The continuously annealed low-carbon-steel strips from industrial production showed an average

aging index of about 30 N/mm². This increase in yield strength caused by the continuous-annealing
process was strongly dependent on the soaking temperature and the soaking time. Whilst the
optimization of the overaging parameters and the use of a higher annealing temperature would reduce
the ageing susceptibility of low-carbon-steel strips, it was considered unlikely that its magnitude could
be reduced to a comparable level to that of the batch-annealed one. Within the limit of low-carbon-
strip specifications, there was very little effect of the C content on the ageing. The aging index of the
temper-rolled materials decreased with the increase in the temper-rolling reductions, and a maximum
increase in yield strength was achieved at a temper-rolling reduction of about 1%. In this work, the
effect of C content, Al content, continuous-annealing cycles, and temper-rolling reduction on the
ageing susceptibility of the continuously annealed low-carbon-steel strips was examined. SEM/EBSD
technique was developed to characterize the temper-rolling strain bands and to assess the effect of
temper-rolling reduction on the yield strength of the low-carbon-steel strips.

1. Introduction
The development of continuous-annealing (CA) technology for steel strips was first started in
1936 [1]. However, continuous-annealing technology did not become of great interest until the first oil
crisis in 1973. The basic metallurgical foundation for CA technology in low-carbon-steel strips is to use
low finishing temperatures and high coiling temperatures to achieve large ferrite-grain sizes for the hot
band and overaging to precipitate the carbon in solid solution [2]. The success of CA technology in
strip production has been attributed not only to its uniform mechanical properties and excellent
flatness but also to its very short processing time. During the short-time annealing cycle, favourable
textures for deep drawing and suitable grain sizes for formability are developed by recrystallization
and grain growth.
However, low-carbon-steel strips, particularly the commercial-quality grade (CQ), processed
through a continuous-annealing line, as opposed to batch-annealing, are often susceptible to ageing
due to the increased levels of interstitial C or N in solution. Ageing has an influence on the material
shelf life, while strain ageing will lead to stretcher-strain markings, which will affect the surface
appearance. The increased surface roughness would reduce the cohesion between the steel
substrate and coating. Significant ageing at elevated temperature, e.g., during paint-curing heat
treatment, could also lead to spring-back problems, resulting in the rejection of the products.
Ageing can be caused by the diffusion of the interstitials in solution, i.e., C and N, at elevated
temperatures or even at room temperature. Except for certain stabilized interstitial-free (IF) steels, CA
processed low-carbon-steel strips always exhibit a certain level of ageing. This is mainly due to the C
in solid solution, since N would be combined with Al after the high-temperature coiling during hot
rolling.
Temper rolling or skin passing is usually used as a means of suppressing the yield-point
elongation (YPE) in low-carbon-steel strips to prevent the formation of strain bands or Lüders bands
during subsequent processing. In addition, temper rolling is also used for shape correction and to
impart the required material properties, such as surface roughness.
There are many studies on the ageing characteristics of CA processed deep-drawing ultra-low-
carbon-steel strips [3] but very little work on commercial-quality low-carbon-steel strips. In this paper,
we study the effect of four variables, i.e., C, Al, CA cycles, and temper-rolling reductions, on the
ageing susceptibility of the CA commercial-quality low-carbon-steel strips.

2. Experimental Method
The low-carbon-steel sheets used in this work were CQ strips produced on an industrial CA line
with a nominal soaking temperature of 750 °C for 20 s and an overaging of 350 °C for 120 s. As the
materials are susceptible to natural ageing, samples received from the production line were stored in
refrigeration (<−25 °C) before any further treatments or tests. The first group of A samples with
variable carbon contents (from 0.015% to 0.05%) was selected with a nominal Al content of 0.039%
and a standard CA cycle, while Group 2 samples contained an increased Al of 0.072% for studying
the effect of Al content on ageing. In addition, Group 3 strip samples were collected from a CA cycle
with a soaking temperature of 725 °C to study the effect of the CA cycle on ageing. In addition,
laboratory temper rolling was carried out to achieve a range of temper-rolling reductions (0–4%).
All strip samples used in this work were cold rolled to a final thickness of 0.8 mm from hot bands
with a nominal coiling temperature of 650 °C. Table 1 lists all the samples with different variables.
Table 1. Nominal compositions of the CQ strip samples used in this work (all in weight percentage).

Samples of 350 mm × 90 mm were heat-treated at a laboratory CA simulator to simulate double-

annealing paint-curing cycles at 240 °C soaking for 30 s or at 225 °C soaking for 5 s (Figure 1). The
temperatures were controlled by thermocouples welded on the sample, while a constant cooling rate
of about 20 °C/s was achieved using compressed nitrogen.

Figure 1. Simulated paint-curing cycles.

The tensile properties were measured from at least four 50 mm gauge-length tensile specimens,
with a crosshead speed of 2.5 mm/min through the yield point and 50 mm/min for the remainder of the
test. The tensile tests showed good repeatability with overall experimental error within 10%. When a
sample showed no obvious yielding, the 0.2% proof strength (R p) was quoted, while, for the others,
the lower yield strength (ReL) was used. All tensile tests were conducted along the rolling direction on a
Zwick 1474 universal testing machine.
Aging index (AI) is used to study the ageing susceptibility of the low-carbon-steel strips. As
shown in Figure 2, AI is the difference between the flow stress at a specific pre-strain and the lower
yield stress after 100 °C/1 h artificial ageing in oil bath. The increase in yield stress after the pre-
straining and artificial ageing is the total hardening due to both ageing and the work hardening. The
purpose of the pre-strain is to remove the yield-point elongation; therefore, the amount of pre-strain
needs to exceed the yield-point elongation, varying between 2~10%. Throughout this work, a 2% pre-
strain was used for measuring the aging index.
Figure 2. Schematic diagram showing the aging index and the total hardening.
TEM carbon extraction replicas, prepared from the middle thickness of the strip samples, were
examined on Philips EM400T operated at 100 kV and the associated ISIS300EDA analytical facility to
study the distribution and the details of the carbide phases in the CA samples. The EBSD
measurements were carried out on the cross sections of the samples along the rolling direction on a
JOEL 9500 SEM with HKL system. The EBSD samples were prepared by electropolishing and
scanned for an area of approximately 0.9 mm × 0.5 mm at the middle thickness of the samples using
a step size of 1 µm.

3. Results
3.1. Effect of Carbon Content
Carbon is generally considered to be the main cause of ageing in low-carbon-steel strips, as
nitrogen would be combined with alloying elements, such as Al or B. Samples with various C contents
(0.016–0.05%) within the range of low-carbon CQ strip products were heat-treated with the two paint-
curing cycles. Tensile tests were carried out on both the as-received and the heat-treated samples.
The as-received CA samples showed less than 1% YPE. The average aging index between the
samples with different C contents was very similar, about 32 N/mm 2, though the CQ strips with lower
C contents showed higher total hardening than those with C contents at 0.037 or above (Table 2).
Table 2. Average tensile test results on samples with various C contents.
 Paint-curing treatment at 240 °C for 30 s resulted in an increase of about 60 N/mm² in yield
strength and an increase of about 4.3% in yield-point elongation. The effect of C contents on the
increase in yield strength and YPE was within test errors.
Samples with four different C contents were also heat-treated using a shorter annealing cycle of
225 °C/5 s. The increase in yield strength after the heat treatment was only about 34–43 N/mm². By
lowering the paint-curing temperature with a shorter soaking time, the average ageing obtained from
the CA low-carbon-steel strips was reduced by 30~45% (Figure 3). Though the amount of ageing
appeared to decrease slightly with the increase in C contents within the range of this study, the
variations were within the range of test errors, and the lines in Figure 3 were for guiding reference
only. The total C content in continuously annealed CQ strips had relatively small impact on the level of
ageing after paint-curing cycles, whereas the paint-curing cycles had a significant effect on age
hardening of the CA low-carbon-steel strips.

Figure 3. The effect of total C content on aging index and age hardening (The lines are for reference
only).
3.2. Effect of Aluminium Content
The contribution of solute nitrogen on ageing of low-carbon-steel strips is about twice that of
carbon in solution [4]. Therefore, it is important to remove all free nitrogen from solution in low-carbon-
steel strips. Al-killed low-carbon-steel strips for CA are usually coiled at a relatively high temperature
of about 650 °C to promote the formation of coarse AlN and carbides because fine AlN precipitates
will pin grain growth and affect the development of favourable texture for deep drawing during
continuous annealing.
Low-carbon CQ strips generally contain about 0.032% Al for deoxidization and the removal of
solute nitrogen. A CA low-carbon strip with double the amount of nominal Al content was selected for
tensile tests to study its ageing response. The as-received material showed a small YPE of less than
0.5%, likely due to room-temperature ageing. A simulated paint-curing treatment was carried out at
225 °C for 5 s, and the strip samples exhibited an average increase in yield strength of 28 N/mm² and
an increase in YPE of about 2.7%. As shown in Figure 4, the continuously annealed CQ strips with
0.072% Al showed a smaller ageing effect than that of the strip samples with standard Al content. The
tensile tests also revealed that the as-received samples with the increased Al content had lower yield
strength but similar ultimate tensile strength (UTS) compared to the standard CQ strips.
Figure 4. The effect of increased Al content on yield strength and UTS.
The increased Al content appeared to reduce the ageing tendency of the continuously annealed
CQ strips. Since the low-carbon CQ strips contained no boron, the solute nitrogen could only be
removed by Al. Although the standard CQ chemistry contains a sufficient amount of Al for deoxidation
and stabilizing solute nitrogen, the kinetics of forming AlN during hot-band cooling may prevent the
complete removal of nitrogen. As the Al content in the strips is further increased, it is expected that
the driving force for forming AlN during hot-band coiling is also increased. In fact, previous work [3]
indicated that an increase in Al content in non-B-bearing low-carbon-steel strips to more than 0.05% is
likely to fix more than 70% of the total nitrogen as AlN even if the hot bands are coiled at 650 °C.
3.3. Effect of CA Cycle
A typical CA cycle for low-carbon-steel strips consists of a short soaking treatment at >700 °C,
followed by rapid cooling, and then overaging at about 300 °C. During the soaking stage,
recrystallization and grain growth occur, and some of the iron carbides dissolve. Fine iron carbides
start to form during cooling and overaging, and their density depends on both the number of
nucleation sites and the degree of carbon supersaturation obtained through the rapid cooling. A CA
cycle for low-carbon-steel strips is usually designed in such way to promote the formation of fine
carbides and to minimize the carbon in solution.
Low-carbon CQ strip samples from two CA cycles with different soaking temperatures (i.e.,
Cycle 1: 750 °C/20 s and Cycle 2: 725 °C/20 s) were selected to study their ageing response. Tensile
tests of the as-received materials indicated that the strip processed with Cycle 1 had no yielding, while
the CQ strip processed with Cycle 2 exhibited a room-temperature ageing of 20 N/mm² after 15 days
compared to the test results of the CA production line. After a simulated paint-curing treatment at 240
°C for 30 s, the samples processed with CA Cycle 1 and Cycle 2 showed increases in yield strength of
63 N/mm² and 72 N/mm², respectively (Figure 5), while both samples had similar increases in YPE of
about 4.6%. Nevertheless, by pre-straining the as-received material to 2%, followed by the ageing
treatment, samples obtained from the two different CA cycles showed almost identical AI values of 30
N/mm² for Cycle 1 and 31 N/mm² for Cycle 2.
Figure 5. The effect of CA soaking temperature on tensile properties.
Although the sample with lower CA soaking temperature showed increased yield and tensile
strength, tests indicated that the aging indices of the strip samples remained the same with the two
CA soaking temperatures. This might be due to the relatively small differences between the two
soaking temperatures. In fact, earlier research indicated that the level of solute carbon in CA
processed low-carbon-steel strips was more sensitive to the cooling rate after soaking and the
overaging treatment than the soaking temperature [5]. However, a high soaking temperature will
increase the level of C supersaturation during fast cooling, which will promote the precipitation of fine
iron carbides and reduce the distance of carbon diffusion.
3.4. Effect of Temper-Rolling Reduction
Temper rolling can effectively remove YPE as well as control the flatness of the CA processed
low-carbon-steel strips. Temper rolling does not change the intrinsic properties of the material but
simply alters the response to further deformation. In this work, laboratory temper-rolling reductions of
0.5–4% have been carried out on a non-temper-rolled CA low-carbon CQ strip. The temper-rolled
samples were then subjected to the simulated paint-curing heat treatment at 240 °C for 30 s.
As shown in Figure 6a, the yield strength of the as-temper-rolled materials decreased first, then
increased with the increase in temper-rolling reduction. This was due to the dislocations introduced by
the initial small amount of temper rolling mainly pinning the interstitial atoms. Once the temper-rolling
reduction was sufficient to remove the YPE, further strain would result in work hardening, leading to
the increase in yield (or proof) strength. For the low-carbon strip samples used here, a temper-rolling
reduction of >1% was sufficient to remove the YPE (Figure 6b).
Figure 6. The effect of temper-rolling reduction on (a) yield (or proof) stress; (b) yield-point
elongation.
After a simulated paint-curing heat treatment at 240 °C/30 s, the temper-rolled samples showed
a gradual increase in yield strength and a decrease in YPE with the increase in the temper-rolling
reduction. However, the ageing hardening after the simulated paint-curing heat treatment increased
initially with the increase in temper-rolling reduction, reaching a maximum at about 1% temper rolling.
Further increase in the temper-rolling reductions led to the decrease in ageing (Figure 7). The aging-
index measurements of the as-temper-rolled samples showed that the AI values remained unchanged
at about 30 N/mm2 and decreased to about 20 N/mm² only when the temper-rolling reductions were
about 3%. Since the 2% pre-strain used for the aging-index measurements did not remove the yield-
point elongation of the non-temper-rolled sample, no aging index data were obtained for the non-
temper-rolled material.

Figure 7. The effect of temper-rolling reduction on ageing and aging index of low-carbon CQ strips.

4. Discussion
 Processes prior to continuous annealing, such as hot-band-coiling temperature, have a
significant influence on the properties of CA low-carbon-steel strips. The presence of fine AlN particles
in Al-killed low-carbon-steel strips will adversely affect the development of favourable texture for deep
drawing during CA. Therefore, the hot band of CA low-carbon-steel strips will be coiled at relatively
high temperatures (~710 °C) to achieve large ferrite grains with coarse carbides and AlN.
The coarse-carbide phases in CQ strips were partially dissolved during the high-temperature
soaking of a CA cycle, and the solute C was subsequently quenched in solid solution. The
supersaturated C then precipitated as iron carbide particles during overaging. TEM examination was
carried out using carbon extraction replicas, and the phase identification was primarily based on EDX
analysis. The CA samples contained many small iron carbide particles within the grains and many
large carbides mainly at grain boundaries, as shown in Figure 8. The large grain-boundary carbides,
often co-existing with MnS phases, are believed to be the undissolved carbide phases from the hot
band. In addition, small AlN particles were also observed.

Figure 8. TEM carbon-replica micrographs from a CA low-carbon CQ strip sample showing (a) small
carbides within grains and coarse carbides at grain boundaries; (b) co-precipitation of carbides with
MnS and AlN.
The complete reprecipitation of carbon is more difficult in CA low-carbon-steel strips due to the
short treatment time. As a result, the solute C and sometimes nitrogen will result in ageing. Nitrogen is
generally combined with Al to form coarse AlN at hot-band coiling, and sometimes a small amount of
boron (~30 ppm) will be added in low-carbon-steel strips to ensure the complete removal of solute
nitrogen. Therefore, solute C in low-carbon CQ strips is the dominant factor in ageing behaviour,
particularly at temperatures above 150 °C when the diffusion rate of carbon is significantly increased.
In this work, the simulated paint-curing double-annealing cycles were used rather than the typical
automotive paint-baking cycle (170 °C for 20 min). The relatively high annealing temperatures caused
a significant amount of ageing, likely due to the further precipitation (such as ε-carbides) on
dislocations and exiting particles [6]. A higher paint-curing annealing temperature with a longer
soaking time (i.e., 240 °C/30 s) generated more ageing than a gentle paint-curing cycle at 225 °C for
5 s.
This study on strip samples with a range of C contents showed that the average aging index of
the as-received CA low-carbon CQ strips was about 30 N/mm², with YPE varying from 0.2% to 0.9%,
where the variation in YPE was likely due to the variation in temper-rolling reduction. For continuously
annealed deep-drawing commercial-quality low-carbon-steel strips, a YPE of 0.2% or less is generally
accepted for non-ageing products, which do not develop stretcher-strains when press formed [7]. Test
results indicate that variation in the total C content in the CQ strips has very little impact on aging
index, which will be predominantly determined by the level of solute carbon. However, increasing Al
content to 0.072% slightly reduced the ageing tendency of the CA low-carbon-steel strips, which might
suggest that the increased Al content in the low-carbon-steel strips increased the tendency of forming
AlN, particularly in the hot band where the coiling temperature was at or below 650 °C [3]. Figure
9 shows the linear correlation of YPE with ageing after pain-curing treatments.
Figure 9. The relationship between aging index and YPE.
The percentage of temper-rolling reduction will determine the amount of strain in the strip, which
is important for ageing or strain ageing. Temper rolling introduces a pattern of localized residual
stresses. When the residual stresses reach certain levels, the yielding behaviour becomes continuous
so that no stretcher-strains are developed during subsequent processing. It is estimated that a 1%
temper-rolling reduction, which is typical for eliminating the yield point in low-carbon-steel strips, will
plastically deform approximately half of the material [3]. Temper-rolling reduction also has direct
influence on the yield strength of the low-carbon strip materials, and an optimum level of temper-
rolling reduction will result in a minimum increase in the yield strength.
In this work, the optimum level of temper-rolling reduction for the CA low-carbon CQ strips was
about 1–1.5%. Higher temper-rolling reduction than the optimum value would lead to work hardening
but reduce the strain-ageing effect due to the increased dislocation density, resulting in a large
incidence of dislocation entanglements and reducing the efficiency of carbon pinning [8].
The grain orientation spread of 0.5° was found to be the suitable value to differentiate the
localized strain bands from the surrounding matrix, as shown in Figure 10. The strain bands are
approximately 30~40° of the rolling direction, and the cross deformation bands increase with the
increase in temper-rolling reduction.
Figure 10. EBSD grain-orientation-spread maps (0–1.5°) showing the strain bands in temper-rolled
CA low-carbon strip with temper-rolling reductions (a) 0%; (b) 0.2%; (c) 0.4%; (d) 0.8%; (e) 1.6%; (f)
3%.
Using EBSD grain orientation spread, we can quantitatively calculate the percentage of areas
covered by the localized strain bands. As shown in Figure 11, the grain area of the strain bands
increases initially with the increase in the temper-rolling reduction and then levels off to approximately
43% after about a 1% temper-rolling reduction, which is in agreement with the conclusion that a 1%
temper-rolling reduction will have plastically deformed about half of the volume of the material [9].

Figure 11. EBSD measurements showing the relationship between the temper-rolling reduction and
the grain areas with orientation spread >0.5° (black rhombus as measured points).

5. Conclusions
The continuously annealed low-carbon CQ strips showed an average aging index of about 30
N/mm², which is regarded as acceptable in terms of room-temperature ageing. The increase in yield
strength after laboratory-simulated paint-curing treatment was due to the return of the YPE and real
ageing. In this work, the effect of C content, Al content, continuous-annealing soaking temperature,
and temper-rolling reduction on the ageing susceptibility of the CA low-carbon-steel strips was
examined. It is found that the ageing hardening of the CA low-carbon-steel strips increases linearly
with the increase in YPE after paint-curing treatments.
Within the low-carbon CQ strip specification, the total C content has little effect on ageing, as the
ageing response is primarily governed by the C in solution. Similarly, the soaking temperatures used
for the two CA cycles appear to have little effect on the aging index of the low-carbon CQ strips
because the solute C is more sensitive to the cooling rate after soaking and the overaging treatment.
On the other hand, doubling the Al content to 0.072% slightly reduced the ageing response of the low-
carbon-steel strips, which is expected to be more pronounced for CA low-carbon-steel strips with low
hot-band-coiling temperature.
The yield strength of the as-temper-rolled CA low-carbon-steel strips decreased first, then
started to increase with the increase in temper-rolling reduction, whereas the aging index remained
unchanged until the temper-rolling reduction was above 2%. The YPE was completely removed at 1%
or higher temper-rolling reduction. EBSD grain-orientation-spread mapping was used to analyse the
localized strain bands induced by temper rolling. The grain area of the strain band increased with the
increase in the temper-rolling reductions and reached about 43% at 1% temper-rolling reduction.
Even if the ageing response of the low-carbon CQ strips is substantially reduced by temper
rolling, a return of YPE will still be observed after paint-curing treatments, and the increase in yield
strength will at least reach the level exhibited before the temper rolling. The relatively small grain size
of CA low-carbon-steel strips will also result in a larger yield-point elongation in the as-annealed
condition and hence a larger increase in yield strength on the return of the yield point through paint-
curing treatment. Whilst optimizing the CA overaging parameters and using higher annealing
temperature to achieve coarse-grain size that may reduce the ageing susceptibility of the low-carbon
CQ strips, it is unlikely that its ageing can be reduced to a comparable level to that in batch-annealed
low-carbon-steel strips.

 The present invention relates to a method of producing a cold rolled steel sheet having good ageing
resistance and small anisotropy and adapted for deep drawing.

Cold rolled steel sheets, which are used for automotive exterior plates and the like, are generally
required to have deep drawability and good ageing resistance.

Among various properties of a steel sheet, the Lankford value, that is, the so-called r value, of the steel
sheet, has the highest influence upon its deep drawability. Further its elongation (EI) and the like have
a minor influence upon its deep drawability. When solute C and N are present in a steel sheet, the
problem known as stretcher strain is apt to occur during pressing due to ageing at room temperature,
and therefore steel sheets for press forming need to have a good ageing resistance.

There has been known a method of producing a non-ageing cold rolled steel sheet for deep drawing by
using low carbon aluminium killed steel. By this method, a high r value is obtained in the resulting cold
rolled steel sheet by the action of AIN precipitated as a consequence of the heating during box
annealing. At the same time N is precipitated and fixed by Al, and C is precipitated and fixed in the
form of Fe3C to give a non-ageing property to the resulting steel sheet. In another method of producing
a cold rolled steel sheet with a good ageing resistance, decarburization and denitrogenization are
carried out by open coil annealing.

Both the above described methods are carried out using a batch system, and therefore these methods
are inferior to continuous annealing methods from the point of view of productivity. Also the resultant
annealed steel sheets have poor homogeneity. Moreover, in these methods, a heat treatment is carried
out for a long period of time and therefore temper color is apt to develop on the surface of the steel
sheet due to the enrichment of Si, Mn and the like. Further, when decarburization or denitrogenization
is carried out, the decarburized or denitrogenized steel sheet exhibits cold-work embrittleness due to
the segregation of P in the grain boundaries during slow cooling.

The continuous annealing method is free from the drawbacks of the above described batch annealing
method. However, in the continuous annealing method, a cycle consisting of a rapid heating, a short
time soaking and a rapid cooling is carried out, and therefore when a low carbon steel is used, the
continuous annealing method cannot develop fully the crystal grains and is inferior to the batch method
in regard to the ductility and r value of the resulting steel sheet. Also it is more difficult to fix C and N
and to produce a non-ageing steel sheet than when using the batch method.

In order to obviate the above described drawbacks of the continuous annealing method, various
methods for producing a cold rolled steel sheet having satisfactory properties from an extra-low carbon
aluminium killed steel, even by a continuous annealing cycle, have been disclosed. Japanese Patent
Application Publication No. 17,490/76, Japanese Patent Laid-Open Application No. 58,333/80 and the
like disclose such methods.
However, these methods still have the following drawbacks.

o (A) It is difficult to produce a steel sheet having substantial non-ageing properties unless an
extra-low carbon aluminium killed steel having a C content of not higher than 20 ppm is used.
o (B) Even when using a steel having a C content as low as not higher than 20 ppm, the
resulting steel sheet still has a large planar anistropy in the r value, elongation and the like,
and thus gives rise to problems in practical use.

There are methods for producing steel sheets having excellent deep drawability and ageing resistance
and further having small anisotropy, wherein C and N contained in the steel are precipitated and fixed
by using powerful elements for forming carbides or nitrides, such as Ti, Nb and the like. The use of Ti
is disclosed in Japanese Patent Application Publication No. 12,348/67, and the use of Nb is disclosed in
Japanese Patent Application Publication No. 35,002/78. However, in these methods, when the steel
contains a large amount of C, the resulting steel sheet is poor in ductility due to the large amount of
precipitates; and reversely when the steel contains a small amount viz not more than 50 ppm of C, the
C cannot be fully precipitated and fixed unless Ti or the like is used in an amount considerably larger
than the stoichiometrically necessary amount for fixing the C. Therefore, unbonded excess Ti and the
like also deteriorate the ductility and adversely affect the formability of the resulting steel sheet.

Further, Japanese Patent Laid-Open Application No. 81,913/75 discloses a method of obtaining a steel
sheet having excellent properties wherein a very small amount of at least one of B, Nb, Zr, V and Ti is
added to a low-carbon aluminium killed steel having a C content of 0.05-0.07%, the steel is formed
into a steel sheet, the steel sheet is subjected to a recrystallization annealing, and the annealed steel
sheet is subjected to an overageing treatment at a temperature not lower than 300°C to precipitate the
major part of C contained in the steel. However, this method always requires a low carbon steel, and an
overageing treatment must be carried out in the continuous annealing.

Further, the inventors have already disclosed a cold rolled steel sheet having ultra-deep drawability,
which consists of an extra-low carbon aluminium killed steel having a C content of 0.004-0.006% and
an Nb content of 0.026-0.043%, and a method of producing the steel sheet in Japanese Patent Laid-
Open Application No. 169,752/81. They have further disclosed a high tensile strength steel sheet
having ultra-deep drawability, which consists of an extra-low carbon aluminium killed steel having a C
content of 0.005-0.009%, an Nb content of 0.027-0.043% and a P content of 0.062-0.082%, and a
method of producing the steel sheet in Japanese Patent Laid-Open Application No. 139,654/81.
However, the present invention is different from these Japanese Laid-open applications in the
following two points viz. (a) C:-50.004% and (b) Nb and other elements 20.01%.

The object of the present invention is to solve the above described drawbacks of the conventional
techniques and to provide a method of producing a cold rolled steel sheet having good ageing
resistance and small anisotropy and adapted for deep drawing.

EP-A1-24 437 discloses the production of cold rolled steel sheets having good ageing resistance and
deep drawability from a steel having a composition comprising, in % by weight, not more than 0.01 %
C, not more than 0.2% Si, from 0.05 to 0.40% Mn, not more than 0.02% P, not more than 0.02% S, not
more than 0.01 % N, acid soluble aluminium in an amount of at least 1.8 times the amount of nitrogen,
Nb in an amount such that log (Nb/C) is within the range of from 0.10 to 1.00, and optionally at least
one element selected from the group consisting of rare earth metals, Ca, B and Cu, the amount of rare
earth element, Ca or B being not more than 0.01 % and the amount of Cu being not more than 0.03%,
with the remainder of the composition being Fe and incidental impurities. The steel is formed into
sheets by hot rolling, cold rolling and annealing. However the annealing is carried out by box
annealing. Moreover there is no teaching as to the planar anisotropy of the sheets.

GB-A-1 176 863 also discloses the production of non-ageing cold rolled steel sheets suitable for deep
drawing. In this case, the steel has a composition comprising 0.001-0.020% C, less than 0.45% Mn,
less than 0.015% 0, and 0.02-0.5% Ti except Ti-oxides, said Ti content being more than 4 times the C
content, with the balance being Fe and unavoidable impurities. The sheets are produced from the steel
by hot rolling, cold rolling and annealing. The annealing may be effected by box annealing, open-coil
annealing or continuous annealing. There is no teaching as to the planar anisotropy of the sheets.
Disclosure of the invention

According to one aspect of the present invention there is provided a method of producing a cold rolled
steel sheet having good ageing resistance and adapted for deep drawing, by cold rolling a steel to form
a sheet and annealing the sheet wherein the steel has a composition consisting of, in % by weight, not
more than 0.004% of C, 0.03-0.30% of Mn, not more than 0.150% of P, not more than 0.020% of S,
not more than 0.007% of N, 0.005-0.150% of acid-soluble AI, and 0.002-0.010% in total of at least one
element selected from Nb, Ti, V, Zr and W, with the remainder being Fe and incidental impurities and
the annealing is effected by continuous annealing at a temperature within the range of 700-950°C
whereby the resultant sheet has small anisotropy.

According to a second aspect of the present invention there is provided a method of producing a cold
rolled steel sheet having good ageing resistance and adapted for deep drawing by cold rolling a steel to
form a sheet and annealing the sheet wherein the steel has a composition consisting of, in % by weight,
not more than 0.004% of C, 0.03-0.30% of Mn, not more than 0.150% of P, not more than 0.020% of
S, not more than 0.007% of N, 0.005-0.150% of acid-soluble Al, 0.002-0.010% in total of at least one
element selected from Nb, Ti, V, Zr and W, and not more than 0.0050% of B, with the remainder being
Fe and incidental impurities and the annealing is effected by continuous annealing at a temperature
within the range of 700-950°C whereby the resultant sheet has small anisotropy.

Thus, in accordance with the present invention, a cold rolled steel sheet having good ageing resistance
and small anisotropy and adapted for deep drawing is produced by a method wherein an aluminium
killed steel having a composition containing not more than 0.004% of C and a very small amount of
0.002-0.010% of a total amount of at least one element selected from Nb, Ti, V, Zr and W, and
optionally containing not more than 0.0050% of B is hot rolled and then cold rolled in a conventional
manner, and the cold rolled sheet is subjected to a continuous annealing at a temperature within the
range of 700-950°C.

An explanation will be made with respect to a basic experiment illustrating the present invention.
Steels having the compositions shown in the following Table 1 were produced by means of an LD
converter, and subjected to an RH degassing treatment and then to continuous casting to produce slabs.
Each slab was hot rolled at a finishing temperature of 870-910°C, and a coiling temperature of 660-
710°C, and the hot rolled sheet was cold rolled at a reduction rate of 75% in conventional manner to
produce a steel sheet having a thickness of 0.8 mm.
Each of the above obtained steel sheets was subjected to a continuous annealing line, wherein the steel
sheet was uniformly heated at a temperature of 800-820°C for about 40 seconds and then cooled
substantially linearly to about room temperature at a cooling rate of 20°C/sec; each of the above
annealed steel sheets was subjected to temper rolling at a reduction of 0.6% to produce a cold rolled
steel sheet. The sample steels were classified into two groups depending upon the C content, and the
relation between the properties, such as r, El, ageing index Al, Ar and ΔEI, of the resulting cold rolled
steel sheets and the Nb content of the steels was investigated. As a result, it was ascertained that the
desired object can be advantageously attained according to the present invention.

Brief description of the drawings

For a better understanding of the invention and to show how the same may be carried out reference will
now be made by way of example to the accompanying drawings, in which:

o Figs. 1 (A),-(B) and (C) and Figs. 2(A) and (B) illustrate the relationships between the Nb
content and r, El, ageing index Al, Ar and ΔEI, respectively, and
o Fig. 3 shows diagrammatically the heat cycles involved in a continuous annealing line and a
continuous hot-dip zinc plating line.

In Fig. 1 and Fig. 2, sample steels having a C content of 0.0009-0.0015% are indicated by the mark
"A", and sample steels having a C content of 0.0026-0.0033% are indicated by the mark "o".

The ageing index AI is indicated by the difference between the flow stress of a steel sheet causing 7.5%
of tensile pre-strain and the lower yield stress of the steel sheet when the steel sheet is subjected to a
tensile force in a direction along the rolling direction after the flow stress has been removed and the
steel sheet has been heat treated at 100°C for 30 minutes.

The definition of El, and r, and that of ΔEI, and Δr, which indicate the planar anisotropy of the EI and r
values respectively, are as follows.

In the above formulae, ro. and Elo. mean the r value and EI value respectively when the angle of the
direction of stress relative to the rolling direction is 0 degree.

It can be seen from Figs. 1(A) and 1(C) that the r value and the AI are remarkably improved
independently of the C content by the addition of a very small amount of at least 0.002% of Nb.
However, the addition of 0.012% or more of Nb deteriorates the EI value as illustrated in Fig. 1(B).
 In the case of steel No. 1 having a C content of 0.0010% and containing no Nb, the resulting cold rolled
steel sheet had a substantial non-ageing property having an AI of not more than 3 kgf/mm2, and further
it had high EI and r values, that is, it had the desired excellent properties. However, the steel sheet had
a very high planar anisotropy in the r and EI values. The inventors have found out that, when a very
small amount of Nb is added to the steel, the resulting cold rolled steel sheet has very small ΔEI and Ar
values, and has a very small anistropy.

Based on the discovery, the inventors have succeeded in the production of a cold rolled steel sheet
having high EI and r values and further having non-ageing properties and small anisotropy by adding
0.002-0.010% of Nb to an extra-low carbon aluminium killed steel.

The inventors have made a further investigation and found out that the above described phenomenon
occurs also even when at least one element selected from Ti, V, Zr and W alone or in admixture is
added to the steel in place of Nb. They have further found out that, when B is further added to the
above described steel containing at least one element of Nb, Ti, V, Zr and W, the ductility of the
resulting steel sheet is improved, that is, the addition of B to a steel is effective for improving the
properties of the resulting steel sheet.

 The reason why the addition of a very small amount of the above described elements, such as Nb and
the like, to aluminium killed steel having a very low content of C gives excellent properties to the
resulting cold rolled steel sheet, is not clear, but is probably as follows. It is firstly suspected that the
effect is caused by the precipitates of these elements because these elements are all carbide- and
nitride-forming elements. However, the amount in which these elements is added is small and
moreover the C content in the steel is very low. Therefore it is suspected that it is very difficult to
precipitate and fix completely C, and that the effect is caused by the solute state of Nb and the like.

An explanation will be made hereinafter with respect to the reason for the limitation of the components
constituting the steel of the present invention.

C: not more than 0.0040%

The C content in the steel must be not more than 0.0040% in order to obtain sufficiently high ductility,
r value and ageing resistance in the steel by the continuous annealing method. It is not, however
necessary to place a lower limit on the C content. Because the annealing used is continuous annealing
and the cooling rate is high, the phenomenon of embrittlement of the steel due to P does not occur to
any substantial extent.

Mn: 0.03-0.30%

The Mn content must be at least 0.03% in order to prevent the red shortness of the steel. However,
when the Mn content exceeds 0.30%, the development of {111} recrystallization texture is disturbed
and the deep drawability of the steel deteriorates. Therefore, the Mn content is limited to 0.03-0.30%.

P: not more than 0.150%

P has a high solid solution hardening ability, and can improve the tensile strength of steel in very small
amounts and hardly deteriorates the deep drawability of the steel. Therefore, P is a very effective
element for obtaining a high tensile strength steel sheet having deep drawability. However, when the P
content in the steel exceeds 0.150%, the spot weldability of the steel is poor. Therefore, the P content is
limited to not more than 0.150%.

S: not more than 0.020%

When the S content in the steel exceeds 0.020%, the steel has very poor ductility. Therefore, the S
content in the steel is limited to not more than 0.020%.

N: not more than 0.007%

 N forms a solid solution in the steel similarly to C and deteriorates the deep drawability, ageing
resistance and the like. Therefore, the N content is limited to not more than 0.007%.

Acid-soluble Al: 0.005-0.150%

 Acid-soluble AI must be contained in the steel in an amount of not less than 0.005% in order to remove
oxygen and to fix N. However, when more than 0.150% of acid-soluble AI is contained in the steel, the
steel has poor ductility, and inclusions in the steel increase. Therefore, the content of acid-soluble AI is
limited to 0.005-0.150%.

Nb, Ti, V, Zr and W: 0.002-0.010%

The addition of these elements to the steel is very important in the present invention. These elements
have the same action in that, when not less than 0.002% of a total amount of these elements is added to
an extra-low carbon aluminium killed steel, not only the deep drawability of the steel, but also the
ageing resistance of the steel can be improved and the planar anisotropy in the r value, elongation and
the like of the steel can be lowered. However, if the amount of these elements exceeds 0.010%, the
elongation of the steel deteriorates noticeably. Therefore, the content of these elements in the steel is
limited within the range of 0.002-0.010% in total.

The above described elements are used, in the amounts defined above, as basic elements in the cold
rolled steel sheet for deep drawing in accordance with the present invention. Further, when B is
additionally added to the cold rolled steel sheet, the object of the present invention can be attained
more effectively. The reason for the limitation of the amount of B is as follows.

B: not more than 0.005%

The addition of B alone to a steel deteriorates the deep drawability of the steel, and therefore B cannot
be used alone. However, when B is added to the steel together with the above described elements, such
as Nb and the like, the yield strength of the steel is decreased and the elongation is improved without
deteriorating the deep drawability of the steel, and the press formability of the steel is improved. B is
preferably used in an amount of not less than 0.0010%, but when the amount of B exceeds 0.0050%,
the effect of B is saturated. Therefore, the B content in the steel should be limited to not more than
0.0050%.

An explanation will be made hereinafter with respect to the production steps for the cold rolled steel
sheet having the above described composition and having deep drawability. The steel making method
is not particularly limited, but a combination system of converter method-degassing method is
effectively used in order to produce a molten steel having a low C content of not more than 0.0040%.
The molten steel can be formed into a slab by any ingot making-slabbing method or continuous casting
method. The hot rolling of the slab can be carried out by a hot strip mill under the commonly used
conditions. The finishing temperature is preferably not lower than 830°C, and the coiling temperature
is preferably within the range of 400-750°C in order to secure the shape of the steel sheet and facilitate
pickling.

The hot rolled steel strip is pickled and then subjected to cold rolling. A cold rolling reduction rate of at
least 50% is desirable in order to secure deep drawability in the resulting cold rolled steel sheet.

It is necessary that the continuous annealing of the cold rolled steel sheet is carried out at a temperature
not lower than 700°C. When the heating temperature is lower than 700°C, recrystallized grains cannot
be fully developed, and excellent workability cannot be obtained. While, when the heating temperature
exceeds 950°C, the ductility and drawability are noticeably deteriorated. Therefore, the heating
temperature at the continuous annealing is limited within the range of 700-950°C, but a heating
temperature within the range of 750―900°C is most preferable. The uniformly heating time in the
continuous annealing of the cold rolled steel sheet is not particularly limited, but is preferably from 10
to 180 seconds in order to achieve the desired properties and economical operation. The cooling
method after the annealing is not particularly limited, but a gradual cooling for the uniformly heating
temperature to about 700°C is effective for improving the ageing resistance. Further, cold-work
 embrittlement of the steel sheet can be easily prevented by the cooling method used in ordinary
continuous annealing. However, it is not preferred for the heating steel sheet to be gradually cooled at a
rate of 0.1°C/sec or less or for the heated steel sheet to be kept for 10 minutes or more at 700-300 0C.
Moreover, even when the steel of the present invention is subjected to an overageing treatment in a
continuous annealing line having an overageing zone, the properties of the steel are not substantially
changed. Therefore, it is not necessary to carry out an overageing treatment. It is not important in the
present invention whether or not an overageing treatment is carried out.

 [The annealed steel sheet of the present invention has an AI of not larger than 3 kgf/mm 2 and has a
good ageing resistance. However, the steel sheet sometimes has a small amount of elongation at the
yield point, and therefore the steel sheet can be additionally subjected to a temper rolling at a reduction
of not more than 2%.

According to the present invention, a cold rolled steel sheet having good ageing resistance and small
anisotropy and adapted for deep drawing is able to be produced by the above described treatment from
an extra-low carbon aluminium killed steel containing a very small amount of Nb and the like added
thereto.

Furthermore, the method of the present invention can be applied to the production of zinc-plated steel
sheet by a continuous hot-dip zinc plating line including an annealing step in the line. The uniform
heating condition and the cooling method down to about 500°C, the temperature of the zinc bath, are
the same as those described above, and the cooling after the plating can be carried out by any method
as desired. Further the zinc-plated steel sheet can be subjected to an alloying treatment. The following
example illustrates the invention:-

Example

Steels having the compositions shown in the following Table 2 were made into hot rolled steel sheets at
the hot rolling and coiling temperature shown in Table 2, and the hot rolled steel sheets were cold
rolled into cold rolled steel sheets. Each cold rolled steel sheet was subjected to a continuous annealing
line or a continuous hot-dip zinc plating line involving the heat cycles shown in Fig. 3. The following
Table 3 shows the tensile properties, ageing resistance and cold-work embrittlement of the above
treated steel sheets.
With each of the steel samples, a cold rolled steel sheet having excellent ageing resistance, deep
drawability, and small anisotropy could be obtained.

Zinc-plated cold rolled steel sheets of steel sample Nos. 3 and 6 could be obtained without difficulty in
the zinc-plating operation.
Steel sample No. 10 was a high tensile strength steel having a tensile strength of 35 kgf/mm 2 and the
resulting cold rolled steel sheet had excellent ageing resistance and deep drawability.

It can be seen from the above results that, according to the present invention, a cold rolled steel sheet
having good ageing resistance and small anisotropy and adapted for deep drawing can be produced by
adding a very small amount of Nb and other elements to an extra-low carbon steel and subjecting a
cold rolled steel sheet obtained from the steel to a continuous annealing at a temperature within the
range of 700-950°C.