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MLZ

Lichtenbergstr.1
85748 Garching

Advanced Materials Group

2020-02-28_Advanced Material Group 2020-02-28_Advanced Material 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 Battery research Battery research using neutrons and positrons (R. Gilles, J. Synch. Investig.: X-ray, Synch. and Neutron Techn. 14, S69–S74 (2020)).

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 methods for the investigation of high-temperature alloys Neutron methods for the investigation of 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)).

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

The challenges in studies with neutron radiation always consist in defining suitable instruments for the specific question as well as in bringing the requirements imposed from the measurement method together with the requirements from the scientific study. Often it is necessary to create and use special sample environments, which need to be adjusted to the geometries of the sample, or vice versa to develop sample cells which fit the instrumental conditions.
  • Neutron diffraction (ND) The method of neutron diffraction allows to gather information on the chemical composition as well as the structure of the involved phases and their changes during electrochemical processes, temperature and mechanical tests. With these one can reveal e.g. loss of active lithium during aging, observes Li-plating or determine solvus temperature of constituting phases of a alloy.
  • Neutron imaging (NI) With imaging methods like radiography (2D) or tomography (3D) visualization of structures inside of a batteries as the distribution of electrolyte or Li during filling or cycling of cells. Cooling channels of turbine plates or other inhomogeneities in submillimeter range of alloys are visible.
  • Small-angle neutron scattering (SANS, resp. GISANS) With the methods of small-angle neutron scattering in transmission (SANS) or in reflection geometry (GISANS) information on size, shape and volume fractions of nano structures can be obtained during aging processes resp. during charging and discharging of batteries or during heating (grains coarsening and phase dissolution) or cooling down (phases precipitation) in superalloys.
  • Neutron depth profiling (NDP) The method of neutron depth profiling allows to determine concentration profiles near the surface of certain isotopes, like 6Li, N, S or B.
  • Prompt gamma activation analysis (PGAA) allows to determine element (resp. isotope) composition of a sample. The analysis allows often the determination even of small contaminations of electrodes (typically down to the ppm-level or even below). In alloys the boron addition on ppm level can be identified.
  • Positron annihilation spectroscopy (PAS) At the FRM II the most intense positron beam in the world is created by the use of neutrons. The unique property of positron radiation is its sensitivity to the presence of perturbations in the crystal lattice. These defects change the energy distribution as well as the life time of the annihilation radiation and allows to draw conclusions on the type and amount of defects in electrode materials correlated to ageing behaviour. Defect characterization in alloys allows to understand order and disorder phenomena in alloys.
  • Classical analytical methods like x-ray diffraction (XRD) as well as small-angle x-ray scattering (SAXS) are also complementarily available at MLZ in the Materials Science Lab of the group. Different wavelengths or a tempered (-30 to +60 °C) sample chamber for operando studies of thin pouch bag cells with XRD are available. Pouch cells in transmission mode and bulk alloys in Bragg Brentano geometry are typical applications for sample characterization.

Selected Publications

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Real-time observation of nucleation and growth of Au on CdSe quantum dot templates
Scientific reports 11(1), 18777 () [10.1038/s41598-021-97485-z] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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On-surface photopolymerization of two-dimensional polymers ordered on the mesoscale
Nature chemistry 13(8), 730 - 736 () [10.1038/s41557-021-00709-y] BibTeX | EndNote: XML, Text | RIS

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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 () [10.3390/met11050719] special issue: "Advances in Superalloys and High Temperature Intermetallics" DBCoverage  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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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 - () [10.1149/1945-7111/abe1db]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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In Situ Raman Characterization of SOFC Materials in Operational Conditions: A Doped Ceria Study
Membranes 10(7), 148 - () [10.3390/membranes10070148] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Carbon‐Carbon Coupling on Inert Surfaces by Deposition of En Route Generated Aryl Radicals
Angewandte Chemie / International edition 59(50), 22785 - 22789 () [10.1002/anie.202010833] BibTeX | EndNote: XML, Text | RIS

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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 () [10.1134/S1027451020070162]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Enhancing the High-Temperature Strength of a Co-Base Superalloy by Optimizing the gamma/gamma' Microstructure
Metals 10(3), 321 - () [10.3390/met10030321] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Surface distortion of Fe dot-decorated TiO$_{2}$ nanotubular templates using time-of-flight grazing incidence small angle scattering
Scientific reports 10(1), 4038 () [10.1038/s41598-020-60899-2] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1107/S160057671901714X]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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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 - () [10.1016/j.jallcom.2019.152157]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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A Kinetic Study on the Evolution of Martensitic Transformation Behavior and Microstructures in Ti–Ta High-Temperature Shape-Memory Alloys During Aging
Shape memory and superelasticity 5(1), 16 - 31 () [10.1007/s40830-018-00200-7] BibTeX | EndNote: XML, Text | RIS

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Competitive Metal Coordination of Hexaaminotriphenylene on Cu(111) by Intrinsic Copper Versus Extrinsic Nickel Adatoms
Chemistry - a European journal 25(8), 1975 - 1983 () [10.1002/chem.201803908] BibTeX | EndNote: XML, Text | RIS

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The Role of Kinetics versus Thermodynamics in Surface-Assisted Ullmann Coupling on Gold and Silver Surfaces
Journal of the American Chemical Society 141(12), 4824 - 4832 () [10.1021/jacs.8b11473] BibTeX | EndNote: XML, Text | RIS

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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 () [10.1149/2.1271915jes]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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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 () [10.1002/cssc.201903139]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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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 20192019-03-242019-03-28
Houston, Texas : National Assoc. of Corrosion Engineers International 13025: 1 - 14 ()  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1016/j.jssc.2019.06.029]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1149/2.0781906jes]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 20192019-03-102019-03-14 Cham : Springer International Publishing, The Minerals, Metals & Materials Series () [10.1007/978-3-030-05749-7_3]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1016/j.actamat.2018.10.014]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Crystallographic Structure Analysis of a Ti–Ta Thin Film Materials Library Fabricated by Combinatorial Magnetron Sputtering
ACS combinatorial science 20(3), 137 - 150 () [10.1021/acscombsci.7b00135] BibTeX | EndNote: XML, Text | RIS

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On-Surface Polymerization of 1,6-Dibromo-3,8-diiodpyrene—A Comparative Study on Au(111) Versus Ag(111) by STM, XPS, and NEXAFS
The journal of physical chemistry <Washington, DC> / C 122(11), 5967 - 5977 () [10.1021/acs.jpcc.7b10403] BibTeX | EndNote: XML, Text | RIS

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The influence of ortho -methyl substitution in organometallic self-assembly – a comparative study on Cu(111) vs. Ag(111)
Chemical communications 54(70), 9745 - 9748 () [10.1039/C8CC04854A] BibTeX | EndNote: XML, Text | RIS

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Evaluation of anisotropic small-angle neutron scattering data from metastable β-Ti alloy
The philosophical magazine 98(34), 3086 - 3108 () [10.1080/14786435.2018.1520403]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1007/s11661-018-4761-6]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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High-Temperature Stability of Phases in Boron Containing Co-Re Alloys for Gas Turbine Applications
Acta physica Polonica / A A 134(3), 829 - 837 () [10.12693/APhysPolA.134.829]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Materials science applications of Neutron Depth Profiling at the PGAA facility of Heinz Maier-Leibnitz Zentrum
Materials characterization 146, 127 - 134 () [10.1016/j.matchar.2018.09.030]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1016/j.nima.2018.09.113]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Quantifying the Distribution of Electrolyte Decomposition Products in Silicon-Graphite Electrodes by Neutron Depth Profiling
Connections / Athena papers Athena papers [...] 165(10), A2340 - A2348 () [10.1149/2.1341810jes]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Conductivity and Morphology Correlations of Ionic-Liquid/Lithium-Salt/Block Copolymer Nanostructured Hybrid Electrolytes
ACS applied energy materials 1(2), 666 - 675 () [10.1021/acsaem.7b00173]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1149/2.0081814jes]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Additional Phases at High Boron Content in High-Temperature Co–Re–Cr Alloys
Metals 8(8), 621 - () [10.3390/met8080621] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1149/2.1231809jes]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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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 () [10.1021/acs.jpcc.8b00395]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1155/2018/5410871] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1016/j.est.2018.03.016]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Cycling capacity recovery effect: A coulombic efficiency and post-mortem study
Journal of power sources 365, 327 - 338 () [10.1016/j.jpowsour.2017.08.090]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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Influence of Particle Morphologies of LiFePO4 on Water- and Solvent-Based Processing and Electrochemical Properties
Sustainability 9(6), 888 - () [10.3390/su9060888] DBCoverage  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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The influence of C/Ta ratio on TaC precipitates in Co-Re base alloys investigated by small-angle neutron scattering
Acta materialia 132, 354 - 366 () [10.1016/j.actamat.2017.04.029]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Nano-metric self-diffusion of Fe: effect of grain size
RSC Advances 7(16), 9573 - 9578 () [10.1039/C6RA28310A]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Aging behavior of lithium iron phosphate based 18650-type cells studied by in situ neutron diffraction
Journal of power sources 345, 85 - 96 () [10.1016/j.jpowsour.2017.01.134]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Post-Synthetic Decoupling of On-Surface-Synthesized Covalent Nanostructures from Ag(111)
Angewandte Chemie / International edition 55(27), 7650 - 7654 () [10.1002/anie.201600684] BibTeX | EndNote: XML, Text | RIS

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Formation of a thermally stable bilayer of coadsorbed intact and deprotonated thymine exploiting the surface corrugation of rutile TiO 2 (110)
Physical chemistry, chemical physics 18(30), 20433 - 20442 () [10.1039/C6CP02541B] BibTeX | EndNote: XML, Text | RIS

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Morphology of Fe nanolayers with Pt overlayers on low-temperature annealing
Journal of applied crystallography 49, 1682 - 1692 () [10.1107/S1600576716011882]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Self-organized in-plane ordering of nanostructures at epitaxial ferroelectric–ferromagnetic interfaces
Journal of applied crystallography 49, 1693 - 1703 () [10.1107/S1600576716012115]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Realizing topological stability of magnetic helices in exchange-coupled multilayers for all-spin-based system
Scientific reports 6, 33986 () [10.1038/srep33986] DBCoverage  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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First-cycle defect evolution of Li$_{1−x}$Ni$_{1/3}$Mn$_{1/3}$Co$_{1/3}$O$_2$ lithium ion battery electrodes investigated by positron annihilation spectroscopy
Journal of power sources 336, 224 - 230 () [10.1016/j.jpowsour.2016.10.050]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Effect of composition on the matrix transformation of the Co-Re-Cr-Ta-C alloys
Metals and materials international 22(4), 562 - 571 () [10.1007/s12540-016-5697-2]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Evolution of strain-induced hafnium carbides in a molybdenum base Mo–Hf–C alloy studied by small-angle neutron scattering and complementary methods
Journal of alloys and compounds 688, 619 - 631 () [10.1016/j.jallcom.2016.06.282]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1107/S1600576716009006]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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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 () [10.1016/j.nima.2016.06.105]  Download fulltext Files  Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

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Self-organization of Fe clusters on mesoporous TiO$_2$ templates
Journal of applied crystallography 47(6), 1921 - 1930 () [10.1107/S1600576714021049]  Download fulltext Files BibTeX | EndNote: XML, Text | RIS

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Half antiperovskites: V. Systematics in ordering and group-subgroup-relations for Pb$_2$ Pd$_3$ Se$_2$ , Bi$_2$ Pd$_3$ Se$_2$ , and Bi$_2$ Pd$_3$ S$_2$
Zeitschrift für Kristallographie / Crystalline materials 225(9), 371 - 381 () [10.1524/zkri.2010.1272]   Download fulltextFulltext BibTeX | EndNote: XML, Text | RIS

Head of the group

Dr. habil. Ralph Gilles
Phone: +49 (0)89 289-14665
E-Mail: ralph.gilles@frm2.tum.de

Lithium ion batteries:

Dr. Neelima Paul
Phone: +49 (0)89 289-11765
E-Mail: neelima.paul@frm2.tum.de

Dr. Stefan Seidlmayer
Phone: +49 (0)89 289-11768
E-Mail: stefan.seidlmayer@frm2.tum.de

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

Advanced alloys:

Dr. Frank Kümmel
Phone: +49 (0)89 289-54827
E-Mail: frank.kuemmel@frm2.tum.de

Dr. Massimo Fritton
Phone: +49 (0)89 289-54826
E-Mail: massimo.fritton@frm2.tum.de

Students:

Robert Herman
Osama Deeb

Links

Current Projects:

  • BMWi: CAESAR
  • BMBF: TUBE
  • BMBF: ExZellTUM III
  • BMBF: HiMat
  • BMBF: LiSI
  • BMBF: CharLiSiKo
  • BMBF: Time resolved N4DP

Former Projects:

  • BMBF: INA780
  • BMBF: ExZellTUM
  • BMBF: ExZellTUM II
  • Bayerische Staatsregierung: EEBatt
  • BMBF: 4D N4DP
  • DFG: CoRe alloys
  • DAAD: CSC High-temperature alloys
  • DAAD: CoRe alloys

MLZ ist eine Kooperation aus:

Technische Universität München> Technische Universität MünchenHelmholtz-Zentrum Hereon> Helmholtz-Zentrum Hereon
Forschungszentrum Jülich> Forschungszentrum Jülich

MLZ ist Mitglied in:

LENS> LENSERF-AISBL> ERF-AISBL

MLZ in den sozialen Medien: