Thickness determination for Cu and Ni nanolayers: Comparison of completely reference-free fundamental parameter-based X-ray fluorescence analysis and X-ray reflectometry

Kolbe, Michael; Beckhoff, Burkhard; Krumrey, Michael; Ulm, G.

doi:10.1016/j.sab.2005.03.018

Cited by 83 publications

(69 citation statements)

References 18 publications

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“…The present cleaning methods [2] do this adequately for relatively inert materials such as SiO 2 . With suitable experimental design, other thickness traceable methods, such as stylus methods [22] , transmission electron microscopy (TEM) [2,23] or XRF analysis, [24] not used in the present work, could also be added to the wavelength methods.…”

Section: Discussionmentioning

confidence: 99%

Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si

Seah

Unger

Wang³

et al. 2009

Surface & Interface Analysis

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Results from a study conducted between National Metrology Institutes (NMIs) for the measurements of the absolute thicknesses of ultra-thin layers of SiO 2 on Si are reported. These results are from a key comparison and associated pilot study under the auspices of the Consultative Committee for Amount of Substance. 'Amount of substance' may be expressed in many ways, and here the measurand is the thickness of the silicon oxide layers with nominal thicknesses in the range 1.5-8 nm on Si substrates, expressed as the thickness of SiO 2 . Separate samples were provided to each institute in containers that limited the carbonaceous contamination to approximately <0.3 nm. The SiO 2 samples were of ultra-thin on (100) and (111) orientated wafers of Si. The measurements from the laboratories which participated in the study were conducted using ellipsometry, neutron reflectivity, X-ray photoelectron spectroscopy or X-ray reflectivity, guided by the protocol developed in an earlier pilot study. A very minor correction was made in the different samples that each laboratory received. Where appropriate, method offset values attributed to the effects of contaminations, from the earlier pilot study, were subtracted. Values for the key comparison reference values (agreed best values from a Consultative Committee study) and their associated uncertainties for these samples are then made from the weighted means and the expanded weighted standard deviations of the means of these data. These results show a dramatic improvement on previous comparisons, leading to 95% uncertainties in the range 0.09-0.27 nm, equivalent to 0.4-1.0 monolayers over the 1.5-8.0 nm nominal thickness range studied. If the sample-to-sample uncertainty is reduced from its maximum estimate to the most likely value, these uncertainties reduce to 0.05-0.25 nm or ∼1.4% relative standard uncertainties. The best results achieve ∼1% relative standard uncertainty. It is concluded that XPS has now been made fully traceable to the SI, for ultra-thin thermal SiO 2 on Si layers, by calibration using wavelength methods in an approach that may be extended to other material systems.

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Section: Discussionmentioning

confidence: 99%

Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si

Seah

Unger

Wang³

et al. 2009

Surface & Interface Analysis

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“…The x-ray spectrometry group of PTB operates several XRF endstations [44,45], which are equipped with radiometrically calibrated instrumentation and thus allow for a reference-free quantitative XRF analysis [46]. By employing both transmission and XRF experiments on free-standing thin-foil samples, the reference-free XRF setups of PTB also allow for an experimental determination of FPs [47][48][49].…”

Section: Methodsmentioning

confidence: 99%

“…Using the Sherman equation for a thin sample [44] we can calculate the measured count rate CR S n ,S n of an x-ray line corresponding to an electron decaying to subshell S n from subshell S n with the corresponding photon energy E S n ,S n as follows:…”

Section: A Nickel L-shell Fluorescence Yields and Coster-kronig Factorsmentioning

confidence: 99%

Theoretical and experimental determination of K - and L -shell x-ray relaxation parameters in Ni

et al. 2018

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Fluorescence yields (FY) for the Ni K and L shells were determined by a theoretical and an experimental group within the framework of the International Initiative on X-ray Fundamental Parameters (FPs) collaboration. CosterKronig (CK) parameters were also measured for the L shell of Ni. Theoretical calculations of the same parameters were performed using the Dirac-Fock method, including relativistic and QED corrections. The experimental values for the FY and CK were determined at the PTB laboratory in the synchrotron radiation facility BESSY II, Berlin, Germany, and are compared to the corresponding calculated values.

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“…The quantification approach relies on the correlation between the mass deposition of an element in an area to its fluorescence intensity [3]. A reference based quantification scheme is applied.…”

Section: Surface Analysis By Combined Xrf and Xps Measurementsmentioning

confidence: 99%

Surface analysis by XRF and XPS for the Avogadro constant and the realization of the kilogram based on silicon spheres

Beyer

Kolbe

Müller

et al. 2017

Ukrainian Metrological Journal

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The determination of the Avogadro constant for the redefinition of the SI unit kilogram as well as the eventual realization of the kilogram by monocrystalline enriched 28 Si-spheres require a reliable surface analysis on silicon spheres. A novel instrumentation for the quantitative surface analysis of silicon spheres combines X-ray fluorescence spectroscopy and X-ray photoelectron spectroscopy techniques in order to enable the characterization and quantification of the oxide layer and unintentional contaminations. The analysis relies on the combination of the complementary X-ray methods. Measurements on 28 Si-spheres were carried out. The surface was characterized regarding the elementary composition including the chemical binding states of the components and the mass of the surface layer

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Thickness determination for Cu and Ni nanolayers: Comparison of completely reference-free fundamental parameter-based X-ray fluorescence analysis and X-ray reflectometry

Cited by 83 publications

References 18 publications

Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si

Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si

Theoretical and experimental determination of K - and L -shell x-ray relaxation parameters in Ni

Surface analysis by XRF and XPS for the Avogadro constant and the realization of the kilogram based on silicon spheres

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Thickness determination for Cu and Ni nanolayers: Comparison of completely reference-free fundamental parameter-based X-ray fluorescence analysis and X-ray reflectometry

Cited by 83 publications

References 18 publications

Ultra‐thin SiO2 on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO2 on Si

Ultra‐thin SiO2 on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO2 on Si

Theoretical and experimental determination of K - and L -shell x-ray relaxation parameters in Ni

Surface analysis by XRF and XPS for the Avogadro constant and the realization of the kilogram based on silicon spheres

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Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si

Ultra‐thin SiO₂ on Si IX: absolute measurements of the amount of silicon oxide as a thickness of SiO₂ on Si