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To cite this article: D. T. Gawne & G. M. H. Lewis (1985) Strengthening mechanisms in high-
strength microalloyed steels, Materials Science and Technology, 1:3, 183-191, DOI: 10.1179/
mst.1985.1.3.183
Article views: 26
Grain
intercept
Composition, wt-% length,
C Si Mn P S Ni AI(sol.) Cu N Nb Sn Ti V Ilm
Mean 0·085 0·051 0'59 0·025 0·017 0·017 0·014 0·020 0·0050 0,072 0·006 0,107 0·103 7·4
Min. 0·046 <0·01 0·25 <0·01 0·008 <0·01 <0·01 <0·01 0·0015 0·018 0·005 0·016 0·011 3·3
Max. 0·220 1·050 1·40 0·287 0·033 0·045 0·063 0·065 0·0256 0·220 0·013 0·197 0·240 13·8
cold rolled and annealed in the laboratory or laboratory where (Jo is the lattice friction stress and (Js, (Jp, (Jg, and (Jf.
vacuum melted, then fully processed to annealed sheet in are the respective strength increments produced by solid-
the laboratory. The works hot-rolled steels were slab solution hardening, precipitate particles, grain boundaries,
. reheated at 1250°C, finished at 900°C, spray cooled, and and dislocations .
coiled at 580°C at a gauge of 2 mm. The laboratory-melted
steels were given a simulation of works hot rolling: Solid-solution hardening
reheating, finishing, and coiling temperatures as above, The effect of phosphorus, nitrogen, manganese, silicon,
spray cooled at 50 K s- 1 on a run-out table with carbon, and grain size on the strength of a series of
motorized rollers, and cooled from 580°C at 0·4 K s- 1. All rephosphorized, nitrogenized, silicon, carbon-manganese,
the hot-rolled steels were cold rolled by 60% to a final and rimmed steels (batch and continuously annealed) was
thickness of 0·8 mm on a laboratory mill, using lubrication examined. The carbon was mostly in the form of cementite
and heavy reductions per pass. Simulated batch annealing particles, which produce strengthening by precipitation
was carried out under an argon atmosphere to soaking hardening and grain refinement. The following equations
temperatures of 660-700°C, using a heating rate of for the nominal yield strength (Jy (MN m - 2) and nominal
O·5 K s - 1 and cooling from 700 to 150°C in 48 h. tensile strength (Jt (MN m - 2), in terms of steel composition
Simulated continuous-annealing treatments were applied and grain size, were obtained from a statistical analysis of
to selected samples with a radiant furnace, using a heating the data:
rate of 12 K s -1 to soaking temperatures between 715
and 800°C, soaking for 3 min, cooling at 12 K s- 1 to (Jy = 27 + 22d-1/2 + 165 x %C +470 x %P
350°C, holding for 5 min, and cooling at 12 K s -1 to room +3000 x %N +60x %Si-665 x %S . (3)
temperature. (Jt = 150+ 16d-1/2+355 x %C+600 x %P
Tensile testing was carried out in an Instron machine, +4505 x %N + 77 x %Si-845 x %S . (4)
using a crosshead speed of 40 Jlm s - 1, with specimens, of
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gauge length and width 50 and 12·5 mm, respectively. The where d represents the grain intercept length (mm) and the
tensile specimens were cut at 0°, 45°, and 90° to the strip element concentrations are in weight per cent. Equations
Tolling direction, and average properties P were obtained (3) and (4) both explained 91% of the observed variations.
using the equation: More approximate equations can be derived from the
P = !(PO+2P4S+P90) . . . . . . . . . . (1)
results when the grain-size data are omitted from the
analysis. Such equations are useful in practice for a
where the subscripts refer to the angles between the specified process route, when the grain size is unknown and
direction in which the testpiece was cut and the rolling predictions of the total strengthening effects of the elements
direction. are required. The total strengthening effect obtained from
Grain sizes were measured on through-thickness sections these equations is the strength increment produced by any
parallel to the rolling direction by the linear intercept grain-refining action of the element, in addition to its
method, using light microscopy. Transmission electron solution-hardening contribution - and its precipitation-
microscopy was carried out on a Philips 300 instrument. hardening effect in the case of carbon. The equations
The precipitates were extracted on carbon replicas from depend upon the composition of a steel controlling the
mid-thickness sections parallel to the rolling plane. grain size, and this can only hold for a fixed process
route, since process variables can alter the grain size
independently. The following equations give the strength of
the steels batch annealed at temperatures between 660 and
Results and discussion 700°C, in terms of composition only:
(Jy = 246+512 x %C+540 x %P+3935 x %N
STRENGTHENING MECHANISMS + 68 x %Si- 2174 x %S . . . . .. (5)
Each steel is strengthened by a combination of different
mechanisms. The results presented later in this paper (Jt = 292+563 x %C+678 x %P+5183 x %N
(Fig. 6), for example, show that a cold-worked mild steel +90 x %Si+ 18 x %Mn-1534 x %S.. (6)
with a tensile strength of 500 MN m - 2 relies upon
180 MN m -2 from cold-work strengthening and the Equations (5) and (6) explain 72% and 83% of the observed
remaining base level of 320 MN m - 2 from lattice friction, variation, respectively. As indicated above, the concen-
solid-solution hardening, grain boundaries, and particle trations of the elements affect the grain size, and this effect
dispersions. Nevertheless, the dominant structure-sensitive changes the values of the strengthening coefficients in
mechanism in this case is cold work. Similarly, the other equations (5) and (6), relative to those in equations (3)
and (4).
materials will possess one dominant mechanism
responsible for generating the strength increment above the The results of the current work and those reported in the
base level, and this forms the basis of the classification literature on the strengthening effects of alloying elements
system used here. Accordingly, the solid-solution-hardened in steel are summarized in Table 2. Differences in
processing conditions are probably the major cause of the
materials consist of the rephosphorized, nitrogenized,
manganese, and silicon steels; the precipitation-hardened differences between the various sets of data. For example,
materials of the titanium, niobium, and vanadium steels; Wilson 17 found ,that the cooling rate has a pronounced
the grain-refined materials of the carbon-manganese steels; effect on ky in a low-carbon steel annealed at 700°C.
the partially annealed materials of the titanium, niobium, Cooling slowly from the annealing temperature to allow
and vanadium steels annealed below their recrystallization the carbon to segregate to the grain boundaries gave
ky = 23 MN m-2 mm1/2, whereas quenching resulted in a
temperatures; and the cold-worked materials of the
as-cold-rolled aluminium-killed mild steel rolled by various value of ky that was only 10 MN m-2 mm1/2• Wilson
amounts up to 70% reduction. In practice, each material is interpreted his results on the basis of Li's theory18 that
strengthened by more than one mechanism, but, to a first yield is controlled by the ability to propagate dislocations
approximation, the strengthening mechanisms may be from grain boundaries: increasing the impurity content
considered to be additive, such that the yield strength (Jy is (especially carbon) at grain boundaries stabilizes grain
given by: boundary ledges, which act as dislocation donors, and
thereby raises kyo The values of ky for the batch-annealed
(2) steels in Table 2 (19·5,22, and 23 MN m-2 mm1/2) cover a
higher range than those of the hot-rolled steels (15'4, 18'1, rephosphorized steels lies in their relatively high ductilities
and 21·6 MN m-2 mm1/2). This may also be due to Li's at high strength levels.22 However, excessively high
mechanism, since the cooling rate of batch-annealed steels phosphorus contents can be detrimental to product
is usually lower than that of hot-rolled coil, owing to the properties: in particular, contents above 0'1-0'2%, the
high thermal mass of the annealing furnace and the close precise limit depending upon the application, are
proximity of the coils. In the current work, for instance, the undesirable because of their effect on weldability23 and
average cooling rate for the batch-annealed steel was brittleness. 13, 24 Studies of spot weldability in the
0·18 K s -1, while the hot-rolled steel experienced 50 K S-1 automotive industry, for example, indicated a maximum of
down to 580°C and 0·4 K s - 1 thereafter. The annealing 0'16% for the combined phosphorus and carbon contents.2
temperature, carbide distribution, alloying element concen- There is thus a limit to the use of phosphorus as a
trations, interactions between elements, grain structure, strengthening agent, but additions below the particular
etc., are also expected to influence the segregation of product ceiling represent an attractive method of raising
carbon and other elements to grain boundaries, hence the yield strength by up to 50-100 MN m-2•
causing variations in the mechanical-property parameters. Nitrogen appears to be the most potent strengthener of
Carbon has a strong grain-refining action, since all the elements investigated (Table 2) and also produces
cementite particles nucleate recrystallized grains19,2o and steels with good formability in the as-annealed condition.22
pin grain boundaries. As a result, the strength coefficients Further increases in strength are obtained by strain aging
for carbon vary markedly, depending upon whether or not after temper rolling and press forming. However, there are
the grain size is omitted from the regression analysis, e.g. certain reservations regarding the use of nitrogen. First,
the coefficient increases from 165 in equation (3) to 512 in variable recoveries in steelmaking and nitrogen losses
equation (5) (see also Table 2). The carbon content in sheet during subsequent processing can result in inconsistent
steel for the automotive industry is normally limited by nitrogen contents in the finished product. An associated
weldability requirements13,21 to a maximum of ",0'12%. problem is the difficulty in maintaining high nitrogen
In practice, this allows increases in carbon content of up to contents, although this can be alleviated in part by
0'05% over existing extra-deep-drawing (EDD) steel, which, additional care in process control, e.g. batch-annealing
on the basis of Table 2, will generate increases in yield temperatures should be kept below about 650°C. Second,
strength of up to '" 25 MN m - 2. The strengthening the strain-aging process can bring disadvantages. The
available from increasing the carbon content, therefore, is strain in a pressed part can vary markedly with position,
relatively small. and so, therefore, will the strengthening produced by strain
The results in Table 2 show that phosphorus is an aging. In addition, strain aging increases the yield strength
effective strengthening agent in steel, the addition of 1%P much more than the tensile strength, thus producing a
raising the yield strength by '" 500 MN m - 2. The pronounced rise in the yield-strengthjtensile-strength ratio.
relationship between the tensile strength of the hot-rolled In adverse circumstances, these factors seem likely to
coil and that of the corresponding annealed sheet for the weaken the resistance of a finished component to collapse.
solution-hardened steels is shown in Fig. 1; the equivalent Silicon and manganese are both shown to be relatively
plots for the precipitation-hardened, grain-refined, and weak strengthening elements (Table 2). They appear to be
partially annealed steels are shown in Fig. 2. The results more effective in hot-rolled steel,8, 11, 12 possibly because of
show that phosphorus, along with the other solid-solution their influence on the austenite-ferrite phase trans-
hardeners, produces· little loss of strength on processing formation during hot rolling and the resulting grain
from hot-rolled coil to annealed sheet, compared with the structure and carbide morphology. Large concentrations of
alloying additions to the precipitation-hardened and grain- silicon and manganese are necessary to generate relatively
refined steels. This effect provides rephosphorized steels small strength increases, and so these elements are not
with a major advantage over the other steel types, since attractive strengthening options in sub-critically annealed
lower rolling-mill loads are required to produce an steels.
annealed steel of a given strength. As may also be seen The effect of sulphur is striking, as it is the only element
from Figs. 1 and 2, continuous annealing is particularly that reduces the strength of annealed steel; a similar effect
efficient in this respect, because its short annealing cycle has been observed by Gladman et al.8 in hot-rolled steels
gives rises to a fine grain structure. A further advantage of (Table 2). There is a large stoichiometric excess of
N
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1-- /
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z
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a:i 400 ANNEALED
a:
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(j)
W
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Ci5 300
z /
W
I-
/
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manganese over sulphur in all the steels, in order to avoid hardening. However, Table 2 indicates that manganese in
hot shortness, and so any increase in sulphur content solution has little significant influence on strength, and so
produces a decrease in the amount of manganese in this is unlikely to explain the effect. There is some
solution and a corresponding reduction in solid-solution indication from that data that increasing the sulphur
800
/
/
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IE 700
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z
2: /
t-='
w /
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(f)
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z
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t- 400
(!)
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(f)
BA = BATCH ANNEALED
W 300
....J / CA = CONTINUOUSLY ANNEALED
CI5 Ti-BA
Z
W / PA = PARTIALLY ANNEALED
t-
Precipitation hardening
Titanium, niobium, and vanadium were used singly and in
combination as precipitation-hardening elements. Titanium
forms coarse dispersions of a nitride and a carbo sulphide,
together with a fine carbide dispersion - the volume
fraction of the latter may be estimated from the data of
Meyer et a1.25 Niobium and vanadium form fine
precipitate dispersions of carbonitrides, the compositions
and volume fractions of which may be estimated from the
data of Meyer,26-28 Mandry and Dornelas,29 and Hudd
et al.30 Examples of the precipitate dispersions in these
steels are shown in Fig. 3.
An experimental value of the precipitation-hardening b
component may be obtained from equations (2) and (3).
Equation (2) can be rearranged to give:
(J"p = (J"y-(J"o-(J"s-(J"g-(J"e • • • • (7)
and equating equations (2) and (3) provides:
(J"o = 27
(J"s = 165 x %C+470 x %P+3000 x %N +60 x %Si
-665 x %S
(J"g = 22d-1/2
The steels under consideration were fully recrystallized, and
so the value of the dislocation-hardening component is
practically zero:
(J"e=O
C\l
I
E
z
2:
~ 0
I- pptdia.,A
z
UJ
100
20
Z
30
0 40
0-
:E 50
0 75
u
100
0
Z
-
Z
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UJ
I 250
I-
0
Z
UJ 500
a:::
I-
t/) 10
I 750
Z 1000
a
I-
4:
I-
~
u 2500
UJ
a:::
0-
5000
a
0·0001 0·001 0·01
This agreement is similar to that found by other workers significantly increased the strength of the hot-rolled
for hot-rolled steels.33,34 In addition, strengthening is product, in accordance with this mechanism.
shown to depend only on the volume fraction and diameter The precipitation and grain-refinement contributions
of the precipitates - providing they are non-deforming - vary throughout processing. In the as-hot-rolled
and is not influenced by their chemical composition (i.e. laboratory-melted titanium steels, for instance, the
whether they are titanium carbide or niobium or vanadium precipitates contributed '" 130 MN m - 2 and the grain
carbonitride) nor by whether the alloying elements are structure 200 MN m - 2 to a measured yield strength of
added singly or in combination. For example, the use of 410 MN m-2• In the batch-annealed condition, however,
titanium or vanadium in conjunction with niobium gave the precipitation-hardening component fell to 60 MN m - 2,
no noticeable advantage in terms of strength over that owing to particle coarsening, whereas that of the grain
expected from the equivalent extra addition of niobium in structure remained at 200 MN m - 2, for a measured yield
a plain niobium steel. It is pointed out, however, that strength of 360 MN m - 2. It is noted that, although the
multiple microalloying additions may make a useful precipitation-hardening component may be less than that
contribution to high-strength steels for other reasons. For of the grain structure, the precipitates exert a crucial,
instance, niobium carbonitride has a relatively low indirect effect on strength through their refinement of the
solubility in iron and requires high solution temperatures. grain structure.
The concentration of niobium taken into solution, and thus The relationship between the strength of the hot-rolled
the resulting volume fraction of fine niobium carbonitride steel and that of the subsequent annealed sheet is shown in
precipitates and the consequent strengthening contribu- Fig. 2. The batch-annealed titanium, niobium, and carbon-
tion, are, therefore, limited by commercial slab-reheating manganese steels show similar behaviour, but the
temperatures. Irvine35 proposed that this limitation could batch-annealed vanadium steels exhibit substantially lower
be overcome by the use of more than one precipitating strengths in the annealed condition for a given hot-rolled
element, since this would lead to .a greater total steel strength. This is directly related to the fact that
concentration of dissolved elements being available for vanadium carbonitride precipitates coarsened much more
precipitation than if only one had been used. His results quickly than titanium· carbide or niobium carbonitride
showed that the addition of vanadium to niobium steels precipitates. The strength of vanadium steels falls relatively
/
/ •
N
'I
E200 /
Z
2:
..-...
/
u
rou /
bci"
"-" 150
Z
o
•....
::l o
co 00 /
~•....
z
•
/
8 100
• o •
o
w
•....
o 0/ •.
4: A AD. /0
...J
::l A ./. A
~ o • •
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4:
u
50
~.h. • - Ti
o - Nb
Steels
Steels
/ A - V Steels
/
o 50 100 150 200 250
rapidly, therefore, -as processing proceeds. Hence, whereas of secondary recrystallization. The final recrystallized grain
satisfactory strength levels may be maintained in hot-rolled size is, therefore, expected to be a multiple of the
steels after coiling at low temperatures (e.g. 580°C), the dislocation cell size. The cell size in low-carbon steel cold
strength after prolonged batch annealing is low. The rolled by about 60% varies with crystallographic orienta-
practical implication of this is that vanadium is a relatively tion,36 but is normally in the range 0·5-2'0 /lm within the
inefficient strengthening agent for high-strength annealed matrix and ",0,2 Jlm within microbands.37,38 The smallest
steels; a relatively high hot-rolled steel strength, which grain size observed in the steels under investigation was
incurs high rolling-mill loads, is required for a given just over 3 /lm (Table 1) and, in view of the above
strength level in the annealed condition. mechanism of grain structure formation, this is likely to be
The production hot-rolled titanium and niobium steels close to the minimum grain size possible in these materials.
were stronger, by '" 50 MN m - 2, than their laboratory- Equations (3) and (4) indicate, therefore, that the maximum
melted counterparts. Their high strength levels are yield and tensile strengths achievable by grain refinement
attributed mainly to their higher manganese contents alone in these materials are '" 450 and '" 500 MN m - 2,
('" 1%, compared with 0'3%). Precipitation in titanium and respectively.
niobium steels is likely to occur mainly during the
austenite-ferrite transformation during· hot rolling. High
manganese contents lower the transformation temperature, EFFECT OF TEMPER ROLLING ON
and thus the precipitation temperature, which is expected PROPERTIES
to result in a finer precipitate dispersion and a higher The materials in the current investigation were tested in the
strength.33 Thus, although manganese alone is a relatively as-annealed condition, whereas commercial steels are
ineffective strengthening agent, it appears to have a usually temper rolled by about 1% for reasons of strip
synergistic effect in combination with titanium or niobium. shape and surface texture, and to avoid stretcher-strain
markings in pressed parts. A limited evaluation on the
Grain refinement effect of temper reduction on properties was carried out in
The relative importance of the grain-refinement component the laboratory.
of the strength is greatest in the carbon-manganese steels, After temper rolling by 1% on a laboratory mill, the
because of their relatively low precipitation-hardening (a yield strength of five nitrogenized steels (as-annealed yield
result of the coarse cementite particles - 0'6 Jlm dia.) and strength 280 MN m - 2) fell by 50-75 MN m - 2, the fall for
solution-hardening contributions. The cementite particles four rephosphorized steels (as-annealed yield strength
do, however, exert a major, indirect influence on strength, 300 MN m - 2) was 40-65 MN m - 2, and that for a titanium
through their grain-refining action, and so carbon content steel (as-annealed yield strength 400 MN m - 2) was
is still an important control variable. 65 MN m - 2. The corresponding fall in n for these steels
The grain structure develops initially by recrystalliza- varied from 0·020 to 0·055. In principle, the property
tion, which involves the growth of dislocation cells in the changes on temper rolling are expected to be influenced by
deformation substructure by a mechanism similar to that factors such as interstitial content, work-hardening rate,
and grain size, but no significant differences were detected relatively weak hot-rolled steel with minimal alloying
between the steels examined. On average, therefore, the additions (Figs. 1 and 2).
yield strength of high-strength cold-rolled steels falls by Solid-solution-hardening elements are useflil strength-
60 MN m - 2 and n by 0·035 on temper rolling by 1%. In
1"0.1 ening agents up to tensile strengths of 400-450 MN m - 2,
comparison, an aluminium-killed EDD mild steel (as- since they minimize rolling-mill loads, maximize duc-
annealed yield strength 225 MN m - 2) exhibited a fall in tility,22 and, unlike precipitation hardeners, are relatively
yield strength of 50 MN m - 2 and in n of
1"0.1 0·03 on 1"0.1 insensitive to variations in slab-reheating temper-
temper rolling by 1%. ature. The last factor could become significant with the
trend towards fast hot mills with lower slab-reheating
temperatures. Nevertheless, tensile strengths of above
COMPARISON OF STRENGTHENING 400-450 MN m - 2 require unacceptably high alloying
METHODS concentrations, in terms of weldability and impact
Figure 6 is a composite diagram plotted from the data properties. Stronger materials can be made by a
obtained, in which the effect of the principal mechanisms combination of strengthening modes, depending upon the
on the strengths of batch-annealed steels is shown. The application. When maximum ductility is required at a high
curve for cold work refers to a low-carbon mild steel. strength level, for instance, solid-solution hardening may
Vanadium is ineffective as a strengthening agent, because be combined with precipitation hardening. Conversely, a
of the rapid coarsening rate of vanadium carbonitride combination of precipitation hardening and cold work is a
precipitates. Vanadium also incurs the disadvantage that relatively inexpensive strengthening mechanism for very-
high strength levels in the hot-rolled condition, and hence high-strength, low-ductility applications.
high rolling-mill loads, are required for moderate strengths The microstructure necessary for the operation of each
in the annealed sheet (Fig. 2). The titanium, niobium, and mechanism can be obtained by suitable control of
carbon-manganese steels are more efficient in this respect composition and processing. There are numerous combin-
(Fig. 2), while the solution-hardened steels are the most ations of methods to achieve a given strength level.
Downloaded by [Universite Laval] at 04:13 09 April 2016
attractive, as they lose little strength on processing from The choice of production route will depend upon the
the hot rolled to the annealed condition (Fig. 1). intended product application and required material
Continuous annealing minimizes precipitate and grain properties, tonnages, availability of equipment, production
coarsening, and offers distinct advantages over batch costs, and compatibility. Production compatibility is of
annealing for high-strength steel production, since a given major importance in defining a process route for a new
strength in the annealed sheet can be derived from a product in existing steelworks. The manufacture of the
Cold
Work ./p
500
/
Nb
/
Ti
/.
//
450 /.
//
')I /.
//
E //
z /.
2: ~
/.
I
I- 400 ~.
~ /C
0
z /
UJ
0:::
l-
V) :I
~. Si /
UJ
-oJ
/ V
350
V)
Z
W
I-
300
10 20 30
COLD REDUCTION 1 °10
2 3
Mn,Si
0-10 0·20 0·30
Nb,Ti, V) P, N, C
CONCENTRATION OF ALLOYING ELEMENT,wt-olo
6 Effect of alloying elements and cold reduction on tensile strength of steel (cold reduced 600/0,batch annealed at
700°C for 20 h); cold-work curve is for low-carbon mild steel