Article 1

High temperature corrosion performance of FeAl based alloys 2

containing carbon in molten salt 3

Munish Kumar1, Ravi Kant1, S. Chand1, U. Prakash2, S. Sehgal3*, K.K. Saxena4, J.P. Davim5, 4

Chander Prakash6* 5

1 Department of Metallurgical & Materials Engineering, Punjab Engineering College (Deemed to be Univer- 6
sity) Chandigarh, India-160012 7
2 Department of Metallurgical & Materials Engineering, IIT Roorkee, Roorkee, India-247667 8
3 UIET, Panjab University, Chandigarh, India-160014 9
4 Department of Mechanical Engineering, GLA University, Mathura, 281406, India 10
5 Department of Mechanical Engineering, University of Aveiro, Aveiro, Portugal 11
6 School of Mechanical Engineering, Lovely Professional University, Phagwara, India 12
* Correspondence: sehgals@pu.ac.in; chander.mechengg@gmail.com 13

Abstract: The corrosion behaviour of FeAl based alloys containing carbon produced through arc 14
melting in argon atmosphere have been studied in molten salt environment at 500oC to 700oC. The 15
corrosion study was performed in the aggressive environment of molten salts 16
(80%V2O5/20%Na2SO4) by the weight change method. The layer products formed and cross-sec- 17
tional view of tested samples were examined using X-ray diffraction (XRD), scanning electron mi- 18
croscopy (SEM) and energy-dispersive spectroscopy (EDS). The protective Al2O3 layer was identi- 19
fied in the scale for all tested samples. However, Ti addition to FeAl based alloys containing carbon 20
shows sufficient protection at high temperature performance. The microstructural examination re- 21
vealed that FeAl based alloys with Ti addition formed an additional TiO layer which prevents better 22
penetration of corrosive media. The corrosion resistance behaviour of FeAl based alloys with Ti 23
addition were addressed on the basis of microstructural evidences. 24

Citation: Lastname, F.; Lastname, F.;

Keywords: FeAl intermetallic alloys; High temperature corrosion; SEM with EDS; XRD 25
Lastname, F. Title. Metals 2021, 11, x.
26
https://doi.org/10.3390/xxxxx

Academic Editor: Firstname Last-

name 1. Introduction 27
Many industrial components of various engineering systems such as fuel oil and coal 28
Received: date operated at high temperature powder generation devices, aircraft gas turbines, fuel cells 29
Accepted: date etc. fail at high temperatures. The degradation of components occurred by accelerated 30
Published: date
attack due to condensation of films composed of molten salts. Transition metal aluminides 31
such as Fe, Ti, Ni etc. are potentially more suitable alternatives to superalloys at high tem- 32
Publisher’s Note: MDPI stays neu-
perature applications in aggressive environmental conditions [1-3]. These materials show 33
tral with regard to jurisdictional
excellent resistance to corrosion, oxidation, sulfidation and carburizing atmospheres even 34
claims in published maps and institu-
at high temperature due to the formation of stable alumina layer [2, 4]. 35
tional affiliations.
Among these, iron aluminides with higher Al content such as Fe3Al (DO3) and FeAl 36
(B2) due to their low cost, are being possible substitute materials for high temperature 37
applications up to 1000oC in aggressive environment [5-9]. However, iron aluminides 38
Copyright: © 2021 by the authors. have been poorly studied in the environment composed of (Na2SO4-V2O5) molten salt. 39
Submitted for possible open access In the past, Baligidad et al. reported that carbon additions have significantly improved 40
publication under the terms and the strength of Fe3Al based alloys attributed to precipitation hardening due to Fe3AlC0.5 41
conditions of the Creative Commons carbide and interstitial solid solution strengthening [10]. In the similar context, carbon 42
Attribution (CC BY) license addition to FeAl based alloys was tried but graphite precipitation limits further develop- 43
(https://creativecommons.org/license
ment of these alloys [11]. Recently, it was reported that Ti addition together with carbon 44
s/by/4.0/).
additions to FeAl based alloys has successfully developed FeAl based alloys with no 45

Metals 2021, 11, x. https://doi.org/10.3390/xxxxx www.mdpi.com/journal/metals

Metals 2021, 11, x FOR PEER REVIEW 2 of 9

graphite precipitation [12]. Addition of Ti to iron aluminides containing carbon leads to 46

improvement in the mechanical properties [12, 13], but it has been established that Ti 47
could also improve the oxidation and corrosion resistance [14, 15]. Li et. al also found that 48
Ti addition to Fe-36.5Al alloy leads to improvement of oxidation resistance due to com- 49
pactness of oxide scales on the surface which deteriorate the further penetration of corro- 50
sive media [14, 15]. 51
Iron aluminide due to their better oxidation/oxidation resistance at elevated temper- 52
ature, are also considered as replacements of ferritic/austenitic steels for applications up 53
to about 500oC. Among iron aluminides, FeAl based alloys with large amounts of Al (~37 54
at.% or above) are generally considered potential candidate for protection at elevated tem- 55
perature applications [15-17]. Ti additions to FeAl alloys with carbon to enhance its me- 56
chanical properties offers an excellent opportunity to improve its corrosion resistance es- 57
pecially supporting oxide adherence [14]. 58
Unfortunately, the literature on the effect of alloying addition on FeAl based alloys 59
on its corrosion/oxidation behaviour are very limited. Previous studies successfully de- 60
veloped FeAl based alloys containing carbon for wear and high temperature applications. 61
The present study deals with the high temperature corrosion behavior of FeAl alloys con- 62
taining carbon and compare with Ti additions. The Ti additions to FeAl based alloys con- 63
taining carbon helps to improve the corrosion resistance at high temperature. 64
should briefly place the study in a broad context and highlight why it is important. 65
It should define the purpose of the work and its significance. The current state of the re- 66
search field should be carefully reviewed and key publications cited. Please highlight con- 67
troversial and diverging hypotheses when necessary. Finally, briefly mention the main 68
aim of the work and highlight the principal conclusions. As far as possible, please keep 69
the introduction comprehensible to scientists outside your particular field of research. Ref- 70
erences should be numbered in order of appearance and indicated by a numeral or nu- 71
merals in square brackets—e.g., [1] or [2,3], or [4–6]. See the end of the document for fur- 72
ther details on references. 73

2. Materials and Methods 74

Iron aluminides containing carbon with and without Ti addition alloys were pre- 75
pared by arc melting under argon using pure iron (99.0%), pure aluminum (99.99%) and 76
pure titanium (99.9%) powders. Four different alloys with composition (in wt%) Fe-22Al- 77
0.1C (C010T), Fe-22Al-1C (C1T0), Fe-22Al-0.1-1Ti (C01T1) and Fe-22Al-1C-5Ti (C1T5) 78
were produced. All the alloys were homogenized and small piece form each alloy was cut 79
and grounded with emery paper of different grades and finally polished with fine alu- 80
mina powder. The polished specimens were etched with reagent having composition of 81
33% CH3COOH + 33% HNO3 + 33% H2O +1% HF by volume. Microstructural examina- 82
tion was done using electron microscope (FEI Qunta 200 F) and elemental analysis was 83
done by using energy dispersion spectroscopy (EDS). Small sections with size of 84
10x10x20mm were cut from the disc using wire cut EDM for corrosion testing. The speci- 85
mens were then polished with different grade emery papers to finish. Before oxidation 86
tests the specimens were cleaned with acetone and dried. 87
For the hot corrosion testing, the specimens were coated with a very thin film of 88
80%V2O5/20%Na2SO4 salt solution and then exposed to the environment at the desired 89
temperature. The specimens covered with the salt were isothermally heated in furnace, 90
followed by cooling down to room temperature. The corrosion tests were performed at 91
temperatures of 500, 600, and 700oC for 70 h. During the experiment, the specimens were 92
first weighed, put into an alumina crucible and then finally placed in the furnace at the 93
desired temperature. After the regular interval of time, the specimen was left to cool down 94
outside the furnace and then immediately reweighted. The change in the weight of the 95
tested specimens were measured in an electronic balance with an accuracy of 0.1 mg. After 96
the completion of 70 h study, the cross-section of the oxidized surfaces were examined 97
under scanning electron microscope (SEM) to study the mechanism of oxide film. EDS 98
Metals 2021, 11, x FOR PEER REVIEW 3 of 9

analysis was performed to analyze the distribution of various elements across the oxide 99
and substrate interface in oxidized specimens. 100

3. Results and Discussions 101

In C01T0 exhibits the fine carbides particles at the grain boundaries with coarse grain 102
structure. In C1T0 alloy, an uneven distribution of course Fe3AlC0.5 particles with few 103
graphite flakes are observed (Fig 1b). These Fe3AlC0.5 carbides are distributed along the 104
grain boundaries as well as inside the grains. With Ti additions in C01T1 and C1T5 alloys, 105
both TiC and Fe3AlC0.5 carbide particles are observed as shown in Fig. 1c & d respec- 106
tively. No graphite formation is found after Ti additions to FeAl based alloys. Both car- 107
bides are randomly distributed in FeAl matrix and their fractions increase with carbon 108
and Ti contents. 109

110

Figure 1. SEM images of FeAl based alloys a) C01T0 with fine Fe3AlC0.5, b) C1T0 with graphite 111
and coarse Fe3AlC0.5, c) C01T1 with Fe3AlC0.5 and TiC and d) C1T5 with Fe3AlC0.5 and TiC. 112

It has been found that carbon addition lead to Fe3AlC0.5 carbides and interstitial 113
solid solution strengthening observed in EDS analysis (Fig 2a). Higher carbon addition 114
causes graphite precipitation (Fig 1b). Incorporation of Ti eliminates the graphite precipi- 115
tation as evident from the above microstructures (Fig 1d). Further, Ti-content was chosen 116
such that the Ti:C ratios used for C01T1 and C1T5 were more than that for TiC formation. 117
This is due to fact that some part of Ti dissolve in the FeAl matrix. EDS analysis of C1T5 118
alloy, confirms the presence of Ti in the matrix (Fig. 2b). The confirmation of these carbides 119
particles in C01T0 and C1T5 is done by EDS analysis and XRD which were reported else- 120
where [12]. 121
In quaternary Fe-Al-Ti-C system, TiC has large negative free energy of formation [18] 122
and thus, TiC may be precipitate from the supersaturated solution. During solidification, 123
both C and Ti may lose its solubility and therefore, Ti and C lead to formation of TiC 124
particles. The reinforcing components in these alloys are formed through in-situ process 125
by solution precipitation or solid solutionizing mechanism. It has been further observed 126
that TiC bond strength is higher than C-C and Ti-Ti bonds. Thus, the graphite flakes in 127
the alloy may reacts with Ti to form TiC and the residual C utilized to form Fe3AlC0.5 128
carbides. For higher Ti and C contents alloy (C1T5), TiC particles appear to be nucleated 129
adjacent to existing TiC particles resulting agglomeration of TiC particles. This is called 130
sympathetic nucleation and may lead to precipitate at the interphase boundary of already 131
existing precipitate with same phase. This is mainly attributed to lower activation energy 132
barrier for precipitate-precipitate interface than precipitate-matrix interface [19]. 133
Metals 2021, 11, x FOR PEER REVIEW 4 of 9

134

Figure 2. EDS analysis of a) C1T5 with Region-A for needle like Fe3AlC0.5, Region-B for blocky 135
TiC and Region-C for matrix. 136

The specific weight loss as a function of exposure time for FeAl alloys at temperatures 137
of 500oC, 600oC and 700oC, respectively, are shown in Fig. 3. From the figure, it is found 138
that the mass loss increases paralinearly with increasing exposure time for all tempera- 139
tures. The deviations from the parabolic behaviour initially corresponds to existence of 140
growing alumina phase at the time during oxidation process. However, the various types 141
of the behaviours have been noticed during the oxidation kinetics at high temperatures 142
such as, exponential, linear and parabolic behaviour [21]. The parabolic nature of curve is 143
the most commonly kinetics behaviour of the layer products that can cover and shield the 144
entire exposed surface of metallic counterpart [22]. The initial linear behaviour of the ki- 145
netics due to the deposition of oxide layer product on the metallic surface and then re- 146
duced due to decrease in the exposed areas. The mass loss is significantly higher in C01T0 147
and C1T0 (without Ti) than that C01T1 and C1T5 (with Ti) at various temperatures. 148
Among the all alloys, C1T0 with Fe3AlC0.5 carbide shows highest weight loss. This is 149
attributed to coarse and large number of Fe3AlC0.5 carbides as compare to C01T0. A. Raja 150
et al have also reported that the mass loss in iron aluminides was found to be increased 151
with carbon content [20]. The isothermal mass loss at different temperatures are obtained 152
and alloys acquired more mass loss at 700oC than other temperatures. However, both 153
C01T1 and C1T5 (with Ti) shows lower weight loss than their corresponding alloys (C01T0 154
and C1T0). The increase in the slope was low for FeAl alloys containing Ti than their coun- 155
terparts. This decrease in the value of slopes is mainly attributed to the present of small 156
amount of Ti in the matrix. It results in the formation of additional TiO layer which causes 157
the compactness of the oxidized layer and may decrease the further corrosion of the alloy. 158
Based on the microstructural and compositional characterization of different alloys, the 159
process of hot corrosion can be understood. 160
Metals 2021, 11, x FOR PEER REVIEW 5 of 9

161

162

Figure 3. Variation of the weight loss of FeAl based alloys with time at exposure of temperature a) 163
500oC, b) 600oC and c) 700oC (Lines joining the data points are for visual aid only). 164

Figure 4 shows the comparative weight loss of C01T0 and C1T5 at different temper- 165
atures. It is evident from the curve that the weight loss was found to be increased with 166
increasing temperature. This increase in the weight loss of the alloys due to increase in the 167
reaction rate and thus causes higher corrosion of the specimens. It can be seen that the 168
corrosion rate increases with temperature, which indicates the diffusion rate is accelerated 169
to produce the oxide-forming components. It has been found that the higher melting point 170
of the salt may act as barrier to oxidation and limits the diffusion rate at lower tempera- 171
ture. This may lead to reduction of rate of reaction compared to that of metal with no 172
Na2SO4 deposit [23]. In alloy C01T0, the oxide surface was composed of thin, adherent 173
oxide based Al2O3 layer, as evidenced by the cross-section view of the oxidized specimen. 174
On the other hand, oxide surface of C1T5 alloy composed of dense adherent oxides with 175
TiO in addition to Al2O3 layer. The formation of both Al2O3 and TiO oxides layers as 176
oxidation products during hot corrosion, are in agreement with other hot corrosion stud- 177
ies of iron aluminides [14]. The better adhesion of complex oxide formed containing both 178
aluminum and titanium (C1T5) may lead to higher oxidation resistance than pure Al2O3 179
layer as in case of C01T0 alloy. The cross-sectional view of the oxidized specimens further 180
confirms that stable and adhered oxide layer was formed on the surface only. In C01T0 181
and C1T0, the layer was found to be Al-rich scale while in C01T1 and C1T5, an oxide layer 182
of Ti-rich was formed in addition to Al-rich scale. This additional oxide layer containing 183
Ti helps to improve the high temperature oxidation resistance of C1T5 alloy. XRD analysis 184
of oxide layer further confirms the formation of titanium oxide layer in C1T5 (Fig. 6). 185
Metals 2021, 11, x FOR PEER REVIEW 6 of 9

186

Figure 4. Comparative study showing the weight loss of a) C01T0 and b) C1T5 at different temper- 187
atures (Lines joining the data points are for visual aid only). 188

In molten salt (80%V2O5/20%Na2SO4), the corrosion process takes place in two steps 189
i.e. oxidation of the alloy, and then decomposition of the protective oxides deposits which 190
can occurs either by basic or acidic reactions by the molten salt [24]. The reaction occurs 191
may result the formation of oxide film by consumption of oxide ions in the melt and may 192
release the complex ions. Now, in alloy with no titanium, their hot corrosion resistance 193
depends upon the formation of Al2O3 layer on the alloy surface only. But, the present of 194
titanium in the alloy, there is an establishment of additional layer on the alloy surface. 195
This would help to increase the compactness of the oxide layer and thus increases the 196
corrosion resistance of the alloy. Further, more the aluminium (Al) or titanium (Ti) con- 197
tents, thicker would be the oxide layer and thus, corrosion resistance of the alloy im- 198
proved. For alloy without titanium i.e. C01T0 and C1T0 which forms only Al2O3 oxide 199
layer, have lower compactness (Fig 5) and may undergo dissolution of the oxide layer 200
more rapidly at metal/melt interface and thus, leads to more weight loss. On the other 201
hand, Ti-containing alloys more compact and adhere oxide layer is formed which reduces 202
the dissolution rate and thus, decreases the rate of weight loss. 203

204

Figure 5. SEM Micrographs of a) C01T0 and b) C1T5 after oxidation at 700°C/70 h and EDS ele- 205
ments analysis of cross-sections show the presence of Fe, O and Al in C01T0 and Fe, O, Ti and Al 206
in C1T5. 207

The examination of the cross-sectional areas of oxidized specimen exposed the oxide 208
layers were formed on the surface at different temperatures. The microstructures of cross- 209
Metals 2021, 11, x FOR PEER REVIEW 7 of 9

sectional areas show that no penetration to the interior of the specimen was observed. The 210
further confirmation was done by the EDS mapping of element distribution and detailed 211
study on the element analysis of the oxidized layer is shown in Fig. 5. In both the samples, 212
it can be observed that there is reduction in the oxygen content and associated drop in 213
aluminum content during movement from layer to matrix. No iron content was observed 214
in the formed layers and appeared only in the region immediately adjacent to the surface. 215
This clearly indicates that the aluminum ions penetrate the nascent oxide layer, possibly 216
accelerating the formation of Al2O3 layer in both the samples (C01T0 and C1T0). The for- 217
mation of oxide layer is correlated using XRD diffraction pattern as shown in Fig 6. The 218
unidentified peaks in the data may be related to Na2SO4 or complex compounds of V2O5 219
and Na2SO4. 220

221
Figure 6. XRD patterns of oxidized samples. 222

In C1T5 sample (Fig. 5b), the oxide layer shows an extra element corresponding to 223
titanium. At elevated temperature exposure of alloys to oxygen-bearing medium, the alu- 224
minum present in matrix is preferentially oxidized which leads to the formation of alu- 225
mina (Al2O3) layer. But due to thermodynamically possibility, the presence of the iron in 226
the matrix may also lead to formation of iron oxide (Fe2O3) layer. It has been found from 227
the previous studies that major oxidized surface product forms between 500 and 700oC 228
has been reported to be α-Al2O3 [22]. The EDS results also confirm the formation of Al2O3 229
layer in all the samples. This agrees with the observations of others, where it was found 230
that in addition to Al2O3 oxides, as well as other metal oxides. Transient formation of 231
aluminium oxides act as nucleation sites for Al2O3, and titanium present in the matrix 232
leads to the formation of more stable TiO layer. The dense concentration of titanium shows 233
the present of the TiO oxide layer in addition to Al2O3 layer in C1T5 (Fig. 5b). The for- 234
mation of additional TiO layer was also observed in Fe-36.5Al-2Ti alloy as reported else- 235
where [13]. This additional TiO layer leads to better corrosion resistance of Ti containing 236
alloys (C01T1 and C1T5) as compare to without Ti alloy (C01T0 and C1T0) at elevated 237
temperature in molten salt applications. 238
Metals 2021, 11, x FOR PEER REVIEW 8 of 9

5. Conclusions 239
Addition of Ti to iron aluminide containing carbon leads to formation of carbides 240
namely TiC and Fe3AlC0.5. Further, the incorporation of Ti is also found in FeAl matrix 241
leads to refining in the grain of the alloy. The difference between alloys on Ti addition is 242
not only the morphology of surface but also in phases present in the matrix. After corro- 243
sion test, only Al2O3 layer was observed on the surfaces of C01T0 and C1T0, while Ti 244
addition leads to formation of an additional layer of TiO with Al2O3 oxides for C01T1 and 245
C1T5 respectively. Thus, Ti addition to iron aluminides with carbon leads to significantly 246
improvement in the compactness of oxide scales in the surface of FeAl based alloys. The 247
compactness of layer formed shows better protective effect. Further, the better adherence 248
of TiO to the substrate of FeAl alloy makes more difficult of scale spalling. The high tem- 249
perature corrosion behavior of the FeAl based alloys confirms that the Al2O3 and TiO 250
oxide layers play significant role in the corrosion protection in corrosive environment at 251
high temperature applications. 252

Author Contributions: Conceptualization, X.X. and Y.Y.; methodology, X.X.; software, X.X.; valida- 253
tion, X.X., Y.Y. and Z.Z.; formal analysis, X.X.; investigation, X.X.; resources, X.X.; data curation, 254
X.X.; writing—original draft preparation, X.X.; writing—review and editing, X.X.; visualization, 255
X.X.; supervision, X.X.; project administration, X.X.; funding acquisition, Y.Y. All authors have read 256
and agreed to the published version of the manuscript.” Please turn to the CRediT taxonomy for the 257
term explanation. Authorship must be limited to those who have contributed substantially to the 258
work reported. 259

Funding: “This research received no external funding” 260

Data Availability Statement: the study did not report any data. 261

Acknowledgments: In this section, you can acknowledge any support given which is not covered 262
by the author contribution or funding sections. This may include administrative and technical sup- 263
port, or donations in kind (e.g., materials used for experiments). 264

Conflicts of Interest: “The authors declare no conflict of interest. 265

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