Frictional Characteristics of Quasicrystals at High Temperatures

AlCuFe quasicrystal coatings were deposited by unbalanced magnetron sputtering for study of their friction and wear properties at high temperatures. It has been shown that growth and annealing conditions can be controlled to produce icosahedral quasicrystal or the approximant cubic phase. The comparison of friction and wear properties between quasicrystal and an approximant with nearly the same stoichiometry permits assessment of the unique quasicrystalline structure for tribological applications. The goals of this study are to determine how crystal structure influences tribological properties and to study the general friction and wear behavior of quasicrystals. Tribological properties were evaluated using a pin-on-disk tribometer and crystal structure was characterized using an X-ray diffractometer. The tests specimens were 10 m thick films deposited on a 1 diameter steel disk and a 1/4 diameter steel ball. Data was collected over a range of temperatures from room to 600°C. Friction coefficients and wear rates of quasicrystals and approximants were nearly identical for room temperature tests. The wear process generated Al, Cu, Fe, and oxide debris on the side of the track, but overall wear was mild. The friction coefficient of the icosahedral phase was 25% lower than the cubic phase at 150 thru 450°C. Generally, only moderate differences in the friction and wear properties were observed between the icosahedral quasicrystal phase and the cubic phase.     

Development of a new wear resistant coating by arc spraying of a steel-based cored wire

In the present study, a cored wire of 304 L stainless steel as sheath material and NiB and WC-12Co as filler materials was designed and deposited to produce a new wear resistant coating containing amorphous phase by arc spraying. The microstructure of the coating was investigated. The porosity and hardness of the coating were determined. The wear performance of the coating was evaluated. The XRD and TEM analyses showed that there are high volume of amorphous phase and very fine crystalline grains in the coating. DTA measurements revealed that the crystallization of the amorphous phase occurred at 579.2°C. Because metallurgical processes for single droplets were non-homogenous during spraying, the lamellae in the coating have different hardness values, which lie between about 700 and 1250 HV_{100 g}. The abrasive wear test showed that the new Fe-based coating was very wear resistant.     

Conventional and back-side focused ion beam milling for off-axis electron holography of electrostatic potentials in transistors

Off-axis electron holography is used to characterize a linear array of transistors, which was prepared for examination in cross-sectional geometry in the transmission electron microscope (TEM) using focused ion beam (FIB) milling from the substrate side of the semiconductor device. The measured electrostatic potential is compared with results obtained from TEM specimens prepared using the more conventional 'trench' FIB geometry. The use of carbon coating to remove specimen charging effects, which result in electrostatic fringing fields outside 'trench' specimens, is demonstrated. Such fringing fields are not observed after milling from the substrate side of the device. Analysis of the measured holographic phase images suggests that the electrically inactive layer on the surface of each FIB-milled specimen typically has a thickness of 100 nm.     

Thermal stability of Ti and Pt nanowires manufactured by Ga+ focused ion beam

Ti and Pt nanowires have been produced by ultra high‐vacuum molecular beam epitaxy deposition of Ti thin films and focused ion beam (FIB) deposition of Pt thin films, followed by cross‐sectional FIB sputtering to form electron‐transparent nanowires. The thermal stability of the nanowires has been investigated by in situ thermal cycling in a transmission electron microscope. Epitaxial single crystal Ti nanowires on (0001)Al₂O₃ substrates are microstructurally stable up to 550–600 °C, above which limited dislocation motion is activated shortly before the Ti‐wires oxidize. The amorphous FIB‐deposited Pt wires are stable up to 580–650 °C where partial crystallization is observed in vacuum. Faceted nanoparticles grow on the wire surface, growing into free space by surface diffusion and minimizing contact area with the underlying wire. The particles are face‐centred cubic (fcc) Pt with some dissolved Ga. Continued heating results in particle spheroidization, coalescence and growth, retaining the fcc structure.     

Focused ion beam milling of vitreous water: prospects for an alternative to cryo-ultramicrotomy of frozen-hydrated biological samples

The feasibility of using a focused ion beam (FIB) for the purpose of thinning vitreously frozen biological specimens for transmission electron microscopy (TEM) was explored. A concern was whether heat transfer beyond the direct ion interaction layer might devitrify the ice. To test this possibility, we milled vitreously frozen water on a standard TEM grid with a 30‐keV Ga⁺ beam, and cryo‐transferred the grid to a TEM for examination. Following FIB milling of the vitreous ice from a thickness of approximately 1200 nm to 200–150 nm, changes characteristic of heat‐induced devitrification were not observed by TEM, in either images or diffraction patterns. Although numerous technical challenges remain, it is anticipated that ‘cryo‐FIB thinning’ of bulk frozen‐hydratred material will be capable of producing specimens for TEM cryo‐tomography with much greater efficiency than cryo‐ultramicrotomy, and without the specimen distortions and handling difficulties of the latter.     

SAF2906双相不锈钢超塑性研究

通过恒温拉伸机对固溶处理与冷轧加工后的SAF2906双相不锈钢进行恒温拉伸试验,分析其在不同条件下超塑性伸长率的变化。利用扫描电镜与透射电镜对其进行内部组织观察,了解其两相比例的变化情况。试验结果表明,SAF2906双相不锈钢中铁素体相(δ相)与奥氏体相(γ相)的两相体积比随固溶温度的变化而改变,随着固溶温度的升高铁素体比例不断上升,其中当铁素体与奥氏体的两相体积比接近1∶1的情况下,SAF2906双相不锈钢展现出良好的超塑性性能;在机械加工方面可以通过提高冷轧压下量的方法提高SAF2906双相不锈钢的超塑伸长率,试验中试样的伸长率随着冷轧变形量的提高而明显增大,当固溶温度为1 100 ℃,冷轧压下量为85%时,变形温度为960 ℃,应变速率为1×103 s1的条件下,SAF2906双相不锈钢伸长率为1 430%。     

A method for determining void arrangements in inverse opals

The periodic arrangement of voids in ceramic materials templated by colloidal crystal arrays (inverse opals) has been analysed by transmission electron microscopy. Individual particles consisting of an approximately spherical array of at least 100 voids were tilted through 90° along a single axis within the transmission electron microscope. The bright‐field images of these particles at high‐symmetry points, their diffractograms calculated by fast Fourier transforms, and the transmission electron microscope goniometer angles were compared with model face‐centred cubic, body‐centred cubic, hexagonal close‐packed, and simple cubic lattices in real and reciprocal space. The spatial periodicities were calculated for two‐dimensional projections. The systematic absences in these diffractograms differed from those found in diffraction patterns from three‐dimensional objects. The experimental data matched only the model face‐centred cubic lattice, so it was concluded that the packing of the voids (and, thus, the polymer spheres that composed the original colloidal crystals) was face‐centred cubic. In face‐centred cubic structures, the stacking‐fault displacementvector is . No stacking faults were observed when viewingthe inverse opal structure along the orthogonal <110>‐type directions, eliminating the possibility of a random hexagonally close‐packed structure for the particles observed. This technique complements synchrotron X‐ray scattering work on colloidal crystals by allowing both real‐space and reciprocal‐space analysis to be carried out on a smaller cross‐sectional area.     

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.     

Low damage lamella preparation of metallic materials by FIB processing with low acceleration voltage and a low incident angle Ar ion milling finish

Metallic materials are known to be very sensitive to Gallium (Ga) focused ion beam (FIB) processing. Crystal defects formed by FIB irradiation degrade the transmission electron microscope image quality, and it is difficult to distinguish original defects from FIB process-induced damage. A solution to this problem is the low acceleration voltage and low incident angle (LVLA) Argon ion milling, which can be incorporated as an extensional countermeasure for FIB damage removal and eventually for preparation of high-quality lamellae. The transmission electron microscope image quality of iron single crystal could be improved by removing crystal defects using the low acceleration voltage and low incident angle Argon ion milling finish. Lamella quality of the processing result was almost similar with that of the conventional electrolytic polishing. As a practical application of the process, low damage lamella of stainless cast steel could be prepared. Effectiveness of the FIB system equipped with the low acceleration voltage and low incident angle Argon ion milling function as a tool to make high-quality metallic material lamellae is illustrated.     

Corrosion-wear behaviour of thermal sprayed nanostructured FeCu/WC-Co coatings

The corrosion and corrosion-wear behaviour of a thermal sprayed nanostructured FeCu/WC-Co coating were investigated in a Hank's solution and compared to stainless steel AISI 304 and nanostructured WC-Co coatings. Electrochemical noise and potentiodynamic polarization measurements were conducted along with an ex situ scanning electron microscopy to unfold the response of these materials under these corrosive and corrosion-wear test conditions. The multiphase structure of the FeCu/WC-Co coating induces a complex corrosion behaviour. Under corrosion-wear conditions, the nanostructured FeCu/WC-Co coating exhibits a depassivation/repassivation behaviour comparable to the behaviour of stainless steel AISI 304 and nanostructured WC-Co coatings.     

Relation Between Tribolayers and Wear Behavior During Dry Sliding of Fe-Al Hot-Dipped Coating

An Fe-Al coating consisting of FeAl and Fe₃Al was prepared on AISI 1045 steel by hot-dip aluminizing and subsequent high-temperature diffusion. Dry sliding wear tests were performed for Fe-Al coating against AISI 52100 steel under various sliding speeds and loads. During sliding, thin tribolayers formed on the worn surfaces of the Fe-Al coating. After wear, they were observed to be a nonoxidized mechanically mixed layer (MML) at 0.5 m/s, an oxide-containing MML at 0.75–2.68 m/s, and an in situ oxide layer at 4 m/s. The tribolayers presented a close relation with the wear behavior. Because of their different ingredients, structures, and types, the tribolayers resulted in significant changes in the wear behavior. At 0.75–2.68 m/s (except for 2.68 m/s, 40 N), the compact tribooxide layers exerted a protective function for Fe-Al coating to reduce the wear rate. However, for the tribolayers containing no or trace tribooxides at 0.5 m/s or the unstable ones formed at 2.68 m/s, 40 N and 4 m/s, no protection was presented. In these cases, the Fe-Al coating would be partly or totally ground off, thus presenting poor wear resistance at high wear rates.     

熔渗法制备铁铝合金涂层组织分析

采用熔渗法在超低碳钢表面制备铁铝合金涂层。利用金相显微镜、扫描电镜(SEM)以及X-射线衍射仪分析了熔渗层的组织结构,结果表明,熔渗层从表面向基体内存在多相结构,依次为FeAl3,Fe2Al5(FeAl2),FeAl相,链珠状组织及α-Fe(Al)固溶体。     

Understanding the deformation behavior of 17-4 precipitate hardenable stainless steel produced by direct metal laser sintering using micropillar compression and TEM

Micropillar compression testing and transmission electron microscopy were used to investigate the deformation mechanisms under compression in 17-4 precipitation-hardening stainless steel, fabricated by direct metal laser sintering. The as-built specimen as well as that aged for 4 h at 866 K contained fractions of retained austenite, while that aged for 60 min at 755 K was fully martensitic. It was observed that the columnar elongated grains underwent martensite/austenite phase changes with changes in the aging temperature. The precipitate phase that developed with aging enhanced the material hardness and yield strength, with values being higher in the case of the specimen aged at a lower temperature for a shorter time. The results showed that the microstructures and properties of 17-4 stainless steel specimens fabricated by DMLS vary significantly from those of specimens produced using conventional methods.     

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.     

Femtosecond near-field scanning optical microscopy

We have developed an instrument for optically measuring carrier dynamics in thin-film materials with ≈150 nm lateral resolution, ≈250 fs temporal resolution and high sensitivity. This is accomplished by combining an ultrafast pump–probe laser spectroscopic technique with a near-field scanning optical microscope. A diffraction-limited pump and near-field probe configuration is used, with a novel detection system that allows for either two-colour or degenerate pump and probe photon energies, permitting greater measurement flexibility than that reported in earlier published work. The capabilities of this instrument are proven through near-field degenerate pump–probe studies of carrier dynamics in GaAs/AlGaAs single quantum well samples locally patterned by focused ion beam (FIB) implantation. We find that lateral carrier diffusion across the nanometre-scale FIB pattern plays a significant role in the decay of the excited carriers within ≈1 μm of the implanted stripes, an effect which could not have been resolved with a far-field system.     

Transmission electron microscopy of fluorapatite–gelatine composite particles prepared using focused ion beam milling

In this paper, synthetic fluorapatite–gelatine composite particles are prepared for transmission electron microscopy (TEM) studies using two methods based on focused ion beam (FIB) milling. TEM studies on the FIB‐prepared specimens are compared with TEM observations on samples prepared using an ultramicrotome. The results show that ultramicrotome slicing causes significant cracking of the apatite, whereas the ion beam can be used to make high‐quality, crack‐free specimens with no apparent ion beam‐induced damage. The TEM observations on the FIB‐prepared samples confirm that the fluorapatite composite particles are composed of elongated, preferentially orientated grains and reveal that the grain boundaries contain many small interstices filled with an amorphous phase.     

Experimental Evaluation of Friction and Wear Properties of Solid Lubricant Coatings on SUS440C Steel in Liquid Nitrogen

The friction and wear properties of the prevailing different solid lubricant coatings (Ion-plated Au, Ion-plated Ag and RF-sputtered PTFE on SUS440C stainless steel) used in the bearings of high-speed cryogenic-turbo-pumps of liquid rocket engines were experimentally evaluated in liquid nitrogen immersed conditions. Also the above experiments were carried out with two newly proposed solid lubricant coatings of sputter-ion-plated MoSTi and a new ion-plated Pb on SUS440C stainless steel. The friction coefficient and wear rates of the coatings of ion-plated Au, ion-plated Ag, RF-sputtered PTFE, the new ion-plated Pb and MoS₂Ti-SIP (with coating thickness of 0.7±0.1 μm) on SUS440C steel against SUS440C stainless steel ball in liquid nitrogen were compared. Worn surfaces were examined microscopically with a microscope and a profilometer for understanding the mechanisms of friction and wear and transfer film lubrication in liquid nitrogen. It is found that the newly proposed solid lubricant coatings are showing promising results for their use in liquid nitrogen immersed conditions. The sputter-ion-plated MoSTi coating on SUS 440C steel shows a minimum value of friction coefficient (μ=0.015) and wear rate (w_c=0.56 × 10⁻⁶ mm³/N m ) in liquid nitrogen.     

Abrasive and Adhesive Wear Behavior of Arc-Evaporated Al<Subscript>1−<Emphasis Type="Italic">x</Emphasis></Subscript>Cr<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>N Hard Coatings

During the last decade, the usage of difficult-to-machine materials such as austenitic stainless steels has increased continuously in various industrial applications. Tools such as blind hole taps, punches, or deep drawing molds are often exposed to severe wear while machining/forming these materials, mainly due to excessive adhesion and material transfer. On combination with abrasive wear due to work-hardened wear debris, tool lifetime in these applications is often limited. In this study, ball-on-disc experiments were carried out with arc-evaporated AlCrN coatings with different Al/(Al + Cr) ratios against Al₂O₃ and austenitic stainless steel balls in ambient atmosphere. Test temperatures of 25, 500, and 700°C were chosen for the hard Al₂O₃ balls simulating severe abrasive loads, whereas 25, 150, and 250°C were used for the softer stainless steel material to evaluate the adhesive wear behavior. Characterization of the wear tracks was done by scanning electron microscopy in combination with energy-dispersive X-ray analysis and optical profilometry. The best abrasive wear resistance during testing against Al₂O₃ was observed for the coating with the highest Al content. In the case of the austenitic stainless steel balls, sticking of the ball material to the coating surface was the dominating wear mechanism. The influence of test temperature, chemical composition, and surface roughness was studied in detail.     

High-temperature dislocation plasticity in the single-crystal superalloy LEK94

The evolution of the dislocation structure that forms during uniaxial creep deformation in the single‐crystal superalloy LEK94 of low density and with Re additions was analysed using transmission electron microscopy. The material has a γ/γ′‐microstructure consisting of γ′‐cubes (L12 phase, 80 vol.%) separated by thin γ‐channels (face‐centred cubic). <100> tensile creep tests were performed at 980 and 1020 °C at stresses of 200 and 240 MPa. The microstructure was investigated at three characteristic stages of creep (directly after loading, at 5% strain and after rupture) to show the evolution of the dislocation structure during high‐temperature creep. It was found that in the early stages of creep, a₀/2<011> dislocations form within the γ‐channels. Later on, dislocation networks form and γ′ cutting processes with a₀/<001> superdislocations are observed. The results are in line with observations made for other superalloy single crystals in the high‐temperature low‐stress creep regime.     

Fabrication of a versatile substrate for finding samples on the nanometer scale

With increasing interest in nanometer scale studies, a common research issue is the need to use different analytical systems with a universal substrate to relocate objects on the nanometer scale. Our paper addresses this need. Using the delicate milling capability of a focused ion beam (FIB) system, a region of interest (ROI) on a sample is labelled via a milled reference grid. FIB technology allows for milling and deposition of material at the sub 20-nm level, in a similar user environment as a standard scanning electron microscope (SEM). Presently commercially available transmission electron microscope (TEM) grids have spacings on the order 100 μm on average; this technique can extend this dimension down to the submicrometre level. With a grid on the order of a few micrometres optical, FIBs, TEMs, scanning electron microscopes (SEMs), and atomic force microscopes (AFM) are able to image the ROI, without special chemical processes or conductive coatings required. To demonstrate, Au nanoparticles of ∼ 25 nm in size were placed on a commercial Formvar^®- and carbon-coated TEM grid and later milled with a grid pattern. Demonstration of this technique is also extended to bulk glass substrates for the purpose of sample location. This process is explained and demonstrated using all of the aforementioned analytical techniques.