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1.
Phenomena accompanying electrochemical doping of solid fullerene films with potassium were studied by sputter ion depth profiling
(XPS and SIMS). The potassium distribution was determined, and artifacts associated with possible damage of the layer composition
caused by ion impact were investigated and discussed. To compare the charge transfer while reductive doping is taking place
at fullerene/solution interface with doping from gas phase, model layers were prepared and doped by potassium under UHV conditions.
It was found that sputtering by Ar+ primary ions yields both accurate information on the alkaline metal distribution and on its concentration. Sputtering by
O+ ions led to an enrichment of potassium, apparently due to the reactivity of oxygen with the fullerene matrix. It is shown
that the reductive doping starts at the fullerene/solution interface. The concentration of potassium in the doped films was
found to be lower than expected from the charge transferred during the electrochemical reduction. Other phase transformations
such as hydrogenation are discussed.
Received March 4, 2002; accepted July 26, 2002 相似文献
2.
Alexander G. Fitzgerald Yongchang Fan Phillip John Clare E. Troupe John I. B. Wilson Anthony O. Tooke Brian E. Storey 《Mikrochimica acta》2000,132(2-4):315-321
The characteristics of the interface microstructures between a CVD diamond film and the silicon substrate have been studied
by transmission electron microscopy and electron energy loss spectroscopy. The investigations are performed on plan-view TEM
specimens which were intentionally thinned only from the film surface side allowing the overall microstructural features of
the interface to be studied. A prominent interfacial layer with amorphous-like features has been directly observed for CVD
diamond films that shows a highly twinned defective diamond surface morphology. Similar interfacial layers have also been
observed on films with a <100> growth texture but having the {100} crystal faces randomly oriented on the silicon substrate.
These interfacial layers have been unambiguously identified as diamond phase carbon by both electron diffraction and electron
energy loss spectroscopy. For the CVD diamond films that exhibit heteroepitaxial growth features, with the {100} crystal faces
aligned crystallographically on the silicon substrate, such an interfacial layer was not observed. This is consistent with
the expectation that the epitaxial growth of CVD diamond films requires diamond crystals to directly nucleate and grow on
the substrate surface or on an epitaxial interface layer that has a small lattice misfit to both the substrate and the thin
film material. 相似文献
3.
Thomas Kolber Kurt Piplits Leopold Palmetshofer Herbert Hutter 《Mikrochimica acta》2000,135(1-2):105-111
The distribution of the relevant elements within TiN coatings, made with two different physical deposition methods as the
conventional dc vacuum arc method and the filtered high current pulsed arc method (Φ-HCA) are characterized and finally compared.
Despite the rougher surface of the dc-arc produced TiN layer, which is due to accumulated droplets, there is no evidence of
different stoechiometric composition of Ti and N on the surface. The interface of the dc-arc produced TiN layer (600 nm) is
10 times wider than the one made with the new filtered high current pulsed arc method (60 nm). However the TiN layer made
by Φ-HCA shows an inhomogeneous distribution of aluminum and chlorine in the vertical direction, whereas the dc-arc sample
is homogeneous. Furthermore, the TiN layer made by Φ-HCA shows vertically an obvious local maximum of chlorine at a depth
of about 130 nm. This vertical local maximum has an homogeneous distribution in horizontal direction, which means that a thin,
chlorine enriched layer has been incorporated inside the TiN layer. Nevertheless, quantification by SIMS shows that aluminum
as well as chlorine concentrations of both samples are too low to influence any TiN properties.
Received January 3, 2000. Revision April 4, 2000. 相似文献
4.
Vacuum deposited films of immiscible metal–metal systems can be applied as tribological coatings for plain bearings in high
performance diesel engines. These industrially manufactured coatings show higher lifetimes than conventional electroplated
coatings. For our investigations we used aluminum-tin coatings of 1 μm thickness on a glass substrate produced by sequential
deposition from two separate targets under working gas pressure of 0.4 Pa. The tough Al matrix takes high mechanical loads
and the soft inclusions of Sn act as solid lubricant. While Sn is deposited it migrates on the Al surface and grows as islands.
We characterized the conformation and the distribution of the Sn islands on the surface and to the interstitial area between
the islands with 3-D secondary ion mass spectroscopy (SIMS). The existence of a Sn layer between the islands (“wetting layer”)
has been detected by SIMS and verified by measurements with Auger electron spectroscopy (AES). 相似文献
5.
Yongchang Fan Alexander G. Fitzgerald Phillip John Clare E. Troupe John I. B. Wilson 《Mikrochimica acta》2000,132(2-4):435-441
The surface morphology and electronic properties of as-deposited CVD diamond films and the diamond films which have been
subjected to boron ion implantation or hydrogen plasma etching have been systematically studied by high resolution scanning
probe microscopy and spectroscopy techniques. AFM and STM image observations have shown that (a) both the as-deposited CVD
diamond films and the boron ion implanted films exhibit similar hillock morphologies on (100) crystal faces and these surface
features are formed during the deposition process; (b) boron ion implantation does not cause a discernible increase in surface
roughness; (c) atomic flatness can be achieved on crystal faces by hydrogen plasma etching of the film surface. Scanning tunnelling
spectroscopy analysis has indicated that (a) the as-deposited diamond films and the hydrogen plasma etched diamond films possess
typical p-type semiconductor surface electronic properties; (b) the as-deposited diamond films subjected to boron implantation
exhibit surface electronic properties which change from p-type semiconducting behaviour to metallic behaviour; (c) the damage
in the boron implanted diamond films is restricted to the surface layers since the electronic properties revert to p-type
on depth profiling. 相似文献
6.
Sabine Dreer Peter Wilhartitz Kurt Piplits Herbert Hutter Michael Kopnarski Gernot Friedbacher 《Mikrochimica acta》2000,133(1-4):75-87
Silicon- and aluminium oxynitride films have gained attention because of their interesting properties in various fields of
technology. The specific properties strongly depend on the concentration of oxygen and nitrogen in the films. For the quantitative
analysis of homogeneous silicon- and aluminium oxynitride films, EPMA has been proven a very reliable and precise method of
analysis. In order to characterise films with graded composition or interface effects between the film and the substrate it
is necessary to use sputter depth profiling techniques such as SIMS, hf-SNMS, AES, or hf-GD-OES. Unfortunately, stoichiometric
silicon- and aluminium oxynitride films are insulating and therefore charge compensation has to be applied.
For the quantification it was necessary to prepare calibration samples which have been analysed by different bulk analytical
techniques such as NRA, RBS and EPMA. With these calibration samples, sensitivity factors have been determined and the functional
dependence of the sensitivity factors on the composition has been derived. The advantages and disadvantages of the different
sputtering techniques and the applicability of the obtained sensitivity functions for the quantitative depth profiling of
silicon- and aluminium oxynitride films are discussed. 相似文献
7.
The content and the three dimensional distribution of impurities play an important role in the production process of high
purity rhenium powder (99.99% purity grade) and for its further use as alloying and coating agent in high temperature applications.
In this paper the characterization of raw Re granulate, Re powder, cleaned by heat treatment, Re coatings, produced by most
common preparation methods (PVD and VPS) and PM Re by means of SIMS is presented. The analysis of the three dimensional distribution
of trace elements is performed by 3D SIMS. The quantification of carbon, which was not possible with other analytical techniques
as a result of the high volatility of Re2O7 until now, has been carried out by SIMS depth profile analysis. It is discussed if internal standards, produced by introduction
of defined amounts of carbon soot to the Re powder lead to useful results. 相似文献
8.
Recently, interest in steel alloyed with∼1% Al increased. These materials are expected to show a higher resistance against
oxidation at high temperatures which will improve their performance when used as high-speed-steels. Furthermore, efforts have
been made to combine the advantages of Al-steels with those of powder-metallurgic methods like hotisostatic-pressing (hip).
This should result in a better macro- and microscopic homogeneity of the distribution of all compounds, yielding less waste-production
and a longer life-time of products.
In order to gain deeper insights in the process of “hipping” of the considered material and to see the distribution of both
main as well as trace components, 2D and 3D-SIMS measurements of the material were performed before and after having undergone
the hip process.
The measurements showed enrichments of Na, K, Mg, Ca, and S at the particle boundaries before as well as after the hip-process.
In the hipped material, the enrichments are significantly stronger in the spatial domains in-between larger particles. They
also reveal, that the concentration of C is not equal in all particles and that the particles are covered with an Al2O3-layer which is not dispersed by the hip-process. There were also found small (∼50–100 nm) nitride-precipitates before as
well as after the hip-process. 相似文献
9.
Secondary ion mass spectrometry (SIMS) was optimised for characterisation of uranium- and plutonium-containing particles
in soils, swipes and forensic samples. This was done by analysing in-house produced spherical UO2-particles. Screening techniques as α-autoradiography together with SIMS analysis were employed to detect UO2-particles in a soil sample from Chernobyl.
The use of SIMS was exploited for the identification of uranium- and plutonium-containing particles and for the determination
of their isotopic composition. The particles collected on swipe samples were transferred to a special adhesive support for
the analysis by SIMS. Particles containing highly enriched uranium with diameters up to 10 μm were also detected in a forensic
sample. For the measurements of the isotopic ratios a mass resolution of 1000 was used. At this resolution flat-top peaks
were obtained which greatly improve the accuracy of the measurement. The isotopic composition of the particles was measured
with a typical accuracy and precision of 0.5%. Statistically meaningful results can be obtained, for instance, from a specimen
containing as few as 1010 atoms/μm3 of uranium in particles of UO2 weighing a few picograms. 相似文献
10.
In the last years the development of light emitting electrochemical cells on a polymer base has made a great progress. They
are extremely interesting due to their low cost, but still, problems concerning the stability and lifetime of these elements
remain.
The performance of light-emitting electrochemical cells (LEC) is strongly influenced by the inhomogeneous distribution of
the three main components (light emitting polymer, ion conductive polymer, ionic molecules) in the device. The local ions
distribution of lithium and triflate (short for the CF3SO3
− species) ions in a blend with the ionic conducting polymer poly(ethylene oxide) (PEO) and the conjugated polymer m-LPPP (methyl
substituted poly(para phenylene)) throughout the polymer layer has been investigated by secondary ion mass spectroscopy (SIMS).
Different combinations of top- and base-electrodes have been investigated and have been found to influence the distribution
of the ions strongly.
Received January 13, 1999. Revision June 16, 2000. 相似文献
11.
Markus Pidun Norbert Lesch Silvia Richter Peter Karduck Wolfgang Bock Michael Kopnarski Peter Willich 《Mikrochimica acta》2000,132(2-4):429-434
A solar control coating was analysed by different methods of surface analysis with respect to the layer sequence and the
composition and thickness of each sublayer. The methods used for depth profiling were Auger electron spectroscopy, electron
probe microanalysis, secondary neutral mass spectroscopy and secondary ion mass spectroscopy based on MCs+. The structure of the coating was unknown at first. All methods found a system of two metallic Ag layers, embedded between
dielectric SnOX layers. Additionally, thin Ni-Cr layers of 1–2 nm were detected on top of the Ag layers. Thus the detected layer sequence
is SnOX/Ni-Cr/Ag/SnOX/Ni-Cr/Ag/SnOX/glass. The Ni:Cr ratio in the nm-thin layers could be quantified by every method, the Cr fraction corresponding to less than
one monolayer. We compare the capabilities and limitations of each method in routinely investigating this solar control coating.
Importance was attached to an effective investigation. Nevertheless, by combining all methods, measuring artefacts could be
uncovered and a comprehensive characterisation of the system was obtained. 相似文献
12.
Torsten Barfels Bernd Schmidt Andreas von Czarnowski Hans-Joachim Fitting 《Mikrochimica acta》2002,139(1-4):11-16
For investigation of the luminescent center profile cathodoluminescence measurements are used under variation of the primary
electron energy E
0 = 2…30 keV. Applying a constant incident power regime (E
0·I
0 = const), the depth profiles of luminescent centers are deduced from the range of the electron energy transfer profiles dE/dx.
Thermally grown SiO2 layers of thickness d = 500 nm have been implanted by Ge+-ions of energy 350 keV and doses (0.5–5)1016 ions/cm2. Thus Ge profiles with a concentration maximum of (0.4 – 4) at% at the depth of dm≅240 nm are expected. Afterwards the layers have been partially annealed up to T
a = 1100 °C for one hour in dry nitrogen. After thermal annealing, not only the typical violet luminescence (λ = 400 nm) of
the Ge centers is strongly increased but also the luminescent center profiles are shifted from about 250 nm to 170 nm depth
towards the surface. This process should be described by Ge diffusion processes, precipitation and finally Ge nanocluster
formation. Additionally, a Ge surface layer is piled-up extending to a depth of roughly 25 nm. 相似文献
13.
Gabriele Tamborini Maria Wallenius Olivier Bildstein Leena Pajo Maria Betti 《Mikrochimica acta》2002,139(1-4):185-188
Methodologies based on secondary ion mass spectrometry (SIMS) for isotopic measurements in nuclear forensic applications
relevant to the age determination of Pu particles and isotopic composition of oxygen for geolocation assignment are described.
For the age determination of Pu particles, a relative sensitivity factor (RSF) to correct for the different ionisation efficiencies
of U and Pu, was obtained by analysing standard Pu materials with known ages. An RSF of 2.41±0.05 was obtained for PuO2 from measurements on samples with different Pu/U ratios. In a sample of known origin, using this RSF value, the age calculated
from the 238Pu/234U and 240Pu/236U ratios agreed well with the reported age of 2.3 years. For geolocation assignment, a new approach based on the measurement
of differences in the natural abundance of 18O and 16O isotopes and their ratio was developed. The instrumental mass discrimination of the 18O/16O ratio was determined using three O-isotope samples of different chemical composition. The measured precision (the standard
error of 100 cycles/analysis) obtained for the oxygen isotopic measurement on the samples was typically ±1.1‰. 相似文献
14.
We use a multiple-analytical approach based on secondary-ion mass-spectrometry (SIMS), X-ray single-crystal structure refinement
(SREF) and electron-probe micro-analysis (EPMA) to derive the complete crystal-chemical formula of a B-rich kornerupine-group
mineral, prismatine, from Hrarigahy, Madagascar: (Ca0.01Li0.02Mg0.20Fe2+
0.10) (Mg3.57Fe2+
0.06 Al5.37) (Si3.84B0.91Al0.26)O21 (OH1.08F0.07). SIMS matrix effects related to crystal structure were investigated by analyzing two grains with a known crystallographic
orientation relative to the ion beam.
Boron orders at the T3 site. The refined site-scattering for T3, 6.33 eps (electrons per site) agrees well with the mean bond-length for this site (1.512 ?), which indicates nearly complete
occupancy by B (85% rel.). B2O3 (∼ 4 wt%), derived by SREF, agrees with the SIMS data within analytical uncertainty using Si as the inner reference for the
matrix. The occupancy of the X site obtained by combining the SIMS and EPMA data (5.30 eps; electrons per site) agrees with the refined site-scattering
value (5.75 eps). Trace quantities of Li and Ca are ordered at this site. SIMS data for H2O is in accord with the stoichiometric value, indicating complete occupancy at O10 by OH. Fluorine (∼ 0.17 wt%) orders at O10: it corresponds to ∼ 0.07 atoms per formula unit (apfu) vs. 0.15 apfu (atoms per formula unit) by SREF, indicating a slight
overestimation of F with SREF, as previously observed in fluoborite.
Our data show that SIMS chemical matrix effects are well-calibrated, and emphasize the usefulness of independent micro-analytical
techniques in testing the mutual accuracy and consistency of experimental data. 相似文献
15.
Masashi Nojima Masayuki Toi Ayaka Maekawa Takeshi Yamamoto Tetsuo Sakamoto Masanori Owari Yoshimasa Nihei 《Mikrochimica acta》2006,155(1-2):219-223
Shave-off depth profiling completely differs from ultra shallow depth profiling and has an absolute depth scale and a 50 μm
wide dynamic range. In this paper we report on shave-off depth profiling of a nano-device with a complex nano-structure consisting
of dynamic random access memory and introduces an analytical tool for advancing of nano-devices. 相似文献
16.
Silica sol-gel single layer AR coatings are used in high peak power pulsed lasers due to their high laser induced damage threshold (LIDT) and their low refractive index (1.22). We have used sol-gel processing to spin and dip coat multilayers of alternating high index (zirconia/hafnia) and low index (base catalysed silica) sol-gels on to fused silica substrates. When tailored at the correct thickness these stacks have shown >95% reflectivity at 355 nm and normal incidence whilst retaining a high LIDT. Depth profiling using Dynamic Secondary Ion Mass Spectrometry (DSIMS) and Rutherford back scattering (RBS) through these multilayer coatings has revealed the effect of increasing the number of layers in the stack. Results are presented for both spin and dip coated multilayers and a significant difference in the interfacial boundary is seen between the two coating processes. These differences are related to changes in the LIDT of the coatings. Individual layer thicknesses were estimated using this technique and compared to values gained from UV-Visible spectroscopy. TEM analysis of an ion-milled cross-section of the multilayers was performed showing the colloidal silica coatings and the depth of interpenetration of the interfaces. 相似文献
17.
A. G. Shard P. J. Brewer F. M. Green I. S. Gilmore 《Surface and interface analysis : SIA》2007,39(4):294-298
Sputter‐depth profiles of model organic thin films on silicon using C60 primary ions have been employed to measure sputtering yields and depth resolution parameters. We demonstrate that some materials (polylactide, Irganox 1010) have a constant and high sputtering yield, which varies linearly with the primary ion energy, whereas another material (Alq3) has lower, fluence‐dependent sputtering yields. Analysis of multi‐layered organic thin films reveals that the depth resolution is a function of both primary ion energy and depth, and the sputtering yield depends on the history of sputtering. We also show that ~30% of repeat units are damaged in the steady‐state regime during polylactide sputtering. Crown Copyright © 2006. Reproduced with the permission of Her Majesty's Stationery Office. Published by John Wiley & Sons, Ltd. 相似文献
18.
Electrospray droplet impact (EDI) was applied to the analysis of peptides. The etching rate of bradykinin was estimated to be ~2 nm/min. This value is about one order of magnitude greater than the etching rate for SiO2 (0.2 nm/min). Considering that the etching rate of argon cluster ions Ar700+ for organic compounds is more than two orders of magnitude larger than that for inorganic materials, the rather small difference in etching rates of EDI for organic and inorganic materials is unique. When water/ethanol (1/1, vol%) solution of gramicidin S and arginine was dried in air, [gramicidin S + H]+ was observed as a predominant signal with little [Arg + H]+ right after the EDI irradiation, indicating that EDI is capable of detecting the analytes enriched on the sample surface. Copyright © 2011 John Wiley & Sons, Ltd. 相似文献
19.
The present paper focuses on the characterisation of surface composition and alloying element in-depth distribution of water-atomised
Al–Zn–Mg–Cu alloy powders by secondary ion mass-spectrometry and Auger electron spectroscopy. A pronounced segregation of
Mg and some impurities (Fe, Ca, S) concurrently with some Zn depletion are observed on the powder surface. The oxide film
formed on the powder surface mainly consists of Al and Mg oxides. The film is non-uniform in thickness: rather coarse surface
oxide islands coexist with surface areas covered by a thin (<1.8 nm) oxide layer. The extent of surface oxidation is strongly
affected by solidification conditions: The average thickness of the surface oxides increases with increasing particle size
or with decreasing cooling rate. All alloying elements are homogeneously distributed in the bulk of individual particles.
No significant differences in chemical composition between different particles of a given powder are observed.
Received November 26, 1999. Revision September 25, 2001. 相似文献
20.
Stanislav Kúdela Steffen Oswald Stanislav Kúdela Jr. Stefan Baunack Klaus Wetzig 《Mikrochimica acta》2000,133(1-4):29-34
Fibre/matrix interfaces in δ-Al2O3/Mg8Li and δ-Al2O3/Mg composites have been investigated using XPS and SIMS analysis of extracted δ-Al2O3 fibres in context with previous XRD observations. Results obtained indicate that in MgLi based composites lithium enters
preferentially the interfacial redox reactions producing Li+ ions that occupy vacant cation positions in the defect δ-Al2O3 lattice which results in a strong fibre/matrix interfacial bond. On the other hand, in Mg matrix composites the magnesium
oxide appears to be the final reaction product that does not enter the solid state reaction with adjacent δ-Al2O3 fibre during the melt infiltration process, so that only relatively weak interfacial bond is created. 相似文献