效稳定地加工出了工件,从而验证了这种防钝化物产生方法的可行性,为进一步提高锗晶体的放电加工工艺指标奠定了基础.     

Growth,structure and optical characterization of Al‐doped ZnO nanoparticle thin films

Al‐doped ZnO nanoparticle thin films were prepared on glass substrate at the optimum temperature of (410±10) °C by spray pyrolysis technique using zinc nitrate as a precursor solution and aluminium chloride as a dopant. The dopant concentration (Al/Zn at%) was varied from 0 to 2 at%. Structural analysis of the films shows that all the films are of polycrystalline zinc oxide in nature, possessing hexagonal wurtzite structure. The films exhibit variation in peak intensities corresponding to (100), (002) and (101) reflection planes on Al‐doping. The crystallite size calculated by Scherrer formula has been found to be in the range of 35‐65 nm. The optical absorption study shows that the optical band gap in the Al‐doped films varies in the range of 3.11 – 3.22 eV. The width of localized states in the band gap estimated by the Urbach tail analysis has been found to be minimum in case of the 1 at% Al‐doped zinc oxide thin film. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)