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In the 50 years since the first mating of semiconductor-based energy-dispersive X-ray spectrometry (EDS) with the scanning electron microscope (SEM), this hybrid instrument has become an indispensable microanalytical tool. In the last two decades a new detector, the silicon drift detector (SDD), has overtaken earlier Si(Li) technology and has made EDS in the SEM and TEM faster and better. This article tells the story of the SDD development and describes improvements in count rate capability, energy resolution, and detector geometry that bring to SEM microanalysis exceptional precision and stability. Quality maps of element distributions can now be obtained in minutes instead of hours.

Modern quantitative TEM methods such as the ζ -factor technique require precise knowledge of the electron beam current. To this end, a macroscopic Faraday cup was designed and constructed. It can replace the viewing screen in the projection chamber of a TEM and guarantees highly accurate measurement of the electron beam with precision only limited by the used amperemeter. The easy to install, affordable device is shown to be highly apt for precision measurement of currents > 5 pA . The Faraday cup results are used for an assessment and a comparison of various other beam current measurement methods. It is found that the built-in screen amperemeter of the used TEM is quite inaccurate and that measurements using the screen in general tend to underestimate the current. If present, the drift tube of a spectrometer can also be used as a Faraday cup, but certain described peculiarities have to be taken into account. Direct ultrafast electron detection cameras allow precise measurement at very small currents. For the electron counting technique, which exploits single electron detection capabilities of STEM detectors, a systematic current underestimation was observed and investigated. This results in a reformulated routine for the method and with these improvements it is demonstrated to be capable of accurate high-precision measurements for currents 5 pA .

4D-scanning transmission electron microscopy (4D-STEM) can be used to measure electric fields such as atomic fields or polarization-induced electric fields in crystal heterostructures. The paper focuses on effects occurring in 4D-STEM at interfaces, where two model systems are used: an AlN/GaN nanowire superlattice as well as a GaN/vacuum interface. Two different methods are applied: First, we employ the centre-of mass (COM) technique which uses the average momentum transfer evaluated from the intensity distribution in the diffraction pattern. Second, we measure the shift of the undiffracted disc (disc-detection method) in nano-beam electron diffraction (NBED). Both methods are applied to experimental and simulated 4D-STEM data sets. We find for both techniques distinct variations in the momentum transfer at interfaces between materials: In both model systems, peaks occur at the interfaces and we investigate possible sources and routes of interpretation. In case of the AlN/GaN superlattice, the COM and disc-detection methods are used to measure internal polarization-induced electric fields and we observed a reduction of the measured fields with increasing specimen thickness.

Images acquired in transmission electron microscopes can be distorted for various reasons such as e.g. aberrations of the lenses of the imaging system or inaccuracies of the image recording system. This results in inaccuracies of measures obtained from the distorted images. Here we report on measurement and correction of elliptical distortions of diffraction patterns. The effect of this correction on the measurement of crystal lattice strain is investigated. We show that the effect of the distortions is smaller than the precision of the measurement in cases where the strain is obtained from shifts of diffracted discs with respect to their positions in images acquired in an unstrained reference area of the sample. This can be explained by the fact that diffraction patterns acquired in the strain free reference area of the sample are distorted in the same manner as the diffraction patterns acquired in the strained region of interest. In contrast, for samples without a strain free reference region such as nanoparticles or nanoporous structures, where we evaluate ratios of lattice plane distances along different directions, the distortions are usually not negligible. Furthermore, two techniques for the detection of diffraction disc positions are compared showing that for samples in which the crystal orientation changes over the investigated area it is more precise to detect the positions of many diffraction discs simultaneously instead of detecting each disc position independently.

The charge density is among the most fundamental solid state properties determining bonding, electrical characteristics, and adsorption or catalysis at surfaces. While atomic-scale charge densities have as yet been retrieved by solid state theory, we demonstrate both charge density and electric field mapping across a mono-/bilayer boundary in 2D MoS2 by momentum-resolved scanning transmission electron microscopy. Based on consistency of the four-dimensional experimental data, statistical parameter estimation and dynamical electron scattering simulations using strain-relaxed supercells, we are able to identify an AA-type bilayer stacking and charge depletion at the Mo-terminated layer edge. Published version

The Mercury Imaging X-ray Spectrometer (MIXS) will be launched on board of the 5th ESA cornerstone mission BepiColombo. The two channel instrument MIXS is dedicated to the exploration of the elemental composition of the mercurian surface by imaging x-ray spectroscopy of the elemental fluorescence lines. One of the main scientific goals of MIXS is to provide spatially resolved elemental abundance maps of key rock-forming elements. MIXS will be the successor of the XRS instrument, which is currently orbiting Mercury on board of NASAs satellite MESSENGER. MIXS will provide unprecedented spectral and spatial resolution due to its innovative detector and optics concepts. The MIXS target energy band ranges from 0.5 to 7 keV and allows to directly access the Fe-L line at 0.7 keV, which was not accessible to previous missions. In addition, the high spectroscopic resolution of FWHM ≤ 200 eV at the reference energy of 1 keV after one year in Mercury orbit, allows to separate the x-ray fluorescence emission lines of important elements like Mg (1.25 keV) and Al (1.49 keV) without the need for any filter. The detectors for the energy and spatially resolved detection of x-rays for both channels are identical DEPFET (DEpleted P-channel FET) active pixel detectors. We report on the calibration of the MIXS flight and flight spare detector modules at the PTB (Physikalisch-Technische Bundesanstalt) beamlines at the BESSY II synchrotron radiation facility. Each detector was calibrated at least at 10 discrete energies in the energy range from 0.5 to 10 keV. The excellent spectroscopic performance of all three detector modules was verified.

The ability to observe ultrafast structural changes in nanoscopic samples is essential for understanding non-equilibrium phenomena such as chemical reactions(1), matter under extreme conditions(2), ultrafast phase transitions(3) and intense light-matter interactions(4). Established imaging techniques are limited either in time or spatial resolution and typically require samples to be deposited on a substrate, which interferes with the dynamics. Here, we show that coherent X-ray diffraction images from isolated single samples can be used to visualize femtosecond electron density dynamics. We recorded X-ray snapshot images from a nanoplasma expansion, a prototypical non-equilibrium phenomenon(4,5). Single Xe clusters are superheated using an intense optical laser pulse and the structural evolution of the sample is imaged with a single X-ray pulse. We resolved ultrafast surface softening on the nanometre scale at the plasma/vacuum interface within 100 fs of the heating pulse. Our study is the first time-resolved visualization of irreversible femtosecond processes in free, individual nanometre-sized samples.

Scientific data 3, 160060 (2016). doi:10.1038/sdata.2016.60, Free-electron lasers (FEL) hold the potential to revolutionize structural biology by producing X-ray pules short enough to outrun radiation damage, thus allowing imaging of biological samples without the limitation from radiation damage. Thus, a major part of the scientific case for the first FELs was three-dimensional (3D) reconstruction of non-crystalline biological objects. In a recent publication we demonstrated the first 3D reconstruction of a biological object from an X-ray FEL using this technique. The sample was the giant Mimivirus, which is one of the largest known viruses with a diameter of 450 nm. Here we present the dataset used for this successful reconstruction. Data-analysis methods for single-particle imaging at FELs are undergoing heavy development but data collection relies on very limited time available through a highly competitive proposal process. This dataset provides experimental data to the entire community and could boost algorithm development and provide a benchmark dataset for new algorithms., Published by Nature Publ. Group, London

For many years pnCCDs have been well known as X-ray detectors for spectroscopic imaging in many fields of science: X-Ray Fluorescence analysis (XRF), X-ray Diffraction (XRD) with light sources in large accelerator facilities as well as with laboratory light sources or with X -rays from celestial sources in X-ray astronomy. A brief introduction in GEXRF (Grazing Emission XRF) measurements with a laboratory laser produced plasma source will be given, PIXE (Particle Induced X-ray Emission) measurements and D2XRF (Double Dispersive X -Ray Fluorescence) and Slicing experiments with pnCCDs coupled to polycapillary optics performed at the BESSY synchrotron will be shown. Energy - dispersive Laue diffraction with ultra - hard X-rays for the analysis of defects in metals will conclude the overview of spectroscopic X-ray imaging measurements in the field of structure and dynamics of matter. pnCCDs are radiation detectors on high resistivity 450 μm thick fully sensitive silicon [1]. They are back-illuminated devices with an ultra-thin, homogeneous radiation entrance window, enabling the proper detection of X-rays up to 30 keV with high quantum efficiency. As all pnCCDs are equipped with a fully column parallel readout, frame rates on more than 1200 frames per second are achieved, keeping the read noise level at 3 electrons (rms). Some of the key performance figures are (1) a quantum efficiency above 90% from 1 keV up to 10 keV, (2) single photon counting capability starting at only 30 eV, (3) extreme radiation hardness due to the avoidance of active MOS structures, and (4) energy resolution of 130eV (FWHM) at 6 keV and 37 eV (FWHM) at 90 eV. These properties have enabled a variety of spectacular measurements. (a) GEXRF: By combining a highly brilliant laser produced plasma (LPP) source with a scanning - free setup, grazing emission X-ray fluorescence (GEXRF) measurements in the soft X - ray range were realized [2]. The detector, a pnCCD, was operated in a single photon counting mode in order to utilize its energy dispersive properties. GEXRF profiles of the Ni - Lα line of a carbon - nickel multilayer sample, which displays a lateral (bi-)layer thickness gradient, were recorded at several positions. Simulations of theoretical profiles predicted a prominent intensity dip at emission angles between 5° and 12°, depending strongly on the bi-layer thickness of the sample (see Fig.1). This information was used to retrieve the bi - layer thickness gradient. The results are in good agreement with values obtained by X-ray reflectometry, conventional X-ray fluorescence and transmission electron microscopy measurements and serve as proof of principle for the suggested GEXRF setup. (b) PIXE: The unique properties pnCCDs, coupled to polycapillary X-ray optics, allows a fast position resolved overview over a large detection area with first results visible in real time. The maximum field of view exceeds 1 cm2 and the spatial resolution approaches a few microns when using sub-pixel algorithms by centroiding the signal charge cloud in the pixel structure [3] . The device has been used as an X-ray detector at the PIXE beamline at the Helmholtz-Zentrum Dresden Rossendorf (see Fig. 2). In addition to the above measurements (c) D2XRF and Slicing experiments performed at the BESSY synchrotron will be presented (see Fig. 3) as well as (d) Energy Dispersive Hard X-ray Laue Diffraction measurements at the ESRF.

X-ray free-electron lasers provide unique opportunities for exploring ultrafast dynamics and for imaging the structures of complex systems. Understanding the response of individual atoms to intense X-rays is essential for most free-electron laser applications. First experiments have shown that, for light atoms, the dominant interaction mechanism is ionization by sequential electron ejection, where the highest charge state produced is defined by the last ionic state that can be ionized with one photon. Here, we report an unprecedentedly high degree of ionization of xenon atoms by 1.5 keV free-electron laser pulses to charge states with ionization energies far exceeding the photon energy. Comparing ion charge-state distributions and fluorescence spectra with state-of-the-art calculations, we find that these surprisingly high charge states are created via excitation of transient resonances in highly charged ions, and predict resonance enhanced absorption to be a general phenomenon in the interaction of intense X-rays with systems containing high-Z constituents. Researchers create high ionization states, up to Xe36+, using 1.5 keV free-electron laser pulses. The higher than expected ionization may be due to transient resonance-enhanced absorption and the effect may play an important role in interactions of intense X-rays with high-Z elements and radiation damage.

The Mercury imaging X-ray spectrometer (MIXS) on board of ESA's fifth cornerstone mission BepiColombo will be the first space instrument using DEpleted P-channel FET (DEPFET) based detectors. The MIXS spectrometer comprises two channels with identical focal plane detectors and is dedicated to energy resolved imaging of X-ray fluorescence from the mercurial surface. We report on the characterization, integration, and spectroscopic qualification of MIXS flight detectors. Detector chips were precharacterized at die level in order to select the best dies for integration and to do homogeneity and yield studies. Then, the detector chips were integrated to MIXS Detector Plane Arrays (DPAs), a complicated process due to the sophisticated mechanical structure, which allows the thermal decoupling of the detector from its readout and control chips. After integration, spectroscopic qualification measurements were done in order to analyze the detector performance and to prove the excellent spectroscopic performance of the DEPFET Macropixel detectors over a wide temperature range. The integration and spectroscopic qualification of all flight grade modules is now successfully completed.

Protein crystallization in cells has been observed several times in nature. However, owing to their small size these crystals have not yet been used for X-ray crystallographic analysis. We prepared nano-sized in vivo-grown crystals of Trypanosoma brucei enzymes and applied the emerging method of free-electron laser-based serial femtosecond crystallography to record interpretable diffraction data. This combined approach will open new opportunities in structural systems biology.

We present a new high resolution X-ray imager based on a pnCCD detector and a polycapillary optics. The properties of the pnCCD like high quantum efficiency, high energy resolution and radiation hardness are maintained, while color corrected polycapillary lenses are used to direct the fluorescence photons from every spot on a sample to a corresponding pixel on the detector. The camera is sensitive to photons from 3 to 40 keV with still 30% quantum efficiency at 20 keV. The pnCCD is operated in split frame mode allowing a high frame rate of 400 Hz with an energy resolution of 152 eV for Mn K α (5.9 keV) at 450 kcps. In single-photon counting mode (SPC), the time, energy and position of every fluorescence photon is recorded for every frame. A dedicated software enables the visualization of the elements distribution in real time without the need of post-processing the data. A description of the key components including detector, X-ray optics and camera is given. First experiments show the capability of the camera to perform fast full-field X-Ray Fluorescence (FF-XRF) for element analysis. The imaging performance with a magnifying optics (3×) has also been successfully tested.

Focal plane instrumentation based on DEPFET Macropixel devices, being a combination of the Detector– Amplifier structure DEPFET with a silicon drift chamber (SDD), has been proposed for the MIXS (Mercury Imaging X-ray Spectrometer) instrument on ESA’s Mercury exploration mission BepiColombo. MIXS images X-ray fluorescent radiation from the Mercury surface with a lightweight X-ray mirror system on the focal plane detector to measure the spatially resolved element abundance in Mercury’s crust. The sensor needs to have an energy resolution better than 200 eV FWHM at 1 keV and is required to cover an energy range from 0.5 to 10 keV, for a pixel size of 300 � 300 mm 2. Main challenges for the instrument are radiation damage and the difficult thermal environment in the mercury orbit. The production of the first batch of flight devices has been finished at the MPI semiconductor laboratory. Prototype modules have been assembled to verify the electrical properties of the devices; selected results are presented here. The prototype devices, Macropixel prototypes for the SIMBOL-X focal plane, are electrically fully compatible, but have a pixel size of 0.5 � 0.5 mm 2 . Excellent homogeneity and near

The company PNSensor and the MPI Semiconductor Laboratory are developing and have produced first prototypes of pnCCDs with an avalanche readout which aim at single photon sensitivity in the visible wavelength range. This resolution is provided by an avalanche diode integrated in the readout chain of every CCD column. The diode features a new topology and can collect signal electrons from the CCDs’ depleted buried channel. The pixel-structure has been derived from pnCCDs and was optimized for lowest leakage current and for compatibility with the avalanche structures. All advantages of the pnCCDs are maintained, including high quantum efficiency (between 80% and 100%), high frame rate (up to 1000 frames/s) and low leakage current. Possible applications are in the field of High Time Resolution Astrophysics (HTRA). There, fast imaging of faint objects in the visible, such as, e.g. close binary stars or fast rotating neutron stars, requires single photon sensitivity and high frame rates. We present results from proof-of-principle tests carried out on first laboratory prototypes of such devices.

A so-called PNCCD, a special type of CCD, was developed twenty years ago as focal plane detector for the XMM-Newton X-ray astronomy mission of the European Space Agency ESA. Based on this detector concept and taking into account the experience of almost ten years of operation in space, a new X-ray CCD type was designed by the ‘MPI semiconductor laboratory’ for an upcoming X-ray space telescope, called eROSITA ( e xtended Ro entgen s urvey with an i maging t elescope a rray). This space telescope will be equipped with seven X-ray mirror systems of Wolter-I type and seven CCD cameras, placed in their foci. The instrumentation permits the exploration of the X-ray universe in the energy band from 0.3 up to 10 keV by spectroscopic measurements with a time resolution of 50 ms for a full image comprising 384×384 pixels. Main scientific goals are an all-sky survey and investigation of the mysterious ‘Dark Energy’. The eROSITA space telescope, which is developed under the responsibility of the ‘Max-Planck-Institute for extraterrestrial physics’, is a scientific payload on the new Russian satellite ‘Spectrum-Roentgen-Gamma’ (SRG). The mission is already approved by the responsible Russian and German space agencies. After launch in 2012 the destination of the satellite is Lagrange point L2. The planned observational program takes about seven years. We describe the design of the eROSITA camera system and present important test results achieved recently with the eROSITA prototype PNCCD detector. This includes a comparison of the eROSITA detector with the XMM-Newton detector.