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J Nondestruct Eval (2007) 26: 7987

DOI 10.1007/s10921-007-0022-0

Characterization of Dual-Phase Steels Using Magnetic


Barkhausen Noise Technique
M. Kaplan C.H. Gr M. Erdogan

Published online: 11 October 2007


Springer Science+Business Media, LLC 2007

Abstract The aim of this work is to nondestructively char- Introduction


acterize the dual phase steels using the Magnetic Barkhausen
Noise (MBN) method. By quenching of AISI 8620 steel Dual-phase steels (DPS) were introduced into the market as
new generation of high-strength low alloy steels in 1970s,
specimens having two different starting microstructures,
and are currently materials of commercial interest for the au-
from various intercritical annealing temperatures (ICAT) in
tomotive industry. The dual phase microstructure consists of
the ferrite-austenite region, the microstructures consisting a dispersion of 2025% hard martensite particles in a soft,
of different volume fractions of martensite with morpho- ductile ferrite matrix. The hard martensite laths/plates pro-
logical variations have been obtained. The microstructures vide substantial strengthening while the ductile ferrite ma-
were first conventionally characterized by metallographical trix gives good formability. DPS can be modified by chang-
investigations and hardness tests. Then, the MBN measure- ing the martensite content via thermal or thermomechanical
ments were performed using a SCAN commercial system. processing to obtain higher strength or higher ductility.
Good correlations between the martensite volume fraction, DPS are conventionally produced by partial austenitiza-
hardness and MBN emission have been obtained. MBN sig- tion of low carbon steels within the ferrite-austenite phase
region, followed by rapid cooling to transform the austen-
nal height clearly decreased as the ICAT, therefore the vol-
ite to martensite. In addition to martensite, the resulting mi-
ume fraction of martensite increased. The effect of the initial
crostructures may consist of epitaxial ferrite, pearlite, bai-
microstructure prior to intercritical annealing has also been nite or retained austenite depending on cooling rates and in-
differentiated by the MBN measurements. It has been con- tercritical annealing temperatures used [1]. The amount of
cluded that MBN method can be used as a useful tool for austenite present during the intercritical annealing is con-
nondestructive characterization of dual phase steels. trolled by the annealing temperature, which also controls
the carbon content and hardenability of the austenite. The
critical cooling rates need to avoid pearlite and bainite, and
Keywords Dual phase steel Microstructure Magnetic at which the required amount of austenite transforms to
Barkhausen noise martensite, are factors in the economic production of DPS
[2].
The effect of varying heat treatment temperature, alloy
content, and cooling rate on DPS has been studied by sev-
M. Kaplan C.H. Gr () eral researchers. It has been found that an increase in ten-
Metallurgical and Materials Engineering Department, Middle sile strength of DPS could be obtained through an increase
East Tech. University, 06531 Ankara, Turkey in martensite volume fraction as well as by an increase in
e-mail: chgur@metu.edu.tr the aspect ratio of martensite [3]. Effects of martensite vol-
M. Erdogan
ume fraction and the morphology of the phases have been
Materials Division, Metallurgy Education Department, Faculty of reported [4]. After examining tensile and impact properties
Technical Education, Gazi University, 06500 Ankara, Turkey of high-martensite dual phase steels it has been concluded
80 J Nondestruct Eval (2007) 26: 7987

that equal amount of finely dispersed martensite phases ex- the maximum noise amplitude and the corresponding mag-
hibit the optimum combination of high strength and ductility netic field. Various studies have been published on the char-
with high impact toughness [5]. Finer initial microstructure acterization of steel microstructures using MBN technique.
produced a dual phase structure with more martensite than It has been reported that the peak of MBN signal from low-
the coarser one after annealing at low temperature and par- C steels decreases with grain size since the number of do-
ticular at the slower cooling rates [1]. It has been reported mains and walls that can move is much bigger in the fine
that martensite content was significantly dependent on the grain structures [8]. MBN responses of fully pearlitic, fully
heat treatment condition or the initial microstructure of the pearlitic, and ferritic-pearlitic steels have been differentiated
steel. There was a marginally higher amount of martensite [9]. Measurements performed on plain carbon steels have
in the sample normalized prior to intercritical annealing as shown that the maximum MBN signal was detected in the
compared to the annealed one. The wear behavior is also steel with a composition very close to the eutectoid compo-
dependent on these parameters [6]. A survey on DPS and sition. As the C-content increased the MBN signal increased
micromechanical modeling has been already published [7]. for hypo-eutectoid samples, but decreased for the hyper-
Manufacturing industry spends a great deal of effort eutectoid samples [10]. Transformations between austenite
in determining and ensuring the desired microstructure of and martensite during cold work and annealing have been
steels. In practice, the microstructure is usually determined also studied using MBN measurements [11]. The effect of
by metallographic techniques and hardness test where cer- precipitation of Fe-carbides and Cr-Mo carbides at constant
temperature as a function of tempering time has been inves-
tain regions of the representative samples are investigated
tigated on various steels, using micromagnetic parameters
following the preparation stage. Since these methods are
[12]. Important changes in MBN response have been ob-
time consuming and a hundred percent inspection is im-
served in relation to martensite decomposition after temper-
possible, there is always an interest to develop nonde-
ing of steels between 100o C and 600o C [13, 14]. Okazaki
structive techniques capable of rapid evaluation. Magnetic
et al. has studied detectability of stress-induced marten-
Barkhausen Noise (MBN) method has been considered as
site phase in ferromagnetic shape memory alloy by MBN
an evaluation technique of considerable importance for mi-
method [15]. Effect of hardness and composition gradient
crostructural and mechanical characterization of steels. The on Barkhausen emission in case hardened steels has been
advantages of this method over other methods are that it is reported [16]. Sensitivity of the MBN technique in compar-
a nondestructive economical technique, and can be easily ison to the sound velocity measurements for the characteri-
used to evaluate samples of various shape and sizes and un- zation of steel microstructures, namely as-quenched marten-
der different external conditions. site, tempered martensite, fine pearlite-ferrite, and coarse
Ferromagnetic materials consist of very small magnetic pearlite-ferrite has been studied [17]. It has been reported
regions called domains. Each domain is magnetized along a that MBN measurements could be successfully used for the
certain crystallographic easy direction of magnetization, and characterization of ferrite-martensite steels [18]. Magnetic
domains are separated from one another by domain walls. measurements have been effectively used for studying the
The magnetization process is characterized by the hystere- microstructural changes of duplex stainless steels, i.e., de-
sis curve that is indeed made up of small steps represent- composition of delta-ferrite [19].
ing the movement of the magnetic domains under the effect The aim of the study is to contribute to the studies on
of an external magnetic field. These discontinuous changes the non-destructive characterization of dual phase steels.
are a result of the Barkhausen effect, i.e. small magnetiza- By quenching of AISI 8620 specimens having two dif-
tion jumps due to domain walls becoming pinned and re- ferent starting microstructures (ferrite-pearlite and fully
leased from microstructural obstacles such as grain bound- martensite), from various intercritical annealing tempera-
aries, second phase particles, and inclusions. This results in tures (732o C, 738o C, 758o C) in the ferrite-austenite region,
a change in magnetization within the material and will in- the microstructures consisting of different volume fractions
duce an electrical pulse in a pick-up coil. Amplification of of martensite and morphology have been obtained; and then,
these signals produces noise, which can be observed on an MBN measurement results were compared with the metal-
oscilloscope or spectrum analyzer. The measurement depth lographic investigations and hardness values.
for MBN usually varies between 0.01 to 1.5 mm from the
surface depending on the frequency range of the Barkhausen
signals, conductivity and permeability of the material. Experimental Study
MBN emission is affected by the microstructural state
Material and Samples
and residual stresses in the material. Usually, the envelope
of the signal is plotted as a function of the applied mag- Carbon content was the main concern in the selection
netic field. The envelope generally has a single-peak shape of the material. At low annealing temperatures the car-
and can be characterized by different parameters, such as bon content determines the amount of carbide formation
J Nondestruct Eval (2007) 26: 7987 81

(a) (b)
Fig. 1 Initial microstructures of the AISI 8620 samples prior to intercritical annealing: a Q series (ferrite-pearlite), b QQ series (fully martensite)

which adversely effects the Barkhausen measurements. AISI group, the samples were austenitized at 900o C for 20 min
8620 steel (0.2%C, 0.81%Mn, 0.17%Si, 0.60%Cr, 0.56%Ni, and oil quenched to obtain an initial microstructure of low
0.23%Mo) was used in the experimental studies. Samples of carbon, lath martensite; and these samples were labeled as
13 mm diameter and 5 mm in thickness were cut from a series QQ. Following these heat treatments, the samples
cold-rolled rod by a CNC machine. were heated at the intercritical temperatures chosen for 20
minutes allowing austenite to nucleate and grow. The sam-
Initial Microstructures and Heat Treatments ples were then oil quenched at ambient temperature to obtain
martensite in a ferrite matrix.
The preliminary investigation was to determine the limit
The Hereaus annealing furnace having an accuracy of
temperatures (A1 and A3 ) of the intercritical ferrite-austenite
5C was used in the annealing process. K-type thermocou-
region of AISI 8620, and dependence of martensite volume
ples were spot-welded at the longitudinal center of the sam-
fraction on intercritical annealing temperature. By using (1)
and (2) [20] A1 was approximated as 716C and A3 as ple. Samples were then mounted on and fixed with wires to
896C. the sample holder. Thermocouple wires were long enough
in order to keep the cold junction as far as possible from
A1 = 723 20.7 Mn 6.9 Ni + 29.1 Si the furnace. The effect of the heat differences on the sam-
ple was minimized by placing the sample perpendicular to
+ 16.9 Cr + 290 As + 6.38 W, (1)
the horizontal mid-line of the furnace. During the annealing
A3 = 910 203 C 1/2
15.2 Ni + 44.7 Si process a pre-selected zone inside the furnace was used for
every sample. The temperature of the sample was checked
+ 104 V + 31.5 Mo + 13.1 W. (2)
continuously on the temperature display and any alteration
In order to show the feasibility of MBN measurements for in the annealing temperature was balanced and kept within
industrial dual phase steels, the intercritical annealing was 2 C by displacing the sample incrementally between the
conducted with temperatures close to A1 . However, the steel high and low temperature zones.
type and the heat treatment set-up did not allow produc-
ing the martensite volume fraction (MVF) that is lower than Metallographic Inspections and Hardness Test
25%. As a result of some preliminary studies, three intercrit-
ical temperatures of 732, 738, and 758o C were selected. Heat treated samples were prepared for metallographic in-
Martensitic morphology in ferritic matrix is determined spection with standard grinding and polishing techniques.
mainly by initial microstructure obtained prior to the in- To eliminate effect of the decarburized layer formed during
tercritical annealing. Two different dispersions of marten- heat treatment, about 0.5 mm layer was removed from the
site were produced by applying two different treatments surface of the sample by careful grinding.
prior to dual phase heat treatment (Fig. 1). Dual phase mi- All samples were etched using 2% Nital (%2 HNO3 +
crostructures derived from the as-received initial microstruc- %98 C2 H5 OH). After etching, martensite was observed as
ture (ferrite-pearlite) were labeled as series Q. In the other light brown and ferrite as white in color during microscopic
82 J Nondestruct Eval (2007) 26: 7987

inspection. To differentiate the ferrite-martensite interface of austenite which transforms to martensite during quench-
more clearly an additional etching with sodium meta bi- ing increases with increasing intercritical annealing tem-
sulphite (%3 Na2 S2 O5 + %97 H2 O) was applied. At the perature. Besides, the morphology and the amount of the
final stage martensite was observed as dark brown. The martensite formed show differences in the Q and QQ series
martensite volume fraction of each sample was determined samples that were treated at the same ICAT. For the samples
by point counting. MVF values were obtained from arith- having ferritic-pearlitic initial structure (Q series), needle-
metical means of values derived from the 5 images of 500 like martensite phase (dark gray regions) exists in the ferrite
magnification taken from different points on the samples. matrix while the ferrite grains seem unchanged since they
Leica QM550MW imaging system was used for the opti- did not experience any structural change during intercriti-
cal metallography whereas Jeol JSM 6400 was used for the cal annealing. However, in the case of the samples of QQ
scanning electron microscopy. series having martensitic initial structure, the whole struc-
Hardness of the specimens (HRc) was measured by In- ture transforms to ferrite and austenite during the intercrit-
stron Wolpert hardness tester using a 150 kg load. The hard- ical annealing. Then, quenching from the austenite-ferrite
ness values given are the average of at least five measure- region, parallel narrow laths within prior austenite grains
ments on each sample, with the total scatter being no more causes finer dispersion of acicular martensite in a ferrite ma-
than 2 HRC. trix, and gives rise to a high density of fresh dislocations in
the ferrite grains due to the accommodation strains caused
Magnetic Barkhausen Noise Measurement by the martensitic transformation.
Figures 3 and 4 shows the martensite volume fraction and
Any residual magnetism that may influence MBN emis- hardness values of the dual-phase steel samples that were
sion in the specimens was absent since all specimens were obtained by considering two different initial microstructures
heated at temperatures which are above the Curie temper-
and applying three different intercritical annealing temper-
ature. Barkhausen noise signal was measured with SCAN
atures. It is clearly seen that the initial microstructure prior
500-2 (StressTech) equipment. Measurements were carried
to intercritical annealing significantly affect the MVF, and
out by using the sensor, S1-138-13-01. An excitation mag-
therefore hardness of the DPS. For both series it was ob-
netic field with a frequency of 125 Hz was used. Magne-
served that the higher the ICAT the higher MVF in the dual-
tizing voltage, which adjusts the magnitude of magnetiz-
phase steel. For a given ICAT, martensitic initial microstruc-
ing field applied to the specimen, was set to 10 V. Sam-
ture (QQ series) always resulted in higher hardness and
pling frequency, the parameter determining how many sam-
MVF with a finer martensite morphology compared to the
ples per second are stored for signal analysis was set as
ferritic-pearlitic one (Q series). These results are in agree-
2 MHz. Number of bursts, the parameter determining how
many magnetizing half cycles will be stored for signal analy- ment with those of the previous study which has reported
sis, was set to the highest possible number of half cycles, that increasing the ICAT increases the austenite volume frac-
as 186. The detected Barkhausen emission signals were fil- tion, but also decreases its carbon content and so reduces its
tered (pass-band: 0.1-1000 kHz) and amplified (voltage gain hardenability; and a finer starting microstructure produces
of 20 dB). more martensite than the coarser one [1]. The ferrite growth
The root mean square (RMS) value of the voltage signal rate is dependent upon the degree of under cooling, carbon
detected from the specimens is given as an output in SCAN diffusion rate and carbon concentration in the austenite at
measurements. RMS voltage, which is obtained by averag- the austenite-ferrite interface. Small austenite regions must
ing the MBN signal over the time for magnetization reversal, become enriched in carbon more rapidly than large particles,
gives the average of the Barkhausen activity. The MBN sig- with respect to amount of ferrite growth. The average ferrite
nals were also plotted as a function of the magnetizing field growth rate will be considerably slower for fine dispersions
over a hysteresis cycle in order to produce the MBN finger- than coarse ones when the cooling rate is not a variable.
print. Therefore, less ferrite and more martensite will form and this
difference will increase with increasing austenite dispersion.
On the other hand, the size and distribution of the marten-
Results and Discussion site obtained on quenching reflects the scale of the initial
microstructure. During intercritical annealing of the QQ se-
Samples having similar microstructural properties to those ries more austenite nucleated at lath interfaces, lath colony
of industrial dual phase steels were tried to be produced boundaries and prior austenite grain boundaries. Therefore,
from AISI 8620 steel. In order to minimize uncertainty in the martensite regions formed upon quenching are smaller and
measurements, all samples were cut from the same rod. The has a finer morphology. The results are also in agreement
optical micrographs in Fig. 2 demonstrate that the amount with those of the previous works [35, 21].
J Nondestruct Eval (2007) 26: 7987 83

(a) Q732 (b) QQ732

(c) Q738 (d) QQ738

(e) Q758 (f) QQ758


Fig. 2 Optical micrographs of the AISI 8620 dual-phase steel samples
84 J Nondestruct Eval (2007) 26: 7987

!       It is known that magnetic parameters derived from
 Barkhausen emission signals that are dependent upon do-
 main wall movement and domain nucleation, are strongly
affected by the changes in the microstructure since the di-

mensions of the magnetic domains and the domain walls
 are comparable with those of phases, grains, precipitates,
 etc. Figure 5 shows the correlation between RMS value of

MBN signal and MVF, whereas Fig. 6 gives the correla-
tion between RMS value of MBN signal and hardness of
      the dual-phase steel samples. As the MVF of the specimen,
  and consequently hardness increases, the MBN peak height
decreases proportionally.
Fig. 3 Martensite volume fraction of the AISI 8620 dual-phase steel
samples
In ferrite, the growth of domains is easy since few weak
obstacles impede domain wall motions inside ferrite grains.
 Therefore, pure ferritic samples would show very high MBN
emission. In the case of ferrite-martensite combination, the

MBN emission will be affected from the magnetic properties
 of both phases. Due to the small size of martensite needles,
  

 the domain wall energy plays an important role, so the rela-



tive volume occupied by a wall is larger than in the other
phases of steel. Under the effect of an external magnetic

field, the resistance to the growing domains in martensite
 phase is very high since domain walls are pinned due to high
dislocation density. Domain wall displacements are low and
     
domain walls are difficult to create since the reversal of mag-

 
netization requires a strong field. Hence, the MBN emission
Fig. 4 Hardness (HRc) values of the AISI 8620 dual-phase steel sam- caused by martensite is very weak. Micro residual stresses in
ples the martensite needles, which are inherent to the diffusion-
less austenite-martensite transformation, may also influence
the MBN emission to some extent.

Fig. 5 Correlation between


RMS value of Barkhausen
emission and martensite volume
fraction (MVF) of the AISI
8620 dual-phase steel samples
J Nondestruct Eval (2007) 26: 7987 85
Fig. 6 Correlation between
RMS value of Barkhausen
emission and hardness (HRc) of
the AISI 8620 dual-phase steel
samples

Another measurement parameter used for evaluation is structure, compared with Q series intercritically annealed at
the MBN fingerprint, on which the peak position indicates the same temperature. Also, the MBN peak positions of the
the magnetic field at which the peak value of the MBN signal QQ series move to a higher relative magnetic excitation as
is located. The fact that ferrite and pearlite microstructures the result of higher MVF and finer martensite morphology.
have a strong Barkhausen activity located at a low magnetic In the case of the samples of QQ series, the whole structure
field, whereas a martensite microstructure, which is classi- transforms to ferrite and austenite during the intercritical an-
fied as hard magnetic, has a low Barkhausen emission lo- nealing. Then, quenching from the austenite-ferrite region,
cated at a high field has been widely accepted in the litera- narrow laths within prior austenite grains causes finer dis-
ture [1214, 17]. Concerning DPS, it can be expected that persion of acicular martensite in a ferrite matrix, and gives
the MBN fingerprint exhibits both characteristics of ferrite rise to a high density of fresh dislocations in the ferrite
and martensite. Thus, a low amplitude peak being far away grains. This results in an additional difficulty to the nucle-
from zero can be considered as an evidence for the increase ation and movement of domains, and therefore, lower MBN
in martensite content. However, the overall response cannot emissions located at relatively higher magnetic excitation
be estimated simply from the individual responses of ferrite fields.
and martensite due to the differences in their carbon content
and the correlation phenomena between the single phase and
dual phase steels. It is also known that MBN measurement
of martensite is directly linked to its carbon content; i.e., as Conclusions
the carbon content of martensite increases the peak height
of MBN signal decreases, and the signal shifts to the higher By quenching of AISI 8620 specimens having two dif-
magnetic excitation fields. The relative RMS voltage as a ferent starting microstructures (ferrite-pearlite and fully
function of relative magnetic excitation graphs for the sam- martensite), from various intercritical annealing temper-
ples in Q-series and QQ-series are given in Fig. 7a and b. atures (ICAT) namely 732o C, 738o C, and 758o C in the
As the MVF increased, a remarkable reduction in the peak ferrite-austenite region, the dual-phase steels consisting
height of the MBN signal, and, a slight shift in the peak posi- of different volume fractions of martensite and morphol-
tion towards higher magnetic excitation field were observed. ogy have been obtained. The microstructures and hardness
The results showed that the ferrite peak is dominant, and the values were determined by conventional destructive tech-
changes in the amount of martensite can be determined from niques. The measurements of the Magnetic Barkhausen
the corresponding changes in the MBN peak height. Noise (MBN) were performed by using SCAN sensor con-
In Fig. 7 it is also seen that the RMS voltage decreases nectors. After evaluating and comparing the results, the fol-
prominently for QQ series, having fully martensitic initial lowing conclusions can be drawn:
86 J Nondestruct Eval (2007) 26: 7987
Fig. 7 MBN profile of the AISI
8620 dual-phase steel samples
(relative RMS voltage as a
function of relative magnetic
excitation): a Q-series,
b QQ-series

(a)

(b)

The martensite and ferrite contents of the dual phase height has been obtained. As the ICAT, therefore the vol-
steels are dependent on the ICAT chosen. The higher the ume fraction of martensite increases, MBN peak height of
intercritical temperature the higher the amount of marten- ferrite clearly decreases. Since ferrite signal peak is dom-
site. inant, the shift in the peak position is less sensitive to the
Variations at the MBN peak height can be used for non- variations in the martensite content.
destructive determination of the martensite/ferrite con- The initial microstructure affects the morphology and the
tent in dual phase steels. A good correlation between amount of the martensite formed in dual phase steels.
the martensite volume fraction, hardness and MBN peak Martensitic initial microstructure results in higher amount
J Nondestruct Eval (2007) 26: 7987 87

of martensite that is finely distributed in the ferrite matrix 9. Clapham, L., Jagadish, C., Atherton, D.L.: The influence of
causing higher amount of dislocations, compared to those pearlite on Barkhausen noise generation in plain carbon steels.
of the ferritic-pearlitic one. Both the height and position Acta Metal. Mater. 39, 155562 (1991)
10. Koo, K.M., Yau, M.Y., Dickon, H.L., Ng, Lo, C.C.H.: Charac-
of the MBN signal seems to be sensitive to such varia- terization of pearlite grains in plain carbon steel by Barkhausen
tions in the microstructure of the dual-phase steels. The emission. Mater. Sci. Eng. A 351, 310315 (2003)
finer martensite and higher dislocation density in ferrite 11. Meszaros, I., Kaldor, M., Hidasi, B.: Barkhausen noise energy
grains result in an additional difficulty to the nucleation measurement method for characterizing the ferromagnetic ratio of
and movement of domains, and therefore, lower MBN alloys. Mater. Sci. Forum 210213, 3138 (1996)
emissions located at higher magnetic excitation fields. 12. Moorthy, V., Vaidyanathan, S., Raj, B., Jayakumar, T., Kashyap,
B.P.: Insight into the microstructural characterization of ferritic
Acknowledgements Authors are thankful to Dr. Ibrahim Cam steels using micromagnetic parameters. Metall. Mater. Trans. A
(METU-Central Laboratory) for the MBN measurements, to Mr. 31, 105365 (2000)
Volkan Kilicli for the heat treatments; and to Mr. Kemal Davut for 13. Saquet, O., Chicois, J., Vincent, A.: BN from plain carbon steel:
the metallographic analysis. influence of the microstructure. Mater. Sci. Eng. A 269, 7382
(1999)
14. Gr, C.H., Cam, I.: Investigation of as-quenched and tempered
commercial steels by Magnetic Barkhausen Noise method. Int. J.
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