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Microstructure and Mechanical Properties of Plasma Atomized Refractory Alloys
Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science. Höganäs Sweden AB.ORCID iD: 0009-0005-4360-3375
2023 (English)Licentiate thesis, comprehensive summary (Other academic)Alternative title
Mikrostruktur och mekaniska egenskaper hos plasma-atomiserade svårsmälta legeringar (Swedish)
Abstract [en]

Plasma centrifugal atomization is a method widely used in the production of spherical powders of metals and alloys with relatively low melting points. A novel plasma centrifugal atomization process suitable for high melting point materials (i.e. 3500 ᵒC and above) was developed by Metasphere Technology AB, currently Höganäs Sweden AB. In this process, feedstock material in the form of crushed powder with particle sizes in the range 400-1000 µm is fed into a rotating crucible and subsequently melted by the glow discharge of a plasmatron. Due to high rotational speeds, a melt film forms at the edge of the crucible and breaks into fine droplets that are ejected into the reactor chamber and solidified in a whirl of cold inert gases. Capability of the plasmatron to reach very high temperatures, combined with extremely rapid cooling of the ejected droplets, allow for the fabrication of fine powders of refractory alloys exhibiting metastable phases that cannot be obtained otherwise. 

Oil drilling, ore processing and metal shaping applications, among other, require tool materials capable of withstanding harsh working conditions under heavy loads. Owing to their physical, chemical and mechanical properties, tungsten-carbon alloys are among the most suited materials for such applications. Melting followed by rapid solidification of tungsten-carbon mixtures with 3.9 wt.% C results in a biphasic structure composed of WC lamellae inserted in a W2C matrix, known as cast tungsten carbide (CTC). Due to the metastable nature of both phases present, CTC exhibits exceptional mechanical properties. CTC is mainly used as reinforcing dispersed phase in metal matrix composite hardfacing overlays, which are deposited by plasma transferred arc (PTA) welding or laser cladding onto steel tools.

High-entropy alloys (HEAs) are defined as multi-component solid solutions with equimolar or near-equimolar concentration of all principal elements. Owing to their outstanding mechanical, corrosion, erosion, oxidation and radiation resistance properties compared to conventional alloys, HEAs are among the most suited materials for aerospace and nuclear applications. Several processing routes have allowed for laboratory-scale production of HEAs. Nevertheless, size and shape of bulk components that can be thus produced are largely limited. In a quest for up-scaling the processing of high-end bulk HEA components, plasma centrifugal atomization of pre-alloyed refractory HEA spherical powders suitable for additive manufacturing was envisaged.

In this work, capabilities of the novel plasma centrifugal atomization for processing of refractory alloys into fine spherical powders have been evaluated based on two different material systems, namely CTC and a refractory HEA containing Ti, V, Zr, Nb, Mo, Hf, Ta, W. Challenges of local mechanical characterization of micron-sized powders have been addressed and a robust method for testing of individual particles has been developed. Mechanical properties such as hardness and fracture toughness of plasma atomized CTC powders have been extensively investigated and related to the corresponding thermal stories. Experimental results suggest significant straining of the crystal lattice in the case of as-atomized CTC, possibly due to extremely high cooling rates experienced by the solidifying particles. This has been ruled out the main reason for the outstanding mechanical properties of plasma atomized CTC compared to both spheroidized CTC and conventional cast & crushed CTC. Effective stress relieve was possible upon heat treatment. Plasma atomization of the refractory HEA yielded similar results, where an extremely fine microstructure with no noticeable chemical segregation was obtained. Indentation hardness of this novel microstructure was found to be approximately 25% higher than that of similar alloys reported in literature. HEA powder thus produced was then consolidated into bulk HEAs with very simple geometries, proving that this powder can be further processed into components of more or less complexity for pre-defined applications.

Place, publisher, year, edition, pages
Luleå: Luleå University of Technology, 2023.
Series
Licentiate thesis / Luleå University of Technology, ISSN 1402-1757
Keywords [en]
plasma atomization, spherical powder, tungsten carbide, high entropy alloy, refractory
National Category
Other Materials Engineering
Research subject
Engineering Materials
Identifiers
URN: urn:nbn:se:ltu:diva-96278ISBN: 978-91-8048-291-2 (print)ISBN: 978-91-8048-292-9 (electronic)OAI: oai:DiVA.org:ltu-96278DiVA, id: diva2:1747752
Presentation
2023-05-25, E632, Luleå tekniska universitet, Luleå, 09:00 (English)
Opponent
Supervisors
Available from: 2023-03-31 Created: 2023-03-30 Last updated: 2025-10-21Bibliographically approved
List of papers
1. Use of AFM topography images to determine microindentation hardness of cast tungsten carbide powders
Open this publication in new window or tab >>Use of AFM topography images to determine microindentation hardness of cast tungsten carbide powders
2022 (English)In: International journal of refractory metals & hard materials, ISSN 0263-4368, Vol. 107, article id 105878Article in journal (Refereed) Published
Abstract [en]

Hardness is defined as the resistance of a material to localized plastic deformation. Owing to their non-destructive nature, static indentation hardness tests are widely used in industry. Hardness testing is particularly useful for the mechanical characterization of materials that cannot be tested otherwise, e.g. powdered materials. In this study, challenges related to Vickers microindentation hardness testing of hard brittle cast tungsten carbide (CTC) powders were extensively investigated. Test load was optimized to obtain sufficiently large crack-free indentations allowing for precise measurement of the diagonal lengths. The influence of the operator and imaging technique on the measured hardness value was evaluated. Topography of residual imprints was investigated using atomic force microscopy (AFM) and a systematic and operator bias-free method to locate the indentation vertexes was developed. Results suggested that measurement variability introduced by AFM scanning and post-processing was as low as 3.1% and 1.3% with respect to the mean hardness value, respectively. Since the variability due to the measuring system can be isolated, the homogeneity of powders can be reliably evaluated from the hardness measurements thus obtained.

Place, publisher, year, edition, pages
Elsevier, 2022
Keywords
Microindentation, Hardness, Vickers, Atomic force microscopy, Image analysis, Cast tungsten carbide
National Category
Metallurgy and Metallic Materials
Research subject
Engineering Materials
Identifiers
urn:nbn:se:ltu:diva-90623 (URN)10.1016/j.ijrmhm.2022.105878 (DOI)000806791500005 ()2-s2.0-85130573927 (Scopus ID)
Funder
The Kempe Foundations, SMK-2546
Note

Validerad;2022;Nivå 2;2022-06-08 (sofila);

Funder:  Swedish Foundation for Strategic Research (ID19-0071)

Available from: 2022-05-12 Created: 2022-05-12 Last updated: 2025-10-21Bibliographically approved
2. Effect of residual stresses on the hardness, toughness and fatigue behavior of cast tungsten carbide powders
Open this publication in new window or tab >>Effect of residual stresses on the hardness, toughness and fatigue behavior of cast tungsten carbide powders
(English)Manuscript (preprint) (Other academic)
National Category
Other Materials Engineering
Research subject
Engineering Materials
Identifiers
urn:nbn:se:ltu:diva-96276 (URN)
Funder
Swedish Foundation for Strategic Research, ID19-0071
Available from: 2023-03-30 Created: 2023-03-30 Last updated: 2025-10-21
3. Plasma centrifugal atomization of Ti-V-Zr-Nb-Mo-Hf-Ta-W high entropy alloy powder: microstructural and mechanical characterization
Open this publication in new window or tab >>Plasma centrifugal atomization of Ti-V-Zr-Nb-Mo-Hf-Ta-W high entropy alloy powder: microstructural and mechanical characterization
(English)Manuscript (preprint) (Other academic)
National Category
Other Materials Engineering
Research subject
Engineering Materials
Identifiers
urn:nbn:se:ltu:diva-96277 (URN)
Funder
Swedish Foundation for Strategic Research, ID19-0071
Available from: 2023-03-30 Created: 2023-03-30 Last updated: 2025-10-21

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Ciurans Oset, Marina

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