Top-down design of magnonic crystals from bottom-up magnetic nanoparticles through protein arrays.

We show that chemical fixation enables top-down micro-machining of large periodic 3D arrays of protein-encapsulated magnetic nanoparticles (NPs) without loss of order. We machined 3D micro-cubes containing a superlattice of NPs by means of focused ion beam etching, integrated an individual micro-cube to a thin-film coplanar waveguide and measured the resonant microwave response. Our work represents a major step towards well-defined magnonic metamaterials created from the self-assembly of magnetic nanoparticles.

Preparation of location-specific thin foils from Fe-3% Si bi- and tri-crystals for examination in a FEG-STEM.

Bi-crystals and tri-crystals of a nominal Fe-3% Si (wt%) of well-defined orientations have been grown using a floating-zone technique with optical heating. The manufacture of these unique crystals and the preparation technique involved in harvesting thin foils from specific locations for transmission electron microscopy are described in detail. In particular, the grain boundary triple junction has been extracted from the tri-crystal and examined in high-resolution aberration-corrected FEG-STEM instruments. To achieve the necessary resolution, the foils have to be uniformly thin, in the range 50-100 nm over large areas of the specimen. For ferromagnetic materials, there are further challenges arising from the magnetic field interaction, with the electron beam placing significant demands on the aberration correction system. One way to minimise this interaction is to reduce the total mass of magnetic material. To achieve this, an in situ focused ion beam lift-out technique has been combined with an additional precision ion-polishing stage to reproducibly provide thin-foil specimens suitable for high-resolution EELS and EDX analysis. Examination of the foils reveals that the final precision ion-polishing stage removes residual damage arising from the use of focused ion beam milling procedures.

A comparison of two high spatial resolution imaging techniques for determining carbide precipitate type and size in ferritic 9Cr-1Mo steel.

Two high spatial resolution imaging techniques, focused gallium ion beam imaging in conjunction with XeF2 gas (FIB/XeF2) and high-speed atomic force microscopy (HS-AFM), were used to analyse 9Cr-1Mo ferritic steel samples, which had been exposed for extended periods to hot CO2 gas containing traces of CO, H2, H2O and CH4. The carbide precipitates embedded in the metal matrix were observed and their morphology, size and spatial distribution were quantified using these two techniques. The lower resolution of the FIB/XeF2 imaging technique suggested that small carbide precipitates (<50 nm) may be missed, while the existence of a limited flow layer introduced by sample preparation may influence the HS-AFM results. The gallium ion beam was used to remove a thin oxide layer of approximately 50 nm from sample surfaces prior to FIB/XeF2 imaging, avoiding the influence of surface contamination. HS-AFM provided higher resolution (∼5 nm) than FIB/XeF2 imaging. A quantitative comparison of the experimental data confirmed the value of both FIB/XeF2 and HS-AFM for imaging carbide precipitates, while clarifying their strengths and limitations.

The role of the surface chemistry of CoCr alloy particles in the phagocytosis and DNA damage of fibroblast cells.

Surface chemistry of CoCr particles is demonstrated to be fundamental to the process of phagocytosis by fibroblast cells in vitro. Particles preincubated in serum for 5 days and washed in water before addition to cell cultures were phagocytosed less readily than were particles preincubated in minimal essential medium (MEM) for 1 h and washed in water. This was explained by the coating of calcium phosphate and protein on the serum-immersed particles investigated by time-of-flight secondary ion mass spectroscopy. The cells incubated with the serum-immersed particles had a reduced mitotic index when compared with the MEM-immersed particles, indicating that the phagocytosed particles were causing cell cycle arrest. The release of soluble ions measured by electrothermal atomic absorption spectroscopy within the first hour of particle immersion in MEM was identified as the most likely cause for the DNA damage measured by single cell gel electrophoresis ("Comet" assay). Cryofocused ion beam SEM with a spatial resolution of 8 nm was used to cross section cells, to investigate the location of the phagocytosed particles, some of which were found within the nuclear membrane. This paper demonstrated that consideration of the surface chemistry is essential to understand the processes of the effects of orthopedic wear debris.

The entrapment of corrosion products from CoCr implant alloys in the deposits of calcium phosphate: a comparison of serum, synovial fluid, albumin, EDTA, and water.

Physical wear of orthopedic implants is inevitable. CoCr alloy samples, typically used in joint reconstruction, corrode rapidly after removal of the protective oxide layer. The behavior of CoCr pellets immersed in human serum, foetal bovine serum (FBS), synovial fluid, albumin in phosphate-buffered saline (PBS), EDTA in PBS, and water were studied using X-ray Photoelectron Spectroscopy (XPS) and Time-of-Flight Secondary Ion Mass Spectroscopy (ToF-SIMS). The difference in the corrosive nature of human serum, water, albumin in PBS and synovial fluid after 5 days of immersion was highlighted by the oxide layer, which was respectively 15, 3.5, 1.5, and 1.5 nm thick. The thickness of an additional calcium phosphate deposit from human serum and synovial fluid was 40 and 2 nm, respectively. Co and Cr ions migrated from the bulk metal surface and were trapped in this deposit by the phosphate anion. This may account for the composition of wear debris from CoCr orthopedic implants, which is known to consist predominantly of hydroxy-phosphate compounds. Known components of synovial fluid including proteoglycans, pyrophosphates, phospholipids, lubricin, and superficial zone protein (SZP), have been identified as possible causes for the lack of significant calcium phosphate deposition in this environment. Circulation of these compounds around the whole implant may inhibit calcium phosphate deposition.

The effects of calcium phosphate deposition upon corrosion of CoCr alloys and the potential for implant failure.

Physical wear of orthopedic implants is inevitable. CoCr metal samples, typically used in joint reconstruction, corrode rapidly after removal of the protective oxide layer. The behavior of CoCr pellets immersed in human serum, fetal bovine serum (FBS), synovial fluid, and water were studied using time-of-flight secondary ion mass spectroscopy (ToF-SIMS). The differences in the corrosive nature of human serum, FBS, synovial fluid, and water after 5 days immersion were highlighted by the oxide/hydroxide layer, which was, respectively, 25, 10, 1.5, and 3-3.5 nm thick. The thickness of calcium phosphate deposit from human serum, FBS, and synovial fluid was, respectively, 30, 20, and 2 nm. Co and Cr ions migrated from the bulk metal surface and were trapped in the serum deposits, where chromium existed as oxides, hydroxides, and phosphates, whereas the cobalt chemistry was dominated only by phosphates and hydroxides. This may account for the composition of wear debris from CoCr orthopedic implants, which are predominantly hydroxyphosphate compounds. From the literature, proteoglycans, pyrophosphates, phospholipids, lubricin, and superficial zone protein (SZP) have been identified as possible causes for the insignificant deposit of calcium phosphate from synovial fluid. Circulation of these compounds around the whole implant may inhibit calcium phosphate deposition and therefore contribute to osteolysis.

The oxidative corrosion of carbide inclusions at the surface of uranium metal during exposure to water vapour.

The reaction between uranium and water vapour has been well investigated, however discrepancies exist between the described kinetic laws, pressure dependence of the reaction rate constant and activation energies. Here this problem is looked at by examining the influence of impurities in the form of carbide inclusions on the reaction. Samples of uranium containing 600 ppm carbon were analysed during and after exposure to water vapour at 19 mbar pressure, in an environmental scanning electron microscope (ESEM) system. After water exposure, samples were analysed using secondary ion mass spectrometry (SIMS), focused ion beam (FIB) imaging and sectioning and transmission electron microscopy (TEM) with X-ray diffraction (micro-XRD). The results of the current study indicate that carbide particles on the surface of uranium readily react with water vapour to form voluminous UO(3) · xH(2)O growths at rates significantly faster than that of the metal. The observation may also have implications for previous experimental studies of uranium-water interactions, where the presence of differing levels of undetected carbide may partly account for the discrepancies observed between datasets.

A new detection system for extremely small vertically mounted cantilevers.

Detection techniques currently used in scanning force microscopy impose limitations on the geometrical dimensions of the probes and, as a consequence, on their force sensitivity and temporal response. A new technique, based on scattered evanescent electromagnetic waves (SEW), is presented here that can detect the displacement of the extreme end of a vertically mounted cantilever. The resolution of this method is tested using different cantilever sizes and a theoretical model is developed to maximize the detection sensitivity. The applications presented here clearly show that the SEW detection system enables the use of force sensors with sub-micron size, opening new possibilities in the investigation of biomolecular systems and high speed imaging. Two types of cantilevers were successfully tested: a high force sensitivity lever with a spring constant of 0.17 pN nm(-1) and a resonant frequency of 32 kHz; and a high speed lever with a spring constant of 50 pN nm(-1) and a resonant frequency of 1.8 MHz. Both these force sensors were fabricated by modifying commercial microcantilevers in a focused ion beam system. It is important to emphasize that these modified cantilevers could not be detected by the conventional optical detection system used in commercial atomic force microscopes.

Small Fermi surface pockets in underdoped high temperature superconductors: observation of Shubnikov-de Haas oscillations in YBa2Cu4O8.

We report the observation of Shubnikov-de Haas oscillations in the underdoped cuprate superconductor YBa2Cu4O8 (Y124). For fields aligned along the c axis, the frequency of the oscillations is 660+/-30 T, which corresponds to approximately 2.4% of the total area of the first Brillouin zone. The effective mass of the quasiparticles on this orbit is measured to be 2.7+/-0.3 times the free electron mass. Both the frequency and mass are comparable to those recently observed for ortho-II YBa2Cu3O6.5 (Y123-II). We show that although small Fermi surface pockets may be expected from band-structure calculations in Y123-II, no such pockets are predicted for Y124. Our results therefore imply that these small pockets are a generic feature of the copper oxide plane in underdoped cuprates.

Anomalous scaling for thick electrodeposited films.

Anomalous surface roughness scaling, where both the local and the large-scale roughness show a power-law dependence on the film thickness, has been widely observed. Here we show that the value of the local roughness exponent in the early stages of Cu electrodeposition depends on the deposition potential. However, initial anomalous scaling can lead to two qualitatively different types of behavior for large film thickness (t>/ or =4 microm). For Cu films electrodeposited with forced convection at high potential and current density, the anomalous scaling is transient: the local roughness saturates for the thickest films studied. When Cu films are electrodeposited at similar potential and current density but with reduced convection, no saturation of the local roughness is observed. Instead the film forms overhangs such that the surface height becomes a multivalued function of the lateral position.

Angular dependence of domain wall resistivity in artificial magnetic domain structures.

We exploit the ability to precisely control the magnetic domain structure of perpendicularly magnetized Pt/Co/Pt trilayers to fabricate artificial domain wall arrays and study their transport properties. The scaling behavior of this model system confirms the intrinsic domain wall origin of the magnetoresistance, and systematic studies using domains patterned at various angles to the current flow are excellently described by an angular-dependent resistivity tensor containing perpendicular and parallel domain wall resistivities. We find that the latter are fully consistent with Levy-Zhang theory, which allows us to estimate the ratio of minority to majority spin carrier resistivities, rho downward arrow/rho upward arrow approximately 5.5, in good agreement with thin film band structure calculations.

Analysis of boron-10 in soft tissue by dynamic secondary ion mass spectrometry.

We report here a preliminary study in which dynamic secondary ion mass spectrometry (SIMS) has provided images of boron-10 (10B) in biological tissue as used in research into boron neutron capture therapy. Cultured tumour cells incubated in media containing known concentrations of a 10B-containing compound, p-boronophenylalanine (BPA), and intracranial tumour tissue from animals previously injected with BPA were analysed by an in-house constructed SIMS. Investigations were conducted in positive secondary ion detection mode using a 25-keV, 5-nA gallium primary ion source. For calibration purposes, tissue standards were also analysed and their boron-to-carbon signal ratios correlated to bulk boron concentrations measured by inductively coupled plasma atomic emission spectroscopy (ICP-AES). Ion maps of 10B, 12C, 23Na and 39K showing gross tissue and cell features were acquired. SIMS and ICP-AES standard measurements were in good agreement. Tissue regions with high or low 10B concentrations were identified along with 10B hotspots in normal brain areas. Cultured cells revealed the intracellular localization of 10B. SIMS is capable of producing images showing the distribution of 10B at p.p.m. levels in cells and in normal and tumour-bearing brain tissue.