COMMISSION OF THE EUROPEAN COMMUNITIES

technical steel research

Steelmaking

Microsegregation of alloying elements in

structural steel plates

Blow-up from microfiche original

1980 EUR 6655 EN

 COMMISSION OF THE EUROPEAN COMMUNITIES

technical steel research

Steelmaking

Microsegregation of alloying elements in

structural steel plates

J. BEGUINOT, J. FALCE, P. MARTINON

Creusot-Loire, Le Creusot

Contract No 6210-50/3/302
(1.12.1974 - 30.5.1978)

FINAL REPORT

Directorate-General
'Scientific and Technical Information and Information Management'

1980 EUR 6655 EN

 Published by the
COMMISSION OF THE EUROPEAN COMMUNITIES

DirectorateGeneral
'Scientific and Technical Information and Information Management'

Btiment Jean Monnet

LUXEMBOURG

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ECSC-EEC-EAEC, Brussels-Luxembourg, 1980

Printed i n Italy

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CONTENTS

1. Introduction Page 1

2. Preliminary determination of the area of the ingot

having the highest rates of microsegregation. 2

2.1 Tests of ingot 2

2.1.1 Sampling 2
2.1.2 Results 2
2.1.2.1 Major segregation 2
2.1.2.2 Microsegregation 3

2.2 Tests on plate 4

2.2.1 Sampling 4
2.2.2 Results 4
2.2.2.1 Major segregation 4
2.2.2.2 Microsegregation 5

3. Study of microsegregation as a function of chemical

composition. 5

3.1 Microsegregation of manganese 6

3.2 Microsegregation of nickel 7
3.3 Microsegregation of chromium 8

4. Effect of homogenising anneal 9

4.1 Theoretical determination of the homogenisation

treatment conditions. 9
4.2 Effect of annealing on the microsegregation and the
microstructure. 11
4.3 Effect of annealing on the anisotropy of the ductility. 12
4.3.1 Degree of anisotropy of the various ductility
properties. 12
4.3.2 Contributions of microsegregation and elongated
inclusions to the ductility anisotropy. 13
4.3.3 Effect of homogenising anneal on the ductility
anisotropy. 14
4.3.3.1 Experimental procedure 14
4.3.3.2 Results 15
 IV

Contents (continued)
Page

4.4 Conclusions on the value of a homogenising anneal 16

5. General conclusions 17

Appendix 19
References 23
Figures 28
 -

SUMMARY

At first, the spatial distribution of microsegregation in the

ingot and in the corresponding plate was studied. In both cases,
microsegregation ratio is a maximum in the axis of the upper
part. The evolution of the microsegregation's ratios of Mn, Ni Cr
was then investigated versus the chemical composition of the
upper-axis parts of 115 plates representing a wide range of
structural steels. Formulations of the microsegregation ratios
were derived for manganese and nickel.

The time-temperature parameters were defined for an anneal able to

homogenise the microsegregation and the microstrueture. Also it
was demonstrated in the range of steels studied, that elongated
inclusions (Mn S, clusters of oxides) are mainly responsible for
the anisotropy of the ductility; the microsegregation and the banded
structure have then a second order influence. This explains that
the homogenisation anneal, effective for the equalisation
of microsegregation and microstructure, have no real influence
on the ductility. The interest of such an anneal for other
metallurgical properties is discussed.
 -VI-

Zusammenfassung

Aus einer vorherigen Untersuchung der Verteilung von Mikroseigerungen in

Blcken und Blechen ergab sich, dass in beiden Fallen der Mikroseigerungs-
grad an der Kopfseite und in Lngsrichtung des Produkts einen Hchstwert
aufweist. Anschliessend ist der Verlauf des Mikroseigerungsgrads der Bes-
tandteile Mn, Ni, Cr untersucht worden. Dies geschah in Abhngigkeit der
chemischen Zusammensetzung, anhand von axialen, kopfseitigen Probestucken,
die aus 115 Blechen entnommen wurden Diese Bleche gehren zu einer umfan-
greichen Reihe von Bausthlen. Die Mikroseigerungen von Mn und Ni sind
ermittelt worden.

Andererseits ging man daran, die Parameter fur eine Gluhung festzulegen,
die eine zweckmassige Homogenesierung der Mikroseigerungen und des Mikro-
gefuges sicherstellt.

Darberhinaus ist der Nachweis erbracht worden, dass in den untersuchten

Baustahlen des Vorhandensein von langgestreckten Einschlssen (Sulfide,
oxydische Streifen) auf die Anisotropie der Verformungseigenschaften eine
entscheidende Rolle spielt wobei die Mikroseigerungen und das Streifen-
gefuge eine untergeordnete Bedeutung haben. Dieser Umstand verdeutlicht,
dass sich eine Diffusionsgluhung auf die Mikroseigerung und das Mikroge-
fuge gunst ig auswirkt ; sie verbessert aber kaum die Verformungseigens-
chaften. Ob diese Diffusionsgluhung fur weitere metallurgischen Eigens-
chaften von Interesse ist, wurde aucherortert.
 -VII

RESUME.

Une tude pralable de la distribution de la microsgrgation sur lingot et

sur tle a montr que, dans les deux cas, le taux de microsgrgation pr-
sente une valeur maximale en tte axe de produit. L volution des taux de
microsgrgation des lments Mn, Ni, Cr a t ensuite tudie, en fonction
de la composition chimique, sur prlvements tte-axe de 115 tles repr-
sentant une vaste gamme d'aciers de construction. Des formulations du taux
de microsgrgation de Mn et Ni ont t tablies.
On a d'autre part dtermin les paramtres d'un recuit assurant une homog-
nisation correcte de la microsgrgation et de la microstructure.
Par ailleurs il a t montr que, dans la gamme d'aciers tudis, la prsen-
ce d'inclusions allonges (sulfures, plages d'oxydes) jouent un rle dter-
minant sur l'anisotropie des caractristiques de ductilit, la microsgr-
gation et la structure en bandes ayant alors une influence secondaire. Ceci
explique que le recuit d'homognisation, efficace au niveau de la micros-
grgation et de la microstructure, n'amliore pratiquement pas les caract-
ristiques de ductilit. L'intrt d'un tel recuit d homognisation sur
d'autres proprits mtallurgiques est discut.
 - 1-

1. INTRODUCTION

The development of the micrographie study of steels during the last

century made it possible to reveal the structure of alternating bands
rich and poor in carbides in rolled products. This arrangement of
the structure contributes, with the presence of inclusions flattened
by the rolling, to the anisotropy of ductility in relation to the
principle direction of rolling, known for a long time in forges.

In its turn, the link between banded structure and mircosegregation

of impurities or alloying elements in the interdendritic spaces of
the solidification structure was established at the beginning of this
century (see J.I.S.I.) and as early as 1915 Stead (1) demonstrated
the special part played by phosphorus in the banded structure at a
time when the content of this impurity in steels was much greater
than that normally obtained today.

Much work has been done since on microsegregation, banded structure

and anisotropy of ductility (cf. bibliographical review of Kohn (2)).

The primary aim of the present work was to determine the relations
between the rate of microsegregation of the elements Mn, Ni, Cr and
the chemical composition of the steel and to put forward a formulation
of these microsegregation rates for a wide range of structural carbon,
carbon-manganese and low alloy steels. To this end 115 samples were
taken from the upper axis of plates from industrial melts and analysed
with the microprobe.

We then attempted to discover precisely the effect of a homogenising

anneal at high temperature on the microsegregation rate and the
improvement in ductility, particularly in the case of rupture by
impact (toughness).

The results obtained are discussed in relation to recent work

published in this field.
 -2 -

2. PRELIMINARY DETERMINATION OF THE AREA OF THE INGOT WITH THE

HIGHEST MICROSEGREGATION RATES

Before carrying out a systematic study of the microsegregation of

alloying elements as a function of the composition, we examined the
pattern of microsegregation in the various zones:

a) of a slab ingot of low alloy steel

b) of a plate of the same grade in the usual heat treated
condition.

For that, 2 slab ingots of 2.750 t (e = 250 mm)* of low alloy

steel (16 MNCD 5) were cast uphill.

2.1 Tests on the 2.750 t ingots

2.1.1. Taking the samples

Samples were taken from the first ingot in accordance with the diagram
in Fig. 1. A slice halfway along the thickness was taken from each
of the samples.

Each slice was polished on one face. This face was etched with
Dickenson's reagent in order to bring out the primary structure of
the ingot and thus choose the place from which to take the specimen
to be used for measuring the microsegregation. The chemical analysis
was verified on the same specimen.

2.1.2. Results

2.1.2.1. Maj_or_segregation

The speciment taken from the outer area lie in the region of dendritic
solidification. The specimens taken from the axis lie in the region
of equiaxed solidification (top and centre of ingot) and in the region
of globular structure at the bottom of the ingot.

The major segregation of the principle elements (carbon, sulphur,

manganese, nickel, chromium and molybdenum) in the 2.750 t ingot was
measured_by_ conventional analysis. Comparison of the concentrations

e = thickness
measured at the outer edge and the axis, at the top, centre and
bottom, gives the results in Table 1.

Comparison of the results obtained shows that major segregation

hardly exists in practice.

2.1.2.2 Microsegregation

The microsegregation was measured by spot determinations using an

electron probe microanalyser. The measurements were taken halfway
through the specimen (thus halfway through the ingot).

The segregation was measured for manganese, nickel and chromium.

It should be noted, in fact, that the relative accuracy depends on
the content of the element concerned. As each measurement is made
to within 0.05 %, for a content of 0.5 % the accuracy is 10 %; it
becomes 3 % if the content of the element is 1.5 %. That is why we
did not think it possible to measure the segregation of molybdenum
(0.23 % ) .

In view of the quite random ar angement of the most segregated areas

(interdendritic spaces) in relation to the less segregated ones
(dendritic axes), the measurements are tricky, particularly in the
equiaxed zone.

In this zone we have been able, however, to mark the most segregated
areas either by sulphide inclusions (in particular in the upper
axis) or by sodium bisulphite etch (interdendritic areas more
strongly etched) (Fig. 2).

The mean of five points was used to mark the maximum concentration
C w in the segregated areas and the minimum concentration C in
b
M m
the least segregated areas.
To assess the amount of segregation the absolute deviation of
concentration (C - C ) related to the overall content of the
M m
element concerned in the ingot at the point of measurement (C product)
was preferred to the segregation rate usually used in the literature
(C./C (. This rate is, however, quoted in Table 2, where the results
M m
obtained are brought together. To this segregation rate has been
linked the effective distribution coefficient ke = C /C product
m
defined by Doherty and Melford (3).
 -4-

The values obtained are in good agreement with those encountered

in the literature (4), (5) ,

We found, like a number of writers (2, 3, 3, 6-8), a noticeable

increase in the segregation rate from the outer edge (dendritic
zone) to the core (equiaxed zone) of the ingot.

To this increase in segregation rate there corresponds a decrease

in the distribution coefficient ke.

These variations are attributable to the different solidification

conditions between the outer edge and the centre of the ingot (5).

Moreover the segregation rate does not vary hardly at all from
the top to the bottom of the ingot.

Indeed the segregation rate of manganese is greater than that

of nickel. The segregation of nickel is roughly the same as that
of chromium.

2.2 Tests on plate

2.2.1 Taking the samples

The second ingot from the same melt, after holding at about 1300 C
for 4 hours, was rolled down to plate 20 mm thick.

After conventional industrial heat treatment for the grade

concerned (hardening + tempering ) sections were cut out in
accordance with the diagram in Fig. 3 in such a way that the
position of the specimens corresponds as well as possible to
those chosen in the ingot. From these sections specimens were
taken for measuring the major segregation and the microsegregation.

2.2.2. Results

2.2.2.1 Major segregation

The chemical analyses carried out on the specimens from axis and
outer edge, top centre and bottem, are shown in Table 3.

Hardly any major segregation can be discerned from these results.

2.2.2.2 Microsegregation

The microsegregation measurements were carried out in the same

way as for the ingot. The results are brought together in Table 4.
An example of the record is illustrated in Fig. 4.

We find that the rate of segregation of the elements manganese,

nickel, and chromium is about twice as high in the axis of the
plate (slightly banded structure) as at the outer edge (homogen-
eous structure). On the other hand the variation in segregation
between the top and bottom of the plate is slight.

Finally, we find.that the microsegregation rates for the same

element measured in the similar areas of the ingot and the plate
are very similar except for the higher levels of microsegregation
where a slight homogenisation has started in the plate (Fig. 5).
It thus appears that heating the ingot (1300 C - 4h) before
rolling brings about hardly any homogenisation of the micro-
segregation (cf. 4.1).

3. STUDY OF THE MICROSEGREGATION AS A FUNCTION OF THE CHEMICAL

COMPOSITION

As with the results of the previous study, the analysis of the

microsegregation on plates was carried out on sections cut from
the upper axis.

The contents of C, Mn, Ni and Cr of the 115 plates examined are

given in Table 5. They illustrate a representative selection of
the grades of structural steel plate produced at the Creusot
works.

The segregation rates for manganese, nickel and chromium were

determined using the microprobe.

Figs. 6 and 7 give two examples of the pattern of the contents

of microsegregated elements.

The intensity of the microsegregation of an element is primarily

a function of the mean content of that element.
To understand the effect of the chemical composition on the
microsegregation of a given element it is thus preferable to
relate the deviation C - C . of the maximum and minimum
max mm
contents of that element to the mean content C , we thus
mo y
define the relative rate of microsegregation by:

C max - C min
=
C moy

The search for a formulation of the rates of segregation as a

function of the composition was carried out in two stages:

a plot in graph form provides a first approximation of the

relations between the rate of microsegregation and the contents
of carbon, manganese, nickel and chromium in the carbon steel.
A series of plausible literal formulations can thus be put
forward.

a regression calculation carried out on these formulae enables

us to choose the one which offers the maximum statistical signi
ficance and to adjust the coefficients proper to the different
variables used.

3.1. Microsegregation of manganese

The experimental values of the segregation rate of manganese,

, are shown in Fig. 8 against statistically significant
variables - manganese and carbon contents. We observe firstly
that the distribution T = f (Mn %) has a minimum for a mean
Mn
manganese content in the region of 0.9 %. We used a parabolic
dependence as a function of the manganese content leading to
a basic formulation as a function of Mn % in the form:
2
T.. = a. Mn + b. Mn +c
Mn

On the other hand the segregation rate of manganese increases

in roughly linear fashion with the carbon content (Fig. 9)
when the Mn content is less than - 1%. A linear term as C %,
d.C, should thus be added to the expression of T w .
Mn
 7

However this dependence of on the carbon content becomes

Mn
progressively more blurred when the manganese content increases
and becomes noticeably unclear for manganese contents greater
than 1 %. In order to take into account this progressive weak
ening of the dependence on the carbon, a term covering C Mn
with a negative ceofficient should in its turn be added to
the basic formulation of . Thus we finally have it in the
J
Mn
following literal form, the contents being expressed in %
2
T = a.Mn + b. Mn + d.C + e. C + c

The regression calculation provides the following values for

the constants:
a = 0,245 ; b = 0,394 ; c = 0, 366
d = 1,25 ; e = 0,532

This equation is valid for 0.4 % M n ^ 1.7 %.

The double standard deviation on T in this formulation is

Mn
equal to 2 = 0.16. All the variables are 100 % significant.

Note
When the sulphur content of the steel is high a significant
part of the manganese segregated in the interdendritic spaces
may be fixed in the form of manganese sulphide inclusions, which
tends to reduce the microsegregation rate of that element. In
the population representative of the steels studied the sulphur
contents are relatively low, however, (0.005 % < S < 0.036 %)
so that the proportion of manganese fixed should be negligible.

This point has been verified by statistical analysis which shows

that the term S does not emerge as significant in the
formulation of T w .
Mn

3.2 Microsegregation of nickel T.

In the range of contents from 0 to 1 % the microsegregation

rate of nickel decreases almost linearly with the Ni content
(Fig. 10). The effect of the carbon on T. is less clear than
Ni
for manganese.
 8-

A look at the diagram suggested to us a parabolic dependence -

very slightly marked, however - of the slope of .(Ni) on the
carbon content. The formulation obtained on this basis leads
to the expression of T.:
v
Ni

T. = 0.396 - 3.498 Ni C + 16.11 Ni C

Ni
with a. double standard deviation 2 = 0.34. This formula is
valid in the range 0.1-1 % nickel.
2 . . .
The variables Ni C and Ni C are 100 % significant.

3.3. Microsegregation of chromium

The rate of microsegregation of chromium as a function of the
content shows considerable scatter, and no trend of variation
as a function of chromium appears clearly (Fig. 11).

The mean value of T is approximately 0.35 for a chromium

Cr
content between 0.1 % and 2.5 %.
In spite of the considerable scatter in the results it seems
that the carbon tends to increase the microsegregation of the
chromium. This observation is in agreement with the results of
Doherty and Melford (3), Fredrikson and Hellner (9), Flemings
et al. (10).

Note regarding the ingot size effect

The microsegregation at the moment of solidification, like the

macrosegregation, increases when the cooling rate decreases. Yet,
in contrast to the macrosegregation, the microsegregation is
sensitive to homogenisation by diffusion, particularly for high
temperatures below the solidus, because of the much more restr
icted diffusion distances. The intensity of the homogenisation
decreases when the cooling rate increases because of the reduct
ion in the time at high temperature below the solidus.

The effect of the homogenisation by diffusion on cooling is thus

slight for fast cooling (short time at high temperature) and
marked for slower cooling, although the interdendritic spaces
are then greater.
 - 9

Thus the cooling rate exerts two contradictory influences on

the value of the microsegregation obtained after cooling -
the decrease in the cooling rate increases the initial
microsegregation but favours an incipient homogenisation
immediately below the solidus.

Thus it seems that in the range of industrial ingot sizes

the microsegregation is less sensitive than the macrosegreg-
ation to the effect of size. Indeed we find that the size of
ingots has no significant effect on the microsegregation rate
in the tonnage range of the 115 ingots analysed (between 3 and
20 tonnes).

4. EFFECTS OF A HOMOGENISING ANNEAL

Microsegregation being characterised by a heterogeneity in the

distribution of the alloying elements on a microscopic scale,
an appropriate diffusion treatment should enable the intensity
of this microsegregation to be greatly reduced. We attempted
in succession:

to determine theoretically the diffusion treatment condit-

ions likely to greatly reduce the microsegregation of alloying
elements

to check experimentally the validity of these calculations

using microprobe analyses before and after heat treatment

to examine the homogenisation of the microsegregation on

the attenuation of the banded microstructure

finally, to study the consequences of a microsegregation-

-homogenising anneal on the anisotropy of the ductility.

4.1. Theoretical determination of the homogenisation treatment

conditions

We tried to determine the heat treatment conditions likely to

homogenise the distribution of the elements Mn, Ni and Cr. The
distribution of carbon equalises very rapidly in austenite
 - 10 -

because of its comparatively very great diffusivity.

We chose to carry out the homogenising anneal at 1225 C. At

this temperature the values of the diffusion coefficients of
the elements Mn, Ni and Cr in austenite are as follows:

-10 2
D Mn - 1,34 . 10 cm /S (11)
-10 2
D Ni - 1,53 . 10 cm /S (12)
-10 2
D Cr - 2,1 .10 cm /S (10)

The duration of heat treatment will thus be determined to

ensure the homogenisation of the manganese, the diffusion
coefficient of which is the lowest.

The details of the calculation and the discussion are pres

ented in the Appendix. The annealing time necessary to obtain
a given degree of homogenisation is expressed by:

1 a2
. a n (/Tf) (1)
2
4 D

in which a is the interdendritic distance, D the coefficient

of diffusion of the element under consideration (here Mn) at
the annealing temperature, To the initial rate of microsegreg
ation and Tf the microsegregation rate after the heat treat
ment.

For a treatment carried out at 1225 C Equation (1) indicates

that an annealing time of 3 hours is necessary to obtain a
reduction in the microsegregation by a factor of 10 (/tf = 10).

In view of the calculation hypotheses, the uncertainty on the

value of D and the variations in interdendritic distance from
one plate to another we finally chose an anneal of 8 hours at
1225C (cf. Appendix).

It will be noted, moreover, that the annealing time varies as

the square of the interdendritic distance a. The interdend
ritic distance evolves, as a first approximation, as the
 - 11

inverse of the degree of rolling reduction and the relation

between the annealing times necessary to produce the same
homogenisation of the microsegregation on ingot or plate is
_2
thus of the order of Z>

As the mean value of the degree of rolling reduction for the

plated examined was roughly 10 an anneal of the order of 800
hours at 1225 C would be necessary to homogenise the contents
in the ingot. This explains the almost complete absence of
homogenisation during reheating of the ingots before rolling
(1250C, 6 hours or 1300C, 4 hours) related in section 2.2).

4.2 Effect of anneal on microsegregation and microstructure

We examined the evolution of the microsegregation by homogen

isation treatment on a carbon steel (plate A) and a carbon-
-manganese steel (plate B) with high rates of microsegregation.

a) plate A (C = 0.28 %, = 0.022 %, Mn = 0.64 %,

Si = 0.36 %, Ni = 0.14 %, Cr = 0.15 %)

The mean manganese content is 0.64 % and the rate T w = 0.71.

Mn
This corresponds to an absolute microsegregation rate
T' = C - C . = 0.45 %
Mn max mm

Figs. 12 and 13 offer a comparison of the distribution of

manganese through the thickness of the plate measured with the
microprobe before and a ter heat treatment at 1225 C for 8 hours.
We find that the initial heterogeneity of distribution of the
manganese is very much attenuated. The consequence of this
homogenisation of the manganese on the microstructure is
particularly clear (Fig. 14). The very marked banded structure
before treatment has completely disappeared afterwards.

b) plate B (C = 0.175 %, = 0.017 %, Si = 0.41 %,

= 0.46 %, Ni = 0.15 %, Cr = 0.13 %)
 - 12

The mean manganese content is 1.31 % and the rate = 0.46,

that is an absolute microsegregation rate.

T' = C - C . = 0.60 %
Mn max mm
Comparison of Figs. 15 and 16 shows that after 8 "hours'
annealing at 1225 C a correct homogenisation has occurred at
the interdendritic level but a certain heterogeneity remains on
a larger scale (0.2 mm approx.). The micrographie appearance is
in agreement with this analysis; the original banded structure
has disappeared but residual bands remain about 0.2 mm apart.
Expression (1) indicated an annealing time of about 120 hours
to ensure the homogenisation of these residual bands (a - 200 ym),
Microprobe analysis after 120 additional hours' anneal at 1225 C
(Fig. 17) reveals in fact an overall homogenisation of the'
manganese content.

The effectiveness of a high temperature anneal to considerably

reduce the microsegregation and the banded structure is thus
demonstrated, in agreement with the theoretical calculations.

4. 3 E f f ect_of _anneal_on_aniso trop_y__of _ductility

4.3.1 Degree of anisotropy of the various ductility properties

As earlier work has already shown (13) we must differentiate,

from the point of view of the degree of anisotropy, between the
elongation at fracture in the tensile test on the one hand and
the reduction of area in the tensile test or the energy of
ductile fracture in the impact toughness test on the other.

The elongation at fracture presents little anisotropy; for all

the melts studied earlier the mean value of the elongation
lengthways only exceeds by 1.5 % the value measured crossways.
This difference, which is comparable with the uncertainties of
measurement of the elongation, thus seems of little significance,
and we may regard the elongation as practically isotropic.

In contrast the values for reduction of area after tensile

testing and energy of rupture in the ductile range during the
 13

impact toughness test show considerable anisotropy.

The Charpy V tests carried out at 150 C (totally ductile

fracture for all the melts studied) show that the mean ratio
of the values across and lengthways for the energy of fracture
(EmT/EmL) is equal to ^0.75 (Fig. 18),

It should, however, be noted that this anisotropy may result

not only from the banded microstructure but equally from the
presence of inclusions elongated by the rolling (manganese
sulphides, type II, and plated of oxide inclusions). Grange,
working with synthetic melts, has shown that the elongated
inclusions even play a predominant part in the anisotropy in
a carbon-manganese steel containing 19 thousandths % sulphur,
so that the homogenisation of the microstructure only slightly
improves the anisotropy (13). It is thus worthwhile to examine,
on a larger population of industrial melts with varied
composition as regards alloying elements and sulphur content,
on the one hand the respective contributions made by the
microsegregation and the elongated inclusions to the anisotropy
of the ductility, and on the other the part played by the
homogenisation anneal in this anisotropy.

4.3.2. Contributions of the microsegregation and elongated

inclusions to the anisotropy

To evaluate roughly the relative share of the microsegregation

and the elongated sulphide inclusions in the anisotropy we
examined the variations in the latter with the parameters
rate of microsegregation and sulphur content respectively.

The (EmT/EmL) anisotropy diagrams as a function of the rates

of relative microsegregation (T ) and absolute microsegregation
(T' = C - C . ) (see Fig. 18) for the carbon and
Mn max min
carbon-manganese grades show that the anisotropy hardly
increases with the microsegregation.
 -14-

On the contrary, the anisotropy depends on the sulphur content;

it increases very much with it up to a sulphur content of about
10 thousandths % then stabilises thereafter (Figs.. 18 and 19).

The considerable scatter in the results observed results

notably from:

the more or less marked elongation of the inclusions in

relation to the degree of rolling reduction (Fig. 20).

the heterogenious distribution of the sulphides in the metal

matrix. The amount of sulphides present in the plane of
fracture of impact toughness testpieces taken in identical
fashion from the same section of plate may thus vary consider-
ably from one specimen to the other.

However these results confirm, over a varied range of steels,

the observations of Grange - relatively minor role of the
microsegregation and the microstructure on the anisotropy of
ductility compared with the influence of the elongated sulphide
inclusions.
ii

Micrographie examination shows on the one hand that the anneal

at 1225 C hardly spheroidises the sulphides; its role is
limited to homogenising the microsegregation and the microstructure,
Consequently it may be thought that this anneal will have only
a negligible effect on the anisotropy. Around this mean value
- zero the variation in anisotropy after homogenising anneal
may vary from one plate to another by a positive or negative
value because of the heterogeneity in distribution of the
sulphides mentioned above.

4.3.3. Effect of the homogenising anneal on the anisotropy

of the ductility

4.3.3.1 Experimental procedure

We examined the influence of homogenisation on 11 plates of

 - 15

very different composition as regards alloying elements and

sulphur content, and having initially a high microsegregation
rate (Table 6). Each of the sections cut from the upper axis
of these plates was divided into two parts:

- one part was annealed at 1225 C for 8 hours under an

argon-hydrogen atmosphere then after cooling was reaustenitised
at 940C for half an hour then cooled at about 300/h (V at
700C).

the control part only received this last treatment and so

was not homogenised.

Eight standard Charpy V testpieces were taken from each part

- four lengthways and four across. For some plates four
testpieces were also taken in the direction of the thickness.
These testpieces were fractured on a pendulum hammer at 150 C
so as to ensure in every case a completely ductile fracture.
For each direction of the specimen we took the mean of the
four values measured for the energy of fracture.

4.3.3.2 Results

The variation in anisotropy with the homogenising anneal may

be represented by the index:

(EmT/EmL) h - (EmT/EmL) o
H '
(EmT/EmL) o

in which the indices h and o correspond to the homogenised

and control specimen defined in the experimental procedure.

It is interesting to compound H to the value H* which would

result from a complete disappearance of the anisotropy
(EmT/EmL = 1)
1 - (EmT/EmL) o
H* = (EmT/EmL) o
 - 16

The results obtained (Table 7) conform to the indications

put forward in 4.3.2:

- negligible part played (on average) by the homogenising

anneal in the anisotropy: H = -0.25 %
r
mean
- considerable scatter in (2 () = 21.7 % resulting
from values which may be either positive or negative.
The negative values obviously do not mean that the homogen
isation has increased the anisotropy (which would be aberrant)
but must correspond to the scatter in the results due to the
heterogeneity of distribution of the sulphides.

We thus confirm that, in the plates studied, it is the

sulphides of manganese which play the major part in the
anisotropy of the toughness properties. The homogenising
anneal, effective as regards homogenisation of the microseg
regation and the microstructure, but having practically no
effect on the sulphides, thus has hardly any effect on the
anisotropy of the toughness properties.

4.4 Conclusions on the value of a homogenisation treatment

An appropriate anneal at high temperature (1225 C for a hours
in the cases studied) is likely to reduce considerably the
microsegregation of the elements Mn, Ni* and Cr and the banded
microstructure, in accordance with the theory.

In contrast, this anneal has a negligible effect on the

anisotropy of the ductility properties, which is explained by
the fact that the microsegregation and the banded microstructure
affect the anisotropy much less than the elongated manganese
sulphide inclusions in the wide range of structural steels studied,
A significant improvement in the anisotropy would require an
anneal at a higher temperature to spheroidise the sulphides (14).
In industrial practive it is in fact more worthwhile to prevent
the flattening of the sulphides during rolling by making
 17

appropriate additions during steelmaking (for example

silico-calcium).

Although the homogenising anneal thus appears of little value

from the point of view of reducing the anisotropy of the
ductility, it is nevertheless not without practical value.

A number of metallurgical properties are in fact linked

directly with the heterogeneity of distribution of the
elements in the metal and consequently sensitive to the
effect of a homogenisation treatment. Among these we may
mention segregation cracks and the presence of bainite
bands in the bands with the greatest segregation of elements
which can be hardened and tempered, within an otherwise
ferrite-pearlite matrix. These bainite bands, even in a
fairly small proportion, are capable of greatly reducing the
apparent elastic limit compared to the entirely ferrite-
-pearlite condition because of the presence of microareas of
residual austenite between the bainite needles. However,
tempering at a fairly low temperature enables this residual
austenite to be destabilised and the normal elastic limit
to be restored at less cost than the homogenising anneal.

The cost of a homogenising anneal is high because of both its

high temperature and its duration. In addition, one must also
take into account the losses by oxidation and decarburisation.
Such an anneal would make it necessary to control strictly
the growth of the austenitic grain either by blocking the
grain boundaries by appropriate precipitates of niobium or
titanium, or by reaustenitisation at normal temperature
after the homogenising anneal.

These findings mean that the homogenisation treatment is in

the end of little value from an economic point of view.

5. GENERAL CONCLUSIONS

The study of microsegregation on 1 ingot and 115 plates of

structural steel covering a wide range of grades has enabled
 18

us to obtain the following main results:

- microsegregation reaches its maximum values at the upper

axis of the ingot (and plate), like the macrosegreaation.

the microsegregation is little affected by the reheating

of the ingot before rolling. In fact, the time for homogenis-
ation by diffusion viries as the square of the interdendritic
distance and would thus be exteemely long for an un-rolled
ingot.

- the macrosegregation of manganese obviously increases with

the manganese content, but the rate of relative microsegregation
has a minimum for 0.9 % manganese approx. The carbon content
increases the rate of microsegregation of mangnaese for
manganese contents up to about 1%.

the microsegreaation of chromium slightly increases with

the carbon content.

the expressions for the rate of microsegregation for

manganese and nickel were obtained, as a function of the
chemical composition, by statistical analysis.

The study of the effect of a microsegregation homogenisation

treatment led to the following main conclusions:

annealing for 8 hours at 1225 C enables the microsegregation

to be correctly homogenised and the banded structure to
disappear for a distance between segregated bands of approxi-
mately 50 \m; in agreement with the theoretical calculations.

- this homogenisation of the microsegregation and micro-

structure has, however, no notable effect on the anisotropy
of the ductility: it has been shown in fact that this is
largely due to the elongated manganese sulphide inclusions.
The temperature adopted for the homogenising anneal does not
allow the sulphides to be spheroidised.
The other advantages produced by the homogenisation of the
microstructure are of little importance in view of the high
cost of the homogenising anneal. The economic value of this
latter thus appears small.
 -19-

APPENDIX

Theoretical approximate determination of the homogenisation

treatment

Let us consider a theoretical distribution of the content of

a given element, composed in the following manner:

The content of the element is distributed in parallel bands

of concentration C and Co alternately. The thickness of the
bands of concentration C is , that of the bands of concen
tration Co is (a - ). Let us assume that the value of is
very much smaller that that of a(e a) .
Under these conditions we can show that the distribution of
the content of this element after heat -treatment of very long
duration t' at temperature is approximately:

- 4 Dt'
2 2 X
(Cx - Co) 1 + 2 e a COS + Co
C (, t')

in which

- C (, t') represents the concentration at a distance from

a band of concentration C

- D is the coefficient of diffusion of the element at temperatute T.

The mean concentration can be written-

eC + (a - ) Co
C moy =

Thus we have

- 4 Dt'
2
2 (C Co) a
C (, t') = C moy 1 + 1 ce COS
COS 2
2 (1)
a
eC + (a - )Co
 20

It will be noted, however, that this equation controls the

trend in the content for an initial distribution of the
element very different from that which characterises the
microsegregated element in the plate. It will not therefore
be used as it is. In fact the distribution of the content
of microsegregated element may be reasonably approximated
in the following sinusoidal form:
To
C () = C moy (1 + COS 2 ) (2)

in which

C moy represents the mean content of microsegregated element

To represents the rate of microsegregation
represents the distance from the interdendritic axis

Equation (1) may be written 2

4 Dt'
2
C(x,f) C 1 2 2 (C
1 Co) e COS 2 x
moy 2 To eC+(a ) Co a

giving
4 D (t' t'o)
2
C(x,f) = C 1 + To e a
COS 2 x
moy 2

with

4
2 <C1 Co>
a L n
t'o =
42 D To (0, + (a e)C )
l o
Postulating t = t' t' , we have:

4 Dt
2
2 x
C (, t) = C 1 + e COS (3)

moy
 -21 -

This equation rules the trend of c (, t) for an initial

condition

To 2 x
C (, o) = C 1 + COS
moy -r

that is exactly the distribution (2) of the microsegregation in

the plate. Thus equation (3) is appropriate for the description
of the homogenisation.

After a homogenisation treatment time t the rate of

microsegregation is brought to T (t) defined by:

- 4TT2 Dt

T (t) = C "ax (t) - C min (t) = TQ & a2 (4)

C moy

Let T f be the rate of microsegregation at the end of the

homogenisation treatment. T /T- represents the degree of
homogenisation. The time t necessary to obtain a homogen
isation T /T, is according to (4):
or

2
t = 1L . aa
. L (T /T.)
7? 5"

Imprecision of t

The values of D and the activation energy Q coming into

o
the expression are known with a certain imprecision. The value
of the interdendritic distance a, equal on average to
50 ym, varies from one plate to another due mainly to the
different degrees of rolling reduction.
The resultant variation in t can be written:

At = 2Aa + + 1 Q AQ +

t a Do R T Q T
 -22 -

At = 1500 and for manganese (Q = 66 . 10 cal),

At 2Aa AQ
= + + 20 +
t a Do q t

Taking

Aa AQ
25% - 10% - 5% - 1%,
a Do Q

We have

= 50% 10% 120% = 180%

For a homogenisation / = 10, t is equal to:

f\
25 10
t = _^__ Ln 10 - 11 000 sec.
. 2 _ ._ -66000
4 0,48e
2.1500

Let t = 3 hours

Taking into account the imprecision calculated on t we

must allow:

t = 3 hours (1 + 180 % ) - 8 hours.

 -23-

REFERENCES BIBLIOGRAPHIQUES

(1) J. STEAD - J.I.S.I., 1915, 1, 140.

(2) A. KOHN - Rev. Metall., Janvier 1970, 23 -36.

(3) R.D. DOHERTY and D.A. MELFORD - J. I.'S. ! . (1966), 204, (11), 1131 - 1143.

(4) H.A. VOGELS and al. - Stahl und Eisen (1966), 86, 945 - 952.

(5) H.J. SPIES und H.J. ECKSTEIN - Freiberger Forschungshelte (1972) 166.

(6) T.B. SMITH - Iron and Steel (1964), 37_, 536 - 541.

(7) W. HOLZGRUBER und E. PLOCKINGER - Stahl und Eisen (1968), 88,

638 - 648.

(8) D.B. CLAYTON and al - J. Inst. Metals (1961/62), 9f\ 224 - 228.

(9) H. FREDIKSON, L. HELLNER - Scand. J. Met (1974), 3, 61 - 68.

(10) M.C. FLEMINGS, D.R. POIRIER, R.V. BARONE, H.D. BRODY

J.I.S.I. (1970), _ , 371 - 381.

(11) E.A. OWEN - J. Inst. Metals (1947), 73, 471 - 489.

(12) K. IRANO, M. COHEN, B.L. AVERBACH

Acta Met (1961), 9, 440 - 445.

(13) R.A. GRANGE

Metal Trans. (1971), 2, 417 - 426.

(14) A.D. WILSON

Metal Trans. (1977), 8 A, 201 - 202.
 -24-

Fig. 1 - Position des zones de prlvement pour 1 'tude de la microsgrga-

t ion sur lingo* .

- Positions of sampling for microsegregation studies on ingot.

- Probenentnahmestellen zur Untersuchung von Mikroseigerungen in

Blocken.

Fig. 2 - Mise en vidence des zones sgrges dans diffrents chantillons

du lingot (prsences d'inclusions de Mn S ; attaque au bisulfite
de sodium).

- Determination of segregated areas in various samples of the ingot.

- Aufgefundene Seigerungszonen in unterschiedlichen Proben des Blo-

ches. (V orhandensein von Mn S Einschlussen-Atzung mit Natriurabi-
sulfit).

Fig. 3 - Position des zones de prlvement pour l'tude de la microsgr-

gation sur tle.

- Positions of sampling for microsegregation studies on plate.

- Probenentnahmenstellen zur Untersuchung von Mikroseigerungen

in Blechen.

Fig. 4 - Exemple d'enregistrement des teneurs en lments microsgrgs

sur tle, la microsonde.

- Type of microanalysis of microsegregared element? on plate.

- Bestimmung mittels der Mikrosonde von Mikroseigerungen in

Blechen,

Fig. 5 - Corrlation entre taux de microsgrgation sur chantillons homo-

logues sur tle et lingot.

- Correlation between the microsegregation ratios for homologous

sampling on plate and ingot.
 - 25 -

Zusammenhang zwischen den Mikroseigerungsgraden Blech-und

Blockprobestcken.

Fig. 6 et 7 - Exemple d'enregistrement la microsonde des teneurs en l-

ments microsgrgs sur tle.

- Type of microanalysis of microsegregated elements on plate.

- Bestimmung mittels der Mikrosonde von Mikroseigerungen in

Blechen.

Fig. 8 - Taux de microsgrgation du manganse en fonction de la teneur en

Mn.

- Microsegregation ratio of manganese as a function of the manganese

content.

- Mikroseigerungsgrad des Mangans in Abhngigkeit des Mn-Gehalts.

Fig. 9 - Influence de la teneur en carbone sur le taux de microsgrgation

du manganse.

- Influence of the carbon content on the microsegregation ratio of

manganese.

- Einfluss der Kohlenstoffgehalts auf die Manganmikroseigerung.

Fig. 10 - Taux de microsgrgation du nickel en fonction de la teneur en

nickel.

- Microsegregation ratio of nickel as a function of nickel content.

 - 26 -

Mikrosseigerungsgrad des Nickels in Abhngigkeit des Nickel-

gehalts .

Fig. 11 - Taux de microsgrgation du chrome en fonction de la teneur en

chrome.

- Microsegregation ratio of chromium as a function of chromium

content.

- Mikrosseigerungsgrad des Chroms in Abhngigkeit des Chromge-

halts.

Fig. 12 et 13 - Distribution du manganse avant et aprs recuit d'homogn-

isation (1225 C - 8 heures), mesure la microsonde dans
le sens paisseur de la tle.

- Manganese distribution before and after the homognisation

anneal (1225 C - 8 hours), by microanalysis in the thick-
ness direction of the plate.

*
- Verteilung des Mangans vor und nach der Diffusionsgluhung
(1225 C - 8 St). Die Ber,' immung erfolgte mit der Mikroson-
de in der Blechdickenrichtung,

Fig. 14 - Microstructure du mme chantillon avant (photo suprieure) et

aprs (photo infrieure) le recuit d'homognisation.

- Microstructure of the same sample before (upper photograph) and

after (lower photograph) the homognisation anneal.

- Mikrogefuge desselben Probestuckes vor der Diffusionsgluhung

(oberes Bild) und nach der Di ffusionsgluhung (unteres Bild).
 27 -

Fig. 13 - 16 - 17 - Distribution du manganse, respectivement :

. avant recuit d'homognisation
. aprs recuit 1225 C - 8 heures
. aprs recuit supplmentaire 1225 C - 120 heures

- Distribution of manganese, respectively :

. before the homognisation anneal
. after 1225 C - 8 hours anneal
. after an extra 1225 C - 120 hours anneal

- Manganverteilung
. vor der Di ffusionsgluhung
. bzw. nach der diffusionsgluhung 1225 C - 8 St
. bzw. nach zustzlicher Gl'uhung 1225 C - 120 St

Fig. 18 - Evolution du rapport travers/long de l'nergie de rupture en

fonction du taux absolu de microsegregation T' = C - C
M m

Evolution of the transverse/longitudinal ratio of the fracture

energy versus absolute microsegregation ratio T' = C - C
M m

Verlauf des Verhltnisses Lngs/Querrichtung der Bruchenergie

in Abhngigkeit der absoluten Mikroseigerung 1" = C - C.

Fig. 19 - 20 - Evolution du rapport long/travers de l'nergie de rupture en

fonction de la teneur en soufre et du taux de corroyage
respectivement

- Evolution of the longitudinal/transvers ratio of the frac-

ture energy versus the sulfur content and the wrought ratio
respectively.

- Verlauf des Verhltnisses La'ngs/Querrichtung der Bruchenergie

in Abhngigkeit, der Schwefelgehalts und des Warraverformungs-
grades.
 28
FlGURE.1

lingot mplat ( 16MNCD5)

( 2 . 7 5 0 )

180

25<
.' "Til -A ~T
+
s
I
tete'

i
Kl50tl U$0^
O

Ui

o r
UI o mili u- - Ul
O
o
150 150*

_. r _._
* V f ur*
I
pied > UI
;' ;
_ , ^ ^ . ^ . .
s o
r r V.
150; Meo* 1
1000

zones de p r l v e m e n t pour l'tude

de la m i c r o s e g r e g a t i o n des e l e m e n t s d'alliage
 -29-
FlGURE'2

TETE AXE 100

. >-,, .:
fiW *;.
1 r
' * ' ' f a ! L

F*ij''\m CM

PIED AXE X100

y'

11*. ft f ? .V ..-J

PIED RIVE 100

co
CM
O
 3 0

FIGUREN

tole(l6MNCD5)
( %000* 2ooo 2o mm)

zones de p r l v e m e n t

pour l'tude

de la m i c r o s e g r e g a t i o n

des e l e m e n t s d'alliage

:^::::. *.
0
0
10
Je
/
-LAL
2 0 0 0
 31

FIGURE:*

* ^rv^J^*v*^^

JL-+- L
Af U

8 ,....., ...,

ti^A*M^/VV^^ Gr
~f4

*9 I. ?V %

.....-,

u S

S

^VvvSv^^ ^ ^ ^^ *~
:
1

..
1

i
40 Ci U r~
 3 2

FIGURED

Taux d segregation sur tol

0.5

0.4

03

R*pr
Mn
Ni
* Cr
02
ffl

Taux de segregation sur lingot

0.3 0.4 0.5

 33 -

FIGURE: 6

V*-
 34 -

FIGUREN

a?

>,i
^^^^^^^ Kw
s!

'

kXWC

a
)i'-
M

1
! Zoo /19 to TZZ ! ^ ^

2i
*h***J> G i .
M
J
roi *o Ar,
 FIGURE: 8

Sign Tonour moyenne carbon

^ 0.078%
. M n JGM-m\ 0.12 *
\ C moy //Mn 0.158 *
0.194 %
0,288 %
^
0.7 \
\ /
\ ^
0.6
\
\

0.5

0.4 \

\ ?0
4 \>
\
/
^, /
0.3 /
^
Q
\ ,
\
cr
0.2 ^>

0,1

JMn*
0.5 1.5 215
 FIGURE*. 9

_/GM-Gm\
Mn
\ C moy
moy /Mn
/I

0.7

os o

os

04
^ 4
a

0.3 J V O)
*
e
a. A
02 . Signo- - Teneur moyenne do
% a 0.55*
0.80*
CM 1.05%
1.45%
0%
004 0.1 0.2 03
 FIGURERO

1.140
SignTeneur moyenne en carbone
09 o 0.077%
\ Cmey /Ni 0.126%
0,170%
OJ

0.7

0.6

05

04 -

-9
03
to_

02

01

0.1 02 03 O. 05 06 07 08 09 1
II 1.9 II II A
3.3
l/1 4.5
M M H\'
4.8
 FIGUREMI

i Signe Teneur moyenne en carbone

o : 0,017*.

TCr /M-CmJ ; 0,126 %
05 \ C moy y Cr e 0,170 *>
: 0,255 %
,
e I

0,4
e
o

e

o
oo
e o
c*
0,3
e
e
o o
o

02
o

o
c

0,1

Cr%
0.5 1.5 25
 FIGURE: 12

Co u p s / l O sec

1400

1300

1200 - OJ
co

1100

1000

900 -

800
 FIGURE: 13

Coups/ sec-

1400 - Sulfures de manganese

1300

ft

V\A^
M
ti
1200
o

v
1100 V
1000

900

Distance en mm

800
 - 41 -

FIGURE:14

Austenitise'940^0 30minutes + refroidissement 3009t heure

Homogeneise71225^c 8 heure puis

Austervtise 9 4 0 % 30 minutes + refroidissement 3 0 0 % heure

 FIGURE:15

2000-

1800-
 FIGURE:I6

_ Coups/1 Osee -
2300 Sulfure de manganese

2200

2100

2000 -
00

1900

1800

1700

Distance en mm

1600
0.4 0.8 1.2 1.6 20
 FlGURE:17

2400 - Coups/lOsec- Sulfures de manganese

2300 -

2200 -

2100 -

2000 -

1900 -

1800 -

1700 -

1600
 FIGUREES

EMT
Teneur du souffre en m i luernes %
EML entre 0 et 10
IO
11 20
21^30
+ 31

09

t
UI

07

06

05

T'Mn en millimes %
Q4J
100 200 300 400 500 600
 FIGURE:I9

1
'

2,6 EML m C ^ 0,15
EMT
0.15 < % C < 0,2
25
% c ?j 0,2

EML
=f(*s)
EMT V /
m

m
2

f

/ en

i
i

1.5 / : !

S % 1
/ "

m


/ : .
e
/ ! ! .


/








LJ
/ D D S "
/
D D
/ 8 g%


1 ' _ iZL
0,01 002 0.03 0.04
 FIGURERO

.6
2.6 ^Mk o %s^aoi
EMT 0.OK%S^0,02
Z5
0,02<%S$0.03
%S>03
EML
f
EMT t

. m

/
O

o

1.5
% O
/ :

I
0 . CD
O

/
m ^

/ " m Taux decorroyage
g
I

10 20 30
 - 4 8 -

a b l e a u 1 (lingot)
I
TETE MILIEU PIED TETE , MILIEU PIED
COULEE
AXE AXE AXE RIVE AXE RIVE

C 155 160 158 155 163 162 165

s 9 8 8 8 8 9 9

Mn 1350 1410 1400 1380 1400 1390 1400

Ni 770 805 780 805 780 805 795

Cr 770 805 795 790 800 790 800

Mo 225 230 230 230 235 230 235

(teneurs en milliemes%)
 tableau 2 (TAUX OE SEGREGATION LINGOT)

Mn Ni Cr
CM* Cm* TAUX Ke CM* Cm* TAUX Ke CM* Cm* TAUX Ke

TETE
AXE
1.80-1.85 1.00-1.05 0.567 0.73 0.85-0.90 0.60-0.65 0.310 0.77 0.90-0.95 0.60-0.65 0.372 0.78
(1.73) (1.4) (1.48)

MILIEU
1.80-185 1.00-1.05
AXE 0.570 0.73 0.85-0.90 0.60-0.65 0.320 0.80 0.90-0.95 0.60-0.65 0 . 3 7 7 0.77
(1.65; 4) (1.48)

PIEO
1.70-1.75 1.05-110
AXE 0.470 0.78 0.90-0.95 0.65-0.70 0.310 0.84 095-1.00 0.65-0 70 0.380 0.78
( 1.60 ) (1.4) (148) J>
co

TETE
1.55-1.60 1.20-1.25 0.250
RIVE 0.87 0.80-0.85 0.65-0.70 0.193 0.86 0.80-0.85 0.65-0.70 0.188 0.84
(1.28; (1.22) (1.22)

MILIEU
0.84 0.190 0.85
RIVE 1.55- 1.60 1.20-1.25 0.250 0.88 0.80-0.85 0.65-0.70 0.187 0.80-0.85 0.65-0.70
0.2e; (1.22) (1.22)

PIED
1.55-160 1.20-1.25 0.250
RIVE 0.87 0.80-0.85 0.65-0.70 0.189 0.85 O.85-O.90 0.70-0.75 0.188 0.90
(1.28) (1.22) (1.22)

^ ' Cm e - "F ,
^produit
 - 50 -

tableau3 (tole)

TETE MILIEU PIED TETE MILIEU PiD

COULEE
AXE AXE AXE RIVE RIVE RIVE

C 155 165 160 159 165 165 165

s 9 8 8 9 8 9 9

Mn 1350 1430 1420 1400 1420 1420 1420

Ni 770 760 765 765 765 765 760

Cr 770 760 770 770 770 770 765

Mo 225 225 230 230 230 230 230

(teneurs en m i l l i e m e s % )
 tableau 4 (TAUX DE SEGREGATION TOLE)

Mn Ni Cr
CM * C*,% TAUX CM * Cm* TAUX CM * Cm% TAUX

TETE
AXE 1.75-1.80 1.00 - 1.05 0.525 0.85-0.90 0 60 - 0.65 0.329 0.90 - 0.95 0.60-0.65 0.395

MILIEU
AXE 1 7 5 - 1.80 1.05- 1.10 0.493 0.85-0.90 0 . 6 0 - 0.65 0.327 0.90-0.95 0.60-0.65 0.390

PIED

AXE 1.70-'.75 1.05 -1.10 0.464 0, 85 -0.90 0 . 6 0 - 0.65 0.327 0.90-0.95 0 . 6 0 - 0.65 0.390

TETE
RIVE 1.55- 1.60 1.20-1.25 0.247 0.80-0.85 0.65 - 0.70 0.196 0.80-0.85 0.65-0.70 0.196

MILIEU
RIVE 1.55- 1.60 1.20-1.25 0.247 0 . 8 0 - 0.85 0.65- 0.70 0.196 0.80-0.85 0.65-0.70 0.195

PIED
RIVE 1.55-1.60 1.20-1.25 0.247 0.80-0.85 0.65-0.70 0.197 0.80-0.85 0.65-0.70 0.195
 c Mn Ni Cr Mn Ni

0,165 0,570 0,250 0,130 0,067 0,805 0,105 0,100

0,086 0,640 0,120 0,075 0,120 0,600 0,180 0,135
0,210 0,770 0,145 0,070 0,105 0,790 0,280 0,080
0,170 0,635 0,220 0,125 0,215 1,340 0,110 0,120
0,205 0,90 0,210 0,165 0,165 1,710 0,500 0,100

0,205 0,510 0,130 0,100 0,170 1,630 0,490 0,140

0,210 0,690 0,145 0,145 0,230 1,500 0,040 0,080
0,307 0,630 0,090 0,045 0,240 1,440 0,025 0,070
0,287 0,638 0,140 0,155' 0,085 1,020 0,080 0,090
0,201 0,738 0,170 0,155 0,193 1,350 0,080 0,040
0,168 0,645 0,155 0,125 0,170 1,320 0,245 0,215
0,158 0,825 0,173 0,150 0,194 1,410 0,115 0,085
Ol
0,168 0,500 s
0,183 0,130 0,174 1,255 0,203 0,080
0,124 0,720 0,180 0,155 0,162 1,195 0,155 0,115
0,175 0,705 0,095 0,070 0,190 1,195 0,125 0,088
0,146 0,750 0,120 0,153 0,173 1,305 0,128 0,130
0,062 0,615 0,123 0,050 0,095 1,165 0,170 0,120
0,083 0,785 0,128 0,079 0,170 1,035 0,178 0,103
0,226 0,785 0,120 0,100 0,196 1,045 0,095 0,070
0,137 0,610 0,076 0,045 0,166 1,000 0,120 0,075
0,150 0,688 0,125 0,105 0,218 1,435 0,105 0,130
0,206 0,775 0,125 0,130 0,200 1,430 0,088 0,125
0,095 0,905 0,078 0,053 0,160 1,590 0,580 0,070
0,220 0,790 0,093 0,098 0,146 1,525 0,540 0,133
0,196 0,825 0,150 0,295 0,189 1,235 0,065 0,050
0,054 0,465 0,205 0,210 0,180 1,180 0,145 0,095
 c Mn Ni Cr C Mn Ni Cr

0,185 1,525 0,594 0,129 0,385 1,150 0,220 0,820

0,218 1,225 0,140 0,101 0,168 1,330 0,600 0,900

0,181 1,085 0,202 0,139 0,187 1,380 0,790 0,775

0,151 1,515 0,543 0,100 0,163 1,130 1,010 1,110

0,199 1,325 0,081 0,107 0,277 0,690 0,160 1,010

0,149 1,428 0 , 5 .S 7 0,114 0,105 0,500 0,295 0,945

0,204 1,210 0,090 0,080 0,104 0,495 0,090 0,980

0,192 1,410 0,130 0,130 0,185 1,205 0,320 1,370

0,123 0,920 0,130 0,095 0,140 0,650 0,235 0,955

0,115 1,050 0,155 0,105 0,138 0,590 0,230 0,750

0,095 1,210 0,160 0,100 0,141 0,568 0,360 0,985

0,180 1,000 0,140 0,165 0,160 1,400 0,190 0,780 UI

0,080 0,085 0,251 0,625 0,205 1,000 co
0,155 1,420
0,090 1,160 0,200 0,120 0,242 0,775 0,230 0,980
0,180 1,330 0,130 0,130 0,193 0,720 0,215 1,000

0,150 1,150 0,085 0,070 1,000 1,040 0,780 1,580

0,135 1,380 0,060 0,070 0,222 0,700 0,756 2,670

0,190 1,040 0,100 0,090 0,162 0,470 0,135 1,275
0,120 1,130 1,790 0,070 0,080 1,095 0,779 1,835
0,105 1,280 0,110 0,995 0,086 1,010 0,765 1,693
0,170 1,250 0,760 0,760 0,081 1,023 0,783 1,865
0,170 1,270 0,780 0,770 0,128 0,995 0,930 1,430
0,154 1,340 0,188 0,795 0,135 1,000 0,880 1,350
0,185 1,355 0,233 0,840 0,200 0,770 0,100 1,030
0,200 1,070 0,225 0,750 0,090 0,915 0,765 1,660
 Mn Ni Cr Mn Ni

0,175 0,885 0,780 1,300

0,135 0,550 0,220 0,880
0,235 0,680 0,245 0,960
0,098 0,900 0, 750 1,720
0,165 1,370 0,730 0,845
0,155 1,180 1,010 0,765
0,143 0,338 4,645 0,418
0,117 0,380 4,500 0,330
0,114 0,405 4,540 0,335
0,100 0,550 3,280 0,020
0,095 0,600 0,170 2,220
0,101 0,460 0,225 2,100
UI
f
 - 55 -

T A B L E A U 6

ANALYSE CHIMIQUE TX MICROSEGREGATION

REPERE

C S Mn Ni Cr Mn Ni Cr

A 0,291 0,025 0,640 0,140 0,155 0,526

B 0,175 0,025 1,310 0,150 0,130 0,460

C 0,233 0,004 0,710 0,758 2,670 0,555 0,413 0,381

0 0,293 0,030 0,750 0,175 0,160 0,272

E 0,162 0,034 0,830 0,170 0,150 0,312

F 0,197 0,009 1,210 0,140 0,090 0,376

G 0,212 0,026 1,200 0,065 0,050 0,325

H 0,164 0,014 1,350 0,190 0,800 0,370 0,379

I 0,154 0,017 1,520 0,535 0,130 0,296 0,277

J 0,152 0,020 0,565 0,355 0,980 0,440 0,390 0,360

K 0,132 0,015 0,355 4 , 540 0,365 0,420 0,350 0,360

 56-

REPERE
(EmT/EmL)o (EmT/EmL)h (EmE/EmL)o (EmE/EmL)h H
TOLE

A 0,88 0,96 0,56 0,53 + 9,1 % 1 3 , 6 7.

0,53 0,52 0,29 0,28 - 2 7. 88 %
' 0,53 0,58 - - + 9,4 % 88 7.
C 0,91 0,85 0,45 0,51 - 6,8 % 9 , 9 7.
D 0,82 0,89 - - + 8,5 % 21,9 %
E 0,81 0,78 - 3,7 % 2 3 , 4 7.
F 0,73 0,81 - - + 1 1 , 1 7. 37 %
G 0,97 0,95 - - - 1,4 % 3,1 %
H 0,80 0,93 - - + 16,7 % 25 %
I 0,77 0,75 - - - 2,7 % 29,9 %
J 0,78 0,63 - - - 19 2 8 , 2 7.
0,94 0,82 - 13,3 % 6,4

T A B L E A U

Evolution de l'anisotropie de l'nergie m axim ale de rupture aprs hom ognisation

1225C - 8 heures. (B' : homognisation supplm entaire 1225C - 120 heures de
l'chantillon B ) . Pour les chantillons A, B, C on a examin galem ent l'volution
de l'nergie m axim ale sur prouvettes en sens paisseur.
European Communities Commission

EUR 6655 Microsegregation of alloying elements in structural steel plates

J. BEGUINOT, J. FALCE, P. MARTINON - Creusot-Loire, Le Creusot

Luxembourg: Office for Official Publications of the European Communities

1980 - VII, 56 p., 20 fig. - 21.0 29.7 cm

'Technical Steel Research' series

EN, FR

ISBN 92-825-1647-4

Catalogue number: CD-NC-80-004-EN-C

BFR 460 DKR 88 DM28,50 FF 66,50 IRL 7.70

UT 13200 HFL 31,50 UKL 7.40 USD 16.50

At first, the spatial distribution of microsegregation in the ingot and in the corre
sponding plate was studied. In both cases, microsegregation ratio is a maximum
in the axis of the upper part. The evolution of the microsegregation's ratios of Mn,
Ni Cr was then investigated versus the chemical composition of the upper-axis
parts of 115 plates representing a wide range of structural steels. Formulations of
the microsegregation ratios were derived for manganese and nickel.

The time-temperature parameters were defined for an anneal able to homogenize

the microsegregation and the microstructure. Also it was demonstrated in the ran
ge of steels studied, that elongated inclusions (Mn S, clusters of oxides) are main
ly responsible for the anisotropy of the ductility; the microsegregation and the
banded structure have then a second order influence. This explains that the homo-
genization anneal, effective for the equalization of microsegregation and micro-
structure, have no real influence on the ductility. The interest of such an anneal for
other metallurgical properties is discussed.
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