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MLZ
Lichtenbergstr.1
85748 Garching
Advanced Materials Group
The development of advanced materials is influenced strongly by the use of various material characterization methods. Investigations of crystallographic structures, phase transformations, particle morphologies and sizes, defect characterizations are key aspects. The Advanced Materials Group utilizes various neutron techniques (occasionally positron techniques generated by neutrons at the MLZ) to study central questions in the field of energy related topics as batteries and high-temperature alloys.
Batteries
Battery research using neutrons and positrons (R. Gilles, J. Synch. Investig.: X-ray, Synch. and Neutron Techn. 14, S69–S74 (2020)).
In the field of batteries, a huge demand emerged to follow electrochemical processes in situ or operando to understand in detail the mechanisms of energy storage systems. Neutrons were identified as a highly suitable probe thanks to their special properties, such as large penetration depths in materials, the non-destructive interaction due to meV energy transfer, the high sensitivity for light elements as especially Li and H in the presence of heavy elements and the easy distinction of neighbor elements or various isotopes of a single element.
Besides the well-established method of neutron diffraction using the LiCx peaks to study the intercalation or de-intercalation of Li in the graphite anode, other techniques became available to study other phenomena in battery research. Using the imaging techniques, the visualization of electrolyte filling, gassing or the Na liquid level of a ZEBRA cell in operation could be examined. Small-angle neutron scattering with the method of scattering-contrast variation (protonated and deuterated labelled samples to vary the sensitivity for example of the electrolyte) open another kind of application to receive further information on shell structures of electrode materials. Further techniques as neutron reflectivity, grazing incidence small-angle neutron scattering, positron annihilation spectroscopy using neutrons converted into positrons or prompt gamma activation analysis have been successful used. The available technologies at MLZ offer in situ cell diagnostics and ensure comprehensive process conclusions from combining application based research results with fundamental research. This opens up development potentials in many battery research fields like cost reduction, simplification of production processes, performance and aging of batteries.
High-Temperature Alloys
Neutron and complementary methods for the investigation of high-temperature alloys (R. Gilles, J. Synch. Investig.: X-ray, Synch. and Neutron Techn. 14, S69–S74 (2020)).
High-temperature alloys play a very important role in the strategy of sustainable energy resources. Their typical application fields are engine jets, stationary gas turbines and oil and gas transportation tubes. In addition, high-temperature alloys are used for hot-working tools, fans and furnace mufflers, heat exchangers, turbochargers, exhaust valves, rocket propulsions and medical components (dentistry and prostheses).
The low absorption of neutrons by a majority of materials enable neutron scattering techniques suitable for bulk characterization as well as for in-situ studies at operation conditions (e.g. high temperatures). By neutron diffraction it is possible to determine the phases present in the alloy as well as their volume fractions. With in situ investigations it is possible to determine solvus temperatures of the different phases, to follow the cell parameters evolution with temperature and to study changes in the mechanical response of the different phases under tensile/compressive tests. Small-angle neutron scattering provides information on the microstructures, i.e. morphology, sizes and volume fraction of the nanosized precipitates and by in situ studies it is possible to study the evolution of the precipitates with temperature and under tensile/compressive tests. In parallel a new testing machine that allows tension and compression of up to 100 kN with heating up to 1200 °C is set up to allow under development in order to allow in situ ND and SANS tests under tension and compression and temperature that will provide information about the structural-mechanical properties correlation of the studied materials and even simulate the forging process. Further applications as neutron depth profiling for boron distribution or neutron imaging of complete turbine discs or defect studies on alloys with positrons etc. enables to extend the studies with neutrons in this field.
Applied methods of the Advanced Materials Group
Selected Publications
Journal Article
Combined X-ray and Neutron Powder Diffraction Study on B-Site Cation Ordering in Complex Perovskite La$_{2}$(Al$_{1/2}$MgTa$_{1/2}$)O$_{6}$
Solids 4(1), 87 - 93 (2023) [10.3390/solids4010006]
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Dynamic Structure Evolution of Extensively Delithiated High Voltage Spinel Li$_{1+ x}$Ni$_{0.5}$Mn$_{1.5}$O$_{4}$ x < 1.5
Journal of the American Chemical Society 145(8), 4450 - 4461 (2023) [10.1021/jacs.2c09621]
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Monitoring the precipitation of the hardening phase in the new VDM® Alloy 780 by in-situ high-temperature small-angle neutron scattering, neutron diffraction and complementary microscopy techniques
Journal of alloys and compounds 928, 167203 - (2022) [10.1016/j.jallcom.2022.167203]
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Journal Article
Cracking during High-Temperature Deformation of a High-Strength Polycrystalline CoNi-Base Superalloy
Metals 12(9), 1520 - (2022) [10.3390/met12091520]
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Evolution of adsorption heights in the on-surface synthesis and decoupling of covalent organic networks on Ag(111) by normal-incidence X-ray standing wave
Nanoscale horizons 7(1), 51 - 62 (2022) [10.1039/D1NH00486G]
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Journal Article
Steering Self‐Assembly of Three‐Dimensional Iptycenes on Au(111) by Tuning Molecule‐Surface Interactions
Angewandte Chemie / International edition 61(25), e202201044 (2022) [10.1002/anie.202201044]
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Journal Article
Near-Surface and Bulk Dissolution Behavior of γ′ Precipitates in Nickel-Based VDM® Alloy 780 Studied with In-Situ Lab-Source and Synchrotron X-ray Diffraction
Metals 12(7), 1067 - (2022) [10.3390/met12071067]
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Journal Article
Influence of pressure and temperature on the electrolyte filling of lithium-ion cells: Experiment, model and method
Journal of power sources 517, 230668 - (2022) [10.1016/j.jpowsour.2021.230668]
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Journal Article
Detection of hydrate plugs inside submarine pipelines using neutrons
Nondestructive testing and evaluation 36, 1 - 13 (2022) [10.1080/10589759.2021.1990284]
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Journal Article
Morphology–Ionic Conductivity Relationship in Polymer–Titania Hybrid Electrolytes for Lithium-Ion Batteries
ACS applied energy materials 4(12), 13438 - 13443 (2021) [10.1021/acsaem.1c03393]
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Effects of Polymer Coating Mechanics at Solid‐Electrolyte Interphase for Stabilizing Lithium Metal Anodes
Advanced energy materials 0, 2103187 (2021) [10.1002/aenm.202103187]
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Deformation Mechanisms in Ni-Based Superalloys at Room and Elevated Temperatures Studied by In Situ Neutron Diffraction and Electron Microscopy
Metals 11(5), 719 (2021) [10.3390/met11050719] special issue: "Advances in Superalloys and High Temperature Intermetallics"
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TaC Precipitation Kinetics during Cooling of Co‐Re Base Alloys
Advanced engineering materials 23(11), adem.202100129 (2021) [10.1002/adem.202100129]
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Journal Article
Impact of Silicon Content within Silicon-Graphite Anodes on Performance and Li Concentration Profiles of Li-Ion Cells using Neutron Depth Profiling
Journal of the Electrochemical Society 168(2), 020519 - (2021) [10.1149/1945-7111/abe1db]
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How Neutrons Facilitate Research into Gas Turbines and Batteries from Development to Engineering Applications
Journal of surface investigation 14(S1), S69 - S74 (2020) [10.1134/S1027451020070162]
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Journal Article
A Liquid Electrolyte-Based Lithium-Ion Battery Cell Design for Operando Neutron Depth Profiling
Journal of the Electrochemical Society 167(10), 100554 - (2020) [10.1149/1945-7111/ab9b20]
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Journal Article
SEI Growth Impacts of Lamination, Formation and Cycling in Lithium Ion Batteries
Batteries 6(2), 21 - (2020) [10.3390/batteries6020021]
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Enhancing the High-Temperature Strength of a Co-Base Superalloy by Optimizing the gamma/gamma' Microstructure
Metals 10(3), 321 - (2020) [10.3390/met10030321]
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Li-ion half-cells studied operando during cycling by small-angle neutron scattering
Journal of applied crystallography 53(1), 210 - 221 (2020) [10.1107/S160057671901714X]
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HRTEM analysis of the high-temperature phases of the newly developed high-temperature Ni-base superalloy VDM 780 Premium
Journal of alloys and compounds 814, 152157 - (2020) [10.1016/j.jallcom.2019.152157]
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Journal Article
Effect of Cr and Ni on the microstructural evolution in Co–Re–Cr–Ni alloys
International journal of materials research 110(12), 1092 - 1104 (2019) [10.3139/146.111855]
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Linear and Nonlinear Aging of Lithium-Ion Cells Investigated by Electrochemical Analysis and In-Situ Neutron Diffraction
Journal of the Electrochemical Society 166(16), A3908 - A3917 (2019) [10.1149/2.1271915jes]
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Low‐Temperature Charging and Aging Mechanisms of Si/C Composite Anodes in Li‐Ion Batteries – An Operando Neutron Scattering Study
ChemSusChem 12, 1 (2019) [10.1002/cssc.201903139]
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Contribution to a conference proceedings/Report/Contribution to a book
Study of Phase Distribution on Alloy UNS N07718 in Different Hardening Conditions and Its Relationship with Hydrogen Embrittlement Susceptibility
NACE - International Corrosion Conference Series
Corrosion Conference and Expo 2019, NACE2019, NashvilleNashville, United States, 24 Mar 2019 - 28 Mar 2019
Houston, Texas : National Assoc. of Corrosion Engineers International 13025: 1 - 14 (2019)
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Proton conductivity in a hureaulite-type compound, Mn$_{5}$[(PO$_{4}$)$_{2}$(PO$_{3}$(OH))$_{2}$](HOH)$_{4}$
Journal of solid state chemistry 277, 290 - 302 (2019) [10.1016/j.jssc.2019.06.029]
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Contrast Matched SANS for Observing SEI and Pore Clogging in Silicon-Graphite Anodes
Journal of the Electrochemical Society 166(6), A1051 - A1054 (2019) [10.1149/2.0781906jes]
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Book/Proceedings
In Situ Characterization at High Temperature of VDM Alloy 780 Premium to Determine Solvus Temperatures and Phase Transformations Using Neutron Diffraction and Small-Angle Neutron Scattering
TMS 2019 Annual Meeting & Exhibition, TMS2019, San Antonio, TexasSan Antonio, Texas, USA, 10 Mar 2019 - 14 Mar 2019
Cham : Springer International Publishing, The Minerals, Metals & Materials Series (2019) [10.1007/978-3-030-05749-7_3]
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Differentiation of γ′- and γ″- precipitates in Inconel 718 by a complementary study with small-angle neutron scattering and analytical microscopy
Acta materialia 163, 28 - 39 (2019) [10.1016/j.actamat.2018.10.014]
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Journal Article
In Situ Characterization at Elevated Temperatures of a New Ni-Based Superalloy VDM-780 Premium
Metallurgical and materials transactions / A Physical metallurgy and materials science A 49(9), 4373 - 4381 (2018) [10.1007/s11661-018-4761-6]
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Journal Article
High-Temperature Stability of Phases in Boron Containing Co-Re Alloys for Gas Turbine Applications
Acta physica Polonica / A A 134(3), 829 - 837 (2018) [10.12693/APhysPolA.134.829]
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Journal Article
Materials science applications of Neutron Depth Profiling at the PGAA facility of Heinz Maier-Leibnitz Zentrum
Materials characterization 146, 127 - 134 (2018) [10.1016/j.matchar.2018.09.030]
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The new neutron depth profiling instrument N4DP at the Heinz Maier-Leibnitz Zentrum
Nuclear instruments & methods in physics research / A Accelerators, spectrometers, detectors and associated equipment Section A 911, 30 - 36 (2018) [10.1016/j.nima.2018.09.113]
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Journal Article
Quantifying the Distribution of Electrolyte Decomposition Products in Silicon-Graphite Electrodes by Neutron Depth Profiling
Connections / Athena papers Athena papers [...] 165(10), A2340 - A2348 (2018) [10.1149/2.1341810jes]
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Journal Article
Conductivity and Morphology Correlations of Ionic-Liquid/Lithium-Salt/Block Copolymer Nanostructured Hybrid Electrolytes
ACS applied energy materials 1(2), 666 - 675 (2018) [10.1021/acsaem.7b00173]
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Introduction to Electrochemical Impedance Spectroscopy as a Measurement Method for the Wetting Degree of Lithium-Ion Cells
Connections / Athena papers Athena papers [...] 165(14), A3249 - A3256 (2018) [10.1149/2.0081814jes]
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Journal Article
Additional Phases at High Boron Content in High-Temperature Co–Re–Cr Alloys
Metals 8(8), 621 - (2018) [10.3390/met8080621]
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In Situ Neutron Diffraction Study of Lithiation Gradients in Graphite Anodes during Discharge and Relaxation
Journal of the Electrochemical Society 165(9), A1846 - A1856 (2018) [10.1149/2.1231809jes]
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Journal Article
Electrodeposited Na$_2$Ni[Fe(CN)$_6$] Thin-Film Cathodes Exposed to Simulated Aqueous Na-Ion Battery Conditions
The journal of physical chemistry <Washington, DC> / C 122(16), 8760 - 8768 (2018) [10.1021/acs.jpcc.8b00395]
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Journal Article
Coexistence of Two Cubic-Lattice Co Matrices at High Temperatures in Co-Re-Cr-Ni Alloy Studied by Neutron Diffraction
Advances in materials science and engineering 2018, 1 - 6 (2018) [10.1155/2018/5410871]
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Aging in 18650-type Li-ion cells examined with neutron diffraction, electrochemical analysis and physico-chemical modeling
Journal of energy storage 17, 383 - 394 (2018) [10.1016/j.est.2018.03.016]
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Stability of TaC precipitates in a Co–Re-based alloy being developed for ultra-high-temperature applications
Journal of applied crystallography 49(4), 1253 - 1265 (2016) [10.1107/S1600576716009006]
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Journal Article
The new small-angle neutron scattering instrument SANS-1 at MLZ—characterization and first results
Nuclear instruments & methods in physics research / A 832, 297 - 305 (2016) [10.1016/j.nima.2016.06.105]
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Head of the group
Dr. habil. Ralph Gilles
Phone: +49 (0)89 289-14665
E-Mail: ralph.gilles@frm2.tum.de
Lithium ion batteries:
Thien An Pham
Phone: +49 (0)89 289-11774
E-Mail: thienan.pham@frm2.tum.de
Ivana Pivarnikova
Phone: +49 (0)89 289-54819
E-Mail: ivana.pivarnikova@frm2.tum.de
Dr. Lukas Grossmann
Phone: +49 (0)89 289-54725
E-Mail: lukas.grossmann@frm2.tum.de
Dr. Gilles Möhl
Phone: +49 (0)89 289-54827
E-Mail: gilles.moehl@frm2.tum.de
Advanced alloys:
N.N.
Phone: +49 (0)89 289-54827
E-Mail: N.N.
Dr. Massimo Fritton
Phone: +49 (0)89 289-54826
E-Mail: massimo.fritton@frm2.tum.de
Alexander Mutschke
E-Mail: alexander.mutschke@frm2.tum.de
Faryal Serwat
E-Mail: faryal.serwat@frm2.tum.de
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