I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[29851]
Open Access
Abstract: The formation of heterogeneous Li structures at the anode/solid polymer electrolyte (SPE) membrane interphase of solid-state Li-metal batteries (SSLMBs) is one of the key factors that impede SSLMB performance. The relationship between Li+-ion transport kinetics and Li0 structural evolution at the buried interphase is critical but challenging to characterize. Here, we report an operando correlative X-ray Compton scattering and computed tomography imaging technique that quantifies the changes of Li+-ion concentrations in the bulk cathode, SPE membrane, and anode of the SSLMB full cell using a commercially standard configuration. We then visualize Li+-ion concentration distributions as well as Li0 microstructures at the buried anode/SPE interphase. Mechanistic analyses show that the Li-stripping step forms more irregular interfacial Li morphologies at the expense of bulk anode volume shrinkage compared to the Li-plating step during the first cycle.
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May 2024
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B16-Test Beamline
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B. D.
Cline
,
D.
Banks
,
S.
Bell
,
I.
Church
,
A.
Davis
,
T.
Gardiner
,
J.
Harris
,
M.
Hart
,
L.
Jones
,
T.
Nicholls
,
J.
Nobes
,
S.
Pradeep
,
M.
Roberts
,
D.
Sole
,
M. C.
Veale
,
M. D.
Wilson
,
V.
Dhamgaye
,
O.
Fox
,
K.
Sawhney
Diamond Proposal Number(s):
[32772]
Open Access
Abstract: In this paper, results are presented from the characterisation of Redlen Technologies high-flux-capable Cadmium Zinc Telluride (HF-CZT) hybridised to the HEXITECMHz ASIC, a novel 1 MHz continuous X-ray imaging system. A 2 mm thick HF-CZT HEXITECMHz detector was characterised on the B16 Test Beamline at the Diamond Light Source and displayed an average FWHM of 850 eV for monochromatic X-rays of energy 20 keV. Measurements revealed a shift in the baseline of irradiated pixels that results in a movement of the entire spectrum to higher ADU values. Datasets taken to analyse the effect's dynamics showed it to be highly localised and flux-dependent, with the excess leakage current generated equivalent to per-pixel shifts of ∼ 543 pA (8.68 nA mm-2) at a flux of 1.26×107 ph s-1 mm-2. Comparison to results from a p-type Si HEXITECMHz device indicate this `excess leakage-current' effect is unique to HF-CZT and it is hypothesised that it originates from trapping at the electrode-CZT interface and a temporary modification of the potential barrier between the CZT and metal electrode.
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Apr 2024
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B16-Test Beamline
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B. D.
Cline
,
D.
Banks
,
S.
Bell
,
I.
Church
,
S.
Cross
,
A.
Davis
,
C.
Day
,
M.
French
,
T.
Gardiner
,
N.
Ghorbanian
,
J.
Harris
,
M.
Hart
,
J.
Holden
,
J.
Lipp
,
T.
Nicholls
,
J.
Nobes
,
S.
Pradeep
,
M.
Prydderch
,
M.
Roberts
,
A.
Schneider
,
P.
Seller
,
D.
Sole
,
M. C.
Veale
,
M. D.
Wilson
,
W.
Helsby
,
V.
Dhamgaye
,
O.
Fox
,
K.
Sawhney
Diamond Proposal Number(s):
[32772]
Abstract: Spectroscopic X-ray imaging techniques including Compton X-ray Imaging, X-ray Fluorescence Imaging and Hyperspectral X-ray Tomography require energy-resolving detectors capable of operating at high incident X-ray fluxes to make time resolved measurements. HEXITECMHz, operates at a continuous 1 MHz frame rate and can make fully spectroscopic measurements at >106 ph s−1 mm−2. This is enabled by an integrating Front End, in-pixel digitisation and high-speed serialisers. A 300 μm thick p-type Si HEXITECMHz detector was characterised on the B16 Test Beamline at the Diamond Light Source and are the first measurements taken at a 1 MHz frame rate. At 10 keV and 15 keV) the device displayed average FWHM of 656 eV and 682 eV respectively, with minimal changes in spectroscopic performance over ∼8 h. Analysis of charge-sharing events show low charge loss and a linear energy-signal response. Higher-flux measurements illustrated the capability of the ASIC to operate as a photon-counting device.
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Sep 2023
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B16-Test Beamline
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M. C.
Veale
,
S.
Bell
,
B. D.
Cline
,
I.
Church
,
S.
Cross
,
C.
Day
,
M.
French
,
T.
Gardiner
,
N.
Ghorbanian
,
M. D.
Hart
,
L. L.
Jones
,
J.
Lipp
,
T.
Nicholls
,
J.
Nobes
,
M.
Prydderch
,
A.
Schneider
,
P.
Seller
,
D.
Sole
,
M. D.
Wilson
,
V.
Dhamgaye
,
O.
Fox
,
K.
Sawhney
Diamond Proposal Number(s):
[32491]
Open Access
Abstract: The HEXITECMHz ASIC is the next generation of the STFC's High Energy X-ray Imaging Technology (HEXITEC). With a ×100 increase in the camera frame rate to 1 MHz, the new ASIC is capable of delivering fully spectroscopic X-ray imaging at photon fluxes of 2×106 photons s-1 mm-2. The improved flux capability ensures the relevance of the technology at a new generation of difraction-limited storage ring (DLSR) synchrotrons as well as enabeling dynamic spectroscopic imaging with sub-keV energy resolution to be carried out on millisecond timescales. In this paper preliminary results from X-ray testing of a 0.3 mm thick p-type Si sensor and 2.0 mm thick HF-CdZnTe sensor at the Diamond Light Source Synchrotron are presented for the first time. Each module consists of 80 × 80 pixels on a 250 μm pixel pitch operated at a temperature of 20°C and a frame rate of 1 MHz. For these preliminary measurements, testing was completed using a prototype test system which limited readout to a portion of the 1 MHz output sampled over an SPI test interface at ∼50 Hz. Despite this limitation these measurements allow the spectroscopic performance of the ASIC to be characterised ahead of the full DAQ system. The prototype detectors were characterised using monochromatic X-rays with energies 12–35 keV at fluxes of (0.6 – 2.5) × 106 photons s-1 mm-2. At an X-ray energy of 12 keV, the energy resolution of the p-type Si and HF-CdZnTe detectors were measured to be 1.0 keV and 1.1 keV respectively. At the higher energies of 20 keV and 35 keV the energy resolution in the HF-CdZnTe was measured to be 1.2 keV and 1.4 keV respectively.
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Jul 2023
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I12-JEEP: Joint Engineering, Environmental and Processing
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Chu Lun Alex
Leung
,
Matthew D.
Wilson
,
Thomas
Connolley
,
Stephen P.
Collins
,
Oxana V.
Magdysyuk
,
Matthieu N.
Boone
,
Kosuke
Suzuki
,
Matthew C.
Veale
,
Enzo
Liotti
,
Frederic
Van Assche
,
Andrew
Lui
,
Chun
Huang
Diamond Proposal Number(s):
[23400]
Open Access
Abstract: Increasing electrode thickness is gaining more attention as a potential route to increase energy density for Li ion batteries although the realizable capacity and rate capability are usually limited by Li+ ion diffusion during (dis)charge, especially at increased (dis)charge rates. It remains challenging to visualize and quantify the low atomic number Li+ chemical stoichiometry distribution inside the electrode within commercially standard battery geometry, e.g., coin cells with stainless steel casings. Here, we map the distribution of Li+ chemical stoichiometry in the electrode microstructure inside a working coin cell battery to show the amount of electrode materials contributing to energy storage performance using innovative in situ correlative full-field X-ray Compton scattering imaging (XCS-I) and X-ray computed tomography (XCT). We design and fabricate an ultra-thick (∼1 mm) cathode of LiNi0.8Mn0.1Co0.1O2 with a microstructure containing vertically oriented pore arrays using a directional ice templating method. This novel technique paves a new way to map low atomic number elements in 3D structures and study how the microstructure improves Li+ ion diffusivity and energy storage performance.
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Dec 2022
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I10-Beamline for Advanced Dichroism - scattering
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Diamond Proposal Number(s):
[27196]
Abstract: Isotropic helimagnets are known to host a diverse range of chiral magnetic states. In 2016, Rybakov et al., theorized the presence of a surface-pinned stacked spin spiral phase [F. N. Rybakov et al., New J. Phys. 18, 045002 (2016)], which has yet to be observed experimentally. The phase is characterized by surface spiral periods exceeding the host material's fundamental winding period
L
D
. Here, we present experimental evidence for the observation of this state in lamellae of FeGe using resonant x-ray holographic imaging data and micromagnetic simulations. We find images of FeGe lamellae, exceeding a critical thickness of 300 nm (
4.3
L
D
), exhibit contrast modulations with a field-dependent periodicity of
λ
≥
1.4
L
D
, consistent with theoretical predictions of the stacked spiral state. The identification of this spiral state has significant implications for the stability of other coexisting spin textures, and will help complete our understanding of helimagnetic systems.
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Aug 2022
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I12-JEEP: Joint Engineering, Environmental and Processing
|
Chun
Huang
,
Matthew
Wilson
,
Kosuke
Suzuki
,
Enzo
Liotti
,
Thomas
Connolley
,
Oxana
Magdysyuk
,
Stephen
Collins
,
Frederic
Van Assche
,
Matthieu N
Boone
,
Matthew C.
Veale
,
Andrew
Lui
,
Rhian-Mair
Wheater
,
Chu Lun Alex
Leung
Diamond Proposal Number(s):
[23400]
Open Access
Abstract: The performance of Li+ ion batteries (LIBs) is hindered by steep Li+ ion concentration gradients in the electrodes. Although thick electrodes (≥300 µm) have the potential for reducing the proportion of inactive components inside LIBs and increasing battery energy density, the Li+ ion concentration gradient problem is exacerbated. Most understanding of Li+ ion diffusion in the electrodes is based on computational modeling because of the low atomic number (Z) of Li. There are few experimental methods to visualize Li+ ion concentration distribution of the electrode within a battery of typical configurations, for example, coin cells with stainless steel casing. Here, for the first time, an interrupted in situ correlative imaging technique is developed, combining novel, full-field X-ray Compton scattering imaging with X-ray computed tomography that allows 3D pixel-by-pixel mapping of both Li+ stoichiometry and electrode microstructure of a LiNi0.8Mn0.1Co0.1O2 cathode to correlate the chemical and physical properties of the electrode inside a working coin cell battery. An electrode microstructure containing vertically oriented pore arrays and a density gradient is fabricated. It is shown how the designed electrode microstructure improves Li+ ion diffusivity, homogenizes Li+ ion concentration through the ultra-thick electrode (1 mm), and improves utilization of electrode active materials.
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Apr 2022
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B16-Test Beamline
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R. M.
Wheater
,
L.
Jowitt
,
S.
Richards
,
M. C.
Veale
,
M. D.
Wilson
,
O. J. L.
Fox
,
K. J. S.
Sawhney
,
A. D.
Lozinskaya
,
A.
Shemeryankina
,
O. P.
Tolbanov
,
A.
Tyazhev
,
A. N.
Zarubin
Diamond Proposal Number(s):
[23500]
Abstract: A newly supplied 80 × 80 chromium compensated GaAs sensor with a matrix of 80 × 80 pixels on a 250
m pixel pitch has been characterised utilising microbeam mapping techniques at the Diamond Light Source. The GaAs:Cr sensor was mounted to a HEXITEC DAQ system before raster scanning an x-ray beam with area 25 × 25
m
in steps of 25
m, providing sub-pixel resolution spectroscopic imaging. Scans were performed with incident x-ray energies ranging from 12 to 45 keV. Following processing of the data in MatLab 2019b an analysis of defects previously observed in etched GaAs wafers occured. Findings indicate the presence of regions with reduced charge collection efficiency where up to 88 % of incident events show significant charge loss, and changing charge carrier lifetimes across the sensor.
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Mar 2021
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I12-JEEP: Joint Engineering, Environmental and Processing
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Diamond Proposal Number(s):
[16771]
Open Access
Abstract: An experimental technique is described for the collection of time-resolved X-ray diffraction information from a complete commercial battery cell during discharging or charging cycles. The technique uses an 80 × 80 pixel 2D energy-discriminating detector in a pinhole camera geometry which can be used with a polychromatic X-ray source. The concept was proved in a synchrotron X-ray study of commercial alkaline Zn–MnO2 AA size cells. Importantly, no modification of the cell was required. The technique enabled spatial and temporal changes to be observed with a time resolution of 20 min (5 min of data collection with a 15 min wait between scans). Chemical changes in the cell determined from diffraction information were correlated with complementary X-ray tomography scans performed on similar cells from the same batch. The clearest results were for the spatial and temporal changes in the Zn anode. Spatially, there was a sequential transformation of Zn to ZnO in the direction from the separator towards the current collector. Temporally, it was possible to track the transformation of Zn to ZnO during the discharge and follow the corresponding changes in the cathode.
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Dec 2020
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I12-JEEP: Joint Engineering, Environmental and Processing
|
Abstract: Over the last decade, the High-Energy X-ray Imaging Technology
(HEXITEC) detector system for spectroscopic imaging of hard X-rays
and γ-rays has been developed by the Science & Technology Facilities
Council (STFC). The system is based upon the room-temperature compound
semiconductor cadmium telluride (CdTe) which, due to its high
density and large band gap, allows the measurement of X-ray and γ-ray
spectra up to energies of 200 keV with an energy resolution of <1 keV
without the need for cryogenic cooling systems. The technology differs
significantly from single photon counting detector systems, where
a count is registered each time the output of a pixel is above a threshold.
In the HEXITEC system, each 250 μm pixel is able to record the precise
energy deposited by an interaction and, over multiple frames, compiles
energy-resolved X-ray spectra on a per-pixel basis rather than a simple
2D image. The system has been used at synchrotrons in applications
which wish to discern mechanical, structural, or chemical information
from within thick samples or to determine the chemical composition
of samples containing multiple high Z materials which, typically, have
closely spaced K-line X-ray emissions. While originally developed for
materials science applications, the system has been successfully
used across a diverse range of fields, including pure science, solar
physics, medical imaging, and security applications. This
article will review the current status of the technology and the performance
of the latest system, and demonstrate the use of the system on a
synchrotron beamline.
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Nov 2018
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