Materials Science Forum Vol 753 (2013) pp 522-525 Online: 2013-03-26

© (2013) Trans Tech Publications, Switzerland

doi:10.4028/www.scientific.net/MSF.753.522

Effect of inter-pass ageing during cold rolling on magnetic properties of

Fe-3%Si
AMORIM, Dirceni Souza Costa1,a; CUNHA, Marco Antônio2,b;
SANTOS, Dagoberto Brandão3,c; BRANDÃO, João Henrique4,d
and GONZALEZ, Berenice Mendonça5,e
1
Research Department, Aperam South America, Praça 1º Maio, 09, Centro, Timóteo, MG, Brazil.
2
Department of Materials Engineering, Centro Universitário do Leste de Minas Gerais (Unileste),
Av. Tancredo Neves, 3500, B. Universitário, Coronel Fabriciano, MG, Brazil.
3,4,5
Department of Metallurgical and Materials Engineering, Universidade Federal de Minas Gerais,
Av. Antônio Carlos, 6627, Pampulha, Belo Horizonte, MG, Brazil.
a
dirceni.amorim@aperam.com, bmarco.cunha@unilestemg.br, cdsantos@demet.ufmg.br,
d
jhbrandao.88@yahoo.com, egonzalez@demet.ufmg.br

Keywords: Grain oriented electrical steel; Inter-pass ageing treatment; Primary recrystallization;
Secondary recrystallization; Goss texture; Magnetic and Mechanical properties.

Abstract. The effects of inter-pass ageing temperature during cold rolling on structure, magnetic
properties and mechanical properties of high permeability grain oriented electrical steel was
studied. The samples were processed in a single-stage cold rolling to 0.27 mm thickness, with 88 %
reduction, without and with inter-pass ageing treatment in order to determine the magnetic
properties. To determine the changes in mechanical properties due to strain ageing, the samples
underwent overlapped ageing, after pre-strain by rolling, under the same conditions of inter-pass
ageing and then were subjected to tensile test. The effect of strain ageing was more pronounced in
the thickness of 0.7 mm and the largest variation in yield strength was at 200 °C in all evaluated
thicknesses. At this temperature the largest amount of 110 〈001〉 orientation after primary
recrystallization was also observed, as well as the lowest final grain size and consequently the best
results of core loss. The magnetic induction had almost no alterations.

Introduction
Generally, high permeability grain oriented electrical steel is cold rolled by reversing mill and
maintained a few minutes between cold rolling passes. The use of short time inter-pass ageing
treatment has been reported to improve the magnetic properties in the high permeability grain
oriented electrical steel by increasing the amount of 110 〈001〉 component in the primary
recrystallization texture [1,2]. In another reports it has been said that inter-pass aging also makes
sharp 012 〈001〉 primary texture [3].
The inter-pass ageing, through the effects of static strain ageing, influences the plastic
deformation due to pinning action of solute C and N on dislocations formed in the cold rolling [4,5].
This fact favors the occurrence of shear bands in cold rolling. The Goss oriented grains nucleate in
shear bands [6,7], which enhance the development of this component in the primary
recrystallization texture to originate the secondary recrystallization grains with Goss orientation,
thus refining the grain size after secondary recrystallization and ensuring high performance to the
final product due to the reduction of core loss.
In this paper the variation on the magnetic properties of high permeability grain oriented
electrical steel, after its processing by varying the inter-pass ageing temperature during cold rolling,
is associated with the structure, texture and mechanical properties changes due to strain ageing
treatment performed on the samples after pre-straining by rolling.

Experimental Procedure
The starting material was a 2.3 mm thick hot rolled band of high permeability grain oriented silicon
steel manufactured industrially, which chemical composition is given in table 1.

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 Materials Science Forum Vol. 753 523

Table 1 – Chemical composition of specimen [wt %]

C Mn Si Al N Sn S Cu P
0.075 0.059 3.101 0.023 0.007 0.081 0.024 0.104 0.007
In the laboratory study, the hot bands were annealed at 1105 °C for 100 s and quenched in
boiling water. The annealed hot bands were cold rolled in a Fenn pilot reversible mill to 0.27 mm,
with 88 % reduction, without and with inter-pass ageing treatments in the temperature range of
100~300 °C at intervals of 50 °C, for ten minutes, at intermediate gauges of 1.0 mm, 0.7 mm and
0.5 mm. The cold rolled sheets were primarily recrystallized during decarburization annealing and
were secondarily recrystallized in the high temperature annealing at 1200 °C with 15 h soaking in
an atmosphere containing 25 % N2 and 75 % H2, in order to observe structure, texture and magnetic
properties.
To determine the changes in mechanical properties due to strain ageing, the samples underwent
overlapped ageing, after pre-straining by rolling, under the same conditions of inter-pass ageing and
then were subjected to tensile tests in thicknesses of 1.0 mm, 0.7 mm and 0.5 mm, representing
57 %, 70 % and 78 % of reduction, respectively.
The primary recrystallization texture was measured by X-ray diffraction and volume fraction of
the texture components were calculated within 11° around the ideal orientation, using MTM-FHM
(Department of Metallurgy and Materials Engineering – Fast Harmonic Method) software.
Magnetic induction at 800 A/m, B8, and core loss at 1.7 T/50 Hz, W1.7/50, were measured in the
strips of final product cut in the rolling direction, by using a single sheet tester Brokhauss
MPG100D. Finally, the samples were pickled in HCl 20 % to allow the evaluation of grain size
after secondary recrystallization.

Results and Discussion

The presence of fine carbides, about 20 nm, was detected in the hot band annealing by transmission
electron microscopy. Carbides of this size can be partly dissolved (strain induced decomposition)
thereby releasing solute carbon to lock dislocations during the cold rolling, producing a strain
ageing effect in the material [4].
Fig. 1 shows the variation in yield stress induced by strain ageing as a function of ageing
temperature and pre-strain reduction applied on the samples. The strain ageing effect is more
pronounced in the thickness of 0.70 mm, 70 % reduction. The temperature of 200 °C had the
highest yield stress variation for all reductions evaluated, indicating that the strain ageing is more
effective at this temperature.
Inter-pass ageing makes cold rolling difficult by the increase of yield stress. Since the
deformation is imposed by rolling, the material tends to form shear bands. So, higher strain ageing
is expected to favour shear band formation and enhance texture components that are present at shear
bands, such as of 110 〈001〉 and 012 〈001〉. The sum of the volume fractions of these two
components after cold rolling increase with inter-pass ageing and is maximum at 200 °C, as shown
in Fig. 2.
140 0,0076
Fraction {110}<001> + {012}<100>

57% reduction 70% reduction 78%reduction

120 0,0073

100 0,0070

0,0067
∆σe (MPa)

80

60 0,0064

0,0061
40
0,0058
20
0,0055
0
No 100°C 150°C 200°C 250°C 300°C
100°C 150°C 200°C 250°C 300°C Ageing
Pass Ageing Temperature Pass Ageing Conditions

Fig. 1 - Variation in yield stress as a function of Fig. 2 – Cold rolled texture as a function of pass
pass ageing temperature. ageing temperature.
524 Recrystallization and Grain Growth V

The decrease in the volume fraction of 110 〈001〉 plus 012 〈001〉 orientations at temperatures
of 250 °C and 300 °C for the material after cold rolling is consistent with the reduction in yield
stress variation observed in the mechanical properties for the same temperatures after strain ageing
treatment.
The main primary recrystallization texture changes associated with inter-pass ageing treatment
during cold rolling are the decrease in 554 〈225〉 and 111 〈112〉 major textures components and
the increase in 110 〈001〉 and 012 〈001〉 components, as shown in Fig. 3(a-b). The volume
fraction of 012 〈001〉 orientation increases with inter-pass ageing temperature, showing a
maximum at 200 °C and then a decrease at temperatures of 250 °C and 300 °C. The volume fraction
of 110 〈001〉 orientation also increases, being practically the same at 200 °C and 250 °C, and then
decreases at higher temperature. The volume fraction of 111 〈112〉 and 554 〈225〉 components
show the following behavior: reduction with inter-pass aging temperature up to 250 °C, and then
increase at 300 °C.

{111}<112> {012}<001>
0,198 0,010
{554}<225> {110}<001>
Volume Fraction

0,193
Volume Fraction
0,009
0,188
0,008
0,183
0,178 0,007
0,173 0,006
0,168
0,005
0,163
0,158 0,004
0,153 0,003
No P. A. 100 150 200 250 300 No P. A. 100 150 200 250 300
Pass Ageing Temperature (°C) Pass Ageing Temperature (°C)

(a) (b)
Fig. 3 – Primary recrystallization texture as a function of inter-pass ageing temperature:
(a) 111 〈112〉 and 554 〈225〉; (b) 012 〈001〉 and 110 〈001〉.

Fig. 4 shows the macrostructures of secondary recrystallized samples with and without inter-pass
ageing treatment. Final grain size is reduced by inter-pass ageing, being minimum around 200 °C,
which can be attributed to the largest volume fractions of 110 〈001〉 and 012 〈001〉 orientations
at this temperature after primary recrystallization. This is in agreement with prior works [1-3].

Fig.4 – Macrostructures of secondary recrystallization.

The results of magnetic properties as a function of inter-pass ageing temperature are shown in
Fig. 5. The core loss, W1.7/50, showed a significant improvement when inter-pass ageing was used. It
is observed that the core loss decreases with inter-pass ageing temperature reaching the best result
 Materials Science Forum Vol. 753 525

at 200 °C. At the higher inter-pass ageing temperature 250 °C and 300 °C, the core loss increases,
but is still lower than that without inter-pass ageing treatment. The magnetic induction presents
practically no alterations with inter pass-aging temperature contradicting previous works [1,2].
The core loss is mainly influenced by grain size and magnetic induction. When the core loss
values are corrected to a constant value of B8, 1.9 T, as can be observed in Fig. 6, the core loss
decreases with the reduction of grain size after secondary recrystallization. The same trend was also
observed in prior work [1].

Core Loss Magnetic Induction 1,23

1,25 1950
1,20

W 1.7/50 (W/kg)
1,20 1900 1,17
W 1.7/50 (W/kg)

1,14

B8 (mT)
1,15 1850
1,11
1,10 1800 1,08
1,05
1,05 1750
1,02
1,00 1700 0,0 5,0 10,0 15,0 20,0 25,0 30,0
No P. A. 100°C 150°C 200°C 250°C 300°C Final Grain Size(mm)
Pass Ageing Conditions adjustment experimental data
Fig. 5 – Effect of inter pass ageing on the Fig. 6 – Core loss as a function of final grain
magnetic properties. size.

Conclusions
1) Inter-pass ageing treatment at 200 °C during cold rolling reduces the grain size of Fe-3%Si grain
oriented electrical steel after secondary recrystallization and improves its core loss.
2) The magnetic induction presents practically no alterations with inter-pass ageing temperature.
3) The largest variation in yield stress took place at the temperature of 200 °C in all evaluated
thicknesses, showing that strain ageing is more effective at this temperature.
4) The strain ageing effect is more pronounced in the thickness of 0.70 mm, 70 % reduction.
5) Inter-pass ageing treatment during cold rolling decreases the 554 〈225〉 and 111 〈112〉
components and increases 110 〈001〉 and 012 〈001〉 components on the primary
recrystallization texture.
6) The sum of volume fraction 110 〈001〉 plus 012 〈001〉 orientations after cold rolling reaches
a maximum at inter-pass ageing temperature of 200 °C in agreement with the strain ageing effect at
the same temperature.

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[4] Y. Yoshitomi and S. Arai: European patent application nº 0393508, 1990.
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Recrystallization and Grain Growth V
10.4028/www.scientific.net/MSF.753

Effect of Inter-Pass Ageing during Cold Rolling on Magnetic Properties of Fe-3%Si

10.4028/www.scientific.net/MSF.753.522