M.-I. Richard

Imaging of strain and lattice orientation by quick scanning X-ray microscopy combined with three-dimensional reciprocal space mapping

Numerous imaging methods have been developed over recent years in order to study materials at the nanoscale. Within this context, scanning X-ray diffraction microscopy has become a routine technique, giving access to structural properties with sub-micrometre resolution. This article presents an optimized technique and an associated software package which have been implemented at the ID01 beamline (ESRF, Grenoble). A structural scanning probe microscope with intriguing imaging qualities is obtained. The technique consists in a two-dimensional quick continuous mapping with sub-micrometre resolution of a sample at a given reciprocal space position. These real space maps are made by continuously moving the sample while recording scattering images with a fast two-dimensional detector for every point along a rocking curve. Five-dimensional data sets are then produced, consisting of millions of detector images. The images are processed by the user-friendly X-ray strain orientation calculation software (XSOCS), which has been developed at ID01 for automatic analysis. It separates tilt and strain and generates two-dimensional maps of these parameters. At spatial resolutions of typically 200–800 nm, this quick imaging technique achieves strain sensitivity below Δa/a = 10−5 and a resolution of tilt variations down to 10−3° over a field of view of 100 × 100 µm.

Strain and lattice orientation distribution in SiN/Ge complementary metal–oxide–semiconductor compatible light emitting microstructures by quick x-ray nano-diffraction microscopy

This paper presents a study of the spatial distribution of strain and lattice orientation in CMOS-fabricated strained Ge microstripes using high resolution x-ray micro-diffraction. The recently developed model-free characterization tool, based on a quick scanning x-ray diffraction microscopy technique can image strain down to levels of 10−5 (Δa/a) with a spatial resolution of ∼0.5 μm. Strain and lattice tilt are extracted using the strain and orientation calculation software package X-SOCS. The obtained results are compared with the biaxial strain distribution obtained by lattice parameter-sensitive μ-Raman and μ-photoluminescence measurements. The experimental data are interpreted with the help of finite element modeling of the strain relaxation dynamics in the investigated structures.

Inversion Domain Boundaries in GaN Wires Revealed by Coherent Bragg Imaging

Interfaces between polarity domains in nitride semiconductors, the so-called Inversion Domain Boundaries (IDB), have been widely described, both theoretically and experimentally, as perfect interfaces (without dislocations and vacancies). Although ideal planar IDBs are well documented, the understanding of their configurations and interactions inside crystals relies on perfect-interface assumptions. Here, we report on the microscopic configuration of IDBs inside n-doped gallium nitride wires revealed by coherent X-ray Bragg imaging. Complex IDB configurations are evidenced with 6 nm resolution and the absolute polarity of each domain is unambiguously identified. Picoscale displacements along and across the wire are directly extracted from several Bragg reflections using phase retrieval algorithms, revealing rigid relative displacements of the domains and the absence of microscopic strain away from the IDBs. More generally, this method offers an accurate inner view of the displacements and strain of interacting defects inside small crystals that may alter optoelectronic properties of semiconductor devices.

Scanning force microscope for in situ nanofocused X-ray diffraction studies

An atomic force microscope has been developed for combination with sub-micrometer focused X-ray diffraction at synchrotron beamlines and in situ mechanical tests on single nanostructures.

In situ investigation of the island nucleation of Ge on Si(001) using x-ray scattering methods

The growth of Ge on Si(001) is investigated in situ at 500 and 600°C, combining grazing incidence diffraction, multiple wavelength anomalous diffraction, and small angle scattering. This allows probing simultaneously the island shape, strain state, composition, and the transition from wetting layer to island growth. At 500°C no intermixing occurs. The wetting layer is found to decrease by one atomic layer at the onset of island nucleation. At 600°C interdiffusion plays an important role in strain relaxation leading to a more stable wetting layer. Small angle scattering yields the island morphology and shows the transition from pyramids to multifacetted domes.

Concentration and Strain Fields inside a Ag/Au Core-Shell Nanowire Studied by Coherent X-ray Diffraction

Three-dimensional coherent diffraction patterns of an isolated, single-crystalline Ag/Au core-shell nanowire were recorded at different X-ray beam energies close to the Au LIII absorption edge. Two-dimensional slices of the three-dimensional diffraction pattern, with the diffraction vector oriented perpendicular to the wire axis, were investigated in detail. In reciprocal space, facet streaks with thickness fringes were clearly observed in the two-dimensional diffraction patterns, from which the shape and size of the corresponding cross sections of the nanowire could be revealed. Comparison with simulated diffraction patterns exhibited the coherency strain field in the nanowire. During in situ annealing at temperatures which would lead to significant intermixing by volume diffusion in bulk material, according to literature data, a core-shell morphology was preserved; that is, intermixing in the nanowire was pronouncedly decelerated compared to bulk diffusion.

Fast computation of scattering maps of nanostructures using graphical processing units

Scattering maps from strained or disordered nanostructures around a Bragg reflection can be either computed quickly using approximations and a (fast) Fourier transform or obtained using individual atomic positions. In this article, it is shown that it is possible to compute up to 4 × 1010 reflections atoms s−1 using a single graphics card, and the manner in which this speed depends on the number of atoms and points in reciprocal space is evaluated. An open-source software library (PyNX) allowing easy scattering computations (including grazing-incidence conditions) in the Python language is described, with examples of scattering from non-ideal nanostructures.

Imaging Structure and Composition Homogeneity of 300 mm SiGe Virtual Substrates for Advanced CMOS Applications by Scanning X-ray Diffraction Microscopy

Advanced semiconductor heterostructures are at the very heart of many modern technologies, including aggressively scaled complementary metal oxide semiconductor transistors for high performance computing and laser diodes for low power solid state lighting applications. The control of structural and compositional homogeneity of these semiconductor heterostructures is the key to success to further develop these state-of-the-art technologies. In this article, we report on the lateral distribution of tilt, composition, and strain across step-graded SiGe strain relaxed buffer layers on 300 mm Si(001) wafers treated with and without chemical-mechanical polishing. By using the advanced synchrotron based scanning X-ray diffraction microscopy technique K-Map together with micro-Raman spectroscopy and Atomic Force Microscopy, we are able to establish a partial correlation between real space morphology and structural properties of the sample resolved at the micrometer scale. In particular, we demonstrate that the lattice plane bending of the commonly observed cross-hatch pattern is caused by dislocations. Our results show a strong local correlation between the strain field and composition distribution, indicating that the adatom surface diffusion during growth is driven by strain field fluctuations induced by the underlying dislocation network. Finally, it is revealed that a superficial chemical-mechanical polishing of cross-hatched surfaces does not lead to any significant change of tilt, composition, and strain variation compared to that of as-grown samples.

In situ three-dimensional reciprocal-space mapping during mechanical deformation

Mechanical deformation of a SiGe island epitaxically grown on Si(001) was studied by a specially adapted atomic force microscope and nanofocused X-ray diffraction. The deformation was monitored during in situ mechanical loading by recording three-dimensional reciprocal-space maps around a selected Bragg peak. Scanning the energy of the incident beam instead of rocking the sample allowed the safe and reliable measurement of the reciprocal-space maps without removal of the mechanical load. The crystal truncation rods originating from the island side facets rotate to steeper angles with increasing mechanical load. Simulations of the displacement field and the intensity distribution, based on the finite-element method, reveal that the change in orientation of the side facets of about 25° corresponds to an applied pressure of 2-3 GPa on the island top plane.

Multiple scattering effects in strain and composition analysis of nanoislands by grazing incidence x rays

Experiments and numerical simulations based on finite element modeling show that the x-ray intensity scattered by comparatively large nanostructures on a substrate is not simply related to their strain in experiments using either grazing incidence or exit because of multiple scatteringeffects. However, whatever the nanostructure size, the composition profiles are correctly extracted from grazing incidence multiwavelength anomalous scattering. These effects are illustrated for the structural analysis of Ge dome-shaped islands grown on Si(001).