X-ray computed tomography using partially coherent Fresnel diffraction with application to an optical fiber.

A reconstruction algorithm for partially coherent x-ray computed tomography (XCT) including Fresnel diffraction is developed and applied to an optical fiber. The algorithm is applicable to a high-resolution tube-based laboratory-scale x-ray tomography instrument. The computing time is only a few times longer than the projective counterpart. The algorithm is used to reconstruct, with projections and diffraction, a tilt series acquired at the micrometer scale of a graded-index optical fiber using maximum likelihood and a Bayesian method based on the work of Bouman and Sauer. The inclusion of Fresnel diffraction removes some reconstruction artifacts and use of a Bayesian prior probability distribution removes others, resulting in a substantially more accurate reconstruction.

Transmission electron imaging and diffraction of asbestos fibers in a scanning electron microscope.

Test protocols for airborne clearance of asbestos abatement sites define the collection, imaging and quantification of asbestos with transmission electron microscopy (TEM). Since those protocols were developed 35 years ago, scanning electron microscope (SEM) capabilities have significantly improved and expanded, with improvements in image spatial resolution, elemental analysis, and transmission electron diffraction capabilities. This contribution demonstrates transmission electron imaging and diffraction using NIST Asbestos Standard Reference Materials and a conventional SEM to provide comparable identification and quantification capabilities in the SEM as the current regulatory methods based on TEM techniques. In particular, we demonstrate that the 0.53 nm layer line spacing that is characteristic of asbestos can be quantified using different detection methods, and that other identifying diffraction signatures of chrysotile are readily obtained. The results demonstrate a viable alternative to the current TEM-based methods for asbestos identification and classification.

Orientation mapping of graphene using 4D STEM-in-SEM.

A scanning diffraction technique is implemented in the scanning electron microscope. The technique, referred to as 4D STEM-in-SEM (four-dimensional scanning transmission electron microscopy in the scanning electron microscope), collects a diffraction pattern from each point on a sample which is saved to disk for further analysis. The diffraction patterns are collected using an on-axis lens-coupled phosphor/CCD arrangement. Synchronization between the electron beam and the camera exposure is accomplished with off-the-shelf data acquisition hardware. Graphene is used as a model system to test the sensitivity of the instrumentation and develop some basic analysis techniques. The data show interpretable diffraction patterns from monolayer graphene with integration times as short as 0.5 ms with a beam current of 245 pA (7.65×105 incident electrons per pixel). Diffraction patterns are collected at a rate of ca. 100/s from the mm to nm length scales. Using a grain boundary as a 'knife-edge', the spatial resolution of the technique is demonstrated to be ≤5.6nm (edge-width 25 % to 75 %). Analysis of the orientation of the diffraction patterns yields an angular (orientation) precision of ≤0.19∘ (full width at half maximum) for unsupported monolayer graphene. In addition, it is demonstrated that the 4D datasets have the information content necessary to analyze complex and heterogeneous multilayer graphene films.

Transmission imaging with a programmable detector in a scanning electron microscope.

A new type of angularly selective electron detector for use in a scanning electron microscope is presented. The detector leverages a digital micromirror device (DMD) to take advantage of the benefits of two-dimensional (2D) imaging detectors and high-bandwidth integrating detectors in a single optical system. The imaging detector provides direct access to the diffraction pattern, while the integrating detector can be synchronized to the microscope scan generator providing access to a real space image generated by integrating (pixel-by-pixel) a portion of the diffraction pattern as quantitatively defined by the DMD. The DMD, in effect, takes the place of the objective aperture in a transmission electron microscope (TEM) or an annular detector in a scanning transmission electron microscope (STEM), but has the distinct advantage that it can be programmed to take any shape in real time. Proof-of-principle data collected with the detector show diffraction contrast in samples ranging from a polycrystalline gold film to monolayer graphene.