Bull. Mater. Sci., Vol. 29, No. 1, February 2006, pp. 5966. Indian Academy of Sciences.

Microstructures and properties of low-alloy fire resistant steel

BIMAL KUMAR PANIGRAHI
R&D Centre for Iron and Steel, Steel Authority of India Limited, Ranchi 834 002, India
MS received 10 June 2004; revised 2 November 2005
Abstract. Microstructures and properties of weldable quality low-alloy fire resistant structural steels (YS:
287415 MPa) and TMT rebar (YS: 624 MPa) have been investigated. The study showed that it is possible to obtain
two-thirds of room temperature yield stress at 600C with 020025% Mo and 030055% Cr in low carbon
hot rolled structural steel. Microalloying the CrMo steel by niobium or vanadium singly or in combination
resulted in higher guaranteed elevated temperature yield stress (250280 MPa). The final rolling temperature
should be maintained above austenite recrystallization stop temperature (~ 900C) to minimize dislocation
hardening. In a quenched and self-tempered 600 MPa class TMT reinforcement bar steel (YS: 624 MPa), low
chromium (055%) addition produced the requisite yield stress at 600C. The low-alloy fire resistant steel will
have superior thermal conductivity up to 600C (> 30 W/mk) compared to more concentrated alloys.
Keywords.

1.

Fire resistant steel; thermomechanical processing; microstructure; strength; thermal conductivity.

Introduction

Steel structures using mild steel in fire sensitive areas are

protected from fire by providing fire resistant coating or
insulation. This adds to the constructional cost. The problem
with unprotected carbonmanganese mild steel is its poor
strength at temperatures above ~ 350C, which can make
a structure unsafe after a major fire. In case of short duration
fire, it is rather difficult to assess the damage to structures
caused by fire and may call for demolition/renovation of the
structures. Most of the research efforts relating to construction
in fire sensitive areas were directed towards development
of steels that can retain adequate strength after prolonged
exposure in fire. The building codes of some specifications
require the steel to have a minimum of one-half (ASTM
1996) to two-thirds (Fushioni et al 1995; BIS 2002) of room
temperature yield strength at 500600C compared to the
mild steel which retains about one-third of room temperature
yield strength at 600C. In order to achieve this strength
level, the steel chemistry and manufacturing process are
closely controlled. Previous studies on microstructure and
mechanical properties of fire resistant steels carried out
by Chijiwa et al (1993) and Assefpour-Dezfully et al (1990)
focussed on processing, structure and properties of fire
resistant steels with different combinations of alloying
elements. In the present investigation, the effect of lower
alloying addition, particularly molybdenum, on the elevated
temperature properties will be discussed which is important
due to increasing alloy cost. Over and above, there is hardly

(panigrahi@[Link])

any information on alloying required to obtain two-thirds

of room temperature yield stress at 600C for thermomechanically treated (TMT) rebar particularly, the high strength
variety with yield strength above 600 MPa. The present
work was carried out to ascertain minimum requirement of
molybdenum/chromium in steels with and without microalloying elements in order to achieve the guaranteed
strength at 600C in plate, structurals and TMT rebar and
their effects on structure and properties.
2.

Experimental

Six experimental laboratory heats (steels AF) and one

industrial heat (steel G) were melted in 01 T air induction
(IF) and 6 T electric arc furnace (EAF), respectively for processing to plate and beam. The ingots from IF heats were
soaked at 1250C for 2 h and thermomechanically processed
(TMP) in an experimental rolling mill to 1214 mm thick
plates in nine passes. The ingot from EAF heat was soaked
at 1320C for 4 h and rolled to blooms of size 230
160 mm. These blooms were soaked at 1250C and subsequently thermomechanically processed to 200 100 mm
beam section. The finishing rolling temperatures (FRT)
for plates and beam were measured with an infrared pyrometer up to an accuracy of 5C and were between 800 and
925C. The finishing pass reduction was 2030% for plates
and about 10% for beam. The plates and beam were allowed
to cool in natural air after rolling. Another heat (steel H)
was made in 250 T twin hearth furnace and cast as 9 T
ingots for processing to TMT rebar. The ingots were rolled
to billets of size 100 100 mm after soaking at 1300C
for 4 h. These billets were subsequently reheated at 1250C
59

60

Bimal Kumar Panigrahi

and processed to TMT rebar of 32 mm diameter through a

Thermex cooling system.
Round tensile specimens (dia. 625 mm) were machined
from the quarter width position of the plates (width of
plate: 135 mm) in the longitudinal direction as per ASTM A
370 standard and tested at room temperature (30C) and
at elevated temperatures up to 600C at cross head speed of
2 mm/min in a servohydraulic test machine as per ASTM
E 8 and E 21 standards, respectively. Tensile testing of
plates was also carried out selectively at room temperature after exposure at 600C for 3 h under applied stress
of 140 MPa. The specimens after exposure were allowed to
cool to room temperature inside the furnace. In the elevated
temperature test of plates the specimens were heated from
room temperature to the test temperature and soaked at
the desired temperature for 15 min before tensile stress
was applied. The accuracy of the test temperature was controlled within 1C. Charpy V-notch impact test specimens
of size 10 10 55 mm from steels AF were machined
across the plate width in the longitudinal direction and
tested at RT to 30C as per ASTM E 23 standard. The
optical microstructure was examined in the longitudinal
through thickness direction after polishing and etching by
2% nital. The average grain size was measured by linear
intercept method. Transmission electron microscopic (TEM)
investigation was carried out using thin foils prepared
from mechanically thinned strip of thickness below 01 mm.
The electropolishing was done in a twin jet polisher using
a solution of 5% perchloric acid and 95% glacial acetic
acid at 20C and 60V operating voltage. The foils were
observed at 200 keV.
Flat tensile specimens (gauge length: 565 area) were
prepared in the longitudinal direction from the web of the
beam as per IS 2062 standard (BIS 1998). The ambient
and elevated temperature tensile testing was conducted as
described for plates. Tensile testing was also done after
an aging treatment at 600C for 3 h under applied tensile
stress of 140 MPa. Charpy V-notch specimens (size
75 10 55 mm) were prepared from the flange region
as described in IS 2062 standard and tested as described
for plate in the longitudinal direction. The optical microstructure was examined in the longitudinal through thickness
direction after polishing and etching by 2% nital. The
average grain size was measured by linear intercept method.
TEM specimens were prepared from the flange region as
described for plate and observed at 200 keV. Full scale
fire resistance test was carried out on beam section (size
200 100 3900 mm) as per ASTM E 119 standard (ASTM
1996) at Fire Research Laboratory, CSIR, Roorkee, India.
The bare beam was mounted on the specimen frame
holder of a gas fired furnace. The furnace was rectangular in
shape. The casing was made up of steel reinforced sections. The refractory lining of the furnace consisted of
front layer of kyanite insulation bricks backed by hot face
insulation. The burner casing was made up of fire bricks.
The complete furnace assembly consisted of four walls

and the open roof top for mounting the beam specimen.
The flue gas for heating passed through a duct surrounding
the sides of the walls and then was disposed off through a
chimney. There were ten long flame burners. The capacity
of each burner was 3540 l/h. The furnace was run on positive
pressure. The heating of the specimen was done as specified
in ASTM E119 standard. The thermocouples were fixed
at four different sections of the beam to measure the rise
of temperature at different intervals. While plotting the temperature vs time curves, average temperature measured by
concerned thermocouples in a section was used.
Tensile testing of rebar was done using unmachined
rebar (gauge length: 5 dia.) at ambient temperature in a
60 T servo hydraulic tensile testing machine at a cross
head speed of 10 mm/min. For the elevated temperature
test at 600C, round specimens were used from the core
region of rebar and tested as described for plate material.
Charpy V-notch impact specimens were also prepared
from the location described previously (Panigrahi and
Jain 2002) and tested similar to plate. The optical microstructure was examined in the transverse section after
polishing and etching by 3% nital. TEM specimens were
prepared from the rim and core regions of the rebar as
described for plate and observed at 200 keV.

3.

Results and discussion

3.1

Chemical composition

In a structural steel, the composition will be determined

by the requirement of strength, toughness and weldability. The chemical composition of steels is given in table 1.
The carbon was 011013% in plate, 017% in structural
beam and 025% in TMT rebar. The conventional way to
improve moderately the strength at elevated temperature
(up to ~ 350C) is by increasing the carbon content (Houdremont 1953). Lower carbon in hot-rolled steel improves
notch toughness and weldability. In TMT rebar carbon
increases the hardenability. Manganese increases the strength
by solid solution hardening (Baird and Jamieson 1972) in
hot rolled steel. Manganese tends to lower the eutectoid
carbon content in steel and promotes segregation particularly in hot rolled structural steel with carbon > 010%.
This can adversely affect the mechanical properties. Manganese was restricted to 1% in fire resistant hot rolled plate
and structural with carbon 010020% and 15% in TMT
rebar where manganese is a potential hardenability enhancing element. Silicon content in steels AG varied
from 029035%. Silicon is a solid solution strengthener
and a deoxidizer. Silicon retards softening at high temperatures (Irvine 1962) and also increases the hardenability.
However, in steel H, its content was low due to technoeconomic reasons. The aluminium (001002%) is
required to tie-up free nitrogen to improve toughness. In
the steels A, D, E and F, the content of aluminium was

Fire resistant steel

Table 1.

Chemical composition of steels (wt.%).

Steel

C
Mn
Si
S
P
Cr
Mo
Nb
V
Al
N

011
102
035
0022
0019
031
026

00033
00042

B
012
102
035
0032
0025
029
020

0099
00063

012
108
029
0029
0027
040
014

0097
00067

013
099
031
0025
0021
038
026
002

00034
00047

013
100
031
0026
0022
039
026

007
00039
00047

lower than the prescribed range. The rebar steel was

semi-killed. Chromium in small percent forms (FeCr)3C
(Houdremont 1953) in the cementite of pearlite. It is a
ferrite stabilizer and increases the hardenability. However,
its potential as a solid solution strengthening element is
small due to its high affinity to carbon. The amount of chromium was 029040% in plate and 055% in structural
beam and TMT rebar. Molybdenum increases elevated
temperature yield strength (Argent et al 1970; Honeycombe 1981) even when present in small percent (~ 025%)
in solid solution in low carbon steel. It also forms carbide
(Fe, Mo)3C in the cementite of pearlite resisting softening
on prolonged exposure in a fire (Houdremont 1953). Molybdenum tends to hinder self-diffusion of iron (Houdremont
1953), thus increasing the recrystallization temperature of
steel. Microalloying elements, vanadium and niobium,
increase the elevated temperature strength (Pickering 1978;
Sage 1983). They also increase the recrystallization temperature of steel (Borato et al 1988). Their carbides also offer
resistance to softening when the steel is exposed to fire.
The chemistry of the present investigation differs from
the previous studies (Assefpour-Dezfully et al 1990; Chijiwa et al 1993; Fushioni et al 1995) in the following
ways: (a) the content of molybdenum and chromium is
low, (b) low niobium and vanadium are used in microalloyed steels and (c) chromium without molybdenum has
been used in TMT rebar.

F
012
096
030
0025
0021
038
026
002
012
00039
00070

G
017
074
031
0034
0027
054
022

0052
00124

H
025
142
0056
0024
0024
055

0004
00075

As the finish rolling temperatures (FRT) of all steels except steel F and a few structurals of steel G were above tnr,
an equiaxed ferrite microstructure could be obtained with
low dislocation density. Steel F was finish rolled at 800C,
quite below tnr (8841C) but above Ar3 temperature (771C)
(Ouchi et al 1982). Deformation in this region strain
hardened the austenite, increasing its dislocation density.
Deformation bands are also formed (Tanaka 1981). Since
ferrite nucleates both on austenite grain boundaries and
deformation bands, the grains are finest (77 m). However, the cellular structure retained by rolling below tnr,
lowered the yield strength at elevated temperatures.
In the processing of TMT rebar (figure 1), initially at
higher temperatures (12001100C) the material recrystallizes statically. At the intermediate and finishing stages
of processing (10001050C), static, dynamic as well as
metadynamic recrystallization of austenite can occur (Poliak
and Jonas 2003) depending upon strain at different passes
producing an equiaxed austenite structure. On leaving the
finishing stand at 10001050C, the bar enters a Thermex
cooling chamber where the surface of the bar is cooled by
pressurized water at ~ 200C/s forming a thin rim of lath
martensite while the core is still austenite. On emergence
from the cooling chamber, the martensite rim gets selftempered by the heat of the core and the core finally
transforms to bainite.
3.3

3.2

61

Microstructure

Thermomechanical processing (TMP)

Processing plays an important role since it determines the

final microstructure and mechanical properties of hot
rolled steel (Panigrahi 2004). The TMP schedule for plate
and beam is shown in figure 1. TMP of plate and beam
involves controlled deformation of austenite at higher
temperatures above the recrystallization stop temperature
(tnr) (Borato et al 1988) during which static and dynamic
restoration processes occur (Tanaka 1981). Table 2 shows
data on total reduction, approximate recrystallization stop
temperature, finishing temperature and grain size of steels.

Typical optical microstructures of some steels in as-rolled

condition are shown in figure 2. The CrMo (steel A) and
CrMoNb (steel D) alloyed plates (figures 2a and b) and
beam (figure 2c) showed a predominantly polygonal ferritepearlite microstructure. At higher magnification, steel
A (figure 2d) also showed upper bainite (arrow mark). The
bainite in steel A resembles pearlitic bainite (Bhadeshia
1992) as the colonies tend to have crystallographic facets
rather than nicely rounded colonies of conventional pearlite. The vanadium (steel E) and niobium plus vanadium
(steel F) microalloyed steels also showed similar micro-

Bimal Kumar Panigrahi

62

Schematic of TMP schedule for plate, beam and TMT rebar (M, martensite; , austenite).

Figure 1.

Figure 2. As hot rolled microstructures of a. CrMo plate (steel A), b. CrMoNb plate
(steel D), c. CrMo beam (steel G) and d. pearlitic bainite of CrMo plate (steel A).
Table 2.
Steels
A
B
C
D
E
F
G
H

Process parameters and microstructural data.

Thickness
Total
(mm)
reduction (%)
14
12
12
12
12
12

86
88
88
88
88
88
94*
92

tnr (C)

FRT
(C)

Structure

Grain size
(m)

Product

8140
8535
8743
8769
8285
8841
874
9844

900
900
900
900
875
800
850925
1000

F+P+B
F+P
F+P
F+P+B
F+P+B
F+P+B
F+P+B
M+B

104
135
125
110
125
77
103

Plate
Plate
Plate
Plate
Plate
Plate
Beam
Rebar

F, Ferrite; P, pearlite; B, bainite; M, tempered martensite; *flange region; tnr = 887 +

464%C + (6645%Nb664%Nb) + (732%V230%V) + 890% Ti + 363%Al357%Si.

Fire resistant steel

Figure 3.

63

Bright field TEM of a. CrMoNbV plate (steel F), b. and c. CrMo beam (steel G) and d. TMT rebar.

structures. The bainite colonies in steel G were coarser

than steels A, D, E and F and were more numerous possibly due to presence of somewhat higher carbon and
chromium in this steel, lower reduction per pass and
coarser austenite grains prior to transformation. The bainite
was not observed in steels B and C. The finishing rolling
in the austenite region above recrystallization stop temperature helped to form polygonal ferrite grain structure in
CrMo, CrMoNb and CrMoV plate steels. In this
case ferrite nucleates on austenite grain boundaries (Tanaka
1981). CrMoNbV plate (steel F) was finish rolled in
the unrecrystallized austenite region producing grain size
finer than other steels (table 2) due to nucleation of ferrite
on austenite grain boundaries, transgranular twins and
deformation bands (DeArdo 1995; Panigrahi 2001) after
transformation. The partial cellular structure of steel F
with dislocations retained is shown in figure 3a. The beam
steel also showed upper bainite (figure 3b) with cementite
particles distributed between ferrite platelets (figure 3c).
An exposure treatment up to 3 h at 600C did not show
changes in the appearance of microstructure. Unlike
martensite in which dissolved carbon in solid solution is
high, bainite has little carbon in solid solution and is
much less sensitive to tempering at low temperatures
(~ 600C). However, cementite particles can coarsen and
a general recovery of dislocation substructure occurs
(Bhadeshia 1992). The TMT rebar steel showed a tempered
martensite rim. The core structure was bainitic (figure 3d)
due to high hardenability of this steel.

3.4

Elevated temperature yield stress

The dependence of yield stress and UTS with temperature

for steels AG is shown in figure 4. Steel F showed a
faster drop of yield stress after 500C. However, except
steel C (014%Mo) whose yield stress was marginally
below the desired level at 600C, all other steels retained
two-thirds of their room temperature yield strength at
600C (table 3). The elevated temperature yield stress depends mainly on the stability of microstructure at higher
temperatures. Chromium and molybdenum have a stabilizing effect on cementite of pearlite (Houdremont 1953).
A higher amount of chromium in steel C prevented excessive drop of yield stress at 600C despite low molybdenum
(014%) in it. Steels D and E that are microalloyed with
Nb and V, respectively have highest level of yield stress
at 600C viz. 82% and 85%, respectively. Nb and V have
added advantages due to their precipitation hardening
potential and the loss of strength at higher temperature is
minimal. The rapid drop of yield stress of steel F above
500C was due to lowering of dislocation density on
soaking above 500C. The UTS of all steels fell sharply
above 400C (figure 4). The elongation of all steels at
600C was higher than elongation at the ambient temperature. Exposure at 600C for 3 h increased the yield
stress by about 50 MPa without significant change in
elongation in steels A, D, E, F and G. The core of rebar steel
H with bainitic structure also showed two-thirds of room
temperature yield stress at 600C (table 3). Due to presence of

Bimal Kumar Panigrahi

64

Temperature (C)
Figure 4.

Temperature (C)

Dependence of (a) yield stress and (b) UTS on temperatures of fire resistant steels and mild steel (MS).

Table 3.

Tensile properties of the investigated steels.

Steel

287
505
380

293
486
362

298
539
320

338
582
300

293
530
378

415
622
268

320
541
273

624
819
125

Elevated temperature (600C)

YS (MPa)
219
UTS (MPa)
326
El. (%)
422
% of room temperature YS 763

191
259
417
651

188
247
490
630

279
332
404
825

250
327
362
853

280
338
460
674

214
292
330
668

419
426
305
671

408
523
308

348
475
340

469
584
228

369
492
270

Ambient temperature (RT)

YS (MPa)
UTS (MPa)
El. (%)

After thermal exposure at 600C under applied stress

YS (MPa)
360

UTS (MPa)
432

El. (%)
225

tempered martensite rim, the overall strength of TMT

rebar at 600C should be higher than two-thirds of its
room temperature yield strength. In a composite microstructure comprising tempered martensite rim and bainitic
core, the overall yield stress is given by area fraction of
rim multiplied by yield stress of rim plus area fraction of
core multiplied by yield stress of core. The area fraction
of bainite core was 0766 and that of tempered martensite
rim was 0234. Previous investigation (Panigrahi 2002)
showed that low-alloyed tempered martensite structure
had more than two-thirds of room temperature yield
stress at 600C.

3.5

Impact toughness

The ambient temperature impact toughness, 50% energy

ductile brittle transition temperature (DBTT) (Dahl 1992)
and fracture characteristics are given in table 4. The upper
shelf energy of as-rolled plate and beam varied from 65
118 J (figure 5). The steels A, D, E and F showed DBTT
at 4C to 12C. The DBTT of steel B was below 30C
and that of steel C was 28C. Presence of upper bainite
in all steels except steels B and C, low aluminium content
(steels A, D, E and F) and cellular structure (steel F)
were responsible for increase in DBTT. Notwithstanding

Fire resistant steel

higher carbon content, steel H showed a DBTT of 14C
due to presence of tempered martensite and some acicular
ferrite in it. Steel G showed a DBTT of 5C in as rolled
condition and 34C in aged condition. The DBTT of
steel G in as rolled condition was higher than steel A possibly
due to presence of relatively coarser colonies of pearlitic
bainite in its microstructure and a higher carbon content
(017%) (Pickering 1978) compared to steel A (011%

65

carbon). On exposure at 600C, the improved toughness

(DBTT: 34C) of steel G could be due to lowering of
dislocation density of bainite and diffusion of embrittling
atoms present on the grain boundaries to the dislocations.
Improvement of impact transition temperature by diffusion
of phosphorus from prior austenite grain boundaries to
lattice defects was reported earlier for spring steel (Wettlaufer
and Kasper 2000). However, upper shelf energy of aged
steel was lower than the as-rolled beam possibly due to
microstructural heterogeneity leading to formation of localized carbide rich areas that aided lowering of the absorbed
energy.

3.6 Fire resistance

The average temperature rise of fire resistant steel (FRS)
beam and mild steel (MS) beam (017C, 069Mn, 004Si,
0048S, 0028P, 0007Al) is shown in figure 6 for section

Table 4.
Steel

Temperature (C)
Figure 5.
beam.

Charpy energy vs temperature curves of plates and

Charpy toughness data.

Toughness at RT
(Joule)

A
118
B
116
C
100
D
94
E
82
F
73
G (as rolled)
87
G (after thermal exposure 50
at 600C)
H
88

DBTT
Fracture
(C) surface at RT
12
< 30
28
9
8
4
5
34

Dimple
Dimple
Dimple
Dimple
Dimple
Dimple
Dimple
Dimple

14

Quasi cleavage

Temperature ( C)

Note: All values of toughness are for full size specimens.

Temperature (C)
Figure 6. Typical timetemperature curves for CrMo beam
(steel G) and mild steel (T1, T2 and T3 are locations of thermocouples at section 1).

Figure 7. Dependence of thermal conductivity of dilute steel

alloys on temperatures.

Bimal Kumar Panigrahi

66

1 (inset). The rise of temperatures up to 600C for other

sections was similar to section 1. It was observed that the
temperature of the fire resistant steel was at a lower level
compared to mild steel. The data points for these curves
remain below the ASTM E 119 standard timetemperature
curve in a fire test (ASTM 1996). The time to reach the
critical temperature (538C) was 32 min and 21 min for
fire resistant steel and mild steel, respectively. The rate of
heating is dependent on the thermal conductivity which is
a material property governing the flow of heat through a
material at steady state. Figure 7 shows the dependence
of thermal conductivity with temperature for pure iron
and some constructional steels (Riemann 1953; McGannon
1966). The thermal conductivity of pure iron and dilute
alloys decreases with rising temperature. The likely behaviour of 05Cr022Mo fire resistant steel which is a
dilute alloy is also shown in this figure. Its conductivity
should be higher than 30 W/mk at 600C. The dominant
carrier of the thermal conduction in pure metals and dilute
alloys is electrons (Ho et al 1975; Isachenko et al 1980;
Touloukian and Ho 1981; Landolt 1991). When small
amount of alloying elements (impurities) are introduced
in iron, it causes discontinuities in the crystal lattice structure and promotes scattering of free electrons decreasing
the room temperature thermal conductivity (Riemann 1953;
McGannon 1966). With rising temperature, the scattering
of free electrons is intensified (Isachenko et al 1980). This
causes a net reduction of thermal conductivity at higher
temperature. Even then the thermal conductivity of dilute
steel alloy is still high (> 30 W/mk) at 600C. Since in a
fire, temperature gradients are encountered, a high thermal conductivity material is desired to avoid degradation
by local necking.
4.

Conclusions

Small additions of Mo (020025%) and Cr (030055%)

in low carbon steel produced hot rolled fire resistant steel
with a minimum of two-thirds of room temperature yield
stress at 600C. Microalloying by niobium and vanadium
improved the ratio of YS600C/YSRT. However, final rolling
temperature should be maintained in the recrystallized
austenite region to ensure a microstructure free from high
dislocation density. The steels should be adequately treated
by aluminium to tie-up free nitrogen in order to realize
lower DBTT. In the quenched and self-tempered TMT
rebar steel, addition of ~ 055% chromium was adequate
to ensure the guaranteed strength at 600C due to transformation to tempered martensite rim and bainitic core. Despite
decreasing trend of thermal conductivity with the rise of
temperature in dilute alloys, the low alloy fire resistant
steel will have higher thermal conductivity up to 600C
(> 30 W/mk) compared to more concentrated alloys and
is less expensive.

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