kth.sePublications
Change search
Link to record
Permanent link

Direct link
Publications (10 of 15) Show all publications
Zhou, T., Spartacus, G., Li, X., Guehairia, S., Fischer, T., Blankenburg, M. & Hedström, P. (2025). Direct evidence and kinetics of Cu precipitation in the austenite phase of a maraging stainless steel. Materials & design, 252, Article ID 113835.
Open this publication in new window or tab >>Direct evidence and kinetics of Cu precipitation in the austenite phase of a maraging stainless steel
Show others...
2025 (English)In: Materials & design, ISSN 0264-1275, E-ISSN 1873-4197, Vol. 252, article id 113835Article in journal (Refereed) Published
Abstract [en]

In this study, we investigate the precipitation kinetics of Cu in 15–5 PH maraging stainless steel during high-temperature thermal treatments in the fully austenitic state. This provides direct evidence that Cu precipitation can occur in the austenite phase of martensitic or ferritic steels. The kinetics of Cu precipitation in austenite are examined at 700 and 800 °C using in situ synchrotron small-angle and wide-angle X-ray scattering, complemented by atom probe tomography investigations to analyze the precipitates, particularly their chemistry, following heat treatment. The resulting experimental data, which include the evolution of size, volume fraction, number density and chemical composition, are used to inform precipitation kinetics modelling using the Langer-Schwartz-Kampmann-Wagner (LSKW) approach coupled with CALPHAD thermodynamic and kinetic databases. The simulations accurately capture the experimental data by adjusting the interfacial energy in an inverse modelling approach. The insight that Cu precipitation occurs in austenite and subsequently in martensite paves the way for design of hierarchical structures with a bi-modal particle size distribution of Cu precipitates with varying crystal structures and compositions. Additionally, the validated LSKW modelling approach establishes a foundation for designing Cu-alloyed high-performance steels, taking into account various manufacturing routes.

Place, publisher, year, edition, pages
Elsevier BV, 2025
Keywords
CALPHAD-based modelling, Cu precipitation in austenite, In situ synchrotron SAXS/WAXS, Maraging stainless steel, Precipitation kinetics
National Category
Metallurgy and Metallic Materials Other Materials Engineering
Identifiers
urn:nbn:se:kth:diva-361784 (URN)10.1016/j.matdes.2025.113835 (DOI)001448297900001 ()2-s2.0-86000742744 (Scopus ID)
Note

QC 20250331

Available from: 2025-03-27 Created: 2025-03-27 Last updated: 2025-03-31Bibliographically approved
Salliot, F., Borbély, A., Sornin, D., Logé, R., Spartacus, G., Leguy, H., . . . de Carlan, Y. (2024). Dislocation Hardening in a New Manufacturing Route of Ferritic Oxide Dispersion-Strengthened Fe-14Cr Cladding Tube. Materials, 17(5), Article ID 1146.
Open this publication in new window or tab >>Dislocation Hardening in a New Manufacturing Route of Ferritic Oxide Dispersion-Strengthened Fe-14Cr Cladding Tube
Show others...
2024 (English)In: Materials, E-ISSN 1996-1944, Vol. 17, no 5, article id 1146Article in journal (Refereed) Published
Abstract [en]

The microstructure evolution associated with the cold forming sequence of an Fe-14Cr-1W-0.3Ti-0.3Y2O3 grade ferritic stainless steel strengthened by dispersion of nano oxides (ODS) was investigated. The material, initially hot extruded at 1100 °C and then shaped into cladding tube geometry via HPTR cold pilgering, shows a high microstructure stability that affects stress release heat treatment efficiency. Each step of the process was analyzed to better understand the microstructure stability of the material. Despite high levels of stored energy, heat treatments, up to 1350 °C, do not allow for recrystallization of the material. The Vickers hardness shows significant variations along the manufacturing steps. Thanks to a combination of EBSD and X-ray diffraction measurements, this study gives a new insight into the contribution of statistically stored dislocation (SSD) recovery on the hardness evolution during an ODS steel cold forming sequence. SSD density, close to 4.1015 m−2 after cold rolling, drops by only an order of magnitude during heat treatment, while geometrically necessary dislocation (GND) density, close to 1.1015 m−2, remains stable. Hardness decrease during heat treatments appears to be controlled only by the evolution of SSD.

Place, publisher, year, edition, pages
Multidisciplinary Digital Publishing Institute (MDPI), 2024
Keywords
cold rolling, dislocation density, EBSD, microstructure, ODS steel, X-ray diffraction
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-344802 (URN)10.3390/ma17051146 (DOI)2-s2.0-85187689530 (Scopus ID)
Note

QC 20240403

Available from: 2024-03-28 Created: 2024-03-28 Last updated: 2024-07-04Bibliographically approved
Spartacus, G., Malaplate, J., De Geuser, F., Mouton, I., Sornin, D., Guillou, R. & Deschamps, A. (2024). Precipitation kinetics of ferritic / martensitic oxide dispersion strengthened steels: Influence of the matrix phase transformation. Acta Materialia, 280, Article ID 120328.
Open this publication in new window or tab >>Precipitation kinetics of ferritic / martensitic oxide dispersion strengthened steels: Influence of the matrix phase transformation
Show others...
2024 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 280, article id 120328Article in journal (Refereed) Published
Abstract [en]

ODS steels are candidate materials for the future generation of nuclear power plants. Ferritic / Martensitic (F/M) ODS steels display better formability thanks to high temperature austenitic transformation. The precipitation kinetics of a F/M Fe‑9Cr ODS steel during powder consolidation up to 1100 °C has been characterized by in‑situ Small Angle X-ray Scattering (SAXS). The influence of the matrix phase transformation has been established, showing an increase of the growth rate of the nano‑oxides in austenite, leading to nano‑oxides ∼ 2x larger in diameter than in Fe‑14Cr ferritic ODS grades at the end of the thermal treatment. These results are further supported by local atom probe tomography (APT) performed across grains showing contrasted microstructure and composition. Anomalous SAXS as well as comparison between APT and SAXS provide evidence that the nano‑oxides stabilize with a Y2Ti2O7 or Y2TiO5 stoichiometry around 1100 °C.

Place, publisher, year, edition, pages
Elsevier BV, 2024
Keywords
Atom probe tomography (APT), Ferritic/Martensitic steel, Nano-oxides, ODS steel, Precipitation, Small angle X-ray, scattering (SAXS)
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-353468 (URN)10.1016/j.actamat.2024.120328 (DOI)001388571600001 ()2-s2.0-85202526809 (Scopus ID)
Note

QC 20250122

Available from: 2024-09-19 Created: 2024-09-19 Last updated: 2025-01-22Bibliographically approved
Zhou, T., Spartacus, G., McCluskey, D., Hedström, P. & Eriksson, F. (2024). Streamliningin-situ SAXS/WAXS heat treatment experimentsat the PETRA III Swedish Materials Science beamline. Stockholm: Center for X-Rays in Swedish Materials Science
Open this publication in new window or tab >>Streamliningin-situ SAXS/WAXS heat treatment experimentsat the PETRA III Swedish Materials Science beamline
Show others...
2024 (English)Report (Other academic)
Place, publisher, year, edition, pages
Stockholm: Center for X-Rays in Swedish Materials Science, 2024. p. 23
Series
TRITA-ITM-RP ; 2024:2
Keywords
steels, precipitates, in situ
National Category
Materials Engineering
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-351850 (URN)978-91-8040-904-9 (ISBN)
Funder
Swedish Research Council, 2021-00157
Note

The PETRA III Swedish Materials Science beamline is a high energy X-ray beamline, which was established for research and innovation in materials science and engineering.  This beamline is tailored to particularly suit the research interests of the Swedish community.  

In-situ/-operando measurements are a key opportunity that the Swedish Materials Science beamline offers.  In particular, this beamline’s combined SAXS and WAXS (Small- and Wide-Angle X-ray Scattering) instrument setup provides the possibility to capture quantitative information about materials that comprise of structures that a wide range of length scales. 

This SAXS/WAXS setup has been refined, resulting in an instrument with outstanding capability. The outstanding SAXS/WAXS capability can provide researchers with new insights into heat treatments because phase information and precipitate information can be captured simultaneously - at temporal resolutions down to 1 second.  Thus enabling the kinetics of precipitation and phase transformations to be assessed in detail.  For example, microstructural evolution can be quantitatively tracked. 

This report therefore aims to enabling more Swedish researchers to make the most of the heat treatment research opportunities that the combined SAXS/WAXS instrument setup offers.

Using the heat treatment of austenitic steels that contain precipitates as an example, this report presents a description of how to streamline the research process - from preparing beamtime proposals at your home lab to analysing the beamtime data.  Process descriptions are brought to life using information from the research case, with the case also exemplifying details of each stage of the research process.

This report starts with an introduction to the case as well as the PETRA III Swedish Materials Science beamline, and its combined SAXS/WAXS instrument setup.  The streamlined research process, and its various stages, are presented and exemplified.  In these descriptions, references are provided so that researchers can so further and delve deeper into details.

QC 20240819

Available from: 2024-08-15 Created: 2024-08-15 Last updated: 2024-08-19Bibliographically approved
Bidola, P. M., Abreu-Faria, G., Klingenberg, J., Brehling, J., Burmester, H., Tietze, U., . . . Beckmann, F. (2023). A high-speed X-ray Radiography Setup for in-situ Electron Beam Powder Bed Fusion at PETRA III. In: Advances in X-Ray/EUV Optics and Components XVIII: . Paper presented at Advances in X-Ray/EUV Optics and Components XVIII 2023, San Diego, United States of America, Aug 22 2023. SPIE-Intl Soc Optical Eng, Article ID 1269402.
Open this publication in new window or tab >>A high-speed X-ray Radiography Setup for in-situ Electron Beam Powder Bed Fusion at PETRA III
Show others...
2023 (English)In: Advances in X-Ray/EUV Optics and Components XVIII, SPIE-Intl Soc Optical Eng , 2023, article id 1269402Conference paper, Published paper (Refereed)
Abstract [en]

A high-energy white synchrotron X-ray beam enables penetration of relatively thick and highly absorbing samples. At the P61A White Beam Engineering Materials Science Beamline, operated by Helmholtz-Zentrum Hereon at the PETRA III ring of the Deutsches Elektronen-Synchrotron (DESY), a tailored X-ray radiography system has been developed to perform in-situ X-ray imaging experiments at high temporal resolution, taking advantage of the unprecedented X-ray beam flux delivered by ten successive damping wigglers. The imaging system is equipped with an ultrahigh-speed camera (Phantom v2640) enabling acquisition rates up to 25 kHz at maximal resolution and binned mode. The camera is coupled with optical magnification (5x, 10x) and focusing lenses to enable imaging with a pixel size of 1,35 micrometre. The scintillator screens are housed in a special nitrogen gas cooling environment to withstand the heat load induced by the beam, allowing spatial resolution to be optimized down to few micrometres. We present the current state of the system development, implementation and first results of in situ investigations, especially of the electron beam powder bed fusion (PBF-EB) process, where the details of the mechanism of crack and pore formation during processing of different powder materials, e.g. steels and Ni-based alloys, is not yet known.

Place, publisher, year, edition, pages
SPIE-Intl Soc Optical Eng, 2023
Keywords
Electron beam Powder Bed Fusion, High-speed X-ray radiography, In-situ X-ray imaging
National Category
Atom and Molecular Physics and Optics
Identifiers
urn:nbn:se:kth:diva-339975 (URN)10.1117/12.2678913 (DOI)2-s2.0-85176588853 (Scopus ID)
Conference
Advances in X-Ray/EUV Optics and Components XVIII 2023, San Diego, United States of America, Aug 22 2023
Note

Part of ISBN 9781510666023

QC 20231127

Available from: 2023-11-27 Created: 2023-11-27 Last updated: 2023-11-27Bibliographically approved
Zhou, T., Spartacus, G., Dahlström, A., Babu, P., Davydok, A. & Hedström, P. (2023). Computational thermodynamics and kinetics-guided re-engineering of a high-performance tool steel. Scripta Materialia, 232, Article ID 115496.
Open this publication in new window or tab >>Computational thermodynamics and kinetics-guided re-engineering of a high-performance tool steel
Show others...
2023 (English)In: Scripta Materialia, ISSN 1359-6462, E-ISSN 1872-8456, Vol. 232, article id 115496Article in journal (Refereed) Published
Abstract [en]

Targeting to obtain fine dispersions of nanoscale precipitates to enhance the mechanical properties of a highperformance tool steel, re-engineering of the alloy composition and heat treatment was guided by computational thermodynamics and kinetics. A prototype alloy was prepared using the designed chemistry and heat treatment. Thereafter, advanced microstructural characterization and mechanical testing confirmed the successful design to reach a high number density of (V, Mo)C precipitates with an average diameter of about 5 nm in the peak-hardened condition, after tempering the martensite at 600 degrees C for 2 h.

Place, publisher, year, edition, pages
Elsevier BV, 2023
Keywords
Alloy development, Computational thermodynamics, Precipitation kinetics, Advanced characterization, Tool steels
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-328315 (URN)10.1016/j.scriptamat.2023.115496 (DOI)000987838100001 ()2-s2.0-85152604140 (Scopus ID)
Note

QC 20230607

Available from: 2023-06-07 Created: 2023-06-07 Last updated: 2023-12-07Bibliographically approved
König, H.-H., Semjatov, N., Spartacus, G., Bidola, P., Ioannidou, C., Ye, J., . . . Lindwall, G. (2023). MiniMelt: An instrument for real-time tracking of electron beam additive manufacturing using synchrotron x-ray techniques. Review of Scientific Instruments, 94(12), Article ID 125103.
Open this publication in new window or tab >>MiniMelt: An instrument for real-time tracking of electron beam additive manufacturing using synchrotron x-ray techniques
Show others...
2023 (English)In: Review of Scientific Instruments, ISSN 0034-6748, E-ISSN 1089-7623, Vol. 94, no 12, article id 125103Article in journal (Refereed) Published
Abstract [en]

The development of a sample environment for in situ x-ray characterization during metal Electron Beam Powder Bed Fusion (PBF-EB), called MiniMelt, is presented. The design considerations, the features of the equipment, and its implementation at the synchrotron facility PETRA III at Deutsches Elektronen-Synchrotron, Hamburg, Germany, are described. The equipment is based on the commercially available Freemelt ONE PBF-EB system but has been customized with a unique process chamber to enable real-time synchrotron measurements during the additive manufacturing process. Furthermore, a new unconfined powder bed design to replicate the conditions of the full-scale PBF-EB process is introduced. The first radiography (15 kHz) and diffraction (1 kHz) measurements of PBF-EB with a hot-work tool steel and a Ni-base superalloy, as well as bulk metal melting with the CMSX-4 alloy, using the sample environment are presented. MiniMelt enables time-resolved investigations of the dynamic phenomena taking place during multi-layer PBF-EB, facilitating process understanding and development of advanced process strategies and materials for PBF-EB.<br />

Place, publisher, year, edition, pages
AIP Publishing, 2023
National Category
Production Engineering, Human Work Science and Ergonomics
Identifiers
urn:nbn:se:kth:diva-342336 (URN)10.1063/5.0177255 (DOI)001118876200001 ()38059765 (PubMedID)2-s2.0-85179024070 (Scopus ID)
Note

QC 20240116

Available from: 2024-01-16 Created: 2024-01-16 Last updated: 2024-01-16Bibliographically approved
Spartacus, G., Hedström, P., McCluskey, D., Zhou, T. & Eriksson, F. (2023). Overview of sample enironments for research use at the PETRA III Swedish Materials Science beamline. Stockholm
Open this publication in new window or tab >>Overview of sample enironments for research use at the PETRA III Swedish Materials Science beamline
Show others...
2023 (English)Report (Other (popular science, discussion, etc.))
Abstract [en]

This technical report presents an overview of sample environments which are usable at the PETRA III Swedish Materials Science beamline (potentially requiring arrangement or development of the beamline layout). Alongside the description of each sample environment, illustrative materials science studies are presented that exemplify the use of these sample environments for in situ and/or in operando measurements.  The sample environments are catalogued according to the research application areas, which are categorised as Thermal treatments, Electrochemistry, Catalysis, Thin films, Mechanical response of materials and Levitation. Such cataloguing means that researchers can now start their search for relevant sample environments by looking up a relevant research application area. Citations and links to specifications, published research cases and the organisation that is responsible for a given sample environment, are also provided as a basis for researchers to proceed with their research planning.

Place, publisher, year, edition, pages
Stockholm: , 2023. p. 28
Series
TRITA-ITM-RP ; 2022:3
Keywords
Sample environments, synchrotrons, PETRA III, Swedish beamline
National Category
Materials Engineering
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-323697 (URN)978-91-8040-448-8 (ISBN)
Funder
Swedish Research Council, 4.3-2018-06942
Note

QC 20230328

Available from: 2023-02-09 Created: 2023-02-09 Last updated: 2023-12-07Bibliographically approved
Spartacus, G., Malaplate, J., De Geuser, F., Mouton, I., Sornin, D., Perez, M., . . . Deschamps, A. (2022). Chemical and structural evolution of nano-oxides from mechanical alloying to consolidated ferritic oxide dispersion strengthened steel. Acta Materialia, 233, 117992, Article ID 117992.
Open this publication in new window or tab >>Chemical and structural evolution of nano-oxides from mechanical alloying to consolidated ferritic oxide dispersion strengthened steel
Show others...
2022 (English)In: Acta Materialia, ISSN 1359-6454, E-ISSN 1873-2453, Vol. 233, p. 117992-, article id 117992Article in journal (Refereed) Published
Abstract [en]

Ferritic Oxides Dispersion Strengthened (ODS) steels are of great interest for nuclear fission and fusion power plants. The nano-oxides embedded into the matrix provide the main contribution to the ODS steel strength. Understanding of the precipitation mechanism of ODS steels is thus critical for optimizing the fabrication process, involving Mechanical Alloying (MA) of Fe-14Cr, Y2O3 and TiH2 powders. In this study, results from small-angle X-ray and neutron scattering, atom probe tomography and electron microscopy have been combined to investigate the nano-oxides evolution throughout the whole consolidation thermal treatment until 1100 degrees C. After MA clusters are observed, composed of Y, O and Ti. During heating these clusters grow and new ones nucleate, together with a sequential enrichment in Ti (from as-MA to 700 degrees C) and Y (between 900 and 1100 degrees C). A small quantity of Al is also found in the nano-oxides between 70 0 and 110 0 degrees C. At 1100 degrees C the nano-oxides are found to be mainly Y2Ti2O7 and subsequently progressively transform to Y2TiO5 during isothermal holding. Nano-oxides display however an unchanged extremely low coarsening rate, demonstrating the outstanding stability of both Y2Ti2O7 and Y2TiO5 at 1100 degrees C.

Place, publisher, year, edition, pages
Elsevier BV, 2022
National Category
Metallurgy and Metallic Materials
Identifiers
urn:nbn:se:kth:diva-315232 (URN)10.1016/j.actamat.2022.117992 (DOI)000805863400001 ()2-s2.0-85129701245 (Scopus ID)
Note

QC 20220701

Available from: 2022-07-01 Created: 2022-07-01 Last updated: 2022-07-07Bibliographically approved
Zhou, T., McCluskey, D., Hedström, P., Spartacus, G. & Eriksson, F. (2022). Inventory of data reduction and analysis software used in high-energy X-ray research at PETRA III: WAXS, SAXS, GIWAXS, GISAXS, PDF.
Open this publication in new window or tab >>Inventory of data reduction and analysis software used in high-energy X-ray research at PETRA III: WAXS, SAXS, GIWAXS, GISAXS, PDF
Show others...
2022 (English)Report (Other (popular science, discussion, etc.))
Abstract [en]

This inventory catalogs the software programs that have proven to be useful to the Swedish research community that conducts research at the PETRA III synchrotron, including the PETRA III Swedish Materials Science beamline.

Based on publications from 2018, the inventory categorizes the various software programs used in research as either data reduction software for 2D area detector X-ray scattering images or data analysis software for WAXS, SAXS, GIWAXS, GISAXS, and PDF.

Each software program has a short description of its functionality, a note of its developer, links to the original publication describing the scientific method that the software is based upon, as well as the site for downloading the software program. 

Publisher
p. 17
Series
TRITA-ITM-RP ; 2020:2
Keywords
X-rays, synchrotrons, data reduction software, data analysis software, PETRA III, Swedish beamline
National Category
Physical Sciences
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-316635 (URN)978-91-8040-319-1 (ISBN)
Projects
Center for X-rays in Swedish Materials Science
Funder
Swedish Research Council, 4.3-2018-06942
Note

QC 20220902

Available from: 2022-08-25 Created: 2022-08-25 Last updated: 2023-12-07Bibliographically approved
Organisations
Identifiers
ORCID iD: ORCID iD iconorcid.org/0000-0001-7096-1200

Search in DiVA

Show all publications