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The Effect of Nb and Ti on Structure and Mechanical Properties of 12Ni-25Cr-

0.4C Austenitic Heat-Resistant Steel after Aging at 900 °C for 1000 h

Article  in  Journal of Materials Engineering and Performance · July 2014

DOI: 10.1007/s11665-014-1009-5

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The Effect of Nb and Ti on Structure and Mechanical

Properties of 12Ni-25Cr-0.4C Austenitic Heat-Resistant
Steel after Aging at 900 C for 1000 h
Vahid Javaheri, Farzad Shahri, Mahyar Mohammadnezhad, Morteza Tamizifar, and Masaab Naseri

(Submitted June 9, 2013; in revised form March 18, 2014)

Austenitic heat-resistant steels are particularly suitable for applications where service conditions comprise
high temperature. The demand for better performance has motivated developments in these steels. In this
work, Ti and Nb were added to austenitic heat-resistant steels, Fe-12Ni-25Cr-0.4C, wt.% simultaneously.
Microstructural changes were studied via scanning electron microscopy equipped with energy dispersive
spectrum (EDS), optical microscopy, and x-ray diffraction (XRD) in as-cast condition and after aging in
900 °C for 1000 h. Mechanical properties were measured using tensile tests, impact energy, and Vickers
hardness. It was observed that by formation of NbC and TiC, the level of fragmentation of the chromium
carbides increased, as a positive aspect for mechanical properties. XRD and EDS results show increasing
the amount of Ti can inhibit G-phase transformation.

years, research interest has been focused on a large group of

Keywords aging, chromium carbide, heat-resistant steel,
microstructural evolution alloying elements such as Ti (Ref 4), Mn (Ref 5), Cu (Ref 6), Zr
(Ref 7, 8), Yt (Ref 1, 9), Nb (Ref 10), Al, and Si (Ref 11) etc.
These elements are added to the cast steel separately or jointly
in amounts varying from a few tenths of a percent to several
percentages. For example, Zhang et al. (Ref 12) reported the
1. Introduction effect of titanium and tungsten on the structure and properties
of Fe-9Ni-29Cr-0.35C heat-abrasion resistant steel. Piekarski
(Ref 13) also studied the effect of Nb and Ti additions on
Austenitic heat-resistant steels play an important role in high
microstructure, and identification of precipitates in stabilized
temperature structural applications (Ref 1). One of the most
Fe-30Ni-18Cr-0.30C cast austenitic steels. Latha et al. (Ref 4)
popular austenitic heat-resistant steels is Fe-12Ni-25Cr-0.4C,
reported the effect of titanium on the creep deformation
wt.% which has widespread uses in the cement and mine
behavior of 14Cr-15Ni-Ti stainless steel.
industry and in metallurgical furnaces. This alloy has a high
In austenitic heat-resistant steels, Nb reacts with carbon
strength and excellent resistance against oxidation at tempera-
resulting in NbC thereby hindering the precipitation of
tures up to 1100 C; therefore, it has many applications (Ref 2).
chromium carbides and improving the mechanical properties
Although this steel is designed for use at elevated temperatures,
(Ref 10). During aging, transformation of primary Nb carbide
metallurgical degradation may occur after long time service
to a NiNb silicide (G phase) was reported. In modified alloys,
exposure above 800 C, potentially resulting in embrittlement.
the G-phase transformation has a strong influence on the
The embrittlement is associated with a change in the nature of
mechanical properties. As an opposite effect, Ti is reported to
precipitates in the interdendritic areas of the cast structure
be an inhibitor to the G-phase transformation (Ref 14).
during extended service (Ref 3). Therefore, research interest to
Considering the fact that no systematic work has been
enhance the performance characteristics of austenitic heat-
performed to study the effects of Nb and Ti on properties of
resistant steels is still going on. A typical approach used in
Fe-12Ni-25Cr-0.4C, in the present study, various percentages
industries for many years is the addition of alloying elements to
of Nb and Ti were added to this alloy. The effects of Nb and Ti
modify the microstructure and mechanical properties. In recent
addition on the microstructure and mechanical properties in
as-cast and after aging condition were investigated.
Vahid Javaheri, Department of Material Engineering, Iran University
of Industries and Mines, 87145-25564 Tehran, Iran; and Research and
Development Department, Isfahan Casting Industries (ICI), Isfahan,
Iran; Farzad Shahri, Department of Advanced Materials and
Renewable Energy, Iranian Research Organization for Science and 2. Experimental
Technology (IROST), Tehran, Iran; Mahyar Mohammadnezhad,
Department of Materials Science and Engineering, Islamic Azad In this study, austenitic heat-resistant steel (Fe-25%Cr-
University Najafabad Branch, 85141-43131 Najafabad, Iran; Morteza
Tamizifar, Department of Materials Science and Engineering, Iran
12%Ni-0.4%C) without and with different amounts of niobium
University of Science and Technology, Tehran, Iran; and Masaab (Nb) and titanium (Ti) addition were prepared in a 400 kg
Naseri, Research and Development Department, Isfahan Casting medium frequency induction furnace with acidic lining. The
Industries (ICI), Isfahan, Iran. Contact e-mail: vahidjavaheri@ gmail.com. melting temperature was about 1550 C and alloys were cast

Journal of Materials Engineering and Performance

into CO2-silicate molds. The size of the specimen was
200 mm 9 200 mm 9 300 mm. The chemical compositions of
the alloys are presented in Table 1. Samples were aged at
900 C (as the normal operating temperature of this steel) for
1000 h in the ambient atmosphere. The phase transformation
was specified by x-ray diffraction (XRD; Philips XÕPERT
MPD) using filtered Cu Ka radiation (k = 0.1542 nm) at 40 kV
with a step size of 0.05 over the wide angle range of 0-100
2h. The microstructures of the alloys were characterized using
the Olympus optical microscope (OM) and scanning electron
microscopy (SEM) in a Philips XL30 at an accelerating voltage
of 20 kV equipped with an energy dispersive x-ray spectrom-
eter (EDS). Metallography samples (15 9 15 9 10 mm) for OM
and SEM observations were etched with Marbel etchant (10 g
CuSO4 + 50 mL HCl + 50 mL H2O). The volume fraction of
carbides and average carbide diameter (D) were calculated by
using the Clemex V3.2 (Image analysis software) from eight
OM images of each alloy (randomly selected) at magnification
of 1009.
Mechanical properties have also been determined according
to standard ASTM-A370.
Tensile test was performed by the servo-hydraulic test
machine without any protective atmosphere on the round bar
sample at both room and 900 C temperature. Impact test was
carried out on the Charpy V-notch specimens. Moreover, the
effects of aging time (0, 10, 100, 200, 400, 600, 800, and
1000 h) on the hardness were evaluated by the Vickers method
(load of 100 N).
3. Result and Discussion
3.1 Microstructures
Figure 1 shows the microstructure of the alloys in the
as-cast condition. The microstructures comprise the austenitic
matrix and primary different type of carbides such as chromium
and niobium, titanium, or mixed carbides at the grain
boundaries and in the interdendritic regions (Ref 15-17). In
addition, increasing the combined content of modifying
additives (Ti, Nb) significantly influences the refinement of
carbides changing their morphology (Ref 13). More details of
structures evaluation of alloys are presented elsewhere. Car-
bides are formed in steels only by iron and metals that stand to
the left of iron (transition metals) in the periodic table, so Nb
and Ti are stronger carbide-forming elements in comparison to
chromium (Ref 18). Figure 2 demonstrates the image analysis
results. It can be seen that by the increasing the amount of
niobium and titanium, the volume fraction of primary chro-
mium carbides decreased because Nb and Ti additions pro-
moted a partial replacement of the primary chromium carbide
with MC (M = Nb or Ti) and promoted also a fragmentation of
the carbide network and decreased the average carbide diameter
(Ref 10).
Table 1 Chemical composition of all specimens (wt.%)
Sample no. C Si Mn Cr
1 0.37 1.91 1.27 25.40
2 0.42 1.83 1.28 25.30
3 0.39 1.96 1.21 24.90
4 0.40 2.01 1.25 25.60
Figure 3 shows the microstructure of the alloys after aging
at 900 C for 1000 h. A fine secondary chromium carbide
precipitation can be observed in addition to the primary phase
coarsening. This secondary precipitation is also observed at the
resolution of the SEM. Moreover, it illustrates that the primary
carbides after aging in alloy 1 are more coarsened. Generally,
comparison between microstructures of alloys before and after
aging dedicates two main events in the structure as a result of
service for a long time. A coarsening of primary chromium
carbides and the secondary carbide precipitates can be distin-
guished in the austenitic matrix and along the grain boundaries.
The SEM microstructure of the alloy1 before and after aging
is observed in Fig. 4. It can be seen that the secondary
precipitates and the Cr-rich carbides coarsened significantly.
The carbides became large and blocky exhibiting a larger area
fraction in the matrix compared to the as-cast condition. It has
been reported that these carbides were in the form of Cr23C6 or
Cr7C3 (Ref 7, 13).
Figure 5 shows the SEM microstructure of alloy 2 before
aging which indicates the primary carbides have two different
types identified by their tonality. The spectra taken by EDS
analysis show that the dark regions are chromium and iron rich,
and the white regions are niobium and titanium rich, probably
MC (where M is Nb/Ti) (Ref 10, 17). Moreover, for better
understanding of elemental distribution, x-ray micro analysis was
carried out. The elements C, Cr, Fe, Mn, Nb, Ni, Si, and Ti were
chosen for analysis. Figure 6 shows the distribution of analyzed
elements of alloy 2 in as-cast condition. Titanium- and niobium-
rich regions are approximately close together. Probably, addition
of titanium and niobium jointly causes the formation of mixed
niobium-titanium carbides with variable properties of Nb and Ti.
Alloy 2 after aging developed extensive secondary precip-
itation of the M23C6 type and some needlelike precipitates were
also observed and identified by SEM/EDS analysis as a (Nb/Ti)
C phase (Fig. 7). SEM image shows that most precipitates have
been formed from two parts. Primary precipitates and second-
ary carbides. Secondary precipitates of chromium carbides are
formed in the temperature range of about 600-900 C. These
carbides are not stable at higher temperatures (Ref 19). It seems
that the presence of niobium and titanium simultaneously
stabilized them during aging.
Niobium is one of the main modification elements in heat-
resistant steels. It is acknowledged that niobium promotes the
carbide network refinement and the homogeneous distribution
of MC phase. However, in heat-resistant austenitic alloys
during aging transformation of primary Nb carbide to a
undesirable phase rich in silicon, nickel, and niobium that has
been named as ÔÔGÕÕ phase and the formula of Ni16Nb6Si7 were
reported (Ref 1, 7, 13). In contrast, as an opposite effect, Ti is
reported to be an inhibitor to the G-phase transformation in
these alloys (Ref 14). Figure 8 shows the SEM microstructure
of alloy 3, in which a phase enriched in Nb, Ni, and Si was
detected. It seems that this alloy exhibited partial transforma-
tion of NbC to G phase. It revealed the formation of G-phase
Mo Ni Co Cu Nb Ti
0.26 12.90 0.14 0.31 … …
0.25 13.00 0.10 0.18 0.46 0.19
0.30 13.10 0.10 0.31 0.72 0.19
0.27 12.70 0.10 0.27 0.70 0.30
Journal of Materials Engineering and Performance
Fig. 1 Optical microstructures of the alloys before aging condition
Fig. 2 Variation of the carbide volume fraction and average of carbide diameter for the different alloys
particle (identified as point 2) adjacent to chromium carbides
(identified as point 1).
Figure 9a shows the XRD pattern for alloy 1 after aging.
The crystalline austenite- and chromium-rich carbides are
observed. Figure 9b shows XRD patterns for all alloys after
aging with the slower scan rate under step size of 0.01 between
55 and 58 for detection of G phase. As it is illustrated, in
alloy 2, the G-phase diffraction peaks were observed in Nb
presence, which confirms the transformation of NbC to G
phase. According to cubic FCC structure of G phase and
BraggÕs law; the lattice parameter of G phase can be calculated
based on sin2h = (k2/4a) (h2 + k2 + l2) equation. Using h from
Journal of Materials Engineering and Performance
the diffraction pattern (2h  56.45 and 2h  57.40) and a graph
of (4sin2h)/k2 versus h2 + k2 + l2, the unit cell length can be
calculated from the slope, which is 1/a2. Therefore, measured
lattice parameter was obtained 1.18 nm. Moreover, with an
increase in the Nb percent in alloy 3 compared to alloy 2, the
intensity of G phase peaks increased. With an increase in the Ti
amount in alloy 4, the peaks of G phase were totally removed.
3.2 Thermodynamic of Formation Carbides
Titanium (Ref 20) and niobium (Ref 21), two of the stronger
carbide-forming elements, are widely used in iron and steel
Fig. 3 Optical microstructures of the alloys after aging condition
Fig. 4 SEM microstructure of alloy 1; (a) before aging and (b) after aging condition
industries as effective alloying elements for partitioning to the
matrix as well as modification of carbide (Ref 22). From OM
and SEM microstructures of all alloys, it can be seen that the
carbides and, in particular, the primary carbides are refined
gradually with an increase in Ti and Nb concentration. In the
present study, all the alloys were solidified at the same rate and
the differences observed are attributed to the effect of titanium
and niobium. Such differences are due to the precipitation of
TiC and NbC prior to primary chromium carbides. The
formation of these carbides consumes part of the carbon
present in the alloy so that the volume of chromium carbides is
diminished. The blow thermodynamic results indicate that TiC
and NbC particles form before the precipitation of primary
chromium carbides. Moreover, the formation of the first
precipitated TiC and NbC depletes certain carbon, thus
reducing the volume fraction of chromium carbides. On the
other hand, TiC and NbC act as effective heterogeneous nuclei
of chromium carbide because these carbides can act as the
substrate for the heterogeneous nucleation of chromium carbide
in steel.
Journal of Materials Engineering and Performance
Fig. 5 SEM microstructure and EDS pattern of alloy 2 before aging condition

Fig. 6 Elemental map and distribution of major elements in alloy 2

The standard free energy change for each reaction DG0f is
related to the standard enthalpy change (DH0f ) and the standard
entropy change (DS0f ) by the following equation:
DG0f ¼ DHf0  T DSf0 (Ref 23).
Only one carbide of Ti is known to exist, (Ref 23-25) TiC
(melting point 3340 K). Richardson (Ref 23-26) first time
reported the Gibbs energy of formation of TiC corresponding to
the reaction Ti + C fi TiC to be:

Journal of Materials Engineering and Performance

 DG0f (TiC) = 44,600 + 3.16T Cal/mole (±3000 Cal) in the DG0f (NbC) = 31,100 + 0.4T Cal/mole (±600 Cal) for the
temperature range 1150-2000 K. temperature range 1180-1370 K and for reaction
Moreover, two carbides of Nb have been identified: Nb2C 2Nb + C fi Nb2C:
(melting point 2777 K) and NbC (melting point 3881 K). DG0f (Nb2C) = 46,000 + 1.0T Cal/mole (±900 Cal) for
Previous research (Ref 23) determined the DG0f (NbC) for the the same temperature range (Ref 23).
reaction Nb + C fi NbC: Finally, three carbides of Cr have been reported (Ref 27):
Cr23C6 (melting point 1848 K), Cr7C3 (melting point 2038 K),
and Cr3C2 (melting point 2083 K). Measured DG0f for reaction
23 1
6 Cr + C fi 6 Cr23C6 is:
0
DGf (Cr23C6) = 12,833  3.05T Cal/mole (±1200 Cal)
7
for the temperature range 1150-1300 K, for reaction 27
23
Cr23C6 + C fi 7 Cr7C3 is:
DG0f (Cr7C3) = 29,985  7.41T Cal/mole (±400 Cal) for
the temperature range 1100-1720 K and for reaction 35
Cr7C3 + C fi 75 Cr3C2 is:
DG0f (Cr2C3) = 9840  2.64T Cal/mole (±400 Cal) for the
temperature range 1300-1500 K.

3.3 Mechanical Properties

The result of the variation of the mechanical properties
including the tensile test and impact energy at temperature are
presented in Fig. 10. From given data, it is observed that by
increasing the content of niobium and titanium, tensile strength,
and yield strength at room temperature were increased, but
there were not many variations in impact energy and
Fig. 7 SEM microstructure of alloy 2 after aging condition elongation.

Fig. 8 SEM microstructure and EDS pattern of alloy 3 after aging condition

Journal of Materials Engineering and Performance

Fig. 9 X-ray diffraction results of (a) alloys 1, 3 and (b) all specimens after aging condition
Fig. 10 Variation of mechanical properties of the alloys before
aging condition at room temperature
Nb and Ti addition promote a partial replacement of the
primary chromium carbide and also a fragmentation of the
carbide network. That is the most important mechanism for
increasing the tensile strength in modified alloys with niobium
and titanium (Ref 18).
Figures 11, 12 show the mechanical properties of alloys
after aging in both room and 900 C temperatures. In alloy 3,
there is a sharp decrease in yield stress and tensile strength in
both conditions. It can be inferred that G-phase formation in
alloy 3 is the main reason for mechanical properties reduction.
G phase shows deleterious effects on mechanical properties
because it is hard and fragile; hence, it leads to toughness and
Journal of Materials Engineering and Performance
Fig. 11 Variation of mechanical properties of the alloys after aging
condition at room temperature
tensile strength reduction (Ref 28). Previous investigations
indicated that in Fe-12%Ni-25%Cr-steel, if the carbon were
more than 0.35 (wt.%), the brittle sigma phase was not formed
during aging (Ref 29, 30). Therefore grain growth, diffusion of
carbon in grain boundary, coarsening of primary carbides, and
precipitation of secondary carbides cause a decrease in
mechanical properties after aging.
Figure 13 illustrates the results of Vickers hardness of all
alloys after aging for different times. As said before, a fine
chromium carbide precipitation occurred during exposure to
high temperature. Therefore, hardness increased, but in alloy 1

Fig. 12 Variation of mechanical properties of the alloys before
aging condition at 900 C
Fig. 13 Vickers hardness profile of all specimens during aging time
hardness increased up to 400 h and then carbide coarsening
occurred. Therefore, hardness decreased. Alloys 2 and 4 show
the same behavior, Nb and Ti addition delays the carbides
coarsening and hardness increase up to 600 h. Alloy 3 exhibits
maximum hardness after aging at 600 h; it seems that in this
time transformation of NbC to G phase occurred. Aging for
long time causes significant variations in the mechanical
properties, especially elongation and toughness. Such changes
in mechanical properties are due to metallurgical variations that
occur during aging. Some of these variations include dissolu-
tion of secondary Cr carbide, G-phase formation, and change in
morphology of primary chromium carbide (Ref 13).
4. Conclusions
The following conclusions may be drawn from the results
and experimental evidence about the effects of niobium and
titanium on the microstructure and mechanical properties of
Fe-25%Cr-12%Ni-0.4%C austenitic heat-resistant steel:
• The addition of niobium and titanium causes the forma-
tion of niobium, titanium and mixed niobium-titanium car-
bides with variable properties of Nb and Ti, and promote
a partial replacement of the primary chromium carbide
and also a fragmentation of the primary carbide network.
• In alloy 3, after aging at 900 C, formation of a phase
rich in silicon, nickel, niobium that is very likely to be
the G phase denoted as Nb6Ni16Si7 was observed. In con-
trast, the XRD results indicated that in alloy 4, an increase
in the amount of titanium inhibited the G-phase forma-
tion.
• Thermodynamic results show that titanium and niobium
carbides form before the precipitation of primary chro-
mium carbides. They reduce the volume fraction of chro-
mium carbides because NbC and TiC particles act as
effective heterogeneous nuclei of chromium carbide.
• Aging for long time causes significant variations in the
mechanical properties, especially strength strain and yield
stress. Changes in mechanical properties are due to metal-
lurgical variations that occur during aging.
Acknowledgments
The authors wish to thank Isfahan Casting Industries (ICI) for
financial support.
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