I07-Surface & interface diffraction
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Diamond Proposal Number(s):
[39429]
Abstract: Formamidinium lead iodide (FAPbI3), which has a narrower band gap close to the Shockley-Queisser limit, offers higher power conversion efficiency (PCE) than other perovskite compositions, surpassing 27% [1]–[3]. However, under external stressors like moisture in ambient air processing conditions, its high tolerance factor value causes phase instability because of the larger ion size of FA+ [4]–[6]. Additionally, a higher annealing temperature (>390 K) is needed to reach the cubic α-phase of FAPbI3, whereas lower temperatures result in the formation of a non-photoactive δ-phase [7].
In recent years, FAPbI3 perovskite ink has been extensively incorporated with volatile methylammonium chloride (MACl) as a transitional stabilizer [8]. This substance effectively provides FAPbI3 black phase without annealing by decreasing the formation energy. However, the advantageous effects of MACl as an α-phase FAPbI3 inducer and stabilizer at room temperature are neutralized under ambient conditions and in the presence of non-volatile coordinating DMSO, which is frequently used as a co-solvent with toxic DMF to regulate the crystallization process [9]. DMSO accelerates the α-to-δ phase transition in air by displacing MACl from the intermediate film through the formation of stronger bonds with PbI2.
In this work, we use recently emerged Triethyl Phosphate (TEP) as a green solvent to dissolve FAPbI3 precursors and in-situ study its crystallization kinetics in the presence of MACl and excess PbI2 under ambient condition using transmission wide angle x-ray scattering (T-WAXS) [10] and steady-state photoluminescence (PL) techniques. Our results show that, unlike DMSO containing solvent systems, TEP with appropriate coordination ability allows for direct solvent extraction during anti-solvent quenching process avoiding intermediate phase formation. Furthermore, it has been found that the addition of excess PbI2 to the perovskite solution, along with MACl, not only regulates the pre-nucleation stage, leading to larger and more ordered crystals, as opposed to MACl alone as an additive, but also accelerates the formation of α-phase FAPbI3 at room temperature and stabilizes it under ambient condition during spin casting. This study paves the way for achieving high efficiency FAPbI3 solar cells using a non-toxic solvent system and under ambient conditions.
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May 2026
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I15-1-X-ray Pair Distribution Function (XPDF)
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Diamond Proposal Number(s):
[35312]
Abstract: Lithium batteries with enhanced energy density and safety require solid electrolytes having stability with High voltage cathodes and Li metal. Here, halide solid electrolyte Li3YCl6 is doped with Fluorine to simultaneously increase the cathodic and anodic stability. The anodic and cathodic stability was confirmed cyclic voltammetry, impedance spectroscopy and operando pressure measurement. Further, operando X-ray photoelectron spectroscopy (XPS) during Li plating on Li3YCl5.9F0.1 was done to study effect of Fluorine on reaction kinetics driving the evolution of interphase with Li metal and its composition. Li3YCl5.9F0.1 shows stable plating striping for more than 500 h and has very high critical current density of 8 mA/cm2. Li3YCl5.9F0.1 based ASSB operating at high voltage of 4.8 V vs Li maintains a high discharge capacity of 124 mAhg-1 at C/3 rate at room temperature after 180 cycles confirming excellent electrochemical performance. Further, Li3YCl5.9F0.1 as separator enable Li metal based ASSB.
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May 2026
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I21-Resonant Inelastic X-ray Scattering (RIXS)
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Gaurav C.
Pandey
,
Ashok S.
Menon
,
Valeria
Calani San Miguel
,
José J.
Arroyo‐gómez
,
Harry
Gillions
,
Rebecca
Sellers
,
Matthew J. W.
Ogley
,
Eleni
Fiamegkou
,
Satish
Bolloju
,
Sahil
Tippireddy
,
Mirian
Garcia-Fernandez
,
Steven
Huband
,
Louis F. J.
Piper
Diamond Proposal Number(s):
[38432]
Open Access
Abstract: The electrochemical performance of single-crystalline (SC) Ni-rich layered oxide cathodes is fundamentally limited by bulk Li+ diffusion within micrometre-sized particles. During high-voltage cycling—necessary for high-energy applications—intraparticle Li+ diffusion is further impeded by oxygen-loss-induced surface reconstruction from the layered phase to spinel/rock-salt structures. Therefore, to fully understand how bulk Li+ transport kinetics influences electrochemical degradation, it is necessary to establish the correlation between surface reconstruction and bulk delithiation during the anisotropic structural evolution (i.e., expansion of the layers followed by their contraction) of the cathode particles during long-term cycling. In this work, we accomplish this using multi-rate operando X-ray diffraction studies of SC Ni-rich layered oxide cathodes aged under different voltage windows in single-layer pouch full cells. We quantify how increased surface reconstruction leads to greater heterogeneity in bulk delithiation, thereby promoting phase separation and exacerbating electrochemical capacity fade. These results provide a direct mechanistic link between surface degradation and bulk delithiation in such cathodes and offer a framework for non-destructively probing kinetics-dependent degradation under practically relevant conditions to guide strategies for improved cycling stability.
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May 2026
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E01-JEM ARM 200CF
I13-1-Coherence
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Diamond Proposal Number(s):
[39271]
Open Access
Abstract: Multi-material structures have shown great versatility in wide applications. However, additive manufacturing of multi-metal mechanical composite structures is challenging. Beyond this, a comprehensive and multi-scale understanding of the fracture mechanisms in such structures has not been sufficiently elucidated. In this study, we exploited synchrotron phase contrast X-ray computed tomography and synchrotron X-ray ptychographic tomography to achieve in situ, continuous observation of the fracturing process in large-scale brick-and-mortar multi-metal composite structures, resolving phenomena spanning from the micro- to nano- scale. Findings suggest that nano-pores prevailingly exist in additively manufactured metals, and interfacial porosity as a transitional geometry between different materials can retard the crack growth and improve fracture toughness. This multi-scale study directly informs the designing, manufacturing, and testing of multi-metal composite structures.
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May 2026
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B07-B1-Versatile Soft X-ray beamline: High Throughput ES1
B07-C-Versatile Soft X-ray beamline: Ambient Pressure XPS and NEXAFS
B18-Core EXAFS
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Ainara
Aguadero
,
Federico
Baiutti
,
Monica
Burriel
,
Markus
Kubicek
,
Alexander Karl
Opitz
,
Juergen
Fleig
,
David
Munoz-Rojas
,
Christophe
Vallée
,
Marceline
Bonvalot
,
Alexia
Popescu
,
Nicola H
Perry
,
Francesco M.
Chiabrera
,
Álex
Morata
,
Juan Carlos
Gonzalez-Rosillo
,
Alexander
Stangl
,
Ramon
Escobar-Galindo
,
Mattias
Krause
,
Sivakkumaran
Sukumaran
,
Sarah
Fearn
,
Richard J.
Chater
,
Stephen J.
Skinner
,
John
Kilner
,
Sören
Möller
,
Martin
Finsterbusch
,
Manoj Kumar
Ghosalya
,
Samuli
Urpelainen
,
Christoph
Baeumer
,
Santosh
Kumar
,
Veronica
Celorrio
,
Diego
Gianolio
,
David C.
Grinter
,
Pilar
Ferrer-Escorihuela
,
Georg
Held
,
Jordi
Cabana
,
Sandrine
Lyonnard
,
Dorthe
Bomholdt Ravnsbaek
,
M. Rosa
Palacin
,
Montserrat
Casas-Cabanas
,
Julie
Villanova
,
Aline
Léon
,
Qiucheng
Xu
,
Jakub
Drnec
,
Brian
Seger
,
David R
Diercks
,
Nejc
Hodnik
,
Lluís
Yedra
,
Sonia
Estrade
,
Francesca
Peiró
,
Neus
Domingo
,
Maciej O
Liedke
,
Enric
Menéndez
,
David J.
Keeble
,
Jakub
Čížek
,
Ralf F.
Ziesche
,
Oriol
Sans Planell
,
Nikolay
Kardjilov
,
Ingo
Manke
,
Daniele
Pergolesi
,
Jochen
Stahn
Open Access
Abstract: A strong societal and political drive is motivating the development and optimization of novel
energy
conversion and storage systems for decarbonization. The successful implementation of solid
state devices such as fuel cells and secondary batteries depends, however, on achieving
ambitious targets in terms of performance, reliability and cost competitiveness. Research and
technology are addressing these needs through a holistic approach including exploration of new
materials and nanoarchitectures, as well as system engineering. These significant efforts require
the support of appropriate characterization tools capable of assessing nanometer-scale
phenomena such as concentration profiles of ionic and electronic charges, local chemical
compositions and their evolution over time across interfaces.
This roadmap provides an overview of selected advanced characterization techniques for
energy materials and devices. Specific focus is put on in situ/operando methods for probing
electrochemical phenomena in real-time under realistic working conditions. Experts in the field
provide an extensive review of the current state of the art in 2025 and the current and future
challenges for the characterization of local chemistry and kinetics in the bulk of the material, in
nanoarchitectures (e.g. thin films) and at the interfaces (e.g. grain boundaries, phase contacts,
solid/liquid and solid/gas interfaces) . The aim is to provide a detailed guide to the techniques,
describing opportunities and bottlenecks for their practical deployment and examples of
successful
applications.
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May 2026
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I11-High Resolution Powder Diffraction
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Open Access
Abstract: Polymorphism plays a critical role in determining the performance of bio-derived phase-change materials (PCMs). In this work, we investigate the polymorphism of methyl behenate, a fatty acid ester with potential for sustainable phase-change material for thermal energy storage. Three previously unknown polymorphs were identified, and their thermophysical properties were characterised by differential scanning calorimetry and hot-stage microscopy, highlighting the strong influence of polymorphism on the material properties. The structure of two polymorphs were determined using laboratory and synchrotron powder X-ray diffraction. The comparison with a related fatty acid ester reveals common structural trends, suggesting emerging structure–property relationships within this class of materials. These results provide new insights into ester-based PCMs and support the rational design of sustainable thermal energy storage materials.
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May 2026
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B18-Core EXAFS
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Diamond Proposal Number(s):
[15151]
Open Access
Abstract: The development of efficient and durable electrocatalysts for the formic acid oxidation reaction (FAOR) is central to the progress of direct formic acid fuel cells (DFAFCs). Here, we investigate how the synthesis sequence and reduction pathway influence the surface and electronic structure of PdAgNi(OH)2/C nanocomposites and, consequently, their FAOR performance in acidic media. Binary Pd/Ni(OH)2 catalysts with Pd/Ni(OH)2 mass ratios of 30:70, 50:50, and 70:30 were first screened, revealing 50:50 as the optimal composition. Partial substitution of Pd by Ag (Pd40Ag10 and Pd30Ag20 on Ni(OH)2(50)/C) was then combined with either sequential or simultaneous NaBH4-assisted reduction. Structural characterization by XRD, TEM, and XANES/EXAFS show that simultaneous coreduction tightens the Pd–Ag–Ni interfacial coupling, enhances Pd dispersion, and increases the contribution of Pd–O and Pd–Ni scattering paths, indicative of strong metal–oxide interactions. Electrochemical measurements demonstrate that the Pd30Ag20Ni(OH)2(50)/C catalyst prepared by simultaneous reduction exhibits the highest mass activity toward FAOR (6164 mA mgPd–1), a ca. 23-fold enhancement over commercial Pd/C, together with improved stability under potential cycling. These results demonstrate that controlling the synthesis sequence is an effective method for tuning the interfacial electronic structure of multicomponent Pd-based catalysts, providing practical guidelines for designing FAOR electrocatalysts for DFAFCs and related liquid-fuel energy conversion devices.
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May 2026
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I11-High Resolution Powder Diffraction
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Jamie W.
Gittins
,
Chloe J.
Balhatchet
,
James
Hill
,
Teedhat
Trisukhon
,
Malina
Seyffertitz
,
Seung-Jae
Shin
,
Yashna
Khakre
,
Kangkang
Ge
,
Thomas
Kress
,
Smaranda C.
Marinescu
,
Aron
Walsh
,
Oskar
Paris
,
Ieuan D.
Seymour
,
Alexander C.
Forse
Diamond Proposal Number(s):
[34243]
Open Access
Abstract: Understanding how ions interact with electrode surfaces at the molecular level is essential for improving the performance of energy storage devices and electrocatalysts. However, progress has been limited by the structural disorder and poorly defined surface chemistries of conventional carbon-based electrodes. In this work, we use layered metal–organic frameworks (MOFs) as model systems to investigate how different functional groups influence electric double-layer capacitance. We find that electrodes with deprotonated M–O and M–S groups exhibit significantly enhanced capacities with alkali metal cations, most notably Li+, compared to tetraethylammonium (TEA+), while no enhancement is observed for MOFs with protonated M–NH groups. The largest capacity increase is seen for MOF electrodes with metal–hydroxy linkages paired with Li+ electrolytes, which we attribute to strong Li–O interactions and improved charge screening. This mechanism is supported by solid-state nuclear magnetic resonance spectroscopy experiments and molecular simulations, which reveal specific Li+ binding at oxygen-rich sites, while operando X-ray techniques rule out cation intercalation as a contributing factor. Overall, these results highlight a chemically tunable strategy for enhancing charge storage in porous electrodes and offer new insights into how surface functionality impacts electric double-layer behavior.
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Apr 2026
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B18-Core EXAFS
I20-Scanning-X-ray spectroscopy (XAS/XES)
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Jarrod C.
Lewis
,
Joseph
Fihosy
,
Akhil
Gupta
,
James
Tufnail
,
Kirk
Adams
,
Matthew
Coulson
,
Petr
Zagura
,
William
Iliffe
,
Nianhua
Peng
,
Diego
Gianolio
,
Shusaku
Hayama
,
Rebecca J.
Nicholls
,
Sofia
Diaz-Moreno
,
Susannah C.
Speller
Diamond Proposal Number(s):
[33243]
Open Access
Abstract: Understanding how irradiation degrades superconductivity in REBCO coated conductor is a pressing field of research for the development of compact fusion devices. Here, defect formation in GdBa2Cu3O
coated conductor is studied using a high dose of 2 MeV He
ion irradiation. While laboratory based X-ray diffraction and magnetometry measurements show that the crystal structure becomes less well ordered with the loss of superconductivity in the material, transmission electron microscopy reveals a complex landscape of structural defects within the as-manufactured tape which complicate the identification and characterisation of irradiation induced structural changes. To resolve this, three sets of polarisation dependent extended X-ray absorption fine structure (EXAFS) spectroscopy experiments were carried out to map the local structure of the Gd, Ba, and Cu atomic sites within the material, providing three independent probes for studying irradiation defects within the structurally anisotropic REBCO unit cell. Here the Ba and Cu environments were the more sensitive to the irradiation treatment, with only small changes to the Gd local structure observed. Both the Ba and Cu local structures retained much of the pristine structure in the a/b-plane following irradiation, with greater shifts evident in the c-axis aligned measurements. In the irradiated Cu K edge EXAFS analysis, a shifted peak in the c-axis aligned measurements is observed that is not compatible with the REBCO local structure. This is attributed to an O site irradiation defect motif consistent with a Frenkel defect.
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Apr 2026
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B18-Core EXAFS
I20-Scanning-X-ray spectroscopy (XAS/XES)
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Diamond Proposal Number(s):
[21659, 28356]
Open Access
Abstract: Understanding the interplay between redox behavior and structural stability is crucial for the development of transition metal oxides in electrocatalysis. In this work, we use both X-ray absorption spectroscopy (XAS) and X-ray emission spectroscopy (XES) to investigate the electrochemical response of Mn-based perovskite oxides (La1–xCaxMnO3) under oxygen reduction reaction (ORR) conditions. This dual approach enables tracking of changes in both the oxidation state and local coordination environment. Mn Kβ XES data show that oxidation-state changes are reversible, despite a shift in transition potentials across a range of compositions, including CaMnO3. In contrast, Mn K-edge EXAFS analyses reveal that while LaMnO3 retains structural integrity, CaMnO3 undergoes irreversible structural changes at low potentials, associated with the collapse of the perovskite framework. Intermediate compositions show partially reversible structural behavior. This decoupling of redox reversibility and structural instability, a picture only accessible through the use of XAS and XES, provides critical insight into the complex behavior of these materials under operational conditions. Additionally, our analysis shows that Mn(II) formation is only detected in CaMnO3 at potentials more negative than 0.4 V (vs RHE). The ORR onset is associated with Mn(IV) reduction, while peroxide formation correlates with an increased Mn(III)/Mn(IV) ratio, supporting a 2e– + 2e– reduction pathway. This study demonstrates the power of XAS and XES analyses to disentangle electronic and structural dynamics, providing a more complete understanding of activity–stability relationships in perovskite electrocatalysts.
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Apr 2026
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