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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

High resolution depth profiling using near-total-reflection hard x-ray photoelectron spectroscopy

By adjusting the incidence angle of incoming x rays near the critical angle of x-ray total reflection, photoelectron intensity is strongly modulated due to the variation of x-ray penetration depth. Photoelectron spectroscopy combined with near-total reflection exhibits tunable surface sensitivity, providing depth-resolved information. In this Review, we first describe the experimental setup and specific data analysis process. We then review three different examples that show the broad application of this method. Furthermore, the emphasis is on its applications correlated to oxide heterostructures, especially quantitative depth analyses of compositions and electronic states. In the last part, we discuss the limitations of this technique, mostly in terms of the range of samples that can be studied.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Improved quantitation of SIMS depth profile measurements of niobium via sample holder design improvements and characterization of grain orientation effects

The importance of SIMS analyses for “N-doped” impurity alloyed niobium and other surface-alloyed materials continues to increase. A major hurdle is the uncertainty of instrument calibration due to changes in sample height either from sample surface topography or from the sample holder itself. The CAMECA sample holder design allows for many types of samples to be analyzed. However, a drawback is that the holder faceplate can bend, contributing an uncertainty in the relative sensitivity factor (RSF) used to quantify the SIMS results. Here, we describe an improved sample holder having a reinforced faceplate, which prevents deflection and reduces uncertainty. Simulations show that the new design significantly reduces deflection from 10 μm to 5 nm. Sample measurements show a reduction of RSF uncertainty from this source from 4.1% to 0.95%. Grain orientation has long been suspected to affect RSF measurement as well. A bicrystal implant standard, consisting of randomly oriented and [001] grains, was successively rotated 15° between analyses. It was observed that 20% of the analyses performed on the randomly oriented grain exhibited anomalously high RSF values as well as slow sputter rates. These features were associated with the changing grain normal orientation with respect to the primary Cs + beam. The grain orientation associated with the rise in RSF was simulated and determined to be the [101] crystallographic plane, thus indicating that ion channeling was responsible for the significantly increased RSF. Focused ion beam analysis confirmed slower sputter rates for the cardinal crystallographic orientations, indicating that ion channeling occurred for each.

43 PARTICLE ACCELERATORS↗
NASA NTRS1994

A carbon-14 depth profile in the L5 chondrite Knyahinya

We report on a series of measurements of C-14 in samples of the L-chondrite Knyahinya, as a function of depth. The results show C-14 concentrations ranging from 37 to 58 dpm/kg. These measurements are compared to the levels of Ne-21, Be-10 and noble-gas ratios in this meteorite reported by Graf et al (1990). We also compare the C-14 data to the expected profile based on two sets of model calculations. The behavior of this radioisotope with depth is similar to that expected from the models, and good agreement with the profiles of other nuclides is also observed.

Jull, A. J. T.↗
NASA NTRS1973

Depth profile of Mn-53 in the lunar surface

Measurements of cosmic-ray produced Mn-53 are reported for a series of lunar surface samples down to a depth of 416 g/sq cm. These results clearly illustrate the decrease in activity with depth as the incident galactic cosmic rays are absorbed. Below 60 g/sq cm the production rate decreases exponentially with a mean length of about 220 g/sq cm. These results indicate that, at the Apollo 15 site, the lunar regolith has been unmixed, on a meter scale, for the last 5 m.y. The neutron activation technique for Mn-53, which allowed samples smaller than 200 mg to be used for these measurements, is described.

Imamura, M.↗
NASA NTRS1983

The XPS depth profiling and tribological characterization of ion-plated gold on various metals

Friction properties were measured with a gold film; the graded interface between gold and nickel substrate; and the nickel substrate. All sliding was conducted against hard silicon carbide pins in two processes. In the adhesive process, friction arises primarily from adhesion between sliding surfaces. In the abrasion process, friction occurs as a result of the hard pin sliding against the film, indenting into it, and plowing a series of grooves. Copper and 440 C stainless steel substrates were also used. Results indicate that the friction related to both adhesion and abrasion is influenced by coating depth. The trends in friction behavior as a function of film depth are, however, just the opposite. The graded interface exhibited the highest adhesion and friction, while the graded interface resulted in the lowest abrasion and friction. The coefficient of friction due to abrasion is inversely related to the hardness. The greater the hardness of the surface, the lower is the abrasion and friction. The microhardness in the graded interface exhibited the highest hardness due to an alloy hardening effect. Almost no graded interface between the vapor-deposited gold film and the substrates was detected.

Miyoshi, K.↗
NASA NTRS1983

Compositional depth profile of a native oxide LPCVD MNOS structure using X-ray photoelectron spectroscopy and chemical etching

It is pointed out that there is no report of an unambiguous analysis of the composition and interfacial structure of MNOS (metal-nitride oxide semiconductor) systems, despite the technological importance of these systems. The present investigation is concerned with a study of an MNOS structure on the basis of a technique involving the use of X-ray photoelectron spectroscopy (XPS) with a controlled stopped-flow chemical-etching procedure. XPS is sensitive to the structure of surface layers, while stopped-flow etching permits the controlled removal of overlying material on a scale of atomic layers, to expose new surface layers as a function of thickness. Therefore, with careful analysis of observed intensities at measured depths, this combination of techniques provides depth resolution between 5 and 10 A. According to the obtained data there is intact SiO2 at the substrate interface. There appears to be a thin layer containing excess bonds to silicon on top of the SiO2.

Wurzbach, J. A.↗
NASA NTRS1975

Reaction of sulfur dioxide with modified 440C, studied by Auger electron spectroscopy and depth profiling

Auger electron spectroscopy and sputtering were used to study the interaction of SO2 with modified 440C, which is a nominally 77-wt%-Fe, 14-wt%-Cr, and 4-wt%-Mo bearing steel with C, S, Si, Ni, V, P, and Mn making up the balance. The sample was polycrystalline. Three temperatures were used: room temperature, 500 C, and 600 C. The reaction time was varied from 30 minutes to 2 hours. A surface cleaned of oxides was the starting point for each reaction. For reactions at 500 C, the major constituents Cr, O, Fe, and S were present in the surface film. At 600 C, the principal constituents of the film were Cr, O, and S with no Fe present. Therefore, a transition in film composition occurred between 500 and 600 C. Oxides were the primary constituents of the films at both temperatures. Room-temperature reactions indicated that SO2 adsorbed dissociatively, with approximately equal quantities of S and O on the surface. For the same reaction time (1 hr) and pressure, a strong temperature dependence of film thickness was observed. The film formed at 600 C was approximately seven times thicker than that formed at 500 C.

Ferrante, J.↗
NASA NTRS1974

Depth profiles of Mn-53 in lunar rocks and soils

Results of measurements of cosmic-ray-produced Mn-53 taken down the length of the Apollo 16 deep drill core are presented. They indicate that the lunar regolith has been unmixed, on a meter scale, for the past 5 million years at the location of this core. The data are in agreement with earlier Mn-53 measurements on the Apollo 15 drill core. Mn-53 activity profiles in 14310, 12002, and 14321 are compared to each other; all three rocks have probably been on the lunar surface long enough to saturate their solar cosmic-ray-produced Mn-53 (half-life = 3.7 m.y.) activity.

Imamura, M.↗
NASA NTRS1977

Depositional history of core section 74001 - Depth profiles of maturity, FeO, and metal

Samples from every 0.5-cm interval of soil in core section 74001 have been studied by ferromagnetic resonance (FMR) and magnetic techniques. The values of the FMR maturity index show that the 74001 samples are very immature (the index ranges from 0.14 to 0.29 units) and have not seen appreciable, if any, surface exposure since their deposition. In fact, the small amount of fine-grained metal in the 74001 samples is probably not acquired as a result of their exposure to the micrometeoroid flux at the lunar surface. Thus, the black-glass soil of 74001 was deposited very rapidly, probably in a single episode or several closely spaced episodes of lunar fire fountaining. The average concentration of FeO and its standard deviation for all the 74001 samples are 22.5 + or - 0.3 wt.%. Since the FeO concentration is so uniform, no large variations in the major-element chemistry of 74001 are expected, with the possible exception of the volatile elements. The concentration of coarse-grained metal, which is measured magnetically, and its standard deviation are 0.15 + or - 0.01 wt.%. The coarse-grained metal probably precipitated contemporaneously with the silicate and oxide phases in the black-glass droplets.

Morris, R. V.↗
NASA NTRS1984

Be-10 and Cl-36 depth profiles in an Apollo 15 drill core

The present study of galactic cosmic ray production profiles by means of tandem accelerator mass spectrometry has measured cosmic ray-produced Be-10 and Cl-36, whose half-attenuation lengths are respectively calculated to be 120 and 132 g/sq cm. The measured half-attenuation lengths for Be-10 are noted to be slightly longer than predicted by the Reedy-Arnold (1972) theoretical model. Secondary thermal neutron production from Cl-35 is invoked as an explanation for the flatter and deeper maximum seen in the Cl-36 profile.

Nishiizumi, K.↗
NASA NTRS1984

Al-26 depth profile in Apollo 15 drill core

Accelerator mass spectrometry is used in a study of galactic cosmic ray production profiles based on cosmic ray-produced Al-26 in the Apollo 15 long core. The results, which are in general agreement with earlier nondestructive counting data, are of significantly higher precision, yet systematically lower. The half-attenuation length for Al-26 production is presently calculated to be 122 g/sq cm, after normalizing the data to average chemical composition.

Nishiizumi, K.↗
NASA NTRS1984

A simple method of obtaining concentration depth-profiles from X-ray diffraction

The construction of composition profiles from X-ray intensity bands was investigated. The intensity band-to-composition profile transformation utilizes a solution which can be easily evaluated. The technique can be applied to thin films and thick speciments for which the variation of lattice parameters, linear absorption coefficient, and reflectivity with composition are known. A deconvolution scheme with corrections for the instrumental broadening and ak-alfadoublet is discussed.

Wiedemann, K. E.↗