Volker Rose

A hard X-ray nanoprobe beamline for nanoscale microscopy

The Hard X-ray Nanoprobe Beamline is a precision platform for scanning probe and full-field microscopy with 3–30 keV X-rays. A combination of high-stability X-ray optics and precision motion sensing and control enables detailed studies of the internal features of samples with resolutions approaching 30 nm.

Two dimensional hard x-ray nanofocusing with crossed multilayer Laue lenses

Hard x-ray microscopy with nanometer resolution will open frontiers in the study of materials and devices, environmental sciences, and life sciences by utilizing the unique characterization capabilities of x-rays. Here we report two-dimensional nanofocusing by multilayer Laue lenses (MLLs), a type of diffractive optics that is in principle capable of focusing x-rays to 1 nm. We demonstrate focusing to a 25 × 27 nm(2) FWHM spot with an efficiency of 2% at a photon energy of 12 keV, and to a 25 × 40 nm(2) FWHM spot with an efficiency of 17% at a photon energy of 19.5 keV.

Combining scanning tunneling microscopy and synchrotron radiation for high-resolution imaging and spectroscopy with chemical, electronic, and magnetic contrast

The combination of high-brilliance synchrotron radiation with scanning tunneling microscopy opens the path to high-resolution imaging with chemical, electronic, and magnetic contrast. Here, the design and experimental results of an in-situ synchrotron enhanced x-ray scanning tunneling microscope (SXSTM) system are presented. The system is designed to allow monochromatic synchrotron radiation to enter the chamber, illuminating the sample with x-ray radiation, while an insulator-coated tip (metallic tip apex open for tunneling, electron collection) is scanned over the surface. A unique feature of the SXSTM is the STM mount assembly, designed with a two free-flex pivot, providing an angular degree of freedom for the alignment of the tip and sample with respect to the incoming x-ray beam. The system designed successfully demonstrates the ability to resolve atomic-scale corrugations. In addition, experiments with synchrotron x-ray radiation validate the SXSTM system as an accurate analysis technique for the study of local magnetic and chemical properties on sample surfaces. The SXSTM systems capabilities have the potential to broaden and deepen the general understanding of surface phenomena by adding elemental contrast to the high-resolution of STM.

Demagnetization protocols for frustrated interacting nanomagnet arrays

We report a study of demagnetization protocols for frustrated arrays of interacting single-domain permalloy nanomagnets by rotating the arrays in a changing magnetic field. The most effective demagnetization is achieved by not only stepping the field strength down while the sample is rotating, but also by combining each field step with alternation in the field direction. By contrast, linearly decreasing the field strength or stepping the field down without alternating the field direction leaves the arrays with a larger remanent magnetic moment. These results suggest that nonmonotonic variations in field magnitude around and below the coercive field are important for the demagnetization process.

X-ray-excited photoelectron detection using a scanning tunneling microscope

Detection of x-ray-enhanced electrons emitted by synchrotron radiation with the tip of a scanning tunneling microscope has the potential to open a path to high-resolution microscopy with chemical sensitivity. Nonresonant photoejected electrons typically yield a current background of a few hundred picoamperes at a bare tip. Coating the tip with an insulating boron nitride film can effectively reduce this background. In this configuration, we have quantitatively studied the bias dependent photoelectron collection for tip/sample separations of 400–1600nm, where quantum mechanical tunneling does not contribute.

X-ray nanotomography of SiO2-coated Pt90Ir10 tips with sub-micron conducting apex

Hard x-ray nanotomography provides an important three-dimensional view of insulator-coated “smart tips” that can be utilized for modern emerging scanning probe techniques. Tips, entirely coated by an insulating SiO2 film except at the very tip apex, are fabricated by means of electron beam physical vapor deposition, focused ion beam milling and ion beam-stimulated oxide growth. Although x-ray tomography studies confirm the structural integrity of the oxide film, transport measurements suggest the presence of defect-induced states in the SiO2 film. The development of insulator-coated tips can facilitate nanoscale analysis with electronic, chemical, and magnetic contrast by synchrotron-based scanning probe microscopy.

Elemental fingerprinting of materials with sensitivity at the atomic limit.

By using synchrotron X-rays as a probe and a nanofabricated smart tip of a tunneling microscope as a detector, we have achieved chemical fingerprinting of individual nickel clusters on a Cu(111) surface at 2 nm lateral resolution, and at the ultimate single-atomic height sensitivity. Moreover, by varying the photon energy, we have succeeded to locally measure photoionization cross sections of just a single Ni nanocluster, which opens new exciting opportunities for chemical imaging of nanoscale materials.

The band gap of ultrathin amorphous and well-ordered Al2O3 films on CoAl(100) measured by scanning tunneling spectroscopy

The structural and electronic properties of ultrathin insulator Al2O3 films on CoAl(100) have been studied using a combination of scanning tunneling spectroscopy and microscopy. The analysis of the differential conductance yields a band gap of 2.6–2.9eV for amorphous Al2O3. In the case of a well-ordered alumina film, the band gap is increased to 4.5eV. On each of the oxide phases, the barrier height is to a large extent independent of local variations such as the surface corrugations or oxide steps.

Imaging trace element distributions in single organelles and subcellular features

The distributions of chemical elements within cells are of prime importance in a wide range of basic and applied biochemical research. An example is the role of the subcellular Zn distribution in Zn homeostasis in insulin producing pancreatic beta cells and the development of type 2 diabetes mellitus. We combined transmission electron microscopy with micro- and nano-synchrotron X-ray fluorescence to image unequivocally for the first time, to the best of our knowledge, the natural elemental distributions, including those of trace elements, in single organelles and other subcellular features. Detected elements include Cl, K, Ca, Co, Ni, Cu, Zn and Cd (which some cells were supplemented with). Cell samples were prepared by a technique that minimally affects the natural elemental concentrations and distributions, and without using fluorescent indicators. It could likely be applied to all cell types and provide new biochemical insights at the single organelle level not available from organelle population level studies.

An easy-to-implement filter for separating photo-excited signals from topography in scanning tunneling microscopy

In order to achieve elemental and chemical sensitivity in scanning tunneling microscopy (STM), synchrotron x-rays have been applied to excite core-level electrons during tunneling. The x-ray photo-excitations result in tip currents that are superimposed onto conventional tunneling currents. While carrying important physical information, the varying x-ray induced currents can destabilize the feedback loop causing it to be unable to maintain a constant tunneling current, sometimes even causing the tip to retract fully or crash. In this paper, we report on an easy-to-implement filter circuit that can separate the x-ray induced currents from conventional tunneling currents, thereby allowing simultaneous measurements of topography and chemical contrasts. The filter and the schematic presented here can also be applied to other variants of light-assisted STM such as laser STM.