archives of civil and mechanical engineering 17 (2017) 926–934

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Original Research Article

Nitrogen as an alloying element improving material

properties of the high carbon cast steel for ball mill
liner plates

Józef Gawlik a, Jerzy Schmidt a,*, Tomasz Nowak b, Zygmunt Wójcicki a,

Andrzej Zagórski c
a
Cracow University of Technology, Jana Pawła II 37 Street, Cracow, Poland
b
ABB Corporate Research, Starowislna 13A Street, Cracow, Poland
c
Warsaw University of Technology, Woloska 141 Street, Warsaw, Poland

article info abstract

Article history: This paper presents an experimental analysis, which was carried out to evaluate the
Received 16 January 2017 addition of nitrogen as an element complementing a chemical composition used for such
Accepted 15 April 2017 cast parts. It has been demonstrated that nitrogen is very advantageous in the process of
Available online austenitizing and quenching, improving the stability and homogeneity of the alloy struc-
ture. Plates used as a lining of rotary mills operating in cement plants are castings, which
Keywords: acquire their properties mainly through proper heat treatment. Together with an appropri-
High carbon chromium cast steel ate microstructure and chemical composition, correct heat treatment allow to improve the
Casting wear resistance and significantly reduce the abrasive corrosion. Extensive investigations
Nitrogen enabled establishing an optimum nitrogen content in the chemical composition of thick-
Wear resistance walled castings used in cement industry. Results of experiments, managed for the steel of
Heat treatment ledeburate type containing 0.8–1.2% of carbon, have found that the optimal level of nitrogen
is in the amount of 0.07–0.10%. The proposed modification helped to reduce the amount of
an expensive chromium, increase the hardness of the material (by about 2 HRC to 4 HRC),
and to achieve the uniform microstructure and hardness, which noticeably improved the
lifetime of the rotary mills plates.
© 2017 Politechnika Wrocławska. Published by Elsevier Sp. z o.o. All rights reserved.

media in mills and wearing-out of mill elements, especially

1. Introduction
While grinding is unavoidable in nearly all mineral processing,
it has tremendous impact on the economics of comminution
facilities worldwide. The main contributors to the cost
structure of mineral processing are a consumption of grinding
liner plates [1,2]. The wear out process arises as a consequence
of complex interaction between variables related to processing
conditions and the characteristics of the media [3]. Due to high
efficiency of the industrial mills used in cement industry, there
are also high energies and friction forces generated. The
objects analyzed in this paper, the thick-walled plates lining

* Corresponding author.
E-mail address: schmidt@mech.pk.edu.pl (J. Schmidt).
http://dx.doi.org/10.1016/j.acme.2017.04.007
1644-9665/© 2017 Politechnika Wrocławska. Published by Elsevier Sp. z o.o. All rights reserved.
 archives of civil and mechanical engineering 17 (2017) 926–934
the inner surfaces of the drums of ball mills used in cement
plants, may be affected by the three basic wear mechanisms –
impact, abrasion and corrosion, which simultaneously influ-
ence mass loss in mill components [4]. The effect of the
abrasive mineral on alloy performance in the ball mill has been
studied by Gates et al. [5]. Their results showed, that only very
hard (above 630 HV) martensitic steels and white cast irons
offer large performance benefits when grinding relatively soft
or weak abrasives (Mohs hardness less than about 6). The
researchers studied the relationship between wear perfor-
mance and microstructure [6,7], hardness [8,9], or impact
toughness. For example, Efremenko and co-workers [10]
suggest, that the best wear performance is achieved with
martensitic structure in steels containing not less than 13 wt.%
Cr, while others [11] recommend that the medium chromium
cast iron ball type in the heat-treated condition has the desired
microstructure – mechanical property – wear performance
combination. Azizi reminds that abrasive corrosion was
observed on high carbon chromium steel ball surface, and
that the main corrosion mechanism type for steel balls is
pitting [12]. This article refers to the steel of ledeburite type,
which is mainly used for cutting and shaping tools [13], as well
as high pressure moulds. While used as hammers and jaws in
crushers, ledeburitic steel offers good resistance against
abrasive wear, if proper steel microstructure and its heat
treatment are ensured. Properly heat treated material after the
effective sorbitization process should have uniform hardness
in the range of 46 HRC to 50 HRC [14]. The literature provides
comprehensive reference for investigation of the heat treat-
ment process and the microstructure on and mechanical
properties of steels and cast iron [15–17]. For example, Tao and
co-workers noticed that additional carbides and nitrides
precipitations introduce changes in dislocation structure
and the formation of sub-grains occurring during the process
of tempering [18]. Similarly, Kaputkina [19] and Prokoskina [20]
studied the structure and properties formed as a result of
martensitic transformations during cooling and subsequent
tempering, in metastable carbon- and nitrogen-containing
austenitic iron alloys. The presence of carbides and nitrides
also makes the dispersion hardening of the austenite and
martensite more effective [21,22]. Gavriljuk, who studied
crystal structure of austenite and martensite in nitrogen-
and carbon-containing iron alloys, explains that carbon assists
the covalent character of interatomic bonds, whereas nitrogen
increases the concentration of conduction electrons [23,24]. In
the ledeburitic steels the total volume fraction of carbides is
normally large, and during heating a large amount of carbides
dissolve. But non-dissolved carbides are left behind in the
austenite matrix, which influence the mechanical properties
and improves wear resistance [25,26]. The combined effect of
nitrogen and chromium content on the microstructures of cast
alloys was investigated by Suyalatu and co-workers [27]. They
found that ultimate tensile strength and elongation at break of
the nitrogen-containing alloys increased with increasing
chromium content. It was explained by the change of the
deformation mechanism from strain-induced martensite
transformation to another form, such as twinning or disloca-
tion slip. Their studies, which were focused on the effect of
nitrogen content, did not describe however the thick-walled
castings.
927
This work described in this paper investigates the influence
of nitrogen on the heat treatment process, what results in
improved wear resistance. It concludes that in ledeburitic
steels having between 0.8% and 1.2% C, addition of nitrogen
may significantly reduce the need for chromium, molybdenum
or vanadium content. It has tremendous impact on the
economy of thick-walled castings, used especially in cement
industry, where operating conditions set very demanding
requirements for the extended lifetime of the rotary mill
components.
2. Subject of the study and methodology of
experimentation
2.1. Background information
The study refers to the cast steel material used for ball mill
liner plates. Ball mills are commonly used in cement industry
to process sintered minerals (clinker), and mix them with
gypsum. The typical ball mill is a large rotating drum (about
4.5 m of diameter) containing grinding media, normally steel
balls. As the drum rotates, once every couple of seconds, the
motion of the balls crushes the clinker. The drum is generally
divided into two or three chambers, with different size of
grinding media. The walls of the chambers are waved by liners,
composed of liner plates. The application of the liners
increases the energy of the grinding balls and improves the
efficiency of the milling process. However, during grinding the
cement becomes hot, what additionally accelerates the wear
of the mill elements. The object of the study, a single liner
plate, is shown in Fig. 1.
2.2. Studied materials
The analysis compares two proposals for the material of liner
plates: the standard composition of the ledeburitic steel
(without nitrogen addition) – designated by the symbol ‘‘M’’,
and the high carbon cast steel with nitrogen addition – marked
by the symbol ‘‘N’’. The objective of the study was to driven by
the fact that thick-walled structures, such as liner plates, made
of standard material, may not be properly heat treated across
the whole thickness.
To check the effect of nitrogen addition to high carbon cast
steel, melts for research and industrial tests were prepared
(Table 1).
In the alloy marked by ‘‘N’’, nitrogen dissolved in cast steel
acts as a strong austenite stabilizing element, which allows its
supercooling to low temperatures. In the case of analyzed cast
liner plates, the delayed austenite decomposition, particularly
in the temperature range of 800–650 8C, is important because it
allows slower cooling during quenching. The solubility of
nitrogen in high-chromium alloys is technologically sufficient.
The application of chromium nitride alloys (CrN) or ferroalloys
(e.g. nitrided ferrochromium, FeCrN) enables dissolving up to
0.3% of N in the steel containing 12–17% Cr. The component
alloys introduced to the melted alloy were added at the end of
melting process. According to the experimental results
managed by authors, for a perceivable steel hardenability
improvement, the optimal addition of nitrogen is in an
928 archives of civil and mechanical engineering 17 (2017) 926–934

Fig. 1 – Geometrical model of the analyzed liner plate.

amount of 0.07–0.10%. Larger amounts of nitrogen can result in scenarios of the heat treatment process. The detailed FEM
an excessive formation of the retained austenite, which will study was performed in order to evaluate how different
complicate the process of heat treatment. cooling technologies affect the quenching results. The
The test samples were prepared in two forms. For all numerical calculations showed that forced cooling strategies
laboratory tests (including dilatometric studies, hardness, for gaseous medium could provide sufficient cooling rate to
impact strength, and wear resistance measurements), as well ensure correct microstructure. However, it was realized that
as heat treatment analysis, metallography, microstructure, quenching of such castings requires usage of special measures
and nondestructive testing by acoustic emission – the ensuring rapid cooling in a jet of coolant (a gaseous medium, or
f55 mm
300 mm ingots were prepared. The samples needed water), and it will definitely generate high temperature
for particular tests, as required by respective standards (e.g. 3- gradients.
point bending), were cut out of these ingots. While the full- Next, in order to limit thermal gradients caused by very fast
scale liner plates were cast for testing in the industrial cooling, and to improve alloy hardenability, the addition of the
conditions. They were also subjected to the heat treatment nitrogen, as an alloying element, was investigated. The
analysis and hardness measurements. experimentation started with dilatometric studies, followed
by heat treatment trials and testing of mechanical properties
2.3. Methodology of the experimentation (hardness, impact strength), and ended with microstructure
analysis as well as wear resistance assessments.
At first, the analyzed part, made of the standard composition Dilatometic tests for both analyzed materials (M and N)
of the ledeburitic steel, was evaluated theoretically in different were performed at a constant austenitizing temperature of
1060 8C. Dimensional changes were recorded during heating
and cooling. During heating, the values of ferrite-austenite
transformation temperatures Ac1 and Ac3 were measured. For
Table 1 – The content of main elements in the tested material M, Ac1 = 775 8C and Ac3 = 935 8C, for material N,
materials, alloy M and alloy N.
Ac1 = 825 8C and Ac3 = 955 8C. During cooling, the time–
Alloy Content elements (wt.%) temperature range of austenite decomposition into ferrite,
necessary to determine the critical cooling rate during
C Cr Ni Mn Si N
quenching, was determined.
M 1.12 17.2 0.24 0.95 0.31 Trials of heat treatment were conducted mainly to
N 1.17 16.5 0.59 0.95 0.34 0.096
demonstrate the effect of the addition of nitrogen on the cast
 archives of civil and mechanical engineering 17 (2017) 926–934 929

1100
steel hardenability and possibility to obtain better perfor-
1000
mance of this material after a complete heat treatment cycle. A
900
complete heat treatment cycle of the mill liner components
800
included quenching and tempering. Both materials tested, i.e.

Temperature [°C]
700
materials M and N, were subjected to the same course of heat
600
treatment. 500
Quenching was conducted in a special vacuum furnace for 400 Air, Natural (0.05 °C/sec)
heating and cooling. The batch of castings for quenching 300 Air, Forced (0.1 °C/sec)
consisted of 6 cast mill liner elements and 8 test rods, and it 200 Water, Natural (0.6 °C/sec)
was austenitized in two steps, at a temperature of 1050 8C and 100 Water, Jet (3.2 °C/sec)
1000 8C, respectively, and next cooled with nitrogen at an 0
overpressure of 2 bar. The cooling conditions were measured 1 10 100 1000 10000
LOG Time [sec]
with two thermocouples – one placed on the casting surface
and another placed in an opening made in the test casting
Fig. 2 – Temperature [8C] inside the analyzed sample for
sub-surface zone. Thus measured cooling rate amounted to
different cooling scenarios.
about 0.4 8C/s for the temperature range from 980 8C to
240 8C. Mechanical properties, measured by hardness and
impact strength, were taken before and after the tempering
process.
Later, the microstructure analysis was performed, in order generate significant temperate gradients across the wall
to demonstrate the concentration of carbon and chromium for thickness (Fig. 3).
two analyzed materials. It was followed by non-destructive Therefore, in order to reduce thermal gradients caused by
testing, supported by acoustic emission method, to confirm rapid cooling, and, at the same time, improve alloy hard-
the improvement in material morphology driven by addition enability, an attempt was made to evaluate the use of nitrogen
of nitrogen. Finally, destructive tests (wear resistant measure- as an alloying element. The critical cooling rates were
ments) were executed to show the real benefits of nitrogen measured by dilatometric studies.
addition.
3.2. Dilatometric studies of phase transformations

3. Achieved results As the measurements disclosed, the structure composed of

martensite and retained austenite could be achieved with the
3.1. FEM analysis of heat treatment process critical cooling rate of about 0.16 8C/s for material N. While for
material M, this rate must be much faster, roughly 0.25 8C/s.
The numerical analysis of the heat treatment process was The results of measurements are presented in a graphical form
performed with the help of the general purpose FEM system, of the time–temperature-transformation relationships for
ABAQUS by Dassault Systèmes. The material properties, such both materials tested (Fig. 4). Graph shows marked region of
as thermal conductivity, density and specific heat capacity the austenite decomposition into ferrite and pearlite. Based on
were first measured in the range between 20 8C and 1000 8C, the results obtained, it was found that the addition of nitrogen
and introduced into the system as temperature functions. has a positive effect on the hardenability of material N. The
Boundary conditions, in the form of convection coefficients – start of martensitic transformation is illustrated by Ms points.
also functions of temperature – were set individually for all
surfaces, depending on their orientation (vertical/horizontal),
position within the part (front, side, back, top, bottom), and
scenario (natural/forced cooling, and air/water medium). For
example, the convection coefficients for natural cooling in air
ranged between 1.72 W/m2 K and 10.24 W/m2 K, and in case of
forced cooling with air speed of 10 m/s – between 23 W/m2 K
and 42 W/m2 K. While for water conditions the convection
coefficients reached the levels of 100 W/m2 K and 1000 W/m2 K
– for natural and jet cooling, respectively.
The results describing the temperature in the hottest point
of liner plate for different cooling scenarios are shown in Fig. 2.
Interesting to note, that natural cooling in air requires about
200 000 s to reach 200 8C, while forced cooling in the same
medium shortens it to 70 900 s only. These results correspond
to cooling rates of 0.05 8C/s and 0.1 8C/s, respectively. And they
are however too slow to provide required microstructure of the
liner plate material.
On the other hand, in case of water medium, the cooling Fig. 3 – Temperature profile [8C] within the sample – water
rates are much higher (up to 3.2 8C/s for jet), and they can jet conditions, after 50 s.
930 archives of civil and mechanical engineering 17 (2017) 926–934
Fig. 4 – Changes in the temperature of the start of martensitic transformation (Ms) vs. cooling rate, for alloy M (left) and N
(right).
For material N containing nitrogen, this line is running in the
temperature range lower than for material M.
After the austenitizing process carried out in a vacuum
furnace, the cooling in a forced jet of nitrogen gas at an
overpressure of 2 bar was performed. The parameters of the
cooling process were optimized by FEM-based numerical
simulations. During the real process, the actual cooling rates
were measured with a thermocouple. The temperature
reading in a subsurface layer of the examined casting
corresponded to the level of 0.4 8C/s.
3.3. Hardness after quenching
After quenching, the resulting hardness was measured on the
surface of the test castings and test rods. The measurements
taken at different depth levels from the surface show that
hardness of material N is very homogeneous across the whole
thickness, 58.1  0.8 HRC (Fig. 5). The results indicate that the
Fig. 5 – Hardness [HRC] vs. distance from the surface [mm],
alloy N, cast liner.
same rate of cooling promotes material N, which is more
effective in the heat treatment process – the reference material
M generally had the lower hardness, by about 2 HRC to 3 HRC
(measured at the same points).
3.4. Tempering
Studies covered quenched samples of each material tempered
within the temperature range of 495–525 8C. As a result of the
tests, the tempering time and temperature were established
for use in further experiments. Based on the results obtained,
the tempering temperature of 505 8C and the process time of
225 min were recommended. After the tempering process,
hardness measurements were taken once again. The achieved
result of 50 HRC was considered sufficient for complete
transformation of the remaining martensite into a post-
martensitic structure.
The impact strength values were examined for both alloys
and stable values were obtained – alloy M: 5.5  0.5 J; and alloy
N: 4.85  0.7 J. The Charpy impact tests were executed
according to the standard procedure described by PN-EN ISO
148-1 norm.
3.5. Microstructure analysis
The microstructure examinations showed that the base
material M in as-cast state contained well visible dendrites
of chromium ferrite with carbides of the M3C type and M7C3
type. The interdendritic spaces were filled with the trans-
formed ledeburite, in which there were slender rods of primary
cementite forming a cementite lattice (Fig. 6).
The dendritic system of matrix formation has resulted in
microsegregation of carbon and chromium. One should
remember that local differences in the content of C and Cr
may result in the quenching treatment not be able to produce a
homogeneous martensitic structure (what manifests in lower
resistance to abrasive wear). To examine local variations in the
carbon and chromium content, microanalysis (EDS) of the
 archives of civil and mechanical engineering 17 (2017) 926–934
Fig. 6 – An image of the microstructure in as-cast state,
alloy M.
Fig. 7 – Image of the microstructure with marked
concentrations of carbon, alloy M.
chemical composition was performed. The qualitative studies
were made using variations in the color intensity of structural
images, for carbon and chromium concentrations, respective-
ly. Fig. 7 presents the dendritic structure of the material with
light-outlined interdendritic areas of high carbon concentra-
Fig. 8 – An image of the microstructure with marked
locations of measurements, as-cast state, alloy M.
931
Table 2 – The content of major alloying elements (C, Cr) at
marked locations in the image of microstructure, num-
bers 1–5, alloy M.
Location (Fig. 6) Content of alloying
element (wt.%)
C Cr
1 1.7 21.6
2 0.8 12.3
3 0.7 13.6
4 2.5 31.1
5 1.9 23.8
tion. The numerous bright points in the field of dendrites are
just carbides and the precipitates of primary cementite. In the
dendrites of the matrix, the M7C3 carbide is prevalent.
To demonstrate differences in the concentration of carbon
and chromium, the contents of C and Cr were measured in
various places, as marked in Fig. 8, and presented in Table 2.
Analysis of the results shows that in as-cast state there are
no significant differences in the distribution of C and Cr
concentration in both materials tested (thus N was not
presented). The disclosed differences in concentration be-
tween the interdendritic zones and alloy matrix indicate the
need for transfer of some carbon and chromium amounts to
the matrix.
In the structure of material M are more pronounced
martensitic areas near the dendrite edges characterized by
the same distribution as areas with high carbon content. The
structure of material N consisting of martensite and retained
austenite is more homogeneous, and the disproportions
between the center and the periphery of dendrites are smaller.
The structure of material N after tempering is quite aligned,
but not free from the precipitates of exploded martensite
which indicates the need for additional tempering.
After two-step tempering, in accordance with the pre-
assumed objective of the toughening process, material N
finally acquires the structure of tempered martensite, as
shown in Fig. 9.
The X-ray diffractometry, performed for both materials
exposed to the properly managed heat treatment process,
allowed to reveal a low content of the retained austenite at
alloy M (2.22%), and even lower at alloy N (0.82%).
3.6. Nondestructive testing
In addition to the evaluation of the destruction process, the
acoustic emission (AE) technique was used. The three-point
bending was performed on the samples 10 mm

10 mm
160 mm, and the AE signals were recorded during
sample loading. Tests at constant rate of deformation were
performed until the sample fracture. The AE activity,
expressed by signal amplitude distribution for materials M
and N, is shown in Fig. 10.
The loading curve for material N is more linear, and a bit
shorten in time – the sample breaks at almost the same force,
but at slightly lower deformation. Since the material is more
elastic and flows less – much lower activity of AE signals (in
terms of number of signals and their amplitudes) was observed
932 archives of civil and mechanical engineering 17 (2017) 926–934

Table 3 – Wear resistant test (alloy M and alloy N).

Alloy Weight reduction (g)

Test rods Cast liners

M 0.1210 0.1107
N 0.1099 0.1032

during the loading. It confirms the improvement in material

morphology, driven by the addition of nitrogen.

3.7. Destructive testing

Fig. 9 – An image of the microstructure after quenching and
two-step tempering, alloy N.
The material structure, which was improved by the addition of
nitrogen, offers better and more stable mechanical properties
achieved after heat treatment. In order to validate the
proposed composition of an alloy with nitrogen and the

Fig. 10 – Three-point bending test for alloy M (top) and N (bottom) – AE activity (amplitude level) vs. load.
 archives of civil and mechanical engineering 17 (2017) 926–934
corresponding heat treatment process, the laboratory wear
tests were performed. The study was managed for 30 min at
rotating speed of 1800 rpm, according to the procedure described
by GOST 23.208-79 norm (‘‘Wear resistance testing of materials
by friction against loosely fixed abrasive particles’’).
The results shown in Table 3 exhibit noticeable higher wear
resistance of alloy N (more than 10%), comparing to the
reference alloy without the addition of nitrogen. Moreover, the
application of nitrogen allows to reduce the content of
chromium, and supplementary elements.
4. Discussion on results and conclusions
In this paper the improvement of the wear resistance of the
thick-walled castings – components of ball mills used in
cement plants, has been studied. It was proved that the
addition of nitrogen (about 0.10% N) to cast steel containing
1.2% C and about 16% Cr facilitates easier quenching of thick-
walled elements, and produces more homogeneous structure.
The proposed modification increased the hardness of the
analyzed material by about 2 HRC to 4 HRC, which positively
affected the lifetime of the rotary mills plates. Similar effects
were reported already by other authors, but for the structures
of standard thickness (cold working tools for cutting and
shaping). It has been shown that relatively small addition of
nitrogen (between 0.07% and 0.10%) was good enough to
provide appropriate cooling rates 0.16 8C/s, lower than in the
case of the cast steel without the addition of nitrogen
(0.25 8C/s). The addition of nitrogen to the cast steel
noticeable lowered the value of Ms point. The area of the
austenite was extended which facilitates martensitic change.
It resulted in the uniform hardness distribution, and the
proper microstructure, measured on the cross-sectional area
of the experimental castings.
The achieved results are in-line with findings of other
researches, confirming improved material properties for the
chromium steels with nitrogen content. For example Kaput-
kina and Prokoskina clarified that during cooling carbon
promotes the a-martensite formation, whereas nitrogen
promotes the e-martensite formation. Similar conclusions
were drawn by Gavriljuk and Widermann, explaining that that
carbon assists the covalent character of interatomic bonds,
whereas nitrogen increases the concentration of conduction
electrons. The combined, positive effect of nitrogen and
chromium content on the microstructures of cast alloys was
also confirmed by Suyalatu and co-workes, who explained the
synergy between nitrogen and chromium contents by the
formation of e-phase.
The conclusions of provided in this paper are also
supported by FEM studies and full-scale tests. The measure-
ments performed on the real samples confirmed the effects of
the heat treatment process, as predicted by numerical
analysis. The proposed chemical composition and parame-
ters of the heat treatment process were optimized for the
given design of rotary mill elements (bulky castings
250 mm
100 mm, with a unit weight of about 50 kg).
Laboratory tests proved that even reasonably small
addition of nitrogen (about 0.10%) improves the lifetime
of the steel plates used in rotary mills about 10–15%. It has
933
noticeable impact on the economy of thick-walled struc-
tures used in mineral processing industry. If properly
designed and processed, cast steels with an addition of
nitrogen will show their benefits also in other demanding
applications.
Funding body
Polish Ministry of Science and Higher Education (Project IN2/
11/181853).
Acknowledgment
The authors express their appreciation for the financial
support of the Polish Ministry of Science and Higher Education
granted to this study (Project IN2/11/181853).
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