642 Homsher

Materials Performance and
Characterization
C. N. Homsher1 and C. J. Van Tyne1
DOI: 10.1520/MPC20150002
Comparison of Two
Physical Simulation Tests
to Determine the
No-Recrystallization
Temperature in Hot
Rolled Steel Plates
VOL. 4 NO. 3 / 2015
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Materials Performance and Characterization
doi:10.1520/MPC20150002 Vol. 4 No. 3 / 0000 / available online at www.astm.org
C. N. Homsher1 and C. J. Van Tyne1
Comparison of Two Physical

Simulation Tests to Determine the
No-Recrystallization Temperature
in Hot Rolled Steel Plates
Reference
Homsher, C. N. and Van Tyne, C. J., “Comparison of Two Physical Simulation Tests to
Determine the No-Recrystallization Temperature in Hot Rolled Steel Plates,” Materials
Performance and Characterization, Vol. 4, No. 3, 2015, pp. 1–14, doi:10.1520/
MPC20150002. ISSN 2165-3992
ABSTRACT
Manuscript received January 16, Two rolling simulations were conducted using a Gleeble 3500 to determine the
2015; accepted for publication no-recrystallization temperature, TNR on six microalloyed plate steels. Double
June 17, 2015; published online
July 24, 2015.
hit deformation tests and multistep torsion tests were performed on steels
1
containing varying amounts of Nb, V, and Ti. TNR for the double hit
Department of Metallurgical and
Materials Engineering, Colorado
deformation tests were determined by finding fractional softening using the
School of Mines, Golden, 5 % true-strain method and the intersection of the sigmoidal fractional
CO 80401.
softening curve with 20 % fractional softening. TNR for the multistep hot
torsion test were determined using a mean flow stress method and finding the
intersection of the two linear regions. TNR values following multistep hot
torsion testing were lower than values measured after double hit deformation
testing. The decrease in measured TNR values for the torsion tests occurs from
the inherent multiple deformations, resulting in refined grains and an increase
in nucleation sites for recrystallization during the subsequent deformation
steps; thus recrystallization can continue to occur at lower temperatures.
Keywords
steel rolling, no recrystallization temperature, double hit compression tests, multistep hot
torsion tests, microalloy
Copyright V
C 2015 by ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959 1
HOMSHER AND VAN TYNE ON PHYSICAL SIMULATION TESTS 2
Introduction
High strength low alloy (HSLA) steels commonly use microalloying additions of V,
Nb, and Ti, generally under 0.10 wt. %, for use in large diameter pipeline steels,
structural and automotive applications, and transmission towers. Microalloying is a
useful way to increase strength while minimizing plate thickness, and thus weight.
Microalloying helps control grain size by influencing the no-recrystallization
temperature (TNR) or phase transformations during processing and/or through pre-
cipitation strengthening during cooling [1].
TNR can be studied and quantified by a variety of methods including (1) direct
observations such as optical microscopy and electron backscatter diffraction, and (2)
external physical simulation methods such as multistep hot torsion testing, double-
hit deformation testing, and stress relaxation testing, which are based on material
softening calculations.
Direct measurement of the recrystallized fraction can be difficult in microal-
loyed steels. The material may transform during cooling and special etching techni-
ques, often following a low-temperature heat treatment, are necessary to reveal the
prior austenite grains (PAGs) [2–7]. The procedure is tedious and may be impossible
to use on quenched austenite in alloys with low hardenability. Once a procedure for
revealing the PAGs is determined, it is then often difficult to distinguish between the
recrystallized and deformed grains, leading to a level of subjectivity in the analysis
methodology.
Hence, the preferred methods for determining TNR include two physical simula-
tion techniques. Multi-deformation tests under continuous cooling, such as multi-
step hot torsion testing, can help identify TNR directly. This type of test is limited,
as it does not allow a fundamental study of the static recrystallization behavior
between two rolling passes for a given temperature, as the temperature is ever
decreasing. Isothermal deformations tests are also popular techniques for analyzing
recrystallization behavior. The most common isothermal tests are double-hit and
stress relaxation. These two tests determine the recrystallized fraction as a function
of temperature in the time interval between or after deformation steps. However,
many methods are reported in the literature to evaluate the softening ratio [8–14],
which influences the separation point between softening due to recovery and soften-
ing due to recrystallization. The results from these tests are therefore open to
ambiguity.
Extensive data on recrystallization kinetics are available in the literature;
however, limited information is available comparing data from various testing tech-
niques and analysis methodologies. Gomez et al. [15] and Vervynckt [16] correlated
isothermal double-hit deformation tests with continuous cooling multistep hot tor-
sion testing for static recrystallization kinetics and precipitation interaction, respec-
tively. Maccagno et al. [17] investigated TNR from industrial rolling mills with
laboratory simulations. Although various studies have been conducted over the
years, no standard method exists for determining TNR causing the values to vary
from one investigation to another. However, each method provides insight into the
influence of certain elements and processing parameters on TNR, i.e., precipitation
interaction, strain-rate dependence, etc. Therefore, comparison of data obtained
from different methods and studies must be assessed with precautions to account for

TABLE 1
Chemical compositions of laboratory Nb-bearing microalloyed steels in wt %.
Material Identification C Mn Si Ti Nb V Al N S P
Lo-Nb 0.063 1.47 0.019 0.006 0.027 <0.001 0.030 0.0041 0.0017 0.012
Hi-Nb 0.066 1.46 0.020 0.007 0.060 <0.001 0.028 0.0039 0.0017 0.011
Lo-V 0.065 1.46 0.016 0.005 0.060 0.021 0.030 0.0046 0.0017 0.012
Hi-V 0.068 1.46 0.017 0.005 0.061 0.056 0.029 0.0040 0.0017 0.012
Lo-Ti 0.062 1.48 0.018 0.028 0.060 <0.001 0.032 0.0050 0.0018 0.011
Hi-Ti 0.065 1.48 0.019 0.099 0.059 <0.001 0.030 0.0040 0.0019 0.011
discrepancies. The current study focuses on comparing double hit deformation test-
ing with multistep hot torsion testing, all performed on a Gleeble 35002.
Experimental Procedures
EXPERIMENTAL MATERIAL
Material for the current study was laboratory-produced, hot-rolled microalloyed
plate steel. The laboratory heats were Nb-microalloyed plate steel to meet API X-70
specifications if processed correctly. Table 1 gives the chemical composition of the six
alloys. The carbon content was held constant at roughly 0.065 wt. % and a base Nb
level of 0.060 wt. %. The alloys have varying levels of V, Nb, and Ti with a low and
high level. The Hi-Nb alloy is the control alloy.
DOUBLE HIT DEFORMATION TESTING

Double-hit deformation tests use cylindrical specimens in an axisymmetric compres-
sion test. The test involves reheating to ensure that most precipitates dissolve back
into solution, cooling to deformation temperature (Tdef), compressing to a given
_ holding for an interpass time (tip), deform-
strain (eÞ and with a given strain rate (e),
ing the specimen again while holding everything else constant, and determining the
percentage recrystallized or fraction of softening (FS) [12,13,18–22]. The current
study used samples with 10 mm diameter and 15 mm length, a true strain of 0.2, and
a strain rate of 5 s1 for all tests. Deformation temperatures (Tdef) were
750 C–1200 C at 50 C increments. The deformation parameters were as follows:
• Soak at austenitizing temperature of 1250 C for 10 min
• Cool to first deformation temperature of 1200 C at a constant cooling rate of
1.25 C/s
• Deform with-e ¼ 0.2, e_ ¼ 5 s1
• Hold for tip ¼ 5 s
• Repeat test with new sample and next Tdef
Figure 1 shows a temperature-time schematic of the double-hit deformation test.

The difference between the deformation curves is calculated by finding the fraction
softening (FS). The general equation for FS is given by [9,10,14,19,21–25]:
2
Dynamic Systems Inc. (DSI), Poestenkill, NY.

FIG. 1
General temperature-time
schematic of a double-hit
deformation test.
rm rr
(1) FS ¼
rm r0
where:
r0 ¼ the stress at 5 % true strain of the first deformation step,
rr ¼ the stress at 5 % true strain of the second deformation step, and
rm ¼ the stress of an extrapolated power-function curve at 5 % true strain of the
second deformation step.
The power function simulates the extrapolated curve without any softening.
Figure 2 shows a double-hit deformation stress-strain plot, extracting specific points
to calculate FS. In the current study, each test was run in triplicates to ensure
repeatability.
MULTISTEP HOT TORSION TESTING

Multistep hot torsion tests simulate the rolling process through a series of deforma-
tion steps (i.e., “hits”) and continuous cooling for a given set of parameters, such as
e, e,_ tip, and temperature range. The torque and the amount of twist are measured
and converted into stress and strain. One sample is used for the entire temperature
range and is deformed through the TNR. The current study used samples with
10 mm diameter and 20 mm gauge length, a true strain of 0.2, and a strain rate of
5 s 1 for all tests. Deformation temperatures were 750 C–1200 C at 25 C incre-
ments. The deformation parameters were as follows:
• Soak at austenitizing temperature of 1250 C for 10 min
• Cool to first deformation temperature of 1200 C at a constant cooling rate of
1.25 C/s
• Cool to next Tdef in 20 s at a cooling rate of 1.25 C/s

FIG. 2
Example of a double-hit
deformation curve used to
determine fractional softening
via the 5 % true-strain method.

• Continue test until the final Tdef (750 C) is reached
Figure 3shows temperature-time schematic for multistep hot torsion tests.

Figure 4 shows an example of the data collected from a multiple step hot torsion test.
FIG. 3
General schematic of a
multistep hot torsion test.

FIG. 4
Example of equivalent torque-
twist data from multiple step
hot torsion test.
From the procedure developed by Richardson et al. [26], the torque-twist data can
be converted into equivalent stress-strain. The Von Mises equivalent stress, r, is
given by,
pffiffiffi
3 3T
(2) r¼
2pa3
where:
T ¼ torque (N-m), and
a ¼ the radius (m) of the gauge section.
Equivalent strain, e, is given by,
0:724ah
(3) e¼ pffiffiffi
3l
where h is the angle of twist (radians), and

l ¼ the length of the gauge section (m).
A value of 0.724 is used as the effective radius following Richardson et al. [26]
and Barraclough et al. [27]. The concept of effective radius to calculate the stress
strain curve mitigates problems associates with the strain gradient across the diame-
ter of the specimen. Figure 5 shows the results of converting the torque-twist data
into stress-strain data. The mean flow stress (MFS) is given by
ð eb
1
(4) MFS ¼ r de
eb ea ea

FIG. 5
Example of equivalent stress-
strain calculated from torque-
twist data shown in Fig. 4 from
a multiple step hot-torsion test.
where:
eb and ea ¼ the final and initial strains per pass, and
r ¼ the summation of the stress per pass.
Once the MFS is calculated, it is plotted against the inverse of absolute tempera-
ture. Multiple stages are seen in the MFS graph, and TNR can be determined from
the transition between two of these stages. Figure 6 shows an example of MFS versus
the inverse absolute temperature. TNR is the intersection of the linear fit between
stages I and II. In this example, TNR is 958 C, which is read as 8.123 104 K1 off
the plot. The linear regions were found using a least squares regression.
Results and Discussion

DOUBLE HIT DEFORMATION TESTING
Figure 7 shows a plot of double-hit deformation true-stress true-strain curves at
1200, 1000, and 750 C for the Lo-V alloy. As expected, the flow stress of the test per-
formed at 1200 C is lower than the tests performed at 1000 and 750 C, while the
flows stress of the test performed at 750 C is higher than the tests at 1000 and
1200 C. Also noticeable in Fig. 7 is the comparison of the two flow curves at each
temperature. The 1200 C curves are almost identical, indicating 100 % fraction soft-
ening (FS). The 1000 C flow curves are similar, with the second curve showing more
work hardening than the first, indicating something less than 100 % FS. The 750 C
curves are similar to an interrupted test, where the second curve appears to be a con-
tinuation of the first, indicating close to 0 % FS. The fraction softening was found
for each alloy at each condition. Figure 8 shows the fraction softening as a function
of temperature for the Lo-V alloy. The circles indicate the average of the three tests

FIG. 6
Example of mean flow stress
versus absolute temperature
calculated from equivalent
stress-strain data.
FIG. 7
Plot of double-hit deformation
true-stress true-strain curves at
1200, 1000, and 750 C.

FIG. 8
Fractional softening of the Lo-V
alloy. TNR is denoted by the
dotted line at 20 pct. FS which
intersects close to 1000 C.
and the line represents a sigmoidal fit to the data. The dashed line indicates the 20 %
FS, which defines TNR [12].
MULTISTEP HOT TORSION TESTING

Following the analysis procedure provided above, the mean flow stress (MFS)
and subsequently the TNR for the six alloys was determined. Figure 6, above,
shows an example of MFS as a function of inverse absolute temperature for the
Lo-V alloy. Figure 9 shows the MFS versus inverse absolute temperature for the
three Lo-V test specimens on a single graph. The plot shows little variation in
MFS for the three specimens, indicating the testing conditions were consistent
for each run. The average TNR for the three specimens is 953 C with a range of
953 C–954 C.
Table 2 gives the TNR values obtained from double hit compression and
from multistep hot torsion for the six alloys in the current study. The TNR values
for hot torsion tests were expected to be lower than the double-hit tests due to
an expected difference in grain size at the TNR. At the measured TNR, the torsion
samples have already undergone a large number of deformation passes with a
large amount of total deformation. Multiple recrystallization cycles have
occurred, leading to grain refinement in the austenite. The grain size in the dou-
ble hit compression sample prior to the first deformation step is expected to be
large due to the high reheating time and temperature. With the refined grains in
the torsion sample, more nucleation sites are available for recrystallization, lead-
ing to a lower TNR.

FIG. 9
Comparison of the three Lo-V
test specimens for MFS as a
function of inverse absolute
temperature. The three tests
were very similar, showing
consistency in testing
procedure.
COMPARING THE TWO TESTING SIMULATIONS

The data follow the predicted outcome, having a lower TNR from multistep hot tor-
sion than from double-hit deformation simulations. However, Fig. 10 shows a weak
trend in the data between hot torsion and double-hit tests. There appears to be no
clear indication of how much influence hot torsion tests have on TNR compared with
double-hit deformation tests, i.e., the difference of TNR between hot torsion and
double-hit simulations is not consistent. Other factors may contribute to the
reported values of TNR. For example, double-hit deformation tests generally only
measure static recrystallization (recrystallization which occurs between passes),
while hot torsion tests may experience dynamic recrystallization (recrystallization
which occurs during deformation) due to a buildup of strain at lower temperatures,
near and below TNR [28]. Specimens in multistep hot torsion tests undergo multiple
deformations, leading to refined grains and a higher likelihood of strain-induced
precipitation. In comparison, each specimen in a double-hit deformation test has
TABLE 2
Comparison of TNR determination through double-hit compression and multistep hot torsion.
Material Identification Double-Hit ( C) Torsion ( C) DT ( C)

Lo-Nb 953 931 22
Hi-Nb 1000 960 40
Lo-V 995 953 42
Hi-V 1025 954 71
Lo-Ti 981 959 22
Hi-Ti 1026 994 32

FIG. 10
Comparison of the
experimental TNR for multistep
hot torsion tests and double-hit
deformation tests. The strain
and strain rate for each test
was 0.2 and 5 s1, respectively.
a long hold at high temperatures, generating larger austenite grains. Any

strain-induced precipitation would only occur in the temperature regime for
strain-induced precipitates, and not in every sample. The increased grain boundary
area in the torsion tests provides more nucleation sites for recrystallization at lower
temperatures; thus driving TNR to lower values. Other considerations include the
temperature for the double-hit deformation tests were controlled using type-K ther-
mocouples, while a dual-frequency pyrometer was used for the hot torsion tests.
There is some evidence in the literature to suggest a “break-down” of the type-K
thermocouples at high temperatures for long holds [29]. It is not believed to be the
main contributing factor in the weak trend between hot torsion and double-hit sim-
ulations. Other possibilities may be due to inconsistencies in test setup, such as
ensuring isothermal tests, use of nickel-paste, tantalum foil, and grafoil to provide a
barrier to carbon diffusion from the tungsten carbide platens and test sample,
extended period of time necessary to run the tests, extending over weeks, resulting
in various opportunities for inconsistencies.
The thermocouples used in the double-hit deformation tests have an uncertainty
of 65 C. Additional uncertainty can be attributed to the analysis methodology. The
pyrometer used in the multistep hot-torsion tests also has an uncertainty of 65 C.
Since a more direct method was used to determine TNR for the torsion test, being
able to determine TNR from a single test, not multiple tests, the uncertainty of the
test is less than that of the double-hit deformation study. The average difference of
calculated TNR values of the multistep hot torsion tests for a given alloy is 2 C, while
double-hit deformation tests have a difference of about 15 C. The variation in TNR
range may be attributed to the analysis method of the two testing procedures. The
double-hit tests were analyzed following the 5 % true strain method to determine
fraction softening. This method required an extrapolated power function line of the

first stress-strain curve as well as the stress value at 5 % true-strain for both curves.
The hot torsion tests were analyzed by determining the mean flow stress. The area
under each stress-strain curve was determined and normalized by dividing the stress
by the amount of strain per pass. The total stress per pass normalized by pass strain
appears to lead to a more robust analysis procedure.
Conclusions
An overview of various physical simulation methods for determining the no-
recrystallization temperature, TNR, was described, focusing on comparing results
from double hit deformation and multistep hot torsion tests to simulate a hot rolling
process. The double hit deformation tests result in higher values for TNR than those
measured from multistep hot torsion testing. The difference is primarily due to the
different grain sizes since multistep hot torsion testing undergoes multiple deforma-
tion passes prior to and after TNR, where double hit deformation tests undergo
deformation at a single temperature after a reheat and cool cycle. The smaller grains
in multistep hot torsion tests lead to more nucleation sites for recrystallization, and
thus a lower TNR.
ACKNOWLEDGMENTS
The writers would like to thank the Colorado School of Mines for supporting this
research through the Advanced Steel Processing and Products Research Center.
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Materials Performance and

doi:10.1520/MPC20150002 Vol. 4 No. 3 / 0000 / available online at www.astm.org

C. N. Homsher1 and C. J. Van Tyne1

Comparison of Two Physical

Materials Performance and Characterization

DOUBLE HIT DEFORMATION TESTING

Figure 1 shows a temperature-time schematic of the double-hit deformation test.

Materials Performance and Characterization

MULTISTEP HOT TORSION TESTING

Materials Performance and Characterization

• Deform with-e ¼ 0.2, e_ ¼ 5 s1

Figure 3shows temperature-time schematic for multistep hot torsion tests.

Materials Performance and Characterization

where h is the angle of twist (radians), and

Materials Performance and Characterization

Results and Discussion

Materials Performance and Characterization

Materials Performance and Characterization

MULTISTEP HOT TORSION TESTING

Materials Performance and Characterization

COMPARING THE TWO TESTING SIMULATIONS

Material Identification Double-Hit ( C) Torsion ( C) DT ( C)

Materials Performance and Characterization

a long hold at high temperatures, generating larger austenite grains. Any

Materials Performance and Characterization

Materials Performance and Characterization

Materials Performance and Characterization

Materials Performance and Characterization

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