Magnetic anisotropy of large floating‐zone‐grown single‐crystals of SrRuO3

SrRuO₃ is a highly interesting material due to its anomalous‐metal properties related with ferromagnetism and its relevance as conductive perovskite layer or substrate in heterostructure devices. We have used optical floating zone technique in an infrared image furnace to grow large single crystals of SrRuO₃ with volumes attaining several hundred mm³. Crystals obtained for optimized growth parameters exhibit a high ferromagnetic Curie temperature of 165 K and a low‐temperature magnetization of 1.6 μ_B at a magnetic field of 6 T. The high quality of the crystals is further documented by large residual resistance ratios of 75 and by crystal structure and chemical analyzes. With these crystals the magnetic anisotropy could be determined.     

Floating zone growth and characterization of ruby single crystals

Large, high optical quality single crystals of ruby have been grown successfully by the floating zone method under air atmosphere. The size of the grown crystal is typically 60‐70 mm in length and 7‐8 mm in diameter. The obtained crystals were red and did not have any macroscopic defects such as cracks and inclusions. Grown crystals were characterized by powder X‐ray diffraction (XRD) methods, polarized optical microscopy, scanning electron microscopy (SEM). The absorption and fluorescence spectra were measured at room temperature and the dielectric constant measurements of ruby crystals were also presented. Defects occurring in single crystals of ruby during crystal growth by floating zone method are described, and their correlation with the growth parameters is discussed. The origin and control of these defects in grown crystals were studied and the optimum method was proposed. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Singular ring‐shaped distribution of Nd in NdxY1‐xVO4 crystals grown by floating zone method

A singular ring‐shaped distribution of high Nd concentration was observed in Nd‐doped YVO₄ single crystals grown by the floating zone (FZ) method. The ring‐shaped distribution appeared 500‐1000 μm inside from the rim of the crystals. Results of growth experiments by the anisotropic heating floating zone (AHFZ) method showed that the Nd concentration was high at the high‐temperature side of the grown crystals. We found a small concave projection at a part of the convex solid‐liquid interface by quenching the molten zone during growth. The cause of the singular ring‐shaped distribution of the Nd‐rich area was discussed in relation with the concave projection at the interface and the convection in the molten zone. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of magneto‐optical YFeO3 crystals

The floating zone growth of magneto‐optical crystal YFeO₃ has been investigated. The polycrystalline feed rod was prepared by a pressure of 250MPa and sintering at about 1500°C. A crack‐ free YFeO₃ single crystal has been successfully grown. The crystal preferred to crystallize along <100> direction with about 10° deviation. The X‐ray rocking curve of the crystal has a FWHM of 24 arcsec, confirming the high crystal quality of the sample. The (100) plane was etched by hot phosphoric acid and the dislocation density was about 10⁴/cm². A thin outer layer with Y₂O₃‐rich composition was found at the periphery of as‐grown crystals, which was attributed to the Fe₂O₃ evaporation during growth. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Growth and characterization of superconductive Nd2‐xCexCuO4‐y single crystals

Nd_2‐xCe_xCuO_4‐y single crystals with different x values have been successfully grown by Traveling Solvent Floating Zone method (TSFZ). Electronic properties of Nd_2‐xCe_xCuO_4‐y single crystals with various x have been studied in detail. The results show that superconductivity can be found in crystals with x > 0.1 (0.13‐0.18) directly grown at oxygen‐reduced atmosphere without post‐annealed, while no superconductivity appears in crystals with x < 0.1 at the same atmosphere. It is also found that, the segregation coefficient of Ce is determined to be 0.946 and transition temperature Tc (onset) reaches maximum value of 23.5 K at nominal composition x = 0.165. With further increase of Ce concentration, transition temperature of single crystals declines due to the precipitation of secondary Phases. In addition, the variation of lattice constants of Nd_2‐xCe_xCuO_4‐y single crystals with different x is also given. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Numerical study of influences of buoyancy and solutal Marangoni convection on flow structures in a germanium‐silicon floating zone

This paper presents a numerical study of Marangoni flows in a floating zone of germanium‐silicon crystals, which was performed by using a commercial finite element program FIDAD^TM. The numerical results point out that for fluids with a small Pr number the influence of buoyancy forces cannot be ignored in the numerical model. Furthermore, the competition between the thermocapillary (TC) and solutocapillary (SC) flows in the floating zones was qualitatively examined. If the TC flow is as strong as that in the Si‐rich floating zone, the SC flow may be restricted to the bottom area near the free surface. Otherwise, the SC flow may overcome the TC flow and induce a surface transfer of species. The numerical predictions agree well with the previous experiment results. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Analysis of the dopant segregation effects at the floating zone growth of large silicon crystals

A computer simulation is carried out to study the dopant concentration fields in the molten zone and in the growing crystal for the floating zone (FZ) growth of large (> 100 mm) Si crystals with the needle-eye technique and with feed/crystal rotation. The mathematical model developed in the previous work is used to calculate the shape of the molten zone and the velocity field in the melt. The influence of melt convection on the dopant concentration field is considered. The significance of the rotation scheme of the feed rod and crystal on the dopant distribution is investigated. The calculated dopant concentration directly at the growth interface is used to determine the normalized lateral resistivity distribution in the single crystal. The calculated resistivity distributions are compared with lateral spreading resistivity measurements in the single crystal.     

Floating zone growth of high-quality SrTiO3 single crystals

Strontium titanate single crystals 15–20 mm in diameter and 40–80 mm in length were grown by a floating zone method with radiation heating. Additional crystal heating just below the molten zone by an in-growth annealing furnace was applied in order to lower the temperature gradients and to achieve slower cooling of the grown crystal. The crystal perfection was studied with X-ray topography and double-crystal diffractometry. The most perfect crystals were grown in [0 0 1] direction with single grain rocking curve widths of about 30″ and subgrain misorientations of 1′–3′ over 10×10 mm² areas of the boule cross-section for both (0 0 1)-, (1 1 0)- and (1 1 1)-oriented slices. Such high-quality crystal can be grown reproducibly with starting materials of 4N grade quality.     

Floating zone growth and high-temperature hardness of CrB2 single crystals

Single crystals of CrB₂ were prepared by the floating zone method. The crystal quality was improved by controlling the molten zone composition. The crystals preferentially grew normal to the plane which has the lowest Vickers hardness, similar to the other refractory boride crystals. On the growth plane, the direction of the a-plane, which longitudinally exists along the crystal rod, was controlled without the seed crystal by the position of the lower sintered rod. The anisotropy in the hardness was also consistent with morphology of the crystals prepared by the flux growth. In addition, the hardness measurement was useful for estimating the quality of refractory crystals in the floating zone growth.     

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.     

Growth and dielectric properties of Ta2O5 single crystal by the floating zone method

Large Ta₂O₅ single crystal with high‐dielectric permittivity was successfully grown by floating zone (FZ) method under air atmosphere. The grown crystal that has been obtained was typically about 8 mm in diameter and 90 mm in length. The crystal growth parameters were optimized. The crystal symmetry, characterized by means of X‐ray diffraction (XRD), was found to be tetragonal. The relative permittivity and loss tangent along growth and [001] direction were measured in the temperature range between ‐200 °C and 200 °C, which showed a strong dielectric anisotropy. At a frequency of 1 MHz and 20 °C, the dielectric permittivity along the growth direction and [001] direction are 81.17 and 25.04 respectively. The stabilization of high‐temperature phase can explain the dielectric enhancement.     

Optimization of thermal conditions during crystal growth in a multi‐zone resistance furnace

The thermal condition is one the of most important control parameters for crystal growth. In this paper we present an effective numerical method in detail for optimizing thermal conditions in multi‐zone crystal growth facilities, especially for crystal growth by the float zone (FZ) technique. A furnace function Ω is introduced to integrate the character of a growth furnace into a linear equation system. The desired power distribution can be therefore approached by solving the linear equation system iteratively. An expert systemlike algorithm has been developed in order to obtain a more suitable solution for practical applications. This method was used to investigate thermal parameters for experiments of SiGe/GeSi single crystal growth by the FZ technique. It is an individual program which can be combined with any commercial finite element/finite volume (FE/FV) program such as FIDAP^TM.     

Growth of Ba2Re(Y,Pr)Ru1‐xCuxO single crystals in a high temperature solution drop using an infrared imaging system

Infrared imaging furnace was used to grow single crystals of Ba₂YRu_1‐xCu_xO₆ and Ba₂PrRu_1‐xCu_xO₆ using high temperature solutions of PbO‐PbF₂ in the form of a bubble attached to the feed rods. Several small crystals were found deposited on the cooler portions of the sintered rod as well as in the drop like portion at the end of the rod. These crystals were collected and the morphology, microstructure and magnetic properties were studied. The details of these investigations are presented. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Bridgman growth of langasite‐type piezoelectric crystals

Three langasite family crystals of Sr₃Ga₂Ge₄O₁₄ (SGG), Ca₃NbGa₃Si₂O₁₄ (CNGS), and Sr₃NbGa₃Si₂O₁₄ (SNGS) were successfully grown by the modified Bridgman method. Among them, SGG crystals up to 2 inches were obtained with the multi‐crucible industrial Bridgman furnace; SNGS crystal grown in any orientation direction other than along a‐axis was realized. Commercially availability SGG boules and the advantage in SNGS crystal indicated that the modified Bridgman technique is a prospective method to realize the mass‐production of the langasite‐type crystals. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystallization of silicon thin films by current‐induced joule heating using a tungsten overcoat

A modified crystallization process using current‐induced joule heating under vacuum is presented. A thin layer of high temperature resistant tungsten was sputtered on the amorphous silicon as the conducting and annealing medium. The thin film thickness was measured by α‐stepper. The high current density provided effective means in crystallizing the amorphous silicon layer. The crystalline morphology was studied by scanning electron microscopy (SEM) after Secco‐etch, transmission electron microscopy (TEM), and x‐ray diffraction (XRD), under different annealing conditions. The grain size was controlled in the range of 0.1‐0.5 μm and could be increased with annealing time. No tungsten silicide was found. Some defects were formed due to electron‐migration effect near the electrodes. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Resistivity distribution of silicon single crystals using codoping

Numerous studies including continuous Czochralski method and double crucible technique have been reported on the control of macroscopic axial resistivity distribution in bulk crystal growth. The simple codoping method for improving the productivity of silicon single-crystal growth by controlling axial specific resistivity distribution was proposed by Wang [Jpn. J. Appl. Phys. 43 (2004) 4079]. Wang [J. Crystal Growth 275 (2005) e73] demonstrated using numerical analysis and by experimental results that the axial specific resistivity distribution can be modified in melt growth of silicon crystals and relatively uniform profile is possible by B–P codoping method. In this work, the basic characteristic of 8 in silicon single crystal grown using codoping method is studied and whether proposed method has advantage for the silicon crystal growth is discussed.     

Fluctuation of crystallization at center part of floating molten zone under reduced gravity condition

Fluctuation of crystallization was observed at floating molten zone under reduced gravity condition on airplane. The zone material was Ba(B_0.9Al_0.1)₂O₄. A pair of Pt tubes was used at the upper and the lower positions, and the molten zone was formed between two Pt tubes. Double peak temperature profile could be performed using two Pt tubes. Crystallization of the molten Ba(B_0.9Al_0.1)₂O₄ was started at center part of side surface of floating molten zone under reduced gravity condition. The formed crystal was melted again during the crystallization by the gravity fluctuation at the center part of the floating molten zone. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Evolution of the growth interface in liquid phase diffusion growth of bulk SiGe single crystals

The article presents a study for the evolution of growth interface in crystal growth by Liquid Phase Diffusion (LPD). Specific LPD experiments were designed to grow compositionally graded, germanium‐rich Si_xGe_1‐x single crystals of 25 mm in diameter with various thicknesses. Measured interface shapes show the evolution of the growth interface. Silicon compositions were measured by the Energy Dispersive X‐ray analysis (EDX) in the growth and radial directions. The study shows the feasibility of extracting the desired seeds of uniform composition from LPD grown crystals, for subsequent use in other epitaxial growth processes. © 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim     

Solution growth and comparative characterization of L‐HFB single crystals

Single crystals of L‐histidine tetrafluoroborate (C₆H₁₀N₃O₂BF_{4 ,} L‐HFB) were grown by solution growth method using two different temperature profiles: conventional, in which the growth temperature was kept constant at 30°C and rapid, in which it was increased in steps of 1 K per day while keeping the other growth conditions same. Crystals grew in nearly 30 and 10 days in the two methods, respectively. The crystals were transparent and showing its characteristic morphology. Both types of crystals were characterized by XRD for their structural comparison. Surface morphology and growth features of the crystals were studied by SEM. Features of two dimensional layer growth steps, rectangular etch pits, slip lines and bands, etc. were observed. The presence of various functional groups and their bonding were studied by FTIR in the range 4000‐400 cm^‐1. Thermal stability of the crystals was determined by thermo‐gravimetric and differential thermal analysis. The generation of green light due to second harmonic generation for fundamental λ =1064 nm has been confirmed in both cases. Dielectric constant measurement was carried out in the range 20Hz‐2MHz. In the UV‐Vis studies, high transmittance and a shorter ‘lower cut off' value (232 nm) were observed. The effect of rapid growth on the structural, morphological and optical properties of the crystals were studied and compared to those of crystals grown in conventional way. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Flux growth and characterization of Ti‐ and Ni‐doped forsterite single crystals

Forsterite monocrystals doped with Ti and Ni were grown by the flux growth technique. A suitable mixture of flux (MoO₃, V₂O₅, Li₂CO₃) and nutrient was slowly cooled down to 750 °C from 1250 °C or 1350 °C. The crystals were then characterized by powder and single‐crystal X‐ray diffraction, scanning electron microscopy and differential scanning calorimetry (DSC). Variations observed in crystal size were attributed by both the varying experimental conditions in which they had been obtained, and to the amount of Ni substituted for Mg in the structure. High abundances of doped forsterite required a cooling rate of 1.8 K h^‐1. These synthetic, well‐characterized Ti and Ni doped forsterite crystals may have potential for exploitation in industrial fields. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)