Burkhard Beckhoff

Burkhard Beckhoff
Physikalisch-Technische Bundesanstalt | PTB · Department 7.2 Cryophysics and Spectrometry

Dr.

About

299
Publications
39,737
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Introduction
Characterization of nanoelectronics and energy materials using X-ray spectrometry The development of novel materials in nanoelectronics and for energy storage and conversion require reliable spatial information on the elemental composition and chemical binding states of these materials that can be revealed by X-Ray Spectrometry (XRS). Reference-free XRS methods using calibrated instrumenation can substantially compensate for the current lack of appropriate reference materials at the nanoscale.
Additional affiliations
March 1997 - present
Physikalisch-Technische Bundesanstalt
Position
  • Head of Department

Publications

Publications (299)
Article
The comparability and reliability of the analysis of the electronic structure of selected cyanates and thiocyanates at the nitrogen K edge based on BSE calculations have been investigated in this work. Using high-resolution x-ray spectroscopy with calibrated instrumentation reliable and reproducible experimental results for x-ray absorption spectro...
Article
Full-text available
Self-assembled monolayers (SAM) of 7-mercapto-4-methylcoumarin (MMC) on a flat gold surface were studied by molecular dynamics (MD) simulations, reference-free grazing incidence X-ray fluorescence (GIXRF) and X-ray photoelectron spectroscopy (XPS), to determine the maximum monolayer density and to investigate the nature of the molecule/surface inte...
Article
The knowledge of atomic fundamental parameters, such as the fluorescence yields with low uncertainties, is of decisive importance in elemental quantification involving X-ray fluorescence analysis techniques. However, especially for the low-Z elements, the available data in the literature is either of poor quality, of unknown or very large uncertain...
Article
Full-text available
Traceable characterization methods allow for the accurate correlation of the functionality or toxicity of nanomaterials with their underlaying chemical, structural or physical material properties. These correlations are required for the directed development of nanomaterials to reach target functionalities such as conversion efficiencies or selectiv...
Preprint
Full-text available
The L subshell Coster Kronig (CK) transition factors of Gd have been experimentally determined by means of two different experimental approaches and compared to available literature data. On the one hand reference-free X-ray fluorescence (XRF) analysis using an energy-dispersive detector was applied. This method permitted in addition to determine t...
Preprint
We used reference-free grazing incidence X-ray fluorescence to measure the density of four thiol Raman-active molecules assembled on gold surfaces. This value is needed to reliably quantify the number of molecules contributing to the SERS signal in a plasmonic substrate in the effort to standardize the enhancement factor calculation and such molecu...
Preprint
A gas cell for in-situ measurements of Volatile Organic Compounds (VOCs) and their adsorption behavior on different surfaces by means of X-Ray Fluorescence (XRF) and X-ray Absorption Fine-Structure (XAFS) spectroscopy has been developed. The cell is especially designed to allow for the efficient excitation and detection of low-Z elements such as ca...
Preprint
Self-assembled monolayers of 7-mercapto 4-methylcoumarin (MMC) on a flat gold surface were studied by Molecular Dynamics (MD) simulations, reference-free grazing incidence X-ray fluorescence (GIXRF) and X-ray photoemission spectroscopy (XPS), to determine the maximum monolayer density and to investigate the nature of the molecule/surface interface....
Article
Full-text available
Synchrotron radiation-based Fourier transform infrared spectroscopy enables access to vibrational information from mid over far infrared to even terahertz domains. This information may prove critical for the elucidation of fundamental bio-molecular phenomena including folding-mediated innate host defence mechanisms. Antimicrobial peptides (AMPs) re...
Article
Knowledge on the temporal and size distribution of particulate matter (PM) in air as well as on its elemental composition is a key information for source appointment, for the investigation of their influence on environmental processes and for providing reliable data for climate models. While cascade impactors allow for time- and size-resolved colle...
Article
A novel double full-cylinder crystal x-ray spectrometer for x-ray emission spectroscopy (XES) has been realized based on a modified von Hamos geometry. The spectrometer is characterized by its compact dimensions, its versatility with respect to the number of crystals used in series in the detection path, and the option to perform calibrated XES mea...
Article
The spatial and compositional complexity of 3D structures employed in today's nanotechnologies has developed to a level at which the requirements for process development and control can no longer fully be met by existing metrology techniques. For instance, buried parts in stratified nanostructures, which are often crucial for device functionality,...
Preprint
Full-text available
The knowledge of atomic fundamental parameters, such as the fluorescence yields with low uncertainties, is of decisive importance in elemental quantification involving X-ray fluorescence analysis techniques. However, especially for the low-Z elements, the available literature data are either of poor quality, of unknown or very large uncertainty, or...
Article
Full-text available
Each battery suffers from degradation effects which lead to capacity fading and life cycle reduction. With electrochemical methods, the battery capacity decrease can easily be monitored, but they are inappropriate to comprehend the underlying chemical and physical properties responsible for the capacity fading. In the present paper, we demonstrate...
Article
In this work, we present the results of the first Round Robin test of different kinds of micro- and nanoscaled samples for Total Reflection X-Ray Fluorescence (TXRF) analysis. Therefore preselected, well-characterized samples including an internal standard were provided to the participants of the Round Robin test. Three different kinds of samples w...
Preprint
For the reliable fabrication of the current and next generation of nanostructures it is essential to be able to determine their material composition and dimensional parameters. Using the grazing incidence X-ray fluoresence technique, which is taking advantage of the X-ray standing wave field effect, nanostructures can be investigated with a high se...
Article
Full-text available
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing EU air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasm...
Preprint
Full-text available
Knowledge on the temporal and size distribution of particulate matter (PM) in air as well as on its elemental composition is a key information for source appointment, for the investigation of their influence on environmental processes and for providing valid data for climate models. A prerequisite is that size fractionated sampling times of few hou...
Article
Full-text available
The quantitative evolution of dissolved polysulfides at both electrode sides of lithium–sulfur batteries is determined with operando X-ray spectrometry.
Article
The enhancement factor (EF) is an essential parameter in the field of surface-enhanced Raman spectroscopy (SERS), indicating the magnification of the Raman signal of molecules interacting with the surface of plasmonic nanostructures. The calculation of EF requires a careful evaluation of both the signal intensities and the number of molecules in SE...
Article
Grazing-Incidence X-ray fluorescence (GIXRF) analysis, which is closely related to total-reflection XRF, is a very powerful technique for the in-depth analysis of many types of technologically relevant samples, e.g. nanoparticle depositions, shallow dopant profiles, thin layered samples or even well-ordered nanostructures. However, the GIXRF based...
Article
The increasing importance of well-controlled ordered nanostructures on surfaces represents a challenge for existing metrology techniques. To develop such nanostructures and monitor complex processing constraints fabrication, both a dimensional reconstruction of nanostructures and a characterization (ideally a quantitative characterization) of their...
Article
Full-text available
We present experimental and theoretical X-ray emission spectroscopy (XES) data of the Fe K\(\beta\) line for Iron(II)sulfide (FeS) and Iron(II)disulfide (FeS$_2$). In comparison to X-ray absorption spectroscopy (XAS), XES offers different discrimination capabilities for chemical speciation, depending on the valence states of the compounds probed an...
Article
Full-text available
In this work, we present a grazing incidence X-ray diffraction study of the surface of a 0.24Pb(In1/2Nb1/2)O3-Pb(Mg1/3Nb2/3)O3-PbTiO3 (PIN-PMN-PT) [011] poled rhombohedral single crystal. The near surface microstructure (the top several tens to hundreds of unit cells) was measured in situ under an applied electric field. The strains calculated from...
Article
Full-text available
The development of new materials and the assessment of nanomaterials require the correlation of the materials’ functionality or toxicity with their chemical and physical properties. To probe these properties, analytical methods that are both sensitive and selective at the nano-and microscales are required. The reliability of most analytical methods...
Article
Full-text available
The development of thin-film thermoelectric applications in sensing and energy harvesting can benefit largely from suitable deposition methods for earth-abundant materials. In this study, p-type copper oxide thin films have been prepared on soda lime silicate glass by direct current (DC) magnetron sputtering at room temperature from a pure copper m...
Article
X-ray fluorescence (XRF) analysis is a widely applied technique for the quantitative analysis of thin films up to the µm scale because of its non-destructive nature and because it is easily automated. When low uncertainties of the analytical results in the few percent range are required, the non-linear secondary fluorescence effect in multi-element...
Preprint
Full-text available
We present Fe K$\beta$ X-ray emission (XES) and Fe K X-ray absorption spectra (XAS) of Iron(II)sulfide (FeS) and Iron(II)disulfide (FeS$_2$). While XES and XAS offer different discrimination capabilities for chemical speciation, depending on the valence states of the compounds probed, XES allows for using different excitation sources. The XES data...
Preprint
Full-text available
The increasing importance of well-controlled ordered nanostructures on surfaces represents a challenge for existing metrology techniques. To develop such nanostructures and monitor complex processing constraints fabrication, both a dimensional reconstruction of nanostructures and a characterization (ideally a quantitative characterization) of their...
Article
Full-text available
In this work, Pt-Ti core-shell nanoparticles (NP) of 2 nm to 3 nm in size and 30000 u ± 1500 u as specified single particle mass, deposited on flat silicon substrates by means of a mass-selected cluster beam source, were used for the investigation of the modification of the X-Ray Standing Wave (XSW) field intensity with increasing NP surface covera...
Preprint
Full-text available
In this work, Pt-Ti core-shell nanoparticles (NP) of 2 nm to 3 nm in size and 30000 u \pm 1500 u as specified single particle mass, deposited on flat silicon substrates by means of a mass-selected cluster beam source, were used for the investigation of the modification of the X-Ray Standing Wave (XSW) field intensity with increasing NP surface cove...
Preprint
Full-text available
X-ray fluorescence (XRF) analysis is a widely applied technique for the quantitative analysis of thin films up to the $\mu$m scale because of its non-destructive nature and because it is easily automated. When low uncertainties of the analytical results in the few percent range are required, the non-linear secondary fluorescence effect in multi-ele...
Preprint
Full-text available
Grazing-Incidence X-ray fluorescence (GIXRF) analysis, which is closely related to total-reflection XRF, is a very powerful technique for the in-depth analysis of many types of technologically relevant samples, e.g. nanoparticle depositions, shallow dopant profiles, thin layered samples or even well-ordered nanostructures. However, the GIXRF based...
Article
Industry-scalable fabrication methods of sulfur-based transition metal dichalcogenides are being developed, which puts strong requirements on the characterization of these mono- and few-layer materials in a cleanroom environment. In this paper, we show that the stoichiometry of ultrathin molydbenum disulfide layers can be determined by inline X-ray...
Article
The International Standard Organization (ISO) 20289 provides a method for determining the elemental concentration of impurities dissolved in water samples. It exploits total reflection X‐ray fluorescence (TXRF) spectroscopy to measure a dried residue on an X‐ray reflector. The scope is to provide a chemical metrology for quantitative analysis to ob...
Article
FeNi Hydroxides (FeNi-HD) have been considered as promising substitutes to noble metal electrocatalysts for oxygen evolution reaction (OER). In this work, we design and realize FeNi-HD nanotube arrays (FeNi-HDNAs) on Ni foam via an in-situ reaction and Kirkendall effect. The obtained catalysts possess higher specific surface area, more catalytic ac...
Article
X-ray absorption and resonant inelastic x-ray scattering measurements are carried out on lithium nitrate LiNO3. The nitrogen σ orbitals exhibit a large lifetime effect. Experimentally, this is manifest as an apparent weakening of the x-ray emission signal from these states, but a closer examination shows that instead it is due to extreme broadening...
Article
Nanolayer stacks are technologically very relevant for current and future applications in many fields of research. A nondestructive characterization of such systems is often performed using x-ray reflectometry (XRR). For complex stacks of multiple layers, low electron density contrast materials, or very thin layers without any pronounced angular mi...
Article
Full-text available
LiMn2O4 is a promising candidate for a cathode material in lithium ion batteries (LIBs) due to its ability to intercalate lithium ions reversibly through its three-dimensional manganese oxide network. One of the promising techniques for depositing LiMn2O4 thin film cathodes is atomic layer deposition (ALD). Due to its unparalleled film thickness co...
Article
Liquid-metal jet X-ray sources promise to deliver high photon fluxes, which are unprecedented for laboratory based X-ray sources, because the regenerating liquid-metal anode is less sensitive to damage caused by an increased electron beam power density. For some quantitative X-ray analysis techniques, knowledge of the absolute photon flux is needed...
Preprint
X-ray absorption and resonant inelastic x-ray scattering measurements are carried out on lithium nitrate LiNO$_3$. The $\sigma$ orbitals around the nitrogen atoms exhibit a large lifetime effect. Experimentally, this is manifest as an apparent weakening of the x-ray emission signal from these states, but a closer examination shows that instead it i...
Preprint
Full-text available
In this work the complete L-emission spectrum of gadolinium with respect to line energies, natural line widths, and relative transition probabilities was investigated using monochromatized synchrotron radiation. The measurements were realized in the PTB laboratory at BESSY II by means of an in-house built von Hamos spectrometer based on up to two f...
Preprint
Liquid-metal jet X-ray sources promise to deliver high photon fluxes, which are unprecedented for laboratory based X-ray sources, because the regenerating liquid-metal anode is less sensitive to damage caused by an increased electron beam power density. For some quantitative X-ray analysis techniques, knowledge of the absolute photon flux is needed...
Preprint
Nanolayer stacks are technologically very relevant for current and future applications in many fields of research. A non-destructive characterization of such systems is often performed using X-ray reflectometry (XRR). For complex stacks of multiple layers, low electron density contrast materials or very thin layers without any pronounced angular mi...
Article
We present valence‐to‐core X‐ray emission spectroscopy of Ti, TiO, and TiO2 by means of a double crystal von Hamos spectrometer based on full‐cylinder highly annealed pyrolytic graphite mosaic crystals. We demonstrate that, using a double crystal configuration, an energy resolution of E/ΔE ≈ 2,700 can be achieved in a compact setup using cylindrica...
Article
Biomedical devices are complex products requiring numerous assembly steps along the industrial process chain, which can carry the potential of surface contamination. Cleanliness has to be analytically assessed with respect to ensuring safety and efficacy. Although several analytical techniques are routinely employed for such evaluation, a reliable...
Article
A Compact Vibration Reduced Set-up for Scanning nm-XRF and STXM. - Volume 24 Supplement - Janin Lubeck, Christian Seim, Aurélie Dehlinger, Andreas Haidl, Philipp Hönicke, Yves Kayser, Rainer Unterumsberger, Claudia Fleischmann, Burkhard Beckhoff
Article
In advance of the 2018 Denver X-ray Conference, we asked leading scientists who will be speaking at the conference about current trends and advances in Xray fluorescence and X-ray diffraction. Here, these investigators discuss their work to advance these techniques, in areas such as new measurement of X-ray fundamental parameters, the analysis of a...
Article
The knowledge of atomic fundamental parameters, such as the mass attenuation coefficients or fluorescence yields with low uncertainties, is of decisive importance in elemental quantification involving X‐ray fluorescence analysis techniques. For example, several databases giving the mass attenuation coefficients are accessible and frequently used wi...
Article
The fluorescence yield of the K- and L3-shell of gallium was determined using the radiometrically calibrated (reference-free) X-ray fluorescence instrumentation at the BESSY II synchrotron radiation facility. Simultaneous transmission and fluorescence signals from GaSe foils were obtained, resulting in K- and L3-shell fluorescence yield values (ωGa...
Article
Full-text available
Reasonably-priced devices for the detection of toxic species in the atmosphere are critical for reasons of health. Previous research work shows the promising detection capabilities of graphene. Thus, we demonstrate the gaseous response of our nanocrystalline graphene field-effect transistors that can be fabricated hundredfold on a two inch substrat...
Article
Solid state gas sensors for monitoring toxins in the environment, chemical exhaust or biological samples have received increasing attention over the recent years. A promising material for this application is graphene, having demonstrated single molecule detection capability and sensitivity towards a variety of gases [1]. In this contribution we pre...
Article
Full-text available
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. Coster-Kronig (CK) parameters were also measured for the L shell of Ni. Theoretical calculations of the same parameters were performed...
Article
The relative transition probabilities of the L3-fluorescence lines from different titanium oxides were determined using high-resolution X-ray emission spectrometry. A reliable deconvolution of the X-ray emission spectra, by means of both experimentally determined response functions and absorption correction, reduces the relative uncertainties of th...
Cover Page
Large‐scale sub‐20 nm regular pattern obtained by self‐assembly of di‐block copolymers. The combination of reference free grazing incidence X‐ray fluorescence (GIXRF) and GIXAS techniques enables a complete characterization of such a 3D system and provides a potential calibration sample for 3D analytical techniques. This is reported by Masoud Diala...
Article
The geometry of a Si$_3$N$_4$ lamellar grating was investigated experimentally with reference-free grazing-incidence X-ray fluorescence analysis. While simple layered systems are usually treated with the matrix formalism to determine the X-ray standing wave field, this approach fails for laterally structured surfaces. Maxwell solvers based on finit...
Article
The continuous and aggressive scaling in semiconductor technology results in the integration of increasingly complex 3D architectures and new materials. The realization of these downscaled 3D structures requires also further improvement in 3D characterization techniques. In this work, a potential route to improve the accuracy and reliability of the...
Article
In this article the question of the certification of calibration samples for the characterisation of advanced thin film materials is addressed within the framework of reliable process control or quality management purposes. Reference measurement techniques can be used in order to address the gap in appropriate certified reference materials (CRMs) f...
Article
With the advent of both modern X-ray fluorescence (XRF) methods and improved analytical reliability requirements the demand for suitable reference samples has increased. Especially in nanotechnology with the very low areal mass depositions, quantification becomes considerably more difficult. However, the availability of suited reference samples is...
Article
There is a strong need in the medical device industry to decrease failure rates of biomedical devices by reducing the incidence of defect structures and contaminants during the production process. The detection and identification of defect structures and contaminants is crucial for many industrial applications. The present study exploits reference-...
Article
A new sample cell concept for the analysis of liquids or solid-liquid interfaces using soft X-ray spectroscopy is presented, which enables the complete sealing of the cell as well as the transport into vacuum via, for example, a load-lock system. The cell uses pressure monitoring and active as well as passive pressure regulation systems, thereby fa...
Article
Bovine fibrinogen monolayers on thin gold films and glassy carbon substrate were investigated using grazing incidence X-ray fluorescence (GIXRF) and spectroscopic ellipsometry (SE). The aim was to determine the amount of protein and to develop models and references for the SE measurement. Both methods were capable of measuring protein amount in the...
Article
The x-ray atomic properties of nickel (Ni) were investigated in a unique approach combining different experimental techniques to obtain new, useful and reliable values of atomic fundamental parameters for x-ray spectrometric purposes and for comparison with theoretical predictions. We determined the mass attenuation coefficients in an energy range...
Article
Full-text available
The electronic structure of hexagonal boron nitride (h-BN) is explored using measurements of x-ray absorption and resonant inelastic x-ray scattering (RIXS) at the nitrogen K edge (1s) in tandem with calculations using many-body perturbation theory within the GW and Bethe-Salpeter equation (BSE) approximations. Our calculations include the effects...