Metal Science and Heat Treatment Vol. 50, Nos.

5 – 6, 2008

PIPE AND CORROSION-RESISTING STEELS

UDC 621.789.669.14.019

CHEMICAL COMPOSITION AND STRUCTURE OF LOW-CARBON

LOW-ALLOY PIPE STEEL FOLLOWING CONTROLLED ROLLING

V. M. Schastlivtsev,1 I. L. Yakovleva,1 N. A. Tereshchenko,1 V. V. Kurban,2

V. L. Kornilov,2 V. M. Salganik,3 and A. M. Lesin3

Translated from Metallovedenie i Termicheskaya Obrabotka Metallov, No. 5, pp. 3 – 8, May, 2008.

We study the patterns of variations in chemical composition for a large number of commercial melts of three
grades of pipe steel: 17G1S-U, 10G2FB, and 12G2Sb via statistical clustering of experimental data. A com-
parative structural study was performed; the effects of various steel alloy components on the amount, distribu-
tion, and morphology of the pearlite component; the size and shape of the ferrite grains; and the development
of dynamic recrystallization processes.

INTRODUCTION daries [7, 8]. The pipe-steel composition includes a variety of

Interest in low-carbon low-alloy steels has increased in
recent years. On the one hand, this interest is due to the
stricter requirements of customer firms with respect to the
fabrication of pipe and strip plate. On the other hand, compe-
tition among manufacturers has resulted in a trend towards
modernization of equipment for steel smelting and subse-
quent rolling of the steel. This improvement of process capa-
bilities has enabled pipe steels to comply with [all relevant]
mechanical and process specifications.
Metallurgical approaches for development of high-
strength pipe steels have been thoroughly discussed in the
scientific literature [1, 2]. One promising area involves opti-
mizing the chemical composition of pipe steels by adding
microscopic amounts of vanadium, niobium, and titanium,
and simultaneously reducing the carbon content [3 – 5]; in
this case, solid-solution hardening is largely replaced by dis-
persion hardening. Alloying such steels with molybdenum
enhances the stability of supercooled austenite, facilitates
precipitation of special carbides, and limits softening after
hot deformation [6]. Boron improves the hardness penetra-
tion of the steel due to braking effect on the process of struc-
ture-free ferrite deposition along the austenite grain boun-
1
Institute for Physics of Metals, Ural Division, Russian Academy
of Sciences, Ekaterinburg, Russia.
2 ethyl alcohol, the structure of the steel was studied using an
Magnitogorsk Metallurgical Complex JSC, Magnitogorsk, Russia.
3
Magnitogorsk State Technical University, Magnitogorsk, Russia.
other chemical elements, with over 15 items being measured.
This paper presents the results from the first phase of a
comprehensive study of pipe steel hardened by controlled
rolling under industrial production conditions at the Mag-
nitogorsk Metallurgical Complex. The purpose of this paper
is to perform a statistical analysis of the chemical composi-
tion of steels, determine the characteristics of the alloying
process for specific grades of steel, and determine how these
characteristics relate to the structure.
METHODS OF STUDY
The studies included 17G1S-U, 10G2FB, and 12G2SB
steels from a total of 32 industrial melts. Blanks were cut
from sheet steel that underwent controlled rolling to a thick-
ness of 9 – 16 mm. The rolling conditions are listed in Ta-
ble 1. The tendency of the steel to form cracks in the ther-
mally affected zone around welds was theoretically esti-
mated based on the carbon equivalent Ce (wt.%). The carbon
equivalent was calculated using equation [9]:
Mn + Si Ni + Cu Cr + Mo + V
Ce = C + + + .
6 15 5
After thin sections were etched in a solution of HNO3 in
Epi-Tip-2 metallographic microscope and a JESM-200SX

207
0026-0673/08/0506-0207 © 2008 Springer Science + Business Media, Inc.
208 V. M. Schastlivtsev et al.

TABLE 1. Parameters for Controlled Rolling of Steel

Temperature at end
Coiling temperature, °C
of rolling process, °C
Grade of steel Shape, mm
minimum maximum minimum maximum
17G1S-U 12 – 9 821 859 515 576
Specifications per TU 14-1-5407–2000 820 – 870 535 – 585
10G2FB 14 – 16 773 874 534 630
12G2SB 15 789 827 545 595
Specifications per TU 14-1-5506–2005 785 – 815 565 – 595

scanning electron microscope. The electron microscopic ments for all melts: Maximum and minimum amounts, range
studies of thin foils were performed using a JSM-200CX mi- (describes variability in absolute units of wt.%), differentia-
croscope. tion factor, defined as the quotient of the maximum and mi-
nimum values (a dimensionless number characterizing the
RESULTS AND DISCUSSION relative variability of the statistic under study. The individual
chemical elements in the set of melts under study do in fact
Each grade of pipe steel studied has its own unique show appreciable variation in the quantitative values of these
chemical composition. However, the specifications for each statistics. Carbon has the highest variability among the addi-
grade of steel do permit a certain amount of melt-to-melt tion elements: It has a larger range of variation (0.14% ver-
variation in the content of alloying elements. If information sus 0.004%) and a higher differentiation coefficient (4.5 ver-
is available on the chemical composition of a fairly large sus 1.8) than nitrogen. The phosphorus content is more vari-
number of melts, the alloying characteristics typical of cer- able than the sulfur content for the set of melts under study.
tain specific metallurgical production conditions can be iden- Of the substitution elements, Mn has the widest range
tified and compared with the mechanical properties of the (0.5%), the differentiation coefficient is largest for Mo (68.3)
hardened steel. and Nb (35.5), and the values for Ni (15.0), Ti (10), Cu (7.5),
Table 2 presents the following data used to describe the V (6.5), and Cr (6.0) show just how highly variable this sta-
variability in the concentrations of various chemical ele- tistic is.
During the next phase, it will be of interest to determine
whether the concentration of chemical elements is random,
TABLE 2. Variability in the Concentrations of Various Elements or whether there are some common laws governing the
in the Chemical Composition of the Steels Under Study changes in concentration from melt to melt. Since carbon is
extremely important for the structure and mechanical proper-
Maximum Minimum Range of varia-
Element concentration, concentration, tion in concen-
Differentiation ties of the steels under study, we shall now rank the full set of
factor melts in monotonic order with respect to the concentration of
% % tration, %
C 0.180 0.040 0.140 4.5
this element. And while maintaining the order in this ordered
series, we shall then examine the concentration of the other
N 0.009 0.005 0.004 1.8
elements.
S 0.009 0.003 0.006 3.0
The results of this grouping in order of decreasing carbon
P 0.020 0.005 0.015 4.0
content are shown graphically in Fig. 1. The ordered series
Cr 0.060 0.010 0.050 6.0 begins with 17G1S-U steel (the first six melts have carbon
Ni 0.150 0.010 0.140 15.0 content 0.18 – 0.16%), half of the melts have carbon contents
Mn 1.690 1.190 0.500 1.4 of 0.10 – 0.12%, and the series ends with melts having car-
Ti 0.020 0.002 0.018 10.0 bon contents of 0.06 – 0.04% (10G2FB and 12G2SB steels).
Nb 0.071 0.002 0.069 35.5 The concentration of nitrogen is an order of magnitude
V 0.065 0.010 0.055 6.5 lower, and changes in the nitrogen content have no effect on
Si 0.480 0.220 0.260 2.2 the melt order determined based on carbon.
Cu 0.150 0.020 0.130 7.5 Figure 1 shows that the sulfur content varies over a rela-
Al 0.049 0.030 0.019 1.6 tively narrow range, and decreases with increasing melt
Mo* 0.205 0.003 0.202 68.3 number, i.e., as the carbon content decreases; phosphorus
Sn* 0.003 0.002 0.001 1.5 varies chaotically over a wide range throughout the ordered
B* 0.0004 0.0003 0.0001 1.3 series. To summarize, the low-carbon steels generally tend to
have low sulfur content (with a maximum value of 0.005%),
* Only determined for 10G2FB and 12G2SB steels. while no such trend exists for phosphorus. Thus, variations
Chemical Composition and Structure of Low-Carbon Low-Alloy Pipe Steel Following Controlled Rolling 209

E, wt.%
in phosphorus content may be one of the factors behind the C
0.200
scatter in the mechanical properties of the steels under study. N
0.150 C+N
The data presented in Fig. 1 suggest that the chromium, 0.100
copper, and nickel contents are fairly stable at carbon con- 0.050
tents of 0.10 – 0.17% (Melts 1 – 24 ), while the contents of 0
these elements have an inter-melt variation of more than an 0.025 P
order of magnitude at low carbon content (Melts 26 – 31 ). 0.020
S
This may have a substantial effect on austenite stability, 0.015
0.010
hardness penetration, and hardenability. Thus, stricter control
0.005
of the chemical composition of low-carbon steels with re- 0
spect to these elements will facilitate reproduction of stable Cr
0.15
mechanical properties for the steel in the hardened state. Cu
0.10 Ni
The change in alloy levels for manganese varies almost
0.05
monotonically within the ordered series (Fig. 1). This means
0
that the carbon content and manganese content of the steels
under study are closely correlated (the correlation coefficient 1.8
between manganese and carbon is 96%). The distribution of 1.6 Mn
the experimental points in a correlation diagram (Fig. 2, “=” 1.4
symbols) indicates that they are inversely proportional. The 1.2
regression coefficient indicates that a decrease of 0.1% in the 1.0
total carbon and nitrogen content is accompanied by an aver- 0.15
age increase of 0.3% in the manganese content. The carbon V
0.10 Nb
and manganese support the required level of austenite stabil- Ti
ity and facilitate hardening; when one of these elements (car- 0.05 V + Nb + Ti
bon) is at a reduced concentration, the deficit is compensated
for by a higher concentration of the other (manganese), as is 0
1 6 11 16 21 26 31
in fact observed in the set of melts studied. This inverse pro- Melt number (arbitrary)
portionality effect indicates that these elements were suc-
cessfully made interchangeable during the smelting process. Fig. 1. Concentration E of chemical elements in the steels under
The alloying characteristics of titanium, niobium, and study, placed in order of total nitrogen and carbon content.
vanadium in these steels are shown in Fig. 1; the amounts of
these elements tend to increase with increasing melt number
in the ordered series. Titanium, niobium, and vanadium are
SV, Nb, Ti; Mn, wt.%
1.8
the alloying element with the highest tendency to form
strong, stable carbonitrides, thereby facilitating dispersion
1.2
hardening, formation of smaller grains, and changes in the
stability of supercooled austenite. These chemical elements
0.6
behave similarly in the austenite solid solution because of the
high similarity between carbon and nitrogen [10].
0
This fact provides us with a basis for adding together 0.19 0.16 0.13 0.10 0.07 0.04
these amounts and comparing them against the total amounts Ñ + N, wt.%
of carbon and nitrogen in each of the melts. The distribution
Fig. 2. Concentrations of Substitution Elements in the Chemical
of the “^” symbols in Fig. 2 indicates that there is a close in- Composition of the Steels Under Study, for Various (C + N) Con-
verse correlation between the variation in these quantities, tents: ^) V + Nb + Ti; =) Mn.
with a correlation coefficient of 95%. When the carbon + ni-
trogen content decreases by 0.1%, the total titanium + nio-
bium + vanadium content also increases by 0.1%. To sum- towards alloying will affect the proportionality of the rela-
marize, as the carbon decreases from 0.18% to 0.04%, the ra- tionship between the concentration of titanium + niobium +
tio (V + Nb + Ti)/(C + N) increases by more than an order of vanadium on the one hand and the concentration of carbon +
magnitude (from 0.17% to 2.85%). Even at a total (C + N) nitrogen on the other; this in turn affects the development of
content of 0.05 – 0.06% and a maximum concentration of phase transitions, affects the strengthening mechanisms, and
0.14 – 0.15% for the carbide-forming elements (V + Nb + Ti), has a substantial effect on the mechanical properties of the
there will not be enough carbide-forming elements to com- steels under study.
pletely bind all of the carbon into special carbides or The change in chemical composition not only affects the
carbonitrides of the form MC or M(CN). However, this trend mechanical properties of the steel, but also enables the pro-
210
Ñ, wt.%
0.4
0.3
0.2 Zone 2
Zone 3
0.1
Zone 1
0
0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9
Ñe
Fig. 3. Carbon content as a function of carbon equivalent (Ce ):
1 ) area safe against cold cracking in the thermally-affected zone
around the weld under any conditions [9]; 2 ) area where safety
against cold cracking depends on additional conditions; 3 ) area
where cold cracking is a risk under any conditions; =) steels studied,
with C content (0.10 – 0.18)% (Mo not specified); ^) steels studied
with (0.04 – 0.07)% C and (0.003 – 0.205)% Mo.
cess requirements on the material in the final structure to be
met. The issue for trunk pipelines is to improve the strength
specifications while maintaining satisfactory weldability.
These steels had calculated carbon equivalents of 0.30 –
0.48%. In the opinion of E. L. Makarov [11], if this criterion
is less than 0.45%, the material is not susceptible to cold
cracking during welding; thus, most of the steels being stu-
died can generally be classified as having good weldability.
The diagram in Fig. 3 enables a more definite prediction
of the condition of the material in the zone thermally affected
by the weld. All of the melts under study are divided into two
groups based on position within the correlation diagram. The
first group (“)” symbols) includes Melts 1 – 25 of 17G-1S-U
steel, in which cold cracks will presumably occur under un-
favorable conditions; the probability of defects increases as
the carbon content of the steel increases. The ratio between
the carbon content and carbon equivalent of the alloying ele-
ments means that the second group of steels (“^”) belongs to
the region of the diagram where cracks will not develop un-
der any conditions. Thus, if the carbon content of 10G2FB
and 12G2SB steels is limited to less than their nominal val-
ues, will make these steels more reliable for welding, despite
the additional alloying with carbide-forming elements.
The microstructure of the steels being studied is primar-
ily determined by the final conversion conditions during the
rolling phase in the inter-critical temperature region, and the
conditions for the cooling from the temperature at the end of
the rolling process and the coiling temperature. When com-
paring the production modes for rolled sheet against the ap-
plicable requirements, note that the 17G1S-U steel melts
largely comply with the process parameters. The following
V. M. Schastlivtsev et al.
15 mm
Fig. 4. Structure of 17G1S-U steel in the plane of the sheet.
competing processes occur during plastic deformation from
the 859 – 821°C temperatures present at the end of the roll-
ing process: Strain hardening of austenite, polymorphic
g ® a transformation, and eutectoid austenite decomposi-
tion. In the final state, the steel consists of a two-phase fer -
rite/pearlite structure (Fig. 4).
The image showing the metallographic structure of
17G1S-U steel in the direction parallel to the sheet indicates
that the pearlite colonies appear to be oriented relative to the
rolling direction. The excess ferrite grains are distributed be-
tween the pearlite areas and grouped into strips. This struc-
ture has a transverse period of 15 – 20 mm (Fig. 4). The fer-
rite grains have a mean size of 20 – 30 mm. The irregular
shape of the ferrite grains indicates that the boundaries are
highly mobile, and that recrystallization processes are well
developed. The strong contrast created by chemical etching
and (probably) the relatively low temperature at which the
pearlite transformation occurred hinder resolution of the in-
ternal structure of the pearlite areas. The scanning-elec-
tron-microscope image in secondary electrons provides a dif-
ferent type of contrast, and enables additional information to
be obtained on the mutual distribution of the phase compo-
nents. On a thin section obtained parallel to the thickness of
the sheet, i.e., in a plane perpendicular to the rolling plane,
the banded structure becomes isotropic (Fig. 5a ). Most of
the ferrite grains contain austenite decomposition products.
Certain grains show noticeable differences in the number and
dimensions of pearlite colonies, which form most frequently
along grain boundaries. The approximate volume fraction of
pearlite in the phase composition is estimated to be
15 – 23%. Note that the steel structure includes sulfur precip-
itates of the form (Mn, Ca)S (Fig. 5a and b ); no phosphorus
precipitates were observed along the grain boundaries.
Electron microscopic studies show that the carbon con-
tent of 17G1S-U steel is sufficient for formation of various
carbon-rich phase components. The structure contains two
forms of pearlite with different morphology: granular
pearlite (Fig. 6b), which apparently formed at higher conver-
sion temperatures, is also observed in addition to the tradi-
tional lamellar pearlite (Fig. 6a). Cementite particles, which
probably formed during post-rolling cooling of the sheet and
which initiate microcrack formation (Fig. 7), are distributed
Chemical Composition and Structure of Low-Carbon Low-Alloy Pipe Steel Following Controlled Rolling 211

2 mm
à 6 mm à

I
S
b
Fe
Mn Mn

Ca 2 mm
S Fe b
Ca
Fig. 7. Precipitates along the grain boundaries and formation of
2 3 4 5 6 7 8 microcracks in 17G1S-U steel (a) and a dark-field image in (103)Ts
G, keV
reflected light (b ).
Fig. 5. Structure of 17G1S-U in the plane normal to the surface of
the sheet (a) and an x-ray spectrum of the precipitates on the surface
of the thin section (b ) (I is the radiation intensity, and G is the energy
of the radiation.

5 mm

5 mm

Fig. 8. Fine structure of ferrite in 17G1S-U steel.

a
3 mm
b of 17G 61S-U steel. Figure 9a shows the microstructure of
Fig. 6. Structure of pearlite in 17G1S-U steel: a) lamellar; b ) gra-
nular.
along the grain boundaries. Fine structural details in the fer-
rite, especially the increased density of dislocations (Fig. 8),
indicate that the crystalline structure shows a large number of
defects inherited from the strain-hardened austenite and
which occur in the a-phase during deformation in the inter-
critical temperature interval.
The modified chemical composition of 10G2FB and
12G2SB steels — in particular, the reduced carbon content —
determines the specific characteristics of the supercooled
austenite conversion process and the nature of grain structure
formation during the ausforming process. These steels have
qualitatively similar microstructure which differs from that
10G2FB steel in the plane of the sheet.
According to the state diagram, the reduced carbon con-
tent causes a change in the proportions of excess ferrite and
pearlite (the maximum pearlite content is 3 – 5%). This
amount of this phase is insufficient to form large extended
precipitates, which means that the pearlite is distributed in
isolated disordered regions (Fig. 9a ). The direction in which
the rolling was performed can be identified based on the di-
212
15 mm
a b
15 mm
c d
Fig. 9. Structure of 10G2FB steel in the sheet plane (a), fine structure (b, d ), and dark-field image in
(120)Ts reflex (c).
rection in which the ferrite grain structure is elongated. The
elongated shape of most of the a-phase grains indicates that
dynamic recrystallization processes are not as well deve-
loped as they are in 17G1S-U steel. The disperse nature of
the structure is another distinguishing trait. Although there is
some spread in grain sizes, the ferrite grains have a mean size
of 5 – 10 mm, which is 3 – 6 times smaller than in 17G1S-U
steel. These structural characteristics indicate that diffusion
is slower, and that the grain boundaries have limited mobi-
lity; this is directly related to the presence of Mo and B in the
chemical composition, as well as the high concentration of
carbide-forming elements.
Electron-microscopic studies confirm that ausforming
has more effect on microstructure evolution in 10G2FB steel
than in 17G1S-U steel. This is apparent in the morphology of
the supercooled-austenite decomposition products. For exa-
mple, in the dark-field image obtained in (120)Ts reflection,
the cementite sheets shine in the form of short, bent crystals
(Fig. 9b and c). The steel apparently underwent plastic defor-
mation in the two-phase region after formation of the
cementite sheets, or there was a transfer of strain hardening
from the austenite to the pearlite, as described in [12]. The
ferrite has a very high dislocation density, and the distribu-
tion of the dislocations indicates that collective motion oc-
curred, and that there was a tendency for the formation of re-
gions and fragments with variant orientations (Fig. 9d ). Only
rare regions of a-phase are free of traces of plastic deforma-
tion, i.e., are free of dislocations. At he metallographic level,
these areas may be correlated with large, regular ferrite
grains. For low-carbon steels, the specifications call for a re-
V. M. Schastlivtsev et al.
5 mm
3 mm
duced interval at the end of the rolling process, which is not
always implemented in practice (see Table 2).
CONCLUSIONS
1. All of the melts of the steels under study (17G1S-U,
10G2FB, and 12G2SB) can be treated as a single set with in-
verse proportionality between the carbon content and the
content of carbide-forming elements (niobium, vanadium).
Limiting the carbon content substantially reduces the total
carbon equivalent and guarantees a lack of cold cracking in
the zone thermally affected by welding.
2. The alloying characteristics of the steels under study
lead to a difference in the structure formed during cold rolling.
The 10G2FB and 12G2SB steels differ from the 17G1S-U
steel in that the ferrite grain size is smaller, the dislocation
substructure is better developed, and there are differences in
the size and disperseness of the pearlite component.
This work was performed as part of the Russian Aca-
demy of Sciences Plan (Topic No. 01.2.00613392), with par-
tial support from Grant NSh-5965.2006.3.
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