Abrasive Wear Behavior of Austempered Ductile Iron With Niobium Additions
Abrasive Wear Behavior of Austempered Ductile Iron With Niobium Additions
Abrasive Wear Behavior of Austempered Ductile Iron With Niobium Additions
Wear
journal homepage: http://www.elsevier.com/locate/wear
A R T I C L E I N F O A B S T R A C T
Keywords: Carbidic Austempered Ductile Iron (CADI) microstructures containing eutectic carbides can be produced by the
Ductile iron addition of carbide stabilizing elements, such as chromium. Carbides formed from the addition of Cr are eutectic
Niobium alloying of M3C type. The presence of such hard phases can enhance the abrasion wear resistance of ductile iron. A new
Abrasion
CADI can be produced by the addition of Nb. Niobium carbide particles are formed in the beginning of solidi
Carbidic austempered ductile iron
fication and remain stable once they are insoluble in solid iron matrix. The dry sand abrasive wear resistance of
ductile irons alloyed with 1.0, 1.8, and 2.4 wt% Nb were tested in both “as-cast” and “heat treated” conditions
using standard ASTM G65. Results were compared to abrasive wear data obtained on ductile iron alloyed with
1 wt% Cr, CADI (1 wt% Cr), and the basic composition of iron without carbide stabilizing elements. In the “as-
cast” condition, the addition of Nb did not lead to a reduction in wear, while CADI with Nb is a promising
substitute for CADI with Cr addition, because both materials showed very similar values of abrasion resistance.
Micro-ploughing and micro-cutting mechanisms were observed on the worn surfaces of ductile irons. Abrasive
wear resistance of these alloys was correlated with the volume fraction of carbides.
* Corresponding author.
E-mail addresses: amandasopimentel@gmail.com, amandaprod@yahoo.com.br (A. Souza Oliveira Pimentel), w.guesser@tupy.com.br (W. Luiz Guesser).
https://doi.org/10.1016/j.wear.2019.203065
Received 29 May 2019; Received in revised form 15 September 2019; Accepted 20 September 2019
Available online 5 October 2019
0043-1648/© 2019 Elsevier B.V. All rights reserved.
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Table 1
Elemental composition of the base ductile iron alloy.
Elements Elemental range [wt.%]
C 3.40–3.60
Si 2.80–2.90
Cu 0.64–0.65
Mo 0.20–0.23
Mn 0.14 (maximum)
Mg 0.05–0.07
Table 2
Content of the alloying element in heat and in matrix, Cr for DI Cr 1 wt% and Nb
for the alloys with Nb.
Elemental range [wt. Alloy Alloy DI Alloy DI Alloy DI Alloy DI
%] DI 1 Cr 1 Nb 1.8 Nb 2.4 Nb
In white cast iron alloy with high Cr, the addition of Nb revealed iron
that has better wear performance than with the addition of Mo [14].
According to the literature, the addition of niobium of up to 2 wt% in
ductile cast iron provides significant enhancement of mechanical
properties [15,16]. Moreover, better resistance to adhesive wear and
abrasive wear resistance results from the addition of 0.40 wt% and
0.60 wt% of Nb [8]. In the case of ADI, the benefits of niobium are not
fully established. For ADI with 0.25 wt% Nb, the mechanical properties
of the material depends on the time of austempering treatment [17].
Some authors found that niobium improved hardness and impact
Fig. 1. Microstructure of “as cast” samples. Nital etched. The composition is
toughness of ADI with 0.2 wt% Nb [18]. For higher niobium additions, indicated in the images. White particles represent ferrite phase, except for DI
as 1.5 wt% Nb in ADI, higher abrasive resistance is reported, as well as Cr, where the white particles are M3C carbides.
high fracture toughness [19].
Some practical examples of cast iron alloyed with Nb are: piston TOP
Carbide particles maximum length was analyzed by SEM (Scanning
and compressing rings of martensitic ductile iron [8], cylinder lines of
Electron Microscopy) in the BSE mode and Image C software was used.
gray iron [20] and brake discs of gray iron [12].
At least 30 fields were analyzed per specimen before the heat treatment.
The purpose of this work is to investigate the performance of
The carbides remain stable, once the solubility of niobium in austenite is
pearlitic and carbidic austempered ductile irons with various Nb con
low. The NbC particles are not eutectic carbides, they are primary car
tents in abrasive tests. These materials were also compared to a carbidic
bides, formed in the beginning of solidification. As observed in Table 2,
austempered ductile iron alloyed with Cr.
the content of niobium in matrix varies from 0.02 to 0.03 wt % Nb.
The volume fraction of ferrite in “as cast” samples were analyzed by
2. Experimental procedures metallography. A contrast analysis was performed using Image Pro Plus
software. The white areas were designated as ferritic, despite the fact
The material used in the present investigation has the base compo that the carbide particles also appear as white areas.
sition showed in Table 1. The study was carried out on pearlitic ductile The mechanical properties of the specimens were analyzed. Micro
iron and austempered ductile iron (ADI). The samples were obtained in hardness tests were performed on the matrix areas, then graphite nod
an industrial foundry, casting 1 inch Y-blocks, according to dimensions ules and carbide particles were avoided. The microhardness was
specified in ASTM A536 [21]. From the base composition, five different measured using a Shimadzu (HMV – 2T) Microhardness Tester under a
alloyed materials were studied: 0–1 wt% Nb – 1.8 wt% Nb – 2.4 wt% Nb load of 500 g (0.5 HV) for 10 s. The tension tests were performed in an
– 1 wt% Cr. EMIC machine (6000 C) at 20 MPa/s. Three samples of each composition
The content of the alloying elements in the as cast matrix was combination and heat treatment were tested.
analyzed using a Jeol microprobe (see Table 2). In contrast to Nb, Cr
goes into solution and shows higher concentration in the matrix. In
consequence, niobium is more effective in forming hard phases than 2.1. Wear tests
chromium. Also noteworthy is the presence of Sb in Nb alloyed cast
irons, which comes from the Ferroniobium as a contamination. A series of abrasive wear tests were performed. The tests were con
The heat treated samples were austenitized at 900 � C for 1 h and ducted on a dry sand/rubber wheel apparatus according to ASTM G65
austempered in a salt bath at 310 � C for 110 min. test method [22]. The dry sand was rounded quartz sand with a U.S.
The samples were sanded, polished and etched with 2 vol % Nital sieve size 50/70. The moisture of the sand was controlled to 0.5 wt %.
solution for metallographic analysis. The carbide volume fraction and The coefficient of angularity of the dry quartz sand (a measurement of
the density of carbides of alloyed with Nb and Cr samples were analyzed the sand roundness) is 1.44 (according to Ref. [23]) and density of
using optical microcopy and Image Pro Plus software. The samples were approximately 1.6 g/cm3, which was fed between 300 and 400 g/min.
etched with Behara etchant (3 g of K2S2O5 and 10 g of Na2S2O3). At least Two procedures of the G65 test were performed: Austempered
20 fields were analyzed per specimen. samples were tested according to procedure A, which is a relatively
2
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Fig. 2. SEM images of DI 1.8% Nb (a) and CADI 1.8% Nb (b). The white particles are niobium carbides. In image (b) the ausferritic matrix. BSE mode.
Fig. 3. CADI 1% Cr. The white particles are M3C carbides. Ausferritic matrix.
Nital etched.
severe test, and the “as cast” samples were tested according to procedure Fig. 4. Volume fraction of ferrite of “as cast” ductile irons in box plot graphic.
B, which is a short variation of procedure A [3]. Considering the rela The squares indicate the average value and the asterisks represent the
tively low mechanical properties of the “as cast” material, low abrasive extreme values.
resistance is expected for these samples. Therefore, procedure B was
chosen for DI. analysis. In Fig. 2, the niobium carbide particles are represented by the
From the bottom section of the Y-blocks the test specimens of size white phase. Image (a) shows DI 1.8% Nb before heat treatment and (b)
75 � 25 � 10 mm3 were machined. The specimens were sanded and shows CADI 1.8% Nb after heat treatment. The carbide particles remain
polished in order to obtain ground surface finishing lower than 0.8 μm. stable. Ausferritic matrix is observed in image (b). Fig. 3 shows CADI 1%
Before the test, the specimens were cleaned in an ultrasonic cleaner and Cr, where the white particles are M3C carbides enriched with Cr.
accurately weighed. After the tests, the specimens were cleaned again The result of the volume fraction of ferrite analysis is shown in Fig. 4.
and weighed. The loss of weight was converted to volume loss in (mm3) The material with Cr reveals the lowest quantity of ferrite because Cr is a
by using a ductile iron density value of 7.2 g/cm3. Three samples of each pearlite promoter. As the content of Nb increases, the volume fraction of
condition were tested. The wear resistance is defined as the inverse of ferrite decreases. It is important to notice that, in this case, addition of
the weight loss. Nb brought together Sb, due the composition of Ferroniobium. Sb is a
After the tests, the specimen surfaces were analyzed using a ZEISS strong pearlite promoter, so the decrease of ferrite is attributed to this
scanning electron microscope, model DSM 940A, under the working element, not to Nb. Many results in the literature [12,13] must be
distance of 10 mm and accelerating voltage between 15 and 20 kV. reviewed with consideration of this contamination. The as-cast materials
exhibited bull-eye ferrite, except the material with Cr. The box plot
3. Results analysis reveals higher quantity of adjacent values for the niobium
addition materials. This is an indication of microstructures with higher
The samples alloyed with Nb or Cr developed carbides throughout heterogeneity when Nb addition occurs.
the matrix. The carbides formed from the addition of Cr have EC4 Experimental results of mechanical properties are given in Table 3.
(eutectic carbide type 4) spatial geometry of arrangement A2, while the The microhardness of austempered samples are higher than the micro
carbides from the addition of Nb are polygonal PC4 (primary carbide hardness of “as cast” samples, as expected. However, higher hardness for
type 4). During heat treating, the carbides remain stable, once they are ductile irons alloyed with Nb or Cr were not observed. Tensile strength is
NbC and M3C carbides enriched with Cr. Fig. 1 shows the ferritic- reduced with Cr and Nb alloying, especially for “as cast” condition. A
pearlitic matrix of the “as cast” ductile iron samples. The white parti great reduction of elongation was detected for samples alloyed with Nb
cles in the images represents the ferrite phase. Bull-eye structures are and Cr. The elongation is lower for samples with Cr because the element
observed, except for Cr. In DI Cr condition, the white particles are M3C segregates to eutectic cells boundaries. The cracks in the material are
carbides. The niobium carbides are also white particles for DI samples, propagated through the carbides connecting the cells boundaries.
however, they are too small to be observed by the magnification of the The wear resistance results from “as cast” samples show the best
3
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Table 3
Mechanical properties and microstructure of the samples. SD is the standard deviation.
Sample Matrix Tensile strength SD Yield strength SD Elongation SD Microhardness (HV SD
(MPa) (MPa) (%) 0.2)
DI 1 wt% Cr Pearlite þ M3C particles 693 23.4 552 5.4 1.4 0.3 356 44.3
DI Pearlite þ ferrite 772 14.0 467 2.6 7.8 1.7 379 22.9
DI 1 wt% Nb Pearlite þ ferrite þ NbC 705 49.9 468 2.4 3.5 1.2 354 46.6
particles
DI 1.8 wt% Nb Pearlite þ ferrite þ NbC 659 29.4 473 11.3 2.2 0.3 336 32.1
particles
DI 2.4 wt% Nb Pearlite þ ferrite þ NbC 617 102.3 476 9.5 2.8 0.5 297 50.5
particles
CADI 1% Cr Ausferrite þ M3C particles 1032 28.7 995 11.9 0.9 0.1 537 44.3
ADI Ausferrite 1295 6.6 1046 15.8 4.1 0.3 537 29.3
CADI 1 wt% Nb Ausferrite þ NbC particles 1232 23.5 1055 9.9 2.1 0.4 531 14.0
CADI 1.8 wt% Ausferrite þ NbC particles 1252 14.6 1058 8.0 2.3 0.3 537 13.8
Nb
CADI 2.4 wt% Ausferrite þ NbC particles 1195 16.0 1050 11.0 1.5 0.2 531 29.3
Nb
Fig. 5. Dry abrasive wear resistance of different ductile irons after abrasive Fig. 6. Worn surface of DI 2.4 wt % Nb, 100 X, SEM, SE mode. The arrows
tests in box plot graphic. The squares indicate the average value. The asterisks indicate pitting.
represent the extreme values.
resistance. Furthermore, large grooves were formed on the “as cast”
samples surface (see Fig. 7 (d and e)). These grooves are larger than the
Table 4 carbide dimensions, which leads to the pulling-out of the niobium car
Wear mechanisms and wear resistance values of “as cast” samples. SD is the bide particles. The carbide particles maximum length analysis is shown
standard deviation.
in Table 5.
3
Material Wear mechanism Wear resistance (mm ) SD Fig. 7 shows the pitting on the DI 1.8 wt% Nb surface in SE (a) and
DI 1 wt% Cr Absence of grooves 0.0182 0.0002 BSE (b) mode. The BSE image confirms that in the deepness of the pitting
DI Ploughing 0.0307 0.0028 remains graphite. The grooves produced on the worn surface are seen in
DI 1 wt% Nb Ploughing, pitting 0.0213 0.0020 Fig. 7 (c, d and e). Typical micro-ploughing features are observable by
DI 1.8 wt% Nb Ploughing, pitting 0.0177 0.0015
the deformation of the matrix, the prows at the end of the grooves and
DI 2.4 wt% Nb Ploughing, pitting 0.0335 0.0202
the ridges adjacent to the grooves. The presence of chips in prow,
especially for DI 1.8 wt%Nb (d), confirms the micro-cutting mechanism.
result for ductile iron with Cr, as seen in Fig. 5. The ductile irons with Nb Aside from the deformation of the matrix, detaching of the material
showed very similar results to ductile iron base result. The niobium occurs due to micro-cutting and low cycle fatigue during micro-
carbide particles are smaller than the abrasive particles. Indeed, they did ploughing [24]. The DI 1 wt% Cr samples presented less deformation
not act as a barrier to scratching on the ferritic-pearlitic matrix, but of the matrix and the absence of grooves. Fig. 7 (f) shows the BSE mode
rather, the carbide particles may have been removed. The box plot analysis of DI 1 wt% Cr. The arrow indicates a graphite nodule, which
analysis shows high dispersion of the result values. The dispersion exists was covered by the matrix deformation.
probably due to the heterogeneity of the samples with carbides. The results for austempered irons with carbides are promising, as
Table 4 summarizes the wear resistance and wear mechanisms of seen in Fig. 8. CADI with Cr and CADI with Nb showed similar wear
ductile cast irons. The main wear mechanism is ploughing due to the performance. The presence of hard particles embedded in the matrix is
presence of a soft matrix. Pitting like craters were observed in the effective when the matrix is hard enough to prevent the removal of the
samples with niobium, according Fig. 6. This indicates that the presence particles. According to the box plot analysis, higher variability of data is
of niobium contributes to the propagation of cracks and reduces its wear observed for CADI 1% Nb, some samples showed lower performance
4
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Table 6
Wear mechanisms and wear resistance values of austempered ductile irons. SD is
the standard deviation.
3
Sample Wear mechanism Wear resistance (mm ) SD
Fig. 7. Worn surfaces of “as cast” ductile irons, 1000 X. (a), (c) and (d): SEM in
SE mode. (b) and (e): SEM in BSE mode. Micro-ploughing was observed for the
samples, except for DI Cr.
Table 5
Maximum length of niobium carbide particles. SD is the standard deviation.
Material Minimum length Maximum length Average SD
(μm) (μm) (μm)
5
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Fig. 11. Dry abrasive wear resistance of austempered ductile irons versus the
yield strength. The proper combination of high abrasive wear and high yield
strength is achieved for CADIs with Nb.
6
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
Fig. 12. Dry abrasive wear resistance of ductile irons versus density of car
bides. High values of wear resistance correlate to low density carbide values Fig. 15. Dry abrasive wear resistance of austempered ductile irons versus
probably due to the removal of carbide particles. carbide volume fraction. The wear resistance of CADI with Nb in “heat-treated”
condition increased with increasing volume fraction of carbide.
5. Conclusions
From the results of the present study with dry sand abrasive wear the
following conclusions can be drawn:
7
A. Souza Oliveira Pimentel et al. Wear 440-441 (2019) 203065
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