Original Research Article

Local composite reinforcements of TiC/FeMn typeobtained in situ in steel castings

E. Olejnik a,b,*, L. Szymanski a,b, T. Tokarski c, B. Opitek a, P. Kurtyka d

a INNERCO Sp. z o.o., 43a Jadwigi Majówny St., 30-298 Krakow, PolandbAGH University of Science and Technology, Faculty of Foundry Engineering, 23 Reymonta St., 30-059 Krakow,PolandcAGH University of Science and Technology, Academic Center of Materials and Nanotechnology, 30 Mickiewicza Av.,30-059 Krakow, PolanddPedagogical University of Cracow, Faculty of Mathematics, Physics and Technical Science, 2 Podchorazych St., 30-048 Krakow, Poland

a r c h i v e s o f c i v i l a n d m e c h a n i c a l e n g i n e e r i n g 1 9 ( 2 0 1 9 ) 9 9 7 – 1 0 0 5

a r t i c l e i n f o

Article history:

Received 19 September 2018

Accepted 12 May 2019

Available online 31 May 2019

Keywords:

Local composite reinforcement

TiC

In situ

Wear resistance

SHS

a b s t r a c t

This dissertation concerns the method of obtaining the in situ local composite reinforce-

ments (LCR – Locally Composite Reinforcement) of the TiC–FeMn type in steel castings. The

reinforcing phase – titanium carbide (TiC) was obtained by placing the pressed substrates of

the synthesis of TiC in the form of compacts into a mold cavity. The basic problem connected

with fabricating TiC local composite reinforcements is the phenomenon of fragmentation. In

order to reduce this phenomenon, a moderator composed of Hadfield steel at 70 and 90% by

weight was introduced to the initial mixture of the TiC substrate powder. As a result,

homogenous and dimensionally stable composite reinforcements of the austenite matrix

were obtained and examined by analyzing their macrostructure, microstructure, structure,

hardness, and wear resistance. An investigation of the phase analysis and microstructure

confirmed the presence of the TiC phase in the structure of the composite zones. The

hardness of the composite reinforcement ranged from 550 HV to 800 HV30 depending on the

proportion between the percentage of the moderator and the content of the pure substrates

of the synthesis reaction of the TiC.

© 2019 Politechnika Wroclawska. Published by Elsevier B.V. All rights reserved.

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1. Introduction

Statistical data shows that about 80% of machine and devicefailures are caused by surface wear due to parts rubbingagainst each other or hydrogen degradation [1]. Abrasive wear

* Corresponding author.E-mail address: eolejnik@agh.edu.pl (E. Olejnik).

https://doi.org/10.1016/j.acme.2019.05.0041644-9665/© 2019 Politechnika Wroclawska. Published by Elsevier B.V

is a costly and serious problem in the mining and mineralprocessing industries [2]. As a consequence, it is necessary todesign materials that offer an attractive combination of priceand industrial output. A couple of good examples are the exsitu and in situ methods of fabricating local compositereinforcements in castings [3]. Metal matrix composites have

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recently become the subject of much research thanks to thepossibility of obtaining a good combination of increased wearresistance and robust strength properties [4]. Additionally,MMCs are characterized by attractive thermal and electricalcharacteristics, which allows them to be considered in theestablished material technology [5]. Aluminum and magne-sium metal matrix composites are characterized by their goodcombinations of mechanical properties and low weights [6].Although most of the research focuses on MMCs that are basedon the matrix that constitutes lightweight metals, there is alsoconsiderable interest in developing iron and steel matrixcomposites [7]. An analysis of the literature indicates thatMMCs based on selected types of steel or iron have broadapplications in the mechanical, mining, chemical, andprocessing industries due to their excellent wear and corrosionresistance [8]. Additionally, alloys based on Fe are commonlyused as the base matrix in MMCs (metal matrix composites) onaccount of their low costs and good mechanical properties [9].The most common ceramic materials used to reinforce varioustypes of Fe alloys are Al2O3, ZrO2, TiN, B4C, WC, and VC [10];however, TiC constitutes the most popular reinforcingparticulate phase on account of its low density, robusthardness, high melting temperature, thermodynamic stabili-ty, wettability, and wear resistance [11,12]. Self-propagatinghigh-temperature synthesis (SHS) has been presented in manyarticles as one of the best methods for obtaining MMCs due toits low energy consumption, increased time efficiency, andhigh product purity; however, the final products are charac-terized by high porosity. Hence, the connection of the SHSreaction and casting process can be a good way to produceceramic particles reinforced with matrix composites based oniron and steel [13]. This connection allows us to eliminate thehigh porosity, agglomeration of the TiC particles, andcontamination of the interface between the reinforcementsand the matrix [14]. Furthermore, the in situ fabricated phasereinforcement (TiC) is well-bonded with the metallic matrix asa result of the infiltration process of the chain containing theTiC substrates throughout the liquid metal [15]. Over the lastdecade, many groups of scientists have presented the resultsof their research in the area of obtaining TiC–Fe composite-type alloys. Their research methods were generally inagreement and usually involved placing packets containingthe pure substrates of TiC or substrate carriers in the moldcavity and initiating the synthesis reaction under the influenceof high temperatures. Jiang et al. [16] prepared the preformfrom a mixture of such powders as Ni, C, and Ti. After thepressing process, the readied green compacts were placed inthe sand mold before the casting process. In the next part ofthe process, the liquid steel was poured into the mold cavity,where the synthesis reaction of the TiC was initiated by theheat of the [16]. Hu et al. [17] and Feng et al. [18] presented asimilar method of producing a local composite reinforcement.The authors produced their green compacts based on pure Tior ferroalloys containing high amounts of titanium (ferrotita-nium) and carbon, which were then mounted inside their sandmolds. In a further step in their experiments, the ferrous alloywas poured into the mold cavity to ignite the combustionreaction. After the solidification process, the composite zonereinforced by TiC was formed in both cases [17,18]. Themajority of the above authors did not describe their methods

of taking their samples from their readied castings but onlystated the presence of a local composite reinforcementfabricated in situ. Wang et al. presented the scheme of areactive infiltration process where the compacts were sus-pended and moved to the upper part of the mold cavity afterthe synthesis reaction due to the differences in density. Afterthe solidification process, the samples were taken from theselected part of the mold cavity known as the feeder [19]. It cantherefore be assumed that the MMCs produced by the reactiveinfiltration method in the above works were a result of thesuspension of the crystallized particles in the metal matrix, sothe obtained materials can be treated as composites that arereinforced by volume. However, no description of theirmacrostructure can be found in the subject literature, whichseems to be essential regarding the industrial application ofMMCs.

The reaction of TiC synthesis is highly exothermic (asconfirmed by Merzhanov's research) [20]. In his work,Merzhanov determined the enthalpy of the TiC formation(which amounted to �187 kJ/mol). Intensive energy produc-tion in the form of the generated heat results in the localincrease of the temperature of the liquid metal, significantlyintensifying the phenomenon of infiltration within the localcomposite reinforcement. The composite zone is separatedinto parts that move within the casting mold due to their lowerdensity and convective motion. This phenomenon is calledcomposite zone fragmentation. Accordingly, it is difficult tofind any research in the literature that presents the macro-structure of composite casting based on Fe alloys reinforced byTiC.

The main goal of our research was to manufacture a localcomposite reinforcement in a steel casting. The reinforcingphase in the form of TiC was fabricated in situ during themetallurgical process. Due to the exothermic reaction of theTiC, a moderator was introduced to the initial mixture of thepowders. In this way, the authors lowered the temperaturelocally within the composite zone, which helped us obtain adimensionally stable local composite reinforcement in thesteel casting. The addition of a moderator eliminated theunfavorable phenomenon of fragmentation caused by reactiveinfiltration [21,22].

2. Materials and method

The mixture of the substrates that was essential for carryingout the synthesis in situ of the TiC in the casting alloy wasprepared with an atomic ratio of 1:1. In order to do this,titanium powder with a purity of above 99.95% and an averagediameter of 45 mm (manufactured by ‘‘Stanchem,’’ Poland) andflake graphite with a purity of above 96% and average diameterof 5 mm (manufactured by ‘‘Sinograf,’’ Poland) were used.

In order to control the process of reactive infiltration duringthe high exothermic reaction into the mixture of thesubstrates of the synthesis reaction of the TiC, a moderatorwas introduced that was composed of Hadfield steel 70 and90% by weight. The chemical composition of the compacts andthe moderator used for the synthesis reaction of the localcomposite reinforcements in the steel casting are shown inTable 1.

Table 1 – Chemical composition: compacts used forsynthesis reaction in situ LCR and moderator (Hadfieldsteel).

Symbol Percentage of substrates insynthesis reaction of

TiC (wt.%)

Percentage ofmoderator (wt.%)

A 30 70B 10 90

Chemical composition of moderator (wt. %)

C Mn Si Fe

1.2 21 0.5 Residual

Table 2 – Chemical composition of base alloy (wt.%).

Chemical composition (wt.%)

C Mn Cr Si Fe

0.4 1.4 0.3 0.8 Residual

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The powder of the substrates of the TiC and the moderatorwere subjected to mixing without air for 6 h. Next, a so-prepared surplus weight of 170 g was cold-pressed in auniaxial hydraulic press under a pressure of 550 MPa. Theobtained 15 mm � 15 mm � 50 mm compacts were placed intothe mold cavity according to the diagram presented in Fig. 1.The cavity was poured with cast steel L35GSM (the chemicalcomposition of which is given in Table 2). The pouringtemperature amounted to 1625 8C.

The readied cast product was cut into pieces in order to takesamples containing composite zones with 70 and 90% of themoderator and base alloy by weight. The sample was subjectedto grinding and polishing before it was investigated inmetallographic, structural, and mechanical test examinations.The metallographic examinations were carried out with theapplication of scanning electron microscopy (SEM), using a FEIVersa 3D microscope and BSE detector. The surface fraction ofthe reinforcement phase in the ‘‘Image J’’ program is specifiedon the basis of the differences in contrast between the phasesthat can be found in the microstructure and are automaticallydetermined by the software. The diameter of the TiC particleswas determined by using Olympus Basic Stream software. Thephase analysis within the region of the composite zone wasperformed by means of the X-ray diffraction method. Theanalysis was carried out with the use of a Siemens Kristalloflex4 Hz applying the following parameters: X-radiation with CuKa – 0.154 nm, a voltage of 30 kV, and an intensity of 26 mA.The hardness was measured by applying the Vickers method

Fig. 1 – Diagram of mold cavity with compacts mounted

using a load of 294.8 (HV30) and a 10-s duration. The deviceused for the measurements was a United Test hardness tester.The abrasive wear resistance was tested using the ball-on-discmethod by means of an Ebit tribotester coupled with acomputer – the friction couple: the composite zone and anabrasive ball made of Al2O3. The process parameters were asfollows: a corundum ball diameter of 3 mm, a friction radius ofca. 3 mm, a disc rotational speed of 192 rpm, a loading of 10 N,and a friction path of 503 m.

3. Results and discussion

3.1. Macrostructure

Fig. 2a demonstrates the macrostructure of the steel castingwith the TiC–FeMn local composite reinforcement type.Introducing the moderator allowed us to obtain homogenousand dimensionally stable composite reinforcement. Fig. 2bpresents a cross-section of the casting from which the sampleswere taken for the structural and mechanical tests. Anevaluation of the macrostructure of the casting shows nodefects in the transition area between the composite zone andbase alloy.

3.2. Phase analysis

Fig. 3 presents the results of the phase analysis (XRD) carriedout in the LCR A and LCR B zones. The diffractogramsdemonstrate the peaks made by the crystallographic planesof the TiC, which proves the synthesis reaction of the TiCin situ into the mold cavity during the metallurgical process.The intensities of these peaks are higher than in the case ofLCR A, which is related to the difference in the percentage ofpure substrates of the reaction of the 30%-by-weight TiC.

for synthesis reaction in situ of composite zones.

Fig. 2 – (a) Macrostructure of casting with local composite reinforcement and (b) cross-section of casting with local compositereinforcement.

Fig. 3 – Phase analysis (XRD) of A and B zones manufactured in situ in steel casting.

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Reflections from the phase Fea-ferrite are visible in both theLCR A and LCR B structures. This phenomenon is evidence ofthe reactive infiltration through the liquid base alloy in thecompacts, which is characterized by a ferritic matrix. Therelative height of the peaks from the Fea is higher for the LCR Azone. This confirms the fact that the process of reactiveinfiltration is limited with the growth in the moderator'spercentage, which contributes to the stabilization of thedimension of composite reinforcement. In turn, the intensityof the peaks from the Feg phase is significantly higher for LCRB. It is connected with the introduction of the moderator (the

Hadfield steel, which is characterized by an austenitestructure) to the initial mixture of the powder. The presenceof Feg proves that the degree of infiltration is lower, as the Feaphase participation is lower.

3.3. Microstructure

Fig. 4A and B illustrates the transition area between thecomposite reinforcement and the casting core in LCR A and B,respectively. In both cases, it can be agreed that the boardingarea is relatively even. In the case of LCR A, we can observe

Fig. 4 – (A and B) SEM BSE microstructures of transitionareas between A and B zones and cast steel casting core;(A.1–B.3) SEM BSE microstructures of A and B zonesobtained in situ in steel casting.

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local separations by the base alloy in the composite zone. Thiseffect is related to the high exothermic reaction synthesis ofthe TiC. On the other hand, the area the transition areabetween LCR B and the base alloy is more continuous onaccount of the increased amount of the moderator (whichstabilized the process of the synthesis of the TiC). Fig. 4A.1–A.3and B.1–B.3 presents the microstructure of in situ fabricatedcomposite reinforcements A and B in which the dark sections

Fig. 5 – Surface fractions of porosity, TiC, and mat

of the TiC are visible against the background of the lightmatrix. The analyzed microstructures are characterized byareas in which freely scattered agglomerates of the sphericalparticles of the TiC can be found. The in situ fabricated phasereinforcement (TiC) is well-bonded with the metallic matrix,and the transition area remains free of impurities. LCR A has a34% reinforcing phase, which is 13% more when compared toLCR B. The model microstructures (with the outlined surfacefraction of porosity, phase reinforcement, and matrix) aredemonstrated in Figs. 5 and 6. This was confirmed by aninvestigation of the phase analysis. The introduction of themoderator is connected with the reduction of pure substratesof the TiC; in effect, a lower surface average of the ceramicphase can be observed. It should be noted that, by introducingthe moderator in the form of a powder mixture of the specificchemical composition, the properties of the compositereinforcement matrix can be shaped. Applying a moderatorcomposed of high-manganese steel can increase the plasticityof the composite reinforcement.

The nucleation rate and the rate of growth of the nucleationagents directly depend on the degree of undercooling, whichaffects the size and number of the particles. At the beginning ofthe process, the aforementioned values increase with thedegree of undercooling; however, the nucleation rate is higherthan the rate of growth of the nucleation agents. As aconsequence, the grains after crystallization become finerwith the growth of the degree of undercooling (Fig. 7).Introducing the moderator as a synthesis reaction stabilizeraffects the nucleation process and growth of the reinforcingphase through the considerable lowering of the temperature inthe reaction area. In the described experiment, this increasesalong with the percentage of the moderator composed ofHadfield steel. Lowering the percentage of the pure substratescontributes to the lowering of the emitted energy during TiCsynthesis; this contributes to the increase in the degree ofundercooling. The confirmation of the demonstrated crystal-lization scheme can be seen in the results shown in Fig. 8. Thesizes of the particles are smaller in Composite Area B with thehigher content of the moderator.

rix within regions of LCR A and LCR B zones.

Fig. 6 – Microstructures of outlined surface fractions (in red) for in situ LCR A (A–A.3) and LCR B (B–B.3) composite zones.

Fig. 7 – Dependence of nucleation rate and rate of growth of nucleation agents on degree of supercooling.

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Fig. 8 – Size distribution of TiC particles fabricated in situ (a) LCRA and (b) LCRB.

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Figs. 9 and 10 present maps of the element distribution: C,Si, Ti, Mn, and Fe for the fabricated in situ compositereinforcements with the different percentages of the modera-tor. The relative Ti and C concentrations as TiC substrates arehigher in the case of the maps of Composite Reinforcement A.However, special attention should be paid to the fractions ofMn and Fe. The applied base alloy was characterized by arelatively low content of Mn, which was the main chemicalelement of the introduced moderator. On the basis of amicrostructural examination, the transition area between thecomposite zone and base alloy was evaluated to be highlystable. This indicates the minimal degree of infiltration of thein situ-fabricated composite reinforcement by the base alloy.Therefore, special attention should be paid to the concentra-tion of Mn and Fe that is visible on the maps of the elements of

Fig. 9 – SEM-image and distribution maps of chemical elementsmapping; (c) Si mapping; (d) Ti mapping; (e) Mn mapping; (f) Fe

Composite Reinforcement B (which is much higher than thatof Composite Reinforcement A). This stems from the fact thatthe application of the Hadfield steel moderator has a lessimportant influence on the microstructure and limits thephenomenon of reactive infiltration.

3.4. Hardness and wear resistance

Fig. 11a shows a graph that illustrates the hardness in the areaof the base alloy and composite reinforcement. It can beobserved that there is a distinct increase in hardness in theLCR zone containing particles of the TiC phase as compared tothe base alloy (ranging from 200 to 300 HV). The averagehardness of LCR A and LCR B amounts to 785 and 580 HV30,respectively. This is related to the greater surface average of

in area of LCR A: (a) selected area on the sample; (b) Cmapping.

Fig. 10 – SEM-image and distribution maps of chemical elements in area of LCR B: (a) selected area on the sample; (b) Cmapping; (c) Si mapping; (d) Ti mapping; (e) Mn mapping; (f) Fe mapping.

Fig. 11 – (a) Vickers hardness HV30 of LCR A and B as well as base alloy and (b) wear rate indexes of base alloy, LCRs A and B,and reference material.

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the TiC and the necking of the particles of TiC (which affectsthe stiffness of the composite). The matrix of the LCR iscomposed of Hadfield steel, which is characterized by anaustenite structure. Therefore, using this material in applica-tions that work under conditions of high abrasive wear anddynamic loading can cause an additional increase in themechanical and usable properties. This stems from the factthat this material has a tendency to self-harden when exposedto heavy dynamic loading and cold work. As a result, we canobserve the phenomenon of twinning in the microstructure.

Fig. 11b demonstrates the wear resistance of the base alloy,both LCRs, and the reference material (Hadfield steel) as-castand after hardening. The L35GSM steel has the highest wearvolume index (803.9 � 10�6 mm3/Nm), which is countedamong the group of materials with a high resistance to wear.

In situ-fabricated Composite Reinforcements A and B werecharacterized by greater wear resistance when compared tothe base alloy. Application of the moderator composed ofHadfield steel in powder form obtains homogenous compositereinforcements and limits the process of infiltration. LCR Aand B show wear volume indexes of 15.30 � 10�6 mm3/Nm and48.81 � 10�6 mm3/Nm, respectively (which were both severaldozen times lower than in the base alloy). The differences inthe values of the wear indexes between the zones come fromthe surface average and reinforcing phase of the TiC. Theresults confirm the research done on the microstructure aswell as the phase and hardness analyses.

Composite Reinforcement A is characterized by a consid-erably lower wear volume as compared to the Hadfield steelused for manufacturing machinery elements that are exposed

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to severe abrasive wear conditions. The obtained resultssuggest that introducing pure TiC substrates at 10% by weightresults in a considerable improvement in the casting'sfunctional properties. The as-cast Hadfield steel has a wearvolume that is more than 50 times greater than CompositeReinforcement B that contains the moderator at 90% by weightin its chemical composition.

4. Conclusion

Local composite reinforcements in steel casting were obtainedin the in situ synthesis reaction of TiC as a result of the processtaking place directly in the mold cavity. The addition of themoderator (70 and 90% by weight) enabled us to obtainhomogenous and dimensionally stable composite reinforce-ments. The microstructural investigation indicated that thetransition area between the composite zone and base alloywas more stable for LCR B. This result was associated with thehigher content of the moderator in the initial mixture of thepowders, which lowered the enthalpy of the synthesis reactionof the TiC. A phase analysis showed the presence of TiC in thestructure. The peaks originating from the TiC planes had ahigher intensity in LCR A (which contained 30% of the puresubstrates of the synthesis reaction of the TiC). The addition ofthe moderator with the chemical composition of Hadfield steelgreatly influenced the microstructure of the composite zone,which was manifested by the presence of Fey peaks. Theaverage size of the TiC particles decreased with increasingpercentages of the moderator (which decreased the degree ofundercooling). The carried-out mechanical investigationrevealed a growth in the hardness of the composite zone thatwas several hundred times greater when compared to the basealloy. Due to the higher percentage of the pure substrates ofthe TiC, LCR A showed a nearly 30% increase in hardness. Inthe area of the highest concentration of TiC, the local hardnessachieved a value of nearly 900 HV30. The obtained compositezones were characterized by a significantly lower wear ratewhen compared to the base alloy and reference materials(Hadfield steel).

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