TECHNICAL FIELD
[0001] The present invention relates to a cold-rolled steel sheet and a method of manufacturing
a cold-rolled steel sheet.
BACKGROUND ART
[0002] A steel sheet used in automobile parts, for example, is required to have high strength
and also good formability.
[0003] WO 2018/030502 A1 discloses a high-strength steel sheet having a tensile strength not lower than 980
MPa and good formability. This steel sheet contains predetermined amounts of Cr and
Mo, where the average grain size of the ferrite phase is not larger than 1.5 pm, the
area ratio of the ferrite phase is not lower than 2 % and not higher than 15 %, the
area ratio of the tempered martensite phase is not lower than 75 % and not higher
than 96 %, and, per unit area, the sum of the interface length between the untempered
martensite phase and the ferrite phase and the interface length between the untempered
martensite phase and the tempered martensite phase is not smaller than 6.3 × 10
8 µm/m
2 and not larger than 5.0 × 10
11 µm/m
2.
[0004] JP 2016-194139 A discloses a high-strength cold-rolled steel sheet with a tensile strength not lower
than 980 MPa and good formability as evaluated based on ductility and flange properties,
as well as good collisional properties. This steel sheet has a microstructure, as
seen at 1/4 of the sheet thickness, in which the area ratio of ferrite to the total
microstructure is higher than 10 % and not higher than 65 % when the microstructure
is observed by scanning electron microscopy, and the balance is a hard phase containing
quenched martensite and retained austenite and composed of at least one selected from
the group consisting of bainitic ferrite, bainite and tempered martensite.
[0005] JP 2015-193897 A discloses a high-strength cold-rolled steel sheet with a tensile strength not lower
than 980 MPa and good ductility and bendability. This steel sheet has a microstructure,
as seen at 1/4 of the sheet thickness of the steel sheet, in which the area ratio
of ferrite to the total microstructure is not lower than 5 % and lower than 50 % when
observed by scanning electron microscopy, and the balance is a hard phase. Furthermore,
when analyzed by an electron-beam microprobe analyzer, the regions with an Mn concentration
not lower than 1.2 times the Mn concentration in the steel sheet are present in 5
area % or more and, when for a 2 pm square section the fraction of regions with an
Mn concentration not lower than 1.2 times the Mn concentration in the steel sheet
is measured, the standard deviation of the measurements for 100 sections is not lower
than 4.0 %.
[0006] WO 2008/042982 A2 describes a method of processing an iron-based alloy, including the steps of: raising
the temperature of an iron-based alloy having a first microstructure capable of transforming
to a second microstructure to the austenite transformation temperature; rapidly heating
the iron-based alloy to a temperature higher than the austenite transformation temperature,
and immediately quenching at least a portion of the iron-based alloy using quenching
equipment adjacent to the heating equipment.
PRIOR ART DOCUMENTS
PATENT DOCUMENTS
SUMMARY OF THE INVENTION
PROBLEMS TO BE SOLVED BY THE INVENTION
[0008] A problem to be solved by the present invention is to provide a cold-rolled steel
sheet having high strength and good formability, and, more specifically, to provide
a cold-rolled steel sheet having high strength and good hole expandability.
MEANS FOR SOLVING THE PROBLEMS
[0009] A cold-rolled steel sheet according to one embodiment of the present invention has
a chemical composition of, in mass %: 0.10 to 0.30 % C; up to 2.50 % Si; 0.50 to 3.50
% Mn; up to 0.100 % P; up to 0.020 % S; 0.010 to 0.100 % Al; up to 0.0100 % N; 0 to
0.100 % Ti; 0 to 0.100 % Nb; 0 to 0.50 % V; 0 to 0.50 % Mo; 0 to 0.50 % W; 0 to 0.0050
% B; 0 to 0.0100 % Ca; 0 to 0.0100 % Mg; 0 to 0.0100 % REM; and balance Fe and impurities,
a microstructure containing tempered martensite and bainite in not less than 85 volume
% in total, a structure other than the tempered martensite, bainite and ferrite being
present in not more than 5 volume %, regions where an Mn concentration in the microstructure
is not lower than 8.0 mass % being present in 0.05 to 1.5 area %.
[0010] A method of manufacturing a cold-rolled steel sheet according to one embodiment of
the present invention is a method of manufacturing the above-described cold-rolled
steel sheet, including: performing a heat treatment by holding a hot-rolled steel
sheet in a temperature range from 620 to 700 °C for not shorter than 10 minutes; cold
rolling the heat-treated steel sheet; holding the cold-rolled steel sheet in a temperature
range from 880 to 1050 °C for not shorter than 10 seconds and then cooling the steel
sheet to a temperature not higher than 450 °C at a cooling rate not lower than 20
°C/s; and, after cooling the steel sheet to a temperature not higher than 450 °C in
the cooling step, performing one of the following sub-processes, (A) and (B):
- (A) a sub-process for cooling to a temperature not higher than 350 °C and not higher
than a martensite transformation start temperature (Ms point) and then reheating and
holding in a temperature range from 300 to 450 °C; and
- (B) a sub-process for holding in a temperature range from 300 to 450 °C during the
cooling without performing reheating.
EFFECTS OF THE INVENTION
[0011] The present invention provides a cold-rolled steel sheet having high strength and
good hole expandability.
EMBODIMENTS FOR CARRYING OUT THE INVENTION
[0012] To solve the above-identified problem, the present inventors conducted various research
and obtained the following discoveries.
[0013] To increase the strength of a cold-rolled steel sheet, the sheet must be subjected
to an appropriate heat treatment to transform the microstructure into a microstructure
mainly composed of tempered martensite and bainite. Further, to obtain good hole expandability,
it is effective to provide a uniform Mn distribution in the microstructure. Providing
a uniform Mn distribution prevents production of the martensite-austenite constituent
(MA) during heat treatment. In regions where Mn has concentrated, hardenability increases
and thus MA can easily be produced. MA is a very hard structure and can easily provide
initiation points for cracks during hole expansion. Preventing production of MA will
improve hole expandability.
[0014] Specifically, the microstructure is to be a microstructure containing tempered martensite
and bainite in not less than 85 volume % in total and, as seen in a cross section
of the steel sheet, the area ratio of regions where the Mn concentration in the microstructure
is not lower than 8.0 mass % is to be 0.05 to 1.5 area %. A low area ratio of regions
with an Mn concentration not lower than 8.0 mass % (hereinafter referred to as "Mn
concentration regions") means a uniform Mn distribution. Reducing the area ratio of
Mn concentration regions prevents production of MA to improve hole expandability.
On the other hand, if the Mn concentration regions completely disappear, good elongation
cannot be provided. Ensuring that Mn concentration regions are still present in a
low area ratio (not lower than 0.05 area %) promotes hardening during working of the
steel, thereby improving elongation of the steel.
[0015] To provide such a microstructure, the following heat treatment is effective: first,
a hot-rolled steel sheet is subjected to a heat treatment where it is held in the
temperature range from 620 to 700 °C for not shorter than 10 minutes; this produces
cementite in the steel, in which not lower than 10 mass % Mn typically concentrates;
this steel sheet is cold rolled and, thereafter, held at a temperature of 880 to 1050
°C to cause Mn in the microstructure to diffuse, providing a uniform Mn distribution;
this steel sheet is cooled to a temperature not higher than 450 °C at a cooling rate
not lower than 20 °C/s to produce martensite and bainite.
[0016] According to a preferred embodiment, the microstructure is a microstructure further
containing ferrite in not less than 5 volume %, and the average crystal grain size
of ferrite is not larger than 10.0 pm. Providing a microstructure containing ferrite
in not less than 5 volume % will further improve elongation.
[0017] The present invention was made based on these discoveries. Now, a cold-rolled steel
sheet according to one embodiment of the present invention will be described.
[Cold-Rolled Steel Sheet]
[Chemical Composition]
[0018] The cold-rolled steel sheet according to one embodiment of the present invention
has such a chemical composition as specified below. In the description below, "%"
for the content of an element means mass %.
C: 0.10 to 0.30 %
[0019] Carbon (C) improves the strength of steel. On the other hand, if C content is too
high, this decreases elongation of the steel. In view of this, C content is to be
0.10 to 0.30 %. A lower limit of C content is preferably 0.12 %, and more preferably
0.15 %. An upper limit of C content is preferably 0.25 %, and more preferably 0.20
%.
Si: up to 2.50 %
[0020] Silicon (Si) is a solid-solution strengthening element; however, an excessive content
decreases the hot workability of the steel. In view of this, Si content is to be not
higher than 2.50 %. An upper limit of Si content is preferably 2.00 %, and more preferably
1.50 %. A lower limit of Si content is preferably 0.10 %, and more preferably 0.30
%.
Mn: 0.50 to 3.50 %
[0021] Manganese (Mn) increases the hardenability of steel to improve the strength of the
steel. On the other hand, if Mn content is too high, this decreases elongation of
the steel. In view of this, Mn content is to be 0.50 to 3.50 %. A lower limit of Mn
content is preferably 0.80 %, more preferably 1.20 %, yet more preferably 1.55 %,
and still more preferably 1.60 %. An upper limit of Mn content is preferably 3.30
%, more preferably 3.00 %, and yet more preferably 2.80 %.
P: up to 0.100 %
[0022] Phosphorus (P) is an impurity. P segregates on grain boundaries to decrease elongation
of the steel. In view of this, P content is to be not higher than 0.100 %. P content
is preferably not higher than 0.050 %, and more preferably not higher than 0.030 %.
S: up to 0.020 %
[0023] Sulfur (S) is an impurity. S decreases the hot workability of steel. In view of this,
S content is to be not higher than 0.020 %. S content is preferably not higher than
0.015 %, and more preferably not higher than 0.010 %.
Al: 0.010 to 0.100 %
[0024] Aluminum (Al) is contained in steel to serve as a deoxidizer. On the other hand,
if Al content is too high, this produces inclusions, thus decreasing elongation of
the steel. In view of this, Al content is to be 0.010 to 0.100 %. A lower limit of
Al content is preferably 0.015 %, and more preferably 0.020 %. An upper limit of Al
content is preferably 0.080 %, and more preferably 0.060 %.
N: up to 0.0100 %
[0025] Nitrogen (N) is an impurity. N decreases elongation of the steel. In view of this,
N content is to be not higher than 0.0100 %. An upper limit of N content is preferably
0.0060 %, and more preferably 0.0040 %. On the other hand, excessively reducing N
increases manufacturing costs. A lower limit of N content is preferably 0.0005 %,
and more preferably 0.0010 %.
[0026] The chemical composition of the cold-rolled steel sheet according to the present
embodiment may include one or more elements selected from the group consisting of
Ti, Nb, V, Mo, W, B, Ca, Mg and REM. All of these elements are optional elements.
In other words, the chemical composition of the cold-rolled steel sheet according
to the present embodiment may not include all of Ti, Nb, V, Mo, W, B, Ca, Mg and REM,
or may include none of them.
Ti: 0 to 0.100 %
Nb: 0 to 0.100 %
V: 0 to 0.50 %
Mo: 0 to 0.50 %
W: 0 to 0.50 %
[0027] Titanium (Ti), niobium (Nb), vanadium (V), molybdenum (Mo), and tungsten (W) all
have the effect of improving the strength of steel by forming carbides. This effect
is produced if small amounts of Ti, Nb, V, Mo, and W are contained in the steel. On
the other hand, excessive contents of Ti, Nb, V, Mo, and W decrease elongation of
the steel. In view of this, each of the contents of Ti and Nb is to be 0 to 0.100
%, and each of the contents of V, Mo and W is to be 0 to 0.50 %. A lower limit for
Ti and Nb is preferably 0.005 %. An upper limit for Ti and Nb is preferably 0.060
%, and more preferably 0.040 %. A lower limit for V, Mo and W is preferably 0.01 %.
An upper limit for V, Mo and W is preferably 0.40 % and more preferably 0.30 %.
B: 0 to 0.0050 %
[0028] Boron (B) increases hardenability to improve the strength of the steel. This effect
is produced if a small amount of B is contained in the steel. On the other hand, an
excessive B content decreases elongation of the steel. In view of this, B content
is to be 0 to 0.0050 %. A lower limit of B content is preferably 0.0003 %. An upper
limit of B content is preferably 0.0040 %, and more preferably 0.0030 %.
Ca: 0 to 0.0100 %
Mg: 0 to 0.0100 %
REM: 0 to 0.0100 %
[0029] Calcium (Ca), magnesium (Mg) and rare earth elements (REM) all improve the hot workability
of steel. This effect is produced if small amounts of Ca, Mg and REM are contained.
On the other hand, excessive contents of Ca, Mg and REM produce inclusions, thus decreasing
elongation of the steel. In view of this, each of the contents of Ca, Mg and REM is
to be 0 to 0.0100 %. A lower limit of each of the contents of Ca, Mg and REM is preferably
0.0001 %. An upper limit of each of the contents of Ca, Mg and REM is preferably 0.0060
%, and more preferably 0.0040 %. REM is the collective term for a total of 17 elements,
namely, Sc, Y and the lanthanoids, and REM content means the total amount of these
elements.
[0030] The balance of the chemical composition of the cold-rolled steel sheet according
to the present embodiment is Fe and impurities. Impurity as used herein means an element
originating from ore or scrap used as raw material for steel or an element that has
entered from the environment or the like during the manufacturing process. Although
not limiting, examples of impurities include Cu, Ni, Cr and O.
[Microstructure]
[0031] The microstructure of the cold-rolled steel sheet according to the present embodiment
contains tempered martensite and bainite in not less than 85 volume % in total. The
required strength cannot be obtained if the total volume ratio of tempered martensite
and bainite is lower than 85 %. As used herein, "bainite" encompasses bainite that
has undergone tempering. Part of the bainite in the microstructure of the cold-rolled
steel sheet according to the present embodiment may be tempered. Further, even though
cementite is present in the tempered martensite and bainite, the cementite in the
tempered martensite and bainite is not treated as an independent structure, and its
volume is included in the total volume of the tempered martensite and bainite.
[0032] The average particle size of the cementite contained in the tempered martensite and
bainite is larger than 30 nm. The average particle size of cementite is measured by
taking, from a cold-rolled steel sheet, an extraction replica film and then using
transmission electron microscopy (with an accelerating voltage of 200 kV) to observe
three or more fields of view at a magnification for observation of 10,000 to 100,000
times. An average particle size means an equivalent circle diameter. If the microstructure
is mainly composed of martensite containing no cementite (i.e., mainly composed of
as-quenched martensite), it is not possible to provide sufficient hole expandability.
The average particle size of cementite is preferably larger than 50 nm.
[0033] In the cold-rolled steel sheet according to the present embodiment, the regions where
the Mn concentration in the microstructure is not lower than 8.0 mass % are present
in 0.05 to 1.5 area %. A low area ratio of the regions with an Mn concentration not
lower than 8.0 mass % (hereinafter referred to as "Mn concentration regions") means
a uniform Mn distribution. Reducing the area ratio of Mn concentration regions prevents
production of MA to improve hole expandability. On the other hand, if the Mn concentration
regions completely disappear, good elongation cannot be provided. Ensuring that Mn
concentration regions are still present in not less than 0.05 area % promotes hardening
during working of the steel, thereby improving elongation of the steel.
[0034] A lower limit for Mn concentration regions is preferably 0.10 area %, and more preferably
0.20 area %. An upper limit for Mn concentration regions is preferably 1.0 area %.
[0035] The microstructure of the cold-rolled steel sheet according to the present embodiment
preferably further contains ferrite in not less than 5 volume %, where the average
crystal grain size of the ferrite is not larger than 10.0 pm. Providing a microstructure
containing ferrite in not less than 5 volume % further improves elongation. A lower
limit of the volume ratio of ferrite is more preferably 10 %. However, the effect
of improving elongation cannot be produced if the average crystal grain size of ferrite
is too large. An upper limit of the average crystal grain size of ferrite is more
preferably 5.0 pm.
[0036] Although not limiting, the balance of the microstructure of the cold-rolled steel
sheet according to the present embodiment may be pearlite, MA, and/or retained austenite,
for example. In the microstructure of the cold-rolled steel sheet according to the
present embodiment, the volume ratio of the balance excluding martensite, tempered
martensite and ferrite is not higher than 5 %. An upper limit of the volume ratio
of the balance is preferably 3 %.
[0037] The cold-rolled steel sheet according to the present embodiment preferably has a
tensile strength not lower than 980 MPa. A lower limit of tensile strength is more
preferably 1050 MPa, and more preferably 1180 MPa. Although not limiting, an upper
limit of tensile strength may be 1450 MPa, for example.
[0038] The cold-rolled steel sheet according to the present embodiment preferably has a
breaking elongation not lower than 8.0 %. A lower limit of breaking elongation is
more preferably 10.0 %.
[Method of Manufacturing Cold-Rolled Steel Sheet]
[0039] Next, an exemplary method of manufacturing the above-described cold-rolled steel
sheet will be described. The manufacturing method described below is merely illustrative,
and is not intended to limit the method of manufacturing the cold-rolled steel sheet
according to the present embodiment.
[0040] A hot-rolled steel sheet having such a chemical composition as specified above is
prepared. The hot-rolled steel sheet may be produced by, for example, preparing a
slab having such a chemical composition as specified above, hot rolling the slab by
a common method, and coiling the resulting sheet. The method is not limited to any
particular reduction in sectional area during hot rolling, sheet thickness after rolling,
method of cooling to room temperature, or coiling conditions, for example.
[0041] The hot-rolled steel sheet is held in the temperature range from 620 to 700 °C for
not shorter than 10 minutes. This heat treatment will be hereinafter referred to as
"post-hot-rolling heat treatment". This post-hot-rolling heat treatment produces cementite
in the steel, in which Mn concentrates. Mn does not sufficiently concentrate if the
holding temperature is too low or the holding time is too short, in which case it
may not be possible to ensure that the area ratio of Mn concentration regions in the
microstructure of the eventual cold-rolled steel sheet is not lower than 0.05 area
%. On the other hand, if the holding temperature is too high, austenite may be produced
in portions of the microstructure, leading to insufficient Mn concentration. A lower
limit of the holding temperature for the post-hot-rolling heat treatment is preferably
630 °C. An upper limit of the holding temperature for the post-hot-rolling heat treatment
is preferably 680 °C. A lower limit of the holding time for the post-hot-rolling heat
treatment is preferably 30 minutes, and more preferably 60 minutes. Although not limiting,
an upper limit of the holding time for the post-hot-rolling heat treatment may be
300 minutes, for example. Any cooling rate after the holding may be used.
[0042] Further, depending on the thermodynamic properties of the cementite, performing the
post-hot-rolling heat treatment near 600 °C may excessively increase the Mn concentration
in the cementite. As such, if the temperature for the post-hot-rolling heat treatment
is lower than 620 °C, local Mn concentration may be excessively high, which may make
it impossible to cause Mn to sufficiently diffuse during the post-cold-rolling heat
treatment, in which case it may not be possible to ensure that the area ratio of Mn
concentration regions is not higher than 1.5 %.
[0043] The steel sheet subjected to the post-hot-rolling heat treatment is subjected to
cold rolling. The reduction in sheet thickness during the cold rolling may be 30 to
80 %, for example.
[0044] The steel sheet subjected to the cold rolling is held in the temperature range from
880 to 1050 °C for not shorter than 10 seconds and, thereafter, cooled to a temperature
not higher than 450 °C at a cooling rate not lower than 20 °C/s. This heat treatment
will be hereinafter referred to as "post-cold-rolling heat treatment".
[0045] As the steel sheet is held in the temperature range from 880 to 1050 °C for not shorter
than 10 seconds, Mn in the microstructure diffuses, providing a uniform Mn concentration
distribution. Mn does not sufficiently diffuse if the holding temperature is too low
or the holding time is too short, in which case it may not be possible to ensure that
the area ratio of Mn concentration regions in the microstructure of the eventual cold-rolled
steel sheet is not higher than 1.5 area %. On the other hand, if the holding temperature
is too high, Mn diffuses and thus decreases concentration in the Mn concentration
regions to below the lower limit of Mn concentration. A lower limit of the holding
temperature for the post-cold-rolling heat treatment is preferably 900 °C, and more
preferably 920 °C. An upper limit of the holding temperature for the post-cold-rolling
heat treatment is preferably 1000 °C. A lower limit of the holding time for the post-cold-rolling
heat treatment is preferably 20 seconds, and more preferably 30 seconds. Although
not limiting, an upper limit of the holding time for the post-cold-rolling heat treatment
may be 300 seconds, for example.
[0046] After the steel sheet has been held in the temperature range from 880 to 1050 °C,
it is cooled to a temperature not higher than 450 °C at a cooling rate not lower than
20 °C/s. At this time, part of the microstructure transforms to martensite. A microstructure
containing ferrite in not less than 5 volume % is obtained if the cooling rate at
this time is 20 to 30 °C/s, which is relatively low. If the cooling rate is lower
than 20 °C/s, an excessive amount of ferrite is produced, in which case it is not
possible to ensure that the total volume ratio of tempered martensite and bainite
in the microstructure of the eventual cold-rolled steel sheet is not lower than 85
%. Although not limiting, an upper limit of the cooling rate may be 200 °C/s, for
example.
[0047] After the sheet has been cooled to a temperature not higher than 450 °C, one of the
following sub-processes is further performed: (A) the sheet is cooled to a temperature
not higher than 350 °C and not higher than the martensite transform start temperature
(Ms point) and, thereafter, the sheet is reheated and held in the temperature range
from 300 to 450 °C for a predetermined period of time (preferably not shorter than
100 seconds) ("quench & partitioning process"); and (B) the sheet is held in the temperature
range from 300 to 450 °C during the cooling for a predetermined period of time (preferably
not shorter than 100 seconds), without being reheated ("austempering process").
[0048] The cementite that precipitated during the post-hot-rolling heat treatment is dissolved
during the post-cold-rolling heat treatment. The amount of dissolution of cementite
at this time is to be not smaller than 90 volume % of the cementite prior to the post-cold-rolling
heat treatment, and preferably not smaller than 95 volume %. After the post-cold-rolling
heat treatment and the subsequent cooling, one of sub-processes (A) and (B) above
is performed to cause cementite to precipitate once again in the microstructure. This
results in a microstructure containing tempered martensite and bainite in not less
than 85 volume % in total. If the holding temperature is lower than 300 °C, cementite
may not precipitate in a sufficient amount (i.e., the average particle size of cementite
may not be larger than 30 nm).
[0049] The above-described process results in the cold-rolled steel sheet according to the
present embodiment. The manufacturing method described above provides a cold-rolled
steel sheet containing tempered martensite and bainite in not less than 85 volume
% in total and having a microstructure with structures other than tempered martensite,
bainite and ferrite in not more than 5 volume %, wherein the regions where the Mn
concentration in the microstructure is not lower than 8.0 mass % are present in 0.05
to 1.5 area %.
[0050] A cold-rolled steel sheet according to one embodiment of the present invention, as
well as a method of manufacturing the same, have been described. The present embodiment
provides a cold-rolled steel sheet with high strength and good hole expandability.
EXAMPLES
[0051] The present invention will be described more specifically below by means of examples.
The present invention is not limited to these examples.
[0052] 180 kg steel ingots having the chemical compositions shown in Table 1 were smelted
in a high-frequency vacuum melting furnace and subjected to hot forging to produce
slabs with a thickness of 30 mm. Each slab thus obtained was hot rolled by a hot-rolling
test instrument to a finish temperature of 850 to 900 °C to produce a hot-rolled steel
sheet with a thickness of 2.0 mm. After the hot rolling had been completed and 3 to
10 seconds had passed, the steel sheet was cooled to a wind-up temperature of 200
to 650 °C and, thereafter, cooled to a temperature not higher than 200 °C at a cooling
rate of 20 °C/s to imitate the coiling of the steel sheet, thus producing a hot-rolled
steel sheet.
[Table 1]
[0053]
TABLE 1
| Steel type |
Chemical composition (in mass %, balance Fe and impurities) |
| C |
Si |
Mn |
P |
S |
sol. Al |
N |
Others |
| A |
0.15 |
0.92 |
2.81 |
0.013 |
0.005 |
0.036 |
0.0021 |
- |
| B |
0.17 |
1.43 |
2.34 |
0.014 |
0.004 |
0.021 |
0.0034 |
Ti: 0.023 |
| C |
0.13 |
0.64 |
1.77 |
0.017 |
0.003 |
0.041 |
0.0020 |
V: 0.21 |
| D |
0.19 |
0.74 |
1.55 |
0.011 |
0.007 |
0.028 |
0.0023 |
Mo: 0.23, Mg: 0.0026 |
| E |
0.23 |
1.18 |
2.53 |
0.022 |
0.004 |
0.033 |
0.0025 |
Nb: 0.022 |
| F |
0.14 |
0.68 |
2.11 |
0.015 |
0.006 |
0.039 |
0.0034 |
W: 0.11, REM: 0.0019 |
| G |
0.20 |
0.66 |
3.23 |
0.013 |
0.004 |
0.027 |
0.0027 |
Ti: 0.019, Nb: 0.011, B: 0.0015 |
| H |
0.22 |
0.62 |
1.87 |
0.019 |
0.003 |
0.039 |
0.0030 |
Ca: 0.0033 |
| I |
0.18 |
0.38 |
0.40 |
0.011 |
0.007 |
0.024 |
0.0028 |
- |
| J |
0.01 |
0.02 |
0.17 |
0.012 |
0.005 |
0.027 |
0.0034 |
- |
[0054] The hot-rolled steel sheet was subjected to heat treatment (i.e., post-hot-rolling
heat treatment) at the relevant temperature and for the relevant holding time shown
in Table 2 and, thereafter, subjected to cold rolling at a reduction in sheet thickness
(i.e., reduction during cold rolling) of 50 % to produce a piece of steel material
with a thickness of 1.0 mm.
[Table 2]
[0055]
TABLE 2
| Test No. |
Steel type |
Post-hot-rolling heat treatment |
Cold rolling |
Post-cold-rolling heat treatment |
| Holding temp. (°C) |
Holding time (min) |
Cold-rolling ratio (%) |
Holding temp. (°C) I |
Holding time (s) |
Cooling rate (°C/s) |
After cooling at 450 °C |
| 1 |
A |
650 |
80 |
50 |
900 |
60 |
40 |
quench & partitioning |
| 2 |
A |
650 |
80 |
50 |
950 |
60 |
40 |
quench & partitioning |
| 3 |
A |
650 |
80 |
50 |
1000 |
60 |
40 |
quench & partitioning |
| 4 |
A |
650 |
30 |
50 |
900 |
60 |
40 |
quench & partitioning |
| 5 |
A |
650 |
120 |
50 |
900 |
60 |
40 |
quench & partitioning |
| 6 |
A |
650 |
80 |
50 |
900 |
45 |
25 |
quench & partitioning |
| 7 |
A |
650 |
80 |
50 |
900 |
35 |
25 |
quench & partitioning |
| 8 |
A |
650 |
120 |
50 |
920 |
60 |
40 |
austempering |
| 9 |
B |
650 |
80 |
50 |
950 |
80 |
35 |
austempering |
| 10 |
B |
650 |
80 |
50 |
950 |
120 |
35 |
austempering |
| 11 |
C |
650 |
80 |
50 |
950 |
60 |
20 |
austempering |
| 12 |
D |
650 |
80 |
50 |
900 |
60 |
20 |
quench & partitioning |
| 13 |
E |
650 |
80 |
50 |
920 |
60 |
50 |
quench & partitioning |
| 14 |
F |
650 |
80 |
50 |
920 |
60 |
50 |
quench & partitioning |
| 15 |
G |
650 |
80 |
50 |
900 |
60 |
70 |
quench & partitioning |
| 16 |
H |
650 |
80 |
50 |
900 |
60 |
100 |
austempering |
| 17 |
A |
650 |
80 |
50 |
830 |
60 |
40 |
quench & partitioning |
| 18 |
A |
550 |
80 |
50 |
950 |
60 |
40 |
quench & partitioning |
| 19 |
A |
650 |
80 |
50 |
800 |
60 |
40 |
quench & partitioning |
| 20 |
A |
650 |
80 |
50 |
950 |
60 |
5 |
quench & partitioning |
| 21 |
A |
650 |
80 |
50 |
950 |
5 |
40 |
quench & partitioning |
| 22 |
A |
600 |
120 |
50 |
920 |
60 |
40 |
austempering |
| 2.3 |
A |
650 |
120 |
50 |
920 |
60 |
40 |
- |
| 24 |
B |
650 |
80 |
50 |
820 |
120 |
40 |
austempering |
| 25 |
C |
650 |
80 |
50 |
830 |
60 |
40 |
austempering |
| 26 |
D |
650 |
80 |
50 |
900 |
3 |
40 |
quench & partitioning |
| 27 |
E |
400 |
80 |
50 |
830 |
60 |
40 |
quench & partitioning |
| 28 |
F |
650 |
80 |
50 |
920 |
60 |
5 |
quench & partitioning |
| 29 |
G |
650 |
80 |
50 |
830 |
60 |
70 |
quench & partitioning |
| 30 |
H |
650 |
80 |
50 |
830 |
60 |
100 |
austempering |
| 31 |
I |
650 |
80 |
50 |
950 |
60 |
40 |
quench & partitioning |
| 32 |
J |
650 |
80 |
50 |
950 |
60 |
40 |
austempering |
[0056] From the piece of steel material thus obtained were taken test samples with a width
of 160 mm and a length of 230 mm. Each test sample thus obtained was subjected to
heat treatment (i.e., annealing) under the relevant conditions indicated in the "Post-cold-rolling
heat treatment" columns in Table 2.
[0057] Specifically, the test sample was heated to the relevant temperature in Table 2 and
soaked for the relevant holding time shown in Table 2. After the soaking, the test
sample was cooled to a temperature not higher than 450 °C at the relevant cooling
rate in Table 2. Furthermore, the test samples labeled Test Nos. 1 to 7, 12 to 15,
17 to 21, 26 to 29 and 31 were cooled to a temperature not higher than 350 °C and
not higher than the martensite transformation start temperature (Ms point) and then
reheated and held in the temperature range from 350 to 400 °C for 300 seconds (quench
& partitioning process), before being cooled to room temperature. The test samples
labeled Test Nos. 8 to 11, 16, 22, 24, 25, 30 and 32 were subjected to a sub-process
for holding in the temperature range from 350 to 400 °C for 300 seconds during the
cooling without reheating (austempering) before cooling to room temperature. The test
sample labeled Test No. 23 was cooled to room temperature without being subjected
to any of the above-mentioned sub-processes.
[0058] The test samples after heat treatment were used for microstructure observation, tensile
testing and hole expansion testing.
[0059] To evaluate tensile properties, from each test sample after heat treatment were taken
two JIS No. 5 test specimens with a longitudinal direction parallel to the direction
of rolling (i.e., L-direction), which were tested at a tension rate of 10 mm/min.
From the results, tensile strength (TS/MPa) and breaking elongation (tEL/%) were determined.
The tensile strength and breaking elongation were represented by the average values
for the two tensile test specimens.
[0060] To measure hole expansion ratio, two 90 mm × 90 mm test specimens were taken from
each test sample after heat treatment, and a punching hole was formed in the middle
with the original hole diameter
d0 = 10 mm. This hole was expanded using a conical punch with a tip angle of 60°; the
expanding was stopped when the edge of the punched hole developed a crack extending
through the sheet thickness, and the load was removed. In the test specimen, the hole
diameters in the direction parallel to, the direction perpendicular to, and two directions
angled at 45° relative to, the direction of rolling were measured, and the average
thereof was treated as the hole diameter after hole expansion, d. The hole expansion
ratio HER was evaluated by the expression provided below. The hole expansion ratio
HER was represented by the average for the two test specimens.

[0061] The microstructure of the test sample after heat treatment was measured by the following
method.
[0062] First, from each test sample after heat treatment was taken an observation sample
with an observation surface represented by a cut surface parallel to the direction
of rolling and the sheet-thickness direction. Electron backscatter diffraction (EBSD)
analysis was performed in a 200 pmL × 100 pmT region in the L-cut surface of the test
sample (i.e., cut surface parallel to the direction of rolling and the sheet-thickness
direction). The scan step was 0.1 pm, and the measurement points were on a hexagonal
grid.
[0063] The EBSD data was analyzed, where crystal phases were identified in the EBSD pattern
for the measurement points; a region identified as in the BCC phase was classified
as tempered martensite, bainite or ferrite; a region identified as in the FCC phase
was classified as retained austenite; and a region where the microstructure could
not be identified (e.g., with an EBSD system from TSL Solutions Co. Ltd., the confidential
index value was lower than 0.1) was classified as cementite contained in MA or pearlite.
[0064] The regions identified as in the BCC phase were further classified as ferrite and
non-ferrite (i.e., tempered martensite or bainite) in the following manner.
[0065] In the EBSD data, a grain boundary was defined as a boundary with a crystal misorientation
not smaller than 15 °, and the region surrounded by grain boundaries was treated as
a crystal grain. Where the number of EBSD measurement points contained inside a crystal
grain in the BCC phase is denoted by
m, and a rotation matrix representing the crystal orientation at an individual measurement
point is denoted by
Pj(
j= 1 ...
m), all the combinations of the crystal misorientations
Δθ (in degrees) between adjacent measurement points were calculated using the following
expressions, and the average value of these misorientations, M, was determined.

[0066] Pi and
Pj are rotation matrices that can be calculated using the Euler angles for each measurement
point determined by EBSD measurement. Specifically,
Pi was obtained by substituting the Euler angles (
ϕ1, Φ and
ϕ2) for the
ith measurement point (i = 1 ...
m) obtained by EBSD measurement into the following expression.

[0067] Rk (
k= 1 ... 24) is a rotation matrix for conversion of the basis vectors of a cubic crystal,
where such a value of k was selected as to minimize the rotational angle of
Rk·Pi·Pj. Adjacent measurement points were selected for the
ith and jth measurements.
D[
i,
i] expresses the value of the component at the
ith row and
ith column of a 3 × 3 matrix D. A BCC crystal grain with an average crystal misorientation
M not larger than 0.5° was treated as ferrite, and a crystal grain in excess of 0.5°
was treated as tempered martensite or bainite.
[0068] After the structures were thus classified, the proportion of the measurement points
determined to be in the non-ferrite BCC phase (i.e., tempered martensite or bainite)
and the proportion of the measurement points determined to be ferrite in all the measurement
points were determined, and these proportions were treated as the total volume ratio
of tempered martensite / bainite and the volume ratio of ferrite, respectively. The
remaining regions contained pearlite, MA and retained austenite (i.e., regions identified
as in the FCC phase based on EBSD), and were classified as "other regions".
[0069] The average crystal grain size of ferrite was determined by calculating the average
value
d of equivalent circle diameters from EBSD measurements using the expression indicated
below. However, a test sample with a volume ratio of ferrite lower than 5 % was excluded
from evaluation.

[0070] Here,
Ai is the area of the
ith ferrite crystal grain determined through analysis of EBSD data, and
di is the equivalent circle diameter of the
ith ferrite crystal grain. An equivalent circle diameter means the diameter of a circle
with an area equal to the area of the
ith ferrite crystal grain (=
Ai).
[0071] Using the same samples for observation as mentioned above, mapping measurement of
Mn concentration in the microstructure was performed using an electron probe microanalyzer
(EPMA). JXA-8530F from JEOL Ltd. was used, where the accelerating voltage of the electron
beam was 7 kV, the amount of current for illumination was 20 nA; a 30 pm × 30 pm region
in the observation surface was divided into sub-regions that each contained 500 points
× 500 points (arranged on a square lattice) and the electron beam was scanned, and
the fluorescent X-ray (i.e., Kα line) of Mn generated from each point was measured
by a wavelength resolving detector.
[0072] From the obtained counts of the fluorescent X-ray,
I, the Mn concentration
XMn for each point was determined using the following evaluation expression based on
ZAF correction:

[0073] Here,
I0 indicates the count of a fluorescent X-ray (i.e., Kα line) obtained from a pure-Mn
standard sample in advance by EPMA measurement under the same electron beam conditions.
Z, A and
F indicate atomic-number correction, absorption correction coefficient and fluorescent
correction coefficient, respectively, where the values used were known values determined
based on the illumination conditions for the electron beam for EPMA and the component
values of steel in accordance with SOEJIMA, Hiroyoshi: "Electron Probe Microanalysis",
Nikkan Kogyo Shimbun, Ltd.
[0074] From the Mn concentration distribution obtained was determined the proportion of
measurement points with an Mn concentration not lower than 8.0 mass % in all the measurement
points (250,000 points), and was treated as the area ratio of regions with an Mn concentration
not lower than 8.0 mass %.
[0075] The results are shown in Table 3. In Table 3, "TM+B" indicates the total volume ratio
of tempered martensite and bainite, and "α" indicates the volume ratio of ferrite.
"A*" indicates the area ratio of regions with an Mn concentration not lower than 8.0
mass %.
[Table 3]
[0076]
TABLE 3
| Test No. |
Steel type |
Metal microstructure |
Mechanical properties |
|
| Volume ratio (%) |
Ferrite avg. crystal grain size (µm) |
A* (%) |
TS (MPa) |
tEL (%) |
HER (%) |
| TM+B |
α |
Balance |
| 1 |
A |
97 |
2 |
1 |
- |
0.8 |
1154 |
9.2 |
43.3 |
inv. ex. |
| 2 |
A |
96 |
3 |
1 |
- |
0.3 |
1146 |
9.0 |
45.9 |
| 3 |
A |
98 |
1 |
1 |
- |
0.2 |
1168 |
102 |
46.8 |
| 4 |
A |
96 |
3 |
1 |
- |
0.3 |
1148 |
10.4 |
49.5 |
| 5 |
A |
97 |
2 |
1 |
- |
0.8 |
1145 |
9.2 |
42.5 |
| 6 |
A |
89 |
10 |
1 |
4.4 |
0.4 |
1097 |
11.6 |
42.0 |
| 7 |
A |
86 |
13 |
1 |
4.3 |
0.7 |
1036 |
13.9 |
49.0 |
| 8 |
A |
97 |
2 |
1 |
- |
0.9 |
1058 |
14.3 |
41.5 |
| 9 |
B |
96 |
3 |
1 |
- |
0.6 |
1218 |
9.5 |
59.5 |
| 10 |
B |
95 |
4 |
1 |
- |
0.2 |
1202 |
10.4 |
40.4 |
| 11 |
C |
91 |
8 |
1 |
2.5 |
0.2 |
1011 |
13.2 |
40.4 |
| 12 |
D |
88 |
11 |
1 |
2.1 |
0.8 |
1233 |
10.7 |
41.2 |
| 13 |
E |
95 |
4 |
1 |
- |
0.9 |
1441 |
8.8 |
53.8 |
| 14 |
F |
98 |
1 |
1 |
- |
0.5 |
1073 |
9.3 |
47.7 |
| 15 |
G |
96 |
3 |
1 |
- |
0.6 |
1359 |
8.1 |
43.1 |
| 16 |
H |
95 |
4 |
1 |
- |
0.4 |
1402 |
8.9 |
54.3 |
| 17 |
A |
86 |
11 |
3 |
2.8 |
3.4 |
981 |
11.7 |
32.6 |
comp. ex. |
| 18 |
A |
95 |
2 |
3 |
3.2 |
0.0 |
1135 |
7.4 |
26.7 |
| 19 |
A |
86 |
11 |
3 |
3.3 |
3.7 |
998 |
11.8 |
25.2 |
| 20 |
A |
76 |
23 |
1 |
7.2 |
0.4 |
963 |
11.3 |
29.4 |
| 21 |
A |
94 |
3 |
3 |
- |
3.0 |
1162 |
9.4 |
31.9 |
| 22 |
A |
95 |
3 |
2 |
- |
1.8 |
1065 |
13.9 |
30.6 |
| 23 |
A |
26 |
9 |
65 |
- |
0.9 |
1339 |
6.9 |
38.2 |
| 24 |
B |
87 |
10 |
3 |
- |
2.9 |
1134 |
10.3 |
34.2 |
| 25 |
C |
86 |
12 |
2 |
3.3 |
2.5 |
1018 |
10.3 |
32.4 |
| 26 |
D |
94 |
3 |
3 |
- |
3.2 |
1297 |
8.9 |
25.1 |
| 27 |
E |
86 |
12 |
2 |
7.9 |
0.0 |
1310 |
6.5 |
36.8 |
| 28 |
F |
78 |
20 |
2 |
2.7 |
0.6 |
949 |
11.5 |
28.9 |
| 29 |
G |
86 |
11 |
3 |
3.7 |
3.2 |
1210 |
8.3 |
32.3 |
| 30 |
H |
85 |
11 |
4 |
2.7 |
3.9 |
1229 |
9.7 |
28.0 |
| 31 |
I |
2 |
91 |
7 |
9.2 |
0.3 |
542 |
32.0 |
55.0 |
| 32 |
J |
0 |
99 |
1 |
19.7 |
0.0 |
289 |
53.0 |
183.0 |
| A : Area ratio of regions with an Mn concentration not lower than 8.0 mass % |
[0077] As shown in Tables 1 to 3, each of the test samples labeled Test Nos. 1 to 16 contained
tempered martensite and bainite in not less than 85 volume % in total, and had a microstructure
with the structures other than tempered martensite, bainite and ferrite in not more
than 5 mass %, wherein the regions where the Mn concentration in the microstructure
was not lower than 8.0 mass % were present in 0.05 to 1.5 area %. In each of these
test samples, the average particle size of cementite contained in tempered martensite
and bainite was larger than 50 nm. These test samples had a tensile strength not lower
than 980 MPa, an elongation not lower than 8.0 %, and a hole expansion ratio not lower
than 40.0 %. In particular, the test samples labeled Test Nos. 6, 7, 11 and 12 had
a microstructure further containing ferrite in not less than 5 volume %, where the
average crystal grain size of ferrite was not larger than 10.0 pm. These test samples
had particularly good elongation.
[0078] In contrast, in each of the test samples labeled Test Nos. 17, 19, 21, 22, 24 to
26, 29 and 30, the regions where the Mn concentration in the microstructure was not
lower than 8.0 mass % were present in more than 1.5 area %, and the hole expansion
ratio was lower than 40.0 %. In the test samples labeled Test Nos. 17, 19, 24, 25,
27, 29 and 30, the area ratio of Mn concentration regions was high presumably because
the holding temperature for the post-cold-rolling heat treatment was too low. In the
test samples labeled Test No. 21 and 26, the area ratio of Mn concentration regions
was high presumably because the holding time for the post-cold-rolling heat treatment
was too short. In the test sample labeled Test No. 22, the area ratio of Mn concentration
regions was high presumably because the temperature for the post-hot-rolling heat
treatment was near 600 °C.
[0079] In the test samples labeled Test Nos. 18 and 27, the regions where the Mn concentration
in the microstructure was not lower than 8.0 mass % were present in less than 0.05
area %, and the hole expansion ratio was lower than 40.0 %. The area ratio of Mn concentration
regions of these test samples was low presumably because the temperature for the post-hot-rolling
heat treatment was too low and thus Mn did not concentrate in the cementite in the
steel.
[0080] In each of the test samples labeled Test Nos. 20, 28, 31 and 32, the total volume
ratio of tempered martensite and bainite was lower than 85 %, and the tensile strength
was lower than 980 MPa. In the test samples labeled Test Nos. 20 and 28, the total
volume ratio of tempered martensite and bainite was lower than 85 % presumably because
the cooling rate for the post-cold rolling heat treatment was too low. Further, in
these test samples, an excessive amount of ferrite was produced, which contributed
to a hole expansion ratio lower than 40.0 %. In the test samples labeled Test Nos.
31 and 32, the total volume ratio of tempered martensite and bainite was lower than
85 % presumably because the Mn or C content in the steel material was too low.
[0081] In the test sample labeled Test No. 23, the total volume ratio of tempered martensite
and bainite was lower than 85 %, and the hole expansion ratio was lower than 40.0
%. In the test sample labeled Test No. 23, the total volume ratio of tempered martensite
and bainite was lower than 85 % presumably because the sample was cooled to room temperature
without being subjected to any of the quench & partitioning process and austempering
such that a large portion of the microstructure became martensite without precipitation
of cementite.
[0082] Although embodiments of the present invention have been described, the above-described
embodiments are merely illustrative examples useful for carrying out the present invention.
Thus, the present invention is not limited to the above-described embodiments, and
the above-described embodiments, when carried out, may be modified as appropriate
without departing from the spirit of the invention.