Self-organized amorphous material in silicon (0 0 1) by focused ion beam (FIB) system

A method using a focused ion beam (FIB) to prepare a silicon amorphous material is presented. The method involves the redeposition of sputtered material generated during the interaction of the Ga⁺ ion beam with a silicon substrate material. The shape and dimensions of this amorphous material are self-organized and reproducible. The stability of this amorphous material under electron irradiation was investigated in the transmission electron microscopy (TEM). Electron irradiation can induce recrystallization of the amorphous material, resulting in the lateral and vertical growth, starting at an amorphous-crystalline interface, of polysilicon containing defects.     

Strain relaxation and surface morphology of high indium content InAlAs metamorphic buffers with reverse step

Low-temperature step-graded high indium content InAlAs (In% = 0.75) metamorphic buffer layers with reverse step layer grown on GaAs substrate by molecular beam epitaxy are investigated in this paper. The composition and the strain relaxation of the top InAlAs layer are determined by high-resolution triple-axis X-ray diffraction measurements, which show that the top InAlAs layer is nearly fully relaxed and the growth parameters for these samples have little influence on the strain relaxation ratio. Surface morphology is observed by reflection high-energy electron diffraction pattern and atomic force microscopy. The surface morphology is found to depend strongly on both the growth temperature and the As flux. Compared with other samples, the sample growth under the optimized conditions has the smallest value of root mean square surface roughness. Furthermore, the ω − 2θ and ω scans of the triple-axis X-ray diffraction and transmission electron microscopy result also show the sample grown under the optimized conditions has good crystalline quality.     

A New Method for the Measurement of Thickness in Single Crystals

A new method for thickness determination of single-crystal thin samples at exact zone axis orientation, based on pattern recognition in convergent beam electron diffraction (CBED), is presented. The method is especially well suited to materials with a large unit cell in zone axis directions where the reciprocal lattice is uniformly dense with diffraction points. The new method is based on comparison of a measured CBED zone axis pattern with a set of calculated ones. Its accuracy was estimated to be around 10% in the 5–100 nm thickness range as checked for garnets at the [111] zone orientation.     

Sample preparation by focused ion beam micromachining for transmission electron microscopy imaging in front-view

This article deals with the development of an original sample preparation method for transmission electron microscopy (TEM) using focused ion beam (FIB) micromachining. The described method rests on the use of a removable protective shield to prevent the damaging of the sample surface during the FIB lamellae micromachining. It enables the production of thin TEM specimens that are suitable for plan view TEM imaging and analysis of the sample surface, without the deposition of a capping layer. This method is applied to an indented silicon carbide sample for which TEM analyses are presented to illustrate the potentiality of this sample preparation method.     

Measuring the aspect ratios of ZnO nanobelts

Nanobelts are new materials that have a rectangular cross-section and are characterized by widths and width-to-thickness aspect ratios. In this paper, the thickness and aspect ratios of ZnO nanobelts are measured by a conjunction application of convergent beam electron diffraction (CBED) and electron energy-loss spectroscopy (EELS). The thicknesses of thicker nanobelts are first determined by CBED under two-beam diffracting condition, then they are used to determine the electron inelastic mean-free-path (MFP) length, which is 161±15 nm for ZnO at 200 kV. The thicknesses of the thinner nanobelts are then determined by EELS using the calibrated MFP. The results show that the aspect ratio depends on conditions under which the sample was synthesized.     

Growth and characterization of MOMBE grown HfO2

HfO₂ dielectric layers were grown directly on the p-type Si (1 0 0) by metalorganic molecular beam epitaxy (MOMBE). Hafnium tetra-butoxide was used as a Hf precursor and pure oxygen was introduced to form an oxide layer. The properties of the layers with different thicknesses were evaluated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HRTEM), and capacitance–voltage (C–V) and current–voltage (I–V) analyses. XRD and HRTEM results showed that the HfO₂ films thinner than 12 nm were amorphous while the films thicker than 12 nm began to crystallize in the tetragonal and the monoclinic phases. The XPS spectra of O 1s show that the O---Si binding energies shifted to the lower binding energy with increasing the HfO₂ layer thickness. Moreover, the snap back phenomenon is observed in accumulation capacitance. These changes are believed to be linked with the decomposition of SiO and the crystallization of HfO₂ layer during the film growth.     

Investigation of silicon-on-sapphire structures by means of TEM

The initial stages of the molecular beam epitaxy (MBE) growth of silicon-on-sapphire (SOS) are investigated via transmission electron microscopy (TEM). The sample preparation procedure is improved to study SOS structures by TEM. It is shown that silicon in the shape of 3D islets can form on a continuous silicon layer grown on sapphire.     

Formal conditions for unambiguous residual strain determination by CBED

The method of residual strain determination using convergent beam electron diffraction (CBED) is attractive because of its good spatial resolution. However, attempts to obtain all six independent strain components from a CBED pattern lead to ambiguous results. This paper contains analysis of the ambiguities based on the complete algorithm for matching experimental and strain-dependent simulated CBED patterns. The strain parameters which are not determinable by the CBED method are identified by examination of the most common goodness-of-fit functions. The indeterminable parameters are confirmed to be the ‘13’ and ‘23’ components and a combination of the diagonal components of the tensor given in the Cartesian systems having the ‘3’ axis parallel to the beam direction. The ambiguity can be eliminated based on multiple diffraction patterns. It is shown that two different patterns may be insufficient to get a unique strain tensor. The ambiguity can be removed only if certain characteristics of the two patterns are different, or if more than two patterns are used.     

Large-deformation analysis in microscopic area using micro-moiré methods with a focused ion beam milling grating

In this study, the focused ion beam (FIB) milling method is applied to fabricate sub-micron grating on TiNi shape memory alloy materials. With self-made FIB milling gratings, scanning electron microscope (SEM) micro-moiré and digital moiré methods are successfully used to measure large deformation of porous TiNi shape memory alloys (SMA) in uni-axial compressive tests. The principles of the SEM micro-moiré method and digital moiré method are introduced, and applied to calculate large strain. The full field deformation around shear bands can be measured precisely. During the investigation, the phenomenon of furcated moiré fringes was found, and a corresponding explanation is given in this paper. The furcated fringes are generated in the locations of combined shear bands where sudden changes of strain occur. Successful results also verify that the FIB milling gratings are suitable for micro-moiré measurement and can generate high quality moiré fringes.     

Analysis of polished polycrystalline diamond using dual beam focused ion beam microscopy

This paper presents a study on polycrystalline diamond (PCD) polished by dynamic friction polishing (DFP) with the aid of advanced dual beam FIB (focused ion beam) microscopy. After disclosing a variety of wear tracks by DFP using electron imaging in combination with the ion channelling effect, a dual beam FIB was successfully employed at wear track sites to specifically create both the large cross-sectional specimen for microanalysis and thin foil for nanoanalysis. The study concluded that the polished PCD subsurface was free from microscale cracking. However, the attached debris layer on the top surface contained metal oxides and non-diamond carbon phase with inhomogeneous distributions of C, Fe, Cr, Ni, Si and O across the layer. An attached layer directly above a diamond grain was composed of essentially amorphous carbon, suggesting that a direct phase transformation from diamond crystalline to amorphous occurred during DFP.     

Integration of correlative Raman microscopy in a dualbeam FIB SEM

We present an integrated confocal Raman microscope in a focused ion beam scanning electron microscope (FIB SEM). The integrated system enables correlative Raman and electron microscopic analysis combined with focused ion beam sample modification on the same sample location. This provides new opportunities, for example the combination of nanometer resolution with Raman advances the analysis of sub‐diffraction‐sized particles. Further direct Raman analysis of FIB engineered samples enables in situ investigation of sample changes. The Raman microscope is an add‐on module to the electron microscope. The optical objective is brought into the sample chamber, and the laser source, and spectrometer are placed in a module attached onto and outside the chamber. We demonstrate the integrated Raman FIB SEM function with several experiments. First, correlative Raman and electron microscopy is used for the investigation of (sub‐)micrometer‐sized crystals. Different crystals are identified with Raman, and in combination with SEM the spectral information is combined with structurally visible polymorphs and particle sizes. Analysis of sample changes made with the ion beam is performed on (1) structures milled in a silicon substrate and (2) after milling with the FIB on an organic polymer. Experiments demonstrate the new capabilities of an integrated correlative Raman–FIB–SEM. Copyright © 2016 John Wiley & Sons, Ltd.     

PECVD分层结构对提高氢化非晶硅TFT迁移率的影响

为了进一步提高氢化非晶硅薄膜晶体管 (a-Si:H TFT) 的场效应电子迁移率, 研究了批量生产条件下对欧姆接触层和栅极绝缘层进行多层 制备, 不同的工艺参数对a-Si:H TFT场效应电子迁移率的影响. 研究表明随着对欧姆接触层 (n⁺层) 分层数的增加, 以及低速生长的栅极绝缘层 (GL层) 和高速生长的栅极绝缘层 (GH 层) 厚度比值提高, a-Si:H TFT的场效应迁移率得到提升. 当n⁺层分层数达到 3层, GL层和GH层厚度比值为4:11 时, 器件的场效应电子迁移率达到0.66 cm²/V·s, 比传统工艺提高了约一倍, 显著改善了a-Si:H TFT 的电学特性, 并在量产线上得到了验证. 关键词： 非晶硅薄膜晶体管 电子迁移率 欧姆接触层 栅极绝缘层     

Accurate measurements of crystal structure factors using a FEG electron microscope

An experimental procedure for the accurate measurement of crystal structure factors is described. This procedure is based on the use of a field emission gun electron microscope equipped with a Gatan Imaging Filter (GIF) system. The slow-scan CCD camera of the GIF system is first characterized and a constrained least squares restoration scheme is used for the deconvolution of the experimentally recorded raw elastic CBED patterns. The procedure has been applied for the accurate measurement of the (111) and (222) structure factors of silicon single crystal. A residual χ² value of 2.87 is achieved and the determined structure factors agree well with previous measurements using X-ray and electron diffraction techniques.     

SOIM新结构的制备及其性能的研究

制备在以SiO2为绝缘埋层的SOI材料上的电子器件存在着自加热问题.为减少自加热效应和满足一些特殊器件/电路的要求，利用多孔硅外延转移技术制备出以二氧化硅和氮化硅为多绝缘埋层的SOI新结构.高分辨率透射电镜和扩展电阻测试结果表明得到的SOIM新结构具有很好的结构和电学性能，退火后的氮化硅埋层为非晶结构.     

Correlation between structural and optical properties of ion beam synthesized β-FeSi2 precipitates in Si

The structural and optical properties of β-FeSi₂ precipitates produced by ion beam synthesis have been investigated by transmission electron microscopy, photoluminescence (PL) analysis and near infrared transmission measurements. The PL spectrum of β-FeSi₂ precipitates in a dislocation free sample has been observed to consist of a sharp line at 1.54 μm and a weak peak at 1.46 μm. Optical transmission measurements showed a direct band gap about 0.8 eV smaller than in continuous β-FeSi₂ film. Calculation of the electronic bands of β-FeSi₂ for different values of the lattice parameters indicates that this reduction can be ascribed to band distortion provided by the lattice strain.     

Methods for atom probe analysis of microgradients in functionally graded cemented carbides

Methods to prepare needle-shaped specimens for atom probe field ion microscopy from near surface regions have been developed. The material used was a cemented carbide with a composition gradient towards the surface, but the method is equally applicable for other materials. The preparation technique involves dimple grinding, electropolishing and focused ion beam (FIB) milling. The use of FIB milling allows for specimen preparation of materials which due to the preferential etching of different phases are difficult to electropolish. The technique also allows for preparation of specimens at well defined depth from the sample surface, selection of phase to be analysed, and to sharpen and re-use already analysed specimens.

Atom probe analyses of the near surface zone region in a gradient sintered WC–Ti(C,N)–TaC–Co cemented carbide are presented.     

TEM/CBED determination of strain in silicon-based submicrometric electronic devices

The convergent beam electron diffraction technique (CBED) of the transmission electron microscopy (TEM) has been employed to determine the strain distribution along a cutline parallel to the padoxide/Si interface in a 0.80 micron wide recessed-LOCOS structure. The values of the components of the strain tensor so obtained have been compared with those computed by two simulator codes. It has been found that both the LOCOS morphology and the strain distribution deduced from TEM images and TEM/CBED patterns, respectively, were in agreement with the simulation results, if some oxidation-related parameters were modified.     

A methodology for the fabrication by FIB of needle-shape specimens around sub-surface features at the nanometre scale

A novel methodology for the preparation by focused ion beam (FIB) of needle-shape specimens in specific sites underneath the sample surface for their study by electron tomography (ET) is proposed. In particular, we demonstrate this methodology for the fabrication of needles containing InAs/InP quantum dots (QDs). The main challenge of this methodology is the location of specific QDs in the FIB equipment, as they are not visible with the secondary electrons detector. In order to overcome this difficulty, a series of marks visible both in conventional transmission electron microscopy and in the FIB are introduced before the preparation of the needles. The conditions for the fabrication by FIB of needles with optimized characteristics for their study by ET are also detailed.     

Growth and structural characterization of semiconducting Ru2Si3

Recent band structure calculations indicate that ruthenium silicide (Ru₂Si₃) is semiconducting with a direct band gap. Electrical measurements lead to a band gap around 0.8 eV which is technologically important for fiber communications. This makes Ru₂Si₃ a promising candidate for silicon based optical devices, namely LEDs. We present first results on the epitaxial growth of ruthenium silicide films on Si(1 0 0) and Si(1 1 1) fabricated by the template method, a special molecular beam epitaxy technique. Orientational relationships on Si(1 1 1) have been determined. We characterized the films by Rutherford Backscattering and Channeling, X-ray diffraction and transmission electron microscopy.     

Quantitative evaluation of process induced strain in MOS transistors by Convergent Beam Electron Diffraction

Convergent Beam Electron Diffraction (CBED) experiments and simulations associated with Finite Element calculations were performed in order to measure strain and stress in a complex device such as periodic MOS transistors with a spatial resolution of about 2 nm and a sensitivity that could reach 50 MPa. A lamella of a thickness of about 475 nm was extracted from the wafer with the transistors by Focus Ion Beam (FIB) and was observed in cross-section in a Transmission Electron Microscope (TEM). When approaching the transistors, the HOLZ lines of the CBED patterns acquired in the silicon substrate, become broader and broader. This HOLZ line broadening, which is due to the stress relaxation in the thin foil, was used to determine quantitatively the strain and stress in the lamella and then in the bulk device. We showed that this procedure could be applied to a complex device. Two parameters, the intrinsic material strains – or equivalently the intrinsic material stresses – in the nickel silicide (NiSi) and nitride (Si₃N₄) layers on the top of the transistors gate, were successfully fitted by trial and error, in the procedure.