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Sub-grain structure in additive manufactured stainless steel 316L
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
2017 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The thesis focuses on exploring the sub-grain structure in stainless steel 316L prepared by additive manufacturing (AM). Two powder-bed based AM methods are involved: selective laser melting (SLM) and electron beam melting (EBM). It is already known that AM 316L has heterogeneous property and hierarchy structure: micro-sized melt pools, micro-sized grains, nano-sized sub-grain structure and nano-sized inclusions. Yet, the relation among these structures and their influence on mechanical properties have not been clearly revealed so far. Melt pool boundaries having lower amount of sub-grain segregated network structures (Cellular structure) are weaker compared to the base material. Compared with cell boundaries, grain boundaries have less influence on strength but are still important for ductility. Cell boundaries strengthen the material without losing ductility as revealed by mechanical tests. Cellular structure can be continuous across the melt pool boundaries, low angle sub-grain boundaries, but not grain boundaries. Based on the above understanding, AM process parameters were adjusted to achieve customized mechanical properties. Comprehensive characterization were carried out to investigate the density, composition, microstructure, phase, magnetic permeability, tensile property, Charpy impact property, and fatigue property of both SLM and EBM SS316L at room temperature and at elevated temperatures (250°C and 400°C). In general, SLM SS316L has better strength while EBM SS316L has better ductility due to the different process conditions. Improved cell connection between melt pools were achieved by rotating 45° scanning direction between each layer compared to rotating 90°. Superior mechanical properties (yield strength 552 MPa and elongation 83%) were achieved in SLM SS316L fabricated with 20 µm layer thickness and tested in the building direction. Y2O3 added oxide dispersed strengthening steel (ODSS) were also prepared by SLM to further improve its performance at elevated temperatures. Slightly improved strength and ductility (yield strength 574 MPa and elongation 90%) were obtained on 0.3%Y2O3-ODSS with evenly dispersed nanoparticles (20 nm). The strength drops slightly  but ductility drops dramatically at elevated temperatures. Fractographic analysis results revealed that the coalescence of nano-voids is hindered at room temperature but not at elevated temperatures. The achieved promising properties in large AM specimens assure its potential application in nuclear fusion. For the first time, ITER first wall panel parts with complex inner pipe structure were successfully fabricated by both SLM and EBM which gives great confidence to application of AM in nuclear industry. 

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry, Stockholm University , 2017. , p. 66
Keywords [en]
Additive manufacturing, Selective laser melting, Electron beam melting, stainless steel, Oxide dispersion strengthened steel, Cellular structure, Nano-inclusions
National Category
Materials Chemistry Metallurgy and Metallic Materials
Research subject
Materials Chemistry
Identifiers
URN: urn:nbn:se:su:diva-144519ISBN: 978-91-7649-907-8 (print)ISBN: 978-91-7649-908-5 (electronic)OAI: oai:DiVA.org:su-144519DiVA, id: diva2:1114451
Public defence
2017-09-08, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 4: Manuscript. Paper 5: Manuscript.

Available from: 2017-08-16 Created: 2017-06-23 Last updated: 2022-02-28Bibliographically approved
List of papers
1. Additive manufacturing of 316L stainless steel by electron beam melting for nuclear fusion applications
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2017 (English)In: Journal of Nuclear Materials, ISSN 0022-3115, E-ISSN 1873-4820, Vol. 486, p. 234-245Article in journal (Refereed) Published
Abstract [en]

A feasibility study was performed to fabricate ITER In-Vessel components by one of the metal additivemanufacturing methods, Electron Beam Melting®(EBM®). Solid specimens of SS316L with 99.8% relativedensity were prepared from gas atomized precursor powder granules. After the EBM®process the phaseremains as austenite and the composition has practically not been changed. The RCC-MR code used fornuclear pressure vessels provides guidelines for this study and tensile tests and Charpy-V tests werecarried out at 22C (RT) and 250C (ET). This work provides thefirst set of mechanical and micro-structure data of EBM®SS316L for nuclear fusion applications. The mechanical testing shows that theyield strength, ductility and toughness are well above the acceptance criteria and only the ultimatetensile strength of EBM®SS316L is below the RCC-MR code. Microstructure characterizations reveal thepresence of hierarchical structures consisting of solidified melt pools, columnar grains and irregularshaped sub-grains. Lots of precipitates enriched in Cr and Mo are observed at columnar grain boundarieswhile no sign of element segregation is shown at the sub-grain boundaries. Such a unique microstructureforms during a non-equilibrium process, comprising rapid solidification and a gradient‘annealing’process due to anisotropic thermalflow of accumulated heat inside the powder granule matrix. Relationsbetween process parameters, specimen geometry (total building time) and sub-grain structure are dis-cussed. Defects are formed mainly due to the large layer thickness (100mmÞwhich generates insufficientbonding between a few of the adjacently formed melt pools during the process. Further studies shouldfocus on adjusting layer thickness to improve the strength of EBM®SS316L and optimizing total buildingtime.

Keywords
Electron beam melting, Additive manufacturing, 316L stainless steel, Nuclear fusion, Microstructure, Mechanical properties
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-141056 (URN)10.1016/j.jnucmat.2016.12.042 (DOI)000397373600027 ()
Available from: 2017-03-29 Created: 2017-03-29 Last updated: 2022-02-28Bibliographically approved
2. Additive manufacturing of ITER first wall panel parts by two approaches: Selective laser melting and electron beam melting
Open this publication in new window or tab >>Additive manufacturing of ITER first wall panel parts by two approaches: Selective laser melting and electron beam melting
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2017 (English)In: Fusion engineering and design, ISSN 0920-3796, E-ISSN 1873-7196, Vol. 116, p. 24-33Article in journal (Refereed) Published
Abstract [en]

Fabrication of ITER First Wall (FW) Panel parts by two additive manufacturing (AM) technologies, selective laser melting (SEM) and electron beam melting (EBM), was supported by Fusion for Energy (F4E). For the first time, AM is applied to manufacture ITER In-Vessel parts with complex design. Fully dense SS316L was prepared by both SLM and EBM after developing optimized laser/electron beam parameters. Characterizations on the density, magnetic permeability, microstructure, defects and inclusions were carried out. Tensile properties, Charpy-impact properties and fatigue properties of SLM and EBM SS316L were also compared. ITER FW Panel parts were successfully fabricated by both SLM and EBM in a onestep building process. The SLM part has smoother surface, better size accuracy while the EBM part takes much less time to build. Issues with removing support structures might be solved by slightly changing the design of the internal cooling system. Further investigation of the influence of neutron irradiation on materials properties between the two AM technologies is needed.

Keywords
ITER, First wall, Additive manufacturing, 316L stainless steel, Selective laser melting, Electron beam melting
National Category
Manufacturing, Surface and Joining Technology Metallurgy and Metallic Materials
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-141057 (URN)10.1016/j.fusengdes.2017.01.032 (DOI)000396956500005 ()
Available from: 2017-03-29 Created: 2017-03-29 Last updated: 2022-02-28Bibliographically approved
3. Intragranular cellular segregation network structure strengthening 316L stainless steel prepared by selective laser melting
Open this publication in new window or tab >>Intragranular cellular segregation network structure strengthening 316L stainless steel prepared by selective laser melting
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2016 (English)In: Journal of Nuclear Materials, ISSN 0022-3115, E-ISSN 1873-4820, Vol. 470, p. 170-178Article in journal (Refereed) Published
Abstract [en]

A feasibility study was performed to fabricate ITER In-Vessel components by Selective Laser Melting (SLM) supported by Fusion for Energy (F4E). Almost fully dense 316L stainless steel (SS316L) components were prepared from gas-atomized powder and with optimized SLM processing parameters. Tensile tests and Charpy-V tests were carried out at 22 degrees C and 250 degrees C and the results showed that SLM SS316L fulfill the RCC-MR code. Microstructure characterization reveals the presence of hierarchical macro-, micro- and nano-structures in as-built samples that were very different from SS316L microstructures prepared by other established methods. The formation of a characteristic intragranular cellular segregation network microstructure appears to contribute to the increase of yield strength without losing ductility. Silicon oxide nano-inclusions were formed during the SLM process that generated a micro-hardness fluctuation in the building direction. The combined influence of a cellular microstructure and the nano-inclusions constraints the size of ductile dimples to nano-scale. The crack propagation is hindered by a pinning effect that improves the defect-tolerance of the SLM SS316L. This work proves that it was possible to manufacture SS316L with properties suitable for ITER First Wall panels. Further studies on irradiation properties of SLM SS316L and manufacturing of larger real-size components are needed.

Keywords
ITER, Selective laser melting, 316L stainless steel, Mechanical property, Intragranular cellular structure
National Category
Materials Engineering Environmental Engineering Chemical Sciences
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-128166 (URN)10.1016/j.jnucmat.2015.12.034 (DOI)000370379100020 ()
Available from: 2016-03-29 Created: 2016-03-21 Last updated: 2022-02-23Bibliographically approved
4. Manipulating the sub-grain cellular network structure during selective laser melting
Open this publication in new window or tab >>Manipulating the sub-grain cellular network structure during selective laser melting
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(English)Manuscript (preprint) (Other academic)
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-144515 (URN)
Available from: 2017-06-22 Created: 2017-06-22 Last updated: 2022-02-28Bibliographically approved
5. Oxide dispersion strengthened austenitic steel prepared by selective laser melting with superior strength and ductility
Open this publication in new window or tab >>Oxide dispersion strengthened austenitic steel prepared by selective laser melting with superior strength and ductility
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(English)Manuscript (preprint) (Other academic)
National Category
Metallurgy and Metallic Materials
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-144517 (URN)
Available from: 2017-06-22 Created: 2017-06-22 Last updated: 2022-02-28Bibliographically approved

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