Imaging flux vortices in type II superconductors with a commercial transmission electron microscope

Flux vortices in superconductors can be imaged using transmission electron microscopy because the electron beam is deflected by the magnetic flux associated with the vortices. This technique has a better spatial and temporal resolution than many other imaging techniques and is sensitive to the magnetic flux density within each vortex, not simply the fields at the sample surface. Despite these advantages, only two groups have successfully employed the technique using specially adapted instruments. Here we demonstrate that vortices can be imaged with a modern, commercial transmission electron microscope operating at 300 kV equipped with a field emission gun, Lorentz lens and a liquid helium cooled sample holder. We introduce superconductivity for non-specialists and discuss techniques for simulating and optimising images of flux vortices. Sample preparation is discussed in detail as the main difficulty with the technique is the requirement for samples with very large (>10 μm), flat areas so that the image is not dominated by diffraction contrast. We have imaged vortices in superconducting Bi₂Sr₂CaCu₂O_8−δ and use correlation functions to investigate the ordered arrangements they adopt as a function of applied magnetic field.     

Sample preparation and microscopical investigation techniques for metal and ceramics containing graphite and graphene‐like layered particles

Scanning electron microscopy (SEM) techniques are widely used in microstructural investigations of materials since it can provide surface morphology, topography, and chemical information. However, it is important to use correct imaging and sample preparation techniques to reveal the microstructures of materials composed of components with different polishing characteristics such as grey cast iron, graphene platelets (GPLs)‐added SiAlON composite, SiC and B₄C ceramics containing graphite or graphene‐like layered particles. In this study, all microstructural details of gray cast iron were successfully revealed by using argon ion beam milling as an alternative to the standard sample preparation method for cast irons, that is, mechanical polishing followed by chemical etching. The in‐lens secondary electron (I‐L‐SE) image was clearly displayed on the surface details of the graphites that could not be revealed by backscattered electron (BSE) and Everhart–Thornley secondary electron (E‐T SE) images. Mechanical polishing leads to pull‐out of GPLs from SiAlON surface, whereas argon ion beam milling preserved the GPLs and resulted in smooth surface. Grain and grain boundaries of polycrystalline SiC and B₄C were easily revealed by using I‐L SE image in the SEM after only mechanical polishing without any etching process. While the BSE and E‐T SE images did not clearly show the residual graphites in the microstructure, their distribution in the B₄C matrix was fully revealed in the I‐L SE image.     

Development of high-resolution field emission scanning electron microscopy with multifunctions for chargeless observation of nonconducting surface

We have developed a fully digital field emission scanning electron microscope (FE-SEM) with multifunctions to compensate the charging up of nonconducting surfaces. High-voltage observation, minimum electron dose, variable scanning speed, averaging, integration, tuning of surface potential, and cyclotron movements of secondary electrons have been achieved. This FE-SEM was successfully applied to observe resist, diatomaceous earth, aluminum oxide, and zeolite surfaces. The accelerating voltage is changeable in a range from 0.5 to 30 kV, and the probe current on the sample can be varied from 2×10^-9 to l×10^-13A to supply optimum electron dose. By using a snorkel- type, strongly excited objective lens (OL) immersing the samples in the magnetic field, the secondary electrons are extracted from the sample. For guiding electrons into the built-in lens-type secondary electron detector (SED), newly developed accelerating and retarding electrodes are installed in the OL to tune the surface potential. Furthermore, this FE-SEM can select 10 scan speeds, and the averaging and integration of secondary electron image signals are possible under every selected scan speed.     

Caustic imaging of gallium droplets using mirror electron microscopy

We discuss a new interpretation of mirror electron microscopy (MEM) images, whereby electric field distortions caused by surface topography and/or potential variations are sufficiently large to create caustics in the image contrast. Using a ray-based trajectory method, we consider how a family of rays overlaps to create caustics in the vicinity of the imaging plane of the magnetic objective lens. Such image caustics contain useful information on the surface topography and/or potential, and can be directly related to surface features. Specifically we show how a through-focus series of MEM images can be used to extract the contact angle of a Ga droplet on a GaAs (001) surface.     

Successful application of spatial difference technique to electron energy-loss spectroscopy studies of Mo/SrTiO3 interfaces

The electron energy‐loss near‐edge structure (ELNES) of Mo/SrTiO₃ interfaces has been studied using high spatial resolution electron energy‐loss spectroscopy (EELS) in a dedicated scanning transmission electron microscope. Thin films of Mo with a thickness of 50 nm were grown on (001)‐orientated SrTiO₃ surfaces by molecular beam epitaxy at 600 °C. High‐resolution transmission electron microscopy revealed that the interfaces were atomically abrupt with the (110)_Mo plane parallel to the substrate surface. Ti‐L_2,3 (～460 eV), O‐K (～530 eV), Sr‐L_2,3 (～1950 eV) and Mo‐L_2,3 (～2500 eV) absorption edges were acquired by using the Gatan Enfina parallel EELS system with a CCD detector. The interface‐specific components of the ELNES were extracted by employing the spatial difference method. The interfacial Ti‐L_2,3 edge shifted to lower energy values and the splitting due to crystal field became less pronounced compared to bulk SrTiO₃, which indicated that the Ti atoms at the interface were in a reduced oxidation state and that the symmetry of the TiO₆ octahedra was disturbed. No interfacial Sr‐L_2,3 edge was observed, which may demonstrate that Sr atoms do not participate in the interfacial bonding. An evident interface‐specific O‐K edge was found, which differs from that of the bulk in both position (0.8 ± 0.2 eV positive shift) and shape. In addition, a positive shift (0.9 ± 0.3 eV) occurred for the interfacial Mo‐L_2,3, revealing an oxidized state of Mo at the interface. Our results indicated that at the interface SrTiO₃ was terminated with TiO₂. The validity of the spatial difference technique is discussed and examined by introducing subchannel drift intentionally.     

Material contrast in SEM: Fermi energy and work function effects

‘Is it possible to assign various grey levels of a scanning electron microscope (SEM) image to different components of a given sample? Among other instrumental effects, the answer is not only a function of the respective secondary electron emission (SEE) yields of the components, δ, but also of the angular fraction of the secondary electrons (SE)s being collected, k_α and of a possible voltage contact effect between sample and detector, k_?. Expressed as a function of E_F, Fermi energy, and ?, work function of the components of interest, equations of spectral, (∂δ/∂E_k), and angular, (∂δ/∂α) distributions of the emitted SEs permit to evaluate k_α and k_? for Au and Si. It has been established that collected SE spectra, ∂δ_α/∂E_k, are distorted with respect to the emitted and fraction k_α is material dependent for a solid angle of detection Ω° less than 2π (or maximum semi-apex angle α_max<90°) In particular, for coaxial detections around the normal incident beam the detected fraction of SEs from Au, k_α(Au), is slightly larger than that for Si, k_α(Si). For simple geometries in the vacuum gap, similar investigations show that parameter k_φ is also larger for gold than for n-doped Si as well as for p-doped Si with respect to n-doped Si. Then Au is always quite brighter than n-doped Si in the SEM images while a doping contrast, C, due to a work function effect may reach ∼15% for a Si p/n junction with N_p∼10¹⁶ and N_n∼10¹⁵ cm⁻³. The present analysis may be extended to some metals such as Ag, Cu, Pb, Pd, Pt, and Zn that are expected to appear brighter than Si(n) and Ge in the SEM images.     

The imaging mechanism of single-walled carbon nanotubes on Si/SiO₂ wafer in scanning electron microscopy

Scanning electron microscopy imaging of both suspended single‐walled carbon nanotubes (SWNTs) and contacted SWNTs with Si/SiO₂ substrate has been studied in this paper. The voltage contrast has been investigated by supplying external electric field around the samples. The results show that the image contrast of SWNTs attributes to both voltage contrast from the area surrounding SWNTs (tens of nanometres in both sides of the SWNTs) and electron beam induced emission from SWNTs themselves under low primary beam energy. Under high primary beam energy, however, EBIE dominates the image contrast due to the fact that the voltage contrast caused by implanted charges of the SiO₂ layer is weakened. Imaging under the primary beam energy lower than 1 keV offers widened diameter of SWNTs, which promises that the SWNTs are observable at very low magnification (lower than 100×). At a larger magnification, however, imaging under the primary beam energy higher than 10 keV can display more realistic images of the SWNTs. In addition, an appropriate external electric field can improve the images.     

Combining Ar ion milling with FIB lift-out techniques to prepare high quality site-specific TEM samples

Focused ion beam (FIB) techniques can prepare site‐specific transmission electron microscopy (TEM) cross‐section samples very quickly but they suffer from beam damage by the high energy Ga⁺ ion beam. An amorphous layer about 20–30 nm thick on each side of the TEM lamella and the supporting carbon film makes FIB‐prepared samples inferior to the traditional Ar⁺ thinned samples for some investigations such as high resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS). We have developed techniques to combine broad argon ion milling with focused ion beam lift‐out methods to prepare high‐quality site‐specific TEM cross‐section samples. Site‐specific TEM cross‐sections were prepared by FIB and lifted out using a Narishige micromanipulator onto a half copper‐grid coated with carbon film. Pt deposition by FIB was used to bond the lamellae to the Cu grid, then the coating carbon film was removed and the sample on the bare Cu grid was polished by the usual broad beam Ar⁺ milling. By doing so, the thickness of the surface amorphous layers is reduced substantially and the sample quality for TEM observation is as good as the traditional Ar⁺ milled 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.     

Electron optical property of a charged foil,observed with a transmitted electron detector device in an SEM

Experimental evidence is presented for the electron optical behaviour of a charged foil area, using the transmitted electron detection device of the scanning electron microscope JSM 50 A (JEOL). The primary electron beam scanning a thin pioloform foil on the one hand produces a charged foil region which on the other hand acts as an electron lens to the primary and scattered electrons. Scanning electron microscopical investigations of air particulates in the submicron size range can be eased by using a transmitted electron detection device both of the bright and dark field operation mode. The image contrast thus may be improved by orders of magnitude, also allowing on line operation of an image analysis system. Using a special preparation technique, depositing the particles on a thin supporting foil which is also used for LAMMA analysis – Wieser et al. 1980, the x-ray spectra of single particles provided by an energy dispersive x-ray spectrometer may be quantitatively interpreted on the basis of the peak-to-background method (Statham and Pawley 1978, Small et al. 1979). Figure 1 shows a schematic of the transmission detector device of the JSM 50 A when operated in the dark field mode. Geometrical dimensions and apertures also are given in Fig. 1. The dark field diaphragm (DFD) on the optical axis of the microscope blocks all electrons (primary electrons and scattered electrons) within an angle of about 10^?2 rad from contributing to the video signal. As long as magnifications above about 350 × are used the primary electron beam hits the DFD thus yielding a transmission scanning electron micrograph in dark field mode. Below this limit or above the corresponding maximal scanning angle (about 7 × 10^?3 rad) of the primary electron beam the rim of the DFD becomes visible in the displayed image as shown in Fig. 2a. At the same magnification Figure 2b shows the sharpened contours of the DFD as obtained by focussing the primary electron beam to the plane of the DFD by lowering the objective lens excitation. By means of the thin bar attached to the DFD (left hand upper corner of Fig. 2b) the DFD may be centered to the optical axis or exchanged to the bright field aperture. Looking to the circular center of Fig. 2a, we recognize the black grid bars and a few black particles whereas the supporting foil looks bright. No video signal can be obtained, because both the grid bars, and to a lesser extent the particles, are not transparent to the primary electrons of 15 keV energy. On the other hand all electrons scattered by the thin foil to an angle of more than 10^?2 rad are seen by the scintillator and hence accumulate a measurable video signal: This is also favoured by the large solid angle outside the DFD, which is about 30 times the solid angle of the DFD itself.     

Specimen charging and detection of signal from non-conductors in a cathode lens-equipped scanning electron microscope

This paper concerns the problems connected with the observation of a nonconductive specimen in a scanning electron microscope (SEM) when incident electrons create a surface charge and a corresponding electric field. The special configuration of the cathode lens enables one to control the landing energy of primary electrons via the specimen bias. In the cathode lens, the accelerating electric field at the surface of the specimen combines itself with that of the surface charge in influencing the trajectories of the signal electrons and hence the detected signal level and the possible recapturing of slow secondaries. Recaptured electrons reduce the ultimate positive surface potential, which arises when working below the higher critical energy of electron impact. Computer simulations of electron trajectories were performed for the typical cathode lens configuration and for a model specimen characterized by emission yields similar to those for glass. The simulations brought an extensive set of data about the trajectories of both secondary and backscattered electrons. Furthermore, the data were processed in order to assess the charge balance between the emitted and recaptured electrons as well as the collection efficiency of the detector. The results include values of the ultimate positive surface potential and the detected signal level, both in dependence on the initial energy of the electron impact and the size of the field of view. Finally, the method for the determination of critical energy is reevaluated. This is based on the measurement of the time dependence of the detected signal.     

Do SEII Electrons Really Degrade SEM Image Quality?

Generally, in scanning electron microscopy (SEM) imaging, it is desirable that a high‐resolution image be composed mainly of those secondary electrons (SEs) generated by the primary electron beam, denoted SE_I. However, in conventional SEM imaging, other, often unwanted, signal components consisting of backscattered electrons (BSEs), and their associated SEs, denoted SE_II, are present; these signal components contribute a random background signal that degrades contrast, and therefore signal‐to‐noise ratio and resolution. Ideally, the highest resolution SEM image would consist only of the SE_I component. In SEMs that use conventional pinhole lenses and their associated Everhart–Thornley detectors, the image is composed of several components, including SE_I, SE_II, and some BSE, depending on the geometry of the detector. Modern snorkel lens systems eliminate the BSEs, but not the SE_IIs. We present a microfabricated diaphragm for minimizing the unwanted SE_II signal components. We present evidence of improved imaging using a microlithographically generated pattern of Au, about 500 nm thick, that blocks most of the undesired signal components, leaving an image composed mostly of SE_Is. We refer to this structure as a “spatial backscatter diaphragm.” SCANNING 35:1‐6, 2013. © 2012 Wiley Periodicals, Inc.     

A new aberration-corrected,energy-filtered LEEM/PEEM instrument. I. Principles and design

We describe a new design for an aberration-corrected low energy electron microscope (LEEM) and photo electron emission microscope (PEEM), equipped with an in-line electron energy filter. The chromatic and spherical aberrations of the objective lens are corrected with an electrostatic electron mirror that provides independent control over the chromatic and spherical aberration coefficients C_c and C₃, as well as the mirror focal length, to match and correct the aberrations of the objective lens. For LEEM (PEEM) the theoretical resolution is calculated to be ∼1.5 nm (∼4 nm). Unlike previous designs, this instrument makes use of two magnetic prism arrays to guide the electron beam from the sample to the electron mirror, removing chromatic dispersion in front of the mirror by symmetry. The aberration correction optics was retrofitted to an uncorrected instrument with a base resolution of 4.1 nm in LEEM. Initial results in LEEM show an improvement in resolution to ∼2 nm.     

Contrast in the transmission mode of a low-voltage scanning electron microscope

The contrast thicknesses (x_k) of thin carbon and platinum films have been measured in the transmission mode of a low-voltage scanning electron microscope for apertures of 40 and 100 mrad and electron energies (E) between 1 and 30 keV. The measured values overlap with those previously measured for E (≥ 17keV) in a transmission electron microscope. Differences in the decrease of x_k with decreasing E between carbon and platinum agree with Wentzel-Kramer-Brillouin calculations of the elastic cross-sections. Knowing the value of x_k allows the exponential decrease ∝ exp(—x/x_k) in transmission with increasing mass-thickness (x = ρt) of the specimen and the increasing gain of contrast for stained biological sections with decreasing electron energy to be calculated for brightfield and darkfield modes.     

Electron and ion imaging of gland cells using the FIB/SEM system

The FIB/SEM system was satisfactorily used for scanning ion (SIM) and scanning electron microscopy (SEM) of gland epithelial cells of a terrestrial isopod Porcellio scaber (Isopoda, Crustacea). The interior of cells was exposed by site-specific in situ focused ion beam (FIB) milling. Scanning ion (SI) imaging was an adequate substitution for scanning electron (SE) imaging when charging rendered SE imaging impossible. No significant differences in resolution between the SI and SE images were observed. The contrast on both the SI and SE images is a topographic. The consequences of SI imaging are, among others, introduction of Ga⁺ ions on/into the samples and destruction of the imaged surface. These two characteristics of SI imaging can be used advantageously. Introduction of Ga⁺ ions onto the specimen neutralizes the charge effect in the subsequent SE imaging. In addition, the destructive nature of SI imaging can be used as a tool for the gradual removal of the exposed layer of the imaged surface, uncovering the structures lying beneath. Alternative SEM and SIM in combination with site-specific in situ FIB sample sectioning made it possible to image the submicrometre structures of gland epithelium cells with reproducibility, repeatability and in the same range of magnifications as in transmission electron microscopy (TEM). At the present state of technology, ultrastructural elements imaged by the FIB/SEM system cannot be directly identified by comparison with TEM images.     

一种基于金阴极MCP的冷阴极电子源的研制

采用深紫外光子激发金阴极产生的冷阴极电子源具有诸多优点，将其应用于电子轰击离子源(EI)有助于获得高质量的离子源。本实验分别采用在JGS2石英玻璃上蒸镀金薄膜构成透射式金阴极、在微通道板(MCP)输入面蒸镀金薄膜构成反射式金阴极，将二者以不同的组合方式装配在一起，通过施加不同的间隙电压，从而获得较大范围的电子流输出，研制出电子束流可调(10^-11～10^-5 A)、均匀分布(非均匀度6.5%)的稳定输出(稳定工作时间大于5 h)电子源，有望在高质量EI源中得到推广和应用。     

Electron Beam Induced Growth of Silver Nanoparticles

An electron beam inducing method for sprouting large quantities of silver nanoparticles on the surface of silver chloride particles is reported. The electron beam driven process was characterized by time‐dependent scanning electron microscope (SEM) and energy dispersive spectrum (EDS), allowing for observing several key intermediates in and characteristics of the growth process. Theoretical calculation coupled with experimental observation demonstrated that the growth of silver nanoparticles was mostly related to the current density of electron beam. Decomposition of the silver chloride on the surface of sample was under electron beam irradiation resulted in silver nanoparticles and chlorine. This phenomenon could be useful in developing a novel mechanism for preparation of nanostructures and proposing a reference to avoid image distortion during the characterization of silver compounds under SEM. SCANNING 35: 69‐74, 2013. © 2012 Wiley Periodicals, Inc.