Off-axis electron holography of electrostatic potentials in unbiased and reverse biased focused ion beam milled semiconductor devices

Off‐axis electron holography in the transmission electron microscope (TEM) is used to measure two‐dimensional electrostatic potentials in both unbiased and reverse biased silicon specimens that each contain a single p–n junction. All the specimens are prepared for examination in the TEM using focused ion beam (FIB) milling. The in situ electrical biasing experiments make use of a novel specimen geometry, which is based on a combination of cleaving and FIB milling. The design and construction of an electrical biasing holder are described, and the effects of TEM specimen preparation on the electrostatic potential in the specimen, as well as on fringing fields beyond the specimen surface, are assessed.     

Quantitative phase imaging of nanoscale electrostatic and magnetic fields using off-axis electron holography

Off-axis electron holography in the transmission electron microscope is a powerful interferometric technique that enables electrostatic and magnetic fields to be imaged and quantified with spatial resolution often approaching the nanometer scale. Here, we demonstrate the capabilities of the technique for phase quantification at the nanoscale by briefly reviewing some of our recent studies of nanostructured materials. Examples that are described include determination of the electrostatic potential profiles associated with doped Si- and GaAs-based semiconductor devices, measurement of hole accumulation in Ge quantum dots, mapping of polarization fields in III-nitride heterostructures, and observation of the remanent states and reversal mechanisms of lithographically patterned magnetic nanorings. Some issues associated with sample preparation for doped semiconductor heterostructures are also briefly discussed.     

Off-axis and inline electron holography: A quantitative comparison

Capable of quantitatively imaging static magnetic and electric potentials and even strain electron holography is a very versatile and powerful TEM technique. In this paper we compare off-axis electron holography with a recently developed focal series reconstruction algorithm and phase retrieval based on the transport of intensity equation. Based on theoretical considerations and simulations we compare the different techniques with respect to parameters such as the coherence requirements, field of view, resolution, noise properties, and other required experimental conditions.     

Quantitative off-axis electron holography of GaAs p-n junctions prepared by focused ion beam milling

Focused Ion beam (FIB) prepared GaAs p-n junctions have been examined using off-axis electron holography. Initial analysis of the holograms reveals an experimentally determined built-in potential in the junctions that is significantly smaller than predicted from theory. In this paper we show that through combinations of in situ annealing and in situ biasing of the specimens, by varying the intensity of the incident electron beam, and by modifying the FIB operating parameters, we can develop an improved understanding of phenomena such as the electrically 'inactive' thickness and subsequently recover the predicted value of the built-in potential of the junctions.
PACS numbers: 85.30.De     

Dark-field electron holography for the measurement of geometric phase

The genesis, theoretical basis and practical application of the new electron holographic dark-field technique for mapping strain in nanostructures are presented. The development places geometric phase within a unified theoretical framework for phase measurements by electron holography. The total phase of the transmitted and diffracted beams is described as a sum of four contributions: crystalline, electrostatic, magnetic and geometric. Each contribution is outlined briefly and leads to the proposal to measure geometric phase by dark-field electron holography (DFEH). The experimental conditions, phase reconstruction and analysis are detailed for off-axis electron holography using examples from the field of semiconductors. A method for correcting for thickness variations will be proposed and demonstrated using the phase from the corresponding bright-field electron hologram.     

Quantitative measurements of magnetic stray field dynamics of Permalloy particles in a photoemission electron microscopy

By example of a Permalloy particle (40 × 40 μm(2) size, 30 nm thickness) we demonstrate a procedure to quantitatively investigate the dynamics of magnetic stray fields during ultrafast magnetization reversal. The measurements have been performed in a time-resolving photoemission electron microscope using the X-ray magnetic circular dichroism. In the particle under investigation, we have observed a flux-closure-dominated magnetic ground structure, minimizing the magnetic stray field outside the sample. A fast magnetic field pulse introduced changes in the micromagnetic structure accompanied with an incomplete flux closure. As a result, stray fields arise along the edges of domains, which cause a change of contrast and an image deformation of the particles geometry (curvature of its edge). The magnetic stray fields are calculated from a deformation of the X-ray magnetic circular dichroism (XMCD) images taken after the magnetic field pulse in a 1 ns interval. These measurements reveal a decrease of magnetic stray fields with time. An estimate of the lower limit of the domain wall velocity yields about 2 × 10(3) m s(-1).     

On the interpretation of magnetic and electric fields imaged by low-magnification off-axis electron holography

The interpretation of magnetic and electric fields imaged by off-axis electron holography is not always straightforward. We will demonstrate this by some examples of possible misinterpretations which can result from, for example, comparing a hologram with a second one acquired such that the reference wave travelled on the opposite side of the sample, the diffraction of the electron beam at the biprism fibre, not centring an area to the true centre of the sideband when reconstructing the image wave by Fourier optics, quantification of 'magnetic' and 'electric' phases, procedures to separate electric from magnetic phases and dislocations in the interference fringes of the hologram.     

Morphology visualization of irregular shape bacteria by electron holography and tomography

In the current work, irregular morphology of Staphylococcus aureus bacteria has been visualized by phase retrieval employing off‐axis electron holography (EH) and 3D reconstruction electron tomography using high‐angle annular dark field scanning transmission electron microscopy (HAADF‐STEM). Bacteria interacting with gold nanoparticles (AuNP) acquired a shrunken or irregular shape due to air dehydration processing. STEM imaging shows the attachment of AuNP on the surface of cells and suggests an irregular 3D morphology of the specimen. The phase reconstruction demonstrates that off‐axis electron holography can reveal with a single hologram the morphology of the specimen and the distribution of the functionalized AuNPs. In addition, EH reduces significantly the acquisition time and the cumulative radiation damage (in three orders of magnitude) over biological samples in comparison with multiple tilted electron expositions intrinsic to electron tomography, as well as the processing time and the reconstruction artifacts that may arise during tomogram reconstruction.     

Integral hologram using scanning electron micrographs: a new application of display holography

We produced at 43 times 23 cm, 120° integral hologram of a marine protozoan test to investigate the museum exhibit potential of interfacing scanning electron microscopy with commercially available integral holography. We describe here our procedure and some of the strengths and weaknesses of this holographic medium in exhibit situations.     

Method for determination of the displacement field in patterned nanostructures by TEM/CBED analysis of split high-order Laue zone line profiles

A method to extract accurate information on the displacement field distribution from split high‐order Laue zones lines in a convergent‐beam electron diffraction pattern of nanostructures has been developed. Starting from two‐dimensional many beam dynamical simulation of HOLZ patterns, we assembled a recursive procedure to reconstruct the displacement field in the investigated regions of the sample, based on the best fit of a parametrized model. This recursive procedure minimizes the differences between simulated and experimental patterns, taken in strained regions, by comparing the corresponding rocking curves of a number of high‐order Laue zone reflections. Due to its sensitivity to small displacement variations along the electron beam direction, this method is able to discriminate between different models, and can be also used to map a strain field component in the specimen. We tested this method in a series of experimental convergent‐beam electron diffraction patterns, taken in a shallow trench isolation structure. The method presented here is of general validity and, in principle, it can be applied to any sample where not negligible strain gradients along the beam direction are present.     

Dopant profiling of focused ion beam milled semiconductors using off-axis electron holography; reducing artifacts,extending detection limits and reducing the effects of gallium implantation

Focused ion beam (FIB) milling is one of the few specimen preparation techniques that can be used to prepare parallel-sided specimens with nm-scale site specificity for examination using off-axis electron holography in the transmission electron microscope (TEM). However, FIB milling results in the implantation of Ga, the formation of amorphous surface layers and the introduction of defects deep into the specimens. Here we show that these effects can be reduced by lowering the operating voltage of the FIB and by annealing the specimens at low temperature. We also show that the electrically inactive thickness is dependent on both the operating voltage and type of ion used during FIB milling.     

A systematic investigation of the charging effect in scanning electron microscopy for metal nanostructures on insulating substrates

Scanning electron microscopy is perhaps the most important method for investigating and characterizing nanostructures. A well‐known challenge in scanning electron microscopy is the investigation of insulating materials. As insulating materials do not provide a path to ground they accumulate charge, evident as image drift and image distortions. In previous work, we have seen that sample charging in arrays of metal nanoparticles on glass substrates leads to a shrinkage effect, resulting in a measurement error in the nanoparticle dimension of up to 15% at 10 kV and a probe current of 80 ± 10 pA. In order to investigate this effect in detail, we have fabricated metal nanostructures on insulating borosilicate glass using electron beam lithography. Electron beam lithography allows us to tailor the design of our metal nanostructures and the area coverage. The measurements are carried out using two commonly available secondary electron detectors in scanning electron microscopes, namely, an InLens‐ and an Everhart–Thornley detector. We identify and discriminate several contributions to the effect by varying microscope settings, including the size of the aperture, the beam current, the working distance and the acceleration voltage. We image metal nanostructures of various sizes and geometries, investigating the influence of scan‐direction of the electron beam and secondary electron detector used for imaging. The relative measurement error, which we measure as high as 20% for some settings, is found to depend on the acceleration voltage and the type of secondary electron detector used for imaging. In particular, the Everhart–Thornley detectors lower sensitivity to SE₁ electrons increase the magnitude of the shrinkage of up to 10% relative to the InLens measurements. Finally, a method for estimating charge balance in insulating samples is presented.     

TEM, HRTEM, electron holography and electron tomography studies of γ' and γ" nanoparticles in Inconel 718 superalloy

The aim of the study was the identification of γ' and γ" strengthening precipitates in a commercial nickel-base superalloy Inconel 718 (Ni-19Fe-18Cr-5Nb-3Mo-1Ti-0.5Al-0.04C, wt %) using TEM dark-field, HRTEM, electron holography and electron tomography imaging. To identify γ' and γ" nanoparticles unambiguously, a systematic analysis of experimental and theoretical diffraction patterns were performed. Using HRTEM method it was possible to analyse small areas of precipitates appearance. Electron holography and electron tomography techniques show new possibilities of visualization of γ' and γ" nanoparticles. The analysis by means of different complementary TEM methods showed that γ" particles exhibit a shape of thin plates, while γ' phase precipitates are almost spherical.     

In situ electron beam induced current measurements of the local thickness in semiconductor devices

A quantitative electron beam induced current method is shown, applicable in situ for electron beam current measurement on a semiconductor sample without the need for a Faraday cup. As a validation technique, the measurement of top overlayer thickness in the semiconductor structure was chosen for two reasons. First, the measured thickness is easily verified using the same electron microscope in the secondary electron mode by measuring the layer thickness at the layer edges. Second, the measurement of a layer thickness and its local variations constitute an important issue in semiconductor processing and characterization. The proposed method is used in the planar view of the sample, and also for locations far from the layer edges. Quasi‐three‐dimensional maps of the thickness spatial distribution are presented.     

高速漏磁检测饱和场建立过程及影响因素研究

在高速漏磁检测过程中,随着检测速度增加,有效磁化时间减少,导致被测构件饱和场无法建立,影响磁化效果。采用方波激励模拟外磁场瞬变情况,建立瞬磁场作用下钢管内部磁场响应模型,对钢管内部饱和场建立过程及影响因素进行研究;分析高速漏磁检测时缺陷漏磁场特征,利用有限元方法计算磁场强度和钢管材质对磁化滞后时间及缺陷检测的影响;设计高速漏磁检测实验平台,对不同运行速度和不同外磁场强度下钢管缺陷进行实验研究。结果表明,外磁场瞬变时,钢管内壁中心磁场明显滞后于外磁场,钢管内部饱和场建立时间与磁场强度和材料电导率有关,提高外磁场强度,可快速建立饱和场,减弱磁化滞后时间和涡流效应影响,提升缺陷检测效果和漏磁检测速度,实验结果和理论分析具有很好的一致性。     

Defining the radiation chemistry during liquid cell electron microscopy to enable visualization of nanomaterial growth and degradation dynamics

We present a critical review of methods for defining the chemical environment during liquid cell electron microscopy investigation of electron beam induced nanomaterial growth and degradation. We draw from the radiation chemistry and liquid cell electron microscopy literature to present solution chemistry and electron beam–based methods for selecting the radiolysis products formed and their relative amount during electron irradiation of liquid media in a transmission electron microscope. We outline various methods for establishing net oxidizing or net reducing reaction environments and propose solvents with minimal overall production of radicals under the electron beam. Exemplary liquid cell electron microscopy experiments in the fields of nanoparticle nucleation, growth, and degradation along with recommendations for best practices and experimental parameters are reported. We expect this review will provide researchers with a useful toolkit for designing general chemistry and materials science liquid cell electron microscopy experiments by ‘directing’ the effect of the electron beam to understand fundamental mechanisms of dynamic nanoscale processes as well as minimizing radiation damage to samples.     

Measurement of magnetic domain wall width using energy-filtered Fresnel images

Magnetic domain walls in Nd₂Fe₁₄B have been examined using a series of energy‐filtered Fresnel images in the field emission gun transmission electron microscope (FEGTEM). We describe the changes in the intensity distribution of the convergent wall image as a function of defocus, foil thickness and domain wall width. The effect of tilted domain walls and beam convergence on the fringe pattern is also discussed. A comparison of the experimental intensity profile with that from simulations allows the domain wall width to be determined. Measurement of very narrow walls is made possible only by using a relatively thick foil, which necessitates energy‐filtering to allow quantitative comparison with simulations. The magnetic domain wall width in Nd₂Fe₁₄B was found to be 3 ± 2 nm.     

Some theoretical aspects of type-1 magnetic contrast in the scanning electron microscope

Type-1 magnetic contrast can be obtained in the secondary electron (SE) image in the SEM from a sample having an external magnetic field if the SE detector is directionally sensitive. Gauss' theorem is applied to show that the normal component of induction at the surface of the sample can be calculated from the measured spatial derivative(s) of the SE difference-signal. A method is given in this paper for calculating the three components of the induction in the entire volume above the sample surface. Reasons are given for believing that type-1 magnetic contrast is limited in spatial resolution by the fluxon unit.