Effect of AlN doping on the growth morphology of SiC

AlN doped SiC films were deposited on on‐axis Si‐face 4H‐SiC (0001) substrates by the physical vapor transport (PVT) method. Thick film in the range of 20 μm range was grown and morphology was characterized. Films were grown by physical vapor deposition (PVD) in a vertical geometry in the nitrogen atmosphere. We observed that nucleation occurred in the form of discs and growth occurred in hexagonal geometry. The X‐ray studies showed (001) orientation and full width of half maxima (FWHM) was less than 0.1° indicating good crystallinity. We also observed that film deposited on the carbon crucible had long needles with anisotropic growth very similar to that of pure AlN. Some of the needles grew up to sizes of 200 μm in length and 40 to 50 μm in width. It is clear that annealing of SiC‐AlN powder or high temperature physical vapor deposition produces similar crystal structure for producing AlN‐SiC solid solution. SEM studies indicated that facetted hexagons grew on the top of each other and coarsened and merged to form cm size grains on the substrate. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

An electron microscopy study of the crystal growth of schwertmannite needles through oriented aggregation of goethite nanocrystals

The formation of the iron oxyhydroxide schwertmannite has been monitored by time-resolved transmission electron microscopy (TEM) studies. Schwertmannite aggregates are found to form initially as spherical agglomerates of ferrihydrite crystallites, which then begin to grow characteristic needles on their surfaces. High-resolution images of the needles show that they are initially comprised of aligned goethite nanocrystals, which subsequently coarsen to form crystallographically coherent needles of goethite. Thus, needle formation on schwertmannite aggregates can be considered as the first stage in the phase transformation from schwertmannite to goethite. The results of this study suggest that schwertmannite is not a distinct mineral phase, but may be a mixture of ferrihydrite and poorly crystalline goethite with a distinctive morphology directed by the presence of surface-adsorbed sulfate anions.     

The influence of substrate temperature on the growth of sexiphenyl on mica(001)

Sexiphenyl thin films were grown by Hot Wall Epitaxy on air‐cleaved mica (001) surfaces at substrate temperatures between 293 K and 440 K. For the entire temperature range, organic thin films show nano‐needle like morphology. The nano‐needles grown at low substrate temperature (293 K) are shortest, and their growth is accompanied by a simultaneous formation of flat islands which disturbs the growth of nano‐needles. On the contrary, unusually long nano‐needles with typical lengths up to the mm range evolve during the growth at a substrate temperature close to the material's thermal desorption temperature at about 440 K. X‐ray diffraction reveals two different crystalline orientations for nano‐needles in the entire temperature range. At low substrate temperatures dominantly the (11 ) plane of the β‐phase is formed parallel to the mica (001) surface. At elevated temperatures another strong texture becomes dominant which is close to the (11 ) crystal orientation. In contrast to this, crystallites with the preferred orientation (001) parallel to the surface of the substrate are formed at low substrate temperature (293 K). This crystal orientation can be associated with flat islands observed in the early growth stage. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal Growth of some Urinary Stone Constituents: I. In‐Vitro Crystallization of L‐Tyrosine and its Characterization

L ‐Tyrosine (C₉H₁₁NO₃), having morphology of spherulitic needles and long needles, an amino acid constituent of urinary stone, is crystallized in silica gel under suitable pH conditions and by single diffusion and double diffusion methods. The grown crystals were characterized by density measurement, Fourier transform infrared spectroscopy, X‐ray powder diffraction and thermogravimetric analysis.     

Transmission Electron Microscope Study of Secondary Phases in Cr3+:LiCaAlF6 Single Crystals

Cr³⁺-doped LiCaAlF₆ single crystals, considered as promising laser materials, contain secondary phases of different sizes and shapes which can be observed as "needles" or "dust" by light microscopy. TEM investigations presented in this paper give evidence for precipitation as the reason for the so-called microscopic "dust". The elongated shape of the so-called "needles" seems to be a consequence of the microscopic growth of facets which become visible by the decoration of the facet boundaries with microscopic precipitates.     

VLS Growth of ITO Whiskers Prepared by the Electron Shower Method

Indium tin oxide (ITO) whiskers were grown by VLS (vapour-liquid-solid) mechanism, using the electron shower method. The whiskers were grown above 200 °C, and the deposition rate was above 0.6 nm/s. The electron shower controlled the size of the whiskers, and the size was 30 nm in diameter and 600 nm in length. The whiskers grew along the substrate at t < 300 s, but grew in a direction perpendicular to the substrate at t > 300 s. When the ITO whiskers grown along the substrate were used as NO₂ gas sensor, the sensitivity was 340, and about 300 times higher than those of the whiskers grown in a direction perpendicular to the substrate and plate-like ITO crystallites.     

Growth of Large Needles and Single Crystals of PbCl2 and PbBr2 in Silica Gel. An Improvement of the New Gel Technique

In growing crystals by the new gel technique a principal difficulty may arise in that it may be difficult or at times impossible to choose two nutrients that may react to produce the desired crystals. With some crystals, the pair of nutrients that may appear practically most suitable, may not react at all or the rate of reaction may be exceedingly small. Further work on the new gel technique has now led to an improvement of the technique by which it is feasible to impart activity to nutrients which are normally non-reactive or to enhance the reactivity of generally less reactive nutrients. Large needles of PbCl₂ and PbBr₂ have been grown in silica gel by this improvement of the new gel technique. The interesting phenomenon of transformation of needles of PbCl₂ and PbBr₂ into single crystals has been investigate and the various aspects of growth systematically studied.     

Rapid crystal growth without inherent supersaturation induced by nanoscale fluid flows?

Crystal growth is a process that only takes place under non‐equilibrium conditions and a necessary prerequisite is that the crystal is exposed to a phase that is supersaturated in the material the crystal is composed of, be it a solution, a vapour or a supercooled melt. In industrial mass crystallization the growth rate for a population of crystals (in suspension growth processes [1]) rarely exceeds mean linear velocities of 10^‐7 ms^‐1. Here we present a mass crystallization process which is accompanied by rapid crystal growth several orders of magnitude faster and into a region of solution that is without inherent supersaturation. The material investigated is a solid hydrate that exhibits a solution mediated phase transition to its anhydrous form in the presence of methanol [2]. The phase transition is initiated simply by placing an amount of hydrate crystals into the solvent and is characterized by the rapid emergence of needle‐shaped crystals. The needles emanate from the crystal faces of the hydrate crystals and grow into the solution, which is nominally free of the substance to be crystallized. The high growth rate of the crystals, which of the order of up to 10^‐4 ms^‐1 is surprising. Although rapid needle growth has been observed before [3‐9], to date a satisfactory explanation for needles growing under the abovementioned conditions is still outstanding. Based upon the topology of the crystals we propose a tentative mechanism for this phenomenon capable of explaining the unusually rapid growth and highlight those questions that need addressing in order to verify this mechanism. X‐ray powder diffraction is used to characterize the crystal phase of the needles; confocal fluorescence microscopy reveals that the needles are hollow. The width of these needles is between 0.5 and 5 μm, their length appears to be limited only by the amount of hydrate available for their formation. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The melt growth of semicircular crystals of the pure Pb and its dilute alloys

Semicircular crystals of Pb were grown from the melt by a rotational operation so as to change the orientation of the solid-liquid interface during crystallization. In pure Pb, specimens grew as polycrystals with grain boundaries developed transversely to the growth direction. According to the decrease in purity, the grown crystals consisted of several long grains along the circular arc. A competitive growth between grains was inhibited by a small amount of impurity and then the mode of growth approached to the complete adhesive one.     

Bulk growth of gallium nitride: challenges and difficulties

The present status of the GaN bulk growth by High Pressure Solution (HPS) method and combination of HPS and Hydride Vapor Phase Epitaxy (HVPE) methods is reviewed. Up to now the spontaneous high pressure solution growth of GaN results in crystals having habit of hexagonal platelets of surface area of 3 cm² or needles with length up to 1 cm. Recently, the platelets and needles have been used as seeds for the HVPE growth. On the other hand, the LPE technique under pressure with pressure‐grown GaN (hp‐GaN), GaN/sapphire template, patterned GaN/sapphire template and free standing HVPE GaN as seeds has been examined and developed. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Microhardness studies of GaTe whiskers

Single crystal whiskers of gallium telluride (GaTe) have been grown by the physical vapour deposition (PVD) method. Microindentation studies were carried out on the prism faces of the needles to understand their mechanical behaviour. The variation in the microhardnessof GaTe crystals with applied load has been determined at room temperature using Vickers microhardness indenter. The work‐ hardening exponent has also been computed for different load regions. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Zur Lamellenstruktur von Silizium-Kristallnadeln

Observations are reported on the lamellar structure of silicon needles with different forms of cross-section.     

Growth and characterization of mercurous chloride single crystals

Mercurous chloride was purified by repeated sublimation using multichamber distillation column. Single crystals were grown by Physical Vapour Transport technique. During the process of purification of the material, very interesting habit modifications like dendrites and needles were observed. Vickers hardness tests were carried out on the (110) plane of the crystal for different orientations of the indentor. The shape of the impressions for different orientations of the indentor reveals the non-cubic structure of the plane. No structural phase transition in mercurous chloride was observed in calorimetry and optical studies.     

Crystallization of an organic intercalation compound: cholic acid

Crystals of cholic acid have been grown in silica and tetramethoxy silane gels. Crystals grew with different morphology and Leisegang rings were also seen in some cases. Crystals were analyzed by X-ray, IR and microhardness studies. The grown crystals were found to be monohydrate and the hardness of the crystals were found to decrease with increase of load.     

Growth and characterization of L‐phenylalanine

L‐Phenylalanine (C₉H₁₁NO₂), having the morphology of spherulitic needles, an amino acid constituent, responsible for brain nutrition is crystallized in silica gel of pH 6.0 by single diffusion method in a period of 30 minutes. The grown crystals were characterized by X‐ray powder diffraction, Fourier Transform infrared spectroscopy and Visible Ultraviolet spectroscopy. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Preparation of nickel oxide– and nickel–silica nanocomposites by spray pyrolysis

Nickel oxide–silica and nickel–silica nanocomposites were prepared by spray pyrolysis of aqueous sols of silica nanoparticles containing nickel nitrate hexahydrate, without and with ethanol, respectively. During pyrolysis, the silica nanoparticles were restructured, losing their identities, while the nickel oxide or nickel particles in the composites grew by coalescence and sintering. Compactness of the composites, higher in nickel–silica composites than their counterpart nickel oxide, increased with the temperature of preparation and the concentration of nickel nitrate. Nickel always formed larger crystallites than its counterpart nickel oxide, due to its higher sintering rate. At 500 °C, the crystallite growths of nickel oxide and nickel were inhibited by the low sintering rate and the formation of nickel intermediates, respectively, while at 1000 °C their phase-pure crystallites continuously grew with the increase in the nitrate concentration.     

Modification of interface anisotropy and its effect on microstructural evolution during ostwald ripening

We performed an experiment to study the role of anisotropy in interfacial energy during the coarsening of a complex oxide CaCu₃Ti₄O₁₂ (CCTO) material system. When we altered the interface anisotropy, we observed that evolution and sizes of spherical grains completely altered to facetted cubes. When interface became anisotropic, crystal growth appears to occur by the surface attachment/detachment, the motion of ledges, and the nucleation of new layers. Our observations showed that new layers grew by screw dislocation mechanism. This suggests that nucleation limited coarsening is occurring by the development of a transient bimodal grain size distribution consisting of large growing grains with step. In presence of PbO we always observed the development of shaped nucleus which grew larger. Sometimes very complex shaped crystals grew as a metastable shape. These shapes became uniform as the growth progressed and size of grains became larger. This process produces smaller grains that act as a source of material for the growing less defective larger grains.     

Effect of different solvents on the habit of meta‐nitroaniline single crystals

The habit of the organic non‐linear optical material meta‐nitroaniline (mNA) crystallized from different organic solvents such as acetone, benzene, ethyl acetate, n‐hexane, methanol and toluene were studied. Solubility of mNA in these solvents at various temperatures in the range between 288 and 323 K was determined by gravimetric method. Crystals were grown by restricted evaporation of solvents method. Solutions with different solvents having different chemical nature and polarity yielded crystals with different habits: one‐dimensional needles, two‐dimensional rhombic platelets and three‐dimensional octahedral. In addition, the mNA crystals show unidirectional growth behaviour along its polar [001] direction irrespective of the solvents used. All the grown crystals were found to be orthorhombic system with point group mm2 and space group Pbc2₁ which was confirmed by powder X‐ray diffraction study. Optical transmittance study showed that the grown mNA single crystals have optical transparency in the wavelength range between 430 and 1550 nm. SHG efficiency of the grown mNA crystal was 3 times grater than KDP. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

一步法制备BN/Si复合团簇结构

以球磨的B/BN混合物为原料,采用一步法在蘸有催化剂的硅片上合成了大量BN纳米刺包裹在Si纳米或微米线上的复合团簇结构.EDS和SAED表明外层的纳米刺是六方BN多晶,里面包裹的Si纳米或微米线则是立方的Si单晶.实验结果表明合成温度对BN/Si复合结构形成有重要影响,只有在1250 ℃以上的温度才会生成BN /Si复合团簇结构,另外只有当硅片与样品接触时才会形成复合产物.PL光谱显示复合产物在360 nm的激发下,其发光峰在303 nm(4.1 eV)和423 nm(2.93 eV)处.     

Synthesis,Structure and Electrical Conductivity of (BEDT-TTF)X(BrO4)Y Organic Metals

The electrochemical oxidation of BEDT-TTF (bis(ethylenedithio)-tetrathiafulvalene) in 1,1,2-trichloroethane solution in the presence of (n-Bu4N)Br04 as supporting electrolyte produces three distinct morphologies: needles, thick plates, and thin plates. These crystal habits have been identified with different crystallographic phases: needles as (BEDT-TTF) ₂Br04, thick plates as (BEDT-TTF)₂(Br0₄)(TCE)_0.5, and thin plates as (BEDT-TTF)₃(Br04)₂. The structural characterization and conductivity for these materials is presented.