Scanning tunneling and atomic force microscopy study of the misfit layer compounds (LaS)1.14(NbS2)n (n=1, 2) and [(Pb,Sb)S)]1.14NbS2

The misfit layer compounds (LaS)_1.14(NbS₂)_n (n=1, 2) and [(Pb,Sb)S]_1.14NbS₂ were examined by scanning tunneling microscopy (STM) and atomic force microscopy (AFM). In these compounds the NaCl-type double MS (M=La, Pb, Sb) layers (Q layers) alternate with the NbS₂ layers (H layers) made up of NbS₆ trigonal prisms. It was possible to record AFM and STM images for only the H layers for (LaS)_1.14(NbS₂)_n, but for both the H- and Q-layers for [(Pb,Sb)S]_1.14NbS₂. Partial and total electron density plots of the H and Q layers were calculated to interpret the observed STM and AFM images. The bright spots in the STM and AFM images of the H layer correspond to S atoms, and those of the Q layer to Pb and Sb atoms. The STM images for the Q layers of [(Pb,Sb)S]_1.14NbS₂ suggest that a short-range ordering of the Pb and Sb atoms occurs in the (Pb,Sb)S sheets of the Q layer.     

A TEM and XRD study of the SbNbSe3 misfit layer structures

Two new misfit layer structures have been synthesized within the Sb-Nb-Se system. Powder X-ray diffraction and electron microscopy techniques (electron diffraction, HREM, XEDS) have been used to determine the nature of their structure. According to TEM and XEDS data (for more than 15 crystals studied) both phases are monolayer type, i.e. (SbSe)1+delta (NbSe2). Electron microscopy reveals a composite modulated structure that consists of the periodical intergrowth of a pseudotetragonal SbSe layer, denominated as Q, and a pseudohexagonal layer NbSe2, denominated as H. Both layers fit along b, stack along c and do not fit along a (misfit) giving rise to an incommensurate modulation along this direction. The two phases differ in the symmetry of the Q layers being in one case orthorhombic (for delta = 0.17) and monoclinic in the other (for delta = 0.19). After the characterization of the sample by electron microscopy the unit cells of the basic layers could be refined for both phases by powder X-ray diffraction: aQ = 5.824(2) A, bQ = 5.962(5) A, cQ = 23.927(6) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees and aH = 3.415(5) A, bH = 5.962(6) A,, cH = 11.962(1) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees for the orthorhombic phase; aQ = 5.844(2) A, bQ = 5.981(1) A, cQ = 23.919(5) A, alpha = 90 degrees, beta = 90 degrees and gamma = 96.00(3)degrees and aH = 3.439(1) A, bH = 5.994(2) A, cH = 11.956(3) A, alpha = 90 degrees, beta = 90 degrees and gamma = 90 degrees for the monoclinic phase. The phase with the monoclinic Q-sublattice often appears as twinned crystals. The more abundant crystals are disordered intergrowths of both monolayer phases.     

Electron microscopy study of incommensurate modulated structures in misfit ternary chalcogenides

The study of misfit structures by means of transmission electron microscopy and associated techniques is reviewed. It is complementary to X-ray crystallography and provides a local and direct view of the beautiful complexity of these systems. Three different types are presented in this work. Misfit columnar structures can be contemplated as a case of one-dimensional misfit structures while misfit layer structures are considered as two-dimensional misfit structures. Some extra dimensionality is added when these misfit layer structures wrap to give rise to tubular crystals. Electron microscopy/diffraction shows clearly in many examples the presence of structural modulations as weak satellite reflections that are very difficult to detect by X-ray diffraction methods. Besides, high-resolution images show the presence of stacking defects in some of these misfit layer structures.     

Modulation structure in the STM images of the non-metallic misfit-layer compound (PbS)1.12VS2

This paper presents the scanning tunneling microscopy (STM) results of the misfit-layer compound (PbS)_1.12VS₂, which is constructed of alternately stacking of PbS (Q) and VS₂ (H) layers. Temperature dependent resistivity measurements show a semiconducting behavior with small activation energies. Unlike the metallic 1Q/1H type of compounds we have succeeded to take both the STM images of a Q layer and a H layer, because electron tunneling from the underlying H layer is suppressed when intermediate positive bias voltage (V_b) is applied to a tip. At V_b = 0.15 V the image shows pseudo-tetragonal arrays of bright spots, although it is obscure with decreasing bias voltage and disappears at less than 10 mV. A modulation structure is found on the H layer of a stepped surface on which surface atoms are undulated in a period being twice the V-V interatomic distance in the [1 0]_H or the [1 1]_H direction.     

Epitaxial growth of lattice mismatched SrF2 films on (100) GaAs

For the first time insulating epitaxial SrF₂ films on (100) GaAs substrates have been grown by thermal deposition followed by in situ annealing process. Structural properties of SrF₂ films examined by X-ray diffraction, scanning electron microscopy and transmission electron microscopy indicate a very good crystalline quality. It is observed from the X-ray analysis that SrF₂ layers thinner than 100 nm suffer two dimensional compressive stress due to the lattice misfit while those thicker than 100 nm suffer two dimensional tensile stress due to the difference in the thermal expansion coefficients.NCL Communication No. 5077     

非晶Ni-P合金晶化过程中生成的六角亚稳相

本文利用透射电镜中的双倾台绕c^{*轴旋转晶体,唯一地确定了Ni-P非晶膜晶化后生成成分约为Ni_2.2P的针状亚稳相具有六角点阵,a=6.73?,c=9.42?。堆垛类型为AA…。(001)平面的高分辨点阵象以及衍射斑点沿c*方向拉长成条纹均表明晶体存在一维无序错排。 关键词：}     

Photoinduced transition of [Fe(CN)5NO] nitroprusside anions to metastable states and electron localization in the (BEDT-TTF)4K[Fe(CN)5NO]2 molecular metal

The crystals of (BEDT-TTF)₄K[Fe(CN)₅NO]₂, representing a quasi-two-dimensional organic metal with conducting layers of bis(ethylenedithio)tetrathiofulvalene (BEDT-TTF) and nonconducting layers containing pho-tochromic nitroprusside anions [Fe(CN)₅NO]^2?, were studied by the method of electron spin resonance. Illuminated by light with a wavelength of 514.5 nm, the organic metal crystals feature the formation of localized paramagnetic centers in the conducting cation layers of BEDT-TTF. The phenomenon of electron localization in the BEDT-TTF layers is related to the light-induced formation of long-lived metastable states of nitroprusside anions.     

Lattice imaging of close-packed structures by high resolution electron microscopy: ABO3 perovskite polytypes

Lattice imaging technique of high resolution electron microscopy has been employed to examine 4H, 6H and 9R ABO₃ perovskite polytypes. The lattice images can be correlated with the lattice periodicity and the stacking sequence of AO₃ layers and BO₆ octahedra. The study shows the utility and validity of the lattice imaging technique for the study of relatively close-packed systems. Commonwealth Visiting Professor, University of Oxford (1974–75).     

Step-controlled strain relaxation in the vicinal surface epitaxy of nitrides

On-axis and vicinal GaN/AlN/6H-SiC structures grown under identical conditions have been studied by x-ray diffraction and transmission electron microscopy to demonstrate the distinctive features of vicinal surface epitaxy (VSE) of nitrides on SiC. In VSE, the epilayers are tilted from the substrate due to the out-of-plane lattice mismatch (Nagai tilts), and the in-plane mismatch strains are more relaxed. The majority of misfit dislocations (MDs) at the vicinal AlN/6H-SiC interface are found to be unpaired partial MDs that are geometrically necessary to correct the stacking sequences from 6H to 2H. This mechanism indicates that it is possible to develop "step-controlled-epitaxy" strategies to control strain relaxation by adjusting the substrate offcut angles.     

Sonochemical syntheses of a nanoparticles cadmium(II) supramolecule as a precursor for the synthesis of cadmium(II) oxide nanoparticles

Nanoparticles of a three-dimensional supramolecular Cd(II) compound, [Cd(L)(2)(H(2)O)(2)] (1), (L(-)=1H-1,2,4-triazole-3-carboxylate), have been synthesized by a sonochemical process and characterized by scanning electron microscopy, X-ray powder diffraction, IR spectroscopy and elemental analyses. The thermal stability of compound 1 in both its bulk and nano-size has been studied by thermal gravimetric (TG) and differential thermal analyses (DTA) and compared with each other. Concentration of initial reagents effects on size and morphology of nano-structured compound 1, have been studied. Calcination of the single crystals and nano-sized compound 1 at 650°C under air atmosphere yields CdO nanoparticles.     

Control of symmetric properties of metamorphic In_(0.27)Ga_(0.73)As layers by substrate misorientation

Asymmetry in dislocation density and strain relaxation has a significant impact on device performance since it leads to anisotropic electron transport in metamorphic materials. So it is preferred to obtain metamorphic materials with symmetric properties. In this paper, we grew metamorphic In_(0.27)Ga_(0.73) As epilayers with symmetric low threading dislocation density and symmetric strain relaxation in two (110) directions using In Al Ga As buffer layers on 7°misoriented Ga As(001)substrates. To understand the control mechanism of symmetric properties of In_(0.27)Ga_(0.73) As layers by the substrate miscut angles, In_(0.27)Ga_(0.73) As grown on 2°and 15°misoriented substrates were also characterized as reference by atomic force microscopy, transmission electron microscopy, and high resolution triple axis x-ray diffraction. The phase separation and interaction of 60°misfit dislocations were found to be the reasons for asymmetry properties of In_(0.27)Ga_90.73 As grown on 2and 15°substrates, respectively. Photoluminescence results proved that the In_(0.27)Ga_(0.73) As with symmetric properties has better optical properties than the In_(0.27)Ga_(0.73) As with asymmetric properties at room temperature. These results imply that high quality metamorphic In_(0.27)Ga_(0.73) As can be achieved with controllable isotropic electron transport property.     

Study of Phase Transformations in (Cs,NH4)4(HSO4)3(H2PO4) Crystals

Physics of the Solid State - Phase transitions in crystals of (Cs,NH4)4(HSO4)3(H2PO4) solid solutions have been investigated by synchronous thermal analysis and polarization microscopy at different...     

Total suppression of superconductivity by high magnetic fields in YBa(2)Cu(3)O(6.6)

We have studied the variation of transverse magnetoresistance of underdoped YBCO(6.6) crystals, either pure or with reduced T(c) down to 3.5 K by electron irradiation, in fields up to 60 T. We find evidence that the superconducting fluctuation contribution to the conductivity is suppressed only above a threshold field H(c)'(T), which is found to vanish at T(c)' > T(c). In the pure YBCO(6.6) sample, H(c)' is already 50 T at T(c). We find that increasing disorder weakly depresses H(c)'(0), T(c)', and T(nu), the onset of the Nernst signal. Thus, these energy scales appear more characteristic of the 2D local pairing than the pseudogap temperature which is not modified by disorder.     

Vapor-Phase Synthesis and Magnetoresistance of (Cd0.993Zn0.007)3As2 Single Crystals

JETP Letters - We report a highly anisotropic magnetoresistance of (Cd0.993Zn0.007)3As2 single crystals, which have been synthesized by the vapor-phase growth. Scanning electron microscopy and...     

Scalable synthesis of graphene on single crystal Ir(111) films

We have investigated single crystal Ir(111) films grown heteroepitaxially on Si(111) wafers with yttria-stabilized zirconia (YSZ) buffer layers as possible substrates for an up-scalable synthesis of graphene. Graphene was grown by chemical vapor deposition (CVD) of ethylene. As surface analytical techniques we have used scanning tunneling microscopy (STM), low-energy electron diffraction, scanning electron microscopy, and atomic force microscopy. The mosaic spread of the metal films was below 0.2° similar to or even below that of standard Ir bulk single crystals, and the films were basically twin-free. The film surfaces could be improved by annealing so that they attained the perfection of bulk single crystals. Depending on the CVD conditions a lattice-aligned graphene layer or a film consisting of different rotational domains were obtained. STM data of the non-rotated phase and of the phases rotated by 14° and 19° were acquired. The quality of the graphene was comparable to graphene grown on bulk Ir(111) single crystals.     

Strain relief of heteroepitaxial bcc-Fe(001) films

The strain relief of heteroepitaxial bcc-Fe(001) films, deposited at 520-570 K onto MgO(001), has been investigated by scanning tunneling microscopy. In accordance with real-time stress measurements, the tensile misfit strain is relieved during coalescence of flat, mainly 2-3 monolayers (ML) high Fe islands at the high thickness of approximately 20 ML. To accommodate the misfit between merging strain-relaxed islands, a network of 1/2[111] screw dislocations is formed. A strong barrier for dislocation glide--which is typical for bcc metals--is most likely responsible for the big delay in strain relief of Fe/MgO(001), since only the elastic energy of the uppermost layer(s) is available for the formation of an energy-costly intermediate layer.     

Stabilization of the misfit layer compound (PbS)1.13TaS2 by metal cross substitution

Photoemission microspectroscopy on the layered misfit compound (PbS)1.13TaS2 provides direct evidence for Ta substitution into PbS layers as well as for Pb substitution into TaS2 layers. This metal cross substitution alters the charge balance between alternating layers and can explain the remarkable stability of (PbS)1.13TaS2 and, possibly, of analogous misfit compounds. It is suggested that even formally stoichiometric misfit compounds can be stabilized by this mechanism.     

Low-density dislocation arrays at heteroepitaxial Ge/GaAs-interfaces investigated by high voltage electron microscopy

High-voltage electron microscopy in combination with a large-area thinning technique has been applied to thin epitaxial Ge layers on GaAs substrates. These layers exhibit 60° misfit dislocations along the 〈110〉 directions parallel to the interface. Various dislocation reactions are evaluated from the electron micrographs, e.g. the formation of non-glissile 90° dislocations from two nearly parallel 60° dislocations and the annihilation reaction of two crossing 60° dislocations with identical Burgers vectors. The latter reaction occasionally leads to a dislocation multiplication. The misfit dislocations in very thin layers (～0.5 μm thickness and a linear dislocation density of less than 100 dislocation lines/cm) tend to be arranged in groups rather than being equidistant. Consequences for the interpretation of x-ray topograms are discussed.     

LEED crystallographic analysis for the structure formed by 2 ML of O at the Zr(0001) surface

A tensor LEED analysis is reported for the Zr(0001)-(1 × 1)-O surface which involves oxygen at a total coverage of 2 monolayers. The structure is indicated to have two layers of O: one forms an overlayer in which the O atoms bond to hollow sites of three-fold coordination on the regular metal surface, while the other layer has the O atoms in tetrahedral hole sites between the first and second metal layers. The stacking sequence, designated as (C)B(A)AB... corresponds to the first three layers of anion-terminated cubic ZrO₂, although some lateral compression is needed for superposition on the regular hcp Zr structure. The absorption of O in the tetrahedral holes results in a significant expansion in the first-to-second Zr---Zr interlayer spacing to about 3.44 Å from the bulk vaue of 2.57 Å. The O---Zr bond lengths are estimated to equal 2.07 Å for the overlayer O atoms, and 2.21 Å for the O atoms in tetrahedral hole sites. Comparisons are made with the structures of the corresponding 0.5 and 1 ML surfaces formed by the O/Zr(0001) system.     

Molecular beam epitaxy of organic films investigated by high resolution low energy electron diffraction (SPA-LEED): 3,4,9,10-perylenetetracarboxylicacid-dianhydride (PTCDA) on Ag(1 1 1)

A detailed investigation of the multilayer growth of PTCDA on Ag(1 1 1) by high resolution LEED (SPA-LEED) is reported. The first two monolayers are closed and exhibit a structure, which is commensurate with respect to the underlying Ag(1 1 1) surface. The lattice parameters are close to those of the (1 0 2) plane of the β bulk phase of PTCDA, with deviations ?2%. The vertical stacking of the second layer with respect to the first monolayer (observed at 300 K) corresponds to that in the β bulk phase of PTCDA. At high growth temperatures (400 K), Stranski-Krastanov growth occurs from the third monolayer onward, and PTCDA clusters, preferentially with few well defined facets, grow. The structure of the clusters is that of the thermodynamically more stable α bulk phase of PTCDA. Contrary, at low growth temperatures (200 K), the growth proceeds in the Frank van der Merve mode, with several open layers. From slope selection there is evidence for an Ehrlich-Schwoebel barrier. The lateral packing of the PTCDA grown at low temperatures corresponds within error to that of the β bulk phase. The low temperature structure and morphology is meta-stable. Short annealing at 300 K flattens the PTCDA film, and prolonged annealing at 400 K causes the film to adapt the structure and morphology obtained directly at 400 K growth temperature. Presumably, the formation of layers with a β-phase-like lattice at low temperature is due to the better fit of the β phase, compared to the α phase lattice, to the underlying commensurate monolayer. However, at high growth temperatures, the thermodynamically more stable α phase grows, reducing the area of lattice misfit to the underlying commensurate first two layers by formation of clusters.