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P. Sampathkumaran
Chikkakuntappa Ranganathaiah
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Subramanyam Seetharamu
Central Power Research Institute
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Wear
journal homepage: www.elsevier.com/locate/wear
The effects of manganese content and mould size on abrasion and slurry erosion
behaviour of chromiummanganese iron systems investigated by positron
lifetime spectroscopy
P. Sampathkumaran a , C. Ranganathaiah b, , S. Seetharamu a , Kishore c
a
a r t i c l e
i n f o
Article history:
Received 25 July 2008
Received in revised form 16 March 2009
Accepted 1 June 2009
Available online 11 June 2009
Keywords:
Cast iron
Hardness
Slurry erosion
Abrasion
Thermal effects
Power generation
a b s t r a c t
Abrasion and slurry erosion behaviour of chromiummanganese iron samples with chromium (Cr) in the
range 1619% and manganese (Mn) at 5 and 10% levels have been characterized for hardness followed
by microstructural examination using optical and scanning electron microscopy. Positron lifetime studies have been conducted to understand the defects/microporosity inuence on the microstructure. The
samples were heat treated and characterized to understand the structural transformations in the matrix.
The data reveals that hardness decreased with increase in Mn content from 5 to 10% in the rst instance
and then increase in the section size in the other case, irrespective of the sample conditions. The abrasion
and slurry erosion losses show increase with increase in the section size as well as with increase in Mn
content. The positron results show that as hardness increases from as-cast to heat treated sample, the
positron trapping rate and hence defect concentration showed opposite trend as expected. So a good
correlation between defects concentration and the hardness has been observed. These ndings also corroborate well with the microstructural features obtained from optical and scanning electron microscopy.
2009 Elsevier B.V. All rights reserved.
1. Introduction
The wear resistant materials used in thermal power generation plants are susceptible to metal wastage due to the presence of
quartz in coal. Generally, ferrous based wear resistance materials
are used [1,2]. Among them, high chromium iron is one such material as it contains hard (M7 C3 ) carbides in a martensitic matrix, but
it suffers from the point of poor impact resistance. For improving
the impact behaviour, manganese is added to Cr iron as an austenite
stabilizing agent. From literature reports we found that use of Mn in
Cr iron only up to 4.4% beyond which there is hardly any published
report [3] on this aspect. Further, the inuence of microstructure
on the wear and mechanical properties in high Cr irons has been
investigated by various researchers [4,5]. However, the information
on this aspect in CrMn iron system is scanty. Also there is no report
on a new and novel NDT technique such as positron lifetime spectroscopy (PLS) being used to characterize the CrMn iron samples
for defects quantication, as PLS is a powerful and well established
tool for studying the defects and their concentration levels in any
Corresponding author.
E-mail address: cr@physics.uni-mysore.ac.in (C. Ranganathaiah).
0043-1648/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.wear.2009.06.001
1559
2.5. Hardness
The rubber wheel abrasion tests set up used in the present work
is shown in Fig. 1 and measurements were done as per ASTM G-65
guidelines. In this test, the abrasive silica sand (AFS 60 grade) was
fed at the interface between the rotating rubber wheel (200 rpm)
2.6. Microstructure
NIKON optical metallurgical microscope was used to study the
microstructural features. An image analyzer was employed to determine the carbide volume fraction in the samples. XRD technique
was adopted to measure the retained austenite content using
RIGAKU X-ray analyzer. The ner surface features on select samples were examined using LEICA scanning electron microscope
(SEM).
2.7. Positron lifetime spectroscopy
Positron (e+ ) is the antiparticle of electron (e ). The electromagnetic interaction between electrons and positrons results in
the annihilation of e+ e pairs in which the total energy of the
annihilating pair is transferred to quanta of the electromagnetic
eld-photons ( rays). This process is called positron annihilation
in a material medium. The positron lifetime in a material medium
is dened as the survival time of positron in the medium before it
annihilates. Therefore, the lifetime of a positron is directly related
to the electron density it will run into and annihilates. The electron density of the material governs positron lifetimes in materials;
higher the electron density, shorter is the lifetime [810]. Measurement of positron lifetime constitutes what is known as positron
lifetime spectroscopy (PLS).
Positrons from a radioactive source (commonly 22 Na) are
injected into a material medium. Positrons loose their kinetic
energy and reach thermal energy in a very short time (around 1 ps),
after interacting with medium through inelastic collision processes.
During the thermalized stage, a positron, picks up an electron
from the medium and annihilate producing predominantly two
gamma photons. The annihilation may be from a free state called
free positron annihilation, or get trapped in to defects present in
crystalline, crystalline-amorphous interface regions and then annihilate called trapped annihilation [810]. Since positrons localize
in defects [810] and annihilate from such sites, their lifetime and
intensity provide the information of the nature of the defects and
concentration. Hence this NDT technique found immense use over
the last few decades in the study of microstructural behaviour of
metals, alloys, polymers, etc. [810].
Positron annihilation lifetime spectra were recorded for the
present samples using positron lifetime spectrometer. The spectrometer consists of a fastfast coincidence system with BaF2
scintillators coupled to photo multiplier tubes type XP2020/Q with
quartz window as detectors. The BaF2 conical shaped scintillators
were used to achieve better time resolution. The two identical
pieces of the sample were placed on either side of a 17 Ci 22 Na
positron source, deposited on a pure Kapton foil of 0.0127 mm
thickness. This sample-source sandwich was placed between the
two detectors of the spectrometer to acquire the lifetime spectrum. The 60 Co prompt time spectrum gave 180 ps as the resolution
function. However, to have increased count rate, the spectrometer was operated at 220 ps [14,15]. All lifetime measurements were
performed at room temperature with more than a million counts
under each spectrum recorded in a time of 12 h. Source correction term and resolution functions were estimated from the lifetime
of annealed aluminum using the program RESOLUTION [16]. Since
the single Gaussian resolution function did not yield convergence,
the resolution function was resolved further into three Gaussian
components, which gave quick and good convergence. The net
resolution function for this however, was 220 ps. Therefore three
Gaussian resolution functions were used in the present analysis
of positron lifetime spectra in all the samples. All spectra were
analyzed into two lifetime components with the help of the computer program PATFIT-88 [16] with proper source and background
corrections.
The positron lifetime spectrum consists of a sum of exponential decay components with the lifetime i and their intensities Ii .
Positrons annihilate from the delocalized ground state in a perfect
crystal and a single positron lifetime will be measured, = b (b:
bulk). In the presence of defects of a distinct type, positrons may get
localized in the defects and annihilate with a second lifetime called
trapped positron lifetime 2 = d (d: defect). This lifetime is larger
than b for open-volume defects, such as vacancies, due to decrease
in the electron density in defect compared to bulk material. The lifetime spectrum then consists, of two components. Present lifetime
spectra in CrMn iron systems were resolved in to two lifetime components 1 and 2 with corresponding intensities I1 and I2 . From
these lifetime components and intensities, the positron trapping
rate at defects, K, is determined by calculating the average positron
lifetime as
av =
I1 1 + I2 2
I1 + I2
(1)
where 1 is b and 2 = d .
The positron trapping rate K is proportional to the defect concentration Cd of the system under study [8,9]. The proportionality
constant is the trapping coefcient, and is related to Cd as given
below.
Cd =
1
K
=
b
av
b
d av
(2)
Fig. 3. SEM picture of the silica sand used in abrasion and slurry erosion experiments.
1561
5M12 and 5M40 samples are shown in Figs. 7a and b and 8a and b,
respectively. Fig. 9a and b display the optical features of 10M12 in
respect of as-cast and heat treated samples. The SEM features of
heat-treated 5M12 and 10M12 samples are displayed in Fig. 10ac,
respectively.
3.1. Inuence of manganese content and section size increase on
positron lifetime parameters.
The mean range of positrons in the CrMn iron systems estimated [9] to be 32.93 m. For thick section size samples, positrons
are expected to probe the bulk of the system. Hence, in the
absence of any defects, the mean lifetime in these samples shall
be 104 1012 s or 104 ps. If a higher mean lifetime for sample than
the expected value of 104 ps indicates that there are defects in the
sample. The theoretical estimate of the expected defect lifetime for
these systems assuming monovacancy type defects turns out to be
183 ps, but as we can see from Table 3, it is observed that the lifetime is in the range 200226 ps, which is certainly higher. In the
analysis we xed the rst lifetime component to a value of 107 ps
which is the positron lifetime in defect free iron which is the major
component of the system studied here. This certainly points out to
the fact that the defects are not of mono vacancy type but of bigger
size evolved during the moulding process of the CrMnFe system
and these vary depending upon the section size also due to variation in heat transfer process. Although the mean range of positrons
in all these systems is the same, but their defect lifetime varies with
respect to the thickness as explained below. For each sample section
size, heat transfer process appears to be different with the result;
a different microstructure is evolved as the sample gets cooled. It
is observed that a consistent reduction in mean lifetime for samples after heat treatment (Table 3) indicates that some defects are
indeed annealed out. As the fraction of positrons probing the single
1
2
3
4
5
Sample designation
5M12
5M24
5M40
10M12
10M24
Composition (wt.%)
C
Mn
Si
Cr
Ni
Mo
2.36
2.39
2.55
2.32
2.35
4.5
4.6
4.8
9.7
9.7
2.69
2.78
2.10
1.90
1.85
18.58
18.62
17.90
17.65
17.60
0.91
0.92
0.81
0.80
0.82
1.87
1.82
1.90
1.85
1.80
0.046
0.044
0.057
0.040
0.040
0.080
0.090
0.075
0.090
0.085
Table 2
Abrasion, slurry erosion data and microstructural content of chromiummanganese iron samples.
Sl. no.
1
2
3
4
5
Sample designation
5M12
5M24
5M40
10M12
10M24
Impact (J)
AC
HT
AC
HT
AC
HT
AC
HT
0.99
1.18
1.69
1.58
1.91
0.71
.95
1.57
1.31
1.68
7.58
7.74
9.61
8.60
9.74
7.02
7.21
8.99
8.16
9.42
15.2
17.5
20.8
19.3
22.6
12.5
14.7
19.3
16.8
20.1
1.4
1.8
2.8
2.6
2.5
2.6
2.6
4.0
4.3
4.5
Table 3
Positron lifetime parameters of chromium manganese iron samples.
Sl. no.
Sample
PAS parameters ( 1 = 107 ps was xed in the analysis which corresponds to positron lifetime in Fe system)
I1 0.1 (%)
1
2
3
4
5
5M12
5M24
5M40
10M12
10M24
2 0.02 (ps)
I2 0.1 (%)
avg (ps)
K (109 )
AC
HT
AC
HT
AC
HT
AC
HT
AC
HT
67.7
67.5
66.8
68.8
68.6
69.9
69.2
67.4
69.9
69.5
200.3
215.3
218.4
217.2
226.2
185.3
197.2
201.3
214.6
224.0
32.3
32.5
33.2
31.2
31.4
30.1
30.8
32.6
30.0
30.5
137.0
142.2
144.4
141.3
144.3
130.0
134.7
137.7
139.2
143.0
4.45
4.52
4.64
4.23
4.24
4.02
4.22
4.52
4.08
4.14
Fig. 5. (a) Plot of change in hardness (%) with respect to change in trapping rate (%)
from AC to HT of 5M12, 5M24 and 5M40 samples and (b) plot of change in hardness
(%) with respect to change in trapping rate (%) from AC to HT of 10M12 and 10M24
samples.
Fig. 6. (a) Plot of change in abrasion and slurry erosion losses (%) with respect change
in trapping rate (%) from AC to HT of 5M12, 5M24 and 5M40 samples and (b) plot
of change in abrasion and slurry erosion losses (%) with respect change in trapping
rate (%) from AC to HT of 10M12 and 10M24 samples.
1563
Fig. 10. (a) SEM photograph of HT 5% manganese bearing 12 mm section size sample
at 2000 and (b) SEM photograph of HT 5% manganese bearing 12 mm section size
sample at 4000, (c) SEM photograph of HT 10% manganese bearing 12 mm section
size sample at 2000.
1565