Focused Ion Beam Technique Research Articles

Study of the nanoscale morphology of polythiophene fibrils and a fullerene derivative.

Nanoscale blending of electron-donor and electron-acceptor materials in solution-processed bulk heterojunction organic photovoltaic devices is crucial for achieving high power conversion efficiency. We used a classic blend of poly(3-hexylthiophene)/phenyl-C61-butyric acid methyl ester (P3HT/PCBM) as a model to observe the nanoscale morphology of the P3HT fibrils and PCBM nanoclusters in the mixture. Energy-filtered transmission electron microscopy (EFTEM) clearly revealed a nanoscopic phase separation. Randomly connected and/or nonconnected P3HT fibrous networks and PCBM domains, revealed by 2-dimensional micrographs, were observed by collecting electron energy loss spectra in the range of 19-30 eV. From EFTEM images, the average length and the diameter of P3HT fibrils were found to be approximately 70 ± 5 and 15 ± 2 nm, respectively. Combining the EFTEM, selected area electron diffraction, and X-ray diffraction results, the number and spacing of the ordered chains in P3HT fibrils were determined. There were 18 ± 3 repeating units of P3HT perpendicular to the fibril, ∼184 layers of π-π stacking along the fibril, and ∼9 layers of interchain stacking within the fibril. These conclusive observations provide insight into the number of molecules found in one instance of ordered-plane stacking. This information is useful for the calculation of charge transport in semicrystalline polymers. Using cross-section samples prepared with a focused ion beam technique, the vertical morphology of each phase was analyzed. By collecting 30 eV energy loss images, the phase separation in the P3HT/PCBM system was distinguishable. A higher P3HT concentration was observed at the top of the cell, near Al contact, which could possibly cause loss of carriers and recombination due to a mismatch in the P3HT and Al energy bands.

Biophysical evaluation of cells on nanotubular surfaces: the effects of atomic ordering and chemistry.

After the implantation of a biomaterial in the body, the first interaction occurs between the cells in contact with the biomaterial surface. Therefore, evaluating the cell–substrate interface is crucial for designing a successful implant. In this study, the interaction of MC3T3 osteoblasts was studied on commercially pure and alloy (Ti6Al4V) Ti surfaces treated with amorphous and crystalline titanium dioxide nanotubes. The results indicated that the presence of nanotubes increased the density of osteoblast cells in comparison to bare surfaces (no nanotubes). More importantly, our finding shows that the chemistry of the substrate affects the cell density rather than the morphology of the cells. A novel approach based on the focused ion beam technique was used to investigate the biophysical cell–substrate interaction. The analysis revealed that portions of the cells migrated inside the crystalline nanotubes. This observation was correlated with the super hydrophilic properties of the crystalline nanotubes.

Photoluminescence of focused ion beam implanted Er3+:Y2SiO5crystals

Erbium-doped low symmetry Y2SiO5 crystals attract a lot of attention in perspective of quantum information applications. However, only doping of the samples during growth is available up to now, which yields a quite homogeneous doping density. In the present work, we deposit Er3+-ions by the focused ion beam technique at yttrium sites with several fluences in one sample. With a photoluminescence study of these locally doped Er3+:Y2SiO5 crystals, we are able to evaluate the efficiency of the implantation process and develop it for the highest efficiency possible. We observe the dependence of ion activation after the post-implantation annealing on the fluence value. (© 2014 WILEY-VCH Verlag GmbH &Co. KGaA, Weinheim)

Nanostructural characterization of carbon nanotubes in laser-sintered polyamide 12 by 3D-TEM

Abstract

Inclined slit-based pullout method for determining interfacial strength of multi-walled carbon nanotube–alumina composites

Abstract This paper describes a testing method which enables us to determine experimentally the interfacial strength between multi-walled carbon nanotube (MWCNT) and ceramic matrix in MWCNT/ceramic composites. The testing method developed in this research, named “Inclined slit-based pullout method”, includes a single nanotube pullout technique and a focused ion beam (FIB) technique, which enables MWCNTs to be pulled out from the ceramic matrix during the pullout tests. Single MWCNTs embedded in a fracture surface of an alumina matrix composite are pulled out using a nanomanipulator system in a scanning electron microscope. Embedded lengths of the MWCNTs are controlled by using the FIB technique, i.e., by making an inclined through-slit near the fracture surface of the composite. The average interfacial strength between the MWCNTs and alumina matrix is evaluated to be 19.2 ± 6.6 MPa for 3 MWCNTs tested in this research. This value is found to be approximately close to that estimated from pullout lengths of the MWCNTs on the fracture surface of the composite, supporting the validity of the testing methods developed in this research.

Characterisation of thermal influences after laser processing polycrystalline diamond composites using long to ultrashort pulse durations

The laser processing of cutting tool edges is growing rapidly due to its flexibility, short cycle times and negligible waste. However, the quality of the tool and its cutting edge can vary greatly with different laser parameters and processing strategies. The generation of a graphitic carbon layer and a heat affected zone (HAZ) could occur during laser processing which is expected to reduce the quality and lifetime of the cutting tool. By using focussed ion beam (FIB) techniques to generate a cross section, the graphitic carbon layer and heat affected zone are characterised quantitatively and qualitatively for laser processes and as a reference, lapping and wire electro-discharge machining processes, used in the generation of polycrystalline diamond composite cutting tool edges. A focus is put on laser based techniques which vary in pulse duration from long microsecond pulses down to ultrashort picosecond pulses. A deep insight into the focussed ion beam techniques used and extensive analysis through Raman spectroscopy and energy dispersive X-ray spectroscopy (EDX) into the laser–material interactions are presented.

Micro-contacting of single and periodically arrayed columnar silicon structures by focused ion beam techniques

Micron-sized, periodic crystalline Silicon columns on glass substrate were electrically contacted with a transparent conductive oxide front contact and a focused ion beam processed local back contact. Individual column contacts as well as arrays of >100 contacted columns were processed. Current-voltage characteristics of the devices were determined. By comparison with characteristics obtained from adapted device simulation, the absorber defect density was reconstructed. The contacting scheme allows the fabrication of testing devices in order to evaluate the electronic potential of promising semiconductor microstructures.

Small fatigue crack propagation in Y2O3 strengthened steels

This paper is focused on two type of Y2O3 strengthened steels (Fe–14Cr ODS and ODS-EUROFER). Small fatigue crack propagation was experimentally measured using special small cylindrical specimens (diameter 2 and 2.6mm) with shallow notch grinded in the gauge length. In the middle of this notch, a pre-crack of length of 50μm was fabricated using a focused ion beam technique. Fatigue crack growth rate was measured for different applied total strain amplitudes and described using plastic part of the J-integral. Obtained results were compared with published data of EUROFER 97. The effect of the oxide dispersion on small fatigue crack propagation was found rather insignificant. Ferritic Fe–14Cr ODS steel shows more brittle behaviour, i.e. for the same cyclic plasticity, characterised by the plastic part of the J-integral, the small cracks grow faster. A new methodology for residual lifetime prediction of structures containing physically small cracks, based on plastic part of the J-integral, is presented.

A method for the tin pest presence testing in SnCu solder alloys

Purpose – The purpose of this study is to develop a testing method for tin pest in tin – copper (SnCu) alloys. Tin pest is the allotropic transformation of white β-tin (body-centered tetragonal structure) into gray α-tin (diamond cubic structure) at temperatures < 13.2°C. Design/methodology/approach – Bulk samples of Sn99Cu1 weight per cent (purity, 99.9 weight per cent) were cast in the form of roller-shaped ingots with a diameter of 1.0 cm and a height of 0.7 cm. The samples were then divided into four groups. The first group included samples artificially inoculated with α-tin powder. The second group was inoculated in the same way as the samples from the first group but additionally subjected to mechanical pressing. The third group of ingots was only subjected to mechanical pressing. The fourth group of samples consisted of as-received roller-shaped ingots.All samples were divided into two groups and kept either at −18°C or at −30°C for the low-temperature storage test. For tin pest identification, a visual inspection was made, using a Hirox digital microscope over 156 days at intervals not longer than 14 days. The plot of the transformation rate, presented as the average increase in the area of α-tin warts in time, was also determined. To demonstrate the differences between regions of β- and α-tin, scanning ion microscopy observations using the focused ion beam technique was performed. Findings – The first symptoms of tin pest were observed for the inoculated, mechanically pressed samples stored at −18°C, as well as those at −30°C, after less than 14 days. In the first stage of transformation, the rate was higher at −30°C for some time but, after about 75 days of storage at sub-zero temperatures, the rate at −30°C became lower compared to the rate at −18°C. Inoculation via the application of substances which are structurally similar to α-tin was efficient for the proposed new approach of rapid testing only when applied with simultaneous mechanical pressing. Infection from pressed-in seeds, leading to conventional seeded growth, was more rapid than infection in contact with seeds (without mechanical pressing), where the transition mechanism was induced by the epitaxial growth of metastable ice. Originality/value – The new rapid method for the diagnostic testing of the susceptibility of different SnCu alloys to tin pest in a period much shorter than 14 days (within single days for storage at −30°C) is proposed and described. The test procedure described in this paper produced results several times quicker than conventional procedures, which may take years. In effect, the behavior of tin alloys in the face of tin pest may be predicted much more easily and much earlier. The same procedure can be applied to other SnCu alloys used in electronics (and in other areas), if the test samples are prepared in a similar manner.

Interfacial Reactions during Explosive Bonding

The layers near the interface of explosively welded plates were investigated by means of microscopic observations, mostly with the use of transmission electron microscopy (and Focus Ion Beam technique for the thin foils preparation) equipped with energy dispersive spectrometry. The metal compositions based on steels and Ti, Zr, Ta or Cu, were analyzed. The study was focused on the identification of the intermetallic phases inside the melted zones, the possible interdiffusion between the bonded metals and the changes in the dislocation structure.

Tunable filter based on cavity electro-optic modulation for DWDM applications

In this paper the authors have demonstrated the feasibility and the realization of a wavelength tunable filter with an electro-optic modulation effect realized on diffused Ti:LiNbO3 waveguide. The two reflectors of the cavity consist in two Bragg׳s mirrors of identical period Λ=1.81μm and whose total number N=140. Both mirrors have been engraved using the Focused Ion Beam technique up to the depths l1=l2=2.7μm separated by a distance of lc=500μm. We obtained thanks to electro-optic modulation effect a tunable shift whose value is 0.67nm in a free spectral range FSR=1.59nm for a voltage variation up to 60V. This designed and realized probe will find many DWDM (Dense Wavelength Division Multiplexing) applications.

Fabrication of nanopore on pyramid

There have been tremendous interests about the fabrication of metallic nanopore due to the ultrafast genome sequencing biosensor capability. In this report, the fabrication of the nanopore on the Au coated SiO2 pyramid has been examined using various high energy electron beam irradiation and focused ion beam (FIB) milling techniques. The microfabricated Au nano-apertures on pyramid were irradiated with various high energy electron beam and FIB techniques. The formation of the nanopore dependent on the probe current was also examined using electron probe micro-analysis (EPMA). The nanopore on the Au coated SiO2 pyramid is found to be an AuSi mixture. The Au nanopore on the crater type hole was also fabricated using FIB Ga ion beam scanning. The shrinking rate was found to be the fastest compared with those fabricated with the other electron beam techniques.

AFM and FIB Study of Cyclic Strain Localization and Surface Relief Evolution in Fatigued f.c.c. Polycrystals

Atomic force microscopy (AFM) and focused ion beam technique (FIB) were adopted to study the early stages of surface relief evolution in 316L steel and polycrystalline copper fatigued with constant plastic strain amplitudes at different temperatures (316L steel at 93, 173 and 573 K; copper at 83, 173 and 295 K). Qualitative and quantitative data on the morphology and shape of persistent slip markings (PSMs), occurrence of extrusions and intrusions and the kinetics of extrusion growth are reported. They are discussed in relation with recent physically based theories of surface relief formation leading to fatigue crack initiation.

Fatigue Behaviour of AZ91 Magnesium Alloy in as-Cast and Severe Plastic Deformed Conditions

Fatigue strength, crack initiation and microstructure were experimentally investigated in an as-cast AZ91 alloy and in ultrafine-grained (UFG) AZ91 alloy processed by equal channel angular pressing (ECAP). The microstructure after ECAP is bimodal, consisting of fine-grained regions and clusters of larger grains with lower density of intermetallic particles. It has been found that the ECAP substantially increases the tensile strength (factor of two), improves ductility (factor of five) and improves the fatigue strength in low-cycle fatigue region. The improvement of the endurance limit based on 107 cycles is weak. The cyclic slip bands, as sites of the fatigue crack initiation on material surface, were investigated. Focussed ion beam technique (FIB) was applied to reveal the surface relief and the microstructure in the vicinity of early fatigue cracks. No grain coarsening was observed in the close vicinity of the initiated cracks. Fatigue cracks in ultrafine-grained structure develop both in the regions of larger grains and also in the fine grained areas. Two types of crack initiation were observed.

Electrodeposition and Behavior of Single Metal Nanowire Probes

This paper describes the fabrication of scanning probes with single metal nanowires (NWs) at the probe tip. The porous-template technique can produce NWs of various kinds of metals, with diameters down to 10-20 nm, which compete with multiwall carbon nanotube diameters. Metal NWs are grown by electrodeposition on the scanning probe tip. One NW can be selected to remain by focused ion beam technique. A variety of metals can be chosen as the tip material. Electric potentials of NWs at the probe tip can be measured. Single NW probes can measure surface topographies, electrode potentials, and their mechanical bending properties.

Mechanisms of Film Growth on Copper in Aqueous Solutions Containing Sulphide and Chloride under Voltammetric Conditions

The electrochemical behavior and film formation mechanisms of oxygen-free copper have been studied in aqueous solutions containing a wide range of sulphide and chloride concentrations using rotating disk electrodes and cyclic voltammetry. Scanning electron microscopy, energy dispersive X-ray spectroscopy and focused ion beam techniques were employed to characterize the morphology, composition and structure of the copper sulphide films formed on the copper surface under voltammetric conditions. These studies show that three distinct type of films were formed depending on the sulphide concentration, the flux of sulphide to the electrode surface, and the chloride concentration of the solution. The properties of the film and the mechanism of growth were determined by competition between sulphide diffusion in solution and the rate of interfacial reactions on the Cu surface. Comparison of these properties of electrochemically grown films to those of films grown under corrosion conditions indicates that pitting should not occur under the conditions expected in a nuclear waste repository.

The influence of focused-ion beam preparation technique on microcompression investigations: Lathe vs. annular milling

Two commonly used focused ion beam (FIB) milling techniques were employed for Mg micropillar fabrication to investigate the influence of the individual FIB technique on the microcompression testing method. Results from lathe milled pillars show that the relatively high ion exposure of this technique relative to annular milling greatly affects both stress–strain response and deformation morphology; stresses reached are up to four times higher than for the annular milled pillars and cracking of a surface layer is observed.

Strategies for the chemical analysis of highly porous bone scaffolds using secondary ion mass spectrometry

Understanding the distribution of critical elements (e.g. silicon and calcium) within silica-based bone scaffolds synthesized by different methods is central to the optimization of these materials. Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has been used to determine this information due to its very high surface sensitivity and its ability to map all the elements and compounds in the periodic table with high spatial resolution. The SIMS image data can also be combined with depth profiles to construct three-dimensional chemical maps. However, the scaffolds have interconnected pore networks, which are very challenging structures for the SIMS technique. To overcome this problem two experimental methodologies have been developed. The first method involved the use of the focused ion beam technique to obtain clear images of the regions of interest and subsequently mark them by introducing fiducial marks; the samples were then analysed using the ToF-SIMS technique to yield the chemical analyses of the regions of interest. The second method involved impregnating the pores using a suitable reagent so that a flat surface could be achieved, and this was followed by secondary ion mapping and 3D chemical imaging with ToF-SIMS. The samples used in this work were sol–gel 70S30C foam and electrospun fibres and calcium-containing silica/gelatin hybrid scaffolds. The results demonstrate the feasibility of both these experimental methodologies and indicate that these methods can provide an opportunity to compare various artificial bone scaffolds, which will be of help in improving scaffold synthesis and processing routes. The techniques are also transferable to many other types of porous material.

Role of defects in fatigue damage mechanisms of cast polycrystalline superalloy MAR-M 247

High-cycle fatigue life of nickel-based superalloy MAR-M 247 was experimentally determined for as-cast material and material processed by hot isostatic pressing (HIP). Fatigue testing was conducted at temperatures 650, 800, 900 ∘ C in laboratory air. HIP was done at the following conditions: 1200 ∘ C/100 MPa/240 min. It has been found that HIP significantly improves the fatigue life. Obtained results indicate that main factors which determine the fatigue strength of material in both conditions are grain size, grain orientation and size and distribution of casting defects. The distribution and size of the casting defects were evaluated by light microscopy on metallographic sections. The data were processed by the extreme value statistics, which enables to estimate the maximum size of a defect likely to occur in a defined volume. Light and scanning electron microscopy were used for fractographic investigation of fracture surfaces and fatigue crack initiation sites. Focused ion beam technique and transmission electron microscopy were applied with the aim to reveal the microstructure in the nearest vicinity of the early cracks. The mechanism of crack initiation, early crack propagation and the role of casting defects were described and discussed.

Initiation of Fatigue Cracks in Ultrafine-grained Materials in High-cycle Fatigue Region

Initiation of fatigue cracks in materials with conventional grain (CG) size was investigated very thoroughly in the past. There is an extensive knowledge on the localization of cyclic plasticity and early crack development; however, it cannot be straightforwardly applied to the ultrafine-grained (UFG) structures with the grain size below 1μm, because the crack initiation mechanisms are related to dislocation structures, which cannot develop in UFG materials simply from the size reasons.The paper brings results of an experimental investigation of the cyclic strain localization and crack initiation by means of focused ion beam technique (FIB). Two substantially different materials as regards the crystallographic structure, namely UFG Cu and magnesium alloy AZ91 processed by equal channel angular pressing (ECAP) were investigated and the observed characteristic features of crack initiation were discussed.The observations bring evidence that in the high-cycle fatigue (HCF) region point defects generated by dislocation activity do play very important role in the fatigue crack initiation process in UFG Cu. Fatigue cracks initiate in slip bands which form in areas of near-by oriented grains and are characteristic by surface relief, consisting of extrusions and intrusions. Point defects and formation of cavities and voids along the active slip planes governs the HCF crack initiation. No grain coarsening and development of specific dislocation structure was observed in the regions of crack initiation in UFG Cu. The mechanism of the crack initiation in AZ91 alloy processed by ECAP was found to be similar to that known from CG alloy. The cracks initiate in cyclic slip bands which forms in individual grains due to their relatively large grain size. The initiated cracks propagate along the slip planes in a crystallographic way which corresponds to the quasicleavage mechanism often reported for CG Mg alloys.