Characterization of dislocations in a LiNbO3 single crystal grown by micro pulling down method

LiNbO₃ single crystals grown by the micro pulling down (μ-PD) method have been revealed to be as free of dislocations and subgrain boundaries up to 500 μm in diameter. On the other hand, μ-PD LiNbO₃ single crystals grown along the x-axis in diameter of 800 μm were observed to be dislocated due to the size effect of crystal. The Burgers vectors of dislocations were determined to be [22 01], [101 1], and [01 11] by X-ray topography.     

Dislocations of salol crystals grown by the Czochralski method

Crystals of salol were grown by the Czochralski method in three different pulling directions to examine the crystallographic orientation effect of the seed. They were characterized by the etch pit method and X-ray projection topography. It was found that the dislocation density was 2 × 10³−1 × 10⁴/cm² and that the configuration of dislocations was straight. The running directions of dislocations strongly depend on the pulling directions; i.e., [11 0] and [1 10] for the crystal grown in [100] axis, [11 0], [1 10] and [110] for the crystal pulled along [112] axis and [010] for [010] axis crystal.     

铟掺杂ZnGa2O4纳米线中的结构缺陷分析

用热蒸发的方法合成了铟掺杂的ZnGa2O4纳米线.利用透射电镜和X射线能谱对样品的结构和成分进行了研究.在"之"字形和竹节形两种形貌的纳米线中分别发现了孪晶和面位错两种缺陷."之"字形生长的纳米折线是孪晶,沿<111>方向生长,孪晶角为140°.竹节形的纳米线沿<011>方向生长,竹节处存在两种面位错,面位错与生长方向分别成54°和90°角.缺陷的存在对纳米线的性质将产生重要影响.     

Low-angle boundary investigation in silicon single crystals

Low-angle boundaries in Si single crystals grown from the melt in [111], [100], [112], [110], [118] and [115] directions were investigated by chemical etching, copper decoration technique and X-ray topography. — LAB of four types were found in planes parallel to the crystal growth axes. Rearrangement of dislocations from slip bands into LAB was observed in heavily-doped Si crystals. The origin of LAB in melt grown Si crystals is discussed. It is shown that these boundaries are well interpreted in terms of dislocation alignment formation in the thermal stress field of the growing crystal.     

Sodium acetate tri-hydrate whiskers

A new kind of whisker, which has not been previously reported in the literature, was grown on membranes which were in contact with a saturated aqueous solution of sodium acetate, using several techniques. Cellulose acetate membranes were used in all the cases and growth was successful at 25 ± 2°C and 45–55% relative humidity. A dense colony of whiskers, sometimes stuck together in bundles, usually up to 5 cm in length and ranging in width from 0.3–100 μm, developed within 72 h of growth. The whiskers were identified as sodium acetate tri-hydrate by means of Debye-Scherrer X-ray powder method. Laue transmission photographs indicated the existence of twin crystals within the individual single crystal whiskers as proved by electron diffraction in TEM. Some whiskers included internal and external channels, and there were several secondary effects, such as thickening in the middle of a whisker, formation of arrow-heads or spirals at the tips and various modes of branching. The whisker morphology and the various growth phenomena may be explained as a whisker growth process from their bases, when we consider a continuous crystallization from material which is supplied through and over the membrane.     

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.     

Preparation of copper aluminum borate whiskers via flux method

Single‐crystal and uniform copper aluminum borate whiskers have been synthesized by heating a mixture of boric acid, copper sulfate and aluminum sulfate with potassium sulfate as flux at 870 °C for 4 h. The synthesized whiskers exhibit a well‐crystallized, one‐dimensional structure with diameters ranging from 100 nm to 5 μm, lengths from 5 to 100 μm. Heating temperature and flux addition affect the aspect ratio and morphology of the copper aluminum borate whiskers. A possible growth mechanism of the whiskers is proposed. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Textural properties of AISb films

Textural studies have been carried out in AlSb films deposited by coevaporation method under high vacuum at different substrate temperatures between 450° to 625 °C. The films have been examined by X-ray and electron diffraction techniques. It was observed that the films deposited around 550 °C were found to exhibit [110] and [111] textures and the films deposited at higher substrate temperatures (above 600 °C) were found to exhibit only [111] textures.     

Synthesis of bamboo‐like SiC whiskers from waste silica fume

A process for the utilization of wasted silica fume is proposed in this work. Silicon carbide (SiC) whiskers several tens of micrometers in length and with a bamboo‐like morphology have been successfully synthesized by a carbothermal reduction process using purified silica fume as the silicon source. The morphology and structure of SiC whiskers were investigated by X‐ray diffraction, Raman spectroscopy, scanning electron microscopy, and high‐resolution transmission electron microscopy. Studies found that the as‐synthesized whiskers were grown as single‐crystalline β‐SiC along the (111) growth direction. The whiskers consisted of hexagonal stems randomly decorated with larger‐diameter knots along their whole length. On the basis of the characterization results, a vapor–solid process was discussed as a possible growth mechanism of the β‐SiC whiskers.     

方解石制备碳酸钙晶须的影响因素及机理

以方解石矿石为原料,利用制备的重镁水(Mg(HCO₃)₂)及中间产物氯化钙制备文石型碳酸钙晶须,并采用SEM、XRD及EDS对产品进行表征。探究了重镁水与氯化钙反应过程中反应温度、反应时间、镁钙浓度比、重镁水浓度以及搅拌速度对碳酸钙晶须形貌的影响。通过单因素实验得出了最佳工艺条件:温度40 ℃、反应时间2 h、镁钙浓度比6∶1、重镁水浓度0.14 mol/L、搅拌速度150 r/min。在此条件下,制得了长度为40~65 μm、直径为0.6~1.5 μm、长径比为25~45的文石型碳酸钙晶须。     

The possibility of identifying the spatial location of single dislocations by topo-tomography on laboratory setups

The spatial arrangement of single linear defects in a Si single crystal (input surface {111}) has been investigated by X-ray topo-tomography using laboratory X-ray sources. The experimental technique and the procedure of reconstructing a 3D image of dislocation half-loops near the Si crystal surface are described. The sizes of observed linear defects with a spatial resolution of about 10 μm are estimated.     

煅烧和除碳温度对氮化硼晶须的影响

以三聚氰胺和硼酸为原料通过水浴加热合成晶须前驱体,然后经高温烧结成功制备出BN晶须.扫描电镜显示制备的BN晶须为针状结构,其直径和长径比分别为2～3 μm和40～100.通过X射线衍射分析,制备的BN晶须为六方晶相,晶格参数为a=0.2524 nm和c=0.6592 nm.红外光谱图谱表明在1383 cm-1和 812 cm-1处存在两个明显的B-N特征吸收带.晶须的烧成制度以及除碳温度对晶须形貌和性能的影响研究结果表明,当烧成温度为1700 ℃、除碳温度为600 ℃时可制备出形貌良好和结晶度高的氮化硼晶须.     

A study of the morphology and magnetic properties of silicon whiskers

Methods of growing Si whiskers are considered and the results of studying their magnetic susceptibility χ are reported. Silicon whiskers are grown using the method of chemical transport reactions in a closed bromide system. The crystals studied were divided into four groups: (i) crystals 0.1–0.9 μm in diameter, (ii) twinned crystals 1–2 μm in diameter, (iii) needle-like crystals from 5 to 1500 μm in diameter, and (iv) isometric crystals (the latter were not measured). With an increase in diameter, the whiskers of the first group changed their state from paramagnetic to diamagnetic, while the crystals of the third group showed a transition from a diamagnetic to a paramagnetic state. All these crystals show a nonlinear dependence of χ on the strength of an external magnetic field H; the nonlinearity increases with increasing the sample paramagnetism. The susceptibility of twinned samples is diamagnetic and close to the value of χ for bulk silicon, and the nonlinearity of the dependence χ (H) is insignificant. The measured values of χ of Si whiskers are explained by features of their crystal structure and chemical composition.     

Influence of low-temperature thermocycling on anisotropy of the structural state of commercial purity Beryllium

The influence of low-temperature cycling (300 ← 77 K) on the anisotropy of commerical purity beryllium structural state, obtained by uniaxial hot extrusion has been studied by means of X-ray method. In initial samples the anisotropy of structural state is shown by the preferential orientation of grains relative to extraction axis. Two types of experiments were carried out Two types of samples were investigated the samples cut out along and across the extrusion axis. It was shown that cycling in the samples oriented across the extrusion axis led to essential change in initial structural state due to intense twinning. Considerable changes in structures of the samples oriented along the extrusion axis were not observed. The effects are intensified by load application. Thermocycling leads to considerable decrease in grain size (form about 50 μm in initial state to about 30 μm after cycling) and decrease in structural state anisotropy. Nature of the phenomena found is discussed.     

Study of the specific features of single-crystal boron microstructure

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δa/a ≈ 0.4 and δc/c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [\(2\bar 2013\)] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3–0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50–300 K are indicative of its high structural quality.     

An X-ray scattering study of hydrogenated nanocrystalline silicon with varying crystalline fraction

Using X-ray diffraction (XRD) and small angle X-ray scattering (SAXS), we probed the nanostructural features of several PECVD grown nc-Si:H thin films with varying crystalline volume fraction. XRD results of a mixed phase film, 70% a-Si:H and 30% c-Si:H, show these crystallites have a preferred [220] orientation in the growth direction. Another film with approximately 90% c-Si also shows elongated grains, but with a preferred [111] orientation. The SAXS results also show an increase in scattering intensity when compared to the mixed phase material. In the mixed phase material, models show that the electron density fluctuations between the amorphous and crystalline phases are not enough to explain the measured SAXS scattering. Hydrogen clustered at the crystallite boundaries and in void regions of the a-Si phase must be included as well.     

Oriented growth of whiskers of AIIIBV compounds by VLS-mechanism

The oriented growth of GaAs, GaP, InAs and GaInAs whiskers on the same (GaAs, GaP) or different (InAs/GaAs, GaInAs/GaAs) substrates was studied. A detailed morphological study of GaAs whiskers on polar A(III), B(111 ) and non-polar (001), (011) substrates was performed. The growth conditions for ordered (perpendicular to substrate) growth on the A(111) and B(111 ) faces were determined. There were found discrete spectra of whisker systems on all substrates with the preferential growth of “arsenic” B{111 } faces. The dependence of the growth rate on the whisker diameter is typical for the vapour-liquid-solid (VLS) mechanism and is used for the determination of kinetic coefficients for polar faces. There was observed a periodic instability in growth of InAs and GaInAs whiskers.     

Strain relaxation in InGaAs/GaAs quantum wells grown on GaAs (111)A substrates

We have grown In_0.2Ga_0.8As strained quantum wells (SQWs) on GaAs (111)A just and off-angled substrates by molecular beam epitaxy (MBE). The photoluminescence (PL) peak energy of SQWs grown on (111)A related substrates shows a large redshift as compared with the calculated values. The red-shift observed in SQWs grown on a (111)A 5° off toward [001] substrate can be explained by the presence of a built-in electric field E = 154 kV/cm due to piezoelectric effect. The larger red-shift observed in samples grown on the other substrates is partially due to strain relaxation. A strain relaxation mechanism that consists of coherently grown islands when InGaAs growth begins and the generation of misfit dislocations when these islands coalesce, gives a qualitative explanation of the observed results.     

Manifestation of nonequivalence of the crystallographic {110} and {111} planes and charge-transfer mechanism in Y3Fe5O12 garnet crystals

The nonequivalence of the crystallographic {110} and {111} planes in Y₃Fe₅O₁₂ (YIG) garnet crystals was revealed in the analysis of the crystal density as a function of the intensity ratio of coherent and incoherent X-ray scattering (K/nk). The samples were divided into two groups with different types of variation in their physical properties. For the first time, the quantitative correlation between the absorption coefficient α and K/nk with due account of the crystallographic orientation in the YIG crystals was established. It was found that the samples with the (111) orientation had minimum resistivity at 293 K because it is along this direction that the easy magnetization axis, domain boundaries, and dislocations were oriented. It was shown that the parameter K/nk can be used as a criterion for estimating the part of conduction electrons involved in charge transfer.