A lathe system for micrometre-sized cylindrical sample preparation at room and cryogenic temperatures

Holler, Mirko; Ihli, Johannes; Tsai, Esther H. R.; Nudelman, Fabio; Verezhak, Mariana; Berg, Wilma D. J. van de; Shahmoradian, Sarah H.

doi:10.1107/s1600577519017028

Cited by 12 publications

(12 citation statements)

References 23 publications

(6 reference statements)

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“…[ 30 ] The surface of every sample was trimmed by cylindrical turning such that a VOI in form of a pillar remained. [ 34 ] The pillars' diameter ranged from 60 to 80 μm (Table , Supporting Information).…”

Section: Methodsmentioning

confidence: 99%

X‐ray Stain Localization with Near‐Field Ptychographic Computed Tomography

et al. 2022

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Although X-ray contrast agents offer specific characteristics in terms of targeting and attenuation, their accumulation in the tissue on a cellular level is usually not known and difficult to access, as it requires high resolution and sensitivity. Here, quantitative near-field ptychographic X-ray computed tomography is demonstrated to assess the location of X-ray stains at a resolution sufficient to identify intracellular structures by means of a basis material decomposition. On the example of two different X-ray stains, the nonspecific iodine potassium iodide, and eosin Y, which mostly interacts with proteins and peptides in the cell cytoplasm, the distribution of the stains within the cells in murine kidney samples is assessed and compared to unstained samples with similar structural features. Quantitative nanoscopic stain concentrations are in good agreement with dual-energy micro computed tomography measurements, the state-of-the-art modality for material-selective imaging. The presented approach can be applied to a variety of X-ray stains advancing the development of X-ray contrast agents.

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Section: Methodsmentioning

confidence: 99%

X‐ray Stain Localization with Near‐Field Ptychographic Computed Tomography

et al. 2022

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“…A pristine and used VPO catalyst pellet was first mechanically fractured, after which a central piece from each pellet was mounted on a tomography pin. The mounted samples were then preshaped using a micro-lathe ( 48 ) to a diameter of 100 μm before being reduced to a final diameter between 10 and 12 μm using focused ion beam milling.…”

Section: Methodsmentioning

confidence: 99%

Sparse ab initio x-ray transmission spectrotomography for nanoscopic compositional analysis of functional materials

et al. 2021

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The performance of functional materials is either driven or limited by nanoscopic heterogeneities distributed throughout the material’s volume. To better our understanding of these materials, we need characterization tools that allow us to determine the nature and distribution of these heterogeneities in their native geometry in 3D. Here, we introduce a method based on x-ray near-edge spectroscopy, ptychographic x-ray computed nanotomography, and sparsity techniques. The method allows the acquisition of quantitative multimodal tomograms of representative sample volumes at sub–30 nm half-period spatial resolution within practical acquisition times, which enables local structure refinements in complex geometries. To demonstrate the method’s capabilities, we investigated the transformation of vanadium phosphorus oxide catalysts with industrial use. We observe changes from the micrometer to the atomic level and the formation of a location-specific defect so far only theorized. These results led to a reevaluation of these catalysts used in the production of plastics.

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“…The nanoporous gold sample was prepared via a de-alloying process using an aqueous nitric acid solution (Zinchenko et al, 2013). A tomography pillar, 6 mm in diameter, was produced using a micro-lathe (Holler, Ihli et al, 2020) and a focused ionbeam milling system. The sample pillar was annealed at 600 C prior to the acquisition of both tomograms.…”

Section: Nanotomography Demonstrationmentioning

confidence: 99%

“…(2) The direct fixation of suitably size samples on the pin using adhesives (Holler, Ihli et al, 2020). Equally of concern are environmental stability considerations and ideally an initially low adhesive viscosity, for example, as found in cement and carbon-based adhesives.…”

Section: Sample Mountingmentioning

confidence: 99%

“…The obtained piece of nanoporous gold was then mounted using epoxy resin on a gold-coated OMNY tomography pin (Holler et al, 2017) and pre-shaped, using a micro-lathe (Holler et al, 2020), into a cylindrical pillar with a diameter of ~30 µm and height of 20 µm. The pillar was next reduced in diameter to roughly 6 µm using focused ion-beam milling, before being transferred to an empty OMNY pin made out of bare aluminum.…”

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Environmental control for X-ray nanotomography

Holler¹,

Aidukas²,

Heller³

et al. 2022

J Synchrotron Radiat

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The acquisition speed and spatial resolution of X-ray nanotomography have continuously improved over the last decades. Coherent diffraction-based techniques breach the 10 nm resolution barrier frequently and thus pose stringent demands on sample positioning accuracy and stability. At the same time there is an increasing desire to accommodate in situ or operando measurements. Here, an environmental control system for X-ray nanotomography is introduced to regulate the temperature of a sample from room temperature up to 850°C in a controlled atmospheric composition. The system allows for a 360° sample rotation, permitting tomographic studies in situ or operando free of missing wedge constraints. The system is implemented and available at the flOMNI microscope at the Swiss Light Source. In addition to the environmental control system itself, the related modifications of flOMNI are described. Tomographic measurements of a nanoporous gold sample at 50°C and 600°C at a resolution of sub-20 nm demonstrate the performance of the device.

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A lathe system for micrometre-sized cylindrical sample preparation at room and cryogenic temperatures

Cited by 12 publications

References 23 publications

X‐ray Stain Localization with Near‐Field Ptychographic Computed Tomography

X‐ray Stain Localization with Near‐Field Ptychographic Computed Tomography

Sparse ab initio x-ray transmission spectrotomography for nanoscopic compositional analysis of functional materials

Environmental control for X-ray nanotomography

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