Welcome to I14

I14: Hard X-ray Nanoprobe

The Hard X-ray nanoprobe beamline is a dedicated facility for nanoscale microscopy and welcomed first users in March 2017. The nanoprobe provides a flexible endstation, with a beam size of 50 nm, optimised for scanning X-ray fluorescence, X-ray spectroscopy and diffraction. To maximise the distance from the focusing optic to the sample, the beamline extends beyond the main building to a distance of approximately 185m, and is housed in an external building alongside the eBIC and ePSIC national electron microscopy facilties.

I14 provides:

  • Spatial resolution down to 50nm
  • Wide energy range (5-20 keV)
  • Raster scanning capability for fast acquisition and increased sample area coverage.
  • XANES mapping capability
  • Differential phase contrast imaging
  • Ptychography
  • Simple data acquisition software with a strong emphasis on fast post acquisition data processing
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For more information on the beamline you can also see the beamline paper: (IUCr) The Hard X-ray Nanoprobe beamline at Diamond Light Source.

A collection of dried coccolithophore microalgae, as seen by combined XRF and DPC imaging.<br/>
A collection of dried coccolithophore microalgae, as seen by combined XRF and DPC imaging.

2D elemental mapping at 50 nm spatial resolution provides information on the chemical composition and elemental distribution in the sample. Additional information can be obtained by simultaneously acquiring imaging data. 

9-Energy X-ray fluorescence microscopy of ZnO nanorods after in-situ 1-hour incubation in a simulated sludge (humic acid 10 mg L-1)
9-Energy X-ray fluorescence microscopy of ZnO nanorods after in-situ 1-hour incubation in a simulated sludge (humic acid 10 mg L-1)
Fluorescence map acquired at the maximum of Zn K-edge XANES spectrum (Emax=9669 eV).
Cluster analisys revealing three main regions according to their Zn K-edge XANES spectra.
Speciation maps of the expected Zn-species: ZnO, ZnS, Zn3(PO4)2 and Zn adsorbed to Fe-oxyhydroxides (Zn-Fe(ox)) (from left to right),
where the red colour equals a 100% compound contribution and the blue colour corresponds to 0%
The numbering on the scale bars on the fluorescence map represent fluorescence intensity (arbitrary units). Scale bars equal to 750 nm in all cases.

DOI: 10.1021/acsnano.9b02866

Spatially-resolved X-ray Absorption Near-Edge Structure provides information on the chemical speciation of the element of choice.

Multivariate cluster anaylsis revealing statistically-similar regions acording to their XANES spectra, can be performed by the cross-platform python package - Mantis.

Speciation maps can be calculated through fitting the absorption data from each pixel to the linear combination of the standard spectra, representing the ratio between the expected species (Gomez-Gonzalez et al. 2019 - ACS Nano, 2019, 13, 11049–11061).

XRD mapping at I14. XRF map, showing the Ce signal of a particle. For each pixel in this XRF image a corresponding XRD pattern is recorded, so that local variations in the crystalline structure can be studied.
XRD mapping at I14. XRF map, showing the Ce signal of a particle. For each pixel in this XRF image a corresponding XRD pattern is recorded, so that local variations in the crystalline structure can be studied.

X-ray diffraction (XRD) can be used to spatially map changes in crystallographic direction, d-spacing or strain across a sample. A 2D XRD pattern is collected per pixel, in concert with the XRF signal. Processing in 1D or 2D is later achieved through DAWN.

At I14, XRD mapping is available in both wide- and small- angle scattering geometry. The q range available is ~1-3 A for WAXS.

 

Reconstruction of ptychographic data, recorded with monochromatic beam using the i14-MERLIN detector:
Reconstruction of ptychographic data, recorded with monochromatic beam using the i14-MERLIN detector:
(a) Probe modulus. Reconstructed probe size = 1.845 µm at 7.308 keV (800µm defocus)
(b) Object phase of a corroded Fe nanometric thin-film deposited onto a silicon nitride window. The reconstructed pixel size is 45 nm and the field of view is 16 × 16 µm2 at 7.308 keV.
(c) Object phase of a siemens star test sample, with radial markers representing ~100 nm line spacings.The reconstructed pixel size is 27 nm and the field of view is 18.3 × 18.3 µm2. Reconstructed probe size = 1.62 µm at 12 keV (800µm defocus).

X-ray ptychography imaging, which is a scanning coherent diffractive imaging technique, is now available at i14.

PtyREX, the reconstruction package for electrons and X-rays, was used for the processing and analysis of the ptychographic data. Each channel from the MERLIN detector was processed individually through 100 iterations of ePIE, with position correction and up-sampling.

XRF tomography
Aligned projections from XRF tomography of Au-Ag coated
microspheres, ​​​using the Ag-La signal in each frame.
This image series can then be reconstructed to show
the distribution of Ag around the sphere in 3D
(each sphere = ~4mm diameter). 

Our tomography capabilities are currently in development at I14. We can combine any of the techniques available with tomography to map your sample in 3D.  

Our most common use case is XRF tomography which allows us to display the elemental composition of a sample in 3D. Using DPC or ptychography, we can generate phase images in 3D giving density information. These techniques can be combined to give elemental analysis in context with lighter elements.

 

Schematic of example in situ chips. a) DENSsolutions heating chip that can be used for gas or liquid flow. b) DENSsolutions biasing chip that can be used with liquid.<br/>https://doi.org/10.1080/09603409.2023.2213579
Schematic of example in situ chips. a) DENSsolutions heating chip that can be used for gas or liquid flow. b) DENSsolutions biasing chip that can be used with liquid.
https://doi.org/10.1080/09603409.2023.2213579

Gas flow: samples can be subjected to a mixture of up to three gasses.

Liquid flow: liquid can be flown into the holder through a syringe pump.

Heating: samples can be heated up to 1100℃.

Biasing: samples can be subjected to electric biasing using a three electrode system attached to a Biologic SP200 potentiostat.

A variation of in situ sample environments are available: any type of Protochips and DENSsolutions liquid chip, DENSsolutions gas chips, K-kit liquid TEM holders.

Read more on the Beamline research projects page In-Situ.

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Diamond Light Source is the UK's national synchrotron science facility, located at the Harwell Science and Innovation Campus in Oxfordshire.

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