Materials Science and Engineering A 370 (2004) 213–217

Internal friction in martensitic, ferritic and bainitic carbon steel;

cold work effects
I. Tkalcec∗ , D. Mari
Institut de Physique de la Matière Complexe, Ecole Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, Switzerland

Received 12 July 2002

Abstract

We present the comparative analysis of the temperature dependent internal friction (IF) spectra for 1.23 wt.% carbon steel with martensitic,
bainitic or ferritic structure as well as cold-work effects. Samples that have a martensitic structure at room temperature show a characteristic
spectrum consisting of five peaks and an exponential background. Tempering at 800 K transforms the sample structure to a completely ferritic
one. All peaks are erased upon tempering, except the peak P5 identified as a Snoek–Köster (S-K) relaxation, the amplitude of which is
however drastically reduced. The Snoek–Köster peak is also present in the bainitic structure as well as in initial ferrite, but with an amplitude
much lower than in martensitic samples. Cold work performed on tempered samples at room temperature either by bending or roll milling is
followed by the formation of a very broad double peak between 200 and 300 K. A similar peak is also found in initial ferrite, which has been
subjected to heavy machining. A local minimum in the IF spectrum is found at the temperature of cold work and post-aging. This minimum
is the effect of dislocation pinning by carbon precipitates.
© 2003 Elsevier B.V. All rights reserved.

Keywords: Mechanical spectroscopy; Martensite; Ferrite; Snoek–Köster; Dislocations

1. Introduction (S-K) relaxation [4]. Thus, the presence of hydrogen trans-

Thermal treatments of steels with the same chemical com-
position may produce a broad variety of structures with
very different mechanical properties. In particular, a ferritic,
bainitic or martensitic structure along with iron carbides can
be obtained in carbon steels. Mechanical spectroscopy is
a particularly useful technique to investigate such structure
changes in the material.
Pure body centered cubic (BCC) materials such as Ta,
Nb, W, Mo and Fe exhibit relaxations associated with in-
ternal friction (IF) peaks identified as kink pair formation
on non-screw dislocations (␣-peak) [1] and on screw dis-
locations (␥-peak) [2]. The presence of light interstitial
atoms shifts the peaks observed in pure materials to higher
temperatures [3], as their movement influences the thermal
activation. The interaction of interstitials with kink pairs
formed on dislocations is generally called Snoek–Köster
∗ Corresponding author. Tel.: +41-21-693-3393;
fax: +41-21-693-4470.
E-mail address: iva.tkalcec@epfl.ch (I. Tkalcec).
forms the ␣-peak occurring in ␣-iron at 30 K for 1 Hz to
S-K(H) observed around 100 K [5]. Correspondingly, the
␥-peak is transformed to a S-K peak that appears around
500 K at 1 Hz [6]. The mechanical spectroscopy investiga-
tions available for martensitic steels are much less extended.
Three thermally activated IF peaks have been observed in
Fe–Ni–C virgin martensite at about 185, 215 and 255 K
for 1 Hz measurements [7,8]. The peaks observed at 185
and 255 K are attributed to the kink pair formation on
non-screw dislocations. The 215 K peak is attributed to the
interaction between non-screw dislocations and carbon in-
terstitials. Klems et al. [9] report the presence of a S-K peak
in martensite. The relaxation phenomena in martensitic car-
bon steel have been recently described by Bagramov et al.
[10].
This paper presents a comparative analysis of the internal
friction spectra of a high carbon steel thermally treated in
order to obtain most basic structures: the ferritic, bainitic
and martensitic ones. The effects of cold work are studied in
order to shed light on the relaxations that could be attributed
to dislocations.

0921-5093/$ – see front matter © 2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2003.04.004
214 I. Tkalcec, D. Mari / Materials Science and Engineering A 370 (2004) 213–217

Table 1
Chemical composition of base material (wt.%)
Element Fe C Cr Mn Si S P Ni Mo Cu Al

Content Bal. 1.23 0.64 0.34 0.22 0.006 0.006 0.07 0.02 0.10 0.018

2. Materials and experimental methods amplitudes is recorded. IF is calculated according to:

The material studied here is a high carbon tool steel
used for the production of files. The chemical composi-
tion is presented in Table 1. As a part of the heat treat-
ment, the material is normalized by annealing for 15 min
at 1150 K and subsequent air-cooling, in order to obtain a
ferritic structure with embedded spheroidized carbide par-
ticles. The material is then machined in file shape (bars
2.2 mm thick), and then thermally treated. Rapid quench-
ing after 15 min of austenitization at 1100 K produces a
fully martensitic ferrous phase. The structure of marten-
sitic samples (Fig. 1) consists of a matrix, made of plate
and lath martensite and less than 1% residual austenite
at the former grain boundaries, and of (Fe, Cr)3 C car-
bides (0.2–2 ␮m in diameter). Quenching to intermediate
temperature (720 K) after the austenitization and sub-
sequent air-cooling results in the formation of bainite,
a structure composed of fine aggregates of ferrite and
cementite.
Measurements of internal friction as a function of tem-
perature were made in the temperature range 80–800 K in
a vibrating reed setup (free–free). The sample is excited to
oscillate at the resonant frequency (∼1.5 kHz) and then the
number n of oscillations in free decay between two fixed


1 Ai
IF = ln (1)
nπ Ai+n
Heating and cooling rates used were 1 K min−1 and maximal
oscillation amplitude 2 × 10−7 .
3. Results
IF spectra for the martensitic, ferritic and bainitic structure
are shown in Fig. 2. The IF spectrum that characterizes the
martensitic structure has been discussed in detail previously
[10,11]. It consists of four relaxation peaks (P1 at 130 K,
P2 at 260 K, P4 at 510 K and P5 at 600 K for 2 kHz) and an
IF maximum (P3 at 380 K). Tempering at 800 K transforms
the sample structure into a ferritic one (Fig. 3). It consists
of ferritic grains and carbide particles of comparable size
(0.5–2 ␮m). The increased mobility of dislocations causes
a strong recrystallization producing polygonized cells. The
length of dislocations increases and the dislocation density
is reduced. All peaks are erased upon tempering except for
4

P2
-3 3
8x10
x10-4

2
P1 P5
Internal Friction

6
1

100 150 200 250 300 350

4 P4

martensitic
2 tempered martensitic
bainitic P3

P1 P2
0
100 200 300 400 500 600 700 800
Temperature [K]

Fig. 1. TEM image of martensitic structure with embedded (Fe, Cr)3 C Fig. 2. IF spectra for martensitic, tempered martensitic and bainitic struc-
carbide (on the left end of the image). Matrix is composed of plate and ture. Five peaks (full lines) and an exponential background (dashed line)
lath martensite and residual austenite visible as the dark lines between are visible in IF spectrum of martensite. P1 and P2 are magnified in the
the laths. inset.
 I. Tkalcec, D. Mari / Materials Science and Engineering A 370 (2004) 213–217 215

450x10-6
cold worked by roll milling (right scale) 1.3
cold worked by bending (left scale)
ferritic (left scale)
400
1.2

350
1.1
Internal Friction

x10
300
1.0

-3
250
0.9

200
0.8

150
0.7
150 200 250 300 350 400 450
Temperature [K]

Fig. 3. TEM image of tempered martensite. The structure is composed

Fig. 5. Effects of cold work on tempered martensite and ferrite. A broad
of carbides and ferritic recristallized grains of comparable size.
IF peak distribution ranging from 100 to 400 K is obtained. A local dip
with minimum at room temperature (arrow) is observed.

the peak P5. After tempering, the peak is found at a temper-

ature 20 K higher, with an amplitude reduced by 90%. The the internal friction spectra below 400 K (Fig. 5). Spectra
same peak is present in the bainitic structure as well as in recorded in first heating after cooling to 100 K show the
the primary ferrite (Fig. 4), and it is further decreased by formation of a very broad peak between 100 and 400 K.
tempering of these materials. The same feature is seen in initial ferritic samples which
Samples tempered at 800 K are cold worked at room tem- can be considered as heavily cold worked during the pro-
perature either by bending (ε = 0.2%) or roll milling (ε =
11%). The effects of cold work are most clearly visible in
-6
500x10
A
1.4x10-3 tempered martensitic
ferritic
bainitic B
400
1.2
Internal Friction

1.0 300
Internal Friction

0.8
200
E
0.6

100
0.4
100 150 200 250 300 350 400 450
Temperature [K]
0.2
450 500 550 600 650 700 750 Fig. 6. Time and temperature effects of cold work and post-aging on
Temperature [K] the IF minimum. (A) cold worked and post-aged for 30 min at room
temperature; (B) cold worked and post-aged for 15 h at 273 K; (C) cold
Fig. 4. IF peak found in tempered martensite, bainite and ferrite, corre- worked and post-aged for 20 h at 320 K; (D) cold worked and post-aged
sponding to peak P5 in martensite. The amplitude of these peaks is about for 8 h at room temperature; (E) cold worked and post-aged for 3.5 days
10 times smaller than P5. at 325 K. Arrows mark the positions of IF minima.
216 I. Tkalcec, D. Mari / Materials Science and Engineering A 370 (2004) 213–217
duction process. The common feature in all three spectra
is a local minimum of IF at room temperature, separat-
ing the broad lower temperature part from a sharper peak
above room temperature. Measurements performed at low
frequency (1.5 Hz) in a torsion pendulum show that the posi-
tion of the minimum does not depend on the oscillation fre-
quency. To clarify the origin of the local minimum appear-
ing after cold work, experiments were performed changing
the cold work temperature and the time of aging at that tem-
perature (post-aging). The results are shown at Fig. 6. With-
out a sufficiently long post-aging after cold work (curve A
in Fig. 6), no minimum is observed. On the other hand, too
long post-aging leads to an important reduction of the IF and
the double peak is no longer visible (curve E). A further de-
crease of IF is observed in heating above 390 K (which co-
incides with P3 in the martensitic structure). The clear shift
of the local minimum to the temperature of post-aging is ob-
served for the sample cold worked and post-aged at 273 K
(curve B). For the sample cold worked and post-aged for
20 h at 320 K (curve C), the minimum is shifted to 320 K,
but is much less pronounced.
4. Discussion
The peak present around 600 K in all IF measurements is
identified [10,11] as a Snoek–Köster peak, and is strikingly
high for the martensite. The amplitude of the peak (∆/2 =
4.5 × 10−3 ) is related to the density of dislocations Λ and
their average free length L̄ according to [12]:
2
b2 L̄
∆= (2)
12γJ
where b is the Burgers vector, γ the line tension of a dislo-
cation, and J the elastic compliance of the material (inverse
of its Young modulus E = 214 GPa). Taking γ = 0.5µb2 ,
µ being a shear modulus of the material (83 GPa), and L̄ =
20 nm as an estimation from TEM images, Eq. (2) gives the
dislocation density in martensite  = 5 × 1013 m−2 . This
dislocation density is close to that of a cold worked metal.
The reduction of the peak after tempering is likely to be as-
sociated with the dislocation recovery. Taking L̄ = 100 nm
and the amplitude of the peak measured in tempered marten-
site, ∆/2 = 4.5 × 10−4 , the calculated value for the disloca-
tion density is Λ = 2 × 1011 m−2 , which seems reasonable
looking at the TEM images.
The peak P2 observed in the IF spectrum of the marten-
sitic sample, and the broad increase of IF between 100
and 400 K created by cold work performed on the ferritic
samples, probably have the same origin. Being sensitive
to cold work, the peak is clearly related to the disloca-
tion movement. Screw dislocations should become mobile
at much higher temperatures, when P5 is activated. There-
fore, a possible interpretation of this peak is a relaxation
of Snoek–Köster type [8], involving non-screw dislocations
and interstitial carbon, which is present in a material in
large quantities and is already very mobile around room
temperature. Upon cold work, dislocations break away from
the pinning points issued from aging and simultaneously
new ones are created. The result is the formation of a very
broad peak due to the wide distribution of free disloca-
tion lengths. For the formation of a minimum in the peak
we suggest a mechanism of dislocations–point defects in-
teraction. Post-aging after cold work leads to the pinning
of dislocations, reducing again their mobility. Presuming
that the post-aging has not been too long, the dislocations
can break away from pinning points, probably carbon, upon
cooling, due to the internal stresses that change with tem-
perature. As they pass back through their initial positions
during heating, their mobility is first reduced by the car-
bon atmosphere creating a local minimum. Increasing the
temperature they can break away from carbon atoms and/or
drag them causing the abrupt increase of the IF. The pin-
ning effect is similar to that observed by Vincent [13] in ul-
trasonic attenuation in aluminium submitted to an external
stress. The effect is smaller for the sample cold worked and
post aged at 320 K. In this case weaker pinning points like
carbon interstitials or clusters are already very mobile at the
temperature where the dip should appear and the effect is
decreased.
5. Conclusions
The IF spectrum of the martensite is very rich, showing
four relaxation peaks and an IF maximum. The peak lo-
cated at 600 K for 1.5 kHz is interpreted as the Snoek–Köster
peak involving screw dislocations and interstitial carbon. It
is present also in a bainitic and ferritic structure, but with
the amplitude 10 times smaller, due to the lower dislocation
density.
Cold work performed on a ferritic structure results in the
formation of a very broad peak between 100 and 400 K,
with a local minimum at the temperature of aging after
cold-work. The peak can be explained as a Snoek–Köster
relaxation involving non-screw dislocations and carbon in-
terstitials, and the local minimum as the effect of disloca-
tion pinning by carbon precipitates. The shift of the dislo-
cation position due to changes of internal stress with tem-
perature produces a sort of memory effect of the aging
temperature.
Acknowledgements
The authors would like to thank C. Azcoitia and S.
Crevoiserat for TEM images, and G. Gremaud for helpful
discussions. They furthermore acknowledge the company
UMV SA, Vallorbe (Switzerland) for support and sample
supply and the Swiss “Commission pour la Technologie et
l’Innovation” (project 4743.1) for financial support.
 I. Tkalcec, D. Mari / Materials Science and Engineering A 370 (2004) 213–217
References
[1] A. Seeger, C. Wüthrich, Nuovo Cim. 33B (1976) 39.
[2] H. Schultz, Mater. Sci. Eng. A141 (1991) 149.
[3] A. Seeger, Phys. Stat. Sol. (a) 55 (1979) 457.
[4] M. Weller, J. Phys. 44 (1983) C9.
[5] J. San Juan, G. Fantozzi, M.L. No, C. Esnouf, J. Phys. F 17 (1987)
837.
[6] L.B. Magalas, J.F. Dufresne, P. Moser, J. Phys. C5-42 (1981) 127.
[7] Y. Liu, Acta Metal. Mater. 41 (1993) 3277.
[8] Y. Liu, Acta Metal. Mater. 42 (1994) 621.
217
[9] G.J. Klems, R.E. Miner, F.A. Hultgren, R. Gibala, Metal. Trans. A
7 (1976) 839.
[10] R. Bagramov, D. Mari, W. Benoit, Phil. Mag. A 81 (2001) 2797.
[11] I. Tkalcec, D. Mari, Defect Diffusion Forum 203–205 (2002) 253.
[12] G. Gremaud, Dislocation—Point Defect Interactions, in: R. Schaller,
G. Fantozzi, G. Gremaud (Eds.), Mechanical Spectroscopy Q-1 2001
with Applications to Materials Science, Trans Tech Publications,
Uetikon-Zuerich, Switzerland, 2001, p. 178.
[13] A. Vincent, Réalisation d’un ensamble de mesures ultrasonores; Ap-
plication à l’étude des défauts cristallins dans l’aluminium, Ph.D.
Thesis Universite Claude Bernard de Lyon, Lyon, 1973, pp. 112–124.