Ordered SrTiO_3 Nanoripples Induced by Focused Ion Beam

Ordered nanoripples on the niobium-doped SrTiO_3 surfaces were fabricated through focused ion beam bombardment. The surface morphology of the SrTiO_3 nanoripples was characterized using in situ focused ion beam/scanning electron microscopy. The well-aligned SrTiO_3 nanostructures were obtained under optimized ion irradiation conditions. The characteristic wavelength was measured as about 210 nm for different ion beam currents. The relationship between the ion irradiation time and current and SrTiO_3 surface morphology was analyzed. The presented method will be an effective supplement for fabrication of SrTiO_3 nanostructures that can be used for ferroelectric and electronic applications.

Three-dimensional vertical ZnO transistors with suspended top electrodes fabricated by focused ion beam technology

Three-dimensional(3D)vertical architecture transistors represent an important technological pursuit,which have distinct advantages in device integration density,operation speed,and power consumption.However,the fabrication processes of such 3D devices are complex,especially in the interconnection of electrodes.In this paper,we present a novel method which combines suspended electrodes and focused ion beam(FIB)technology to greatly simplify the electrodes interconnection in 3D devices.Based on this method,we fabricate 3D vertical core-double shell structure transistors with ZnO channel and Al_(2)O_(3) gate-oxide both grown by atomic layer deposition.Suspended top electrodes of vertical architecture could be directly connected to planar electrodes by FIB deposited Pt nanowires,which avoid cumbersome steps in the traditional 3D structure fabrication technology.Both single pillar and arrays devices show well behaved transfer characteristics with an Ion/Ioff current ratio greater than 106 and a low threshold voltage around 0 V.The ON-current of the 2×2 pillars vertical channel transistor was 1.2μA at the gate voltage of 3 V and drain voltage of 2 V,which can be also improved by increasing the number of pillars.Our method for fabricating vertical architecture transistors can be promising for device applications with high integration density and low power consumption.

Monte Carlo Si mulation of Damage Depth in Focused Ion Beam Milling Si_3N_4 Thin Film

The damage properties of Focused Ion Beam(FIB) milling Si3N4 thin film are investigated by the detailed analyzing images of nanoholes and simulation of Monte Carlo. The damage depth in the Si3N4 thin film for two different ion species(Gallium and Arsenic) under various parameters(ion energy, angle of incidence) are investigated by Monte Carlo method. The simulations show the damage depth increases with the increasing ion energy, the damage depth is dependent on the angle of incident ion, the curves of the damage depth for Ga ion and As ion at 30 keV nearly superpose, while the damage depth for Ga with 90 keV ion is more than that for As ion with the same energy.

Co-doped BaFe_(2)As_(2) Josephson junction fabricated with a focused helium ion beam

Josephson junction plays a key role not only in studying the basic physics of unconventional iron-based superconductors but also in realizing practical application of thin-film based devices,therefore the preparation of high-quality iron pnictide Josephson junctions is of great importance.In this work,we have successfully fabricated Josephson junctions from Co-doped BaFe_(2)As_(2)thin films using a direct junction fabrication technique which utilizes high energy focused helium ion beam(FHIB).The electrical transport properties were investigated for junctions fabricated with various He^(+)irradiation doses.The junctions show sharp superconducting transition around 24 K with a narrow transition width of 2.5 K,and a dose correlated foot-structure resistance which corresponds to the effective tuning of junction properties by He^(+)irradiation.Significant J_c suppression by more than two orders of magnitude can be achieved by increasing the He^(+)irradiation dose,which is advantageous for the realization of low noise ion pnictide thin film devices.Clear Shapiro steps are observed under 10 GHz microwave irradiation.The above results demonstrate the successful fabrication of high quality and controllable Co-doped BaFe_(2)As_(2)Josephson junction with high reproducibility using the FHIB technique,laying the foundation for future investigating the mechanism of iron-based superconductors,and also the further implementation in various superconducting electronic devices.

Half-integer Shapiro steps in MgB_(2) focused He ion beam Josephson junctions

Half-integer microwave induced steps(Shapiro steps)have been observed in many different Josephson junction systems,which have attracted a lot of attention because they signify the deviation of current phase relation(CPR)and uncover many unconventional physical properties.In this article,we first report the discovery of half-integer Shapiro steps in MgB_(2)focused He ion beam(He-FIB)Josephson junctions.The half-integer steps'dependence on microwave frequency,temperature,microwave power,and magnetic field is also analyzed.We find that the existence of half-integer steps can be controlled by the magnetic field periodically,which is similar to that of high temperature superconductor(HTS)grain boundary junctions,and the similarity of the microstructures between gain boundary junctions and He-FIB junctions is discussed.As a consequence,we mainly attribute the physical origin of half-integer steps in MgB_(2)He-FIB junctions to the model that a He-FIB junction is analogous to a parallel junctions'array.Our results show that He-FIB technology is a promising platform for researching CPR in junctions made of different superconductors.

Fabrication technique of micro/nano-scale speckle patterns with focused ion beam

The fabrication technique of micro/nano-scale speckle patterns with focused ion beam (FIB) system is studied for digital image correlation (DIC) measurement under a scanning electron microscope (SEM).The speckle patterns are fabricated by directly etching the counterpart of the specimen to the black part of a template.Mean intensity gradient is used to evaluate the quality of these SEM images of speckle patterns fabricated based on different templates to select an optimum template.The pattern size depending on the displacement measurement sensitivity is adjusted by altering the magnification of FIB according to the relation curve of the etching size versus magnification.The influencing factors including etching time and ion beam current are discussed.Rigid body translation tests and rotation tests are carried out under SEM to verify the reliability of the fabricated speckle patterns.The calculated values are in good agreement with the imposed ones.

Imaging the interphase of carbon fiber composites using transmission electron microscopy:Preparations by focused ion beam, ion beam etching, and ultramicrotomy

Three sample preparation techniques, focused ion beam （FIB）, ion beam （IB） etching, and ultramicrotomy （UM） were used in comparison to analyze the interphase of carbon fiber ＇epoxy composites using transmission electron microscopy. An intact interphase with a relatively uniform thickness was obtained by FIB. and detailed chemical analysis of the interphase was investigated by electron energy loss spectroscopy. It shows that the interphase region is 200 mn wide with an increasing oxygen-to-carbon ratio from 10% to 19% and an almost constant nitrogen-to-carbon ratio of about 3%. However, gallium implantation of FIB tends to hinder fine structure analysis of the interphase. For IB etching, the interphase region is observed with transition morphology frona amorphous resin to nano-crystalline carbon fiber, but the uneven sample thickness brings difficulty for quantitative chemical analysis. Moreover, UM tends to cause damage and/or deformation on the interphase. These results are meaningful for in-depth understanding on the interphase characteristic of carbon fiber composites.

Annealing treatment of focused gallium ion beam processing of SERS gold substrate

Raman spectroscopy is a type of inelastic scattering spectroscopy that is widely used in determining and analyzing molecular structure.It also has a number of practical applications in evaluating food safety,medicine,and forensics.The Raman spectral signal is weak,but the development of the surface-enhanced Raman scattering(SERS)technique has overcome this problem and led to further developments in Raman spectroscopy.This paper describes a fundamental study of the use of focused ion beam(FIB)direct writing for preparing gold substrates for SERS.Molecular dynamics and Monte Carlo simulation methods are used to investigate the damage induced by gallium ion implantation of a gold substrate.Based on characterization by x-ray photoelectron spectroscopy(XPS)and scanning electron microscopy,the mechanism by which ion implantation and annealing influence the damage induced by a gallium FIB is analyzed.After annealing at 350 XC,a mixture of metallic gallium,its oxide Ga2O3 conforming to the stoichiometric ratio,and its sub-stable oxide(Ga2Ox)in sub-stoichiometric ratio precipitated on the surface are detected by XPS.Annealing treatment can effectively reduce the effect of gallium ion implantation on a SERS substrate fabricated by FIB direct writing.

Slice Thickness Optimization for the Focused Ion Beam-Scanning Electron Microscopy 3D Tomography of Hierarchical Nanoporous Gold

The combination of focused ion beam (FIB) with scanning electron microscopy (SEM), also known as FIB-SEM tomography, has become a powerful 3D imaging technique at the nanometer scale. This method uses an ion beam to mill away a thin slice of material, which is then block-face imaged using an electron beam. With consecutive slicing along the z-axis and subsequent imaging, a volume of interest can be reconstructed from the images and further analyzed. Hierarchical nanoporous gold (HNPG) exhibits unique structural properties and has a ligament size of 15–110 nm and pore size of 5–20 nm. Accurate reconstruction of its image is crucial in determining its mechanical and other properties. Slice thickness is one of the most critical and uncertain parameters in FIB-SEM tomography. For HNPG, the slice thickness should be at least half as thin as the pore size and, in our approach, should not exceed 10 nm. Variations in slice thickness are caused by various microscope and sample parameters, e.g., converged ion milling beam shape, charging effects, beam drift, or sample surface roughness. Determining and optimizing the actual slice thickness variation appear challenging. In this work, we examine the influence of ion beam scan resolution and the dwell time on the mean and standard deviation of slice thickness. After optimizing the resolution and dwell time to achieve the target slice thickness and lowest possible standard deviation, we apply these parameters to analyze an actual HNPG sample. Our approach can determine the thickness of each slice along the z-axis and estimate the deviation of the milling process along the y-axis (slow imaging axis). For this function, we create a multi-ruler structure integrated with the HNPG sample.

Three-dimensional analysis of micro defect morphologies in cement-based materials using focused ion beam tomography

Although there has been much research of cracks of the cement-based materials using optical and electron microscopy two-dimensional (2D) imaging methods, the real three-dimensional (3D) crack shapes have not previously been revealed. Thanks to the focused ion beam (FIB) tomography and the follow-up image processing, two 3D subsurface cracks and a cluster of inner cracks were picked out and discussed in this research. It was found that the subsurface crack (its length is about 15 part, width about 1-5 prn, and opening about 1 ~tm) was much larger than the inner crack (its length and width are about 1-5 pro, opening is from 200 nm to 1 pan), which arose from the sample preparation process. Besides, it was revealed that most of the inner cracks were in the form of clusters.

Revealing substructure in clock-rolled Ta aided with triple focused ion beam

Clock rolling was developed to make defor- mation microstructure homogenize in high-purity Ta. The substructure of deformed Ta was revealed by electron back-scatter diffraction （EBSD） technique aided with triple focused ion beam （FIB）. The results indicate that the triple FIB method can produce a mirror surface required by EBSD analysis. The clock rolling works well for the homogenization of deformed microstructure. Particularly, the local stored energy in { 111 } orientated grains is largely reduced by clock rolling, whereas it is enhanced in {100} orientated grains because of the occurrence of grain subdivision.

Electrical transport properties of focused ion beam lithography Au contacts on PbTiO_(3)nanorods

PbTiO_(3)nanorods with tetragonal phase were synthesized by hydrothermal method and heat treatment,and temperature-dependent electrical transport properties of individual PbTiO_(3)nanorod were investigated.The results show that the conductivities of PbTiO_(3)nanorods are gradually enhanced with temperature increasing from 77.4 to 295 K,and exhibit the typical nonlinear Ⅰ–Ⅴ char-acteristics.The barrier height between Au electrode and nanorod is reduced from 0.137 to 0.088 eV with increasing bias from 0.2 to 1 V.The corresponding values of thermal activation energies are 0.172 and 0.06 eV below the conduction band for 180–295 and 77.4–180 K,respectively.This semiconductor-like behavior may result from the larger number of surface defects or localized states in the amorphorized PbTiO_(3).

High-Temperature Superconducting YBa_(2)Cu_(3)O_(7-δ)Josephson Junction Fabricated with a Focused Helium Ion Beam

As a newly developed method for fabricating Josephson junctions,a focused helium ion beam has the advantage of producing reliable and reproducible junctions.We fabricated Josephson junctions with a focused helium ion beam on our 50 nm YBa_(2)Cu_(3)O_(7-δ)(YBCO)thin films.We focused on the junction with irradiation doses ranging from 100 to 300 ions/nm and demonstrated that the junction barrier can be modulated by the ion dose and that within this dose range,the junctions behave like superconductor–normal conductor–superconductor junctions.The measurements of the I–V characteristics,Fraunhofer diffraction pattern,and Shapiro steps of the junctions clearly show AC and DC Josephson effects.Our findings demonstrate high reproducibility of junction fabrication using a focused helium ion beam and suggest that commercial devices based on this nanotechnology could operate at liquid nitrogen temperatures.

Effects of operating conditions on the performance degradation and anode microstructure evolution of anode-supported solid oxide fuel cells

Performance degradation shortens the life of solid oxide fuel cells in practical applications.Revealing the degradation mechanism is crucial for the continuous improvement of cell durability.In this work,the effects of cell operating conditions on the terminal voltage and anode microstructure of a Ni-yttria-stabilized zirconia anode-supported single cell were investigated.The microstructure of the anode active area near the electrolyte was characterized by laser optical microscopy and focused ion beam-scanning electron microscopy.Ni depletion at the anode/electrolyte interface region was observed after 100 h discharge tests.In addition,the long-term stability of the single cell was evaluated at 700℃for 3000 h.After an initial decline,the anode-supported single cell exhibits good durability with a voltage decay rate of 0.72%/kh and an electrode polarization resistance decay rate of 0.17%/kh.The main performance loss of the cell originates from the initial degradation.

Fabrication of Windowed Very-Small-Aperture Laser Diodes

A windowed very small aperture laser (VSAL) source for use in high resolution near field optical data storage is fabricated.The windowed regions are introduced to avoid shorting the pn junction with metal coating and suppress the COD effect.It facilitates producing VSAL by simplified technology and improves the laser performance.A VSAL with 400nm small aperture is demonstrated by focused ion beam (FIB) and the output power is 0 3mW at 31mA.

Characterization of 3D pore nanostructure and stress-dependent permeability of organic-rich shales in northern Guizhou Depression,China

The three-dimensional(3D)pore structures and permeability of shale are critical for forecasting gas production capacity and guiding pressure differential control in practical reservoir extraction.However,few investigations have analyzed the effects of microscopic organic matter(OM)morphology and 3D pore nanostructures on the stress sensitivity,which are precisely the most unique and controlling factors of reservoir quality in shales.In this study,ultra-high nanoscale-resolution imaging experiments,i.e.focused ion beam-scanning electron microscopy(FIB-SEMs),were conducted on two organic-rich shale samples from Longmaxi and Wufeng Formations in northern Guizhou Depression,China.Pore morphology,porosity of 3D pore nanostructures,pore size distribution,and connectivity of the six selected regions of interest(including clump-shaped OMs,interstitial OMs,framboidal pyrite,and microfractures)were qualitatively and quantitatively characterized.Pulse decay permeability(PDP)measurement was used to investigate the variation patterns of stress-dependent permeability and stress sensitivity of shales under different confining pressures and pore pressures,and the results were then used to calculate the Biot coefficients for the two shale formations.The results showed that the samples have high OM porosity and 85%of the OM pores have the radius of less than 40 nm.The OM morphology and pore structure characteristics of the Longmaxi and Wufeng Formations were distinctly different.In particular,the OM in the Wufeng Formation samples developed some OM pores with radius larger than500 nm,which significantly improved the connectivity.The macroscopic permeability strongly depends on the permeability of OM pores.The stress sensitivity of permeability of Wufeng Formation was significantly lower than that of Longmaxi Formation,due to the differences in OM morphology and pore structures.The Biot coefficients of 0.729 and 0.697 were obtained for the Longmaxi and Wufeng Formations,respectively.

Influence of oxide scales on the corrosion behaviors of B510L hot-rolled steel strips

The influence of oxide scales on the corrosion behaviors of B510 L hot-rolled steel strips was investigated in this study. Focused ion beams and scanning electron microscopy were used to observe the morphologies of oxide scales on the surface and cross sections of the hot-rolled steel. Raman spectroscopy and X-ray diffraction were used for the phase analysis of the oxide scales and corrosion products. The corrosion potential and impedance were measured by anodic polarization and electrochemical impedance spectroscopy. According to the results, oxide scales on the hot-rolled strips mainly comprise iron and iron oxides. The correlation between mass gain and test time follows a power exponential rule in the damp-heat test. The corrosion products are found to be mainly composed of γ-Fe OOH, Fe3O4, ？-Fe OOH, and γ-Fe2O3. The contents of the corrosion products are different on the surfaces of the steels with and without oxide scales. The steel with oxide scales is found to show a higher corrosion resistance and lower corrosion rate.

Degradation Diagnostics from the Subsurface of Lithium-Ion Battery Electrodes

Despite the long-established rocking-chair theory of lithium-ion batteries(LIBs),developing novel characterization methodology with higher spatiotemporal resolution facilitates a better understanding of the solid electrolyte interphase studies to shape the reaction mechanisms.In this work,we develop a Xenon ion plasma focused ion beam(Xe+PFIB)-based characterization technique to probe the cross-sectional interface of both ternary cathode and graphite anode electrodes,with the focus on revealing the chemical composition and distribution underneath the electrode surface by in-depth analysis of secondary ions.Particularly,the lithium fluoride is detected in the pristine cathode prior to contact with the electrolyte,reflecting that the electrode degradation is in the form of the loss of lithium inventory during electrode preparation.This degradation is related to the hydrolysis of the cathode material and the decomposition of the PVDF binder.Through the quantitative analysis of the transition-metal degradation products,manganese is found to be the dominant element in the newly formed inactive fluoride deposition on the cathode,while no transition metal signal can be found inside the anode electrode.These insights at high resolution implemented via a PFIB-based characterization technique not only enrich the understanding of the degradation mechanism in the LIBs but also identify and enable a high-sensitivity methodology to obtain the chemical survey at the subsurface,which will help remove the capacity-fade observed in most LIBs.

High resolution ultrastructure imaging of fractures in human dental tissues

Human dental hard tissues are dentine, cementum, and enamel. These are hydrated mineralised composite tissues with a hierarchical structure and versatile thermo-mechanical properties. The hierarchical structure of dentine and enamel was imaged by transmission electron microscopy （TEM） of samples prepared by focused ion beam （FIB） milling. High resolution TEM was carried out in the vicinity of a crack tip in dentine. An intricate ＂random weave＂ pattern of hydroxyapatile crystallites was observed and this provided a possible explanation for toughening of the mineralized dentine tissue at the nano-scale. The results reported here provide the basis for improved understanding of the rela- tionship between the multi-scale nature and the mechanical properties of hierarchically structured biomaterials, and will also be useful for the development of better prosthetic and dental restorative materials.

On the Path to High-Temperature Josephson Multi-Junction Devices

We report our progress in the high-temperature superconductor(HTS)Josephson junction fabrication process founded on utilizing a focused helium ion beam damaging technique and discuss the expected device performance attainable with the HTS multi-junction device technology.Both the achievable high value of characteristic voltage V_(C)=I_(C)R_(N)of Josephson junctions and the ability to design a large number of arbitrary located Josephson junctions allow narrowing the existing gap in design abilities for lowtemperature superconductor(LTS)and HTS circuits even with using a single YBa_(2)Cu_(3)O_(7-x) film layer.A one-layer topology of active electrically small antenna is suggested and its voltage response characteristics are considered.