Technical Field
[0001] The present invention relates to steel materials suitable for use in welded structures,
such as pipelines, bridges, and architectural structures, requiring structural safety
and a method for manufacturing the same and particularly relates to one excellent
in resistance of ductile crack initiation from welded heat affected zone and a base
material. Specifically, the invention is targeted to steel materials for structures
having excellent resistance of ductile crack initiation from welded heat affected
zone and a base material and having strength of Tensile strength: 490 MPa or more
in TS and high toughness of Ductile-brittle fracture transition temperature of Charpy
impact test (according to the regulation of JIS Z 2242): vTrs of 0°C or lower.
Background Art
[0002] It is known that when the welded structures, such as pipelines, bridges, and buildings,
are exposed to large external force of an earthquake or the like, ductile crack initiates
in a stress concentration zone, such as a weld toe, and the generated ductile crack
serves as a trigger to cause brittle fracture, resulting in break and fracture of
the structures in some cases.
[0003] In order to avoid such break and fracture of the welded structures, it is important
that steel materials constituting the same are excellent in resistance of ductile
crack initiation.
[0004] Patent Document 1 discloses a high tensile-strength steel material excellent in resistance
of ductile crack initiation in which, in the microstructure a steel material surface
zone, the ferrite area fraction is 10 to 40%, the bainite area fraction is 50% or
more, and the average grain size is 5 µm or lower.
[0005] Patent Document 2 discloses a steel plate excellent in arrestrability and resistance
of ductile fracture in which the microstructure is substantially constituted by a
ferrite structure, a pearlite structure, and a bainite structure and, when divided
into three layers of both surface zones and the central zone in the plate thickness
direction of the steel plate, each zone has a specific microstructure.
[0006] Both the surface zones of the steel plate are constituted by a layer which has 50%
or more of a ferrite structure containing ferrite grains in which the equivalent (circle)
diameter is 7 µm or lower and the aspect ratio is 2 to 4 over 5% or more of the plate
thickness of each of the structure zones and in which the bainite area fraction of
the portion is 5 to 25% or lower. The central zone in the plate thickness direction
of the steel plate is constituted by a layer which contains ferrite grains in which
the equivalent (circle) diameter is 4 to 10 µm and the aspect ratio is 2 or lower
over 50% or more of the plate thickness and in which the bainite area fraction of
the zones is 10% or lower.
More specifically, the technique of Patent Document 2 is directed to a steel plate
in which three layers having a ferrite/pearlite structure containing ferrite grains
different in the aspect ratio are present in the plate thickness direction from the
plate surface of the steel plate and further in which a bainite structure which is
a hard phase is appropriately dispersed in a soft phase which is the ferrite/pearlite
structure. The technique increases the arrestrability by positively forming processed
ferrite grains having a high aspect ratio and also appropriately dispersing a bainite
structure on each of both the surface zones of the three zones of the steel plate
and, in contrast, increases extension characteristics, which are important to ductile
fracture at room temperature, by controlling the central zone of the steel plate to
have a uniform equiaxed ferrite grain structure and also suppressing a bainite structure,
and thus satisfies both opposite characteristics of "arrestrability" and "ductile
fracture characteristics" by controlling both the surface zones and the central zone
of the steel plate to the three-layer structure.
[0007] Also the technique of Patent Document 3 is directed to a technique of obtaining deformed
ferrite grains on the steel plate surface zone of ferrite/pearlite steel and also
controlling the microstructure of the central zone to a uniform equiaxed ferrite grain
structure similarly as the technique of Patent Document 2.
More specifically, Patent Document 3 discloses a method for manufacturing a thick
steel plate excellent in arrestrability and ductile fracture characteristics, in which
the rolling conditions are strictly controlled so that the steel plate surface zone
has a specific microstructure.
[0008] Specifically, when the thickness during plate rolling is defined as t, an equivalent
plastic strain ε of ε ≥ 0.5 in a non-recrystallization temperature zone of Ar
3 transformation point or more and 900°C or lower is given to a surface layer zone
of 0.05 t or more and 0.15 t or lower from both the surfaces in the plate thickness
direction.
[0009] Thereafter, the surface layer zone is cooled to a temperature range of 450 to 650°C
at a cooling rate of 2 to 15°C /s while maintaining the temperature of the central
zone defined as t/4 to 3t/4 of the plate thickness at the Ar
3 transformation point or more within a period of time when the residual and cumulative
equivalent plastic strain sr of the surface layer zone satisfies εr ≥ 0.5, and subsequently
rolling is restarted.
[0010] In the restarted rolling, the residual and cumulative equivalent plastic strain εr
of 0.35 ≤ εr < 0.55 is given to the central zone to complete the rolling at the Ar
3 transformation point or more and also the surface layer is recuperated to the Ar
3 transformation point or lower by processing heat and internal sensible heat, and
thereafter cooling is performed in such a manner that the average cooling rate is
1 to 10°C/s.
The techniques of Patent Documents 1 to 3 all relate to techniques of forming fine
subgrains in austenite to miniaturize the structure after transformation by performing
rolling in a non recrystallization zone (fine grain temperature zone) of austenite
or performing rolling at a rolling finish temperature Ar
3 or more.
Citation List
Patent Literature
[0011]
[Patent Document 1] Japanese Unexamined Patent Application Publication No. 2008-202119
[Patent Document 2] Japanese Unexamined Patent Application Publication No. 2000-328177
[Patent Document 3] Japanese Unexamined Patent Application Publication No. 2003-221619
Disclosure of Invention
Problems to be Solved by the Invention
[0012] However, according to the techniques of Patent Documents 1 to 3, when the surface
layer structure changes to the welded heat affected zone by welding or the like, there
is a concern that the effect of resistance of ductile crack initiation is lost.
[0013] Moreover, in all of a scale breaker for use in treatment of the surface of a slab
extracted from a heating furnace described in Examples of Patent Document 1, two-stage
rolling of rolling in a pulverization temperature range and rolling in a set temperature
zone described in Examples of Patent Document 2, and various kinds of rolling or temperature
control for separately creating the structure of a surface layer and the structure
inside a steel plate described in Patent Document 3, the manufacturing process is
complicated.
[0014] Then, in view of the problems of such former techniques, it is an object of the present
invention to provide steel materials excellent in resistance of ductile crack initiation
from the welded heat affected zone and a base material by a simple method and a method
for manufacturing the same.
Means for Solving the Problems
[0015] In order to achieve the object, the present inventors have conducted extensive researches
on a microstructure of base material excellent in resistance of ductile crack initiation
of a welded heat affected zone and have found that, when a microstructure of base
material has ferrite and a hard phase in which the average aspect ratio of the ferrite
and the area fraction of the hard phase are specified at the 1/4 position of the plate
thickness exhibiting an average structure in the plate thickness direction of a steel
plate, the resistance of ductile crack initiation is excellent also in a welded heat
affected zone and such a steel material is excellent also in the resistance of ductile
crack initiation of the base material, and further manufacturing conditions of a steel
plate having the microstructure.
[0016] The present invention has been accomplished based on the findings and further researches
and is more specifically directed to:
- (1) A steel material excellent in resistance of ductile crack initiation from welded
heat affected zone and a base material has a composition of C: 0.02 to 0.2%, Si: 0.01
to 0.5%, Mn: 0.5 to 2.5%, P: 0.05% or lower, S: 0.05% or lower, Al: 0.1% or lower,
and N: 0.01% or lower in terms of % by mass, and the balance Fe with inevitable impurities,
in which the microstructure at the 1/4 position of the plate thickness contains ferrite
and a hard phase, the area fraction of the hard phase is 50 to 90%, and the average
aspect ratio of the ferrite is 1.5 or more.
- (2) The steel material excellent in resistance of ductile crack initiation from welded
heat affected zone and a base material according to (1), further contains, in the
chemical composition, one or two or more elements selected from Cu: 0.01 to 2%, Ni:
0.01 to 5%, Cr: 0.01 to 3%, Mo: 0.01 to 2%, Nb: 0.1% or lower, V: 0.1% or lower, Ti:
0.1% or lower, B: 0.01% or lower, Ca: 0.01% or lower, and REM: 0.1 % or lower in terms
of % by mass.
- (3) In the steel material excellent in resistance of ductile crack initiation from
welded heat affected zone and a base material according to (1) or (2) above, the structure
on the surface of a steel plate contains ferrite and a hard phase, the area fraction
of the ferrite exceeds 40%, and the average aspect ratio of the ferrite grain size
exceeds 2.
- (4) A method for manufacturing a steel material excellent in resistance of ductile
crack initiation from welded heat affected zone and a base material includes reheating
a steel base material having the chemical compositions of (1) or (2) to 1000°C or
more, rolling the same in such a manner that the rolling reduction rate in a temperature
range of 900°C or more is 50% or more and the rolling finish temperature is Ar3 point to Ar3-50°C, starting water cooling at Ar3-10°C to Ar3-70°C, and terminating the water cooling at 500°C or lower.
- (5) The method for manufacturing a steel material excellent in resistance of ductile
crack initiation from welded heat affected zone and a base material according to (4)
further includes, after the water cooling, performing tempering treatment at a temperature
of lower than the highest heating temperature Ac1 point.
Advantages
[0017] According to the invention, a steel material capable of suppressing ductile crack
initiation from welded heat affected zone and a base material that can suppress ductile
crack initiation from a stress concentration zone, such as a weld toe, and prevent
collapse or break of steel structures even when the steel structures greatly deform
due to an earthquake or the like, for example, can be easily and stably mass-produced
and industrially remarkable effects are demonstrated.
Brief Description of Drawings
[0018]
[Fig. 1] Fig. 1 is a view illustrating a ductile crack initiation test method of a
welded heat affected zone.
[Fig. 2] Fig. 2 is a view illustrating influence of the area fraction of a hard phase
and the average aspect ratio of ferrite on ductile crack initiation of a 1400°C simulated
heat cycle material.
[Fig. 3] Fig. 3 is a view illustrating a ductile crack initiation test method of a
base material.
[Fig. 4] Fig. 4 is a view illustrating influence of the area fraction of a hard phase
and the average aspect ratio of ferrite on ductile crack initiation of a base material.
Best Modes for Carrying Out the Invention
[0019] In the invention, the chemical composition and the microstructure are specified.
In the description of the chemical composition, % by mass is simply represented by
% unless otherwise specified.
[Chemical composition]
C: 0.02 to 0.2%
[0020] C is an element having an action of increasing the strength of steel and, particularly
in the invention, contributes to the generation of a hard phase. In order to obtain
such an effect, the C content of 0.02% or more is required. In contrast, when the
C content exceeds 0.2%, the ductility or the bending workability are reduced and also
the weldability decreases. Therefore, the C content is limited in the range of 0.02
to 0.2%. More preferably, the C content is 0.02 to 0.18%.
Si: 0.01 to 0.5%
[0021] Si acts as a deoxidizing agent and has an action of forming a solid solution to increase
the strength of steel. In order to obtain such an effect, the Si content of 0.01%
or more is required. In contrast, when the Si content exceeds 0.5%, the toughness
is reduced and also the weldability is reduced. Therefor, Si is limited in the range
of 0.01 to 0.5%. More preferably, the Si content is 0.01 to 0.4%.
Mn: 0.1 to 2.5%
[0022] Mn has an action of increasing the strength of steel and also increasing the toughness
through an increase in hardenability. In order to obtain such an effect, the Mn content
of 0.1% or more is required. In contrast, when the Mn content exceeds 2.5%, the weldability
is reduced. Therefore, Mn is limited in the range of 0.1 to 2.5%. More preferably,
the content is 0.5 to 2.0%.
P: 0.05% or lower
[0023] Since P causes degradation of toughness, the P content is preferably reduced as much
as possible, but the content up to 0.05% is permissible. Therefore, the P content
is limited to 0.05% or lower. More preferably, the content is 0.04% or lower.
S: 0.05% or lower
[0024] Since S is present as an inclusion in steel and degrades the ductility and the toughness,
the S content is preferably reduced as much as possible. However, the content up to
0.05% is permissible. Therefore, the S content is limited to 0.05% or lower. More
preferably, the content is 0.04% or lower.
Al: 0.1% or lower
[0025] Al is an element that acts as a deoxidizing agent and also contributes to pulverization
of crystal grains. However, an excessive content of Al in a proportion exceeding 0.1%
causes a reduction in toughness. Therefore, the Al content is limited to 0.1% or lower.
More preferably, the content is 0.05% or lower.
N: 0.01% or lower
[0026] N is an element that increases the strength of steel by solid solution strengthening
similarly as C. However, an excessive content of N causes a reduction in toughness.
Therefore, the N content is limited to 0.01% or lower. More preferably, the content
is 0.005% or lower.
[0027] The chemical compositions described above are basic chemical compositions but, in
the invention, one or two or more elements selected from Cu: 0.01 to 2%, Ni: 0.01
to 5%, Cr: 0.01 to 3%, Mo: 0.01 to 2%, Nb: 0.1% or lower, V: 0.1% or lower, Ti: 0.1%
or lower, B: 0.01% or lower, Ca: 0.01% or lower, and REM: 0.1% or lower may be further
contained according to the desired properties.
Cu: 0.01 to 2%
[0028] Cu is an element that has an action of increasing the strength of steel through an
increase in hardenability or solid solution. In order to secure such an effect, the
content of 0.01% or more is required. In contrast, when the content exceeds 2%, the
weldability decreases and also cracks are likely to generate during manufacturing
of steel materials. Therefore, when Cu is added, the content is in the range of 0.01
to 2%. More preferably, the content is 0.01 to 1%.
Ni: 0.01 to 5%
[0029] Ni is added as required, because Ni contributes to an increase in low temperature
toughness, an increase in hardenability, and prevention of hot ductility of Cu when
Cu is contained. Such an effect is recognized when Ni is contained in the proportion
of 0.01% or more. However, the addition of 5% or more causes a reduction in steel
material cost and also a reduction in weldability. Therefore, when Ni is added, the
content is in the range of 0.01 to 5%. More preferably, the content is 0.01 to 4.5%.
Cr: 0.01 to 3%
[0030] Cr is added as required in order to increase the strength of steel materials through
an improvement of hardenability or an increase in tempering softening resistance.
Such an effect is recognized when Cr is contained in the proportion of 0.01% or more.
In contrast, the addition exceeding 3% reduces weldability and toughness. Therefore,
when Cr is added, the content is in the range of 0.01 to 3%. More preferably, the
content is in the range of 0.01 to 2.5%.
Mo: 0.01 to 2%
[0031] Mo is added as required in order to increase the strength of steel materials through
an improvement of hardenability or an increase in tempering softening resistance.
Such an effect is recognized when Mo is contained in the proportion of 0.01% or more.
In contrast, the addition exceeding 2% reduces weldability or toughness. Therefore,
when Mo is added, the content is in the range of 0.01 to 2%. More preferably, the
content is in the range of 0.01 to 1%.
Nb: 0.1% or lower
[0032] Nb is an element that precipitates as a carbide or a carbonitride in tempering and
increases the strength of steel through precipitation strengthening. Moreover, Nb
also has an effect of pulverizing austenite grains during rolling to increase toughness.
In order to obtain the effects, the content of 0.001% or more is preferable. However,
the content exceeding 0.1% reduces toughness. Therefore, when Nb is added, the content
is 0.1% or lower. More preferably, the content is 0.05% or lower.
V: 0.1% or lower
[0033] V is an element that precipitates as a carbide or a carbonitride in tempering and
increases the strength of steel through precipitation strengthening. Moreover, V also
has an effect of pulverizing austenite grains during rolling to increase toughness.
In order to obtain the effects, the content of 0.001% or more is preferable. However,
the content exceeding 0.1% reduces toughness. Therefore, when Nb is added, the content
is 0.1% or lower. More preferably, the content is 0.05% or lower.
Ti: 0.1% or lower
[0034] Ti is added as required because Ti has an effect of pulverizing austenite in a welded
heat affected zone to increase toughness. In order to obtain the effect, the content
of 0.001% or more is preferable. However, the addition exceeding 0.1% reduces toughness
and also causes a sudden rise of steel material cost. Therefore, when Ti is added,
the content is 0.1% or lower. More preferably, the content is 0.05% or lower.
B: 0.01% or lower
[0035] B is added as required because B has an effect of increasing hardenability and increasing
the strength of steel with a small content thereof. In order to obtain the effect,
the content is preferably 0.0001% or more. However, the addition exceeding 0.01% reduces
weldability. Therefore, when B is added, the content is 0.01% or lower. More preferably,
the content is 0.005% or lower.
Ca: 0.01% or lower
[0036] Ca is added as required because Ca increases the base material toughness by controlling
the shape of a CaS inclusion and further increase the toughness of a welded heat affected
zone. In order to obtain the effects, the content of 0.0001% or more is preferable.
However, the addition exceeding 0.01% reduces toughness due to an increase in the
amount of the CaS inclusion. Therefore, when Ca is added, the content is 0.01% or
lower. More preferably, the content is 0.009% or lower.
REM: 0.1% or lower
[0037] REM is an element that increases the toughness of a welded heat affected zone and
is added as required. In order to obtain the effect, the content is preferably 0.0001%
or more. However, the addition exceeding 0.1% causes a reduction in toughness. Therefore,
when REM is added, the content is 0.1% or lower. More preferably, the content is 0.05%
or lower.
[0038] REM is a general term of Y, Ce and the like that are rare earth elements and the
addition amount as used herein refers to the total amount of these rare earth elements.
[Microstructure]
[0039] The steel material according to the invention has a microstructure in which the structure
at the 1/4 position of the plate thickness contains ferrite and a hard phase, the
area fraction of the hard phase is 50 to 90%, and the average aspect ratio of the
ferrite grain size is 1.5 or more. When the area fraction of the hard phase is lower
than 50% and exceeds 90% or the aspect ratio of the ferrite grain size is lower than
1.5, there is a possibility that ductile crack initiation occurs.
The upper limit of the average aspect ratio of the ferrite grain size does not need
to particularly specify and is 5 or lower in view of the capability and the like of
a rolling mill. The area fraction of the hard phase is more preferably 52 to 90% and
the average aspect ratio of the ferrite grain size is more preferably 1.6 or more.
The average aspect ratio is more preferably 1.7 or more.
[0040] In a two phase mixed structure containing ferrite and a hard phase, the yield ratio(or
Y/T ratio) of a base material decreases, and the strain concentration in a stress
concentration zone is eased even in the base material as it is or even after a simulated
heat cycle of simulating the welded heat affected zone. Such an effect is not obtained
in the case of a single phase of ferrite or a single phase of a hard phase.
[0041] In the steel material according to the invention, the structure of the surface of
a steel plate (1 mm position from the plate surface) contains ferrite and a hard phase,
in which the area fraction of the ferrite exceeds 40% and is more preferably 50% or
more. The average aspect ratio of the ferrite grain size exceeds 2. When the area
fraction of the ferrite is lower than 40% or the average aspect ratio of the ferrite
grain size is 2 or lower, the resistance of ductile crack initiation in a welded heat
affected zone is poor.
[0042] In the invention, the hard phase is bainite, martensite, or a bainite/martensite
mixed structure and contains 5% or lower, in terms of area fraction, of an island
martensite (M-A constituent) (MA).
[0043] Fig. 2 illustrates the results of examining the resistance of ductile crack initiation
using a simulated heat cycle specimen of a welded zone (highest heating temperature
of 1400°C). As illustrated in Fig. 2, when the area fraction of the hard phase of
the base material is 50 to 90% and the average aspect ratio of the ferrite thereof
is 1.5 or more, ductile crack initiation is not observed also after the simulated
heat cycle.
[0044] The results illustrated in Fig. 2 were obtained by specimens of 12 mm thickness (=
plate thickness direction) × 12 mm width × 200 length from the 1/4 center of the plate
thickness (1/2 center of the plate thickness in the case of a plate thickness of 25
mm or lower) from the steel materials obtained by producing steel having a composition
in the range of the invention by various manufacturing methods and changing the microstructure,
and then giving a simulated heat cycle (time for reaching the highest heating temperature:
6 s, cooling rate from the highest heating temperature to room temperature: 40°C/s)
of a welded zone thereto by a Gleeble tester to obtain sample materials.
[0045] Fig. 1 illustrates the specimen shape and the test conditions. The sample material
(specimen 1), to which the simulated heat cycle was given, in which a single through-thickness
edge notch is introduced with the length of 3 mm in the plate thickness direction
into the center of a simulated heat cycle zone 2 of the sample material (specimen
1) was fixed with clamps 5, then a tensile load (arrow 6) was applied to 0.6 mm in
terms of displacement of a clip gage 3 between knife-edges 4 that are screwed, the
load was removed, and then the specimen was ground to the central zone and mirror
polished. Then, the presence of crack initiation at the notch tip was evaluated. The
case where the ductile crack from the notch bottom was 50 µm or more was defined as
crack initiation.
[0046] It is considered that the results illustrated in Fig. 2 are obtained due to the fact
that the yield ratio (or Y/T ratio) (0.2% proof stress/tensile strength) decreased
also in the structure after the simulated heat cycle and the degree of distortion
concentration at the notch tip zone decreased by the use of the base material having
a complex structure of ferrite and a hard phase.
[0047] Such outstanding characteristics were observed in common also in a base material
to which the simulated heat cycle was not given.
More specifically, Fig. 4 illustrates the results of examining the influence of the
microstructure of the base material exerted on the resistance of ductile crack initiation.
As illustrated in Fig. 4, when the area fraction of the hard phase of the base material
is 50 to 90% and the average aspect ratio of the ferrite is 1.5 or more, ductile crack
initiation is not accepted.
The results of the base material illustrated in Fig. 4 were obtained by specimens
of 12 mm thickness (= plate thickness direction) × 12 mm width × 200 length from the
1/4 center of the plate thickness (1/2 center of the plate thickness in the case of
a plate thickness of 25 mm or lower) from steel materials obtained by producing steel
having a composition in the range of the invention by various manufacturing methods
and changing the microstructure.
[0048] Fig. 3 illustrates the specimen shape and the test conditions. The sample material
(specimen 1) in which a single through-thickness edge notch is introduced into the
center was fixed with clamps 5, then a tensile load (arrow 6) was applied to 0.8 mm
in terms of displacement of a clip gage 3 between knife-edges 4 that are screwed,
the load was removed, and then the specimen was ground to the central zone and mirror
polished. Then, the presence of crack initiation at the notch tip was evaluated. The
case where the ductile crack from the notch bottom was 50 µm or more was defined as
crack initiation.
It is considered that the results illustrated in Fig. 4 are obtained due to the fact
that the yield ratio(or Y/T ratio) (0.2% proof stress/tensile strength) decreased
and the degree of distortion concentration at the notch tip zone decreased by the
use of a base material having a complex structure of ferrite and a hard phase.
[0049] Moreover, it is also considered to be one of the factors that the slip plane greatly
leaned to the crack initiation direction in the base material as it is and also after
the simulated heat cycle by increasing the average aspect ratio of the ferrite, i.e.,
the development of the specific aggregate structure. The aspect ratio refers to the
ferrite grain size in the rolling direction (major axis)/the ferrite grain size in
the plate thickness direction (minor axis) in a cross section parallel to the rolling
direction.
[0050] The same results as those of Fig. 2 were obtained also when the highest heating temperature
of the simulated heat cycle was 760°C, 900°C, and 1200°C.
[0051] The steel material according to the invention is obtained by successively subjecting
the steel material of the above-described chemical compositions to a hot rolling process,
a water cooling process, or further a tempering process.
[0052] The hot rolling includes reheating to 1000°C or more and performing rolling in such
a manner that the rolling reduction rate in a temperature range of 900°C or more is
50% or more and the rolling finish temperature becomes Ar
3 to Ar
3-50°C. A more preferable rolling finish temperature is lower than Ar
3 to Ar
3-40°C. By setting the rolling finish temperature in the invention range, processing
strain(or residual strain) can be added to ferrite generated during rolling to thereby
increase the aspect ratio of the ferrite. When the reheating temperature is lower
than 1000°C, hot rolling that gives a desired cumulative rolling reduction rate cannot
be performed to the steel material.
[0053] When the cumulative rolling reduction rate at 900°C or more is lower than 50%, desired
strength and toughness cannot be secured. When the rolling finish temperature exceeds
Ar
3, the aspect ratio of ferrite does not reach 1.5 or more. When the rolling finish
temperature is lower than Ar
3-50°C, the area fraction of the hard phase obtained by the subsequent water cooling
does not reach 50% or more.
[0054] In the water cooling process, the water cooling is started at Ar
3-10°C to Ar
3-70°C immediately after hot rolling, and then the water cooling is terminated at 500°C
or lower. When the water cooling start temperature exceeds Ar
3-10°C, ferrite of lower than 10% in terms of area fraction (hard phase exceeding 90%
in terms of area fraction) precipitates. When the water cooling start temperature
is lower than Ar
3-70°C or water cooling is not started immediately after (within 300 seconds) hot rolling,
ferrite exceeding 50% in terms of area fraction (hard phase not reaching 50% in terms
of area fraction) or pearlite, which is not intended to precipitate in the invention,
precipitates. Thus, desired characteristics cannot be satisfied.
[0055] After performing the cooling, tempering treatment can be further performed at a temperature
of lower than the Ac
1 point. By performing tempering treatment, toughness and ductility increase, and desired
strength and toughness can be achieved. When the tempering temperature exceeds the
Ac
1 point, a large amount of island martensite generates to reduce the toughness.
[0056] The Ar
3 point and the Ac
1 point can be calculated by the following equation based on the content (% by mass)
of each chemical composition.

Hereinafter, the invention will be described in more detail based on Examples.
[EXAMPLES]
[0057] Steel materials containing the chemical compositions shown in Table 1 were subjected
to hot rolling at the conditions shown in Table 2 to thereby obtain steel plates having
a plate thickness of 12 to 100 mm.
[0058] The obtained steel plates were subjected to microstructure observation, a tensile
test, a toughness test, a ductile crack initiation test after a simulated heat cycle,
and a ductile crack initiation test of base materials. The test methods were performed
as described in the following items (1) to (5).
(1) Microstructure observation
[0059] From the obtained steel plates, specimens were extracted in the cross section parallel
to the rolling direction. Then, the specimens were mirror polished, and then etched
with nital. Thereafter, the microstructure at the 1/4 position of the plate thickness
and the microstructure 1 mm below the surface were observed. The observation of each
of the positions was performed with Field number: 20 fields of view. The area fraction
was determined by binarizing the ferrite and the hard phase and observing at a magnification
of 200x. The average aspect ratio of the ferrite was determined by determining the
length in the rolling direction and the length in the plate thickness direction of
each ferrite present in the field of view at a magnification of 400x, determining
the length in the rolling direction/the length in the plate thickness direction, and
then determining the average value thereof.
(2) Tensile test
[0060] From the obtained steel plates, full thickness JIS No. 5 specimens were extracted
so that the tensile direction was perpendicular to the rolling direction of the steel
plate according to the regulation of JIS Z 2201 (1998). The tensile test was performed
according to JIS Z 2241 (1998), and then the 0.2% proof (σ0.2) and the tensile strength
(TS) were determined to evaluate the static tensile properties.
(3) Toughness test
[0061] From the obtained steel plates, V notch specimens were extracted so that the longitudinal
direction was in parallel to the rolling direction according to the regulation of
JIS Z 2242 (2005), and then the ductile-brittle fracture transition temperature was
determined to evaluate the toughness. The specimens were extracted in such a manner
that the 1/4 position of the plate thickness when the plate thickness was 20 mm or
more or the 1/2 position of the plate thickness when the plate thickness was lower
than 20 mm was the center.
(4) Ductile crack initiation test after simulated heat cycle
[0062] From the obtained steel plates, specimens of 12 mm thickness (= plate thickness direction
= t) × 12 mm width and 200 mm in full length were extracted at the 1/4 center of the
plate thickness (1/2 center of the plate thickness when the plate thickness was 25
mm or lower). The specimens were subjected to a simulated heat cycle of a welded heat
affected zone in which the highest heating temperature was 760°C, 900°C, 1200°C, and
1400°C (time for reaching the highest heating temperature: 6s, Cooling rate from the
highest heating temperature to room temperature: 40°C/s) using a Gleeble tester.
Thereafter, as illustrated in Fig. 1, a single through-thickness edge notch was introduced
with the length of 3 mm in the plate thickness direction into the center of the simulated
heat cycle zone. The notch processing was carried out by electrical discharge machining,
and the notch tip radius was 0.1 mm.
In the test, a tensile load was applied while gripping the specimens with both right
and left ends thereof with a constraint length of 50 mm. During the test, the displacement
between the knife-edges screwed near the notch was measured with the clip gage. A
tensile load was applied to 0.6 mm in terms of clip gage displacement, and then the
load was removed. Thereafter, the specimen was ground to the width center and mirror
polished. Then, the crack initiation state at the notch bottom was analyzed under
a microscope with a magnification of 50x. It was defined that the ductile crack initiation
occurred when a ductile crack extended in the length of 50 µm or more from the notch
bottom.
(5) Ductile crack initiation test of base material
[0063] From the obtained steel plates, specimens of 12 mm thickness (= plate thickness direction
= t) × 12 mm width and 200 mm in full length were extracted at the 1/4 center of the
plate thickness (1/2 center of the plate thickness when the plate thickness was 25
mm or lower).
To the obtained specimens, a single through-thickness edge notch was introduced with
the length of 3 mm in the plate thickness direction into the center of the specimens
as illustrated in Fig. 3. The notch processing was carried out by electrical discharge
machining, and the notch tip radius was 0.1 mm.
In the test, a tensile load was applied while gripping the specimens with both right
and left ends thereof with a constraint length of 50 mm. During the test, the displacement
between the knife-edges screwed near the notch was measured with the clip gage. A
tensile load was applied to 0.8 mm in terms of clip gage displacement, and then the
load was removed. Thereafter, the test was ground to the width center and mirror polished.
Then, the crack initiation state at the notch bottom was analyzed under a microscope
with a magnification of 50x. It was defined that the ductile crack initiation occurred
when a ductile crack extended in the length of 50 µm or more from the notch bottom.
[0064] With respect to the specimens that were subjected to the simulated heat cycle, the
obtained experimental results are shown in Table 3. All of the steel plates of Nos.
1 to 10 produced using the chemical compositions and the manufacturing method specified
in the invention have the structure specified in the invention. It is found that the
steel plates have excellent strength and toughness and have excellent resistance of
ductile crack initiation of a welded heat affected zone.
In contrast, the steel plate (Steel type K*) of No. 11 in which the C content does
not satisfy the lower limit of the range of the invention has low tensile strength.
The steel plate (Steel type L*) of No. 12 in which the content of each of C, P, and
S exceeds the upper limit of the range of the invention has low toughness and has
poor ductile crack initiation characteristics of a welded heat affected zone.
The steel plate of No. 13 in which the reheating temperature of slab is lower than
the invention and the cumulative rolling reduction rate at 900°C or more is outside
the range of the invention has low toughness. In the steel plate of No. 14 in which
the rolling finish temperature and the water cooling start temperature exceed the
range of the invention, ferrite is not generated, the microstructure specified in
the invention is not obtained, and the resistance of ductile crack initiation of a
welded heat affected zone is poor.
In the steel plate of No. 15 in which the cooling start temperature is lower than
the range of the invention and the steel plate of No. 16 in which the water cooling
stop temperature exceeds the range of the invention, the hard phase area fraction
and the average aspect ratio of ferrite do not satisfy the values specified in the
invention and both the steel plates have low tensile strength and have poor resistance
of ductile crack initiation of welded heat affected zones. In the steel plate of No.
17 in which the tempering temperature exceeds the range of the invention, since a
large amount of island martensite is generated, the toughness is low and the resistance
of ductile crack initiation of a welded heat affected zone is poor.
[0065] The obtained experimental results of the base material are shown in Table 4. All
of the steel plates of Nos. 18 to 27 produced using the chemical compositions and
the manufacturing method specified in the invention have the structure specified in
the invention. It is recognized that the steel plates have excellent strength and
toughness and have excellent resistance of ductile crack initiation of a welded heat
affected zone. In contrast, the steel plate (Steel type W*) of No. 28 in which the
C content does not satisfy the lower limit of the range of the invention has low tensile
strength. The steel plate (Steel type X*) of No. 29 in which the content of each of
C, P, and S exceeds the upper limit of the range of the invention has low toughness.
The steel plate of No. 30 in which the reheating temperature of slab is lower than
the range of the invention and the cumulative rolling reduction rate at 900°C or more
does not satisfy the range of the invention has low toughness.
In the steel plate of No. 31 in which the rolling finish temperature and the water
cooling start temperature exceed the range of the invention, ferrite is not generated,
the microstructure specified in the invention is not obtained, and the resistance
of ductile crack initiation is poor.
In the steel plate of No. 32 in which the cooling start temperature is lower than
the range of the invention and the steel plate of No. 33 in which the water cooling
stop temperature exceeds the range of the invention, the hard phase area fraction
and the average aspect ratio of ferrite do not satisfy the values specified in the
invention and both the steel plates have low tensile strength and have poor resistance
of ductile crack initiation. In the steel plate of No. 34 in which the tempering temperature
exceeds the value of the invention, a large amount of island martensite (M-A constituent)
is generated, and thus the toughness is low and the resistance of ductile crack initiation
is poor.
Reference Signs List
[0066]
- 1. Specimen
- 2. Simulated heat cycle zone
- 3. Clip gage
- 4. Knife-edge
- 5. Clamp
- 6. Tensile load
[0067] [Table 1]
Table 1
|
Chemical composition (mass%) |
Ar3 [°C] Note (1) |
Ac1 [°C] Note (2) |
Steel type |
C |
Si |
Mn |
P |
S |
Cu |
Ni |
Cr |
Mo |
Nb |
V |
Ti |
B |
Ca |
REM |
Al |
N |
A |
0.14 |
0.33 |
1.59 |
0.005 |
0.002 |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.033 |
0.0048 |
739 |
729 |
B |
0.06 |
0.11 |
1.96 |
0.009 |
0.001 |
0.25 |
0.14 |
0.04 |
0.21 |
0.046 |
0.005 |
0.011 |
0.0003 |
- |
- |
0.032 |
0.0042 |
705 |
697 |
C |
0.18 |
0.04 |
1.16 |
0.006 |
0.005 |
- |
- |
- |
- |
- |
0.048 |
- |
- |
- |
- |
0.044 |
0.0029 |
761 |
708 |
D |
0.12 |
0.39 |
0.54 |
0.008 |
0.003 |
- |
- |
0.22 |
0.35 |
- |
- |
- |
- |
- |
0.097 |
0.029 |
0.0041 |
798 |
729 |
E |
0.03 |
0.26 |
0.52 |
0.003 |
0.005 |
- |
4.49 |
- |
- |
0.012 |
- |
0.049 |
- |
- |
- |
0.018 |
0.0029 |
612 |
657 |
F |
0.09 |
0.31 |
1.32 |
0.042 |
0.007 |
0.98 |
1.33 |
- |
- |
0.022 |
0.015 |
- |
- |
0.0089 |
0.031 |
0.022 |
0.0031 |
684 |
692 |
G |
0.08 |
0.24 |
1.18 |
0.002 |
0.009 |
0.98 |
- |
2.48 |
0.98 |
0 |
0.018 |
- |
- |
- |
- |
0.025 |
0.0028 |
675 |
770 |
H |
0.11 |
0.18 |
1.22 |
0.001 |
0.004 |
- |
0.52 |
0.16 |
0.21 |
0.015 |
0.033 |
0.017 |
0.0046 |
- |
- |
0.018 |
0.0035 |
731 |
706 |
I |
0.05 |
0.32 |
1.38 |
0.002 |
0.043 |
- |
2.43 |
- |
0.25 |
0.033 |
0.019 |
- |
- |
0.0033 |
0.044 |
0.022 |
0.0028 |
630 |
676 |
J |
0.09 |
0.25 |
1.44 |
0.005 |
0.002 |
- |
- |
0.08 |
0.11 |
0.022 |
0.038 |
0.013 |
0.0011 |
- |
- |
0.032 |
0.0041 |
757 |
710 |
K* |
0.1* |
0.21 |
1.56 |
0.004 |
0.003 |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.028 |
0.0039 |
782 |
706 |
L* |
0.32* |
0.18 |
0.55 |
0.193* |
0.183* |
- |
0.15 |
0.23 |
0.14 |
- |
- |
- |
- |
0.0022 |
0.008 |
0.022 |
0.0038 |
739 |
722 |
M |
0.15 |
0.32 |
1.58 |
0.006 |
0.001 |
0.25 |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.032 |
0.0048 |
737 |
729 |
N |
0.06 |
0.12 |
1.95 |
0.008 |
0.004 |
- |
0.15 |
0.02 |
0.21 |
0.045 |
0.004 |
0.012 |
0.0002 |
- |
- |
0.031 |
0.0041 |
706 |
697 |
O |
0.19 |
0.02 |
1.15 |
0.005 |
0.005 |
0.22 |
- |
- |
- |
- |
0.047 |
- |
- |
- |
- |
0.048 |
0.0029 |
759 |
707 |
P |
0.11 |
0.38 |
0.52 |
0.007 |
0.003 |
- |
- |
0.21 |
0.33 |
- |
- |
- |
- |
- |
0.098 |
0.028 |
0.0042 |
85 |
729 |
Q |
0.03 |
0.25 |
0.51 |
0.003 |
0.004 |
- |
4.51 |
- |
- |
0.018 |
- |
0.048 |
- |
- |
- |
0.016 |
0.0028 |
612 |
656 |
R |
0.08 |
0.31 |
1.33 |
0.041 |
0.006 |
- |
1.26 |
- |
- |
0.025 |
0.011 |
- |
- |
0.0091 |
0.032 |
0.017 |
0.0041 |
691 |
693 |
S |
0.09 |
0.20 |
1.14 |
0.003 |
0.004 |
0.95 |
- |
2.45 |
0.97 |
- |
0.009 |
- |
- |
- |
- |
0.022 |
0.0032 |
677 |
769 |
T |
0.12 |
0.16 |
1.25 |
0.004 |
0.003 |
- |
0.55 |
0.15 |
0.22 |
0.043 |
0.032 |
0.018 |
0.0048 |
- |
- |
0.011 |
0.0035 |
723 |
705 |
U |
0.05 |
0.27 |
1.37 |
0.001 |
0.042 |
- |
2.42 |
- |
0.28 |
0.032 |
0.019 |
- |
- |
0.0032 |
0.048 |
0.023 |
0.0028 |
629 |
675 |
V |
0.09 |
0.22 |
1.44 |
0.003 |
0.003 |
- |
- |
0.07 |
0.15 |
0.028 |
0.042 |
0.012 |
0.0015 |
- |
- |
0.032 |
0.0041 |
754 |
709 |
W* |
0.01* |
0.25 |
1.55 |
0.005 |
0.004 |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.031 |
0.0039 |
783 |
707 |
X* |
0.31* |
0.15 |
0.51 |
0.180* |
0.173* |
0.23 |
0.11 |
0.21 |
0.15 |
- |
- |
- |
- |
0.0021 |
0.011 |
0.028 |
0.0037 |
747 |
722 |
Note: The cells marked by * are outside the range of the invention and the steel types
K, L, W, and X are comparative steels.
Note (1): Ar3(°C) = 910 - 310C - 80 Mn - 20 Cu - 15 Cr - 55 Ni - 80 Mo Each alloy
element amount indicates the content (%)
Note (2): Ar1(° C) = 723 - 1 Mn + 22 Si - 14.4 Ni + 13.3 Cr Each alloy element amount
indicates the content (%) |
[0068] [Table 2]
Table 2
No. |
Steel type |
Plate thickness (mm) |
Slab reheating temperature [°C] |
Cumulative rolling reduction rate at 900°C or more [%] |
Rolling finish temperature [°C] |
Water cooling start temperature [°C] |
Water cooling stop temperature [°C] |
Tempering temperature [°C] |
1 |
A |
14 |
1160 |
87 |
702 |
683 |
431 |
- |
2 |
B |
22 |
1190 |
75 |
679 |
665 |
378 |
- |
3 |
C |
12 |
1210 |
92 |
731 |
687 |
298 |
- |
4 |
D |
100 |
1150 |
56 |
782 |
779 |
421 |
- |
5 |
E |
75 |
1240 |
62 |
583 |
578 |
72 |
620 |
6 |
F |
35 |
1190 |
73 |
672 |
634 |
388 |
- |
7 |
G |
24 |
1150 |
81 |
641 |
623 |
28 |
580 |
8 |
H |
68 |
1240 |
55 |
701 |
687 |
426 |
- |
9 |
1 |
34 |
1170 |
72 |
607 |
598 |
426 |
- |
10 |
J |
18 |
1160 |
82 |
718 |
704 |
388 |
- |
11 |
K* |
22 |
1120 |
78 |
748 |
726 |
315 |
- |
12 |
L* |
45 |
1180 |
68 |
725 |
706 |
248 |
- |
13 |
C |
73 |
970* |
34* |
741 |
732 |
42 |
650 |
14 |
A |
14 |
1160 |
87 |
785* |
777* |
413 |
- |
15 |
B |
28 |
1230 |
72 |
695 |
600* |
388 |
- |
16 |
J |
19 |
1240 |
78 |
712 |
699 |
638* |
- |
17 |
D |
75 |
1090 |
64 |
768 |
749 |
62 |
760* |
18 |
M |
15 |
1150 |
86 |
695 |
681 |
401 |
- |
19 |
N |
20 |
1180 |
76 |
686 |
664 |
308 |
- |
20 |
O |
12 |
1200 |
91 |
721 |
697 |
498 |
- |
21 |
P |
100 |
1130 |
55 |
792 |
777 |
418 |
- |
22 |
Q |
75 |
1250 |
61 |
602 |
589 |
25 |
600 |
23 |
R |
35 |
1200 |
72 |
668 |
643 |
418 |
- |
24 |
S |
25 |
1160 |
73 |
647 |
625 |
72 |
500 |
25 |
T |
72 |
1250 |
58 |
708 |
697 |
457 |
- |
26 |
U |
37 |
1170 |
71 |
618 |
605 |
412 |
- |
27 |
V |
15 |
1150 |
83 |
723 |
703 |
378 |
- |
28 |
W* |
25 |
1100 |
84 |
758 |
748 |
258 |
- |
29 |
X* |
48 |
1200 |
69 |
721 |
710 |
243 |
- |
30 |
O |
75 |
930* |
33* |
737 |
717 |
23 |
600 |
31 |
M |
15 |
1150 |
88 |
755* |
747* |
428 |
- |
32 |
N |
25 |
1220 |
71 |
679 |
605* |
352 |
- |
33 |
V |
18 |
1250 |
77 |
715 |
703 |
658* |
- |
34 |
P |
77 |
1080 |
62 |
776 |
748 |
245 |
750* |
Note: The steel types marked by * are outside the range of the invention. |
[0069] [Table 3]
Table 3
No. |
Microstructure of 1/4 Plate thickness/4 |
Microstructure 1 mm below the surface |
σ0.2 [MPa] |
TS [MPa] |
vTrs [°C] |
Ductile crack initiation characteristics Note (2) |
Classification |
Hard phase structure Note (1) |
Hard phase fraction [%] |
Ferrite average aspect ratio |
Hard phase structure Note (1) |
Ferrite phase fraction [%] |
Ferrite average aspect ratio |
760°C |
900°C |
1200°C |
1400°C |
1 |
B |
59 |
1.9 |
B |
55 |
2.4 |
428 |
548 |
-57 |
○ |
○ |
○ |
○ |
Present invention example |
2 |
B |
75 |
2.2 |
B |
68 |
3.1 |
563 |
728 |
-105 |
○ |
○ |
○ |
○ |
Present invention example |
3 |
B,M |
54 |
2.3 |
B,M |
77 |
4.8 |
521 |
689 |
-33 |
○ |
○ |
○ |
○ |
Present invention example |
4 |
B |
64 |
1.6 |
B |
48 |
2.2 |
408 |
521 |
-29 |
○ |
○ |
○ |
○ |
Present invention example |
5 |
TB |
90 |
1.7 |
TM |
41 |
2.6 |
555 |
667 |
-98 |
○ |
○ |
○ |
○ |
Present invention example |
6 |
B |
62 |
1.8 |
B |
59 |
2.3 |
473 |
621 |
-47 |
○ |
○ |
○ |
○ |
Present invention example |
7 |
TM |
55 |
2.1 |
TM |
72 |
2.4 |
481 |
582 |
-92 |
○ |
○ |
○ |
○ |
Present invention example |
8 |
B |
83 |
1.8 |
B |
42 |
2.1 |
529 |
683 |
-64 |
○ |
○ |
○ |
○ |
Present invention example |
9 |
B |
87 |
1.7 |
B |
40 |
2.2 |
433 |
538 |
-41 |
○ |
○ |
○ |
○ |
Present invention example |
10 |
B |
75 |
2.5 |
M |
58 |
3.3 |
428 |
548 |
-72 |
○ |
○ |
○ |
○ |
Present invention example |
11 |
B |
73 |
2.2 |
B |
53 |
3.0 |
325 |
421* |
-18 |
○ |
○ |
○ |
○ |
Comparative example |
12 |
B,M |
72 |
1.7 |
B,M |
43 |
2.3 |
677 |
991 |
15* |
○ |
× |
× |
× |
Comparative example |
13 |
TM |
72 |
2.3 |
TM |
40 |
2.5 |
521 |
609 |
8* |
○ |
○ |
○ |
○ |
Comparative example |
14 |
B |
100* |
- |
B |
0* |
-* |
548 |
678 |
-21 |
× |
× |
× |
× |
Comparative example |
15 |
P |
14* |
1.1* |
P |
87 |
1.4* |
344 |
472* |
-11 |
× |
× |
× |
× |
Comparative example |
16 |
P |
21* * |
1.3* |
P |
81 |
1.4* |
388 |
488* |
-18 |
× |
× |
× |
× |
Comparative example |
17 |
B,MA |
63 |
1.8 |
M,MA |
48 |
2.8 |
521 |
622 |
6* |
× |
× |
× |
× |
Comparative example |
Note: The cells marked by * are outside the range of the invention.
Note (1): B: Bainite., M:Martensite, P: Pearlite, TB: Tempered bainite, TM: Tempered
martensite, MA: Island martensite
Note (2): ○: No ductile crack initiation × : Ductile crack initiation |
[0070] [Table 4]
Table 4
No. |
Microstructure of 1/4 Plate thickness |
Microstructure 1 mm below the surface |
σ0.2 [MPa] |
TS [MPa] |
vTrs [°C] |
Ductile crack initiation characteristics Note (2) |
Classification |
Hard phase structure Note (1) |
Hard phase fraction [%] |
Ferrite average aspect ratio |
Hard phase structure Note (1) |
Ferrite phase fraction [%] |
Ferrite average aspect ratio |
18 |
B |
55 |
1.8 |
B |
57 |
3.1 |
436 |
528 |
-48 |
○ |
Present invention example |
19 |
B |
72 |
2.1 |
B |
42 |
4.9 |
573 |
726 |
-121 |
○ |
Present invention example |
20 |
B,M |
52 |
2.2 |
B,M |
66 |
3.9 |
511 1 |
698 |
-21 |
○ |
Present invention example |
21 |
B |
62 |
1.6 |
B |
48 |
2.2 |
359 |
515 |
-28 |
○ |
Present invention example |
22 |
TB |
89 |
1.8 |
TM |
41 |
4.1 |
552 |
628 |
-111 |
○ |
Present invention example |
23 |
B |
68 |
1.9 |
B |
49 |
2.8 |
487 |
615 |
-35 |
○ |
Present invention example |
24 |
TM |
59 |
2.0 |
TM |
57 |
3.1 |
472 |
577 |
-98 |
○ |
Present invention example |
25 |
B |
84 |
1.6 |
B |
42 |
2.7 |
507 |
641 |
-63 |
○ |
Present invention example |
26 |
B |
88 |
1.7 |
B |
43 |
2.9 |
402 |
513 |
-34 |
○ |
Present invention example |
27 |
B |
77 |
2.4 |
B |
53 |
3.3 |
425 |
538 |
-66 |
○ |
Present invention example |
28 |
B |
74 |
2.1 |
M |
58 |
3.7 |
368 |
411 * |
-38 |
○ |
Comparative example |
29 |
B,M |
78 |
1.8 |
M |
55 |
2.2 |
687 |
983 |
10* |
○ |
Comparative example |
30 |
TM |
69 |
2.4 |
TM |
42 |
2.4 |
513 |
618 |
7* |
○ |
Comparative example |
31 |
B |
100* |
- |
B |
0* |
-:* |
558 |
688 |
-18 |
○ |
Comparative example |
32 |
P |
12* |
1.2* |
P |
89 |
1.4* |
358 |
451 * |
-13 |
× |
Comparative example |
33 |
P |
18* |
1.4* |
P |
83 |
1.4* |
398 |
473* |
-21 |
× |
Comparative example |
34 |
B,MA |
68 |
1.7 |
M,MA |
44 |
2.8 |
535 |
637 |
5* |
× |
Comparative example |
Note: The cells marked by * are outside the range of the invention.
Note (1): B: Bainite., M : Martensite, P: Pearlite, TB: Tempered bainite, TM: Tempered
martensite, MA: Island martensite
Note (2): ○ : No ductile crack initiation × : Ductile crack initiation |