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Keywords: The effects of niobium addition up to 0.11 wt% on the microstructure and tensile properties of as-cast ductile
As-cast ductile iron iron (ACDI) were investigated. Metallographic analyses by both optical microscopy (OM) and scanning electron
Niobium microscopy (SEM) indicated that niobium (Nb) promoted the formation of pearlite, reduced pearlite lamellar
Microstructure spacing and decreased the extent of graphitization taking place in the Nb-alloyed ACDI. The nodularity and
(Nb, Ti) C nano precipitate
nodule counts of graphite changed insignificantly when the Nb content was less than 0.08 wt% in the ACDI. The
Tensile behavior
analysis of precipitates by transmission electron microscopy (TEM) revealed that nano and micro sized (Nb, Ti)
Fracture
C carbides acted as nucleation site for graphites, and promoted the formation of large graphite nodules with low
roundnesses as Nb content rose above 0.08 wt%. The results of tensile testing showed that the yield strength,
ultimate tensile strength and elongation of the ACDI with 0.08 wt% Nb increased by 12.1%, 11.2% and 14.3%
over those of the Nb-free ACDI, respectively. The optimum values of the yield strength, tensile strength and
elongation of the Nb-alloyed ACDI were found to be 418 MPa, 746.0 MPa and 8.0%, respectively, at the Nb
content of 0.08 wt%. The high strain hardening rates of the Nb-containing ACDIs implied that they were capable
of spontaneously strengthening itself increasingly to a large extent, in response to a slight plastic deformation
after yielding.
1. Introduction of carbon steel. Iacoviello et al. [9] found that graphite nodules present
in the matrix of ductile iron behaved almost like voids with regard to
More than 90% by weight of metallic materials used by human mechanical properties. Ductile iron comprising graphite nodules with
beings are ferrous alloys, which are classified into two groups based on high counts and low average diameters exhibited better mechanical
the carbon (C) content in the alloys. Steel generally contains between properties. In the past decades, the implementation of heat treatment
0.04 and 1.7 wt% C, while cast irons have between 1.8 and 4.0 wt% C processes and the introduction of alloying elements have been proven
[1]. Compared to steel, cast irons have relatively low melting tempera- to be critical for the mechanical property improvement of ductile iron.
tures, very good fluidity and castability, and moderate shrinkage during Resulting from the application of heat treatment, austempered ductile
solidification and cooling [2,3]. But, engineering applications of cast iron (ADI) is one of the most studied variants for its excellent tensile
irons were limited until ductile irons were successfully developed by strength, ductility and wear resistance [10–12]. However, increased
adding a small amount of magnesium and/or cerium to the gray iron in manufacturing cost and extended production cycle limit a widespread
1948 [4,5]. Nowadays, ductile irons are widely used for manufacturing application of austempered ductile iron. Research interests [13–18]
wheels, bearings and gears due to its excellent castability, good have also been in developing alloying methods, in which the effects of
mechanical properties and low cost [3–8]. Due to the spherical alloying elements, such as copper, nickel or molybdenum on the
graphite morphology, the strength of ductile iron is equivalent to that improvement of the tensile strength, hardness, wear resistance and
⁎
Corresponding authors.
E-mail addresses: cxr16@shu.edu.cn (X. Chen), shuxujie@163.com (J. Xu), huh@uwindsor.ca (H. Hu), hm@niobelcon.net (H. Mohrbacher), kangming@dfcv.com.cn (M. Kang),
zhangwei3@citic.com (W. Zhang), guoam@citic.com (A. Guo), qjzhai@shu.edu.cn (Q. Zhai).
http://dx.doi.org/10.1016/j.msea.2017.01.032
Received 17 July 2016; Received in revised form 29 December 2016; Accepted 9 January 2017
Available online 30 January 2017
0921-5093/ © 2017 Elsevier B.V. All rights reserved.
X. Chen et al. Materials Science & Engineering A 688 (2017) 416–428
ductility of ductile iron are investigated. The introduction of different niobium addition. The Nb effect on the microstructure of the Ni-
alloying elements into ductile iron enables the control and manipula- containing ductile iron contributed to a small increase in yield and
tion of phase constitution, microstructural refinement and solution tensile strength as well as in hardness along with a decrease in ductility.
strengthening. Consequently, the mechanical properties of ductile iron So far, it appears that Nb addition to ductile iron has not been
are improved and even optimized to achieve both high strengths and extensively studied, in particular at a microalloying level of up to
ductilities. Among various alloying elements, niobium is widely used 0.10 wt%, although, in principal, it could provide microstructural
for microstructural control in nickel-base alloys [19–21], steel [22–24] refinement and precipitation strengthening due to its strong carbide
and cast irons [25–33]. Smith and Patel [21] pointed out that niobium, forming tendency. It is of interest whether similar positive effects of Nb
as a refractory element, was capable of improving mechanical proper- microalloying on the mechanical properties of ductile cast iron could be
ties of nickel-base alloys through carbide formation and precipitation obtained.
hardening despite its limited benefit as a solid solution strengthener In the present work, the effects of Nb microalloying up to 0.11 wt%
due to its relatively low melting point and modulus compared to other on the microstructure of the as-cast ductile iron (ACDI) were studied
refractory elements (Mo. Ta and W). The review given by Morrison [22] using metallographic analyses. The microstructural analyses by optical
recognized the advantages of adding a small amount ( < 0.12 wt%) of microscopy (OM), scanning electron microscopy (SEM) and transmis-
niobium to C–Mn steels for property improvement. The Nb addition sion electron microscopy (TEM) revealed that phase constituents and
not only refined grain structure but also precipitated nano-sized NbC or constitution as well as phase morphology in the ACDI were influenced
NbCN particles during normalizing treatment. Mohrbacher [23] ob- by Nb addition. The mechanical properties of the Nb-alloyed ACDI
served similar phenomena in multiphase steels microalloyed by Nb ( < were evaluated by tensile testing. Based on the results of tensile testing,
0.2 wt%). the optimum content of Nb with respect to both improved tensile
Nb microalloying to grey cast iron and its influence on mechanical strengths and elongations was identified.
properties are widely studied [25–29]. Zhou et al. [25] found that,
adding about 1.48 wt% Nb to grey cast irons increased hardness and 2. Experimental procedure
wear resistance considerably due to the massive presence of large-sized
NbC phases with dimensions over 10 µm, an increase in the number of 2.1. Material preparation
eutectic cells, and a reduction in the graphite size and the pearlite
interlamellar spacing. The study by Devecili and Yakut [27] showed The raw materials employed in this study were pig iron, steel scrap,
that the addition of 0.65 wt% Nb led to the formation of 10 µm chunky 80MnFe, copper, nickel and ferro-niobium (Fe65Nb). All the materials
Nb and Ti containing phases in grey cast irons, and improved their were melted and homogenized at 1520–1540 ℃ in an induction
abrasion resistance and tensile strength. It has been indicated [26] furnace having a maximum capacity of 16 kg. Upon the completion
that, with niobium level above 0.1 wt% primary NbC carbides could be of placing 1.2 wt% Fe-Si-Mg-Ba alloy (41.3 wt% Si, 6.9 wt% Mg and
formed in the liquid iron, which acted as nuclei for the eutectic 1.52 wt% Ba) on the bottom of the preheated ladle (covered with an
reaction, i.e., the transformation of the liquid phase into austenite iron sheet), the melt was poured into the ladle at a temperature of
and graphite or cementite. This explained the observation, that the 1440–1460 ℃ for spherodization. After skimming the slag off the
eutectic cells became finer with niobium additions. When the niobium surface of the spherodized melt, 0.8 wt% Fe-Si-Al alloy (74–79 wt%
content exceeded the alloying limit of 0.2 wt%, such primary carbides Si, 0.8–1.6 wt% Al and 0.5–1.0 wt% Ca) was added for inoculation. At
were formed already at elevated temperature becoming coarser with last, all the melts were poured into a Y-block sand mold as illustrated in
time and could thus be found in the microstructure as NbC even by Fig. 1. It should be noted that a small amount of melt was poured into a
optical microscopy. Zhu et al. [29] introduced 0.11 wt% Nb into grey metal mold for producing white iron specimens with a dimension of
cast irons and observed their improved high-temperature tensile 0.004×Φ0.040 mm, which were used for the chemical composition
strength and oxidation resistance. It was noted that brittle breaking verification. The results of chemical analyses are shown in Table 1.
occurred with the specimen containing niobium of 0.037 wt%, and
ductile breaking occurred with the specimen containing niobium of 2.2. Microstructural analysis
0.11 wt%, and the fracture exhibited ductile dimples. Fraś et al. [30]
studied the effect of small additions of niobium (up to 0.038 wt% Nb) Metallographic specimens were sectioned, mounted, and polished
on structure and mechanical properties of ductile iron. It was indicated from the bottom of Y-type specimens, and prepared following the
that niobium increased graphite nodule count with small diameters standard metallographic procedure. After polishing and 4% Nital
and the fraction of carbides in ductile iron, although the effect of small etching of metallographic specimens obtained from the bottom of Y-
additions of niobium on type of matrix is negligible. The Nb-alloyed
ductile irons exhibited the improved tensile and yield strengths, but the
reduced elongation. The work by Souza et al. [31] showed that the
0.47 wt% Nb addition to nodular cast irons (NCIs) led to a 20%
increase in their yield and tensile strengths over the values for the Nb-
free NCI because of the increase in pearlite content. A modest
increment of tensile ductility and Charpy toughness appeared while
only 0.23 wt% Nb was introduced. Alias et al. [32] alloyed the ductile
iron with 0.5–2.0 wt%. Their results showed that the Nb addition in
ductile iron provided significant enhancement in mechanical properties
when compared to unalloyed ductile iron. Addition of higher amount of
niobium had further increased the strength and impact toughness
properties. Bedolla-Jacuinde et al. [33] investigated the effect of
niobium in the range of 0–0.8 wt% in Ni-containing ductile cast irons.
Niobium was observed to be directly related to the formation of
polygonal niobium carbides of the type NbC, which had the size of as
large as 8 µm in the irons with 0.8 wt% Nb. The amounts of pearlite Fig. 1. Dimensions of the Y-block sand casting employed in the present study, and the
and ferrite phases were not affected by the niobium content added in arrow-pointed location in which specimens were sectioned for metallographic analyses
their study. Neither nodule count nor nodularity was affected by such and mechanical testing.
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X. Chen et al. Materials Science & Engineering A 688 (2017) 416–428
Table 1
Chemical composition of the ACDI in weight percent (wt%); Fe: balance.
Samples C Si Mn P S Cu Ni Cr Ti Mg Nb
1 3.87 1.64 0.30 0.04 0.02 0.45 0.57 0.02 0.03 0.05 0
2 3.86 1.67 0.32 0.03 0.02 0.41 0.70 0.02 0.03 0.04 0.04
3 3.92 1.69 0.25 0.03 0.02 0.44 0.64 0.03 0.03 0.04 0.06
4 3.91 1.76 0.33 0.06 0.02 0.46 0.60 0.02 0.03 0.03 0.08
5 3.86 1.72 0.30 0.04 0.02 0.42 0.71 0.03 0.03 0.04 0.11
Fig. 2. Optical micrographs showing the graphite morphology of the ACDIs with different Nb contents: (a) 0 wt%Nb, (b) 0.04 wt%Nb, (c) 0.06 wt%Nb, (d) 0.08 wt%Nb and (e) 0.11 wt%
Nb.
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Fig. 5. Optical micrographs showing the phase constituents of graphite, ferrite and pearlite in microstructure of the etched ACDIs with different Nb contents: (a) 0 wt% Nb,(b) 0.04 wt
% Nb,(c) 0.06 wt% Nb,(d)0.08 wt% Nb and (e) 0.11 wt% Nb.
(“bullseye”) became notably thinner, and the pearlite content rose with sized particle given in Fig. 8(a) or micro-sized particle clusters revealed
increasing niobium contents. Fig. 6 reveals the effect of Nb addition on in Fig. 8(b). The probe crossed the nano-size particle along the solid
the pearlite and graphite volume percentages in the Nb-alloyed ACDIs. line in Fig. 8(c–f). When the probe went from the graphite to the
Fig. 7 shows the pearlite microstructure in the tested ACDIs with particle, the elements of Ti, Nb and Fe were detected. The selected area
the different Nb contents by SEM micrographs in a backscattered diffraction pattern in Fig. 8(e) revealed the Nb-containing phase was
electron (BSE) mode. A selected circle in Fig. 7(d) represented the area (Nb, Ti) C with a cubic structure. The detection of iron might result
for the measurement of the pearlite lamellae spacing. from the inherent content of the ACDI.
Fig. 8 presents the TEM results showing the nano and micro-sized
niobium carbides present in the ACDI with 0.08 wt% Nb addition. The
Nb-containing precipitates were present in the form of a single nano-
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Fig. 7. SEM micrographs in BSE mode showing pearlite morphology in the ACDIs with different Nb contents: (a) 0 wt% Nb,(b) 0.04 wt% Nb,(c) 0.06 wt% Nb,(d)0.08 wt% Nb and
(e) 0.11 wt% Nb.
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Fig. 8. TEM micrographs of (a) a nano-sized (Nb, Ti)C particle, (b) micro-sized (Nb, Ti) C particle clusters embedded in the graphite nodules of the ACDI with 0.08 wt% Nb, (c) line
scans and the corresponding line scanning pattern for the nano-sized (Nb, Ti)C particle, EDS patterns for (d) Ti, (e) Nb and (f) Fe, and (g) diffraction pattern of nano-sized (Nb, Ti)C
phase.
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Fig. 10. SEM fractographs in SE mode showing the fracture surfaces of the ACDIs with the Nb contents: (a) low magnification and (b) high magnification for 0 wt%Nb; and (c) low
magnification and (d) high magnification for 0.08 wt% Nb.
Table 3 The plastic deformation of the stress-strain curve for metals can
Phase content in the matrix with different Nb contents in the ACDI. described by the power law:
Nb content (wt%) 0.0 0.04 0.06 0.08 0.11 σ = K εn (8)
Pearlite (vol%) 74.4 80.2 79.1 85.2 85.8 where K and n are empirical constants. The regression analysis
Graphite (vol%) 9.9 9.2 9.4 8.6 8.5 indicates that the power law was in good agreement with the tensile
results. The numerical values of these constants in the above equation
with the regression coefficients are listed in Table 5. The above
Table 4
Variation of pearlite lamellar spacing of the ACDI with the different Nb contents.
equation can be differentiated to obtain strain-hardening rates (dσ/dε).
All the tested ACDIs exhibited a pronounced strain hardening
Nb content (wt%) 0.0 0.04 0.06 0.08 0.11 behavior during plastic deformation. The strain hardening rates of
the Nb-alloyed ACDIs were determined based on the measurements of
Pearlite lamellar spacing (µm) 1.04 0.97 0.89 0.87 0.79
tensile testing. Fig. 14 displays the variation of the strain hardening
rates as a function of true strain for all the studied ACDIs with different
Nb contents. It is evident that, for all the five tested ACDIs, their strain-
hardening rates decreased with increasing true strains. As can be seen
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1500 Table 5
Fe + 4.23% C Best fit parameters of power equation.
1450
Sample K (MPa) n R2
from Fig. 14(a), the ACDI with 0.08 wt% had a high strain- hardening
1250 L+ +
graphite
rate (24,325 MPa) with respect to the Nb-free ACDI (21,190 MPa) at
L + NbC + + graphite
the onset of plastic deformation, which resulted in an increase of
1200 14.8%. For the Nb contents up to 0.08 wt%, the strain hardening rates
of the Nb-containing ACDIs increased with increasing Nb addition, and
1150 were consistently higher over the entire plastic deformation stage of the
+ NbC + graphite tensile strain range than that of the Nb-free ACDI. As depicted in
1100 Fig. 13(b), an additional introdution in the Nb content from 0.08 to
0 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.11 wt% led to a minor decrease in the strain hardening rate of the
Niobium content (wt%) Nb-alloyed ACDI by only 5.3%. Hence, the content of 0.08 wt% Nb
Fig. 11. Phases diagram of Nb in eutectic iron (Fe+4.23 wt%C) [25]. could be considered as an optimum level in terms of tensile behavior of
the Nb-alloyed ACDIs. The observation on the strain hardening
behavior suggested that the Nb addition enhanced the ACDI capability
of spontaneously strengthening itself increasingly to a large extent, in
response to a slight plastic deformation after yielding.
5. Conclusions
1. The niobium additions up to 0.08 wt% into the base ductile iron had
insignificant influence on the graphite nodule morphology and
nodule count. In these ACDI alloys, niobium remained in solution
before and after solidification. Increasing amount of solute niobium
promoted pearlite formation and refines lamellar spacing.
2. The relatively high amount of niobium addition, particularly at a
level of 0.11 wt% resulted in partial precipitation of Nb carbide
Fig. 13. Typical true stress-strain curves of the ACDIs with different Nb contents.
particles in the liquid phase. The precipitated particles could provide
nucleation sites for graphite nodules. But, the larger primary Nb
carbide particles as well as particle clusters might exhibit a detri-
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X. Chen et al. Materials Science & Engineering A 688 (2017) 416–428
Fig. 14. Strain hardening of the ACDIs with the Nb contents of (a) 0–0.08 wt%, and (b) 0.08 wt% and 0.11 wt%.
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