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On the Origin and Distributions of the Inclusions in Production-scale ESR and PESR Remelted Ingots and Materials from Different Ingot Sizes and Solidification Structures
KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering. Uddeholms AB ewa.persson@uddeholm.com.ORCID iD: 0000-0001-6019-0676
2021 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The study was carried out with the aim to evaluate the origin, morphology, and distribution of the non-metallic inclusions (NMI) in electro-slag remelted (ESR) steels and in electro-slag remelted steels using a pressured controlled inert atmosphere (PESR). In addition to the NMI studies, the solidification structure in different ingot sizes were studied in order to define the influence of the solidification on the NMI characteristics. The steel grade chosen for the studies was a common martensitic stainless steel. The focus is on the origin and the distribution of oxide inclusions with the assumption that sulfides and nitrides are secondary inclusions in remelted material.

In order to get a good statistical basis, a large number of SEM samples from different axial positions were taken from both an electrode and several ESR and PESR remelted ingots as well as processed (rolling/forging) materials. The inclusions were investigated by using both two-dimensional (2-D) and three-dimensional (3-D) methods. Especially for steels with a higher cleanliness, as for example remelted steels, a large analyzed area is important in order to get a true picture of the inclusion morphology. As an attempt to localize the origin of the inclusions, a pilot trial using a La2O3 as a tracer in the ESR process slag was performed. To study the influence of the solidification structure on the inclusions, horizontal slice/slices were cut from different positions from the electrode as well as from ESR and PESR remelted ingots of different sizes. Beside inclusions and chemical composition determinations across the diameter of the slices, also the second dendrite arm spacing (SDAS) and the angles of the dendrites towards the axial plane were measured.

The result gave rise to a new classification of the inclusions present in ESR or PESR remelted steels, i) Primary Inclusions. They survive from the electrode because they were trapped inside a steel drop or a fallen steel fragment, without having contact with the ESR/PESR process slag. The size depends on the size of the inclusions in the electrode and the size of the steel droplets.  ii) Semi-Secondary Inclusions, primary Al-Mg oxides covered by process slag. Normal size class is ≈ < 30 µm. iii) Secondary Inclusions, precipitated during solidification of the liquid steel as a result of the reactions between alloying elements and the dissolved oxygen. Normal size class is < 10 µm.

The structure study showed that the transition from a columnar-dendritic to an equiaxial structure (CET) in the center of the ingot have a strong effect on the number and size of the inclusions. As long as the center of the ingot solidifies in a columnar-dendritic manner, the increase of the inclusion number and size is almost linear with an increasing ingot size. However, after the CET transition in the center, the inclusion number and sizes are much larger. For this steel grade, the transition from a columnar-dendritic to an equiaxial is between the 800 mm in diameter (PESR-800) ingot and the 1050 mm in diameter (PESR-1050) ingot. The primary arms growth rate needed for the CET transition is less than 4 x 10-7m/s. In order to undertake the transition, the temperature gradient must be less than approximately 103 °C/m.

On the whole, the results illustrated that the overall cleanliness of the electrode (as well as the composition of the inclusions in the electrode) has an extremely large influence on the cleanliness in ESR and PESR remelted steels. The majority of the failure critical inclusions originates direct or indirect from the inclusions in the electrode. Moreover, the solidification structure (ingot size) also has a direct bearing on the inclusion sizes and contents present in ESR and PESR ingots.

 

Abstract [sv]

Detta arbete är utfört  med målet att fastställa källan, morfologin och distributionen av icke-metalliska inneslutningar (NMI) i elektroslaggomsmälta (ESR) stål och i stål elektroomsmälta under en kontrollerad inert atmosfär (PESR). Utöver inneslutningsstudierna har även stelningsstrukturen i olika götstorlekar undersökts. Detta i syfte att definiera strukturens påverkan på de icke-metalliska inneslutningarna. Den valda stålsorten är ett vanligt martensitiskt rostfritt stål. Fokus av arbetet är källan och distributionen av de oxidiska inneslutningar, med ett antagande att sulfider och nitrider är sekundära inneslutningar i omsmält material.

I syfte att få ett bra statistiskt underlag är ett stort antal SEM-prover från både olika vertikala götpositioner uttagna från en elektrod, flera ESR- och PESR-göt samt från bearbetat material (smide, valsning). Inneslutningarna är studerade både med två-dimensionella (2-D) och tre-dimensionella (3-D) metoder. Det är extra viktigt för stål med en högre renhet, som till exempel omsmälta stål, att analysera många och stora ytor för att få en sann bild av inneslutningsmorfologin. I ett försök att lokalisera källan för de oxidiska inneslutningarna är pilot-försök med ett spårämne i processlaggen genomförda. I syfte att studera strukturens inverkan på inneslutningarna är horisontella skivor kapade från flera götstorlekar. Förutom inneslutningarna och den kemiska analysen tvärs skivorna studerades även det sekundära dendritsarmsavståndet (SDAS) och dendriternas vinkel mot det horisontella planet.

Resultatet är en ny klassificering av inneslutningarna i ESR- och PESR-omsmälta stål, i) Primära Inneslutningar,  överlever från elektroden utan kontakt med ESR/PESR:s processlagg, fångade i en fallande ståldroppe eller stålfragment. Deras storlek beror av storleken på inneslutningarna I elektroden samt de fallande ståldropparnas storlek. ii) Semi-Sekundära Inneslutningar, Främst Al-Mg oxider täckta med processlagg. Normal storleksklass är ≈ < 30 µm. iii) Sekundära Inneslutningar, utskilda under stelningen av det flytande stålet som ett resultat av en reaktion mellan legeringselement och löst syre.  Normal storleksklass är < 10 µm. 

Strukturstudien visade att en övergång från riktad dendritisk struktur till enaxlig struktur har en stor påverkan på antalet och storleken av inneslutningarna. Så länge som centrum I ett göt stelnar med en riktad dendritisk struktur är ökningen av antalet inneslutningar linjärt med ökad götstorlek.  Efter övergången till enaxlig struktur i centrum är dock inneslutningarna både större och fler.  För denna stålsort inträffar övergången från riktad dendritisk struktur till enaxlig struktur någonstans mellan en PESR-götdiameter på 800 och 1050 mm. Tillväxthastigheten som behövs av de primära dendritarmarna för att övergången skall ske är under 4 x 10-7m/s. Dessutom krävs en temperaturgradient som är lägre än cirka 103 °C/m.

Sammantaget visar resultatet att både mängden av inneslutningar I elektroden (tillika dess storlek och komposition) är extremt viktig för renheten i ESR-och PESR-omsmälta stål. Majoriteten av de i kritiska inneslutningarna härstammar direkt eller indirekt från inneslutningarna i elektroden. Utöver det är även stelningsstrukturen (götstorleken)  direkt avgörande för inneslutningarnas storlek och antal i ESR- och PESR-omsmälta material.

 

Place, publisher, year, edition, pages
Stockholm, Sweden: Kungliga Tekniska högskolan, 2021. , p. 81
Series
TRITA-ITM-AVL ; 2021:14
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
URN: urn:nbn:se:kth:diva-294069ISBN: 978-91-7873-837-3 (print)OAI: oai:DiVA.org:kth-294069DiVA, id: diva2:1552940
Public defence
2021-05-28, https://kth-se.zoom.us/j/65503064721, Stockholm, 14:00 (English)
Opponent
Supervisors
Available from: 2021-05-07 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
List of papers
1. Origin of the Inclusions in Production-Scale Electrodes, ESR Ingots, and PESR Ingots in a Martensitic Stainless Steel
Open this publication in new window or tab >>Origin of the Inclusions in Production-Scale Electrodes, ESR Ingots, and PESR Ingots in a Martensitic Stainless Steel
2020 (English)In: Metals, ISSN 2075-4701, Vol. 10, no 12, article id 1620Article in journal (Refereed) Published
Abstract [en]

The focus of the study was to define the origin of the inclusions in production-scale electro-slag remelting, (ESR) and electro-slag remelting under a protected pressure controlled atmosphere, (PESR), ingots. The inclusion characteristics in production samples were studied using both polished sample surfaces (two-dimensional (2-D) investigations) and inclusions extracted from steel samples by electrolytic extraction (three-dimensional (3-D) investigations) using SEM in combination with EDS. The results were compared to results from previously reported laboratory-, pilot-, and production-scale trials including electrode, remelted, and conventional ingots. The results show that primary, semi-secondary, and secondary inclusions exist in the remelted ingots. The most probable inclusion to survive from the electrode is a MgO-Al2O3 (spinel). It was also found that the ESR/PESR process slag acts in a similar way to a calcium treatment modification of alumina inclusions. On the whole, the most significant finding is that the overall cleanliness of the electrode including the inclusions in the electrode has an influence on the inclusion content of the ESR and PESR ingots.

Place, publisher, year, edition, pages
MDPI AG, 2020
Keywords
ESR, PESR, inclusions, electrolytic extraction, SEM, stainless steel
National Category
Materials Engineering
Identifiers
urn:nbn:se:kth:diva-289279 (URN)10.3390/met10121620 (DOI)000602500400001 ()2-s2.0-85097161306 (Scopus ID)
Note

QC 20210127

Available from: 2021-01-27 Created: 2021-01-27 Last updated: 2023-03-06Bibliographically approved
2. Differences in inclusion morphology between ESR remelted steel with and without tracer in the process slag
Open this publication in new window or tab >>Differences in inclusion morphology between ESR remelted steel with and without tracer in the process slag
2017 (English)In: Differences in inclusion morphology between ESR remelted steel with and without tracer in the process slag / [ed] Stuart Rudoler, American Flux and Metal, USA, TMS, USA, 2017Conference paper, Published paper (Refereed)
Place, publisher, year, edition, pages
TMS, USA: , 2017
Keywords
ESR, Inclusions, Process slag, Trace elements
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-293981 (URN)
Conference
LMPC 2017, Liquid Metal Processing & Casting Conference,  TMS, USA, Philadelphia, USA, 10-13 September 2017.
Note

QC 20210506

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
3. Impact of solidification on inclusion morphology in ESR and PESR remelted martensitic stainless steel ingots
Open this publication in new window or tab >>Impact of solidification on inclusion morphology in ESR and PESR remelted martensitic stainless steel ingots
2021 (English)In: Metals, ISSN 2075-4701, Vol. 11, no 3, p. 408-424Article in journal (Refereed) Published
Abstract [en]

This study focuses on the impact of solidification on the inclusion morphologies in different sizes of production-scale electro-slag remelting (ESR) and electro-slag remelting under a protected pressure-controlled atmosphere, (PESR), ingots, in a common martensitic stainless steel grade. The investigation has been carried out to increase the knowledge of the solidification and change in inclusion morphologies during ESR and PESR remelting. In order to optimize process routes for different steel grades, it is important to define the advantages of different processes. A comparison is made between an electrode, ESR, and PESR ingots with different production-scale ingot sizes, from 400 mm square to 1050 mm in diameter. The electrode and two of the smallest ingots are from the same electrode charge. The samples are taken from both the electrode, ingots, and rolled/forged material. The solidification structure, dendrite arm spacing, chemical analyzes, and inclusion number on ingots and/or forged/rolled material are studied. The results show that the larger the ingot and the further towards the center of the ingot, the larger inclusions are found. As long as an ingot solidifies with a columnar dendritic structure (DS), the increase in inclusion number and size with ingot diameter is approximately linear. However, at the ingot size (1050 mm in diameter in this study) when the center of the ingot converts to solidification in the equiaxial mode (EQ), the increase in number and size of the inclusions is much higher. The transition between a dendritic and an equiaxial solidification in the center of the ingots in this steel grade takes place in the region between the ingot diameters of 800 and 1050 mm.

Place, publisher, year, edition, pages
MDPI AG, 2021
Keywords
ESR, PESR, inclusions, solidification, SEM, stainless steel
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-293971 (URN)10.3390/met11030408 (DOI)000633878300001 ()2-s2.0-85101881130 (Scopus ID)
Note

QC 20210506

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
4. Differences in inclusion morphology between ESR remelted and ingot casted common martensitic stainless steel
Open this publication in new window or tab >>Differences in inclusion morphology between ESR remelted and ingot casted common martensitic stainless steel
2016 (English)In: Proceedings of the 5th International Conferens on Process Development in Iron and Steelmaking Scanmet-V 2016, 12-15 June, Luleå, Sweden, Mefos, Sweden, 2016Conference paper, Published paper (Refereed)
Place, publisher, year, edition, pages
Mefos, Sweden: , 2016
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-294037 (URN)
Conference
5th International Conferens on Process Development in Iron and Steelmaking Scanmet-V 2016, 12-15 June, Luleå, Sweden
Note

QC 20210710

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
5. Studies of three dimension inclusions from ESR remelted and conventional steel
Open this publication in new window or tab >>Studies of three dimension inclusions from ESR remelted and conventional steel
2017 (English)In: LMPC 2017, Liquid Metal Processing and Casting Conference, TMS, USA, Philadelphia, USA, 10-13 September 2017. / [ed] Stuart Rudoler, American Flux and Metal, USA, TMA, USA, 2017Conference paper, Published paper (Refereed)
Place, publisher, year, edition, pages
TMA, USA: , 2017
Keywords
ESR, Inclusions, Electrolytic Extraction, SEM
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-293984 (URN)
Conference
LMPC 2017, Liquid Metal Processing and Casting Conference, TMS, USA, Philadelphia, USA, 10-13 September 2017.
Note

QC 20210710

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
6. The Importance of Electrode Cleaness in the ESR/PESR Processes
Open this publication in new window or tab >>The Importance of Electrode Cleaness in the ESR/PESR Processes
2018 (English)In: In proceedings of the 3rd International Conference on Ingot Casting, Rolling and Forging,16-19 October 2018, Stockholm, Sweden: ICRF-138, Stockholm, 2018Conference paper, Published paper (Refereed)
Abstract [en]

This study presents results on inclusion morphology in tool steels, intended to investigate inclusion behavior during electroslag remelting (“ESR”). In this study, we investigate the relation between the inclusion content of the ESR electrode and the inclusion content of the corresponding ingot by using a chemical tracer in the process slag.

The goal is to define the extent to which the cleanness of the electrode is likely to influence the cleanness of the ESR ingot made from it. The results demonstrate how the distribution and composition differ between the electrode and the remelted ingot and explain how this regime influences the properties of the ingot.

We find that a significant fraction of the electrode inclusions pass directly through the ESR process without contacting the slag and are therefore are unchanged by the process. In consequence, the cleanness of the electrode has a significant influence on the ingot inclusion content.

Place, publisher, year, edition, pages
Stockholm: , 2018
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-294035 (URN)
Conference
3rd International Conference on Ingot Casting, Rolling and Forging,16-19 October 2018, Stockholm, Sweden
Note

QC 20210710

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
7. The behavior of Inclusions during ESR remelting
Open this publication in new window or tab >>The behavior of Inclusions during ESR remelting
2014 (English)In: Proceedings of the 2nd International Ingot Casting, Rolling and Forging Conference, ICRF 2014, 7-9 May Milano, Italy.: ICRF-30, 2014Conference paper, Published paper (Refereed)
Keywords
ESR, Ingot size, Inclusions, Local Solidification Time (LST), Aluminium
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-294038 (URN)
Conference
2nd International Ingot Casting, Rolling and Forging Conference, ICRF 2014, 7-9 May Milano, Italy.
Note

QC 20210607

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved
8. A novel evolution mechanism of Mg-Al-oxides in liquid steel. Integration of chemical reaction and coalescence-collision.
Open this publication in new window or tab >>A novel evolution mechanism of Mg-Al-oxides in liquid steel. Integration of chemical reaction and coalescence-collision.
Show others...
2020 (English)In: Journal of Alloys and Compounds, ISSN 0925-8388, Vol. 812, p. 152149-Article in journal (Refereed) Published
Keywords
Non-metallic inclusion, Mg-Al-Oxide, Thermodynamic, Coalescence-collision, Phase-field method
National Category
Metallurgy and Metallic Materials
Research subject
Materials Science and Engineering
Identifiers
urn:nbn:se:kth:diva-293974 (URN)10.1016/j.jallcom.2019.152149 (DOI)000490423000006 ()2-s2.0-85071861622 (Scopus ID)
Note

QC 20210710

Available from: 2021-05-06 Created: 2021-05-06 Last updated: 2023-03-06Bibliographically approved

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