Quantitative Composition Maps of Magnetic Recording Media by EFTEM

1999 ◽  
Vol 5 (S2) ◽  
pp. 634-635 ◽  
Author(s):  
J. Bentley ◽  
J.E. Wittig ◽  
T.P. Nolan

Elemental mapping of Co-Cr-X based magnetic recording media at resolutions approaching 1 nm by energy-filtered transmission electron microscopy (EFTEM) can provide quantitative measurements of intergranular Cr segregation for correlation with magnetic properties and materials processing. The thin-film media present many challenges for EFTEM methods, such as diffraction contrast and closelyspaced edges. The goal of this work was to provide robust methods for mapping quantitative compositions in such materials. Results presented here are for a model material of 60 nm of Co84Cr12Ta4 on a 75 nm Cr underlayer; both films were d.c. magnetron sputtered onto a NiP-plated Al substrate pre-heated to 250°C. Other compositions and thinner layers (∼30 nm) have also been studied. EFTEM was performed on back-thinned, plan-view specimens with a Gatan Imaging Filter (GIF) interfaced to a 300 kV LaB6 Philips CM30. Optimized acquisition conditions have been detailed elsewhere. Besides core-loss image series, zero-loss I0 (slit width Δ=10eV), low-loss Ik (Δ=30eV), and unfiltered IT images were recorded, and maps of t/λ. = ln(IT / I0), where t is specimen thickness and λ. is the total inelastic mean free path, were produced.

1998 ◽  
Vol 517 ◽  
Author(s):  
J. Bentley ◽  
J.E. Wittig ◽  
T.P. Nolan

AbstractReliable core-loss spectroscopic methods have been developed for mapping elemental segregation in Co-Cr-X magnetic recording media by energy-filtered transmission electron microscopy. Extraction of quantitative compositions at a spatial resolution approaching 1 nm involves sophisticated treatments for diffraction contrast, variations in specimen thickness, and closely-spaced oxygen K and chromium L23 ionization edges. These methods reveal that intergranular chromium levels are ∼25 at.% for random-angle boundaries and ∼15 at.% for 90° boundaries in films of Co84Cr12Ta4 d.c. magnetron sputtered at 250°C.


2001 ◽  
Vol 7 (S2) ◽  
pp. 1140-1141
Author(s):  
J. Bentley ◽  
J.E. Wittig ◽  
J.F. Al-Sharab ◽  
N.D. Evans

The optimized performance of Co(CrTaPt) thin-film longitudinal magnetic recording media (for computer hard discs) depends critically on the grain size distribution and on intergranular Cr segregation that magnetically isolates the grains. These microstructural aspects of both model and commercial media have been extensively investigated at ∽1 nm resolution with quantitative elemental mapping by energy-filtered transmission electron microscopy (EFTEM) of Cr, Co, and O, but not Ta and Pt which unfortunately are not amenable to quantitative elemental mapping by EFTEM. Procedures for data acquisition and processing have been refined in order to provide robust methods for measuring intergranular compositions for statistically significant numbers of grains. Figure 1 shows results obtained with a Gatan imaging filter (GIF) interfaced to a LaB6 Philips CM30 for a carbon-capped 25-nm-thick film of Co80Cr16Ta4 grown on a Cr underlayer. Typical acquisition parameters have been described previously. to avoid the Cr underlayer, foil thicknesses t<0.2X are used, including the carbon overlayer (λ = inelastic mean free path ≌100 nm).


Author(s):  
R.F. Egerton ◽  
S.C. Cheng

Core-loss spectra of thicker specimens are strongly influenced by plural scattering. Plural inelastic events increase the background Ib underneath an ionization edge by an amount dependent on t/λ, t being the specimen thickness and λ the total-inelastic mean free path. However, plural scattering also contributes to the integral core-loss signal Ic. In fact, if the latter were integrated over a sufficiently large energy window Δ, the signal/background ratio (SBR=IC/Ib) might be expected to be independent of t.Figure 1 shows K-edge signal/background ratios for elemental carbon and silicon, presented as measured data points (for a collection semi-angle of l0mrad, 120keV incident energy and Δ=100eV) and as solid curves calculated by convolving a power-law edge profile with a delta-function approximation of the low-loss region. For silicon, SBR falls off more slowly with increasing t/λ, as expected from its higher edge energy. This trend is confirmed by measurements on amorphous silicon dioxide depicted in Fig.2, which shows the signal/background ratios of the oxygen and silicon K-edges as a function of thickness.


Author(s):  
Suichu Luo ◽  
John R. Dunlap ◽  
Richard W. Williams ◽  
David C. Joy

In analytical electron microscopy, it is often important to know the local thickness of a sample. The conventional method used for measuring specimen thickness by EELS is:where t is the specimen thickness, λi is the total inelastic mean free path, IT is the total intensity in an EEL spectrum, and I0 is the zero loss peak intensity. This is rigorouslycorrect only if the electrons are collected over all scattering angles and all energy losses. However, in most experiments only a fraction of the scattered electrons are collected due to a limited collection semi-angle. To overcome this problem we present a method based on three-dimension Poisson statistics, which takes into account both the inelastic and elastic mixed angular correction.The three-dimension Poisson formula is given by:where I is the unscattered electron intensity; t is the sample thickness; λi and λe are the inelastic and elastic scattering mean free paths; Si (θ) and Se(θ) are normalized single inelastic and elastic angular scattering distributions respectively ; F(E) is the single scattering normalized energy loss distribution; D(E,θ) is the plural scattering distribution,


Author(s):  
J. Bentley ◽  
E. A. Kenik ◽  
K. Siangchaew ◽  
M. Libera

Quantitative elemental mapping by inner shell core-loss energy-filtered transmission electron microscopy (TEM) with a Gatan Imaging Filter (GIF) interfaced to a Philips CM30 TEM operated with a LaB6 filament at 300 kV has been applied to interfaces in a range of materials. Typically, 15s exposures, slit width Δ = 30 eV, TEM magnifications ∼2000 to 5000×, and probe currents ≥200 nA, were used. Net core-loss maps were produced by AE−r background extrapolation from two pre-edge windows. Zero-loss I0 (Δ ≈ 5 eV) and “total” intensity IT (unfiltered, no slit) images were used to produce maps of t/λ = ln(IT/I0), where λ is the total inelastic mean free path. Core-loss images were corrected for diffraction contrast by normalization with low-loss images recorded with the same slit width, and for changes in thickness by normalization with t/λ, maps. Such corrected images have intensities proportional to the concentration in atoms per unit volume. Jump-ratio images (post-edge divided by pre-edge) were also produced. Spectrum lines across planar interfaces were recorded with TEM illumination by operating the GIF in the spectroscopy mode with an area-selecting slit oriented normal to the energy-dispersion direction. Planar interfaces were oriented normal to the area-selecting slit with a specimen rotation holder.


2014 ◽  
Vol 115 (17) ◽  
pp. 17B726 ◽  
Author(s):  
H. Z. Yang ◽  
Y. J. Chen ◽  
S. H. Leong ◽  
C. W. An ◽  
K. D. Ye ◽  
...  

1992 ◽  
Vol 114 (1) ◽  
pp. 61-67 ◽  
Author(s):  
V. J. Novotny ◽  
T. E. Karis ◽  
N. W. Johnson

Lubrication of particulate magnetic recording media improves their mechanical durability in sliding and flying by several orders of magnitude compared with unlubricated media. Lubricant removal, degradation, and recovery were studied using microslit scanning Fourier transform infrared spectroscopy and microspot scanning X-ray photoelectron spectroscopy. These techniques measure the total and surface lubricant amounts in the porous film, respectively. Lubricant dynamics were compared for two physisorbed polyperfluoroalkylether lubricants of similar molecular weight but different molecular structure—Y with a CF3 side group and Z with linear chains. The bulk viscosity of Y was about ten times higher than the viscosity of Z. In sliding, the lubricant removal rate of Y was significantly higher than that of Z while in flying the removal rates were reversed. Removal rates in sliding were orders of magnitude higher than those in flying. Effective lateral diffusion coefficients estimated from the rate of lubricant reflow back to the depleted tracks were close to inversely proportional to the bulk viscosity. During sliding and flying both lubricants degraded as evidenced by chemically altered lubricant detected on the surfaces after dissolution of undegraded lubricant.


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