Specification
DESCRIPTION
TITLE OF INVENTION: Fe-BASED METAL SHEET AND
MANUFACTURING METHOD THEREOF
TECHNICAL FIELD
[0001] The present invention relates to an Fe-based
metal sheet having a high accumulation degree of
{200} planes suitably used for magnetic cores and the
like of electric motors, power generators, and
transformers and capable of contributing to
downsizing of these magnetic cores and reduction in
energy loss, and a manufacturing method thereof.
This application is based upon and claims the benefit
of priority of the prior Japanese Patent Application
No. 2011-100014, filed on April 27, 2011, the prior
Japanese Patent Application No. 2011-101893, filed on
April 28, 2011, and the prior Japanese Patent
Application No. 2012-070166, filed on March 26, 2012,
the entire contents of which are incorporated herein
by reference.
BACKGROUND ART
[0002] Electrical steel sheets alloyed with silicon
or/and the like have been conventionally used for
magnetic cores of electric motors, power generators,
transformers, and the like. Among electrical steel
sheets, non-oriented electrical steel sheets having
relatively random crystal orientations can be
manufactured at a low cost, to thus be used for
motors, transformers, and the like of home electric
appliances, and the like in a multipurpose manner.
- 1 -
The crystal orientations of this non-oriented
electrical steel sheet are random, thus making it
impossible to obtain a high magnetic flux density.
In contrast to this, grain-oriented electrical steel
sheets having aligned crystal orientations can obtain
a high magnetic flux density, to thus be applied to
high-end use for driving motors and the like of HV
vehicles and the like. However, in a manufacturing
method of a grain-oriented electrical steel sheet
that is industrialized currently, a long-time heat
treatment is required, to thus increase the cost.
[0003] As above, in the non-oriented electrical
steel sheet, a sufficiently high magnetic flux
density cannot be obtained, and in the grain-oriented
electrical steel sheet, the direction in which a high
magnetic flux density can be obtained is limited to
one to two direction/directions. On the other hand,
in HV vehicles, and the like, achievement of high
torque and downsizing are required, and there is a
demand for manufacturing a metal sheet capable of
obtaining a high magnetic flux density in an in-plane
circumferential direction thoroughly as a metal sheet
to be used for core materials of driving motors, and
the like. Thus, as methods other than the
industrialized manufacturing method of the grainoriented
electrical steel sheet, there have been
proposed a technique of increasing an accumulation
degree of a specific crystal orientation and various
techniques of decreasing a core loss. However, in
- 2
the technique described in Patent Literature 7, for
example, it is possible to increase an accumulation
degree of {200} planes, but directionality to a
specific orientation occurs, to thus have a high
magnetic flux density in a specific direction, but a
high magnetic flux density cannot be obtained in an
in-plane circumferential direction thoroughly, and
the like, resulting in that in a conventional
technique, satisfactory properties are not
necessarily obtained.
CITATION LIST
PATENT LITERATURE
[0004] Patent Literature 1: Japanese Laid-open
Patent Publication No. 10-168542
Patent Literature 2: Japanese Laid-open Patent
Publication No. 2006-45613
Patent Literature 3: Japanese Laid-open Patent
Publication No. 2006-144116
Patent Literature 4: Japanese Laid-open Patent
Publication No. 10-180522
Patent Literature 5: Japanese Laid-open Patent
Publication No. 01-252727
Patent Literature 6: Japanese Laid-open Patent
Publication No. 07-173542
Patent Literature 7: International Publication
Pamphlet No. WO2011/052654
SUMMARY OF INVENTION
TECHNICAL PROBLEM
[0005] Thus, an object of the present invention is
- 3 -
to provide an Fe-based metal sheet that is likely to
become magnetized in a sheet plane and further has a
texture capable of obtaining a high magnetic flux
density thoroughly in an in-plane circumferential
direction, and a manufacturing method thereof.
SOLUTION TO PROBLEM
[0006] The present inventors, as a result of earnest
examination, found that an orientation ratio to a
specific orientation is controlled with respect to an
Fe-based metal of an iron sheet or the like, and
thereby a <100> orientation in aFe is more densely
and thoroughly distributed in a metal sheet plane to
make it possible to obtain a high magnetic flux
density thoroughly in an in-plane circumferential
direction.
[0007] Further, the present inventors conceived that
in order to manufacture such an Fe-based metal sheet,
a texture in which an accumulation degree of {100}
planes is increased is first formed in a surface
layer portion, and at the time of y-a transformation
by the subsequent heat treatment, the texture is
transformed while taking over its {100} texture.
Then, they earnestly examined a method of forming the
{100} texture in the surface layer portion and
achievement of high accumulation of {200} planes
using the y-a transformation.
[0008] As a result, it was found that when the Febased
metal sheet is manufactured from a slab by
rolling, a rolling temperature and a reduction ratio
- 4 -
are optimized, thereby making it possible to form the
{100} texture in at least the surface layer portion.
Then, it was found that when the {100} texture in the
surface layer portion is taken over by using the y - a
transformation thereafter, a different metal except
Fe is made to diffuse beforehand from the surface and
a diffused region is turned into an a-Fe phase, and
thereby in the region turned into the a-Fe phase, the
{100} texture is formed, and at the time of the 7-a
transformation, an accumulation degree of {200}
planes in the a-Fe phase further generated by the .
transformation increases and the <100> orientation is
distributed more densely and thoroughly, thereby
making it possible to obtain a high magnetic flux
density in the in-plane circumferential direction
thoroughly.
[0009] Further, the present inventors found that in
the case of a large amount of C content being
contained, when the C content is decreased by
decarburization annealing, the decarburization
annealing is performed under predetermined conditions,
thereby also making it possible to form the {100}
texture in at least the surface layer portion, and in
the Fe-based metal sheet obtained finally, the <100>
orientation is distributed more densely and
thoroughly, thereby making it possible to obtain a
high magnetic flux density in the in-plane
circumferential direction thoroughly.
[0010] The gist of the present invention made as a
- 5 -
result of such examinations is as follows.
[0011] (1) An Fe-based metal sheet, includes: at
least one. type of ferrite-forming element except Fe,
in which when intensity ratios of respective
{001}<470>, {116}<6 12 1>, and {223}<692> directions
in a sheet plane by X-ray diffraction are set to A, B,
and C respectively and Z = (A + 0.97B)/0.98C is
satisfied, a Z value is not less than 2.0 nor more
than 200.
(2) The Fe-based metal sheet according to (1), in
which the ferrite-forming element diffuses from a
surface to be alloyed with Fe.
(3) The Fe-based metal sheet according to (1) or
(2), in which a layer containing the ferrite-forming
element is formed on at least one side of surfaces of
the Fe-based metal sheet, and the ferrite-forming
element that has diffused from part of the layer is
alloyed with Fe.
(4) The Fe-based metal sheet according to (3), in
which a thickness of the layer containing the
ferrite-forming element is not less than 0.01 ju m nor
more than 500 ^m.
(5) The Fe-based metal sheet according to any one
of (1) to (4), in which an accumulation degree of
{200} planes is not less than 30% nor more than 99%,
and an accumulation degree of {222} planes is not
less than 0.01% nor more than 30%.
(6) The Fe-based metal sheet according to any one
of (1) to (5), in which the ferrite-forming element
- 6 -
is one type of element or more selected from a group
consisting of Al, Cr, Ga, Ge, Mo, Sb, Si, Sn, Ta, Ti,
V, W, and Zn.
(7) The Fe-based metal sheet according to any one
of (1) to (6), in which at least a partial region
including the surfaces of the Fe-based metal sheet is
an a single phase region made of an a single phase
based component, and a ratio of the a single phase
region to a cross section of the Fe-based metal sheet
is 1% or more.
(8) The Fe-based metal sheet according to any one
of (1) to (7), in which a thickness of the Fe-based
metal sheet is not less than 10 nm nor more than 6 mm,
(9) The Fe-based metal sheet according to any one
of (1) to (8), in which the a single phase region is
formed on a front surface side and a rear surface
side of the Fe-based metal sheet, and a crystal grain
straddling the a single phase region on the front
surface side and the a single phase region on the
rear surface side is formed.
[0012] (10) A manufacturing method" of an Fe-based
metal sheet, includes:
performing hot rolling on a cast slab containing
C: less than 0.02 mass% and made of an Fe-based metal
of an a-y transforming component at a temperature of
an A3 point of the cast slab or higher to obtain a
hot-rolled sheet;
performing a-region rolling on the hot-rolled
sheet at a temperature of higher than 300*0 and lower
- 7 -
than the A3 point of the cast slab to obtain a rolled
sheet;
performing cold rolling on the rolled sheet to
obtain a base metal sheet having a thickness of not
less than 10 /z m nor more than 6 ram;
bonding a ferrite-forming element to one surface
or both surfaces of the base metal sheet;
heating the base metal sheet having had the
ferrite-forming element bonded thereto up to an A3
point of the base metal sheet; and
further heating the heated base metal sheet to a
temperature of not lower than the A3 point of the
base metal sheet nor higher than ISOO'C and holding
the base metal sheet; and
cooling the heated and held base metal sheet to a
temperature of lower than the A3 point of the base
metal sheet.
(11) The manufacturing method of the Fe-based
metal sheet according to (10), in which a reduction
ratio in the a-region rolling is -1.0 or less in
terms of true strain, and the sum of the reduction
ratio in the a-region rolling and a reduction ratio
in the cold rolling is -2.5 or less in terms of true
strain.
(12) The manufacturing method of the Fe-based
metal sheet according to (10) or (11), in which
a reduction ratio in the hot rolling is -0.5 or
less in terms of true strain.
[0013] (13) A manufacturing method of an Fe-based
- 8 -
metal sheet, includes:
heating a steel sheet containing C: not less than
0.02 mass% nor more than 1.0 mass%, having a
thickness of not less than 10 ju m nor more than 6 mm,
and made of an Fe-based metal of an a-y transforming
component to a temperature of an Al point or higher
and a temperature at which a structure is turned into
an a single phase when decarburization is performed
until C becomes less than 0.02 mass%, to obtain a
base metal sheet that has been subjected to
decarburization in a range of not less than 5 urn nor
more than 50 fim. in a depth direction from its surface
until C becomes less than 0.02 mass%;
bonding a ferrite-forming element to one surface
or both surfaces of the base metal sheet;
heating the base metal sheet having had the
ferrite-forming element bonded thereto up to an A3
point of the base metal sheet; and
further heating the heated base metal sheet to a
temperature of not lower than the A3 point of the
base metal sheet nor higher than 1300*0 and holding
the base metal sheet; and
cooling the heated and held base metal sheet to a
temperature of lower than the A3 point of the base
metal sheet.
(14) The manufacturing method of the Fe-based
metal sheet according to (13), in which the steel
sheet made of the Fe-based metal further contains Mn
of 0.2 mass% to 2.0 mass%, and decarburization and
- 9 -
demanganization are performed in a combined manner.
(15) The manufacturing method of the Fe-based
metal sheet according to (13) or (14), further
includes:
performing carburization on a steel sheet
containing C: less than 0.02 mass%, having a sheet
thickness of not less than 10 iim nor more than 6 mm,
and made of an Fe-based metal of an a-y transforming
component to control C to not less than 0.02 mass%
nor more than 1.0 mass%.
ADVANTAGEOUS EFFECTS OF INVENTION
[0014] According to the present invention, it is
possible to manufacture an Fe-based metal sheet
capable of obtaining a high magnetic flux density
thoroughly in an in-plane circumferential direction.
BRIEF DESCRIPTION OF DRAWINGS
[0015] [Fig. 1] Fig. 1 is a view for explaining a
method of calculating an average magnetic flux
density B50;
[Fig. 2] Fig. 2 is a conceptual diagram showing
the relationship between a Z value and a ratio B50/Bs
of the average magnetic flux density B50 to a
saturation magnetic flux density Bs and a magnetic
flux density difference A B ;
[Fig, 3A] Fig. 3A is s view schematically
showing a structure of a cross section of a base
metal sheet having a {100} texture formed in a
surface layer portion;
[Fig. 33] Fig. 3B is a view schematically
- 10 -
showing the structure of the cross section of the
base metal sheet having a different metal layer
formed in the surface layer portion;
[Fig. 3C] Fig. 3C is a view schematically
showing the structure of the cross section of the
base metal sheet in a temperature increasing process;
[Fig. 3D] Fig. 3D is a view schematically
showing the structure of the cross section of the
base metal sheet in a heating and holding process;
[Fig. 3E] Fig. 3E is a view schematically
showing the structure of the cross section of the
base metal sheet in a cooling process;
[Fig. 4A] Fig. 4A is a view schematically
showing the structure of the cross section of the
base metal sheet in a state of being held at a
temperature of an A3 point or higher;
[Fig. 4B] Fig. 4B is a view schematically
showing the structure of the cross section of the
base metal sheet after cooling in the case when the
different metal layers are made to remain;
[Fig. 4C] Fig. 4C is a view schematically
showing the structure of the cross section of the
base metal sheet in the case when the base metal
sheet is alloyed up to its center portion in a state
of being held at the temperature of the A3 point or
higher;
[Fig. 4D] Fig. 4D is a view schematically
showing the structure of the cross section of the
base metal sheet after cooling in the case when the
- 11 -
base metal sheet is alloyed up to the center portion;
and
[Fig. 5] Fig. 5 is a view schematically showing
the structure of the cross section of the base metal
sheet in which a crystal grain becomes coarse.
DESCRIPTION OF EMBODIMENTS
[0016] Generally, an orientation of easy
magnetization exists in a-Fe crystal, and when in a
direction in which direction cosines between <100>,
<010>, <001> orientations, (which will be called a
[100] orientation generically), and the orientation
are large, excitation is performed in a fixed
magnetic field and magnetometry is performed, a high
magnetic flux density is likely to be obtained. On
the other hand, when in a direction in which
direction cosines with respect to a <111> orientation
being an orientation of hard magnetization are large,
excitation is performed and magnetometry is performed,
a high magnetic flux density is unlikely to be
obtained. The present inventors found that more
[100] orientations in the a-Fe crystal exist in a
sheet plane and further the a-Fe crystal is
controlled to a specific texture that is thoroughly
distributed in the sheet plane, and thereby direction
cosines' with respect to the [100] orientation always
become large in an arbitrary direction in the metal
sheet plane, and when a magnetic field is applied in
an arbitrary direction in the metal sheet plane and
magnetometry is performed, a high magnetic flux
- 12 -
density can be obtained.
[0017] It is characterized in that a specific
texture that an Fe-based metal sheet of the present
invention has contains at least one type of ferriteforming
element except Fe, in which when intensity
ratios in respective {001}<470>, {116}<6 12 1>, and
{223}<692> directions in a sheet plane by X-ray
diffraction are set to A, B, and C respectively and Z
= (A + 0.97B)/0.98C is satisfied, a Z value is not
less than 2.0 nor more than 200.
[0018] Next, the previously described Z value will
be explained.
[0019] The main orientations on which attention is
focused in the present invention are {001}<470>,
{116}<6 12 1>, and {223}<692>. When examining the
state of a three-dimensional texture calculated by a
vector method, the present inventors noticed that Xray
random intensity ratios in the above-described
three plane orientations change depending on a
magnetic property of a product, and learned that
mathematizing this makes it possible to quantify the
relationship with a magnetic property of a product
and reached the present invention.
[0020] The X-ray random intensity ratios of these
respective orientations may be obtained from a threedimensional
texture calculated by a vector method
based on a pole figure of {110}, or may also be
obtained from a three-dimensional texture calculated
by a series expansion method using a plurality
- 13 -
(preferably three or more) of pole figures out of
pole figures of {110}, {100}, {211}, and {310}. For
the X-ray random intensity ratios in the abovedescribed
respective crystal orientations by the
latter method, for example, intensities of (001) [4 -7
0], (116) [1 -12 1], and (223) [6 -9 2] at a (^ 2 = 45°
cross-section of the three-dimensional texture may be
used as they are.
[0021] Subsequently, there will be explained a
reason for which the expression of Z = (A +
0.97B)/0.98C was found.
[0022] First, the intensity of the {001}<470>
orientation is set to A. This orientation is in the
{100} plane, so that direction cosines with respect
to the {100} plane are 1.0. In the {100} plane, the
[100] orientation being the orientation of easy
magnetization exists, and thus orientation of this
plane in the metal sheet plane is advantageous for
obtaining a high magnetic flux density in the metal
sheet plane. Thus, the intensity A is weighted with
the direction cosines of 1.0 in terms of the. degree
of contribution to improving a magnetic flux density
to be set to one of parameters in the Z value.
[0023] Next, the intensity of the {116}<6 12 1>
orientation is set to B. An angular difference
between this orientation and the {001} plane is 13.3°
and direction cosines are 0.97. In the {001} plane
as well, the [100] orientation being the orientation
of easy magnetization exists, and thus orientation of
- 14 -
this plane in the metal sheet plane is advantageous
for obtaining a high magnetic flux density in the
metal sheet plane. For this reason, the intensity B
is weighted with the direction cosines of 0.97 in
terms of the degree of contribution to improving a
magnetic flux density to be set to one of parameters
in the Z value.
[0024] Further, the intensity of the {223}<692>
orientation is set to C. An angular difference
between the {223}<692> orientation and a {111} plane
is 11.4° and direction cosines are 0.98. As
described previously, in the {111} plane, the [100]
orientation being the orientation of easy
magnetization is not contained, and orientation of
this plane in the metal sheet plane is
disadvantageous for obtaining a high magnetic flux
density. Thus, the intensity C is set not to have
the degree of contribution to improving a magnetic
flux density, is put in the Z value as a parameter
that performs division, and is multiplied by 0.98
being the direction cosines with respect to the {111}
plane as its weighting.
[0025] From the above thought, it was found that
when the intensity ratios in the respective
{001}<470>, {116}<6 12 1>, and {223}<692> directions
in the metal sheet plane by X-ray diffraction are set
to A, B, and C respectively, the expression of Z = (A
+ 0.97B)/0.98C is created, and as the Z value is
increased, a high magnetic flux density can be
- 15 -
obtained when excitation is performed in the metal
sheet plane to perform magnetometry.
[0026] Further, the present inventors were able to
find from a large number of experiments that a
special condition capable of obtaining a high
magnetic flux density in an arbitrary direction in
the metal sheet plane is that the Z value is not less
than 2.0 nor more than 200. They grasped the fact
that the Z value is limited to this range, and
thereby the [100] orientation being the orientation
of easy magnetization is thoroughly distributed in
the metal sheet plane, but have not obtained evidence
making theoretical explanation of this phenomenon
possible so far.
[0027] The present inventors found that when the Z
value is not less than 2.0 nor more than 200, a ratio
BSO/Bs of an average magnetic flux density B50 to a
saturation magnetic flux density Bs becomes a high
level of 0.80 or more and a magnetic flux density
difference A B measured in the metal sheet plane
becomes a low level of 0.15 T or less. Fig. 2
schematically shows this relationship.
[0028] When the Z value is less than 2.0, crystal
orientation of a-Fe shows a tendency to decrease the
[100] orientations being the orientation of easy
magnetization in the metal sheet plane. Alternately,
it shows a tendency that the distribution of the
[100] orientations in the metal sheet plane becomes
non-uniform. That is, the average magnetic flux
- 16
density B50 in the metal sheet plane becomes small
and the ratio B50/Bs of the average magnetic flux
density B50 to the saturation magnetic flux density
Bs becomes less than 0.8- Alternately, only the
magnetic flux density in a specific direction
increases and the magnetic flux density difference AB
becomes greater than 0.15 T. Thus, the Z value is
set to 2.0 or more in the present invention.
[0029] On the other hand, when the Z value exceeds
200, the increase in the magnetic flux density is
saturated and an increase in uniformity of the
magnetic flux density in the metal sheet plane is
also saturated. In contrast to this, in order to
manufacture a metal sheet such that the Z value
exceeds 200, a heat treatment time is prolonged, or
the like, which becomes difficult industrially, and
thus the condition of the Z value is set to 200 or
less .
[0030] Here, Fig. 1 is a view for explaining a
method of calculating the average magnetic flux
density B50. A manufacturing method will be
described later, but it is found that a-region
rolling is performed at 800"^ and as a different metal,
2.6 mass% of Sn and 0.9 mass% of Al are used, and
thereby in an obtainable Fe-based metal sheet having
a thickness of 0.2 mm, a high magnetic flux density
can be obtained thoroughly in an in-plane
circumferential direction.
[0031] Here, in a metal sheet having a higher
- 17 -
accumulation degree of {200} planes among textures of
the Fe-based metal sheet of the present invention in
which the Z value is not less than 2.0 nor more than
200, a higher magnetic flux density can be obtained.
Specifically, in a texture in which an accumulation
degree of {200} planes in an a-Fe phase is not less
than 30% nor more than 99% and an accumulation degree
of {222} planes in the a-Fe phase is not less than
001% nor more than 30%, a higher magnetic flux
density can be obtained.
[0032] When the accumulation degree of the {200}
planes is less than 30% or the accumulation degree of
the {222} planes is greater than 30%, the average
magnetic flux density B50 tends to slightly decrease
even though the Z value is in the present invention
range. Further, in a metal sheet in which the
accumulation degree of the {200} planes is greater
than 99% or the accumulation degree of the {222}
planes is less than 0.01%, the increase in the
magnetic flux density B50 is saturated and a heat
treatment time is prolonged, and the like, resulting
in that manufacturing conditions become
disadvantageous industrially.
[0033] Next, the manufacturing method of the
previously described Fe-based metal sheet will be
explained.
[0034] (First embodiment)
As a manufacturing method of an Fe-based metal
sheet in this embodiment, a rolling temperature and a
- 18 -
#
reduction ratio are optimized, and thereby a {100}
texture is formed in at least a surface layer portion
of the metal sheet, a ferrite-forming element is made
to diffuse into this partial or whole region from its
surface, and at the time of cooling, the whole Febased
metal sheet is oriented in {100}. This makes
it possible to obtain a high magnetic flux density in
an arbitrary direction in a metal sheet plane.
[0035] This embodiment as above is based on the fact
found by the present inventors that {100} crystal
grains in the texture formed in the surface layer
portion preferentially grow at an A3 point or higher
in a heating process to be performed for the
diffusion of the ferrite-forming element, and further
when the ferrite-forming element is made to diffuse
into the inner portion to make the Fe-based metal
sheet alloyed therewith and then cooling is performed,
an accumulation degree of {200} planes in the sheet
plane of the Fe-based metal sheet increases.
[0036] [Explanation of the basic principle of the
first embodiment of the present invention]
First, the basic principle of this embodiment
capable of obtaining a high accumulation degree of
{200} planes will be explained based on Fig. 3A to
Fig. 3E.
[0037] (a) Manufacture of a base metal sheet
(seeding of a texture)
In a process in which a cast slab containing C:
less than 0.02 mass% and made of an Fe-based metal of
- 19 -
an a-y transforming component is decreased in
thickness by rolling and thereby a metal sheet is
obtained, hot rolling is performed at a sheet
temperature of the A3 point or higher, a-region
rolling is performed at a sheet temperature of lower
than the A3 point and 300*C or higher, and further
cold rolling is performed to a predetermined sheet
thickness. By this process, as shown in Fig. 3A, a
base metal sheet 1 having an inner region 4 made of
Fe in an a phase and having a {100} texture 2 in at
least a surface layer portion 3 is obtained. Further,
a seed of crystal that satisfies the condition of the
Z value is formed in a recrystallized texture by a
particular deformation slip.
[0038] (b) (Formation of a second layer)
Next, as shown in Fig. 3B, the ferrite-forming
element such as Al, for example, is bonded to one
surface or both surfaces of the cold-rolled base
metal sheet 1 by using a vapor deposition method or
the like to form a second layer 5.
[0039] (c) Saving of the texture
Next, the base metal sheet 1 having had the
ferrite-forming element bonded thereto is heated to
the A3 point of the base metal sheet 1 to make the
ferrite-forming element diffuse into the partial or
whole region having the {100} texture 2 in the base
metal sheet 1, to make the base metal sheet 1 alloyed
therewith. As shown in Fig. 3C, an alloyed region 6
is transformed to the a phase from a y phase to have
- 20 -
#
an a single phase component. At this time, the
alloyed region 6 is transformed while taking over
orientation of the {100} texture 2 formed in the
surface layer portion 3, so that a structure oriented
in {100} is formed also in the alloyed region 6.
[0040] (d) Achievement of high accumulation of the
texture
Next, the partially alloyed base metal sheet 1 is
further heated to a temperature of not lower than the
A3 point nor higher than 1300*0 and the temperature is
held. The region of the a single phase component is
an a-Fe phase not undergoing y transformation, and
thus the {100} crystal grains are maintained as they
are, the {100} crystal grains preferentially grow in
the region, and the accumulation degree of the {200}
planes increases. Further, as shown in Fig. 3D, a
region 8 not having the a single phase component is
transformed to the y phase from the a phase.
[0041] Further, when a holding time of the
temperature after the heating is prolonged, the {100}
crystal grains are united to preferentially grow to
large {100} crystal grains 7. As a result, the
accumulation degree of the {200} planes further
increases. Further, with the diffusion of the
ferrite-forming element, the region 6 alloyed with
the ferrite-forming element is transformed to the a
phase from the y phase. At this time, in the region
adjacent to the region to be transformed, crystal
grains in the a phase oriented in {100} are already
- 21 -
#
formed, and at the time of the transformation to the
a phase from the y phase, the region 6 is
transformed while taking over a crystal orientation
of the adjacent crystal grains in the a phase.
Thereby, the holding time is prolonged and the
accumulation degree of the {200} planes increases.
[0042] (e) Growth of the texture
The base metal sheet is cooled to a temperature
of lower than the A3 point. At this time, as shown
in Fig. 3E, a y-Fe phase in an unalloyed inner region
10 is transformed to the a-Fe phase. This inner
region 10 is adjacent to the region in which the
crystal grains in the a phase oriented in {100} are
already formed in a temperature region of the A3
point or higher, and at the time of the
transformation to the a phase from the y phase, the
inner region 10 is transformed while taking over the
crystal orientation of the adjacent crystal grains in
the a phase and larger crystal grains 9 in the a
phase oriented in {100} are formed. Therefore, the
accumulation degree of the {200} planes increases
also in the region. By this phenomenon, the high
accumulation degree of the {200} planes can be
obtained even in the unalloyed region.
[0043] When at the stage of the preceding state
shown in Fig. 3D, the temperature of the A3 point or
higher is held until the whole metal sheet is alloyed,
the structure having the high accumulation degree of
the {200} planes is already formed in the whole metal
- 22 -
#
sheet, and thus the cooling is performed while the
state when the cooling is started is maintained.
[0044] In the above, the basic principle of this
embodiment was explained, and there will be further
explained a limiting reason of each condition that
defines the manufacturing method of this embodiment
and preferable conditions of this embodiment.
[0045] [Fe-based metal to be the base material]
(C content)
In this embodiment, first, crystal grains
oriented in {100} to serve as seeds for increasing
the accumulation degree of the {200} planes in the
sheet are formed in the surface layer portion of the
base metal sheet made of the Fe-based metal. Then,
the 7-a transformation is made to progress in the
metal sheet while taking over a crystal orientation
of the crystal grains in the a phase to serve as the
seeds finally, to thereby increase the accumulation
degree of the {200} planes of the whole metal sheet.
For this reason, the Fe-based metal used for the base
metal sheet has a composition of the a-7
transforming component. When the Fe-based metal used
for the base metal sheet has the a-7 transforming
component, the ferrite-forming element is made to
diffuse into the metal sheet to make the metal sheet
alloyed therewith, thereby making it possible to form
the region having the a single phase based component.
[0046] In.this embodiment, the C content of the base
metal sheet is set to less than 0.02 mass%. Further,
- 23 -
#
in terms of a magnetic property of a product metal
sheet, the C content is preferably 0.01 mass% or less.
Under the condition of the C content being less than
0.02 mass%, the ferrite-forming element is made to
diffuse into the metal sheet to make the metal sheet
alloyed therewith, thereby making it possible to form
the region having the a single phase based component.
Incidentally, C is a component to remain in a process
of manufacturing the slab and the less C is, the more
preferred it is in terms of the magnetic property,
and thus its lower limit is not necessary needed, but
it is preferably set to 0.0001 mass% or more in terms
of the cost of a refining process.
[0047] (Other containing elements)
In principle, being applicable to the Fe-based
metal having the a-7 transforming component, this
embodiment is not limited to the Fe-based metal in a
specific composition range. Typical examples of the
a-7 transforming component are pure iron, steel such
as ordinary steel, and the like. For example, it is
a component containing pure iron or steel containing
C of 1 ppm to less than 0.02 mass% as described above
and a balance being composed of Fe and inevitable
impurities as its base and containing an additive
element as required. Instead, it may be silicon
steel of the a-y transforming component having C:
less than 0.02 mass% and Si: 0.1 mass% to 2.5 mass%
as its basic component. Further, as other impurities,
a trace amount of Ni, Cr, Al, Mo, W, V, Ti, Nb, B, Cu,
- 24 -
Zr, Y, Hf, La, Ce, N, 0, P, S, and/or the like are/is
contained. Further, Al and Mn are added to increase
electric resistance, to thereby decrease a core loss,
and Co is added to increase the saturation magnetic
flux density Bs, to thereby increase a magnetic flux
density, which are also included in the present
invention range.
[0048] (Thickness of the base metal sheet)
The thickness of the base metal sheet is set to
not less than 10 ju m nor more than 6 mm. When the
thickness is less than 10 ju m, when the base metal
sheets are stacked to be used as a magnetic core, the
number of the sheets to be staked is increased to
increase gaps, resulting in that a high magnetic flux
density cannot be obtained. Further, when the
thickness exceeds 6 mm, it is not possible to make
the {100} texture grow sufficiently even though a
reduction ratio of the a-region rolling is adjusted,
resulting in that a high magnetic flux density cannot
be obtained.
[0049] [Rolling conditions]
In this embodiment, as described previously, the
Fe-based metal having, in at least the surface layer
portion, the crystal grains oriented in {100} to
serve as the seeds for increasing the accumulation
degree of the {200} planes in the metal sheet is used
as a starting material. As a method of achieving,
high accumulation of the {100} planes of the base
metal sheet, a method of performing a-region rolling
- 25 -
in a process in which a cast slab is rolled to a
sheet shape is used.
[0050] First, a cast slab containing C: less than
0.02 mass% and made of the Fe-based metal of the a-7
transforming component such as a continuous cast slab
or an ingot is prepared. Then, in a process in which
the cast slab is decreased in thickness by rolling to
obtain the base metal sheet, first the hot rolling is
performed at a temperature of the A3 point or higher.
Next, the a-region rolling is performed at a
temperature of lower than the A3 point and higher
than 300^), and further the metal sheet is subjected
to cold rolling to a predetermined thickness, and
thereby the base metal sheet having the {100} texture
formed in the surface layer portion is obtained.
[0051] As for a reduction ratio in each of rolling
processes to be performed until the base metal sheet
is obtained from the cast slab, the total reduction
ratio in the a-region rolling is preferably set to -
1.0 or less in terms of true strain and the sum of
the total reduction ratio in the a-region rolling and
the total reduction ratio in the cold rolling is
preferably set to -2.5 or less in terms of true
strain. Conditions other than these may create a
possibility that the {100} texture cannot be
sufficiently formed in the surface layer portion. A
method of expressing the reduction ratio by true
strain £ is expressed by the following expression (1),
where in each of the rolling processes, the thickness
- 26 -
#
before the rolling is set to hO and the thickness
after the rolling is set to h.
£ = ln(h/hO) ... (1)
[0052] When the sum of the total reduction ratio in
the a-region rolling and the total reduction ratio in
the cold rolling is in the previously described
preferred range, a deformed structure in which the
{100} texture is formed by recrystallization can be
provided to at least the vicinity of the surface
layer portion of the base metal sheet. Particular
crystal slip and crystal rotation to occur at these
reduction ratios are thought to occur. Thus, they
are preferably in these ranges.
[0053] Further, as for the reduction ratio in each
of the rolling processes to be performed until the
base metal sheet is obtained from the cast slab, the
reduction ratio in the hot rolling is preferably -0.5
or less in terms of true strain, thereby making it
easier to obtain the higher accumulation degree of
the {200} planes. This results from the fact found
by the present inventors that in order that desirable
deformation should be performed in the a-region
rolling and the cold rolling, deformation in the hot
rolling in a y region is also closely affected. Thus,
these ranges are preferred.
[0054] The region of the surface layer portion in
which the {100} texture is formed preferably has 1 /x m
or more of a distance in a sheet thickness direction
from the surface. Thereby, it is possible to bring
- 27 -
^ ^ • • •
#
the accumulation degree of the {200} planes to 30% or
more in the following diffusion treatment. The upper
limit of the distance is not limited in particular,
but it is difficult to form the {100} texture in a
region of 500 /i m or more by rolling.
[0055] Incidentally, the measurement of the
accumulation degree of the {200} planes can be
performed by X-ray diffraction using a MoKa ray. To
be in more detail, in the a-Fe crystal, integrated
intensities of 11 orientation planes ({110}, {200},
{211}, {310}, {222}, {321}, {411}, {420}, {332},
{521}, and {442}) parallel to a sample surface are
measured for each sample, each measured value is
divided by a theoretical integrated intensity of the
sample having a random orientation, and thereafter, a
ratio of the intensity of {200} or {222} is obtained
inpercentage.
[0056] At this time, for example, the accumulation
degree of the {200} planes is expressed by Expression
(2) below.
accumulation degree of {200} planes =
[ {i (200)/I(200) }/S {i (hkl)/I (h)cl) } ] X 100 ... (2)
Here, i(hkl) is an actually measured integrated
intensity of {hkl} planes in the measured sample, and
I(hkl) is a theoretical integrated intensity of the
{hkl} planes in the sample having the random
orientation. Further, E is the sum of the 11
orientation planes in the a-Fe crystal. Here,
instead of the theoretical integrated intensity of
- 28 -
0
the sample having the random orientation, actually
measured values using the sample may be used.
[0057] [Different metal]
Next, a different metal except Fe is made to
diffuse into the base metal sheet manufactured by the
above-described rolling processes to increase the
region of the {100} texture in the thickness
direction of the steel sheet. As the different metal,
the ferrite-forming element is used. As a procedure,
first, the different metal is bonded in a layered
form as the second layer to one surface or both
surfaces of the base metal sheet made of the Fe-based
metal of the a - y transforming component. Then, a
region alloyed by having had elements of the
different metal diffuse thereinto is turned to have
the a single phase based component and to be able to
be maintained as not only the region transformed to
the a phase, but also a seed oriented in {100} for
increasing the accumulation degree of the {200}
planes in the metal sheet. As such a ferrite-forming
element, at least one type of Al, Cr, Ga, Ge, Mo, Sb,
Si, Sn, Ta, Ti, V, W, and Zn can be used alone or in
a combined manner.
[0058] As a method of bonding the different metal in
a layered form to the surface of the base metal sheet,
there can be employed various methods such as a
plating method of hot dipping, electrolytic plating,
or the like, a rolling clad method, a dry process of
PVD, CVD, or the like, and further powder coating.
- 29 -
0
As a method of efficiently bonding the different
metal for industrially implementing the method, the
plating method or the rolling clad method is suitable
[0059] The thickness of the different metal before
the heating when the different metal is bonded is
preferably not less than 0.05 p. m nor more than 1000
Mm. When the thickness is less than 0.05 /xm, it is
not possible to obtain the sufficient accumulation
degree of the {200} planes. Further, when the
thickness exceeds 1000 p,m, even when the different
metal layer is made to remain, its thickness becomes
larger than necessary.
[0060] [Heating and diffusion treatment]
The base metal sheet having had the ferriteforming
element as the different metal bonded thereto
is heated up to the A3 point of the base metal sheet,
to thereby make the ferrite-forming element diffuse
into the partial or whole region of the {100} texture
formed in the surface layer portion of the base metal
sheet to make the base metal sheet alloyed therewith.
The region alloyed with the ferrite-forming element
is turned to have the a single phase component and
the region is transformed to the a phase from the y
phase. At this time, the region is transformed whil
taking over the orientation of the {100} textur
formed in the surface layer portion, and thus th
structure oriented in {100} is formed also in the
alloyed region. As a result, in the alloyed region,
a structure in which the accumulation degree of the
- 30 -
e
:e
le
' #
{200} planes in the a-Fe phase becomes not less than
25% nor more than 50% and in accordance with it, the
accumulation degree of the {222} planes in the a-Fe
phase becomes not less than 1% nor more than 40% is
formed.
[0061] Then, the base metal sheet is further heated
to a temperature of not lower than the A3 point nor
higher than 1300t and the temperature is held. The
region alloyed already is turned into an a single
phase structure that is not transformed to the y
phase, so that the crystal grains in the {100}
texture are maintained as they are, and in the region,
the crystal grains in the {100} texture
preferentially grow and the accumulation degree of
the {200} planes increases. Further, the region not
having the a single phase component is transformed to
the y phase.
[0062] Further, when the holding time is prolonged,
the crystal grains in the {100} texture are united to
one another to preferentially grow. As a result, the
accumulation degree of the {200} planes further
increases. Further, with the further diffusion of
the ferrite-forming element, the region alloyed with
the ferrite-forming element is transformed to the a
phase from the y phase. At this time, as shown in
Fig. 4A, in the regions adjacent to the regions to be
transformed, crystal grains 7 in the a phase oriented
in {100} are already formed, and at the time of the
transformation to the a phase from the y phase, the
- 31 -
#
regions alloyed with the ferrite-forming element are
transformed while taking over a crystal orientation
of the adjacent crystal grains 7 in the a phase. By
these phenomena, the holding time is prolonged and
the accumulation degree of the {200} planes increases.
Further, as a result, the accumulation degree of the
{222} planes decreases.
[0063] Incidentally, in order to finally obtain the
high accumulation degree of the {200} planes of 50%
or more, it is preferred that the holding time should
be adjusted to, at this stage, bring the accumulation
degree of the {200} planes in the a-Fe phase to 30%
or more and bring the accumulation degree of the
{222} planes in the a-Fe phase to 30% or less.
Further, when the A3 point or higher is held until
the whole metal sheet is alloyed, as shown in Fig. 4C,
the a single phase structures are formed up to the
center portion of the metal sheet and grain
structures oriented in {100} reach the center of the
metal sheet.
[0064] A holding temperature after the temperature
is increased is set to not lower than the A3 point
nor higher than 1300"^. Even when the metal sheet is
heated at a temperature higher than 1300^0, an effect
with respect to the magnetic property is saturated.
Further, cooling may be started immediately after the
temperature reaches the holding temperature (in the
case, the temperature is held for 0.01 second or
longer substantially), or cooling may also be started
- 32 -
after the temperature is held for 600 minutes or
shorter. Even when the temperature is held for
longer than 600 minutes, the effect is saturated.
When this condition is satisfied, the achievement of
high accumulation of the seeds oriented in the {200}
plane further progresses to make it possible to more
securely bring the accumulation degree of the {200}
planes in the a-Fe phase to 30% or more after the
cooling.
[0065] [Cooling after the heating and diffusion
treatment]
After the diffusion treatment, when the cooling
is performed while the region that is not alloyed
with the ferrite-forming element is remaining, as
shown in Fig. 4B, at the time of the transformation
to the a phase from the y phase, the unalloyed
region is transformed while taking over the crystal
orientation of the regions in which the crystal
grains 9 in the a phase oriented in {100} are already
formed. Thereby, the accumulation degree of the
{200} planes increases, and the metal sheet having
the texture in which the accumulation degree of the
{200} planes in the a-Fe phase is not less than 30%
nor more than 99% and the accumulation degree of the
{222} planes in the a-Fe phase is not less than 0.01%
nor more than 30% is obtained, the crystal satisfying
the condition of the Z value grows, and a high
magnetic flux density can be obtained in an arbitrary
direction in the metal sheet plane.
- 33 -
•
[0066] Further, as shown in Fig. 4C, when the A3
point or higher is held until the whole metal sheet
is alloyed, and the grain structures oriented in
{100} reach the center of the metal sheet, as shown
in Fig. 4D, the metal sheet is cooled as it is, and
the texture in which the crystal grains 9 oriented in
{100} reach up to the center of the metal sheet can
be obtained. Thereby, the whole metal sheet is
alloyed with the different metal, and the metal sheet
having the texture in which the accumulation degree
of the {200} planes in the a-Fe phase is not less
than 30% nor more than 99% and the accumulation
degree of the {222} planes in the a-Fe phase is not
less than 0.01% nor more than 30% is obtained.
[0067] As above, the value of the accumulation
degree of the {200} planes and the remaining state of
the different metal on the surface of the base metal
sheet change depending on the holding time of the
temperature of the A3 point or higher and the holding
temperature. The example shown in Fig. 4B is in a
state where the grain structures oriented in {100} do
not reach up to the center of the metal sheet, the
different metal also remain on the surfaces, and an a
single phase front surface side region and an a
single phase rear surface side region being the
second layer are formed, but it is also possible to
obtain the grain structures oriented in {100} up to
the center of the metal sheet and to alloy all the
second layers on the surfaces.
- 34 -
[0068] Incidentally, at the time of the cooling
after the diffusion treatment, a cooling rate is
preferably not less than O.lt/sec nor more than 500"C
/sec. When the cooling is performed in this
temperature range, the growth of the seeds oriented
in the {200} plane further progresses.
[0069] Further, when the second layers are made to
remain on the obtainable Fe-based metal sheet having
a thickness of not less than 10 /U m nor more than 6 mm,
the thickness of the second layer is preferably set
to not less than 0.01 (im nor more than 500 /im.
Further, a ratio of the a single phase region alloyed
at this stage is preferably 1% or more in a cross
section of the Fe-based metal sheet.
[0070] Further, at the time of cooling to a
temperature of lower than the A3 point in the state
shown in Fig. 4A, an average cooling rate at the time
of cooling to the A3 point - 50°C from the A3 point
may be set to 50t/minute or less. When the cooling
is performed at the cooling rate in this range, the
adjacent crystal grains oriented in {100} are united
to one another to grow, and as shown in Fig. 5, a
coarse crystal grain 11 straddling part of an a
single phase front surface side region 6a adjacent to
a front surface side second layer 5a and straddling
part of an a single phase rear surface side region 6b
adjacent to a rear surface side second layer 5b is
formed. When the average cooling rate from the A3
point to the A3 point - 50t becomes greater than bO'XZ
- 35 -
/minute, there is no sufficient time for growth of
the crystal grain 11, resulting in that an excellent
core loss property cannot be obtained. On the other
hand, the lower limit of the average cooling rate
from the A3 point to the A3 point - 50*0 is not
limited, but the lower limit is preferably set to I'C
/minute in terms of the productivity.
[0071] Further, in order to obtain a more excellent
core loss property, an average cooling rate at the
time of cooling to the A3 point - lOt from the A3
point is preferably set to 20'C/minute or less. On
the other hand, the lower limit of the average
cooling rate from the A3 point to the A3 point - lOt
is not limited, but the lower limit is preferably set
to I'C/minute in terms of the productivity.
[0072] (Second embodiment)
In the previously described first embodiment,
there was explained the manufacturing method of the
previously described Fe-based metal sheet by using
the cast slab containing C: less than 0.02 mass% and
made of the Fe-based metal of thea-y transforming
component. In contrast to this, in this embodiment,
there will be explained a manufacturing method of the
previously described Fe-based metal sheet by using a
cast slab containing C: 0.02 mass% or more.
[0073] When the C content is large, a good magnetic
property cannot be obtained, so that it is necessary
to remove C by performing decarburization annealing.
Thus, the decarburization annealing is performed
- 36 -
#
under conditions to be explained below, thereby
making it possible to increase the accumulation
degree of the {200} planes.
[0074] In the method of this embodiment, a {100}
texture is formed in a surface layer portion of an
Fe-based metal sheet by using y-a transformation
accompanying decarburization (and further
demanganization), and thereafter a ferrite-forming
element is made to diffuse into a partial or whole
decarburized region and further over the region from
its surface, and at the time of cooling, the whole
Fe-based metal sheet is made to be oriented in {100}.
[0075] This embodiment as above is based on the fact
found by the present inventors that {100} crystal
grains in the texture formed in the surface
preferentially grow at an A3 point or higher in a
heating process to be performed for the diffusion of
the ferrite-forming element and further when the
ferrite-forming element is made to diffuse into the
inner portion to make the Fe-based metal sheet
alloyed therewith and then cooling is performed, an
accumulation degree of {200} planes in a sheet plane
of the Fe-based metal sheet increases.
[0076] [Explanation of the basic principle of the
second embodiment of the present invention]
First, the basic principle of this embodiment
capable of obtaining a high accumulation degree of
{200} planes will be explained based on Fig. 3A to
Fig. 3D, by taking the case of decarburization as an
- 37 -
#
example.
[0077] (a) Seeding of a texture
When being decarburized until C becomes less
than 0.02 mass%, the Fe-based metal sheet containing
C: 0.02 mass% or more and having a composition of the
a-y transforming component is heated to a
temperature at which a structure is turned into an a
single phase and to a temperature of a y single phase
or a two-phase region of a y phase and an a phase
(namely, a temperature of an Al point or higher) to
decarburize the surface layer portion of the Fe-based
metal sheet until C becomes less than 0.02 mass%.
Thereby, the y-a transformation is made to occur in
a process of the decarburization to turn the
decarburized surface layer portion into the a phase.
[0078] At this time, the decarburization progresses
the most in the <110> direction in the y phase having
large gaps between lattices, and in this portion, the
C concentration becomes less than 0.02% and the
transformation to the a phase occurs. A {110} plane
in the y phase becomes the {100} plane when the y
phase is turned into the a-phase in a BCC structure,
and thus in the a phase after the decarburization,
the {100} plane is preferentially formed. Further,
the growth, of the crystal grains in the a phase
formed in the surface, in the sheet thickness
direction is slow because its rate is controlled by a
decarburization rate, and thus the crystal grains in
the a phase formed in the surface grow in a direction
- 38 -
parallel to the sheet plane. Further, in the surface
of the metal sheet, the {100} plane preferentially
grows by taking surface energy as driving force. As
a result, the whole surface of the metal sheet
becomes a structure oriented in {100}' finally. By
this process, as shown in Fig. 3A, a base metal sheet
1 having an inner region 4 made of Fe in the a phase
and having the accumulation degree of the {200}
planes in the decarburized region brought to 20% or
more can be obtained. Further, a seed of crystal
that satisfies the condition of the Z value is formed
in the structure formed at the time of the
decarburization by taking the surface energy as
driving force.
[0079] (b) (Formation of a second layer)
Next, as shown in Fig. 3B, the ferrite-forming
element such as Al is bonded to one surface or both
surfaces of the base metal sheet 1 after the
decarburization by using a vapor deposition method or
the like to form a second layer 5.
[0080] (c) Saving of the texture
Next, the base metal sheet 1 having had the
ferrite-forming element bonded thereto is heated to
the A3 point of the base metal sheet 1 to make the
ferrite-forming element diffuse into the partial or
whole decarburized region in the base metal sheet 1
to make the base metal sheet 1 alloyed therewith.
Thereby, as shown in Fig. 3C, the a phase is formed
in an alloyed region 6. Alternately, the ferrite-
- 39 -
forming element is made to diffuse into the inner
portion over the decarburized region to make the base
metal sheet 1 alloyed therewith, and the alloyed
region is turned to have the a single phase component
partially, and thereby the region is turned into the
a phase. At this time, the region is transformed
while taking over orientation of the region formed by
the decarburization, so that the structure oriented
in {100} is formed also in the alloyed region 6.
Further, the orientation in {100} is further
increased even in crystal grains turned into the a
phase previously. Further, when the ferrite-forming
element is made to diffuse and the crystal is
oriented, the seed of the crystal satisfying the
condition of the Z value preferentially grows.
[0081] (d) Achievement of high accumulation of the
texture
Next, the partially alloyed base metal sheet 1 is
further heated to a temperature of not lower than the
A3 point nor higher than 1300*^ and the temperature is
held. The region of the a single phase component is
an a-Fe phase not undergoing y transformation, and
thus the {100} crystal grains are maintained as they
are, the {100} crystal grains preferentially grow in
the region, and the accumulation degree of the {200}
planes increases. Further, as shown in Fig. 3D, the
region not having the a single phase component is
transfjormed to the y phase from the a phase.
[0082] Further, when a holding time of the
- 40 -
llp
temperature after the heating is prolonged, the {100}
crystal grains are united to preferentially grow to
large {100} crystal grains 7. As a result, the
accumulation degree of the {200} planes further
increases. Further, with the diffusion of Al, the
region alloyed with Al is transformed to the a phase
from the y phase. At that time, in the region
adjacent to the region to be transformed, crystal
grains in the a phase oriented in {100} are already
formed, and at the time of the transformation to the
a phase from the y phase, the region is transformed
while taking over a crystal orientation of the
adjacent crystal grains in the a phase. Thereby, the
holding time is prolonged and the accumulation degree
of the {200} planes increases.
{0083] (e) Growth of the texture
Next, the base metal sheet is cooled to a
temperature of lower than the A3 point. At this time,
as shown in Fig. 3E, a y-Fe phase in an unalloyed
inner region 10 is transformed to the a-Fe phase.
This inner region 10 is adjacent to the region in
which the crystal grains in the a phase orie'nted in
{100} are already formed in a temperature region of
the A3 point or higher, and at the time of the
transformation to the a phase from the y phase, the
inner region 10 is transformed while taking over the
crystal orientation of the adjacent crystal grains in
the a phase and larger crystal grains 9 in the a
phase oriented in {100} are formed. Therefore, the
- 41 -
accumulation degree of the {200} planes increases
also in the region (see the state shown in Fig. 6D).
By this phenomenon, the high accumulation degree of
the {200} planes can be obtained even in the
unalloyed region 10.
[0084] When at the stage of the preceding state
shown in Fig. 3D, the temperature of the A3 point or
higher is held until the whole metal sheet is alloyed,
the structure having the high accumulation degree of
the {200} planes is already formed in the whole metal
sheet, and thus the cooling is performed while the
state when the cooling is started is maintained.
[0085] Further, in the above explained example, the
Fe-based metal sheet containing C: 0.02 mass% or more
is used, but when an Fe-based metal sheet containing
C: less than 0.02 mass% is used, carburization is
performed before the decarburization to bring the C
content in the region to be decarburized to 0.02
mass% or more.
[0086] In the above, the basic constitution of this
embodiment was explained, and there will be further
explained a limiting reason of each condition that
defines a manufacturing method of this embodiment and
preferable conditions of this embodiment.
[0087] [Fe-based metal to be the base material]
(C content)
In this embodiment, first, crystal grains
oriented in {100} to serve as seeds for increasing
the accumulation degree of the {200} planes are
- 42 -
formed in the surface of the base metal sheet made of
the Fe-based metal. Then, the -y - a transformation is
made to progress in the metal sheet while taking over
a crystal orientation of the crystal grains in the a
phase to serve as the seeds finally, to thereby
increase the accumulation degree of the {200} planes
of the whole metal sheet.
[0088] In this embodiment, the seeds of the crystal
grains oriented in {100} are formed in the surface of
the base metal sheet by structure control using the y
-a transformation accompanying decarburization or
demanganization. The Fe-based metal used for the
base metal sheet has a composition of the a - 7
transforming component, and the C content in the
region to be decarburized is brought to 0.02 mass% or
more .
[0089] Further, the Fe-based metal used for the base
metal sheet has the a-7 transforming component, and
the ferrite-forming element is made to diffuse into
the metal sheet to make the metal sheet alloyed
therewith, thereby making it possible to form a
region having the a single phase based component.
Further, the C content in the region to be
decarburized is brought to 0.02 mass% or more,
thereby making it possible to use the 7-a
transformation accompanying the decarburization.
[0090] For bringing the C content in the base metal
sheet to 0.02 mass% or more, there is a method of
using a base metal sheet manufactured from a molten
- 43 -
ma terial adjusted to contain C: 0.02 mass% or more by
undergoing casting and rolling processes (a melting
method). As another method, there is a method in
which a base metal sheet having the C content of less
than 0.02 mass% is used and in a surface layer
portion of the base metal sheet, a region containing
C: 0.02 mass% or more is formed by carburization.
[0091] In the case of the melting method, the range
of the C content is set to not less than 0.02 mass%
nor more than 1.0 mass%. When the C content is less
than 0.02 mass%, it is not possible to use the
formation of a {200} texture using the y-a
transformation accompanying the decarburization.
Further, when the C content is 1.0 mass% or more, a
long time is required for the decarburization. The
preferred range of the C content is not less than
0.05 mass% nor more than 0.5 mass%.
[0092] In the case of the carburization method, the
range of the C content of the Fe-based metal of which
the base metal sheet is made is set to 1 ppm or more
and less than 0.02 mass%. Then, the surface layer of
this Fe-based metal is subjected to the carburization
so that the C concentration may become not less than
0.02 mass% nor more than 1.0 mass% in the same manner
as that in the melting case.
[0093] Further, a carburizing range is set to a
region down to a distance y from the surface, where
the distance in a depth direction from the surface is
set to y. This distance y is not less than 5 fira nor
- 44 -
more than 50 fim. When the distance y is less than 5
urn, it is difficult to bring the accumulation degree
of the {200} planes to 30% or more in the diffusion
treatment after the decarburization, so that the
distance y is set to 5 /x m or more. Further, when the
distance becomes greater than 50 /zm, a long time is
required for the carburization, and further a long
time is required also for the decarburization of the
whole carburized region. Further, an obtainable
effect is also saturated, so that the preferred
distance y is set to 50 nm or less. The carburizing
method is not limited in particular, and a well-known
gas carburizing method or the like may be performed.
[0094] Incidentally, the C content is preferably
0.005 mass% or less in terms of a magnetic property
of a product metal sheet, so that in order to
manufacture a steel sheet excellent in a magnetic
property, silicon steel having the C content of 0.005
mass% or less is used to be subjected to
carburization in a manner to have the above-described
C concentration, which is advantageous for cost.
[0095] (Mn content)
When Mn being an austenite stabilizing element
is contained in the Fe-based metal, it is possible to
form seeds of crystal grains oriented in {100} by
structure control using the 7-a transformation
accompanying demanganization. The demanganization is
performed together with the decarburization, and
thereby the surface layer portion is turned into the
- 45 -
a phase more efficiently and the accumulation degree
of the {200} planes in a decarburized and
demanganized region is more increased. In order to
exhibit such a function, the Mn content before
performing the demanganization treatment is
preferably set to 0.2 mass% or more.
[0096] The above-described structure control using
the 7-a transformation can be performed even by the
decarburization alone, so that Mn does not have to be
contained. However, when Mn is contained, an effect
of increasing electric resistance to decrease a core
loss is also obtained, and thus Mn in a range of 2.0
mass% or less may also be contained according to need
even when no demanganization is performed. From the
above point, the range of the Mn content when Mn is
contained is preferably set to 0.2 mass% to 2.0 mass%
[0097] (Other containing elements)
In principle, being applicable to the Fe-based
metal having the a - v transforming component, this
embodiment is not limited to the Fe-based metal in a
specific composition range. Typical examples of the
a-7 transforming component are pure iron, steel such
as ordinary steel, and the like. For example, it is
a component containing pure iron or steel containing
C of 1 ppm to 0.10 mass% as described above or
further containing Mn of 0.2 mass% to 2.0 mass% and a
balance being composed of Fe and inevitable
impurities as its base and containing an additive
element as required. Instead, it may be silicon
- 46 -
#
steel of the a - y transforming component having C:
1.0 mass% or less and Si: 0.1 mass% to 2.5 mass% as
its basic component. Further, as other impurities, a
trace amount of Ni, Cr, Al, Mo, W, V, Ti, Nb, B, Cu,
Co, Zr, Y, Hf, La, Ce, N, 0, P, S, and/or the like
are/is contained. Incidentally, Al and Mn are added
to increase electric resistance, to thereby decrease
a core loss and Co is added to increase the
saturation magnetic flux density Bs, to thereby
increase a magnetic flux density, which are also
included in the present invention range.
[0098] (Thickness of the base metal sheet)
The thickness of the base metal sheet is set to
not less than 10 ju m nor more than 6 mm. When the
thickness is less than 10 jum, when the base metal
sheets are stacked to be used as a magnetic core, the
number of the sheets to be staked is increased to
increase gaps, resulting in that a high magnetic flux
density cannot be obtained. Further, when the
thickness is greater than 6 mm, it is not possible to
make the {100} texture grow sufficiently after
cooling after the diffusion treatment, resulting in
that a high magnetic flux density cannot be obtained.
[0099] [Decarburization treatment]
In the decarburization treatment for turning the
surface layer portion of the base metal sheet into
the a phase, the base metal sheet is desirably heated
in a decarburizing atmosphere to be decarburized in
the following manner.
- 47 -
[0100] (Temperature of the decarburization
treatment)
The temperature of the decarburization treatment
is set to a temperature of the Al point or higher and
a temperature at which a structure is turned into an
a single phase when the decarburization is performed
until C becomes less than 0.02 mass%. The base metal
sheet containing C: 0.02 mass% or more is heated to a
temperature of a 7 single phase or a two-phase region
of a 7 phase and an a phase (namely a temperature of
the Al point or higher) in order to make the y-a
transformation occur by the decarburization.
[Old] (Atmosphere of the decarburization treatment)
With regard to the decarburizing atmosphere, a
conventionally known method in manufacture of a
grain-oriented electrical steel sheet can be employed,
For example, there is a method in which
decarburization is first performed in a weak
decarburizing atmosphere, in a vacuum of 1 Torr or
less, for example, or in a gas atmosphere of one type
or two or more types of H2, He, Ne, Nr, Kr, Xe, Rn,
and N2 at a temperature of lower than (a dew point -
20)t, and next decarburization is performed in a
strong decarburizing atmosphere, or in a gas
atmosphere in which an inert gas, or CO and CO2 is/are
added to H2 at a temperature of (a dew point -20)^3 or
higher, for example. In this case, if the
decarburization is continued to the end in the weak
decarburizing atmosphere, a long time is required.
- 48 -
1^^
'2^^
[0102] (Period of performing the decarburization
treatment)
The period of jaerforming the decarburization
treatment is preferably not shorter than 0.1 minute
nor longer than 600 minutes. When the period is
shorter than 0.1 minute, it is difficult to bring the
accumulation degree of the {200} planes to 20% or
more after the decarburization, and when the period
is long so as to exceed 600 minutes, too much cost is
needed.
[0103] (Range of performing the decarburization
treatment)
The range of performing the decarburization
treatment is a range down to a distance x, where the
distance in the depth direction from the surface is
set to X, and the distance x is not less than 5 fim
nor more than 50 iim. When the distance x is less
than 5 tim, it is difficult to bring the accumulation
degree of the {200} planes to 30% or more in the
diffusion treatment after the decarburization. For
this reason, the distance x in the depth direction
from the surface is set to 5 /x m or more. Further,
when the distance is greater than 50 /zm, a long time
is required for the decarburization, and further the
accumulation degree of the {200} planes is saturated,
and thus it is not advantageous industrially. Thus,
the distance x is set to 50 /z m or less.
[0104] (Other decarburizing methods)
Further, as described in Patent Literature 6, it
- 49
#
is also possible that a material promoting
decarburization is applied to a surface of a steel
sheet as an annealing separating agent and this is
wound around a coil and is subjected to coil
annealing, to thereby form a decarburized region.
Further, it is also possible that the above-described
annealing separating agent is applied to a surface of
a steel sheet in a single sheet form and the steel
sheets are stacked to be subjected to annealing at
the above-described temperature for a similar time,
to thereby form a decarburized region.
[0105] (C content after the decarburization)
The C content after the decarburization is set
to less than 0.02 mass% in order to obtain an a-phase
single phase structure as described above. It is
preferably 0.005 mass% or less in terms of the
magnetic property of a product.
[0106] (Accumulation degree of the {200} planes
after the decarburization)
It is preferred that the accumulation degree of
the {200} planes in the decarburized region after the
decarburization should become 20% or more by
performing the decarburization annealing under the
above conditions. When the accumulation degree of
the {200} planes is less than 20%, it is difficult to
bring the accumulation degree of the {200} planes to
30% or more in the diffusion treatment to be
performed subsequently. Further, the upper limit of
the accumulation degree of the {200} planes is
- 50 -
•
preferably set to 99%. When it is greater than 99%,
the magnetic property deteriorates. The accumulation
degree of the {200} planes is adjusted to fall within
the above-described range by selecting the conditions
of the decarburizing temperature, the decarburizing
time, the decarburizing atmosphere, and the like.
Incidentally, the measurement of the accumulation
degree of the plane in the above-described
orientation plane can be performed by X-ray
diffraction using a MoKa ray similarly to the first
embodiment.
[0107] [Demanganization treatment]
In this embodiment, the decarburization
treatment and the demanganization treatment may also
be used in combination by containing Mn in the base
metal sheet. The demanganization treatment is
performed simultaneously with the decarburization or
subsequently to the decarburization under the
following conditions. Incidentally, as described in
Patent Literature 6, it is also possible to perform
the decarburization treatment and the demanganization
treatment simultaneously in a state where steel
sheets each have an annealing separating agent
containing a material promoting decarburization and a
material promoting demanganization applied thereto to
be staked.
[0108] (Temperature and range of the demanganization
treatment)
The temperature at which the demanganization
- 51 -
treatment is performed is set to a temperature of the
Al point or higher similarly to the decarburization.
With regard to a demanganizing atmosphere, the
demanganization treatment may be performed under a
reduced pressure atmosphere. Further, the period of
performing the demanganization treatment is
preferably set to fall within a range of not shorter
than 0.1 minute nor longer than 600 minutes similarly
to the decarburization.
[0109] (Range of performing the demanganization
treatment)
The range of performing the demanganization
treatment is a range down to a distance x, where the
distance in the depth direction from the surface is
set to X, and the distance x is preferably not less
than 5 ij.m nor more than 50 fim. When the distance x
is less than 5 nm, it is difficult to bring the
accumulation degree of the {200} planes to 30% or
more in the diffusion treatment after the
demanganization. For this reason, the preferred
distance x in the depth direction from the surface is
set to 5 fim or more. Further, when the distance is
greater than 50 jum, a long time is required for the
demanganization, and further the accumulation degree
of the {200} planes is saturated, and thus it is not
advantageous industrially. Thus, the preferred
distance x is set to 50 /x m or less.
[0110] (Accumulation degree of the {200} planes
after the demanganization)
- 52 -
It is preferred that the accumulation degree of
the {200} planes in the region having been subjected
to the demanganization treatment should become 20% or
more after the demanganization by performing the
decarburization annealing under the above conditions.
When the accumulation degree of the {200} planes is
less than 20%, it is difficult to bring the
accumulation degree of the {200} planes to 30% or
more in the diffusion treatment to be performed
subsequently. The upper limit of the accumulation
degree of the {200} planes is preferably set to 99%.
When it is greater than 99%, the magnetic property
deteriorates.
[0111] [Different metal]
Next, a different metal except Fe is made to
diffuse into the base metal sheet having had the
surface layer portion turned into the a phase by the
decarburization to increase the region of the {100}
texture in the thickness direction of the metal sheet
As the different metal, the ferrite-forming element
is used. As a procedure, first, the different metal
is bonded in a layered form as the second layer to
one surface or both surfaces of the base metal sheet
made of the Fe-based metal of the a - y transforming
component. Then, a region alloyed by having had
elements of the different metal diffuse thereinto is
turned to have the a single phase based component and
to be able to be maintained as not only the region
having been subjected to the decarburization (or
- 53 -
^r
further the demanganization) to be transformed to the
a phase, but also a seed oriented in {100} for
increasing the accumulation degree of the {200}
planes in the metal sheet. As such a ferrite-forming
element, at least one type of Al, Cr, Ga, Ge, Mo, Sb,
Si, Sn, Ta, Ti, V, W, and Zn can be used alone or in
a combined manner.
[0112] As a method of bonding the different metal in
a layered form to the surface of the base metal sheet,
there can be employed various methods such as a
plating method of hot dipping, electrolytic plating,
or the like, a rolling clad method, a dry process of
PVD, CVD, or the like, and further powder coating.
As a method of efficiently bonding the different
metal for industrially implementing the method, the
plating method or the rolling clad method is suitable.
[0113] The thickness of the different metal before
the heating when the different metal is bonded is
preferably not less than 0.05 p.m nor more than 1000
jum. When the thickness is less than 0.05 jum, it is
not possible to obtain the sufficient accumulation
degree of the {200} planes. Further, when the
thickness exceeds 1000 p.m, even when the different
metal layer is made to remain, its thickness becomes
larger than necessary.
[0114] [Heating and diffusion treatment]
The base metal sheet having had the ferriteforming
element bonded thereto is heated up to the A3
point of the base metal sheet, to thereby make the
- 54 -
#
ferrite-forming element diffuse into the partial or
whole region in the base metal sheet to make the base
metal sheet alloyed therewith. The a phase is
maintained in the region alloyed with the ferriteforming
element. Alternately, the ferrite-forming
element is made to diffuse into the inner portion
over the decarburized region to make the base metal
sheet alloyed therewith, and the alloyed region is
"turned to have the a single phase component partially,
and thereby the region is turned into the a phase.
At this time, the region is transformed while taking
over the orientation of the region formed by the
decarburization, so that the accumulation degree of
the {200} planes further increases. As a result, in
the alloyed region, a structure in which the
accumulation degree of the {200} planes in the a-Fe
phase becomes not less than 25% nor more than 50% and
in accordance with it, the accumulation degree of the
{222} planes in the a-Fe phase becomes not less than
1% nor more than 40% is formed.
[0115] Then, the base metal sheet is further heated
to a temperature of not lower than the A3 point nor
higher than ISOO'C and the temperature is held. The
region alloyed already is turned into an a single
phase structure that is not transformed to the y
phase, so that the {100} crystal grains are
maintained as they are, and in the region, the
crystal grains in the {100} texture preferentially
grow and the accumulation degree of the {200} planes
- 55 -
increases. Further, the region not having the a
single phase component is transformed to the y phase.
[0116] Further, when the holding time is prolonged,
the crystal grains in the {100} texture are united to
one another to preferentially grow. As a result, the
accumulation degree of the {200} planes further
increases. Further, with the further diffusion of
the ferrite-forming element, the region alloyed with
the ferrite-forming element is transformed to the a
phase from the y phase. At this time, as shown in
Fig. 4A, in the regions adjacent to the regions to be
transformed, crystal grains 7 in the a phase oriented
in {100} are already formed, and at the time of the
transformation to the a phase from the y phase, the
regions alloyed with the ferrite-forming element are
transformed while taking over a crystal orientation
of the adjacent crystal grains 7 in the a phase.
Thereby, the holding time is prolonged and the
accumulation degree of the {200} planes increases.
Further, as a result, the accumulation degree of the
{222} planes decreases.
[0117] Incidentally, in order to finally obtain the
high accumulation degree of the {200} planes of 50%
or more, it is preferred that the holding time should
be adjusted to, at this stage, bring the accumulation
degree of the {200} planes in the a-Fe phase to 30%
or more and bring the accumulation degree of the
{222} planes in the a-Fe phase to 30% or less.
Further, when the A3 point or higher is held until
- 56 -
the whole metal sheet is alloyed, as shown in Fig. 4C,
the a single phase structures are formed up to the
center portion of the metal sheet and grain
structures oriented in {100} reach the center of the
metal sheet.
[0118] A holding temperature after the temperature
is increased is set to not lower than A3 point nor
higher than 1300^3. Even when the metal sheet is
heated at a temperature higher than 1300^1, an effect
with respect to the magnetic property is saturated.
Further, cooling may be started immediately after the
temperature reaches the holding temperature, or
cooling may also be started after the temperature is
held for 6000 minutes or shorter. When this
condition is satisfied, the achievement of high
accumulation of the seeds oriented in the {200} plane
further progresses to make it possible to more
securely bring the accumulation degree of the {200}
planes in the o-Fe phase to 30% or more after the
cooling.
[0119] [Cooling after the heating and diffusion
treatment]
After the diffusion treatment, when the cooling
is performed while the region that is not alloyed
with the ferrite-forming element is remaining, as
shown in Fig. 4B, at the time of the transformation
to the a phase from the y phase, the unalloyed
region is transformed while taking over the crystal
orientation of the regions in which the crystal
- 57 -
grains 9 in the a phase oriented in {100} are already
formed. Thereby, the accumulation degree of the
{200} planes increases, and the metal sheet having
the texture in which the accumulation degree of the
{200} planes in the a-Fe phase is not less than 30%
nor more than 99% and the accumulation degree of the
{222} planes in the a-Fe phase is not less than 0.01%
nor more than 30% is obtained, the crystal satisfying
the condition of the Z value grows, and a high
magnetic flux density can be obtained in an arbitrary
direction in the metal sheet plane.
[0120] Further, as shown in Fig. 4C, when the A3
point or higher is held until the whole metal sheet
is alloyed and the grain structures oriented in {100}
reach the center of the metal sheet, as shown in Fig.
4D, the metal sheet is cooled as it is, and the
texture in which the grain structures oriented in
{100} reach the center of the metal sheet can be
obtained. Thereby, the whole metal sheet is alloyed
with the different metal, and the metal sheet having
the texture in which the accumulation degree of the
{200} planes in the a-Fe phase is not less than 30%
nor more than 99% and the accumulation degree of the
{222} planes in the a-Fe phase is not less than 0.01%
nor more than 30% is obtained,
[0121] As above, the value of the accumulation
degree of the {200} planes and the remaining state of
the different metal on the surface of the base metal
sheet change depending on the holding time of the
- 58 -
i^Bi
temperature of the A3 point or higher and the holding
temperature. The example shown in Fig. 4B is in a
state where the grain structures oriented in {100} do
not reach up to the center of the metal sheet and the
different metal also remains on the surfaces, but it
is also possible to obtain the grain structures
oriented in {100} up to the center of the metal sheet
and to alloy all the second layers on the surfaces.
[0122] Incidentally, at the time of the cooling
after the diffusion treatment, a cooling rate is
preferably not less than O.l'C/sec nor more than SOOt)
/sec. When the cooling rate is less than 0.lt!^/sec, a
long time is required for the cooling, which is not
appropriate, and when the cooling rate is greater
than 500t/sec, the metal sheet is sometimes deformed,
and thus the cooling rate is prefierably 500t/sec or
less,
[0123] Incidentally, when the second layers are made
to remain on the obtainable Fe-based metal sheet
having a thickness of not less than 10 nm nor more
than 6 mm, the thickness of the second layer is
preferably set to not less than 0.01 jim nor more than
500 Aim. Further, a ratio of the a single phase
region alloyed at this stage is preferably 1% or more
in a cross section of the Fe-based metal sheet.
[0124] Further, it is also possible to form a
structure as shown in Fig. 5, and in this case, an
average cooling rate is set to satisfy the condition
similar to that of the first embodiment, and thereby
- 59 -
#
the above can be achieved.
EXAMPLE
[0125] Next, there will be explained experiments
conducted by the present inventors. Conditions and
the like in these experiments are examples employed
for confirming the applicability and effects of the
present invention, and the present invention is not
limited to these examples.
[0126] (Example 1)
In this example, base metal sheets of No, 1 to
No. 16 each made of a component A or B shown in Table
1 below were manufactured under various rolling
conditions, to then have various different metals
applied thereto as a second layer, and then Fe-based
metal sheets were fabricated, of which the previously
described Z value (= (A + 0.97B)/O.98C) and the
magnetic flux density difference A B were examined.
Further, the relationship between various
manufacturing conditions and an accumulation degree
of {200} planes was also examined. Further, effects
obtained by changing a starting temperature in an aregion
rolling process were also examined in detail.
[0127] [Table 1]
TUBLE I
CdPONENT
SERIES
A
B
C
D
E
A3
POINT
925
toio
915
B7tt
942
C
0.0008
0.0012
0.0032
0.0041
0.0105
Si
0.3
1.1
0.2
0.1
0.2
Mn
0.3
O.B
O.OB
1.5
0.5
Al
0.5
0.1
0.05
0.2
0.7
EiEMENT VASSX
P
0.0003
0.0002
0.0001
0.0001
0.0001
N
0.0002
0.0003
0.0003
0.0002
0^003
S
<0.0004
<0.0004
<0.0004
<0.0004
<0.0004
0
0.0002
0.0001
0.0001
0.0001
0.0001
OTHER
-
-
-
-
Cr: 0.5
- 60 -
#
[0128] First, ingots each having the component A or
B shown in Table 1 and a balance being composed of Fe
and inevitable impurities were melted by vacuum
melting. Then, these were used as rolling materials
to be worked into cold-rolled sheets (the base metal
sheets) each having a predetermined thickness under
conditions of hot rolling, a-region rolling, and cold
rolling shown in Table 2 below.
[0129] [Table 2]
- 61
9
TABLE2
BASE
MATERUl
1
2
1
«
1
1
7
1
•
II
11
IJ
It
U
li
II
17
OOHKMENT
Al
PONT
Ml
m
Uf
m
M
m
i «
IM
HI
iiii
ml
III!
1111
(III
nil
till
IIII
HOTROLUNQ
START
TEMKRATURE
nil
I IH
I I I I
I IU
I IH
itn
I IM
UN
UN
liM
1211
im
t2N
t2M
1211
1211
1211
TWICNESS
MM
IH
7U
7U
«t
m
m
1U
tu
211
211
2M
2N
Ml
2M
211
2M
]M
FN5H
TEMPERATURE
im
1IN
im
MK
INI
im
I IM
im
im
im
im
I IH
INI
IHI
INI
INI
INI
THDKNESS
Dm
M
H
H
H
M
H
H
H
REDUOTDN
RATO
-U2
-M2
-U2
-!«
- I i2
-122
-M2
- 1 ^
-IJ2
-172
-Mi
-IJ72
-1.72
-1.72
-172
-172
-172
a-REQDN ROIUNQ
START
TEMPERATURE
HI
m
ui
Tfi
I I I J
w
4N
IN
211
INI
I I I
I I I
7U
HI
Ml
IN
2fl
TWKNESS
M
H
n
H
H
H
H
i l
FMSH
TEMPERATUR
Et;
IN
IN
Nl
7M
IW
Ml
4n
IM
2M
IN
IN
771
HI
HI
4H
Nl
2H
TWXNESS
MM
2i
»
2J
2i
U
It
21
21
»
IJ
IJ
IJ
»
M
IJ
IJ
IJ
REOUCTDN
RATD
-IJI
-tJI
-IJI
-IJI
- IH
-IJI
-IJI
-IJI
- IH
-Ml
-2JI
-IJI
-2Jt
-2Jt
-2JI
-IJI
-UOOLORKIMQ
START
TICSKNESS
MM
»
2i
21
2J
2J
2J
2J
2J
21
IJ
IJ
IJ
IJ
IJ
IJ
IJ
IJ
FMBH
TMKNEft
M
U
IJ
IJ
IJ
IJ
IJ
IJ
IJ
IJ
l i
M
IJ
IJ
l i
IJ
l i
REDUCnON
RATD
- l i l
->H
-2H
-2il
-2H
-2Ji
• l i i
-2:N
-2n
-1.71
-1.71
-1,71
-1.71
-171
-1.71
-1.71
-171
TOTAL
REDUCTDN
RATO
-7.11
-7.11
-7.11
-7.11
-7.11
-7.11
-7.11
-i.ii
-7.11
- IH
- IM
• IM
- IM
- IM
- IM
MM .
> IM
REDUQTtmRATDOF
aREODN'OOlO
ROLLMa
-Ml
-IJI
-IJI
-IJI
-IJI
Ml
-Ml
, ' ; -Ml .
-Ml •
-IJI
-Ml
-Ml
-Ml
, -Ml
-Ml
-Ml
-Ml
••n
#
[0130] In the case of the component A, the ingots
each having a thickness of 250 mm heated to IISO'C
were first subjected to hot rolling at a reduction
ratio of -3.22 in terms of true strain, and hotrolled
sheets each having a thickness of 10 mm were
obtained. Next, these hot-rolled sheets were each
subjected to a.-region rolling at a reduction ratio of
-1.39 in terms of true strain at a temperature of 300
to lOOO'C. These rolled sheets obtained by the aregion
rolling were pickled, and then the base metal
sheets were obtained by cold rolling. At this time,
the reduction ratio was -2.53 in terms of true strain,
and as a result, the thickness of each of the
obtained base metal sheets was 0.2 mm.
[0131] In the case of the component B, the ingots
each having a thickness of 200 mm heated to 1200"C
were first subjected to hot rolling at a reduction
ratio of -2.93 in terms of true strain, and hotrolled
sheets each having a thickness of 15 mm were
obtained. Next, these hot-rolled sheets were each
subjected to a-region rolling at a reduction ratio of
-1.46 in terms of true strain at a temperature of 300
to 1050t. These rolled sheets obtained by the aregion
rolling were pickled, and then the base metal
sheets were obtained by cold rolling. At this time,
the reduction ratio was -1.95 in terms of true strain,
and as a result, the thickness of each of the
obtained base metal sheets was 0.5 mm.
[0132] With respect to the base metal sheets
- 63 -
#
obtained by the above procedure, a texture of a
surface layer portion of each of the base materials
was measured by X-ray diffraction to obtain an
accumulation degree of {200} planes and an
accumulation degree of {222} planes by the previously
described method. Further, thinning was performed so
that a structure could be observed from a direction
perpendicular to an L cross section, and a region up
to l/4t (t represents a thickness) from the surface
was observed. The main phase of each of the obtained
base metal sheets at room temperature was an a-Fe
phase. Further, as a result of measurement, the A3
point at which the a-y transformation occurred was
925°C in the component A and lOlO'C in the component B.
[0133] Next, both surfaces of each of the base metal
sheets of No. 1 to No. 17 shown in Table 2 were
coated with each of various different metal elements
as the second layer by a vapor deposition method, a
sputtering method, or an electroplating method. As
shown in Table 3 and Table 4 below, as the different
metal element, any one of Al, Si, Mo, Ga, Sn, Ti, Ge,
Sb, V, and W was selected. The thickness of each of
the coatings was as shown in Table 3 and Table 4.
[0134] Next, an experiment was performed in which a
heat treatment was performed on the base metal sheets
to each of which the second layers were bonded under
various conditions. A gold image furnace was used
for the heat treatment, and a holding time was
controlled by program control. During which the
- 64 -
#
temperature increased to be held, the heat treatment
was performed in an atmosphere vacuumed to a pressure
of 10'^ Pa level. At the time of cooling, in the case
of a cooling rate of it/sec or lower, temperature
control was performed in a vacuum by furnace output
control. Further, in the case of the cooling rate of
lO'C/sec or more, an Ar gas was introduced and the
cooling rate was controlled by adjustment of its flow
rate .
[0135] Here, there was examined a change in the
texture among a temperature increasing process of
heating up to the A3 point, a holding process of
heating to a temperature of not lower than the A3
point nor higher than 1300'C and holding the
temperature, and a cooling process of cooling to a
temperature of lower than the A3 point. Specifically,
three base metal sheets with the same combination of
the base material-coating conditions were prepared,
of which a change in the texture was examined by
performing a heat treatment experiment in each of the
processes.
[0136] A sample for the temperature increasing
process was fabricated in such a manner that the base
metal sheet was heated from room temperature to the
A3 point at a predetermined temperature increasing
rate and was cooled to room temperature without any
holding time. The cooling rate was set to lOOX^/sec.
The texture was measured by the method using the
previously described X-ray diffraction method, and
- 65 -
#
the X-ray was emitted from its surface, and the
accumulation degree of {200} planes in the a-Fe phase
and the accumulation degree of {222} planes in the a-
Fe phase were obtained in an inverse pole figure.
[0137] A sample for the holding process was
fabricated in such a manner that the base metal sheet
was heated from room temperature to a predetermined
temperature over the A3 point at a predetermined
temperature increasing rate and was cooled to room
temperature after a predetermined holding time. Then,
the texture of the fabricated sample was measured in
the same manner, and the accumulation degrees of
{200} and {222} planes in the a-Fe phase were
obtained.
[0138] A sample for the cooling process was
fabricated in such a manner that the base metal sheet
was heated from room temperature to a predetermined
temperature over the A3 point at a predetermined
temperature increasing rate and was cooled to room
temperature at a predetermined cooling rate after a
predetermined holding time. Further, in order to
evaluate the accumulation degrees of {200} and {222}
planes at an unalloyed position, a test piece was
fabricated by removing a layer from the surface of
the fabricated sample to a predetermined distance so
that the unalloyed position might become an
evaluation surface. Incidentally, when the whole
metal sheet was alloyed, the evaluation surface was
set to a position of 1/2 of the sheet thickness.
- 66
#
With regard to the measurement of the texture of the
fabricated sample, the X-ray was emitted from the
surface of the test piece and from a predetermined
surface of the test piece from which the layer was
removed, and the accumulation degrees of {200} and
{222} planes in the a-Fe phase of the surfaces were
obtained in the same manner.
[0139] Next, magnetometry was performed in order to
evaluate obtained products. First, the average
magnetic flux density B50 to a magnetizing force of
5000 A/m and the magnetic flux density difference AB
were obtained by using a SST (Single Sheet Tester).
At this time, a measurement frequency was set to 50
Hz. When the average magnetic flux density B50 was
obtained, as shown in Fig. 1, the magnetic flux
density B50 was obtained every 22.5° in a
circumferential direction of the product and an
average value of the magnetic flux densities B50 in
these 16 directions was calculated. Further, of the
magnetic flux densities B50 in these 16 directions,
the difference between the maximum value and the
minimum value was set to the magnetic flux density
difference AB. Next, the saturation magnetic flux
density Bs was obtained by using a VSM (Vibrating
Sample Magnetometer). The magnetizing force applied
at this time was 0.8 X 10^ A/m. An evaluation value
was set to the ratio B50/Bs of the average magnetic
flux density B50 to the saturation magnetic flux
density.
- 67 -
[0140] Further, by the previously described X-ray
diffraction, intensity ratios of {001}<470>, {116}<6
12 1>, and {223}<692> were calculated, and thereby
the previously described Z value was calculated.
[0141] Table 3 and Table 4 below show the
accumulation degrees of the {200} planes and the
accumulation degrees of the {222} planes measured in
the respective processes during the manufacture and
after the manufacture, the Z values of the obtained
Fe-based metal sheets, and evaluation results of the
magnetometry.
[0142] [Table 3]
- 68 -
- 69 -
IV s i q e j . ] [ef'TO]
mmmmmmmmmt^'
piH^^^#Fi«|iPliNli|ii! illTiIIJI1 JMTT!li|iJiii|i|iMili n'
' * * « * « - > > C B t e c 6 s e C B s c > > • « « • « « a « « « « « « • • • » « • • « « ^11
• • > • • • • • • • • • • • • • • i i i i i i i i i i i i i i i i i i i i i i it
:_ __ •' :: :: w< i f f i l i s f i t i i i l l l i i i i i l i i i i l i l i i i i i i l l i i i l l i i « | | |
i l H 1 1 s * c « s « s » s * i B « a | |H • '—= PI • = = ' = ' • = • =.. = .. = .. if
- - -; - - -r
•jl i
" •' — . . = = . . . = = = = = ». ' =. I f
III i
e c s s s c K 3 a f t s e e 5 C B S s C S R B s e B a « & £ e c e e B « « B S i : E C = e s j H B
C B B i l s B B B B e v S i ' B B S S e B l i s E B B C B V I I S E B S S B I I i a B e C " I H
E S ! i ( E i i i S E E i < C ! E E C E E t i I ! I ( C ! E i i ! I t f S i i i S i i i i 'iLl
l i i l l l t i i i t i l t l i l l i l i i l i l i i i i i i i i ' i l i t i B i i ' i i i -' H
t « S C E t I i t S i < t ( C t C E t | { t I t ( f S t l I l t i I I ! i t E ! C S t f S | |
i| i 111 i 1 i 1 i 1 i 1 i |l|i| i 11111 f 1 f 1 i 1 i |i|t| i | i | ! 111! | i 11 |t|t| S | i | i | i 111 i | S |i|i| ! | i | i | f 11 | i | i | i | -t \\ mimimmmmmmmimmmmmm
••• I--M-M---I-Ii
9
#
| | l f i i l l i l l i i ( l i i i | l i ( i i i i i l i i i i t l l i i f l i i i
< liillillHiisSNHJiiiilijiilliliiliigiliiiie^
L '- i ! • ! ! i ; i s ! 1 S ! i ! ! i ! i 1 i i ! ! i ! i ! i i S ! 1 ! i 3 i i ! 1
1 { : S ! i i l i S S I i 9 ! i l S i i l 9 l ! i 3 S 9 S a 3 i S 9 ! I ! 9 : 9 i i
* I- I S ! l : i ! ! ! S ! i ! 9 E i ! ! ! 9 S I S S ! S S 9 9 S ! S t S ! i ! 9 : !
1 « a a « > i ! a a a a s « I S 3 a q 3 ' e i i 3 a a 9 « s ! s > 9 a 3 « ! I « : a
1 i>l
'JF
S i f l S > 3 S a 3 3 a S S 3 9 3 S S S S B s a % l S S S x a 9 3 a 3 3 3 » 3 3 3 3 - 3 3
' 1*1
!.
n n i l S * * 3 - 3 3 3 a 3 « 3 s 3 s s a s a a a a s 3 3 3 ^ 3 3 3 3 3 3 3 9 3 = 3 3 - 3 3
S f i k i i l c * * > « s s : s ! • • • s • « K a s « s • s t s « a s « a • * B a s t s a s B s s a t
i )i
' l l " ! ! > i ! ! i ! l l l l l l i l l i i l l l l l ! ! ! ! ! ! < ! i l l l i l l l
1 I'l
9i>l
l i l M * > * s > * 3 X = i i t s 3 8 x i t = ] t a a l t S B a a 8 = a S & & i a s s B S S « a
1
II i { i : : ! i : ; { 1 : { 1 : ; 1 : ; i i ; 1 i s ; i i t i i i i : i { : i { i
,« i ! l ! l l ! ! i ! [ l i ! ! l ! l i ! l ! ! ! ! ! ! l l l ! ! t ! M I ! !l
S g
1 I s a a a a s c a a s s a s a s s a a a a B s a s a s a s a a a a a s a x s a a s a
. 1 s a s a s a a s a a s a a s a a a a a a a a s a a a a a a a a a a a a a a a a a
1 _ .
1 4 a s s s a a a e a s B a a a a e a s a a y a a e a s v a x a a a r s e v a a a t t
a t » 3 a s s s • > • • • > > • a « B B « • s s s t K s e m * a a c a c a s • • • •
i
[0144] In each of present invention examples, it was
possible to confirm that Z is not less than 2.0 nor
more than 200, the magnetic flux density difference A
B becomes a small value as compared to comparative
examples, and a high magnetic flux density can be
- 70 -
#
obtained thoroughly in an in-plane circumferential
direction. Further, in these Fe-based metal sheets,
it was possible to confirm that an excellent magnetic
property in which the value of B50/Bs is 0.80 or more
is obtained.
[0145] Further, in the present invention examples,
as shown in Table 2 to Table 4, it was possible to
confirm that the {200} plane in the a-Fe phase is
likely to be highly accumulated at each of the stages
of the heat treatment.
[0146] Further, an L cross section of each of the
present invention examples was observed, and thereby
it was confirmed that the a single phase region made
of the a single phase based component exists in at
least a partial region including the surfaces and a
ratio of the a single phase region to the L cross
section is 1% or more.
[0147] When the Z value was not less than 2 nor more
than 200 as defined in the present invention as above,
it was possible to confirm that a high magnetic flux
density is obtained thoroughly in the in-plane
circumferential direction. Further, in order to
obtain the Fe-based metal sheet as above, the aregion
rolling was performed at a temperature of
higher than SOOt and lower than the A3 point between
the hot rolling and the cold rolling, thereby making
it possible to obtain an intended product.
[0148] In contrast to this, when the base metal
sheets obtained by performing the rolling under the
- 71 -
#
conditions not satisfying the requirements of the
present invention were used, it was not possible to
obtain a high magnetic flux density such as that in
the present invention examples in the in-plane
circumferential direction thoroughly.
[0149] (Example 2)
In this example, base metal sheets of No. 18 to
No. 35 each made of a component C, D, or E shown in
Table 1 were manufactured under various rolling
conditions, to then have various different metals
applied thereto as a second layer, and then Fe-based
metal sheets were fabricated, of which the previously
described Z value (= (A + 0.97B)/O.98C) and the
magnetic flux density difference A B were examined.
Further, the relationship between various
manufacturing conditions and an accumulation degree
of {200} planes was also examined. Further, effects
obtained by changing a starting temperature in an aregion
rolling process were also examined in detail.
[0150] First, ingots each having the component C, D,
or E shown in Table 1 arid a balance being composed of
Fe and inevitable impurities were melted by vacuum
melting. Then, these were used as rolling materials
to be worked into cold-rolled sheets (the base metal
sheets) each having a predetermined thickness under
conditions of hot rolling, a-region rolling, and cold
rolling shown in Table 5 below.
[0151] [Table 5]
- 72 -
n^
«
TABL£5
wet
MATEHM.
11
)l
M
11
a
n
H
»
M
»
?k
M
M
II
U
•t
M
M
OOMPONEMT
C
0
0
0
C
, c
0
D
D
D
D
FOMT
I II
Hi
III
I II
Hi
I II
171
171
171
171
V*
Ml
Mi
Mi
Mi
Mi
Ml
Ml
HOTNM.UNQ
START
1IMPERATURE
INI
im
im
INI
im
INI
im
im
IIM
im
IWI
I2N
I2M
liN
liM
tin
liN
liM
THOKNESS
Ml
in
M
iM
iM
HI
iM
HI
in
71
M
H
2M
Ml
Ml
Ml
m
Ml
IW
FNBH
TEMPERATURE
IM
IW
m
IM
IM
Ml
IN
IN
IN
IN
y»
UN
1MI
im
1IN
INI
im
INI
THDKNES8
N
N
M
11
1
«
11
1i
11
II
1i
i l
N
M
H
H
H
N
REDUOTDN
RAID
-Ml
- IM
- i l l
- I JW
-lii
-Ml
- in
- in
-111
- in
- in
-1J7
-117
-117
-1J7
-tJ7
-1J7
-1J7
a-R£QX)N ROU»Q
START
TEMPERATURE
m
TN
7N
7N
7N
7N
IN
HI
in
m
m
7M
7U
7M
7M
7H
711
7n
THNCNESS
n
N
M
N
M
N
n
N
M
N
nsN
TEMPERATURE
1!
HI
HI
HI
HI
HI
HI
171
171
171
171
Vf
171
171
171
171
171
171
171
THOKNESS REDUCTDN
RATD
-Ml
-1.71
-m
•Ml
- in
-in
-Ml
-in
-i.tt
- in
-Ml
-Ml
-Ml
-Ml
-Ml
-Ml
- l it
-Ml
COlDROllMa
START
THCKNESS
FMBH
THCKNESS
IN
in
in
in
i n
in
M
i j
u
M
M
1
i
1
M
1.1
in
111
REDUOnW
RAH)
-174
-U»
- I J«
•m
-1«
-1JI
- in
- in
- in
-Mi
- in
-tm
-1.11
- i j i
-IM
-in
-4JI
- IM
TOTAL
REOUOTIM
RATD
- in
- in
- in
- in
- in
- in
-Ml
-1.71
- i l l
-Ml
- in
-M7
- tn
-M7
- IM
-7i7
-717
-M7
aREQDN«
OOLO
ROOMS
•Lit
-»n
- tn
- in
-I.II
-Mt
- IM
-Ml
- in
-Ml
- in
-m
•m
- in
-U1
-Ul
•Ml
•111
0
[0152] In the case of the component C, first, the
ingots each having a thickness of 200 mm heated to
1050^) were each subjected to hot rolling at a
reduction ratio of -1.20 to -3.22 in terms of true
strain, and hot-rolled sheets each having a thickness
of 4 mm to 60 mm were obtained. Next, a-region
rolling was started at 700*^, and these hot-rolled
sheets were each subjected to the a-region rolling at
a reduction ratio of -0.69 to -3.40 in terms of true
strain to a thickness of 2 mm. Then, these rolled
sheets were pickled, and then the base metal sheets
were obtained by cold rolling. At this time, the
reduction ratio was -1.74 in terms of true strain,
and as a result, the thickness of each of the
obtained base metal sheets was 0.35 mm.
[0153] In the case of the component D, first, the
ingots each having a thickness of 20 mm to 300 mm
heated to 1050^ were each subjected to hot rolling at
a reduction ratio of -0.29 to -3.00 in terms of true
strain, and hot-rolled sheets each having a thickness
of 15 mm were obtained. Next, a-region rolling was
started at esot, and these hot-rolled sheets were
each subjected to the a-region rolling at a reduction
ratio of -1.46 in terms of true strain to a- thickness
of 3.5 mm. Then, these rolled sheets were pickled,
and then the base metal sheets were obtained by cold
rolling. At this time, the reduction ratio was -1.95
in terms of true strain, and as a result, the
thickness of each of the obtained base metal sheets
- 74 -
•
was 0.50 mm.
[0154] In the case of the component E, first, the
ingots each having a thickness of 240 mm heated to
1200t were each subjected to hot rolling at a
reduction ratio of -2.77 in terms of true strain, and
hot-rolled sheets each having a thickness of 15 mm
were obtained. Next, a-region rolling was started at
750"C and these hot-rolled sheets were each subjected
to the a-region rolling at a reduction ratio of -1.61
in terms of true strain to a thickness of 6.0 mm.
Then, these rolled sheets were pickled, and then the
base metal sheets were obtained by cold rolling. At
this time, each of the reduction ratios was -0.69 to
-6.40 in terms of true strain, and as a result, the
thickness of each of the obtained base metal sheets
was 0.01 mm to 3.0 mm.
[0155] With respect to the base metal sheets
obtained by the above procedure, a texture of a
surface layer portion of each of the base materials
was measured by X-ray diffraction to obtain an
accumulation degree of {200} planes and an
accumulation degree of {222} planes by the previously
described method. Further, thinning was performed so
that a structure could be observed from a direction
perpendicular to an L cross-section, and a region up
to l/4t from the surface was observed. The main
phase of each of the obtained base metal sheets at
room temperature was an a-Fe phase. Further, as a
result of measurement, the A3 point at which the a - y
- 75 -
transformation occurred was 915t) in the component C,
SVO'C in the component D, and 942*0 in the component E,
[0156] Next, both surfaces of each of the base metal
sheets of No. 18 to No. 35 shown in Table 5 were
coated with each of various different metal elements
as the second layer by a vapor deposition method, a
sputtering method, an electroplating method, or a hot
dipping method. As shown in Table 6 and Table 7
below, as the different metal element, any one of Al,
Si, Ga, Sn, V, W, Mo, and Zn was selected. The
thickness of each of the coatings was as shown in
Table 6 and Table 7.
[0157] Next, an experiment was performed in which a
heat treatment was performed on the base metal sheets
to each of which the second layers were bonded under
various conditions. As a method of the experiment,
the experiment was performed by the same method
described in Example 1. Further, the observation of
a texture in this period was also performed by the
same method described in Example 1.
[0158] Further, magnetometry was performed in the
same manner as that in Example 1 in order to evaluate
obtained products, and further the Z value was
calculated by X-ray diffraction.
[0159] Table 6 and Table 7 below show the
accumulation degrees of the {200} planes and the
accumulation degrees of the {222} planes measured in
the respective processes during the manufacture and
after the manufacture, the Z values of the obtained
- 76 -
- LL -
IL s i q e x ] [I9I0]
1 1
TITTTTTTT!lT^s|i|i|i|^l i t i l i i * ( l
DlIISiillillllSlliilHiillllllllllll 1 V i ! 1 1 S i ! I 3 ! ! s ! S ! ! i ! i I 1 ! ! ! ! ! i i i i ! i ! ! ; i
j { I S ] l ! ) l I 9 I 9 9 S 9 S S ] 9 i 9 S 3 : i S i i l i S i l i i i 3
' l - 9 S S ! S ! > ! ! 9 ! 9 < S S ! 5 ! ! ! ! i i 5 S S i S i S 5 ! ! S S : S
1 •• • • B s i i « s i i a | a > a 3 a 9 « s i | | a 3 a > > | t 3 3 i s > « I S
']pr
SilS = s a 3 a s s a s 3 s a 5 3 a > 9 a s a a * * a a 9 S 5 a a a s a 5 s s
' ± : : : • : : : : : : • : : : : : : : • : : : : : • • : : • : : : : : : :
IS i l l ! ' - - ' ' - - ' ! = * - - = ^ ' 9 > 3 9 a 9 3 : < a a 9 = s : 9 3 : a : : 9
H o i i i l l l i l l i l l l i l l i l i l l i f i l l l l i l l i l l i i
1 1 i l l s : 9 9 > 3 3 9 « : a : 3 a a s > a : : 3 3 ° « s : a : 9 « r 3 : a a 3
1 | | i 5 s S f t a s = B & a a 8 a K B S B E S S B B 3 « B B s a a x a B s a s s
i H
11 S t S t I 9 l f S ( E ! S ( l i > i i l i l i l l I i I i i i i : 9 I 9
[iJ . .
^ i !
,Hl|l|!tl|i|!|l|lit|i|||||inhh!>!>l!l!l!|!J!|M!l|!pJ!p
h ~ • • .:.T..-7
1 B < B < B a > a a > i i l f f B « a < < < a j < a < < « i « a < a a « a
l l 3 3 3 3 a s 3 a a a 3 a 3 3 a - - - 3 : 9 a - - - 9 : 9 a - - - 3 : 9 9
1 t S ! s a B s i s B i ( g a B | s a B t i i J ! ! B 3 i i i : i i i t i E
[0162] In each of present invention examples, it was
possible to confirm that the magnetic flux density
difference A B becomes a small value as compared to
comparative examples, and a high magnetic flux
density is obtained thoroughly in an in-plane
circumferential direction. Further, in these Febased
metal sheets, it was possible to confirm that
- 78 -
an excellent magnetic property in which the value of
B50/BS is 0.86 or more is obtained.
[0163] Further, in the present invention examples,
as shown in Table 5 to Table 7, it was possible to
confirm that the {200} plane in the a-Fe phase is
likely to be highly accumulated at each of the stages
of the heat treatment.
[0164] Further, an L cross section of each of the
present invention examples was observed, and thereby
it was confirmed that the a single phase region made
of the a single phase based component exists in at
least a partial region including the surfaces and a
ratio of the a single phase region to the L cross
section is 1% or more.
[0165] When the Z value was not less than 2 nor more
than 200 as defined in the present invention as above,
it was possible to confirm that a high magnetic flux
density is obtained thoroughly in the in-plane
circumferential direction. Further, in order to
obtain the Fe-based metal sheet as above, the aregion
rolling was performed at a temperature of 300t)
or higher and lower than the A3 point between the hot
rolling and the cold rolling, thereby making it
possible to obtain an intended product.
[0166] In contrast to this, when the base metal
sheets obtained by performing the a-region rolling
under the condition not satisfying the requirements
of the present invention were used, it was not
possible to obtain a high magnetic flux density such
- 79 -
as that in the present invention examples in the inplane
circumferential direction thoroughly.
[0167] (Example 3)
In this example, as base metal sheets, Fe-based
metal sheets were fabricated in a manner that pure
irons each containing C: 0.050 mass%. Si: 0.0001
mass%, and Al: 0.0002 mass%, and having a balance
being composed of Fe and inevitable impurities were
subjected to decarburization to have Al applied
thereto as a second layer, of which the previously
described Z value (= (A + 0.97B)/O.98C) and the
magnetic flux density difference A B were examined.
Further, the relationship between manufacturing
conditions and an accumulation degree of {200} planes
was also examined.
[0168] First, ingots were melted by vacuum melting,
and then were subjected to hot rolling and cold
rolling to be worked to a predetermined thickness,
and the base metal sheets each composed of the
previously described composition were obtained.
Incidentally, the Al point of the base metal sheets
was 121X:.
[0169] In the hot rolling, the ingots each having a
thickness of 230 mm heated to lOOOT) were thinned down
to a thickness of 50 mm, and hot-rolled sheets were
obtained. Sheet materials having various thicknesses
were cut out from these hot-rolled sheets by
machining and then were subjected to the cold rolling,
and thereby cold-rolled sheets each having a
- 80
#
thickness of 8 fim to 750 fim (the base metal sheets)
were obtained.
[0170] Incidentally, the main phase of each of the
base metal sheets at room temperature was an a-Fe
phase and as a result of measurement, the A3 point at
which the a - y transformation occurred was Silt.
Further, a texture in the a-Fe phase of each of the
base metal sheets was measured by X-ray diffraction,
and by the previously described method, an
accumulation degree of {200} planes and an
accumulation degree of {222} planes were obtained.
Further, as a result that up to the cold rolling was
performed, it was confirmed that of each of the base
metal sheets, the accumulation degree of the {200}
planes is 20 to 26% and the accumulation degree of
the {222} planes is 18 to 24%.
[0171] Next, these base metal sheets were subjected
to decarburization annealing so that a decarburized
depth (a distance x) might become 1 fim to 59 /xm. A
decarburization condition was set that the
temperature is SOOtl and the decarburization time is
0.05 minutes to 550 minutes. With regard to the
atmosphere during the decarburization annealing, a
strong decarburizing atmosphere was applied in the
case of the decarburization annealing being performed
for one minute or shorter, and in the case of the
decarburization annealing being performed for longer
than one minute, a weak decarburizing atmosphere was
applied in the first half of the decarburization
- 81 -
annealing and a strong decarburizing atmosphere was
applied in the second half of the decarburization
annealing.
[0172] Then, after the decarburization annealing was
performed, the decarburized depth and the C content
of a decarburized region were measured and a
structure and a crystal orientation of a surface
layer were examined. The measurement of the crystal
orientation was performed by the method using the
previously described X-ray diffraction method, the Xray
was emitted from the surface, and the
accumulation degree of the {200} planes in the a-Fe
phase was obtained.
[0173] After the decarburization annealing, both
surfaces of each of the base metal sheets were coated
with Al as the second layer by an ion plating method
(hereinafter, an IP method) to each have a thickness
of 1 /z m.
[0174] Next, an experiment was performed in which a
heat treatment was performed on the base metal sheets
to each of which the second layers was bonded under
various conditions. A gold image furnace was used
for the heat treatment, and a temperature increasing
rate, a holding temperature, and a holding time were
variously controlled by program control. During
which the temperature increased to be held, the heat
treatment was performed in an atmosphere vacuumed to
a pressure of 10'^ Pa level. At the time of cooling,
in the case of a cooling rate of lt;/sec or lower,
- 82 -
temperature control was performed in a vacuum by
furnace output control. Further, in the case of the
cooling rate of lOt^/sec or more, an Ar gas was
introduced and the cooling rate was controlled by
adjustment of its flow rate.
[0175] Further, the observation of the texture in
this period was also performed by the same method
described in Example 1. Further, magnetometry was
performed in the same manner as that in Example 1 in
order to evaluate obtained products, and further the
Z value was calculated by the X-ray diffraction.
[0176] Further, an alloyed ratio in the second layer
and a ratio of the a single phase region were defined
and obtained as follows.
[0177] Plane distribution of the Fe content and
plane distribution of the Al content were measured by
using an EPMA (Electron Probe Micro-Analysis) method,
with a field of view of an L direction 1 mm X the
total thickness in an L cross section. First, as the
alloyed ratio in the second layer, areas of a region
satisfying Fe ^ 0.5 mass% and Al ^ 99.5 mass% before
and after the heat treatment were obtained. Then,
the alloyed ratio of the second layer was defined as
(So — S)/So X 100, where an area when Al was applied
and the heat treatment was not performed was set to So
and an area in the Fe-based metal sheet on which the
whole heat treatment was completed was set to S.
[0178] Further, the ratio of the a single phase
region was defined as (T/To) X 100, where an area of
- 83 -
a cross section of the Fe-based metal sheet after the
heat treatment, observed in the L cross section was
set to To and an area of a diffused region of the
different metal after the heat treatment was set to T
Incidentally, when the second layer was Al, an area
of a region satisfying Al ^ 0.9 mass% was set to T.
[0179] Table 8 shows the base metal sheets and
conditions of the decarburization and the heat
treatment, and shows the accumulation degrees of the
{200} planes and the accumulation degrees of the
{222} planes measured during the manufacture (after
the decarburization annealing) and after the
manufacture (after the diffusion treatment), the Z
values of the obtained Fe-based metal sheets, the
alloyed ratios of the second layers, and evaluation
results of the magnetometry.
[0180] [Table 8]
84 -
111! ii!
9- I
h imi
Ii
example 203, and in the case of not heating to a
temperature of the A3 point or higher as in a
comparative example 204, it was not possible to
obtain a high magnetic flux density in the in-plane
circumferential direction thoroughly as in the
present invention examples. Further, even when the
temperature was increased to a higher temperature and
the holding time was made longer as in present
invention examples 228 and 229, the similar effect
was able to be obtained, but the significant effect
did not appear.
[0185] (Example 4)
In this example, as the ferrite-forming element,
Sn, Al, Si, Ti, Ga, Ge, Mo, V, Cr, or As was applied
to the second layer, and the relationship between the
case where demanganization was performed in addition
to decarburization and an accumulation degree of
{200} planes was examined.
[0186] First, base metal sheets containing six types
of components F to K shown in Table 9 below and
having a balance being composed of Fe and inevitable
impurities were prepared. Ingots were each melted by
vacuum melting to then be worked to a predetermined
thickness by hot rolling and cold rolling, and the
above-described base metal sheets were obtained.
Incidentally, the Al point of each of these base
metal sheets was 727*^.
[0187] [Table 9]
- 87 -
#
TABLE 9 (MASS%)
STEEL
TYPE
F
G
H
I
J
K
Ar3
POINT
877
880
867
771
773
859
C
0.03
0.03
0.05
0J50
OilO
0.10
Si
0.06
0.10
0.05
0.1
1.00
030
Mn
0.15
0.25
1.00
030
0.12
150
Al
0.0005
0.0004
0.0003
0.0004
0.0030
0.0030
P
0.0001
0.0002
0.0001
0.0002
0.0020
0.0020
N
0.0002
0.0001
0.0002
0.0002
0.0001
0.0001
S
<0.0004
<0.0006
<0.0004
<0.0004
,
{116}<6 12 1>, and {223}<692> directions in a sheet
plane by X-ray diffraction are set to A, B, and C
respectively and Z = (A + 0.97B)/0.98C is satisfied,
a Z value is not less than 2.0 nor more than 200.
[Claim 2] The Fe-based metal sheet according to
claim 1, wherein
said ferrite-forming element diffuses from a
surface to be alloyed with Fe.
[Claim 3] The Fe-based metal sheet according to
claim 1 or 2, wherein
a layer containing said ferrite-forming element
is formed on at least one side of surfaces of the Febased
metal sheet, and said ferrite-forming element
that has diffused from part of the layer is alloyed
with Fe.
[Claim 4] The Fe-based metal sheet according to
claim 3, wherein
a thickness of the layer containing said ferriteforming
element is not less than 0.01 ^m nor more
than 500 ^m.
[Claim 5] The Fe-based metal sheet according to any
one of claims 1 to 4, wherein
an accumulation degree of {200) planes is not
less than 30% nor more than 99%, and an accumulation
- 97 -
ORIGINAL 9l94^»13i
degree of {222} planes is not less than 0.01% nor
more than 30%.
[Claim 6] The Fe-based metal sheet according to any
one of claims 1 to 5, wherein
said ferrite-forming element is one type of
element or more selected from a group consisting of
Al, Cr, Ga, Ge, Mo, Sb, Si, Sn, Ta, Ti, V, W, and Zn.
[Claim 7] The Fe-based metal sheet according to any
one of claims 1 to 6, wherein
at least a partial region including the surfaces
of the Fe-based metal sheet is an a single phase
region made of an a single phase based component, and
a ratio of the a single phase region to a cross
section of the Fe-based metal sheet is 1% or more.
[Claim 8] The Fe-based metal sheet according to any
one of claims 1 to 7, wherein
a thickness of the Fe-based metal sheet is not
less than 10 ju m nor more than 6 mm.
[Claim 9] The Fe-based metal sheet according to any
one of claims 1 to 8, wherein
the a single phase region is formed on a front
surface side and a rear surface side of the Fe-based
metal sheet, and a crystal grain straddling the a
single phase region on the front surface side and the
a single phase region on the rear surface side is
formed.
[Claim 10] A manufacturing method of an Fe-based
metal sheet, comprising:
performing hot rolling on a cast slab containing
- 98 -
250CT20B
ORIGINAL DLi*ji ^ ,
C: less than 0.02 mass% and made of an Fe-based metal
of an a-y transforming component at a temperature of
an A3 point of the cast slab or higher to obtain a
hot-rolled sheet;
performing a-region rolling on the hot-rolled
sheet at a temperature of 300*^ or higher and lower
than the A3 point of the cast slab to obtain a rolled
sheet;
performing cold rolling on the rolled sheet to
obtain a base metal sheet having a thickness of not
less than 10 /z m nor more than 6 mm;
bonding a ferrite-forming element to one surface
or both surfaces of the base metal sheet;
heating the base metal sheet having had the
ferrite-forming element bonded thereto up to an A3
point of the base metal sheet; and
further heating the heated base metal sheet to a
temperature of not lower than the A3 point of the
base metal sheet nor higher than 1300^^ and holding
the base metal sheet; and
cooling the heated and held base metal sheet to a
temperature of lower than the A3 point of the base
metal sheet.
[Claim 11] The manufacturing method of the Fe-based
metal sheet according to claim 10, wherein
a reduction ratio in the a-region rolling is -
1.0 or less in terms of true strain, and the sum of
the reduction ratio in the a-region rolling and a
reduction ratio in the cold rolling is -2.5 or less
2 5 OCT 2015
- 99 -
ORIGINAL
in terms of true strain. * 5 OCT OMX
[Claim 12] The manufacturing method of the Fe-based
metal sheet according to claim 10 or 11, wherein
a reduction ratio in the hot rolling is -0.5 or
less in terms of true strain.
[Claim 13] A manufacturing method of an Fe-based
metal sheet, comprising:
heating a steel sheet containing C: not less than
0.02 mass% nor more than 1.0 mass%, having a
thickness of not less than 10 nm nor more than 6 mm,
and made of an Fe-based metal of an a - y transforming
component to a temperature of an Al point or higher
and a temperature at which a structure is turned into
an a single phase when decarburization is performed
until C becomes less than 0.02 mass%, to obtain a
base metal sheet that has been subjected to
decarburization in a range of not less than 5 urn nor
more than 50 fim in a depth direction from its surface
until C becomes less than 0.02 mass%;
bonding a ferrite-forming element to one surface
or both surfaces of the base metal sheet;
heating the base metal sheet having had the
ferrite-forming element bonded thereto up to an A3
point of the base metal sheet; and
further heating the heated base metal sheet to a
temperature of not lower than the A3 point of the
base metal sheet nor higher than ISOOtl and holding
the base metal sheet; and
cooling the heated and held base metal sheet to a
100 -
OPiQlWt^^
\ 'p Ma i>.
temperature of lower than the A3 point of the base 2 5 O^T 901^
metal sheet.
[Claim 14] The manufacturing method of the Fe-based
metal sheet according to claim 13, wherein
the steel sheet made of the Fe-based metal
further contains Mn of 0.2 mass% to 2.0 mass%, and
decarburization and demanganization are performed in
a combined manner.
[Claim 15] The manufacturing method of the Fe-based
metal sheet according to claim 13 or 14, further
comprising:
performing carburization on a steel sheet
containing C: less than 0.02 mass%, having a sheet
thickness of not less than 10 /i m nor more than 6 mm,
and made of an Fe-based metal of an a-y transforming
component.to control C to not less than 0.02 mass%
nor more than 1.0 mass%.