Neutron specular reflectometry (SR) and off-specular scattering (OSS) are nondestructive techniques which, through deuteration, give a high contrast even among chemically identical species and are therefore highly suitable for investigations of soft-matter thin films. Through a combination of these two techniques, the former yielding a density profile in the direction normal to the sample surface and the latter yielding a depth-resolved in-plane lateral structure, one can obtain quite detailed information on buried morphology on length scales ranging from the order of ångströms to ∼10 µm. This is illustrated via quantitative evaluation of data on SR and OSS collected in time-of-flight (ToF) measurements of a set of films composed of immiscible polymer layers, protonated poly(methyl methacrylate) and deuterated polystyrene, undergoing a decomposition process upon annealing. Joint SR and OSS data analysis was performed by the use of a quick and robust originally developed algorithm including a common absolute-scale normalization of both types of scattering, which are intricately linked, constraining the model to a high degree. This, particularly, makes it possible to distinguish readily between different dewetting scenarios driven either by the nucleation and growth of defects (holes, protrusions etc.) or by thermal fluctuations in the buried interface between layers. Finally, the 2D OSS maps of particular cases are presented in different spaces and qualitative differences are explained, allowing also the qualitative differentiation of the in-plane structure of long-range order, the correlated roughness and bulk defects by a simple inspection of the scattering maps prior to quantitative fits.

We have developed an electron beam excitation ultra-soft X-ray add-on device for a scanning electron microscope with a reflective zone plate mulichannel spectrometer in order to analyse ultra-light elements such as Li and B. This spectrometer has high (λ/Δλ~100) resolving power in the energy range of 45 eV - 1120 eV. Metallic Li samples were examined and fluorescence spectra successfully measured. Energy resolution of 0.49 eV was measured in the ultra-low energy range using the Al L(2,3) line at 71 eV. High sensitivity of Boron detection was demonstrated on a B(4)C sample with layer thicknesses of 1-50 nm, detecting an amount of metallic Boron as small as ~0.57 fg.

The feasibility of an off-axis X-ray reflection zone plate to perform wavelength-dispersive spectroscopy, on-axis point focusing and two-dimensional (2D) imaging is demonstrated by means of one and the same diffractive optical element (DOE) at a synchrotron radiation facility. The resolving power varies between 3 × 10 1 and 4 × 10 2 in the range from 7.6 keV to 9.0 keV, with its maximum at the design energy of 8.3 keV. This result is verified using an adjustable entrance slit, by which horizontal (H) and vertical (V) focusing to 0.85 µm (H) and 1.29 µm (V) is obtained near the sagittal focal plane of the astigmatic configuration. An angular and axial scan proves an accessible field of view of at least 0.6 × 0.8 arcmin 2 and a focal depth of ±0.86 mm. Supported by the grating efficiency around 17.5% and a very short pulse elongation, future precision X-ray fluorescence and absorption studies of transition metals at their K-edge on an ultrashort timescale could benefit from our findings. or two-dimensional (2D) focusing in the soft [6] and hard regime [7] of photon energies. Femtosecond pump-and-probe experiments can be performed with a very short pulse elongation [7], enabling almost Fourier-limited, spatially or time-resolved spectroscopy. However, the combined all-in-one abilities of RZPs were not yet demonstrated until now, in particular in the band between 6 keV and 10 keV, to examine K-edge radiation from transition metals such as Fe, Co, Ni or Cu. In this letter, we report on wavelength-dispersive spectroscopy and imaging with a resolution down to 20 eV, enabled by a micron-sized focal spot and obtained with the same RZP as it was designed for the preceding proof-of-concept study around E 0 = 8.3 keV [7].For our recent measurements at the 1-BM beamline [8] of the Advanced Photon Source (APS), the off-axis RZP is configured again to operate in its (−1) st diffraction order and the parameters are adopted from the previous setup [7] with one exception: An open entrance slit presumed in Fig. 1, the Xray dipole source illuminates the whole RZP now from a distance R 1,ext. = 34 m [9, 10]. This enlarged entrance arm length Fig. 1. Experimental setup, as modified from its initial design [7]. The distant source and the maintained incidence angle α 0 lead to an astigmatic focal plane separation by ≈ 3 mm. The exit angle varies around β 0 with the photon energy from E < E 0 (red) to E > E 0 (blue). The drawing is not to scale.corresponds to an extension ∆R 1 = 24 m with respect to the initial value R 1 = 10 m. On the other hand, the grazing incidence angle α 0 = 0.301 • and its counterpart β 0 = 0.149 • are maintained within the precision limits of the optics mounting. The focal intensity distribution is hence expected to split up in a sagittal (s) and meridional (m) plane, slightly displaced from the designed detector position R 2 = 0.1 m. We write the sagittal and meridional magnification for the design configuration [7] as M s,m -where the

Specular and off-specular neutron reflectometry have been used in a combined approach to study thin polymer films. Our goal in this work is to illustrate the power of the off-specular scattering technique to probe the properties of the buried interface of immiscible polymer bilayers of deuterated polystyrene (d-PS) and protonated poly(methyl methacrylate) (h-PMMA). The diffuse scattering stemming from these systems is discussed in relation to thermal fluctuations at the polymer/polymer interface, providing a means to extract in-plane correlation lengths from buried interfaces. In addition the onset of hole formation in the top layer is evidenced by the diffuse scattering, not easily detectable by specular reflection alone.