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Monitoring the non-metallic inclusions formed in steels is of the utmost importance. In fact, inclusions, depending on their type, can affect both the properties of the steel and its processing. Once the most problematic inclusions have been detected, solutions can be found and applied to counter the arising issues. One such solution is the addition of calcium during ladle treatment to modify the inclusions shapes and avoid the precipitation of problematic inclusions. The focus was put on the detection, analysis and calcium addition countermeasure of inclusions. No clear conclusion could be drawn as to the effects of calcium addition on the inclusions, due to the very high zirconium content of the inclusions. A high zirconium content has a significant impact on the thermodynamics governing inclusion formation and prevents reliable analysis of the results. After discussion with the company, it has been found that the zirconium is not present in the steel grade but instead originates from the samplers that were used. / Övervakning av icke-metalliska inneslutningar som bildas i stål är av yttersta vikt. Faktum är att inneslutningar, beroende på typ, kan påverka både stålets egenskaper och dess bearbetning. När de mest problematiska inneslutningarna har upptäckts kan lösningar hittas och tillämpas för att motverka de uppkomna problemen. En sådan lösning är att tillsätta kalcium under skänkbehandlingen för att ändra inneslutningarnas form och undvika utfällning av problematiska inneslutningar. Fokus låg på detektering, analys och kalciumtillsats som motåtgärd för inneslutningar. Ingen tydlig slutsats kunde dras om effekterna av kalciumtillsats på inneslutningarna, på grund av inneslutningarnas mycket höga zirkoniuminnehåll. En hög zirkoniumhalt har en betydande inverkan på den termodynamik som styr bildandet av inneslutningar och förhindrar en tillförlitlig analys av resultaten. Efter diskussion med företaget har det visat sig att zirkoniumet inte finns i stålsorten utan istället härrör från de provtagare som användes.

In the present thesis, the correlation between ladle glaze and non-metallic inclusions in the ladle treatment was studied. A number of industrial trials with full scale ladle and laboratory works were performed to investigate the inclusions in the ladle treatment. BaO was used as tracer in the ladle slag to investigate the effect of slag on inclusion composition and the formation of non-metallic inclusions by ladle glaze. BaO was detected in the inclusions of all followed heats. This observation showed strong evidence for the generation of non-metallic inclusions by the ladle glaze. The increase of the fractions of BaO containing inclusions and their average content of BaO in the first heat with tracer suggested that the effect of slag on the composition of inclusions was a very slow process. The detachment of ladle glaze and the chemical transformations of oxide solution in the MgO matrix were investigated. The experimental results evidently showed that the ladle glaze could be the source of inclusions continually during the ladle treatment. Samples of liquid oxide solution to simulate the liquid oxide inclusions carried over from EAF were equilibrated with molten steel under controlled atmosphere. The results along with thermodynamic calculation suggested that the SiO2 content of inclusions from EAF could be considerably reduced by dissolved aluminium in the steel. This would explain the vanishing of inclusions containing high SiO2 content after deoxidation. Due to the lack of experimental data, the viscosities of slags in the Al2O3-CaO-MgO-SiO2 system were measured using the rotating cylinder method in the temperature range of 1720 to 1910 K. Eight different slag compositions related to the secondary steel making operations were selected. Viscosities in this system and its sub-systems were expressed as a function of temperature and composition based on the viscosity model developed earlier at KTH. The activities of oxide components in the Al2O3-CaO-MgO-SiO2 systems at 1873 K were measured by equilibrating liquid slag and metal. Either silicon or copper was used as the metal phase and the oxygen partial pressure was controlled with different mixing rates of Ar and CO gas flow in equilibrium with graphite. Iso-activity lines were drawn from the measured activity values in the isothermal section of the slag systems. Nine series of industrial trials were carried out using the same ladle in each series to examine the effect of ladle slag on the number of non-metallic inclusions in the next heat. It was found that the number of inclusions increased with SiO2 content of the ladle slag in the previous heat. No clear trends were found for the effects of viscosity and MgO activity of the previous slag on the number of inclusions. Theoretical analysis based on the experimental results suggested that the formation of 2CaO∙SiO2 followed but the dusting of the compound made the refractory more porous, which was reasonable for the number of non-metallic inclusions.

<p>The thesis is based on two supplements with two major objectives. In the first supplement equilibrium top slag-steel bulk and inclusions-steel bulk were investigated by comparison between calculated and measured oxygen activity values. This was done by applying different oxide activity models for slags combined with thermodynamic calculations. In the second supplement the inclusion composition is studied during the ladle refining process. The inclusion composition is related to top slag composition and other parameters during ladle</p><p>treatment.</p><p>The work was carried out by collecting data during well controlled sampling procedures at two different steel plants. Extensive inclusion analyses in Scanning Electron Microscope, SEM, were done. The data was used together with thermodynamics for a description of the interaction between slag-steel-inclusion interaction during ladle treatment.</p><p>Evaluation of inclusion composition during the ladle refining have revealed that the majority of the inclusions belonged to the system Al₂O₃-CaO-MgO-SiO₂and showed a continuous composition change throughout the ladle refining process, from high Al₂O_3, via MgO-spinel to finally complex types rich in CaO and Al₂O_3. The final composition after vacuum treatment was found to be close to the top slag composition. Small process parameter changes and practical variations during ladle refining were proven to give large differences of the inclusion composition.</p><p>Finally, it was concluded that equilibrium does not exist between top slag and steel bulk, with respect to oxygen, for the studied conditions. However, the equilibrium does exist between the steel bulk and inclusion.</p>

The thesis is based on two supplements with two major objectives. In the first supplement equilibrium top slag-steel bulk and inclusions-steel bulk were investigated by comparison between calculated and measured oxygen activity values. This was done by applying different oxide activity models for slags combined with thermodynamic calculations. In the second supplement the inclusion composition is studied during the ladle refining process. The inclusion composition is related to top slag composition and other parameters during ladle treatment. The work was carried out by collecting data during well controlled sampling procedures at two different steel plants. Extensive inclusion analyses in Scanning Electron Microscope, SEM, were done. The data was used together with thermodynamics for a description of the interaction between slag-steel-inclusion interaction during ladle treatment. Evaluation of inclusion composition during the ladle refining have revealed that the majority of the inclusions belonged to the system Al2O3-CaO-MgO-SiO2 and showed a continuous composition change throughout the ladle refining process, from high Al2O3, via MgO-spinel to finally complex types rich in CaO and Al2O3. The final composition after vacuum treatment was found to be close to the top slag composition. Small process parameter changes and practical variations during ladle refining were proven to give large differences of the inclusion composition. Finally, it was concluded that equilibrium does not exist between top slag and steel bulk, with respect to oxygen, for the studied conditions. However, the equilibrium does exist between the steel bulk and inclusion. / QC 20101109

It is well known that inclusions affect the properties of steels and alloys. Therefore, it is important to understand what type of inclusions that exist and how they behave and especially with a focus on large size inclusions. Thus, the large size non-metallic inclusions in ferroalloy FeTi70R were investigated in two dimensions (2D) by using scanning electron microscopy (SEM) in combination with an energy dispersive technique (EDS). It was found that the FeTi70R ferroalloy contain complex oxide inclusions consisting mostly of CaO, SiO2 and TiOx. Furthermore, experimental trials were performed to investigate how these inclusions behaved when entering a melt. More specifically, a comparison between pure Fe and an Alloy 825 grade were made. These results determined the parameters effect on the transformation of the inclusions in the melt. The large size non-metallic inclusions in Alloy 825 during the ladle treatment were investigated during industrial trials by using both two dimensional (2D) and three dimensional (3D) microscopic investigations. The results showed that inclusions consisted of spherical oxides and clusters made up of oxides and nitrides. Further investigations found that the spherical inclusions were transformed from existing NMI in the FeTi70R ferroalloy and slag particles. As for the clusters, they originate from deoxidation products. Furthermore, small inclusions precipitated in the local zones around the added FeTi70R ferroalloy and titanium nitrides. Investigations also found that only Al2O3-MgO and TiN clusters exist after casting. Industrial trials were performed during the last period of the ladle treatment and using a combined electromagnetic (EMS) and gas (GS) stirring. The purpose to investigate the effect of different EMS directions on the agglomeration and on the removal of Al2O3-MgO and TiN clusters. The investigations were then performed in 3D after an electrolytic extraction of the metal samples. The results show that electromagnetic stirring in the upwards direction is best for the agglomeration of the Al2O3-MgO and TiN clusters. However, electromagnetic stirring in the downwards direction is more effective to remove clusters from the melt. This is in agreement with the theoretical predictions based on Stokes’, Brownian and Turbulent collisions. Also, the calculations showed that for Al2O3-MgO clusters with sizes &lt;20 μm the Turbulent collision is the defining factor for agglomeration. However, both Stokes’ and Turbulent collisions are dominant for larger inclusions. For the TiN clusters, turbulent collisions is the dominant factor. Further investigations with more heats and stirring modes were done by using 2D microscopic investigations. More specifically, the number, size, composition and morphology of different inclusions were determined by using SEM in combination with EDS and Inca Feature analyses. The results show that the EMS in downwards direction with a 0.04 m3 min-1 gas flow rate promotes a general removal of Al2O3-MgO and TiN inclusions. Furthermore, that the upwards EMS direction promotes a drastically increase of inclusions having an equivalent size smaller than 11.2 μm. Moreover, the stirring with a 0.02 m3 min-1 gas flow rate has a better removal rate for both downwards and upwards stirring directions compared to the stirring with a 0.04 m3 min-1 gas flow rate. However, no influence on the inclusion composition and morphology could be seen from the different stirring modes. / Det är välkänt att inneslutningar påverkar egenskaperna i stål och legeringar. Därför är det viktigt att förstå vilken sorts inneslutningar som existerar samt hur de beter sig, särskilt stora inneslutningar. Således undersöktes de stora icke-metalliska inneslutningarna i ferrolegeringen FeTi70R i två dimensioner (2D) genom att använda svepelektronmikroskopi (SEM) i kombination med energidispersionsteknik (EDS). Det visade sig att ferrolegeringen FeTi70R innehåller komplexa oxidinneslutningar bestående huvudsakligen av CaO, Si02 och TiOx. Vidare utfördes laborativa försök för att undersöka hur dessa inneslutningar uppträder när de kommer ner i det smälta stålet. Mer specifikt så gjordes en jämförelse mellan rent Fe och Alloy 825 legeringen. Dessa resultat fastställde hur olika parametrar påverkade inneslutningarnas omvandling i smältan. De stora icke-metalliska inneslutningarna i Alloy 825 legeringen under skänkugnsbehandlingen undersöktes vid industriella försök med hjälp av både tvådimensionella (2D) och tredimensionella (3D) mikroskopiska undersökningar. Resultaten visade att inneslutningarna bestod av sfäriska oxider och kluster uppbyggda av oxider och nitrider. Ytterligare undersökningar visade att de sfäriska inneslutningarna omvandlades från befintliga icke-metalliska inneslutningar i ferrolegeringen FeTi70R och slaggpartiklar. När det gäller kluster härrör de från desoxidationsprodukter. Vidare så bildades små inneslutningar i de lokala zonerna kring den tillsatta FeTi70R legeringen och kring titanitriderna. Undersökningarna fann också att endast Al2O3-MgO och TiN-kluster existerar efter gjutning. De industriella försöken utfördes under den sista perioden av skänkugnsbehandlingen och med en kombinerad elektromagnetisk (EMS) och gas (GS) omröring. Syftet med detta var att undersöka effekten av olika riktningar på EMS omrörningen på agglomerationen och avskiljningen av Al2O3-MgO- och TiN klustren. Undersökningarna utfördes sedan i 3D efter en elektrolytisk extraktion av metallproverna. Resultaten visar att en uppåtriktad elektromagnetisk omröring är bäst för agglomereringen av Al2O3-MgO inneslutningar och TiN kluster. Emellertid så är en nedåtriktad elektromagnetisk omröring effektivare för att avlägsna kluster från smältan. Dessa resultat överensstämmer med de teoretiska förutsägelserna baserade på Stokes, Brownian och Turbulent kollisionsvolymer. Dessutom visade beräkningarna att för Al2O3-MgO kluster med storlekar &lt;20 μm är det turbulenta kollisioner som är den avgörande faktorn för agglomerering. Dock är det både Stokes och de Turbulenta kollisionerna som dominerar för större inneslutningar. För TiN klustren är det de turbulenta kollisionerna som är den dominerande faktorn. Ytterligare undersökningar med fler charger av Alloy 825 och olika omrörningsmetoder gjordes baserade på 2D mikroskopiska undersökningar. Mer specifikt så bestämdes antalet, storleken, sammansättningen och morfologin för olika inneslutningar med användning av SEM i kombination med EDS och Inca Feature analyser. Resultaten visar att en nedåtriktad EMS i kombination med ett gasflöde på 0,04 m3 min-1 främjar ett generellt avlägsnande av Al2O3-MgO och TiN inneslutningar. Vidare främjar den uppåtriktade EMS omrörningen en drastisk ökning av inneslutningar med en ekvivalent storlek av 11,2 μm eller mindre. Vidare har omröringen med ett gasflöde på 0,02 m3 min-1 en bättre avskiljningshastighet för inneslutningar i både nedåt och uppåtgående omrörningsriktningar jämfört med omrörningen med ett gasflöde på 0,04 m3 min-1. Emellertid kunde inget inflytande på sammansättningen och morfologin ses från de olika omrörningssätten. / <p>QC 20171122</p>

It is well known that inclusions affect the properties of steels and alloys. Therefore, it is important to understand what type of inclusions that exist and how they behave and especially with a focus on large size inclusions. Thus, the large size non-metallic inclusions in ferroalloy FeTi70R were investigated in two dimensions (2D) by using scanning electron microscopy (SEM) in combination with an energy dispersive technique (EDS). It was found that the FeTi70R ferroalloy contain complex oxide inclusions consisting mostly of CaO, SiO2 and TiOx. Furthermore, experimental trials were performed to investigate how these inclusions behaved when entering a melt. More specifically, a comparison between pure Fe and an Alloy 825 grade were made. These results determined the parameters effect on the transformation of the inclusions in the melt. The large size non-metallic inclusions in Alloy 825 during the ladle treatment were investigated during industrial trials by using both two dimensional (2D) and three dimensional (3D) microscopic investigations. The results showed that inclusions consisted of spherical oxides and clusters made up of oxides and nitrides. Further investigations found that the spherical inclusions were transformed from existing NMI in the FeTi70R ferroalloy and slag particles. As for the clusters, they originate from deoxidation products. Furthermore, small inclusions precipitated in the local zones around the added FeTi70R ferroalloy and titanium nitrides. Investigations also found that only Al2O3-MgO and TiN clusters exist after casting. Industrial trials were performed during the last period of the ladle treatment and using a combined electromagnetic (EMS) and gas (GS) stirring. The purpose to investigate the effect of different EMS directions on the agglomeration and on the removal of Al2O3-MgO and TiN clusters. The investigations were then performed in 3D after an electrolytic extraction of the metal samples. The results show that electromagnetic stirring in the upwards direction is best for the agglomeration of the Al2O3-MgO and TiN clusters. However, electromagnetic stirring in the downwards direction is more effective to remove clusters from the melt. This is in agreement with the theoretical predictions based on Stokes’, Brownian and Turbulent collisions. Also, the calculations showed that for Al2O3-MgO clusters with sizes &lt;20 μm the Turbulent collision is the defining factor for agglomeration. However, both Stokes’ and Turbulent collisions are dominant for larger inclusions. For the TiN clusters, turbulent collisions is the dominant factor. Further investigations with more heats and stirring modes were done by using 2D microscopic investigations. More specifically, the number, size, composition and morphology of different inclusions were determined by using SEM in combination with EDS and Inca Feature analyses. The results show that the EMS in downwards direction with a 0.04 m3 min-1 gas flow rate promotes a general removal of Al2O3-MgO and TiN inclusions. Furthermore, that the upwards EMS direction promotes a drastically increase of inclusions having an equivalent size smaller than 11.2 μm. Moreover, the stirring with a 0.02 m3 min-1 gas flow rate has a better removal rate for both downwards and upwards stirring directions compared to the stirring with a 0.04 m3 min-1 gas flow rate. However, no influence on the inclusion composition and morphology could be seen from the different stirring modes. / Det är välkänt att inneslutningar påverkar egenskaperna i stål och legeringar. Därför är det viktigt att förstå vilken sorts inneslutningar som existerar samt hur de beter sig, särskilt stora inneslutningar. Således undersöktes de stora icke-metalliska inneslutningarna i ferrolegeringen FeTi70R i två dimensioner (2D) genom att använda svepelektronmikroskopi (SEM) i kombination med energidispersionsteknik (EDS). Det visade sig att ferrolegeringen FeTi70R innehåller komplexa oxidinneslutningar bestående huvudsakligen av CaO, Si02 och TiOx. Vidare utfördes laborativa försök för att undersöka hur dessa inneslutningar uppträder när de kommer ner i det smälta stålet. Mer specifikt så gjordes en jämförelse mellan rent Fe och Alloy 825 legeringen. Dessa resultat fastställde hur olika parametrar påverkade inneslutningarnas omvandling i smältan. De stora icke-metalliska inneslutningarna i Alloy 825 legeringen under skänkugnsbehandlingen undersöktes vid industriella försök med hjälp av både tvådimensionella (2D) och tredimensionella (3D) mikroskopiska undersökningar. Resultaten visade att inneslutningarna bestod av sfäriska oxider och kluster uppbyggda av oxider och nitrider. Ytterligare undersökningar visade att de sfäriska inneslutningarna omvandlades från befintliga icke-metalliska inneslutningar i ferrolegeringen FeTi70R och slaggpartiklar. När det gäller kluster härrör de från desoxidationsprodukter. Vidare så bildades små inneslutningar i de lokala zonerna kring den tillsatta FeTi70R legeringen och kring titanitriderna. Undersökningarna fann också att endast Al2O3-MgO och TiN-kluster existerar efter gjutning. De industriella försöken utfördes under den sista perioden av skänkugnsbehandlingen och med en kombinerad elektromagnetisk (EMS) och gas (GS) omröring. Syftet med detta var att undersöka effekten av olika riktningar på EMS omrörningen på agglomerationen och avskiljningen av Al2O3-MgO- och TiN klustren. Undersökningarna utfördes sedan i 3D efter en elektrolytisk extraktion av metallproverna. Resultaten visar att en uppåtriktad elektromagnetisk omröring är bäst för agglomereringen av Al2O3-MgO inneslutningar och TiN kluster. Emellertid så är en nedåtriktad elektromagnetisk omröring effektivare för att avlägsna kluster från smältan. Dessa resultat överensstämmer med de teoretiska förutsägelserna baserade på Stokes, Brownian och Turbulent kollisionsvolymer. Dessutom visade beräkningarna att för Al2O3-MgO kluster med storlekar &lt;20 μm är det turbulenta kollisioner som är den avgörande faktorn för agglomerering. Dock är det både Stokes och de Turbulenta kollisionerna som dominerar för större inneslutningar. För TiN klustren är det de turbulenta kollisionerna som är den dominerande faktorn. Ytterligare undersökningar med fler charger av Alloy 825 och olika omrörningsmetoder gjordes baserade på 2D mikroskopiska undersökningar. Mer specifikt så bestämdes antalet, storleken, sammansättningen och morfologin för olika inneslutningar med användning av SEM i kombination med EDS och Inca Feature analyser. Resultaten visar att en nedåtriktad EMS i kombination med ett gasflöde på 0,04 m3 min-1 främjar ett generellt avlägsnande av Al2O3-MgO och TiN inneslutningar. Vidare främjar den uppåtriktade EMS omrörningen en drastisk ökning av inneslutningar med en ekvivalent storlek av 11,2 μm eller mindre. Vidare har omröringen med ett gasflöde på 0,02 m3 min-1 en bättre avskiljningshastighet för inneslutningar i både nedåt och uppåtgående omrörningsriktningar jämfört med omrörningen med ett gasflöde på 0,04 m3 min-1. Emellertid kunde inget inflytande på sammansättningen och morfologin ses från de olika omrörningssätten.