Soft X-ray refractive index by reconciling total electron yield with specular reflection: experimental determination of the optical constants of graphite.

The complex refractive index of many materials is poorly known in the soft X-ray range across absorption edges. This is due to saturation effects that occur there in total-electron-yield and fluorescence-yield spectroscopy and that are strongest at resonance energies. Aiming to obtain reliable optical constants, a procedure that reconciles electron-yield measurements and reflection spectroscopy by correcting these saturation effects is presented. The procedure takes into account the energy- and polarization-dependence of the photon penetration depth as well as the creation efficiency for secondary electrons and their escape length. From corrected electron-yield spectra the absorption constants and the imaginary parts of the refractive index of the material are determined. The real parts of the index are subsequently obtained through a Kramers-Kronig transformation. These preliminary optical constants are refined by simulating reflection spectra and adapting them, so that measured reflection spectra are reproduced best. The efficacy of the new procedure is demonstrated for graphite. The optical constants that have been determined for linearly polarized synchrotron light incident with p- and s-geometry provide a detailed and reliable representation of the complex refractive index of the material near π- and σ-resonances. They are also suitable for allotropes of graphite such as graphene.

Efficient high-order suppression system for a metrology beamline.

High-quality metrology with synchrotron radiation requires in particular a very high spectral purity of the incident beam. This is usually achieved by a set of transmission filters with suitable absorption edges to suppress high-order radiation of the monochromator. The at-wavelength metrology station at a BESSY-II bending-magnet collimated plane-grating monochromator (c-PGM) beamline has recently commissioned a high-order suppression system (HiOS) based on four reflections from mirrors which can be inserted into the beam path. Two pairs of mirrors are aligned parallel so as not to disturb the original beam path and are rotated clockwise and counter-clockwise. Three sets of coatings are available for the different energy ranges and the incidence angle is freely tunable to find the optimum figure of merit for maximum suppression at maximum transmission for each photon energy required. Measured performance results of the HiOS for the EUV and XUV range are compared with simulations, and applications are discussed.

The at-wavelength metrology facility for UV- and XUV-reflection and diffraction optics at BESSY-II.

A technology center for the production of high-precision reflection gratings has been established. Within this project a new optics beamline and a versatile reflectometer for at-wavelength characterization of UV- and XUV-reflection gratings and other (nano-) optical elements has been set up at BESSY-II. The Plane Grating Monochromator beamline operated in collimated light (c-PGM) is equipped with an SX700 monochromator, of which the blazed gratings (600 and 1200 lines mm(-1)) have been recently exchanged for new ones of improved performance produced in-house. Over the operating range from 10 to 2000 eV this beamline has very high spectral purity achieved by (i) a four-mirror arrangement of different coatings which can be inserted into the beam at different angles and (ii) by absorber filters for high-order suppression. Stray light and scattered radiation is removed efficiently by double sets of in situ exchangeable apertures and slits. By use of in- and off-plane bending-magnet radiation the beamline can be adjusted to either linear or elliptical polarization. One of the main features of a novel 11-axes reflectometer is the possibility to incorporate real life-sized gratings. The samples are adjustable within six degrees of freedom by a newly developed UHV-tripod system carrying a load up to 4 kg, and the reflectivity can be measured between 0 and 90° incidence angle for both s- and p-polarization geometry. This novel powerful metrology facility has gone into operation recently and is now open for external users. First results on optical performance and measurements on multilayer gratings will be presented here.

Interface-induced room-temperature multiferroicity in BaTiO3.

Multiferroic materials possess two or more ferroic orders but have not been exploited in devices owing to the scarcity of room-temperature examples. Those that are ferromagnetic and ferroelectric have potential applications in multi-state data storage if the ferroic orders switch independently, or in electric-field controlled spintronics if the magnetoelectric coupling is strong. Future applications could also exploit toroidal moments and optical effects that arise from the simultaneous breaking of time-reversal and space-inversion symmetries. Here, we use soft X-ray resonant magnetic scattering and piezoresponse force microscopy to reveal that, at the interface with Fe or Co, ultrathin films of the archetypal ferroelectric BaTiO3 simultaneously possess a magnetization and a polarization that are both spontaneous and hysteretic at room temperature. Ab initio calculations of realistic interface structures provide insight into the origin of the induced moments and bring support to this new approach for creating room-temperature multiferroics.

Quadratic X-ray magneto-optical effect upon reflection in a near-normal-incidence configuration at the M edges of 3d-transition metals.

We have observed a quadratic x-ray magneto-optical effect in near-normal-incidence reflection at the M edges of iron. The effect appears as the magnetically induced rotation of approximately 0.1 degrees of the polarization plane of linearly polarized x-ray radiation upon reflection. A comparison of the measured rotation spectrum with results from x-ray magnetic linear dichroism data demonstrates that this is the first observation of the Schäfer-Hubert effect in the x-ray regime. Ab initio density-functional theory calculations reveal that hybridization effects of the 3p core states necessarily need to be considered when interpreting experimental data. The discovered magneto-x-ray effect holds promise for future ultrafast and element-selective studies of ferromagnetic as well as antiferromagnetic materials.

At-wavelength metrology facility for soft X-ray reflection optics.

A new Optics Beamline coupled to a versatile UHV reflectometer is successfully operating at BESSY-II. It is used to carry out at-wavelength characterization and calibration of in-house produced gratings and novel nano-optical devices as well as mirrors and multilayer systems in the UV and XUV spectral region. This paper presents most recent commissioning data of the beamline and shows their correlation with initial beamline design calculations. Special attention is paid to beamline key parameters which determine the quality of the measurements such as high-order suppression and stray light behavior. The facility is open to user operation.

Tissue pH in human kidney transplants during hypothermic ischemia.

Ex vivo NMR spectroscopy was used to investigate pH in 67 human kidney transplants. (1)H and (31)P spectra were recorded at 1.5 T during regular hypothermic storage in histidine-tryptophane-alpha-ketoglutarate (HTK) solution. Estimations of cytosolic pH from chemical shift differences between inorganic phosphate and phosphodiesters and of extracellular pH from the varepsilon1 and delta2 protons of histidine were based upon systematic titration studies. The possibility to predict acute tubular necrosis (ATN) by measuring pH was compared to results obtained with peak area ratios of phosphomonoesters (PME) and Pi and of the gamma-phosphorus of nucleoside 5'-triphosphate (gamma-NTP) and Pi. Cytosolic pH was 6.86+/-0.10 in kidneys showing immediate post-transplant function and 6.84+/-0.10 in those with ATN. Time-dependent studies demonstrated a monoexponential pH decay (velocity constant: 0.14+/-0.07 h(-1)). Extracellular pH varied between 7.40 and 7.15. Grafts with immediate function showed higher PME/Pi (2.24+/-0.57 vs. 1.77+/-0.50, p<0.05) and gamma-NTP/Pi (0.33+/-0.16 vs. 0.16+/-0.08, p<0.001). Intra- and extracellular pH can be monitored non-invasively during hypothermic transplant storage. The pH gradient between both compartments provides quantitative information about the buffer capacity of the preservation medium. Acidification is not a primary cause of ATN during regular HTK storage. The total nucleotide pool is a determinant of the reversibility of ischemic injury.

Kinetics of metabolism in human kidney transplants measured by dynamic 31P NMR spectroscopy.

The technique of ex vivo 31P NMR spectroscopy has been used for the investigation of metabolic turnover in 15 cadaveric human kidneys obtained from brain-dead donors for transplantation. Measurements were carried out at 1.5 T time-dependently during regular hypothermic storage in histidine-tryptophan-alpha-ketoglutarate solution. The minimum delay between explanation and spectroscopy was 2 h 41 min. In one case of a discarded organ the measurements could be extended over a period of 161 h 35 min. A detailed kinetic model describing monoexponential ischemic phosphate turnover, which accounts for various interrelations of the NMR visible metabolites, has been derived. Averaged velocity constants of the decays of nucleotides and phosphomono- and -diesters ranged from 0.0047 to 0.294h-1 at approximately 4 degrees C. Intracellular pH decreased monoexponentially with an averaged velocity constant of 0.31 h-1.

Phase-retardation and full-polarization analysis of soft-x-ray synchrotron radiation close to the carbon K edge by use of a multilayer transmission filter.

We have produced a multilayer transmission filter with 100 periods of Cr/C to achieve a significant phase retardation while maintaining good transmission for photon energies just below the carbon K edge. This device was installed into a polarimeter behind the SX700/3 monochromator at the Berlin synchrotron radiation laboratory, BESSY. The phase-retardation properties were observed as theoretically predicted. Agreement between experiment and calculation could be obtained by introduction of a rather small interface roughness in the simulation code (σ = 0.65 nm rms). An observed phase retardation of 5° was sufficient to permit, for the first time we believe, a complete and unambiguous polarization analysis of soft-x-ray synchrotron radiation (265-eV photon energy) with primary standards.

Insertion devices for BESSY II.

The high-brilliance synchrotron radiation source BESSY II will provide space for the installation of 14 insertion devices. At the time of writing (July 1997), eight insertion devices are funded. The first light for use by scientists will be available in January 1999. The undulators are designed for a scanning operation in parallel with the monochromator. This modus requires tight tolerances concerning the drive system. The first insertion device to be installed, a U-49 undulator, has been assembled and magnetically measured. The r.m.s. phase error is 2 degrees. An endpole configuration using coils with less than 64 amp-turns makes the angular kick smaller than +/-3 micro rad over a gap range 15-50 mm.

Observation of the x-ray magneto-optical Voigt effect.

The existence of the x-ray magneto-optical Voigt effect is demonstrated. By means of polarization analysis the Voigt rotation and ellipticity of linearly polarized synchrotron radiation are measured at the Co L3 edge upon transmission through an amorphous Co film. The observed x-ray Voigt rotation is about 7.5 degrees /microm. On the basis of ab initio calculations it is shown that the x-ray Voigt effect follows sensitively the amount of spin polarization of the 2p core states. Therefore it provides a unique measure of the spin splitting of the core states.

A plane-grating monochromator for circularly polarized undulator radiation at BESSY II.

At BESSY II, a third-generation 1.7 GeV storage ring is under construction. A planar elliptical undulator will be installed as a source of X-rays that have a high degree of circular polarization. Radiation in the first, third and fifth harmonics will cover the energy range 87-1330 eV. The beamline will essentially consist of a plane-grating monochromator working with collimated light in the dispersion plane. A single set of optical elements can be used to handle the two angularly separated beams of opposite helicity from the double undulator. The degree of circular polarization ranges from 73 to 100%, and a flux of up to 5 x 10(13) photons s(-1) (100 mA)(-1) can be achieved. A maximum spectral resolution of about 13 000 will be possible at 100 eV using a 20 micro m slit.

Soft-x-ray polarimeter with multilayer optics: complete analysis of the polarization state of light.

The design of a versatile high-precision eight-axis ultrahigh-vacuum-compatible polarimeter is presented. This multipurpose instrument can be used as a self-calibrating polarization detector for linearly and circularly polarized UV and soft-x-ray light. It can also be used for the characterization of reflection or transmission properties (reflectometer) or polarizing and phase-retarding properties (ellipsometer) of any optical element. The polarization properties of Mo/Si, Cr/C, Cr/Sc, and Ni/Ti multilayers used in this polarimeter as polarizers in transmission and as analyzers in reflection have been investigated theoretically and experimentally. In the soft-x-ray range, close to the p edges of Sc, Ti, and Cr, resonantly enhanced phase retardation of the transmission polarizers of as much as 18 degrees has been measured. With these newly developed optical elements the complete polarization analysis of soft-x-ray synchrotron radiation can be extended to the water-window range from 300 to 600 eV.