AISTech 2019 — Proceedings of the Iron & Steel Technology Conference

6–9 May 2019, Pittsburgh, Pa., USA

DOI 10.1000.377.107

Designing a Graphitic White Iron: Microstructures and Properties

Jie Wan1, Jingjing Qing2, Mingzhi Xu2

1
Missouri University of Science and Technology
1400 N Bishop, Rolla, MO, USA, 65409
Phone: (573) 578-3874
Email: jwvt7@mst.edu
2
Georgia Southern University
1332 Southern Dr, Statesboro, GA, USA, 30458

Keywords: Graphitic White Iron, Wear-Resistant Material, Microstructure, Thermal Diffusivity, Wear Performance

INTRODUCTION

The word “tribology” was first reported by Jost [1] in a landmark report. Its popular English language equivalent is “wear”,
which is defined as “alteration of a solid surface by progressive loss or progressive displacement of material due to relative
motion between that surface and a contacting substance or substances” by ASTM G40 [2]. As a major problem in modern
machinery parts, wear is very crucial in metal-to-metal wear systems, such as rolling bearing, gears, and seals. The wear of
parts, the cost of repair and replacement of these parts, and the associated downtime related to these activities results in
significant costs to the industry [3]. A wide variety of hard facing materials have been invented to slow down the wear rate
and reduce the associated cost. The most popular ones, today, are silicon carbide, tungsten carbide, Ni-Resist cast iron,
Stellite and aluminum oxide [4], but most of these hard facing materials are too expensive, due to either the cost of alloy
addition or manufacturing processing. Alternative option for such application is high Cr white iron. Containing M7C3
carbide of high hardness (1100-1600 HV) [5] makes it relatively wear resistant, while its alloy cost is much lower compared
with foresaid hard facing materials. The M7C3 carbides in high Cr white iron are the primary phases of hexagonal shape and
can work as the “stoppers” to decrease the wear rate during the wear application [6]. However, with about 10-30 wt.%
chromium addition, high Cr white iron has a poor thermal diffusivity. Frictional heating generated during the wear
application can over heat the wear surfaces and induce severe adhesive wear to the wear components [7-9]. It was also
reported that the wear rate increases substantially at elevated temperatures [9,10].
One of the solutions to reduce the effect of frictional heating, and extend the service life of the wear components is increasing
their thermal diffusivity, which accelerates heat dissipation and decreases the wear rate of the wear components. This idea
was firstly used to produce the so-called mottled cast iron [11-17], which generally contains spheroidal graphite and is widely
used for mill rolls [11-13]. However, it was reported by Matsushita, that the thermal diffusivity of a cast iron increases with
decreasing nodularity [7], and flake graphite has the best thermal diffusivity compared with graphite with other morphology.
To maximize the graphite contribution on the thermal diffusivity, the authors introduced flake graphite into the white iron
and developed the first generation graphitic white iron [7,19,20].
In the present investigation, the authors studied the microstructure, hardness, thermal diffusivity and wear performance of the
first generation graphitic white iron. Wear mechanism was investigated using an optical microscope and a scanning electron
microscope (SEM). A numerical model was established by taking both hardness and graphite volume percent into volume
loss prediction.
MATERIALS AND EXPERIMENTAL PROCEDURE

Materials
Five iron-based alloys at different carbon and chromium contents were designed and produced with high purity charge
materials to develop the first generation of graphitic white iron. The rational for the material design was described in authors’
previous publication [8]. Chemical compositions for the five alloys shown in Table I were analyzed with an optical emission

© 2019 by the Association for Iron & Steel Technology. 1041

spectrometer and a Leco combustion C/S analyzer. The five alloys produced were named as 3Cr, 5Cr, 7Cr, 9Cr and 11Cr,
based on their approximate Cr content individually.
Table I. Chemical composition of the five graphitic white irons produced.
Chemical composition (wt.%) Inoculant
Alloys
Leco C Leco S (ppm) Si Mn Cr (wt.%)
3Cr 4.45 154 2.06 0.44 2.79 0.15
5Cr 4.72 157 2.00 0.47 5.11 0.15
7Cr 4.88 184 2.07 0.49 7.08 0.15
9Cr 4.93 198 2.05 0.50 9.08 0.15
11Cr 5.00 170 2.03 0.50 11.03 0.15

Experimental Procedure
 
Metallographic Samples Preparation and Characterization
Two sets of metallographic samples were prepared to study the phase constituent for graphitic white irons studied. The first
set of samples was as-polished and used to study the graphite morphology as well as the graphite volume percent. The second
set of samples was etched with 2% Nital to reveal different carbides and the matrix structure. A Nikon FX-35DX camera was
used to observe and capture the microstructures for all five graphitic white iron alloys. The graphite volume percent was
measured from the as-polished micrographs with ImageJ software by adjusting the contrast threshold [8]. Rockwell hardness
indentation was conducted following ASTM E18 in C scale [9] for all five alloys studied.

Thermal Diffusivity Sample Preparation and Characterization

A laser flash apparatus was utilized to measure the thermal diffusivity for each alloy following ASTM E1461 [10]. As shown
in Figure 1, five laser flash samples were prepared for each alloy with a dimension of 12.7 mm x 12.7 mm x 3.0 mm. A
thermographite standard sample was used as the reference for the measurement. The top and bottom surfaces of each sample
were spray coated by graphite at 75 °C to promote the heat absorption [10] and achieve a consistent emissivity for each
sample during the tests [23,24]. The thermal diffusivity of each sample was tested three times at temperatures of 200 ºC, 300
ºC, 400 ºC, 500 ºC, 600 ºC and 800ºC, respectively.

3Cr‐1  3Cr‐2  3Cr‐3  3Cr‐4  3Cr‐5 

5Cr‐1  5Cr‐2  5Cr‐3  5Cr‐4  5Cr‐5 

7Cr‐1  7Cr‐2  7Cr‐3  7Cr‐4  7Cr‐5 

9Cr‐1  9Cr‐2  9Cr‐3  9Cr‐4  9Cr‐5 

11Cr‐1  11Cr‐2  11Cr‐3  11Cr‐4  11Cr‐5 

Figure 1. Pictures of laser flash samples for thermal diffusivity measurement.

Wear Test Sample Preparation and Characterization
A dry sand/rubber wheel apparatus was utilized to evaluate the wear performance of five alloys studied in accordance with
ASTM G65 Procedure A [11]. Three samples were prepared for each alloy for dry sand/rubber wheel wear testing. As shown
in Figure 2, the dimension of each sample was 12.7 mm x 25.4 mm x 76.2 mm. Each of the prepared sample was weighed
before and after 6000 testing revolutions to obtain the weight loss. The Archimedes Principle was applied to measure the
density of each alloy, which was then used to convert the weight loss into volume loss. The wear scars of each studied alloys

1042 © 2019 by the Association for Iron & Steel Technology.

were evaluated via SEM to investigate the wear mechanism for the alloys studied. The electron beam was operated at an
accelerating voltage of 20.0 kV and an emission current of 5.5 nA during image acquisition.

Figure 2. Illustration and dimension of the dry sand/rubber wheel specimens.

RESULTS AND DISCUSSION

Metallographic Microstructure
As shown in Figure 3, the graphite morphologies and distributions for the five alloys studied were revealed on the as polished
micrographs. Type A (green arrows) and Type C (red arrows) flake graphite can be observed in alloy 3Cr, 5Cr and 7Cr. Type
D flake graphite (purple arrows) can be observed in the dendritic regions in all five alloys. Ideally, all these graphite flakes
not only increase the thermal diffusivity for graphitic white irons, but also will be partially abraded off and work as lubricant
during the wear application. Both of these two factors can reduce the detrimental frictional heating during the wear
application and extend the lifetime of this novel material designed for metal-to-metal wear systems.

(a) (b) (c)

(d) (e)
Figure 3. As polished microstructures for alloy (a) 3Cr; (b) 5Cr; (c) 7Cr; (d) 9Cr; (e) 11Cr; Red arrows indicate the Type C
graphite, blue arrows indicate the Type A graphite, and purple arrows indicate the Type D graphite.
The second set of metallographic samples was etched with 2% Nital to reveal all other phase constituents. As shown in
Figure 4, different carbides (white phases) of various morphologies were differentiated. The plate carbides (indicated by red
arrows) in all five alloys are cementite. The cluster carbides (indicated by green arrows) in Figure 3(c) are M7C3 carbides.
The hexagonal shaped carbides (indicated by purple arrows) in Figures (d) and (e) are also M7C3 carbides. Comparing
Figures (c), (d) and (e), as the Cr content increases in the alloy, the morphology of the M7C3 carbide becomes closer to
hexagonal. The detailed carbides characterization and discussion were stated in authors’ previously published article [8].

© 2019 by the Association for Iron & Steel Technology. 1043

 (a) (b) (c)

(d) (e)
Figure 4. Micrographs etch with 2% Nital for alloy (a) 3Cr; (b) 5Cr; (c) 7Cr; (d) 9Cr; (e) 11Cr. Red arrows indicate plate
cementite, green and purple arrows indicate M7C3 carbide.

Graphite Volume Percent Analysis

The graphite volume percent for each alloy was measured on the as polished optical micrographs to quantitatively study the
amount of graphite effect on the thermal diffusivity and the wear resistance of graphitic white iron. Ten measurements were
conducted on ten different as-polished micrographs for each of the five alloy studied. Figure 5 shows the average of ten
measurements and the error bars represent 95% CL uncertainty range [12]. It turned out that the graphite volume percent
continuously decreases with increasing chromium content in the bulk material, which is mainly because that chromium is a
strong carbide former and it restricts the formation of graphite. Carbon equivalent is an important controlling factor for
graphite formation in cast iron [27,28]. To fully understand how the graphite volume percent is affected by the carbon
equivalent, a carbon equivalent equation was developed to determine the carbon equivalent for graphitic white iron, which
was then used to establish a numerical model to predict the graphite volume percent in graphitic white iron for any given
chemistry. The developed carbon equivalent equation and numerical model for graphitic white irons are listed as Eq. (1) and
Eq. (2).

𝐶 𝐶 0.4𝐶 0.33𝐶 0.027𝐶 0.25𝐶 (1)

𝑉 𝐺𝑟 4.1046𝐶 9.0513 (2)

More details of these equations can be found in authors’ previously published paper [8]. The values of these graphite volume
percent is being used in later sections for discussion of the thermal diffusivity and wear test results.

1044 © 2019 by the Association for Iron & Steel Technology.

 Figure 5. Plot of measured graphite volume percent for the five graphitic white iron studied.

Hardness Analysis
It is necessary to study the hardness change among five studied alloys, since hardness is closely related to the wear resistance
of metals [13]. However, due to their poor ductility, it is impractical to obtain Brinell hardness for neither of the five studied
alloys. Instead, Rockwell hardness was performed following ASTM E18 in C scale [9]. Figure 6 shows an average of ten
measurements with an error bar showing 95% CL uncertainty range [12]. Unlike the graphite volume percent, the Rockwell
hardness does not change continuously with the chromium content in the bulk material. With increasing Cr content in the
bulk material, the overall hardness increases for alloys from 3Cr to 9Cr, and then starts to decrease from alloy 9Cr to alloy
11Cr. By comparing the microstructure shown in Figure 4(d) and Figure 4(e), this is possibly due to the lack of plate
cementite in alloy 11Cr compared with alloy 9Cr. In this case, during the Rockwell hardness testing, the indentations
covered a larger area of the pearlitic matrix in the alloy 11Cr. The wear scars shown in Figure 9 further validates this
explanation.

Figure 6. Plot of Rockwell hardness measurement for five graphitic white irons in C scale.

Thermal Diffusivity Analysis

Laser flash method is commonly used to measure the thermal diffusivity for metals [18,30]. To ensure that graphite has a
positive contribution to graphitic white irons, the thermal diffusivity for all five studied alloys was measured using laser flash
method following ASTM E1461 [10]. Figure 7(a) shows an average of fifteen measurements of each alloy at each testing
temperature. The small error bars represent 95% CL uncertainty range [12] and indicate that laser flash method has a very
good repeatability in terms of measuring thermal diffusivity for the studied alloys. It turned out that the overall thermal
diffusivity decreases with increasing temperature for each individual graphitic white irons, especially for these with higher
graphite volume percent. As expected, thermal diffusivity for graphitic white iron increases with increasing graphite volume
percent. To emphasize the amount of graphite effect, thermal diffusivity is also plotted against graphite volume percent at
different temperature in Figure 7(b). It turned out that the thermal diffusivity increases exponentially with increasing graphite
volume percent.

© 2019 by the Association for Iron & Steel Technology. 1045

 (a) (b)
Figure 7. Plots of: (a) Thermal diffusivity change against temperature; (b) Thermal diffusivity change against graphite
volume percent.

Wear Performance Analysis

Due to the ease of utilization and testing reproducibility, dry sand/rubber wheel test is usually adopted to assess the wear
performance for materials used in sliding and rolling wear application [6,31,32]. It is used to assess the wear performance of
the five graphitic white irons studied. As shown in Figure 8, the volume loss result has well differentiated the five studied
alloys. Overall, the volume loss is consistent with the Rockwell hardness measurement shown in Figure 6. Within all the
studied graphitic white irons, alloy 3Cr had the largest volume loss and alloy 9Cr had the best wear performance. It is worth
noting that the chromium content is not always helping on the wear resistance for metals. The wear property model in later
section also proved that graphite is also contributing to the wear resistance of the graphitic white irons.

Figure 8. Plot of volume loss from the dry sand/rubber wheel test for the five graphitic white irons studied.

Wear Resistance Investigation

Both of the wear scar and the cross section of the worn specimens were analyzed to study the wear mechanism of graphitic
white irons. Figure 9 shows the SEM images of the wear scar for all five studied graphitic white iron alloys. There are not
many hard phases in alloy 3Cr, so the matrix was worn down almost evenly. As the chromium content increases, a lot of hard
plate cementite were found in alloy 5Cr and they worked as wear “stoppers” during the wear test. As for alloy 7Cr, not only
the plate carbide but also M7C3 carbide worked as “stoppers” to decrease the wear rate. When the chromium content was
increased to 9Cr, more M7C3 carbides were found. While M7C3 is harder than plate cementite [5], M7C3 appears taller than
the plate cementite in the wear scar images in Figures 9(c) and 9(d). Finally, at 11Cr, more hard M7C3 carbides but few plate
cementite was found in the matrix.

1046 © 2019 by the Association for Iron & Steel Technology.

 300 μm 300 μm 300 μm
(a) (b) (c)

300 μm 300 μm
(d) (e)
Figure 9. SEM back scattered electron images showing the topography information of wear scars for alloy (a) 3Cr; (b) 5Cr;
(c) 7Cr; (d) 9Cr; (e) 11Cr.
As shown in Figure 10, differential interference contrast (DIC) images were taken from the cross section of the wear scars to
further prove the topography information shown in Figure 9. Similar to the SEM images in Figure 9, the DIC images from
the cross section revealed that the hard carbides sticking out worked as “stoppers” to inhibit the removal of matrix and
slowed down the wear rate during the test. Comparing the Figure 10(d) and Figure 10(e), the height differences between the
matrix and M7C3 carbides in alloy 11Cr was larger than those in alloy 9Cr, which is consistent with the volume loss
comparison shown in Figure 8. According to the previously published work on Plasma Transferred Arc (PTA) study, the
removal of the metal matrix due to lower hardness is the dominating wear mechanism in abrasive wear [14]. However,
inadequate bonding strength between the coating and substrate leads to the reduction of the performance for the coating
layers [15]. Similar phenomenon was also reported by Tolfree’s [16]. He found that when the hardness of a material reaches a
certain point, the wear resistance did not increase any more. Instead, the controlling factor of a material’s wear resistance
becomes the removal of the hard phase. Taking the above mentioned into consideration, one can conclude that the plate
cementite in alloy 9Cr works as a “buffer”, provided bonding strength between the matrix and the hard M7C3, and prevents
the matrix and the hard M7C3 from being worn out too quickly.

© 2019 by the Association for Iron & Steel Technology. 1047

 (a) (b) (c)

(d) (e)
Figure 10. DIC images taken from the cross section of the wear scars for alloy: (a) 3Cr; (b) 5Cr; (c) 7Cr; (d) 9Cr; (e) 11Cr.
The hard carbides sticking out of the bakelite (top black) show the topography information of different phases on the wear
scars after wear tests.
The graphite original sites were located on the carbon EDS mappings taken from the wear scars for all five graphitic white
irons studied. As shown in Figure 11, graphite flakes were partially abraded off, leaving the rest of the graphite flakes in the
original site. These original graphite sites can work as reservoirs to hold lubricant and slow down the wear rate during the
wear application [17]. In addition, the abraded graphite was also found on the wear scars manifested in the carbon EDS
mappings. As shown in Figure 12, the abraded graphite was distributed on the wear scars for all five studied graphitic white
irons. These abraded and dispersed graphite can work as lubricant and slow the wear rate further down during the wear
application [17]. On the other hand, graphite with smaller and uniformly dispersed flakes is intended for metal-to-metal wear
application to avoid the graphite flakes being totally pulled out and leaving big original graphite sites, because big reservoirs
may induce serve gouging failure and lubricant leakage to the wear systems. A range of preferred graphite flake size needs to
be determined in future’s study.

1048 © 2019 by the Association for Iron & Steel Technology.

 (a) (b) (c)

(d) (e)
Figure 11. Carbon EDS mapping taken from the wear scars of alloys: (a) 3Cr; (b) 5Cr; (c) 7Cr; (d) 9Cr; (e) 11Cr. The red
spots indicate graphite original sites.

(a) (b) (c)

(d) (e)
Figure 12. Carbon EDS mapping taken from the wear scars of alloys: (a) 3Cr; (b) 5Cr; (c) 7Cr; (d) 9Cr; (e) 11Cr. The red
spots indicate the abraded graphite dispersed on the wear scars.
Wear Property Model
To validate that graphite has a positive effect on the wear performance of graphitic white iron, the volume loss determined
from dry sand/rubber wheel test was plotted against their Rockwell hardness, as shown in Figure 13(a). Besides all five

© 2019 by the Association for Iron & Steel Technology. 1049

graphitic white irons tested, Hardox 400, Alloy Fe15Mo19Cr, Alloy 1 and Alloy 2 were also included in Figure 13(a) to
facilitate the model development. Hardox 400 is a commercially used wear-resistant steel. Alloy Fe15Mo19Cr is a premium
wear-resistant white iron that is currently used in metal-to-metal wear application. Alloy 1 and Alloy 2 are other graphite
containing white irons produced by the authors. Details for Alloy 1 and Alloy 2 will be published in a future article. It is
believed that there is a linear correlation between the volume loss and hardness for a similar type of material [3,36,37].
However, the volume loss versus hardness data in Figure 13(a) did not fall into a straight line. Instead, the data for graphitic
white irons fell into the lower left side of the plot. Since neither Hardox 400 nor alloy Fe15Mo19Cr contains graphite, a black
dashed line was created in Figure 13(a) to represent the linear relation for the regular wear resistant alloys. As alloy 7Cr,
Alloy 1 and Alloy 2 all contained approximately 6 vol.% graphite, a blue dashed line was created to show the linear relation
for materials containing approximately 6 vol.% graphite. As the black dashed line is approximately parallel to the blue
dashed line, one can conclude that introducing graphite pushes the linear relation to the low hardness but also low volume
loss region as shown by the arrow. Namely, graphitic white iron has a better wear resistance compared with the material
having the same hardness, which is a result of faster heat dispensation due to graphite and extra lubrication from the chipped-
off graphite.
As both the graphite and carbide help on the wear resistance for graphitic white iron, a numerical model was established to
quantitatively correlate the amount of graphite with the wear performance of graphitic white iron. As shown in Figure 13(b),
when both the graphite volume percent and the hardness were taken into account for volume, a linear relation can be
established. This equation can be used to mathematically predict the wear performance of any given hardness and graphite
volume percent in future study.

(a) (b)
Figure 13. Plots showing: (a) volume loss versus hardness of alloys studied; (b) volume loss as a function of alloy hardness
and graphite volume percent.

CONCLUSIONS

The microstructure, thermal diffusivity, and wear performance of the first generation of graphitic white irons have been
investigated. Thermal diffusivity analysis showed that introducing graphite flakes into white iron increased the thermal
diffusivity. Wear resistance analysis indicated that graphite had a positive contribution on the wear performance of graphitic
white irons. A numerical model was established by correlating hardness, graphite volume percent, and material volume loss.
Future work will focus on correlating the thermal diffusivity with the volume loss to optimize the graphite volume percent for
graphitic white irons to guide future alloy design.

ACKNOWLEDGEMENTS

This work was financially supported by Caterpillar Inc. The authors are grateful for the technical discussion with Dr. David
C. Van Aken. Logan Bader and Perrin W. Habecker are acknowledged for their assistance with the experiments and sample

1050 © 2019 by the Association for Iron & Steel Technology.

preparations. The FEI Helios NanoLab EBSD was obtained with a Major Research Instrumentation grant from the National
Science Foundation under contract DMR-0723128.

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1052 © 2019 by the Association for Iron & Steel Technology.