Electron Storage Ring BESSY Research Articles

Depth profile characterization of ultra shallow junction implants

A need for analysis techniques, complementary to secondary ion mass spectrometry (SIMS), for depth profiling dopants in silicon for ultra shallow junction (USJ) applications in CMOS technologies has recently emerged following the difficulties SIMS is facing there. Grazing incidence X-ray fluorescence (GIXRF) analysis in the soft X-ray range is a high-potential tool for this purpose. It provides excellent conditions for the excitation of the B-K and the As-L(iii,ii) shells. The X-ray standing wave (XSW) field associated with GIXRF on flat samples is used here as a tunable sensor to obtain information about the implantation profile because the in-depth changes of the XSW intensity are dependent on the angle of incidence. This technique is very sensitive to near-surface layers and is therefore well suited for the analysis of USJ distributions. Si wafers implanted with either arsenic or boron at different fluences and implantation energies were used to compare SIMS with synchrotron radiation-induced GIXRF analysis. GIXRF measurements were carried out at the laboratory of the Physikalisch-Technische Bundesanstalt (PTB) at the electron storage ring BESSY II using monochromatized undulator radiation of well-known radiant power and spectral purity. The use of an absolutely calibrated energy-dispersive detector for the acquisition of the B-Kalpha and As-Lalpha fluorescence radiation enabled the absolute determination of the total retained dose. The concentration profile was obtained by ab initio calculation and comparison with the angular measurements of the X-ray fluorescence.

Characterisation of High-k Containing Nanolayers by Reference-Free X-Ray Fluorescence Analysis with Synchrotron Radiation

Using reference-free X-ray fluorescence analysis (XRF) in different geometries carried out in the laboratory of the Physikalisch-Technische Bundesanstalt at the electron storage ring BESSY II in Berlin various nanolayered systems have been investigated. As an example the investigation of Hf containing thin oxide layers is shown. For comparison reasons these samples have been also measured by X-ray reflectometry (XRR) in the PTB laboratory and by other partners within the ANNA project, which confirmed the thickness of the Hf containing top layers determined by XRF within their respective uncertainties. The XRF spectra were deconvolved employing the detector response functions to deduce the intensity of the corresponding Hf L3 fluorescence lines. The investigation of nanolayered systems especially in the lower energy range shows advantages, like different absorption conditions which allow for better dynamics and the suppression of the silicon fluorescence signal from the substrate, but needs more effort in determining the respective fundamental parameters.

Comparison of scattering experiments using synchrotron radiation with Monte Carlo simulations using Geant4

Monte Carlo techniques are powerful tools to simulate the interaction of electromagnetic radiation with matter. One of the most widespread simulation program packages is Geant4. Almost all physical interaction processes can be included. However, it is not evident what accuracy can be obtained by a simulation. In this work, results of scattering experiments using monochromatized synchrotron radiation in the X-ray regime are quantitatively compared to the results of simulations using Geant4. Experiments were performed for various scattering foils made of different materials such as copper and gold. For energy-dispersive measurements of the scattered radiation, a cadmium telluride detector was used. The detector was fully characterized and calibrated with calculable undispersed as well as monochromatized synchrotron radiation. The obtained quantum efficiency and the response functions are in very good agreement with the corresponding Geant4 simulations. At the electron storage ring BESSY II the number of incident photons in the scattering experiments was measured with a photodiode that had been calibrated against a cryogenic radiometer, so that a direct comparison of scattering experiments with Monte Carlo simulations using Geant4 was possible. It was shown that Geant4 describes the photoeffect, including fluorescence as well as the Compton and Rayleigh scattering, with high accuracy, resulting in a deviation of typically less than 20%. Even polarization effects are widely covered by Geant4, and for Doppler broadening of Compton-scattered radiation the extension G4LECS can be included, but the fact that both features cannot be combined is a limitation. For most polarization-dependent simulations, good agreement with the experimental results was found, except for some orientations where Rayleigh scattering was overestimated in the simulation.

A quarter‐century of metrology using synchrotron radiation by PTB in Berlin

AbstractFor more than 25 years, the Physikalisch‐Technische Bundesanstalt has been strongly engaged in the field of metrology using synchrotron radiation. In Berlin, this research programme started together with the user operation of the electron storage ring BESSY I in the early 1980s. At the beginning, the work was focused on fundamental radiometry, i.e. using the storage ring as a primary radiation source standard and operating beamlines for source and detector calibration in the vacuum ultraviolet spectral range. Meanwhile, at the electron storage rings BESSY II and Metrology Light Source in Berlin‐Adlershof, the activities have been extended to a broad range of fundamental and applied photon metrology in the range from the far infrared to hard X‐rays, including methods like cryogenic radiometry, reflectometry and X‐ray fluorescence spectroscopy. In the present review, we give a short historical introduction to this work, describe our laboratories and the basic radiometric principles, and present examples of recent applications, largely performed within the framework of scientific cooperations with external partners from industry and research. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

NickelLIIIfluorescence and satellite transition probabilities determined with an alternative methodology for soft-x-ray emission spectrometry

An accurate determination of the nickel ${L}_{\text{III}}$ x-ray transition probabilities was performed employing a wavelength-dispersive spectrometer (WDS) at the plane grating monochromator beamline for undulator radiation of the Physikalisch-Technische Bundesanstalt, Germany's national metrology institute, at the electron storage ring BESSY II. An absolute calibration method developed for this spectrometer improves the reliability of the determination significantly because the calibration method does not require measurements of reference samples and provides a traceable uncertainty budget. The device was calibrated with respect to both its absolute detection efficiency and its response behavior. Therefore, a method to obtain the detection efficiency of a WDS in comparison to an absolutely calibrated energy-dispersive detector was successfully applied. In addition, response functions were developed and experimentally validated. The present results for the $\text{Ni}\text{ }{L}_{\text{III}}$ transition probabilities differ clearly from theoretical calculations and tabulated data found in the literature. Perspectives of a quantitative study of the interactions causing the satellite transitions are outlined and discussed in view of shake-off and Coster-Kronig processes.

Cryogenic radiometry in the hard x-ray range

For many applications in radiometry, spectroscopy or astrophysics, absolute measurement of radiant power with low uncertainty is essential. Cryogenic electrical substitution radiometers (ESRs) are regarded as the highest-accuracy primary standard detector in radiometry, from the infrared to the ultraviolet region; in combination with tuneable monochromatized synchrotron radiation from electron storage rings, their range of operation has been extended to the soft x-ray region. ESRs are absolute thermal detectors, based on the equivalence of electrical power and radiant power that can be traced back to electrical SI units and be measured with low uncertainties. Their core piece is a cavity absorber, which is typically made of copper to achieve a short response time suitable for use with synchrotron radiation. At higher photon energies, the use of copper prevents the operation of ESRs due to increasing transmittance. A new absorber design for hard x-rays has been developed at the laboratory of the Physikalisch-Technische Bundesanstalt (PTB) at the electron storage ring BESSY II. The Monte Carlo simulation code Geant4 was applied to optimize its absorptance for photon energies of up to 60 keV, resulting in a cavity absorber with a gold base and a cylindrical shell made of copper, in combination with a thermal sensitivity of around 150 mK µW−1 and a time constant of less than 3 min, which is short compared with the lifetime of many hours for the storage ring current. The measurement of the radiant power of monochromatized synchrotron radiation was achieved with relative standard uncertainties of less than 0.2%, covering the entire photon energy range of three beamlines from 50 eV to 60 keV. Monochromatized synchrotron radiation of high spectral purity was used to calibrate silicon photodiodes against the ESR for photon energies up to 60 keV with relative standard uncertainties below 0.3%.

Speciation of deeply buriedTiOxnanolayers with grazing-incidence x-ray fluorescence combined with a near-edge x-ray absorption fine-structure investigation

Nondestructive methods based on electron emission may encounter serious difficulties when probing the chemical state of deeply buried nanolayers due to restricted information depth. The purpose of the present work is to evaluate to which extent photon emission can overcome these restrictions. Grazing-incidence x-ray fluorescence combined with a near-edge x-ray absorption fine-structure investigation (GIXRF-NEXAFS) offers access to depth-resolving analysis of buried nanolayers with respect to both the chemical speciation and the layer composition. By varying the angle of incidence, the penetration depth can be tuned from a few to several hundreds of nanometers. The information depth of the emitted fluorescence radiation is in the same general range as the soft x-ray regime. Initial measurements were performed on nominally 30 nm thick titanium nanolayers oxidized to different extents and buried below 5 nm carbon layers. These layered structures were produced by means of ion beam sputtering deposition. The plane grating monochromator beamline for undulator radiation in the laboratory of the Physikalisch-Technische Bundesanstalt at the electron storage ring BESSY II provides tunable radiation of both well-known flux and high spectral purity for GIXRF-NEXAFS studies. The current results confirm that GIXRF-NEXAFS has the potential to substantially contribute to the speciation of deeply buried nanolayers. The analysis of measurements at a constant incident angle demonstrated that it is not possible to find an angle of incidence for the NEXAFS region to ensure a stable penetration depth. However, appropriate angular corrections can ensure a constant mean penetration depth, in particular, in the vicinity of absorption edges.

Gas detectors for x-ray lasers

We have developed different types of photodetectors that are based on the photoionization of a gas at a low target density. The almost transparent devices were optimized and tested for online photon diagnostics at current and future x-ray free-electron laser facilities on a shot-to-shot basis with a temporal resolution of better than 100 ns. Characterization and calibration measurements were performed in the laboratory of the Physikalisch-Technische Bundesanstalt at the electron storage ring BESSY II in Berlin. As a result, measurement uncertainties of better than 10% for the photon-pulse energy and below 20 μm for the photon-beam position were achieved at the Free-electron LASer in Hamburg (FLASH). An upgrade for the detection of hard x-rays was tested at the Sub-Picosecond Photon Source in Stanford.

Characterisation of a TES-Based X-ray Microcalorimeter in the Energy Range from 150 to 1800 eV Using an Adiabatic Demagnetisation Refrigerator

We characterised a TES-based X-ray microcalorimeter in an adiabatic demagnetisation refrigerator (ADR) using synchrotron radiation. The detector response and energy resolution was measured at the beam-line in the PTB radiometry laboratory at the electron storage ring BESSY II in the range from 200 to 1800 eV. We present and discuss the results of the energy resolution measurements as a function of energy, beam intensity and detector working point. The measured energy resolution ranges between 1.5 to 2.1 eV in the investigated energy range and is weakly dependent on the detector set point. A first analysis shows a count-rate capability, without considerable loss of performance, of about 500 counts per second.

Polarization-dependent vacuum-ultraviolet reflectometry using elliptically polarized synchrotron radiation

In the laboratory of the Physikalisch-Technische Bundesanstalt (PTB) at the Berlin electron-storage ring BESSY II, a procedure has been developed to investigate the dependence of vacuum-ultraviolet reflection on polarization. It is based on characterizing the elliptically polarized synchrotron radiation at PTB's normal-incidence monochromator beamline for reflectometry by means of polarization-sensitive photodetectors. For this purpose, the polarization dependency in the detector responsivity was determined at a small, low, solid angle of acceptance for the synchrotron radiation, i.e., within the orbital plane of the storage ring where the degree of linear polarization is known to be almost 100%. Our method allows the polarization dependence of reflection samples to be measured with relative standard uncertainties ranging from 2.4% to 11% in the spectral range between 60 and 160 nm. The method has been applied to the optimization of polarizing mirrors at the Lyman-alpha wavelength of 121.6 nm.

Reference-Free Total Reflection X-ray Fluorescence Analysis of Semiconductor Surfaces with Synchrotron Radiation

Total reflection X-ray fluorescence (TXRF) analysis is a well-established method to monitor lowest level contamination on semiconductor surfaces. Even light elements on a wafer surface can be excited effectively when using high-flux synchrotron radiation in the soft X-ray range. To meet current industrial requirements in nondestructive semiconductor analysis, the Physikalisch-Technische Bundesanstalt (PTB) operates dedicated instrumentation for analyzing light element contamination on wafer pieces as well as on 200- and 300-mm silicon wafer surfaces. This instrumentation is also suited for grazing incidence X-ray fluorescence analysis and conventional energy-dispersive X-ray fluorescence analysis of buried and surface nanolayered structures, respectively. The most prominent features are a high-vacuum load-lock combined with an equipment front end module and a UHV irradiation chamber with an electrostatic chuck mounted on an eight-axis manipulator. Here, the entire surface of a 200- or a 300-mm wafer can be scanned by monochromatized radiation provided by the plane grating monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. This beamline provides high spectral purity and high photon flux in the range of 0.078-1.86 keV. In addition, absolutely calibrated photodiodes and Si(Li) detectors are used to monitor the exciting radiant power respectively the fluorescence radiation. Furthermore, the footprint of the excitation radiation at the wafer surface is well-known due to beam profile recordings by a CCD during special operation conditions at BESSY II that allow for drastically reduced electron beam currents. Thus, all the requirements of completely reference-free quantitation of TXRF analysis are fulfilled and are to be presented in the present work. The perspectives to arrange for reference-free quantitation using X-ray tube-based, table-top TXRF analysis are also addressed.

Femtosecond Undulator Radiation from Sliced Electron Bunches

At the 1.7-GeV electron storage ring BESSY II, a first source of synchrotron radiation with 100 fs pulse duration, variable (linear and circular) polarization, tunable photon energy (300 to 1400 eV), and excellent signal-to-background ratio was constructed and is now in routine operation.

Calibration and characterization of semiconductor X-ray detectors with synchrotron radiation

Quantitative measurements of X-rays require absolutely calibrated detectors. In the laboratory of the Physikalisch-Technische Bundesanstalt (PTB) at the electron storage ring BESSY II in Berlin, X-ray detectors can be calibrated with low uncertainties. Two complementary approaches are realized for energy-dispersive detectors. One approach uses the storage ring as primary source standard and the detector response to the calculable spectral photon flux is measured in the undispersed synchrotron radiation. This requires the operation of the storage ring with only a few stored electrons. The other approach is the comparison to a primary detector standard, mainly a cryogenic electrical substitution radiometer. Here, monochromatized radiation of very high spectral purity has to be used which is available at different beamlines in the laboratory in the photon energy range from the UV up to about 120 keV. This method can also be applied for the calibration of non-energy-dispersive detectors. With monochromatized radiation, the response function of energy-dispersive detectors is recorded and compared to Monte Carlo simulations. A photon-energy-dependent parameterization of the response function allows deconvoluting the experimental spectra. The responsivity of Si photodiodes and the detection efficiency of Si(Li), HPGe and CdTe detectors are determined with low uncertainties in a broad spectral range.

Nitrogen and sulfur compounds in coastal Antarctic fine aerosol particles—an insight using non-destructive X-ray microanalytical methods

The capabilities of X-ray microanalytical methods, such as a near edge X-ray absorption fine structure (NEXAFS) investigation in conjunction with total reflection X-ray fluorescence (TXRF) analysis, as well as low- Z particle electron probe X-ray microanalysis (EPMA) to characterize fine Antarctic aerosol samples are demonstrated. Both techniques provided information on low- Z elements such as C, N and O. Size-segregated fine aerosol samples were collected at the Italian base at Terra Nova Bay (Antarctica) in February 2004. For comparative purposes, aerosol samples were also collected near the sea-shore in Alghero (Sardinia, Italy), in June 2004. The TXRF-NEXAFS measurements were carried out at the PGM monochromator beamline for undulator radiation in the PTB laboratory at the electron storage ring BESSY II. It was possible to quantify the molar ratio of ammonium and nitrate based on linear combinations of standard reference spectra of (NH 4) 2SO 4 and NaNO 3. Using TXRF-NEXAFS, the ammonium-to-nitrate ratio was determined in Antarctic fine aerosols collected from less than 2 m 3 of air, i.e. considerably lower than the sampling volumes usually used for ion chromatography analyses (30 m 3). This reduced sampling volume can enable the characterization of Antarctic aerosols to be done in higher temporal resolution. For Antarctic fine aerosols in the size range of 0.25–0.5 μm, nitrogen was observed to be present as almost entirely ammonium species. When the size of aerosol particles increases in the range of 0.25–2 μm, the content of ammonium decreases and yet the content of nitrate increases. An aerosol sample collected at Terra Nova Bay was investigated by the use of low- Z particle EPMA at a liquid nitrogen temperature in order to minimize beam damage of nitrogen-rich particles. Single-particle analytical results of 160 individual particles supported the TXRF-NEXAFS's observation that both ammonium-rich and nitrate-rich particles exist in the size range of 1–2 μm. Some particles were observed to contain both ammonium and nitrate species and yet pure ammonium nitrate particles were not encountered. The stoichiometry of the main chemical component of particles containing nitrogen and sulfur as major elements was found to be NH 4HSO 4.

Absolute measurement of F_2-laser power at 157 nm

We report a comparison of laser power measurements at the F2-laser wavelength of 157 nm made at two facilities of the Physikalisch-Technische Bundesanstalt (PTB), the German national metrology institute. At the PTB laboratory at the electron storage ring BESSY II in Berlin, the scale for laser power was directly traced to a cryogenic radiometer operating at 157 nm, whereas at the PTB laser radiometry facility in Braunschweig the calibration of transfer detectors was performed with a newly developed standard for laser power at 157 nm, which is traceable in several steps to a cryogenic radiometer operating at 633 nm. The comparison was performed under vacuum conditions with laser pulse energies of approximately 10 microJ, however with different average powers because different primary standard radiometers were used. The relative deviation for the responsivity of the transfer detector was 4.8% and thus within the combined standard uncertainty.

Detector Calibration and Measurement of Fundamental Parameters for X-Ray Spectrometry

Energy-dispersive X-ray spectrometry offers the opportunity for a fast and reliable determination of the composition of a specimen. For fundamental parameter based quantification, detailed knowledge of the X-ray generation cross sections and of the detection system’s efficiency is required. The detection efficiency is determined comparing the measured and calculated spectrum of undispersed synchrotron radiation (SR) from the electron storage ring BESSY II in the spectral range from 0.1 keV to 100 keV. Alternatively, monochromatized SR in the spectral range from 0.1 keV to 60 keV is used to determine the detection efficiency with a typical relative uncertainty of 1% to 2% by direct comparison with a reference detector. Employing well-calibrated detectors and monochromatized SR of well-known radiant power and high spectral purity, fluorescence yields have been investigated and resonant Raman scattering was studied as an example of a basic effect creating spectral background.

The PTB high-accuracy spectral responsivity scale in the VUV and x-ray range

At the electron storage ring BESSY II, the Physikalisch-Technische Bundesanstalt operates ten experimental stations at six synchrotron radiation beamlines for photon metrology in the spectral range from ultraviolet radiation to x-rays. Five of these beamlines are used to realize and disseminate a scale of spectral responsivity for photodetectors. Detector calibration is based on the use of cryogenic radiometers as primary detector standards. The current status of instrumentation and measurement capabilities is described. Best measurement capabilities (k = 2) for the calibration of photodiodes vary between 0.4% and 2.3%.

The EUV metrology program of PTB

The development of EUV lithography (EUVL) is critically based on the availability of a suitable metrology. The industrial demand for high accuracy characterization of EUV components is met at the laboratory of the Physikalisch-Technische Bundesanstalt (PTB) operated at the electron storage ring BESSY II. Using stable and well-characterized synchrotron radiation, PTB performs – in cooperation with industry – the characterization of optical components (reflectometry), the calibration and characterization of EUV radiation detectors and sources and lifetime characterization of optics and sensors. Recent examples from either of these working areas are presented.

X-ray resonant Raman scattering on Ni employing polarized and unpolarized exciting radiation

The X-ray resonant Raman scattering effect on nickel was studied by means of monochromatic polarized and unpolarized exciting radiation, respectively. Experiments involving polarized exciting radiation were carried out at the four crystal monochromator beamline of the Physikalisch-Technische Bundesanstalt for synchrotron radiation from 4 to 10 keV at the electron storage ring BESSY II. Resonant Raman spectra of thin Ni foils were recorded at the Cu-K α (8041 eV) exciting beam energy. In the Institute of Nuclear Physics of the N.C.S.R. Demokritos, the resonant Raman spectrum of a thick nickel target was also recorded for an unpolarized Cu-K α (8041 eV) exciting beam produced after the ionization of a thick Cu target by 1.7 MeV protons in a triaxial, orthogonal geometry. In the present work, the individual spectral characteristics and the methodological approaches adopted for the extraction of the Ni-RRS cross sections, with respect to each mode of excitation, are presented, compared and discussed. An excellent agreement was found between the Ni KL-RRS cross sections determined for polarized and unpolarized exciting radiation confirming the theoretical predictions within the experimental uncertainties achieved.

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

Monochromatized synchrotron radiation of the electron storage ring BESSY II has been used for the non-destructive thickness determination of nanolayered materials by two different methods. The aim of these investigations was the comparison of completely reference-free fundamental parameter-based X-ray fluorescence analysis with X-ray reflectometry to validate the quantification of X-ray fluorescence analysis as an absolute method. For this purpose, Cu and Ni layers with a thickness varying between 5 nm and 50 nm as well as double layers of both metals deposited on Si have been studied. In X-ray reflectometry characterization experiments, the tunability of the photon energy allows the determination of not only the total layer thickness but also the individual layer thicknesses of the Cu/Ni double-layer systems. Reference-free X-ray fluorescence analysis involves both the fundamental parameter approach and the knowledge of all relevant experimental parameters obtained by instrumentation calibrated absolutely. The layer thickness determined by both methods agreed within their combined uncertainties. In view of the limits of X-ray reflectometry for very thin layers, laterally inhomogeneous samples, and multi-elemental layer compositions, reference-free X-ray fluorescence analysis offers the potential for the thickness determination of such samples.