An accurate dynamical electron diffraction algorithm for reflection high-energy electron diffraction

The conventional multislice method (CMS) method, one of the most popular dynamical electron diffraction calculation procedures in transmission electron microscopy, was introduced to calculate reflection high-energy electron diffraction (RHEED) as it is well adapted to deal with the deviations from the periodicity in the direction parallel to the surface. However, in the present work, we show that the CMS method is no longer sufficiently accurate for simulating RHEED with the accelerating voltage 3–100 kV because of the high-energy approximation. An accurate multislice (AMS) method can be an alternative for more accurate RHEED calculations with reasonable computing time. A detailed comparison of the numerical calculation of the AMS method and the CMS method is carried out with respect to different accelerating voltages, surface structure models, Debye–Waller factors and glancing angles.     

Ga束流低温辅助清理GaAs衬底表面氧化物的研究

采用低流量Ⅲ族Ga束流在分子束外延中低温辅助清理GaAs衬底表面氧化物.采用高能电子衍射监控衬底表面氧化物清理过程并得出氧化物清理速率及氧化层对高能电子的吸收系数.根据清理速率对衬底温度依赖的Arrhenius关系,估算了Ga辅助清理过程中发生化学反应所需要的活化能.Ga束流辅助清理衬底表面氧化物技术在外延生长中具有实...     

扫描透射电子显微镜及电子能量损失谱的原理及应用

扫描透射电子显微镜是透射电子显微镜的一种,近几年随着球差校正器的问世,扫描透射电子显微镜的分辨率达到亚埃级,结合能量分辨率为亚电子伏特的电子能量损失谱,可以对材料进行高空间分辨率及高能量分辨率的微结构和成分分析。文章简述了扫描透射电子显微镜的发展历程和工作原理,重点讲述了高角环形暗场像的成像机理以及基于高角环形暗场像对材料结构和成分进行分析的原理和应用;电子能量损失谱的成谱过程、谱的特征及其在材料化学和电子结构分析方面的优势和主要应用。     

温度对p-InN薄膜光电导灵敏度的影响

研究了p型InN的光电导效应。利用分子束外延技术(MBE)法生长出高质量的InN薄膜,在此基础上利用Mg掺杂获得了p-InN。原位反射高能电子衍射(RHEED)表明样品在生长过程中保持二维生长模式,原子力显微镜(AFM)测试结果显示台阶流的生长模式。实验发现,p型InN的光电导灵敏度随温度的升高而降低。其主要原因是当温度升高时,光生载流子浓度降低和样品背景浓度升高共同造成的。     

Thermal stability of ultrathin amorphous carbon films synthesized by plasma-enhanced chemical vapor deposition and filtered cathodic vacuum arc

Abstract

Ultrathin hydrogenated amorphous carbon (a-C:H) films deposited by plasma-enhanced chemical vapor deposition (PECVD) and hydrogen-free amorphous carbon (a-C) films of similar thickness deposited by filtered cathodic vacuum arc (FCVA) were subjected to rapid thermal annealing (RTA). Cross-sectional transmission electron microscopy (TEM) and electron energy loss spectroscopy (EELS) were used to study the structural stability of the films. While RTA increased the thickness of the intermixing layer and decreased the sp³ content of the a-C:H films, it did not affect the thickness or the sp³ content of the a-C films. The superior structural stability of the FCVA a-C films compared with PECVD a-C:H films, demonstrated by the TEM and EELS results of this study, illustrates the high potential of these films as protective overcoats in applications where rapid heating is critical to the device functionality and performance, such as heat-assisted magnetic recording.     

关于RHEED振荡技术优化GaAs(110)量子阱生长的研究

在GaAs(110)衬底上生长的半导体材料有诸多优良性能，使得在非极性GaAs(110)衬底上获得高质量各类异质结材料，成为近年来分子束外延生长关注的课题.考虑GaAs(110)表面是Ga和As共面，最佳生长温度窗口很小；反射式高能电子衍射的(1×1)再构图案对生长温度和V/Ⅲ束流比不敏感，难于通过观察再构图案的变化，准确地找到最佳生长条件.作者在制备GaAs(110)量子阱过程中，观察到反射式高能电子衍射强度振荡呈现出的单双周期变化.这意味着不同工艺条件下，在 GaAs(110)衬底上量子阱有单层和双层两种生长模式.透射电子显微镜和室温光致荧光光谱测量结果表明：在双层生长模式下量子阱样品光学性能较差，而在单层生长模式下量子阱光学性能较好，但是界面会变粗糙.利用这一特点，我们采用反射式高能电子衍射强度振荡技术，找到了一种在GaAs(110)衬底上生长高质量量子阱的可行方法. 关键词： 反射高能电子衍射 量子阱 分子束外延     

Adsorption and dissociation of Si2H6 on Ge(001)2 × 1

Adsorption and thermally-induced dissociation of disilane (Si₂H₆) on clean Ge(001)2 × 1 surfaces have been investigated using a combination of Auger electron spectroscopy (AES), electron energy loss spectroscopy (EELS), reflection high-energy electron diffraction (RHEED), and scanning tunneling microscopy (STM). With initial Si₂H₆ exposure at room temperature, the Si surface coverage increased monotonically, the EELS surface dangling bond peak intensities continuously decreased, and the intensity of half-order RHEED diffraction rods decreased. The low-coverage Si₂H₆ sticking probability at 300 K on Ge(001) was found to be 0.5 while the saturation coverage was 0.5 ML. A new EELS feature, GSH, involving Si-H and Ge-H bond states was observed at Si₂H₆ exposures φ 3.4 × 10¹³ cm⁻². In contrast to Si₂H₆ -saturated Si(001), the saturated Ge(001) surface significant fraction of dimerized bonds. Adsorbed overlayers were highly disordered with the primary species on saturated surfaces being SiH₂, GeH, and undissociated SiH₃· Si₂H₆-saturated Ge(001)2 × 1 substrates were annealed for l min at temperatures T_a between 425 and 825 K. Admolecules were mobile at T_a = 545 K giving rise to significant ordering in one-dimensional chains. By T_a = 605 K, essentially all of the admolecules were captured into coarsened islands. Dangling-bond EELS peaks reappeared by 625 K and the intensities of the half-order RHEED diffraction rods increased. Ge segregation to the surface, which began at T_a 625 K, occurred rapidly at T_a 675 K. All H was desorbed by 725 K.     

InAs(001)表面脱氧动力学分析

利用反射式高能电子衍射(RHEED)实时监控对InAs衬底进行两步完全脱氧的过程, 对比了有低(高)砷等效束流压强保护下采用两步法对InAs衬底缓慢长时间的高温脱氧过程. InAs衬底两步完全脱氧法的第一步为传统的缓慢升温脱氧方法, 第二步为高温In束流辅助脱氧方法. 衬底高温脱氧的RHEED衍射图样说明了高温In束流辅助脱氧最终完全清除传统的缓慢升温法无法去掉的残留氧化物, 通过脱氧完成同质外延生长后的扫描隧道显微镜图像, 说明高砷等效束流压强保护下的脱氧方法是可行的; 分析了高温In束流能完全清除衬底表面残余In氧化物的原理. 关键词： 热分解 Ⅲ-V族半导体 反射式高能电子衍射     

Computer modeling of morphological evolution and RHEED intensity oscillations of thin-film growth by laser molecular beam epitaxy

The morphological evolution of the unit cell by unit cell layer growth of thin films by laser molecular beam epitaxy (laser MBE) is simulated by the Monte Carlo (MC) method. As a more realistic simulation, the effect of the surface terrace on reflection high-energy electron diffraction (RHEED) intensity oscillations is considered in our model. The calculation shows that the surface terrace effect has an obvious influence on the intensity oscillation shapes. Moreover, we consider the growth units impinging on the surface batch by batch rather than one by one. It is found that the surface morphologies are different, with different numbers of units impinging by a laser pulse on the surface. Furthermore, the surface roughness increases with a decrease in substrate temperature and with an increase in the unit impinging rate (which is determined by the energy of each laser pulse). The validity of the growth model is demonstrated by comparing our MC-simulated RHEED intensity oscillations with those observed in laser MBE experiments.     

Epitaxial growth of Au and Pt on Fe3O4(1 1 1) surface

We have studied the epitaxial growth of Au and Pt layers on Fe₃O₄(1 1 1) as a function of the deposition temperature and thickness. The layers were deposited by UHV sputtering and the structural properties were investigated by reflection high energy electron diffraction (RHEED), X-ray experiments and transmission electron microscopy (TEM). The epitaxial growth of both metals was obtained whatever the deposition conditions but the wetting is however different for the two metals. Comparison between the coverage ratios of Au and Pt is correlated with their surface and interfaces energies. The optimum conditions to achieve a 2D flat epitaxial metallic layer are determined.     

Fast measurement of rocking curve of reflection high-energy electron diffraction by using quasi-1D convergent beam

In order to investigate dynamic change in surface structure, we tried to measure the rocking curve of reflection high-energy electron diffraction (RHEED) by using a quasi-1D convergent beam method, which means a superposition of a hundred RHEED patterns at different glancing angles on one image. After we have checked the experimental accuracy, it is confirmed that the measurement time is shortened to 0.3 s by using this method. We also show an application of this method to a real time observation of surface segregation of B atoms while a highly B-doped Si is annealed.     

Growth of Co nanoparticles on a nanostructured θ-Al2O3 film on CoAl(1 0 0)

We have investigated the growth of Co nanoparticles on θ-Al₂O₃/CoAl(1 0 0) by means of Auger electron spectroscopy (AES), high-resolution electron energy loss spectroscopy (EELS), low energy electron diffraction (LEED) and scanning tunneling microscopy (STM). Due to Volmer-Weber growth, Co forms particles with a mean diameter of approximately 2.5 nm and height of 0.8 nm. Even on the entirely covered oxide, there is no Ostwald ripening and Co particles stay structurally isolated. The nanoparticles exhibit a small size distribution and tend to form chains, as predetermined by the streak structure of the oxide template. For sufficient high coverages Co-core-CoO-shell nanoparticles may be evidenced, which is explained as a result of surfactant oxygen. The nanostructured particles may open the door to numerous applications, such as in catalysis and magnetoelectronic applications, where large areas of ordered nanodots are desired.     

Elemental steps in the growth of thin β-Ga2O3 films on CoGa(1 0 0)

The oxidation of CoGa(1 0 0) at 700 K was studied by means of high resolution electron energy loss spectroscopy (EELS), scanning tunneling microscopy, low energy electron diffraction and Auger electron spectroscopy (AES). At 700 K, thin well-ordered β-Ga₂O₃ films grow on CoGa(1 0 0). The EEL spectrum of the Ga-oxide films exhibit Fuchs–Kliewer phonons at 305, 455, 645, and 785 cm⁻¹. For low oxygen exposure (<0.2 L), the growth of oxide-islands starts at step edges and on defects. The oxide films have the shape of long, rectangular islands and are oriented in the [1 0 0] and [0 1 0] directions of the substrate. For higher oxygen exposure, islands of β-Ga₂O₃ are found also on the terraces. After an exposure of 200 L O₂ at 700 K, the CoGa(1 0 0) surface is homogeneously covered with a thin film of β-Ga₂O₃.     

Anisotropic kinetics on growing Ge(0 0 1) surfaces

Reflection high-energy electron diffraction (RHEED), reflectance difference spectroscopy (RDS), and scanning tunneling microscopy (STM) have been used to study the anisotropic kinetics on the growing Ge(0 0 1) surface. While switching of dimer direction in alternate (2 × 1)/(1 × 2) layers causes the bilayer-period oscillations in RD response, RHEED oscillations are governed by variations in surface step densities. We show that the RHEED oscillations are strongly affected by the growth front morphology: when the growth front becomes distributed over several layers, the transition from bilayer- to monolayer-period occurs in RHEED oscillations.     

Initial stages of MnAs/GaAs(0 0 1) epitaxy studied by RHEED azimuthal scans

We study the nucleation phase of molecular beam epitaxy of (hexagonal) MnAs on (cubic) GaAs (0 0 1) using reflection high-energy electron diffraction (RHEED) azimuthal scans. The nucleation proceeds from a non-reconstructed initial stage through randomly oriented small nuclei and two orientation stages to the final single-phase epitaxial orientation. The fascinatingly complex nucleation process contains elements of both Volmer-Weber and Stranski-Krastanov growth. The measurement demonstrates the potential of high-resolution RHEED techniques to assess details of the surface structure during epitaxy.     

Growth and structure of vanadium oxide on anatase (1 0 1) terraces

The interaction of vanadium oxide with epitaxial anatase films exposing (1 0 1) terraces was characterized. The TiO₂ films were grown on vicinal LaAlO₃ (1 1 0) substrates by oxygen plasma-assisted molecular beam epitaxy (OPA-MBE); reflection high energy and low energy electron diffraction (RHEED and LEED) indicated that the films exposed (1 0 1) terraces of the anatase TiO₂ polymorph. When a vanadium oxide monolayer was deposited onto the anatase surface by OPA-MBE at 725 K, only (1 × 1) RHEED and LEED patterns were observed. The V X-ray photoelectron spectroscopy (XPS) peak intensities indicated that the monolayer wetted the anatase surface and so the diffraction patterns were attributed to an epitaxial vanadia layer. Analysis of the vanadium oxide monolayer by X-ray and ultraviolet photoelectron spectroscopies revealed that the V was predominantly 5+. When the vanadia coverage was increased at 725 K, Auger electron spectra showed only very slow attenuation of the anatase Ti peaks while spots began to develop in RHEED patterns recorded along the LaAlO₃ direction; both indicative of 3-D cluster formation. In the orthogonal direction, the RHEED patterns showed unusual diagonal streaks. Meanwhile, the (1 × 1) LEED pattern persisted even after 30 nm of vanadia was deposited. This was attributed to gaps between the 3-D clusters exposing the epitaxial monolayer. Core level XPS spectra of the 3-D clusters revealed a broad V 2p_3/2 peak that was centered at the position expected for V⁴⁺ but could be deconvoluted into three peaks corresponding to V³⁺, V⁴⁺, and V⁵⁺. It is shown that crystallographic shear that accommodates such variations in the oxygen content of V oxides can lead to the diagonal streaks in RHEED patterns recorded along the LaAlO₃ [0 0 1] direction even as the pattern in the orthogonal direction shows sharp transmission spots. The results show that vanadia growth on anatase (1 0 1) proceeds through the Stranski-Krastanov mode with a strong vanadia-titania interaction stabilizing a dispersed vanadia monolayer. The results are compared with previous data for vanadia growth on anatase (0 0 1) where smooth, epitaxial VO₂ films grow ad infinitum.     

Atomic and Electronic Structure of V/MgO Interface

Thin films of vanadium were deposited on the (001) surface of a MgOsubstrate by molecular beam epitaxy (MBE) and the V/MgO interface wasinvestigated by cross-sectional high resolution electron microscopy(HREM) and electron energy loss spectroscopy (EELS). In order todetermine the location of atoms at the interface, computersimulations were performed for four possible models, and bestmatching between the experimental and simulated images was obtainedfor the model where the V atoms are located directly on top of the Mgatoms at the interface. Interface bonding mechanism was investigatedby a first principles molecular-orbital (MO) calculation using thediscrete-variational (DV)-X method for a modelcluster of the interface, i.e., (Mg₉O₉V₅).The V-3d band was located in between the band-gap of MgO, and nearly empty Mg-3sp orbitals werefound to overlap with the V-3d band. The Mg-3sp and V-3d hybridizedin a bonding manner, thereby generates strong covalent bondingbetween V and Mg. Nearly filled O-2p orbitals were also found tohybridize with the V-3d orbitals in an antibonding manner. The bondoverlap population of the V–O bond was approximately four timessmaller than that of the V–Mg bond when the bond-length was thesame. The near edge structure of EELS specific to the interface wasobtained using a V/MgO multilayer specimen at both Mg-K and O-Kedges. Comparison between the experimental and theoretical spectra bythe present MO calculation clearly found the presence of hybridizedorbitals of V-3d with Mg-3p.     

Interpretation of initial stage of 3C-SiC growth on Si(1 0 0) using dimethylsilane

The initial stage of cubic silicon carbide (3C-SiC) growth on a Si(0 0 1) surface using dimethylsilane (DMS) as a source gas was observed using scanning tunneling microscopy (STM) and reflection high-energy electron diffraction (RHEED). It was found that the dimer vacancies initially existing on the Si(0 0 1)-(2 × 1) surface were repaired by the Si atoms in DMS molecules, during the formation of the c(4 × 4) surface. From the STM measurement, nucleation of SiC was found to start when the Si surface was covered with the c(4 × 4) structure but before the appearance of SiC spots in the RHEED pattern. The growth mechanism of SiC islands was also discussed based on the results of RHEED, STM and temperature-programmed desorption (TPD).     

Fe3O4/MgO(100)薄膜外场诱导电阻变化特性

采用激光分子束外延（L-MBE）方法,以MgO(100)为基底生长了Fe3O4单晶薄膜, 研究了Fe3O4/MgO(100)薄膜外场（温度、磁和激光场）诱导电阻变化特性。X射线衍射(XRD)分析表明Fe3O4薄膜是沿MgO(200)晶面外延生长的单晶薄膜;反射高能电子衍射（RHEED）强度振荡曲线分析表明Fe3O4薄膜表面平整,而且生长模式为2维层状生长;原子力显微镜（AFM）分析表明Fe3O4薄膜表面粗糙度为0.201 nm,说明薄膜表面达到原子级平整度。外场作用下Fe3O4薄膜的电阻测试表明:薄膜样品的电阻在120 K(Verwey转变温度)出现一峰值,略微下降后继续增大, 展现出半导体型的导电特性; 在激光作用下,整个测量温度范围内薄膜样品的电阻减小,样品展示出瞬间光电导的特性;从降温曲线可以看出, Verwey转变温度由无激光作用时的120 K上升到有激光作用时的140 K; 光致电阻变化率随着温度的降低而增大,这主要是由于激光作用导致电荷有序态的退局域化。     

Deposition and properties of highly C-oriented GaN films on diamond substrates

High-quality GaN films are deposited on freestanding thick diamond films by electron cyclotron resonance plasma enhanced metal organic chemical vapor deposition (ECR-PEMOCVD). The TMGa flux dependent structural, morphological, and electrical characteristics of GaN films were investigated by x-ray diffraction analysis (XRD), reflection high-energy electron diffraction (RHEED), atomic force microscopy (AFM) and Hall effect measurement. The results indicate that it is feasible to deposit GaN films on freestanding thick diamond films under the proper deposition procedures. The high-quality GaN films with small surface roughness of 4.9 nm and high c-orientation are successfully achieved at the optimized TMGa flux of 0.5 sccm. The GaN/diamond structure has great potential for the development of SAW devices with high frequencies and low insertion.