Low-temperature SEM studies of beam-induced voltage contrast in YBCO thin films

Beam-induced voltage contrast has been demonstrated in a superconducting thin film of YBa₂Cu₃O_7-x (YBCO) grown on MgO. Copper-rich inclusions in the material contribute to spatially varying resistive behaviour but do not account for all the observed details. A new method of scanning in which the beam was moved away from the sample between each data acquisition point was found to increase the resolution by limiting thermalisation, to allow imaging of resistive features as small as 0.5 μm. Direct comparisons of beam-induced contrast and micro-structure at 9000 times magnification were possible using simultaneous image acquisition via a purpose-built image store. Mounting a preamplifier within the scanning electron microscope chamber, to give a variable overall gain of 1000–100,000, was also found to significantly improve the signal-to-noise ratio.     

Diffraction patterns of artificial two-dimensional crystals synthesized in situ in an environmental scanning transmission electron microscope

In this study, we demonstrated the use of electron‐beam‐induced deposition for synthesis of artificial two‐dimensional crystals with an in situ scanning transmission electron microscope. The structures were deposited from W(CO)₆ in an environmental scanning transmission electron microscope on a 30‐nm‐thick Si₃N₄ substrate. We present clear electron beam diffraction patterns taken from those structures. The distance between the diffraction peaks corresponded to the dot spacing in the self‐made surface crystal. We propose using these arrays of dots as anchor points for making artificial crystals for diffraction analysis of weakly scattering or beam‐sensitive molecules such as proteins.     

Field emission studies on electrochemically synthesized ZnO nanowires

Nanocrystalline zinc oxide (ZnO) films were synthesized using cathodic reduction of Zn foil in aqueous electrolyte of different molar concentrations containing ZnCl₂ and H₂O₂, followed by annealing at 400 °C in air. An X-ray diffractometer (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM) were used for characterization. The XRD patterns exhibited a set of well-defined diffraction peaks corresponding to the wurtzite phase of ZnO. SEM and TEM images clearly revealed the formation of randomly oriented ZnO nanowires having lengths of several microns and diameters less than 100 nm. From the field emission studies, the threshold field values, required to draw emission current density of ∼1 μA/cm² were found to be 1.44, 1.36 and 1.5 V/μm for nanowires synthesized using 0.002, 0.004 and 0.016 M electrolyte concentrations, respectively. All Folwer–Nordheim (F–N) plots showed non-linear behavior indicating semiconducting nature of the emitters. The ZnO nanowires exhibited good emission current stability at the pre-set value of ∼10 μA over a duration of 6 h. The simplicity of the synthesis route coupled with the promising emission properties made the electrochemically synthesized ZnO nanowires a suitable candidate for high-current density applications.     

Quantitative determination of electric field strengths within dynamically operated devices using EBIC analysis in the SEM

Although electron beam-induced current (EBIC) technique was invented in the seventies, it is still a powerful technique for failure analysis and reliability investigations of modern materials and devices. Time-resolved and stroboscopic microanalyses using sampling Fourier components decomposed by modulated charge carrier excitation are introduced. Quantitative determination of electric field strengths within dynamically operated devices in the scanning electron microscope (SEM) will be demonstrated. This technique allows investigations of diffusion and drift processes and of variations of electric field distributions inside active devices.     

Experimental simulation of phosphites additives tribochemical reactions by gas phase lubrication

Abstract

Tribochemical reactions of phosphites additives on steel surface have been simulated by gas phase lubrication. Trimethylphosphite (TMPi), P(OCH₃)₃, has been used as model molecule for phosphites additives. It has been introduced under gas phase up to 5 hPa in a new tribometer dedicated to gas phase lubrication. Friction tests have been carried out at ambient temperature and 100°C. Chemical analyses by X-ray photoelectron spectroscopy and by Auger electron spectroscopy have been conducted inside and outside of the track. Two kinds of analysis have been carried out: ex situ and in situ surface analyses after tribological test. Indeed, a new environmentally controlled tribometer allows friction test then accurate analyses without air exposure of the formed tribofilm. Tribotests conducted under TMPi gas phase show a reduction of friction coefficient until 0˙2 instead of 1˙4 under high vacuum. Jointly, formation of tribofilm has been confirmed by optical microscopy and ex situ chemical analysis. Comparison between analyses performed inside and outside of the wear scar indicates that the friction induces the formation of phosphide compound that could reduce friction. Moreover analyses show the formation of methoxy group (CH₃O) and carbonate originally from the decomposition of TMPi under friction into H₂ and CO. In situ analyses clearly show the importance to investigate an uncontaminated tribofilm in order to obtain a better characterisation of it and then a better comprehension of the tribochemical mechanisms.     

Local phase measurements of light in a one-dimensional photonic crystal

For the first time the local optical phase evolution in and around a small, one-dimensional photonic crystal has been visualized with a heterodyne interferometric photon scanning tunnelling microscope. The measurements show an exponential decay of the optical intensity inside the crystal, which consists of a periodic array of subwavelength air rods fabricated in a conventional ridge waveguide. In addition it is found that the introduction of the air rods has a counterintuitive effect on the phase development inside the structure. The heterodyne detection scheme allows the detection of low-intensity scattered waves. In the vicinity of the scattering air rods phase singularities are found with a topological charge of plus or minus one.     

A study of recrystallization in single-phase aluminium using in-situ annealing in the scanning electron microscope

In‐situ annealing experiments were performed in the scanning electron microscope on a single‐phase Al?0.13Mg alloy cold rolled to different strain levels. Once the validity of the technique had been verified by comparison of the recrystallization kinetics and final grain size with bulk annealed samples, the method was used in combination with electron back‐scattered diffraction (EBSD) to study the potential mechanisms for recrystallization in this alloy. During annealing of material rolled to moderate strains (?_t < 0.7), the primary mechanism was strain‐induced boundary migration (SIBM). In material rolled to higher true strains (?_t > 1.4), recrystallization occurred extensively along pre‐existing cube bands and EBSD measurements showed that the mean size of cells within the cube bands was larger than for all other orientations measured, suggesting a size advantage was responsible for the strengthening of cube texture during recrystallization. SIBM was shown to occur concurrently with the nucleation along cube bands but this contributed a lower proportion of nucleation sites during recrystallization.     

Scanning tunneling microscope combined with scanning electron microscope

A scanning tunneling microscope (STM) has been installed in a usual scanning electron microscope (SEM) with a vacuum of 10⁻⁶ Torr. The STM image is displayed on the cathode ray tube of the SEM, 512 × 512 pixels, with a scanning rate of 80 s/picture. The spatial resolution of the STM is about 1 Å, while that of the SEM is several tens of ångströms. The combined scanning microscope covers a wide magnification range from 10 to 10⁷, where STM covers the high magnification region from 10⁵ to 10⁷.     

Comparative study on tribology and microhardness of laser synthesized Ti-Al2O3/Zn coatings on Ti-6Al-4V alloy

ABSTRACT

The study of laser cladding of 90Ti-10Al₂O₃, 90Ti-8Al₂O₃-2Zn and 90Ti-4Al₂O₃-6Zn coatings onto Ti-6Al-4V alloy, with intention to produce defect-less, high microhardness and wear resistant coating was carried out. The coatings were deposited onto Ti-6Al-4V alloy at 900 W laser power and 0.6 m/min laser scan speed. Microstructures and phase constituents of the developed coatings were investigated by using a scanning electron microscope (SEM) and X-ray diffractometer correspondingly. Vickers microhardness tester and pin-on-disk tribometer were employed to characterize microhardness and wear behaviour of the Ti-Al₂O₃/Zn coatings respectively. SEM was also used to examine the worn track. It was observed that 90Ti-10Al₂O₃ coating yielded optimal microhardness along with maximal wear resistance in comparison to the other coatings and Ti-6Al-4V alloy. It has been established that laser cladding of Ti-Al₂O₃ coating with Zn contents on Ti-6Al-4V alloy alleviates the formation of cracks, however, microhardness and wear properties are negatively affected.     

A spectroscopic study of some high-temperature superconductors using a low-temperature STM

We used a scanning tunnelling microscope (STM) to measure both the tunnel current, I, and the dynamic conductance, dI/dV, at 4·2 K for a number of high-transition temperature oxide superconductors. Large spatial variations in the tunnelling characteristics are observed. At low tunnel resistances, all samples show evidence of single electron tunnelling and incremental charging. Results on BiSrCaCu₂O_x show the coexistence of charging with Josephson coupling between grains within the sample. Results on both the Bi sample and a single crystal of YBa₂Cu₃O_6·5+x reveal possible energy gap (2A) values of 17 and 20 meV, respectively. A very sharp 5 meV gap, observed in ceramic samples of YBa₂Cu₃O_6·5+x and Y_0·5Al_0·05Ba₂Cu₃O_6·5+x, may indicate the presence of a lower temperature phase in these samples.     

Properties and structures of Co-based metallic glasses

A fundamental study on Co-based metallic glasses has been conducted. The study focused on understanding the changes of the properties and structures of an Fe-B-Si glass as a function of Co, Co-Ni, Co-Mn, and Co-Ni-Mo additions. The separate addition of Co, Co-Ni, Co-Mn, and Co-Ni-Mo elements was successful in such a way that four new metallic glasses were produced. The compositions of the new glasses are Fe₆₆Co₁₈B₁₅Si₁, Co₆₆Fe₄B₁₄Si₁₅, Co₇₆Fe₂Mn₄B₁₂Si₆, and Co₆₉Fe₄Mo₂B₁₂Si₁₂. Consequently, an evaluation of the physical and magnetic properties was determined. Furthermore, the internal and surface structures of the glasses have been characterized by a transmission electron microscope (TEM), and a scanning tunneling microscope (STM), respectively. A comparison between the internal and surface structures of the glasses was carried out on both amorphous and crystalline forms. As a result, a correlation between the properties and structures of the glasses is established.     

Electron microscopic studies of CuS nanocrystals formed in Langmuir-Blodgett films

The morphology and structure of CuS crystals formed during sulfidation of copper behenate films obtained by the Langmuir-Blodgett (LB) method have been studied using high resolution electron microscopy. The average size of these crystals is about 3 nm and increases by a factor of approximately 2.2 after annealing at a temperature of 150 °C or above. Analysis of interplanar distances has shown that in the range of annealing temperatures of 150–200 °C, CuS nanocrystals have a P6_3/mmc hexagonal crystal lattice with parameters a = 0.38 nm and c = 1.64 nm. At annealing temperatures of 250 °C or above, the Cu₂S crystalline phase begins to form, in addition to CuS nanocrystals. The proportion of this phase increases with increasing annealing temperature. Cu₂S nanocrystals have a hexagonal crystal lattice type with the P6_3/mmc spatial group and unit cell parameters a = 0.39 nm and c = 0.68 nm. Quantitative evaluation of copper and sulfur in individual CuS and Cu₂S nanocrystals was performed by local analysis of characteristic X-ray spectra.     

SEM characterization of silicon nanostructures: can we meet the challenge?

The current semiconductor technology road map for device scaling champions a 4.5 nm gate length in production by 2022. The scanning electron microscope (SEM) as applied to critical dimensions (CD) metrology and associated characterization modes such as electron beam-induced current and cathodoluminescence (CL) has proved to be a workhorse for the semiconductor industry during the microelectronics era. We review some of the challenges facing these techniques in light of the silicon nanotechnology road map. We present some new results using voltage contrast imaging and CL spectroscopy of top-down fabricated silicon nanopillar/nanowires (<100 nm diameter), which highlight the visualization challenge. However, both techniques offer the promise of providing process characterization on the 10-20 nm scale with existing technology. Visualization at the 1 nm scale with these techniques may have to wait for aberration-corrected SEM to become more widely available. Basic secondary electron imaging and CD applications may be separately addressed by the He-ion microscope.     

Electron-beam-induced reduction of Fe in iron phosphate dihydrate,ferrihydrite, haemosiderin and ferritin as revealed by electron energy-loss spectroscopy

The effect of high-energy electron irradiation on ferritin/haemosiderin cores (in an iron-overloaded human liver biopsy), its mineral analogue; six-line ferrihydrite (6LFh), and iron phosphate dihydrate (which has similar octahedral ferric iron to oxygen coordination to that in ferrihydrite and ferritin/haemosiderin cores) has been investigated using electron energy-loss spectroscopy (EELS). Fe L_2,3-ionisation edges were recorded on two types of electron microscope: a 200 keV transmission electron microscope (TEM) and a 100 keV scanning transmission electron microscope (STEM), in order to investigate the damage mechanisms in operation and to establish a methodology for minimum specimen alteration during analytical electron microscopic characterisation. A specimen damage mechanism dominated by radiolysis that results in the preferential loss of iron co-ordinating ligands (O, OH and H₂O) is discussed. The net result of irradiation is structural re-organisation and reduction of iron within the iron hydroxides. At sufficiently low electron fluence and particularly in the lower incident energy, finer probe diameter STEM, the alteration is shown to be minimal. All the materials examined exhibit damage which as a function of cumulative fluence is best fitted by an inverse power-law, implying that several chemical and structural changes occur in response to the electron beam and we suggest that these are governed by secondary processes arising from the primary ionisation event. This work affirms that electron fluence and current density should be considered when measuring mixed valence ratios with EELS.     

SEM analyses of cathodoluminescence in MgO,CdS and GaAs/GaxAl1–xAs crystals

The method of analysis developed for the study of cathodoluminescence in the scanning electron microscope is briefly outlined. Current studies of cathodoluminescence in three types of crystal are presented. These are: (1) deformed and annealed MgO, (2) CdS into which Ga has been diffused, and (3) double heterostructure GaAs/Ga_xAl_1–xAs laser material.     

Effect of Al element in Zn-Al fillers on the corrosion resistance of Cu/Al brazed joints

In this paper, we describe experimental torch welding 1061 aluminum alloy to T2 copper. The corrosion behavior and performance of Cu/Al brazed joints were systematically investigated. This investigation was conducted using an optical microscope (OM), scanning electron microscope (SEM), energy disperse spectroscopy (EDS) and other methodologies. The results showed that the corrosion resistance of brazed joints was closely associated with Al content in filler metal. The corrosion behavior in 3.5 % NaCI solution belonged to micro-electrochemical corrosion and depended mainly on electrochemical imbalance between different phases. The excessive dissolution of Al atoms led to the occurrence of the corrosion of brazed joints and the corrosion product may be Al(OH)₃, Zn(OH)₂ and ZnO. It can be also found that an increase of aluminum content controlled largely formation and distribution of α-Al phase and Al₂O₃ protective film in brazing alloys, resulting in reducing the electrochemical corrosion current density and improving the corrosion resistance and shear strength of the joint.

     

Toward structural/chemical cotailoring of phase‐change Ge–Sb–Te in a transmission electron microscope

Ge₂Sb₂Te₅, as the prototype material for phase‐change memory, can be transformed from amorphous phase into nanoscale rocksalt‐type GeTe provided with an electron irradiation assisted by heating to 520°C in a 1250 kV transmission electron microscope. This sheds a new light into structural and chemical cotailoring of materials through coupling of thermal and electrical fields.     

Phase-selective staining of metal salt for scanning electron microscopy imaging of block copolymer film

Three metal salts, i.e., AgNO₃, HAuCl₄, and KCl, were proposed as novel staining reagents instead of traditional RuO₄ and OsO₄ labeled with expensive price and extreme toxicity for scanning electron microscopy (SEM) imaging of microphase separated block copolymer film. A simple and costless aqueous solution immersion procedure could ensure selective staining of the metal slat in specific phase of the nanostructured copolymer film, leading to a clear phase contrasted SEM image. The heavy metal salt has better staining effect, demonstrating stable and high signal-to-noise SEM image even at an acceleration voltage as high as 30 kV and magnification up to 250,000 times.     

Transient analysis of gaseous electron-ion recombination in the environmental scanning electron microscope

Most of the work carried out in relation to contrast mechanisms and signal formation in an environmental scanning electron microscope has yet to consider the time dependent aspects of image generation at a quantitative level. This paper quantitatively describes gaseous electron‐ion recombination (also known as ‘signal scavenging’) in an environmental scanning electron microscope at a transient level by utilizing the dark shadows/streaks seen in gaseous secondary electron detector images of alumina (Al₂O₃) immediately after a region of enhanced secondary electron emission is encountered by a scanning electron beam. The investigation firstly derives a theoretical model of gaseous electron‐ion recombination that takes into consideration transients caused by the time constant of the gaseous secondary electron detector electronics and external circuitry used to generate images. Experimental data of pixel intensity versus time of the streaks are then simulated using the model enabling the relative magnitudes of (i) ionization and recombination rates, (ii) recombination coefficients and (iii) electron drift velocities, as well as absolute values of the total time constant of the gaseous secondary electron detection system and external circuitry, to be determined as a function of microscope operating parameters such as gaseous secondary electron detector bias, sample‐electrode separation, imaging gas pressure, and scan speed. The results revealed, for the first time, the exact dependence that the effects of secondary electron‐ion recombination on signal formation has on reduced electric field and time in an environmental scanning electron microscope. Furthermore, the model implicitly demonstrated that signal loss as a consequence of field retardation due to ion space charges, although obviously present, is not the foremost phenomenon causing streaking in images, as previously thought.