review the solidification behavior of slags: phenomena

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Review

ISIJ International, Vol. 54 (2014), No. 12, pp. 2665–2671

The Solidification Behavior of Slags: Phenomena Related to Mold Slags

Alan William CRAMB*

Illinois Institute of Technology, Chicago, IL 60616-3793 USA.

(Based on Honorary Member Lecture; held at Tokyo Denki University on March 27, 2013. Manuscriptreceived June 11, 2014.)

The solidification behavior of slags is a complex subject due to the varied chemical compositions ofsteelmaking slags. However, recent experimental developments, using the fact that slags that do not con-tain significant quantities of transition metal oxides are transparent, has allowed the development of opti-cal techniques to observe slag solidification behavior. While “curiosity based research” was the initiator ofsuch studies, it has quickly become apparent that observation of the phenomenon of slag solidificationhas lead to a much deeper understanding of the role of slag solidification behavior in the process of thecontinuous casting of steel. In this paper findings from observation of slag solidification will be discussedwith reference to developments in continuous casting.

KEY WORDS: slags; solidification behavior; continuous casting; TTT diagrams; steel.

1. Introduction

In the steelmaking process, slags react with liquid steel toeither refine or contaminate depending upon local chemicalconditions. Slags also absorb second phase particles such asalumina, cover liquid steel to prevent re-oxidation, wet liq-uid steel and act as a lubricant or a heat transfer promoteror reducer depending upon local thermal conditions. Slagsgenerally are used in extreme thermal gradients in continu-ous casting and the solidification behavior of a slag is ofextreme interest in the mold of a continuous caster.

Slags are also part of the family of oxides that can formglasses during cooling, rather than precipitate the most ther-modynamically stable phase and, as such, can have a varietyof solidification morphologies depending on their thermalhistory. They can be glasses, partially crystalline – a mixtureof a solid and a glass, or fully crystalline. Their morphologycan also vary with time depending upon thermal history. Forexample, reheating after cooling will almost always increasethe crystalline volume fraction of solidified slags.

When glasses, slags are generally colorless when iron andmanganese oxide contents are low but can darken signifi-cantly with the addition of FeO and MnO. Thus, their overallheat transfer characteristics are a function of their chemistryand their crystallized volume fraction as radiation heattransfer rates are important at the shell temperatures thatoccur in the mold of a continuous casting machine whereheat transfer characteristics vary markedly with molddesign, flux design and time of casting, as the slag solidifi-cation structure can age.

In slags mass transfer is the predominant mechanism

which controls the solidification rate (unlike metal solidifi-cation) and rapid cooling quickly leads to a low volume ofcrystallite or glass formation. Slags can also be chemicallyunstable, especially those containing fluorine and sodiumoxide and certain slags vary in chemistry with holding timedue to evaporation. Slags can also dissolve gasses of whichwater vapor is perhaps the most important and the presenceof dissolved water in slags markedly changes their solidifi-cation behavior and can lead to the formation of bubbleswithin the slags during cooling.

In this paper I will discuss the solidification behavior ofslags and highlight the work that resulted in my collabora-tion with a number of Professors, post doctoral and graduatestudents during my career. In particular, I will discuss theeffect of mold slag solidification phenomenon on the oper-ation of a continuous casting mold.

2. Background

When I began my academic career in 1986 I was fortu-nate to immediately begin a long-term collaboration withProf. Itaru Jimbo. Without this collaboration, I would nothave been successful in my academic career.1–18) Our worktogether was focused on interfacial energies between slagsand steels and began my interest in interfacial considerationsduring the continuous casting of steel. My first presentationin Japan occurred in 19903) and was a joint publication withProf. Jimbo. My first publication in ISIJ5) occurred in 1992and was also co-authored with Prof. Jimbo.

I first visited Japan in 1983 as part of a delegation inter-ested in the state of the art of the continuous casting ofsteel. My memories of vising Nippon Steel, KawasakiSteel, Sumitomo Metal and Kobe Steel are still very freshas Japanese technology in this area significantly had sur-

* Corresponding author: E-mail: [email protected]: http://dx.doi.org/10.2355/isijinternational.54.2665

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passed anything in the United States at that time. In 1990 Imade my fourth visit to Japan but this time as a young pro-fessor accompanying Prof. Richard Fruehan who had beentasked by the National Science Foundation (NSF) to studyfundamental and long-term research in both universities andindustry as it related to steel processing.19,20) During this vis-it I met Prof. Fuwa, Prof. Sano, Prof Ban-ya and Prof. Morita,the great metallurgical professors of that time and wouldknow all four well for the next twenty years. At that time Ialso met again Professors Hino and Sasaki, both who hadbeen postdoctoral fellows at the University of Pennsylvaniawhere Prof Sasaki was in the same lab as I (under ProfessorBelton), while Prof Hino was working with ProfessorGaskell. I also met Professor Iguchi, Professor Iwase andProfessor Suzuki. In industry I met Prof. Emi, also a Pennalumni (with Prof. Bockris). I visited Tokyo, Kyoto, Osakaand Sendai and met the leaders of the thermodynamics andkinetics of steelmaking community in Japan. I, with Prof.Iguchi, subsequently organized a US-Japan symposium inTokyo.

Starting in 1987 I developed a close relationship withProfessors from Japan that has continued to this day. Ihave been fortunate to do research with Prof. Nagasaka(Tohoku),21–23) Professor Suzuki (Tokyo),24–28) ProfKashiwaya (Hokkaido),29–39) Professor Ueda (Tohoku)40–43)

and Professor Shibata (Tohoku).44–47) In addition, I had fourexcellent graduate students from Japan: Dr. K. Shimizu,48–50)

Dr. H. Todoroki,24–27) M. Nakata51–53) and K. Fuchigami.46)

My Japanese connection has lead to over 50 publications ina span of 18 years.

2.1. SlagsTo the chemical metallurgist slags were very important as

the medium that allowed the removal of oxides, sulfur andphosphorus from liquid iron and liquid steel. Understandingslag chemistry and its manipulation brought about the era of“Clean Steel” ladle technology. Of course, Professors Fuwa,Ban-ya and Sano, all who studied at MIT with ProfessorsChipman and Elliott, made great contributions in our under-standing of the thermodynamics of slags and slag-steelinteractions. The kinetics of slag metal reactions would beclarified by Prof. Fruehan’s group and our understandingof refining would be led by the pioneering work of Prof.Szekely and his group in understanding the importance offluid flow in liquid steel processing.

One area that was not well understood or studied was thatof slag solidification phenomena as, until the advent of con-tinuous casting, there was no apparent need for such anunderstanding. While ladle slags were designed to be liquidat steelmaking temperatures, to be able to react with sulfurand to absorb solid oxides, mold slags had significantlygreater requirements due to the extreme thermal gradients inthe mold of a continuous caster.

2.2. Observation of the Solidification Behavior of MoldSlags

Liquid slags that are used during the continuous castingof steel must be stable and liquid at steelmaking tempera-tures, wet both liquid and solid steels, adsorb solid oxides,remain liquid and fluid in extreme conditions of thermalgradient and solidify (or crystallize) under defined condi-

tions. The liquid flux layer that infiltrates between the caststrand and the mold wall can be less than 1 mm in thicknesswith a temperature differential that varies from 1 530°C to200°C depending on position between the solidifying shelland the water cooled copper molds used during the contin-uous casting of steel.

Liquid slags in ladle metallurgy are based on the CaO–Al2O3 system and usually contain some MgO to reduce ladlelining wear rate. FeO, MnO and SiO2 can also be presentand amounts that are determined by one’s ability to controlfurnace slag carry over. In electric furnace steelmaking it iscommon to find FeO + MnO levels below 1%, while in BOFoperations higher FeO+MnO levels are common (3 to 5%).In operations with limited slag control, slag killing with alu-minum or calcium carbide is common as a means to reduceFeO+MnO levels. Additions of Calcium Fluoride can aid inliquid slag formation; however, it is unusual for such addi-tions to result in significant fluoride content in the ladleslags due to evaporation of CaF2 and SiF4.

Mold slags are chemically different from ladle slags astheir operating temperatures are much lower than that foundin ladles. First all of liquid formation at low temperatures isdesired, thus the starting point of mold fluxes is the CaO–SiO2 system. Additions of the glass formers Na2O, K20,Li2O and B2O3 are also common. In addition significantquantities of CaF2 can also be found. FeO, MnO, Al2O3,ZrO2, and MgO can also be added or adsorbed from the steelor the submerged entry nozzle. As such mold slags are notchemically stable in contact with killed liquid steels and theactual flux chemistry in contact with liquid steel is depen-dent on both the initial powder chemistry and its interactionwith the liquid steel. In addition, above 900°C, NaF vaporis stable and fumes off the top of the mold slag if surfacetemperature rise above 900°C.

Slags are ionic liquids, can conduct electricity and aregenerally easy glass formers. Slags can also interact withwater vapor and, even, at high temperatures, have water sol-ubility that can lead to bubble formation or even outgassingduring crystallization.

To understand the solidification behavior of slags onemust accept that they are glass formers and, as such, can besignificantly undercooled with respect to their thermody-namically predicted transformation temperature. A range ofsolidification morphologies is possible and actual structuresdepend upon cooling rate and thermal history. Thus one canfind glass formation, a mixture of glass and crystallized sol-id or a fully solidified structure that exhibits segregation.During dynamic cooling, as nucleation behavior determinesthe first phase to form, not the phase diagram, metastablephases can be found. Time-Temperature-Transformation(TTT) diagrams are useful in understanding solidificationbehavior and an example by Kashiwaya33) is given in Fig. 1.

In this diagram one can observe that (1) at high coolingrates a glass can be formed; (2) depending on the coolingpath the phase that nucleates and grows is different – di-calcium silicate at high temperatures and cuspidine at lowertemperatures and (3) that it is possible to significantlyundercool this slag before the initiation of solidification.

The effect of chemistry change can also be easily mea-sured using TTT diagrams as shown in Fig. 2 where theeffect of sodium oxide content on the solidification behavior


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of a slag is documented.These TTT diagrams can be measured using either a sin-

gle (SHTT) or a Double Hot thermocouple technique(DHTT).33,34, 51–53) Of course, actual operations occur not inisothermal slices but in a continuously cooling environmentthat leads to the necessity of developing CCT diagramsbased upon actual mold operations where the hot face nextto the shell and the cold face next to the mold wall are sim-ulated. An example of the difference between a CCT and aTT curve is given in Fig. 3 where the onset of solidificationis indicated by the solid dots on the CCT cooling ratecurves. During continuous cooling the time to onset of solid-ification can be significantly increased when compared toisothermal cooling.

A simulation of mold solidification is shown in Fig. 4using the DHTT where one thermocouple follows the cool-ing curve of the mold wall and the other the cooling curveof the solidified steel shell. To the right of the photographis the cold face and to the left the hot face. In this photo-graph, taken after approximately one minute after initiationof the experiment, a glassy area can be seen against the coldface (approximately 300°C), liquid slag is against the hotface (approximately 1 100°C) and between these two limitsis a crystallized mass that grows with time. At time zero the

liquid slag and all chemistries in the liquid are equivalent.Immediately on cooling of the cold face thermocouple aglass forms against the cold thermocouple and the extent ofthis glass phase increases with time. Crystallization occursby nucleation of Cuspidine in the liquid and the first crystalsform ahead of the glass phase, the remaining liquid on thehot side of the experiment then changes composition due to

Fig. 1. TTT diagram for an industrial mold slag.33)

Fig. 2. The effect of sodium oxide on the TTT curve of a calciumsilicate based slag.35)

Fig. 3. Comparison of a TTT and a CCT curve for a slag.57)

Fig. 4. Photograph of a simulated solidification of a mold slagusing a DHTT apparatus where the hot face is cooling as ifit were the shell of continuous caster and the cold face is atthe temperature of a water cooled mold.33) Thermal fieldsare courtesy of calculations by Professor Brian Thomas.64)

Fig. 5. A continuous casting simulation where the shell is removedfrom the mold. On the left (a) is a water cooled mold withthe slag layer attached. On the right (b) is the solidifiedshell. Photographs by Badri.55)

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segregation. With time the extent of the crystallized areaincreases towards the hot thermocouple. Thus, as the liquidmold slag is sheared and moves down the mold its chemistrychanges and it can either remain liquid longer than expectedfrom the phase diagram or solidify at a higher temperature,depending on chemistry changes in this liquid. The lubrica-tion behavior depends upon the details of solidificationbehavior of the slag and the fluid flow conditions betweenthe shell and the mold.

Initially there is a significant portion of heat transferredby radiation across the liquid film; however, once crystalli-zation occurs radiation is blocked and the total heat transferrate decreases. If one envisions a small volume of mold slagthat is moving down the mold as the strand is removed thenone can understand that the glass area sticks to the mold sur-face and remains in contact with mold unless physicallyremoved. The liquid film will slowly transform over time ascrystallization occurs with the crystallized fraction growingmore slowly as one moves down the mold as crystal growthrate is dependent on diffusion rates in the liquid mold slag.The slag continues to evolve with time and heat transferrates in molds can be seen to decrease as a function of timeto the point that casting speeds must be reduced. The solu-tion to this problem is to pause casting speed, allow the shellto bulge against the mold, cool, strengthen and then onincreasing casting the glass film is removed and a new filmis deposited on the mold wall. Heat transfer rates thenincrease to their initial state.

Often in continuous casting it is assumed that a gapoccurs between the mold wall and the slag film and often agap interface resistance to heat transfer is ascribed to allowmathematical models to be tuned to actual data from moldsin continuous casting machines. One should be careful whenone uses a mathematical process (the adding of an additionaltunable parameter) to a complex process in describing thatparameter in physical terms. For example, in ingot, billet orstrip casting, where there is intermittent contact between theshell and the mold, it is clear that there must be a parameterto account for the fact that one does not have perfect contactand a gap interface resistance parameter has some relation-ship to the physical reality, even though this cannot be cal-culated from first principles and is a tuning parameter of themodel. In the mold of a continuous caster there is no phys-ical unfilled gap between the shell and the mold, but inter-mittent contact between the shell and the mold where allother spaces are filled with a liquid mold slag. In the bestof possibilities, at the top of the mold there is no physicalcontact when the mold is oscillating and a liquid flux isbeing fed into the pace between the shell and the mold. InFig. 5, the flux layer from a mold simulator is seen to wetand stick to the mold wall and become a replica of the solid-ifying shell where the flux layer thickness varies with thevariation in the shell profile, being deeper in the oscillationmarks and shallower elsewhere.54,55)

As the slag moves down the mold it cools and flows overpreviously cooled slag and the thermal gradients within theslag film are a function of position and time. Crystallizationof the slag reduces the radiative heat transfer rate as shownby Wang.56) As the crystallization phenomena causes signif-icant stresses, the slag film may crack or buckle leading toa changing interface contact especially in the lower parts of

the mold. The radiative heat transfer rates can decrease byup to 20% and the contact conditions lower in the mold canchange and affect conduction heat transfer rates. Therefore,the heat transfer in the mold is intimately affected by thenature of solidification and its effects on transport mecha-nisms.

3. Solidification Structure

The double hot thermocouple technique as developed byKashiwaya et al. at CMU30–35) has become an excellent toolfor understanding the solidification structure of slags. Theextreme sensitivity of solidification structure to both coolingrate and final temperature can be easily photographed inslags that are transparent. For example, a morphologicalTTT diagram was developed by Orrling57) is shown in Fig.6 and indicates that solidification structure is extremelysensitive to the exact solidification thermal conditions.Photographs of the various structures are given in Fig. 7. Itis surprising that slag solidification is very similar in mor-phology to that of water solidification where crystal snow-flakes are easily identifiable within these structures.

3.1. Effect of Water VaporA surprising development from the DHTT studies was the

realization that humidity affects the solidification behaviorof slags, changes the TTT diagram (making solidificationoccur earlier) (Fig. 8) and increases the observed nucleationfrequency and growth rate58,59) of any precipitated crystals.Also in the presence of water vapor, bubble formation canoccur during solidification where water vapor bubblesnucleate and grow ahead of growing crystals. This is againsimilar to ice formation where dissolved oxygen precipitatesas bubbles ahead of growing ice crystals giving rise to bub-bles in ice.

3.2. DHTT IssuesOne major issue in relation to the DHTT technique is the

care one must take when attempting to make measurementsusing slags that contain significant quantities of fluorine dueto the highly volatile nature of NaF and SiF4. This meansthat the measurements are function of time due to changing

Fig. 6. TTT diagram showing type of solidification morphologydepending on isothermal temperature observed by Orrling.57)


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chemistry as in the DHTT slag sample size is small and itssurface area is large. Only one measurement is possible onany slag sample and experimental time must be short andchemistry must be determined after the experiment toendure the chemical changes are small. Another issue inusing mold slags in the DHTT is that slags containing sig-nificant quantities of FeO, MnO and TiO2 are not fullytransparent and difficult to observe. DHTT experimentswork best with stable oxides.

4. Crystal Growth Rates

In liquid metals that are cooling, the transfer of heat con-trols the solidification rate and normal solidification, wherethe temperature gradient is positive across the interface andheat transfer is through the growing shell, is the predomi-nant mechanism for solidification until one reaches the pointwhere equiaxed formation can occur – when liquid is under-cooled.

In slags the solidification behavior is controlled primarilyby diffusion in the liquid rather than heat transfer and allsolidification occurs predominantly in an undercooled melt.Glass formation is possible when cooling rates are high.Thus equiaxed crystal growth is quite common in slags

unless one nucleates from a surface (such as the thermocou-ple in a DHTT experiment.

The solidification behavior of slags is quite different thanmost metals as crystal growth rates decrease with tempera-ture. For example in Fig. 9, which chronicles the under-cooled solidification rate for liquid iron, the growth rateincreases with undercooling46) where growth rates are sig-nificant and measured in mm per second. In Fig. 10, thegrowth rates in calcium aluminate are shown where growthdecreases with undercooling and rates are small - measuredin micrometers per second.

Orrling showed that the growth rates of equiaxed crystalsin slags fits the diffusion theory growth rate as outlined byIvantsov by using confocal microscopy.60) As growth rateand dissolution rate are similar phenomenon, diffusion ratesin these liquids have been estimated using such techniquesas measuring dissolution rates of particles in liquid slags atconstant temperature. It should be noted that growth canalso be used in isothermal experiments for a similarpurpose61–63) and Sridhar Seetharaman63) developed the fol-lowing diagram (Fig. 11) to choose slag chemistries for high

Fig. 7. Variations of crystal morphology with temperature. Photographs by Orrling.57)

Fig. 8. Effect of water vapor on the TTT curve.57)

Fig. 9. Undercooled growth rate in liquid iron.46)

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dissolution rates of alumina in a CaO–Al2O3–SiO2 slag asindicated by the concentration difference and the inverse ofviscosity (ΔC/μ), where the flux J units are gm/cm2 sec andthe equation can be written as:

.......................... (1)

assuming that one can relate diffusivity (D) to viscosity (μ)according to the Stokes-Einstein relation where Dμ/T = con-stant. Thus the maximum dissolution rate should occurwhen ΔC/μ is a maximum.

In mold slags the solubility of alumina and zirconia (ΔC)can be significant and the viscosity of mold fluxes (μ) canbe quite low (thus diffusion rates can be high). This can leadto severe erosion of Submerged Entry Nozzles (SEN) in themold of a continuous casting machine as ΔC/μ is a maxi-mized. Liquid steel dissolves graphite in the SEN andspreads (wetting) removing graphite. The liquid steel thencontacts the ceramic and retracts (de-wetting) leading to acyclic flow of slag and steel at the slag/steel interface. Thusthe potential for extreme levels of erosion are high as thereis a large capacity for dissolution in the slags, high diffusionrates and a continual mechanism to bring fresh ceramic tothe slag. Of course this leads to local chemical inhomoge-neity in the mold slag that can affect its solidification behav-ior and induce cracks in continuously cast product.

4.1. Potential Future ConsiderationsThe mold in a continuous caster is the key to understand-

ing the surface created during casting. Significant modelingwork has been focused on our understanding the initiationof steel solidification and the subsequent growth of thesolidified shell. Unless the solidification processes in a liq-uid slag are fully understood, it will be impossible to devel-op an appropriate model of the mold of a continuous casterthat enables mold design, nozzle design, slag chemistry andmold operational parameters such as oscillation pattern, fre-quency, stroke and casting speed to be coupled for a givensteel grade. Initial work on this subject was documented inthe thesis of Moinet.65)

Future work in this area should be focused on the mea-surement and prediction of both TTT and CCT diagrams asa function of slag chemistry. In addition, development ofappropriate heat transfer models to accurately predict thethermal profile within the slag film as a function of positionand time in the mold are necessary in order to fully under-stand the temporal nature of the transformations that occurwithin a liquid slag. Of course, the effect of atmosphere,especially humidity, must be documented to enable accurateprediction of solidification structure and porosity due to gasrelease at the growing solidification front to be properlydocumented.

The future for mold powders and the subsequent slagsthat develop upon melting must be towards chemistries thatare stable in contact with liquid steels. Thus future devel-opments will lead to mold fluxes that are: (1) without flu-orine to eliminate fluoride off gassing and acidification ofthe secondary cooling water system; (2) without solid car-bon additions to eliminate CO off gassing and the potentialfor steel surface recarburization; (3) stable with regard tothe ceramic nozzle or at least with a minimal nozzle erosionrate; (4) without easily reducible oxides such as Na2O, FeOand MnO; and, (5) difficult to emulsify (high viscosity andinterfacial tension). The development of mold slags that fitthese requirements and can control heat transfer rates in themold within specified limits will be a significant futurechallenge.

5. Conclusion

The solidification of slags is a fascinating area from botha fundamental and practical point of view. In the continuouscasting of steels it is imperative that one fully understandthis complex behavior in order to understand the complexi-ties of heat transfer and lubrication within the mold.

AcknowledgementWithout my ongoing relationship with my collaborators

from Japan, my career could not have been successful. Iwould like to thank all of my friends in Japan for their sup-port over the years. This research was carried out at the Cen-ter for Iron and Steelmaking Research at Carnegie MellonUniversity and I would like to thank Richard Fruehan andthe member companies of the CISR for their support of myresearch in this area. Some of the topics in this paper werealso discussed in the Fruehan Symposium Proceedings,58) apublication to honor Richard Fruehan in 2011.

Fig. 10. The growth rate of precipitated crystals in three differentcalcium aluminate slags as a function of undercooling.59)

Fig. 11. Areas of highest potential dissolution rate based upon theratio of driving force for dissolution reported by Sridhar.63)

J DC

x

C

x= −

∂∂

∝ΔΔμ


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