Electron microscope study of intrinsic and extrinsic stacking faults,and twins in SOS at the early stage of epitaxial growth

Fine structures of the Si films on (1$\text{1}$02) sapphire have been studied by a lattice resolution TEM. The Si was deposited by the pyrolysis of silane in H₂ at 1000°C at a growth rate of 0.1μm/min. The samples for TEM were prepared by peeling off the Si films from the substrates after HF treatment. A film having a mean thickness of 500 Å was composed of (100) and {110} domains. The volume fraction of the {110} domains was more than 50% and about constant as a function of growth time. The {110} domains contained much higher density of microtwins than the (100) domains. These microtwins had various thicknesses including one atomic layer (intrinsic stacking faults) and two atomic layers (extrinsic stacking faults). The density of the intrinsic stacking faults was higher than those of extrinsic stacking faults and other twins. The {110} and (100) islands were nucleated independently and the microtwins were also present in the islands smaller than 500 Å in diameter.     

Struktur von AIIBVI-Epitaxieschichten in Abhängigkeit von den Aufdampfbedingungen

The structure of epitaxial films of A^IIB^VI-compounds is discussed. Especially the results of investigations concerning the epitaxy of CdSe on cleavage planes of NaCl and CaF₂ using high-vacuum evaporation are treated. Epitaxial films of A^IIB^VI-compounds usually show defect structures due to the co-existence of the zincblende and wurtzite structures, oriented overgrowth of these two phases, twinning and stacking faults. The resulting complex diffraction patterns (for electron diffraction in transmission) are discussed. The nature of the substrate, substrate temperature, and deposition rate besides experimental factors decisively influence the orientation, structure, and phase composition of the films. An influence of deviations from the stoichiometric composition has to be taken into account.     

Growth of freestanding GaN using pillar-epitaxial lateral overgrowth from GaN nanocolumns

Dislocation-free and strain-free GaN nanopillars, grown on Si by molecular beam epitaxy, were used as nanoseeds for a new form of epitaxial lateral overgrowth (ELO) by metalorganic vapour phase epitaxy (MOVPE) until full coalescence. Such overgrown GaN films are almost relaxed and were used as templates for producing thick GaN layers by halide vapour phase epitaxy (HVPE). The final GaN film is easily separated from the starting Si substrate. This is henceforth a new technology to produce freestanding GaN. The GaN crystal quality was assessed by transmission electron microscopy (TEM), photo- and cathodoluminescence (PL, CL). It was seen that the pillar-ELO is produced from a limited number of nanopillars. Some dislocations and basal stacking faults are formed during the coalescence. However, those that propagate parallel to the substrate do not replicate in the top layer and it is expected that the thickened material present a reduced defect density.     

Analysis of synthetic diamond single crystals by X-ray topography and double-crystal diffractometry

Structural features of diamond single crystals synthesized under high pressure and homoepitaxial films grown by chemical vapor deposition (CVD) have been analyzed by double-crystal X-ray diffractometry and topography. The conditions of a diffraction analysis of diamond crystals using Ge monochromators have been optimized. The main structural defects (dislocations, stacking faults, growth striations, second-phase inclusions, etc.) formed during crystal growth have been revealed. The nitrogen concentration in high-pressure/high-temperature (HPHT) diamond substrates is estimated based on X-ray diffraction data. The formation of dislocation bundles at the film-substrate interface in the epitaxial structures has been revealed by plane-wave topography; these dislocations are likely due to the relaxation of elastic macroscopic stresses caused by the lattice mismatch between the substrate and film. The critical thicknesses of plastic relaxation onset in CVD diamond films are calculated. The experimental techniques for studying the real diamond structure in optimizing crystal-growth technology are proven to be highly efficient.     

Mechanism of epitaxial ferrite-spinel layer formation on magnesium oxide substrate

The initial stage of small gap heteroepitaxial growth of magnesium-manganese ferrite films during chemical gas transportation reactions on orientation (100) magnesium oxide substrate was studied. Film growth would begin with origination of parallely oriented three-dimensional nuclei, their shapes at lower (1170 K) and at appear (1420 K) film synthesis temperature limits being different. After little islands had grown together and continuous layer formed the secondary nuclei would appear, their shapes resembling cut-up pyramids. Continuous layer minimum thickness was 0.15 μm. The growing together of little islands results in film block structure. Block sizes could be as big as 300–400 μm if films grow at the speed of 2 μm/min, the density of islands being 10⁶ cm⁻². Linear density of unconformity dislocations at film-substrate boundary would be (3.7 ÷ 7.4) 10³ cm⁻¹. It would depend on magnesium content for a film. Elastic stresses in films would come to 7 · 10⁸ ÷ 3 · 10⁹ dyne/cm². X-ray topography pictures of block structures and of accumulations of admixtures at block boundaries are presented.     

TEM-Untersuchungen von Gitterfehlern in ZnSiP2-Einkristallen

Results are dealt with concerning TEM investigations of lattice defects in ZnSiP₂ single crystals. After the crystal growth dislocations or stacking faults were found in a few cases only. More frequently twins were present in the microstructure. The crystallographic elements of twinning are {112} 〈111〉. After plastic deformation by bending at 900 °C local dislocation arrangements with high defect density (N_v ≈ 10⁶…︁ 10⁷ cm⁻²) were observed. By means of the diffraction contrast one Burgers vector b = 1/2 〈111〉 could be identified. In some cases the crystals also contained wide deformation stacking faults, which were limited by partial dislocations. The density of twins was not increased under the conditions of deformation reported here. As it can be concluded from investigations of Oettel et al. and from the results of the twin analysis, slip and generation of stacking faults take place on {112}-planes in ZnSiP₂ crystals. Crystallographic considerations on both processes are dealt with.     

Partial dislocations and stacking faults in cubic SiC

Numerous stacking faults and dislocations (formed by intersection of stacking faults and dislocations limiting nonintersecting stacking faults) in the 3C-SiC films grown by molecular beam epitaxy on a silicon substrate were studied by electron microscopy with the use of weak beams. A procedure for determining any of possible Burgers vectors of the (1/6)〈116〉-type glide dislocations and the (1/6) 〈110〉-and (1/3)〈001〉-type sessile partial dislocations (in face-centered cubic lattices) is developed based on the criterion of the contrast value. The sessile dislocations formed by intersections of stacking faults were shown to have the (1/6)〈110〉-and (1/3)〈001〈-type Burgers vectors. The width of nonintersecting stacking faults corresponds to the stacking-fault energy ranging within 0.1–2 mJ/m².     

The crystal growth and perfection of 2,4,6-trinitrotoluene

Large crystals of TNT were grown from ethyl acetate solution by both temperature lowering and solvent evaporation. The perfection of crystals grown from seeds under carefully controlled conditions was generally higher than those prepared by uncontrolled solvent evaporation. Examination by X-ray topography revealed the crystals to have a characteristic growth induced defect structure comprising growth sectors and boundaries, growth banding, solvent inclusions and dislocations. Twins and stacking faults (SF) were also observed. Many of the defects noted in the topographs can be attributed to impurities. The influence of the highly anisotropic crystal structure on the nature of growth defects is discussed. A structural model proposed to explain twinning and SF formation is partially supported by topographic evidence.     

Epitaxial growth in the (111)Ag/Cu and (111)Au/Cu systems

The initial stages of epitaxial growth in the (111)Ag/Cu and (111)Au/Cu systems were investigated using UHV-RHEED and TEM on the same specimens. Flat, monocrystalline (111)Cu substrates, 1100 Å thick, were formed in situ in the RHEED system on (111)NaCl/mica bilayers. The latter consisted of air-cleaved mica on which 150 Å of NaCl was vacuum-evaporated to form a (111)NaCl monocrystalline film. The NaCl layer allowed easy removal in water of the subsequently deposited bilayer metal film. RHEED showed that these Cu films grew with extremely flat surfaces at 400°C and 10 Å/sec deposition rates. They were then annealed at 500°C for 15 min to reduce their dislocation content and finally used as substrates for subsequent deposition of thin Ag or Au superlayers. The average Ag and Au superlayer thicknesses were varied from fractions of an Angstrom to approximately 20 Å. It was shown that despite the elongated streaks in the RHEED patterns, film growth occurred by an island mechanism, the islands having flat top surfaces. In the initial growth processes, the islands merely thickened. After a few average monolayers were deposited, the islands began to widen, often by means of much thinner islands, finally coalescing into a continuous film. The Au overgrowths became continuous in the 6–11 Å thickness range. In the case of Ag, there still were some open areas in the overgrowth at 20 Å. In both cases the continuous regions of the Ag and Au overgrowths consisted of sharply delineated thick and thin areas that gave rise to steps on the otherwise flat surface.     

HREM investigations of intermediate ZnO and ZnO/Y–ZrO2 layers in Y–ZrO2 bicrystals and ZnO films grown on Y–ZrO2 bicrystal substrates

The structure of yttrium-stabilized ZrO₂ (YSZ) bicrystals with ZnO and ZnO/YSZ/ZnO/YSZ/ZnO intermediate layers, as well as ZnO films grown on YSZ bicrystal (1 1 0)/90° substrates, has been investigated by means of high-resolution electron microscopy (HREM) and microanalysis. All bicrystals were produced by the solid-phase intergrowth (SPI) method. The internal ZnO film in the bicrystal formed at the SPI temperature of 1400°C consisted of domains with two symmetrical orientations: , and , . A bicrystal with a ZnO/YSZ/ZnO/YSZ/ZnO internal film was formed at the temperature of 1200°C. There was no mixing of ZnO and YSZ films and no traces of any solid-phase reactions were observed. Grains in all internal ZnO films and ZnO films grown on the bicrystal substrates had numerous stacking faults. It was found that SPI does not influence the density and structure of these defects. Orientational relationships between YSZ and ZnO in all samples were determined. The ZnO films grown on (1 1 0)/90° bicrystal substrates inherited the grain boundary (GB) from the substrate. Its structure and geometry is determined by four variants of ZnO grain growth.     

The Process of Formation of Epitaxial Cadmium and Zinc Oxide Films by Interaction of Single-Crystal AIIBVI Layers with Oxygen

The results of electron microscopic and electron diffraction investigation of the surface during annealing of single-crystal A^IIB^VI (CdS, CdSe, ZnSe, ZnS) films in the presence of oxygen are reported. It is shown that the behaviour of islands of cadmium oxide formed by chemical interaction between O₂ and the CdS, CdSe substrate in the process of growth resembles that of the nuclei in film condensation. CdO films become “continuous” more quickly, if the size of blocks of substrate-epitaxial A^IIB^VI film is larger. Epitaxial ZnO films formed on the surface of epitaxial ZnS and ZnSe layers are of a wurtzite structure or a cubic structure with the parameter a = 4.5 Å.     

A model for the growth of anomalous polytype structures in vapour grown SiC

A number of polytype structures observed in vapour grown SiC crystals have a unit-cell which is an integral multiple of the unit-cell of the basic 6H, 15R or 4H structure. The growth of such anomalous structures cannot be understood in terms of spiral growth round a single screw dislocation in a basic matrix. However many of these polytype crystals display a single growth spiral on their (0001) face indicating that they have resulted from spiral growth round a single screw dislocation. It is shown that this anomaly can be resolved if the basic matrix is assumed to contain stacking faults near the surface at the time of the origin of the screw dislocation ledge. This possibility, overlooked in the earlier deduction of polytype structures, must be taken into consideration since vapour grown SiC crystals frequently contain a high concentration of random stacking faults, producing continuous streaks on their X-ray diffraction photographs. The most probable fault configurations that can occur in 6H, 15R and 4H structures of SiC have been deduced from a calculation of their stacking fault energy. These fault configurations are then considered to lie at different distances from the surface at the time of the origin of a screw dislocation ledge. Such a faulted ledge gives rise to polytype structures during subsequent spiral growth even if the screw dislocation has an integral Burgers vector. The most probable series of polytype structures that can result from such a faulted matrix model are deduced. It is shown that nearly all the polytype structures of SiC hitherto regarded as anomalous (such as 36H, 54H, 66H, 45R, 90R etc.) are among the expected structures and there is no need to postulate a complicated configuration of cooperating dislocations to account for their growth.     

Defect Structure in Te-doped GaAs single Crystals after Plastic Deformation (I). Twins and Stacking Faults

At temperatures above the brittle-to-ductile transition (490 °C) in Te-doped GaAs three types of predominant defect configurations have been observed after uniaxial compression along a [001] direction: (i) twins and stacking faults (500 … 520 °C), (ii) slip zones of dislocations (≈ 550 °C) and (iii) dislocation cells (580 … 590 °C). In Part I quantitative details of the appearance of twins and stacking faults are given. Most frequently found were 30° partials in twins and stacking faults.     

Influence of carbon contamination on etched GaSb substrate on the quality of MBE-GaSb film and electrical transport through the film and the substrate

Undoped MBE-GaSb films were grown on undoped GaSb (100) substrates and the influence of carbon contamination on the etched GaSb substrate on the grown film were investigated. It was found that carbon contamination of the etched GaSb substrate was dependent on the chemical treatment method and produced stacking faults in the subsequent MBE growth of the GaSb film. Carbon contamination on the etched GaSb substrate degraded the quality of the GaSb film and affected ohmic characteristics between the film and the substrate. Substrate surface free of carbon contamination and thereby exhibitting no influence on the electrical transport through the film and the substrate could be reproducibly obtained by performing an oxide etch-off chemical treatment on the GaSb substrate.     

Surface morphology,structural and optical properties of polar and non-polar ZnO thin films: A comparative study

The polar and non-polar ZnO thin films were fabricated on cubic MgO (1 1 1) and (0 0 1) substrates by plasma-assisted molecular beam epitaxy. Based on X-ray diffraction analysis, the ZnO thin films grown on MgO (1 1 1) and (1 0 0) substrates exhibit the polar c-plane and non-polar m-plane orientation, respectively. Comparing with the c-plane ZnO film, the non-polar m-plane ZnO film shows cross-hatched stripes-like morphology, lower surface roughness and slower growth rate. However, low-temperature photoluminescence measurement indicates the m-plane ZnO film has a stronger 3.31 eV emission, which is considered to be related to stacking faults. Meanwhile, stronger band tails absorbance of the m-plane ZnO film is observed in optical absorption spectrum.     

Crystal structures of two forms of pentachloropyridine

Tetragonal and monoclinic forms of crystalline pentachloropyridine are described. Both forms may be regarded as layer structures. The basic layer common to the two structures has neighbouring molecules in the same orientation. The tetragonal form has a repeat unit of four layers, whereas the monoclinic form has a repeat unit of two layers. The packing of adjacent layers is essentially the same for both forms.Examples have been found in which the stacking sequences are interrupted, producing faults, twins and diphasic crystals.     

Defect Structure in Te-doped GaAs Single Crystals after Plastic Deformation (II). Dislocation Slip and Cell Formation

At temperatures above the brittle-to-ductile transition (490 °C) in Te-doped GaAs three types of predominant defect configurations have been observed after uniaxial compression along a [001] direction: (i) twins and stacking faults (500 … 520 °C), (ii) slip zones of dislocations (≈550 °C) and (iii) dislocation cells (580 … 590 °C). In Part II quantitative details of the appearance of slip and cell formation are given. Leading segments of gliding half loops are mainly of 60° type. Cell walls were formed by multiple slip of perfect dislocations.     

Growth evolution and microstructural characterization of semipolar (112̄2) GaN selectively grown on etched r-plane sapphire

Semipolar (112?2) GaN was grown on stripe etched r-plane sapphire substrate by a maskless selective growth method. The initial stage of growth is analyzed by describing the competitive nucleation mechanisms, due to the interplay between kinetics and energetics, on disparate crystallographic planes within the diffusion length of adatoms. The microstructure of the final coalesced semipolar GaN film is revealed by x-ray rocking curve (XRC) analysis and transmission electron microscopy (TEM). XRC analysis yields linewidths between 280 and 550 arcsec for all on-axis and off-axis diffractions. Linewidth broadening factors in dislocated crystals are considered, and a large reduction of stacking fault density can be seen from the measured linewidths as fit to this model. TEM shows a change in the defect characteristics as compared to conventional growth on m-sapphire, filtering of stacking faults and confirmation of the low dislocation density of the final GaN film. The microstructural quality of the film substantiates the possibility of using an inclined basal-plane growth to synthesize non-basal-plane active devices, thus removing the rigid restrictions in contemporary GaN nonpolar and semipolar heteroepitaxy.     

Polytypes of the system Fe1−xS

The structures of Fe_1−xS (0 < x < 0.135) are members of a family of derivative structures in the sense of Megaw. The NiAs structure as aristotype is the simplest and most symmetrical member of this family. The other polytypes of Fe_1−xS may be derived as hettotypes by lowering the symmetry. The loss of symmetry in changing from the aristotype to the hettotype may be of various kinds: small displacements of Fe and S atoms from the NiAs positions and/or Fe vacancies in some atomic planes occur. The structures of the system Fe_1−xS are interpreted as OD structures consisting of OD layers. The symmetry relations of the structures of FeS and Fe₇S₈ are described by OD groupoid families. Polymorphism, twinning and stacking faults are explained on this basis.     

采用溶胶凝胶前驱物制备氮化镓纳米晶体

采用溶胶凝胶法制备的前驱物进一步在900℃,氨气气氛中氮化得到粒径相对均匀、平均粒径为11.2nm的六方相氮化镓纳米晶体.XRD, HRTEM, SAED, EDS, FTIR被用于表征产物的微结构及组成.室温光致发光光谱显示产物位于3.46eV的带边发光峰和从 2.6～3.2eV 的宽的发光带.产物可直接用于制备氮化镓量子点复合材料和制备高质量的一维氮化镓晶体.