materials
Article
Softened Microstructure and Properties of 12 µm Thick Rolled
Copper Foil
Rui Feng 1 , Weichao Zhao 1 , Yumei Sun 1 , Xiaowen Wang 1 , Benkui Gong 1, *, Baoping Chang 2 and Tianjie Feng 2






Citation: Feng, R.; Zhao, W.; Sun, Y.;
Wang, X.; Gong, B.; Chang, B.; Feng,
T. Softened Microstructure and
Properties of 12 µm Thick Rolled
Copper Foil. Materials 2022, 15, 2249.
https://doi.org/10.3390/
ma15062249
Academic Editors: Filippo Berto,
Abílio M.P. De Jesus and José
A.F.O. Correia
Received: 13 February 2022
Accepted: 14 March 2022
Published: 18 March 2022
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iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
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4.0/).
Materials 2022, 15, 2249. https://doi.org/10.3390/ma15062249
1 School of Materials Science and Engineering, Shandong University of Technology, Zibo 255000, China;
fengrui@sdut.edu.cn (R.F.); zhaoweichao1998@163.com (W.Z.); sunyumei4243@163.com (Y.S.);
lvhupo@126.com (X.W.)
2 Heze Guangyuan Copper Strip Co., Ltd., Heze 274009, China; gycf@vip.sina.com (B.C.);
gycs@vip.163.com (T.F.)
* Correspondence: gongben69@163.com
Abstract: Up to now, 12 µm thick rolled copper foil is the thinnest rolled copper foil that can be
stably produced. The softened microstructure and properties of 12 µm thick rolled copper foil were
systematically studied in this paper. The softened process consists of thermal treatment at 180 ◦ C for
different times. The results show that the softened annealing texture is mainly cubic texture, and the
cubic texture fraction increases with the increase in annealing time. The cubic texture fraction reaches
the highest (34.4%) after annealing for 60 min. After annealing for 1–5 min, the tensile strength and
the bending times decrease significantly. After annealing for 10–60 min, the tensile strength tends to
be stable, and the bending times increase slightly. With the increase in annealing time, the electrical
conductivity increases gradually, reaching 92% International Annealed Copper Standard (IACS) after
annealing for 60 min. Electrical conductivity can be used as a fast and effective method to analyze the
microstructure of metals.
Keywords: rolled copper foil; microstructure; texture; properties; electrical properties
1. Introduction
Rolled copper foil is widely used in the fields of flexible printed circuit board, lithium-
ion battery, artificial intelligence, aerospace, etc. [1–3]. With the development of being
miniaturized, lightweight, high speed and multi-functional in electronic and electrical
components, higher requirements are put forward for the processing quality [4]. The
etching processing is the key technology used to prepare high-end circuit board, especially
for the fine flexible printed circuit board with the line width and line distance of no less
than 30 µm [5,6]. The etching processing is an unstressed processing method. Firstly, the
photoresist is used to protect the part of the workpiece, then, a strong oxidant is used to
etch the other parts, and finally, the required components are obtained [7]. The etching
processing has strict requirements on the internal stress, warpage, surface quality and
etching performance of rolled copper foil [8,9].
With the continuous development of electronic products and the improvement of etch-
ing performance requirement, higher requirements are put forward for the state of rolled
copper foil of fine flexible printed circuit board [10]. At present, the 180 ◦ C softened rolled
copper foil is mainly used in the field of high-end flexible printed circuit board, while the
rolled copper foil without softened annealing cannot be used in this field [11]. Additionally,
the flexible printed circuit board requires good bending resistance performance [12]. Previ-
ous research has shown that the uniform grain orientation reduces the stress concentration
at the grain boundary, which is helpful to improve the bending resistance performance of
copper foil [13,14]. Obtaining uniform grain orientation by softened annealing is the basis
of improving the bending resistance performance of rolled copper foil.
https://www.mdpi.com/journal/materials
Materials 2022, 15, 2249 2 of 17

Therefore, the softening of copper foil has a very important influence on its etching
and bending resistance performance. The deformation rate of 12 µm thick rolled copper foil
is more than 95%, which leads to the existence of large internal stress. So far, 12 µm thick
rolled copper foil is the thinnest rolled copper foil that can be stably produced. In order to
further improve its etching performance, especially the bending resistance performance,
the research on the softened microstructure and properties has gradually attracted the
attention of scholars [15]. In addition, for the 12 µm thick rolled copper foil, creating a good
sample for microstructure observation and properties testing is a challenging task. In this
paper, the softened microstructure and properties of 12 µm thick rolled copper foil were
systematically studied.

2. Experimental Materials and Methods

The experimental materials are samples of 12 µm thick rolled copper foil (Ag ≤ 0.01%)
produced by a domestic company (Heze Guangyuan Copper Strip Co., Ltd., Heze, China).
They were annealed at 180 ◦ C for 1 min, 3 min, 5 min, 10 min, 15 min, 30 min and 60 min in
101-0BS electric blast drying oven (Shanghai Lichen Instrument Technology Co. Ltd., Shang-
hai, China). Before surface observation and analysis, the samples were electropolished in
60% w/w H3 PO4 with U = 15 V for 60 s, followed by rinsing with tap water and deionized
water to remove any amorphous film formed during the electropolishing process. Then,
the samples were processed by the IM4000 Hybrid Ion Milling System (Hitachi, Tokyo,
Japan). The values of discharge voltage, ion beam irradiation angle, specimen rotation
speed, specimen rotation speed and Ar gas flow were 1.5 kV, 4◦ , 80 r/min, 25 r/min,
1 cm3 /min, respectively. After the electropolishing and ion grinding, the annealed copper
foil was observed by FEI-Apreo Field Emission Scanning Electron Microscope (FESEM,
FEI, Waltham, MA, USA), Tecnai G2F 20 Field Emission Transmission Electron Microscope
(FETEM, FEI, Waltham, MA, USA) and analyzed by electron backscatter diffraction (EBSD,
FEI, Waltham, MA, USA). The HKL Channel 5 system was adopted in the EBSD data analy-
sis, such as the grain orientation, texture type and grain boundary type. The conductivity,
tensile properties and bending properties were tested by FT-330 Four Probe Resistivity
Tester (Ningbo Ruike Weiye Instrument Co. Ltd., Ningbo, China), Instron 5965 universal
material testing machine (Instron, Norwood, MA, USA) and ASIDA-NIR bending tester
(Guangdong Zhengye Technology Co. Ltd., Dongguan, China).

3. Results and Discussion

3.1. Microstructure
Figure 1 shows the micro-morphology of the surface and longitudinal section of the
rolled copper foil. Figure 1a,b exhibit the surface morphology observed by SEM and the
surface morphology after corrosion observed by optical microscope (OM), respectively. It
can be seen that the surface of rolled copper foil is relatively rough, and its Ra and Rz values
are 0.10 µm and 0.80 µm, respectively. Meanwhile, there are a lot of rolling traces on the
surface, and the length direction of rolling traces is perpendicular to the rolling direction
(RD). The surface grains are elongated along the RD orientation, as shown in Figure 1b,c,
which exhibit the SEM morphology of the longitudinal section. It can be seen that the grains
are elongated along the RD orientation to form fibrous grains through the whole thickness
direction, and its length direction of grains is perpendicular to the transverse direction
(TD), which indicates that the copper foil has undergone large plastic deformation.
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Figure 1.
Figure 1. Morphology
Morphologyofofcopper
copperfoil
foilsurface
surfaceand
andlongitudinal
longitudinalsection.
section.(a)
(a)Surface
Surfacemorphology
morphology(SEM);
(SEM);
(b) (b) Surface
Surface morphology
morphology after corrosion
after corrosion (OM); (c)(OM); (c) Longitudinal
Longitudinal section morphology
section morphology (SEM). (SEM).

Figure 2 shows the

Figure the inverse
inverse pole
polefigure
figure(IPF)
(IPF)diagram
diagramofofEBSD
EBSDorientation image
orientation image of
thethe
of longitudinal
longitudinalsection of rolled
section copper
of rolled foil.foil.
copper It canItbe seen
can be that
seenthethatgrains keep the
the grains keepdefor-
the
mation graingrain
deformation characteristics alongalong
characteristics the rolling direction,
the rolling whichwhich
direction, are mainly <111><111>
are mainly and <101>
and
orientations. This is because the copper is a face-centered cubic (fcc) metal, and the defor-
<101> orientations. This is because the copper is a face-centered cubic (fcc) metal, and the
mation results from the dislocation slip. The <111> and <101> orientations are stable ori-
deformation results from the dislocation slip. The <111> and <101> orientations are stable
entations, and
orientations, andthe
thegrain
grainorientation
orientationwill
willcontinuously
continuouslytransfer
transfer to
to these two orientations
these two orientations
during rolling.
during rolling.
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Figure2.2.IPF
Figure IPFdiagram
diagramof
ofEBSD
EBSDorientation
orientationimage
imageof
ofthe
thelongitudinal
longitudinalsection
sectionof
ofcopper
copperfoil.
foil.

Figure33exhibits
Figure exhibitsthe theIPF
IPFdiagram
diagramof of
thethe surface
surface of the
of the rolled
rolled andand annealed
annealed coppercopper
foil.
Itfoil.
canItbecan befrom
seen seenFigure
from Figure
3a that3a
thethat the surface
surface grains ofgrains of thecopper
the rolled rolledfoil
copper foil are
are crushed
crushed
and andby
refined refined
large by large deformation
deformation rate and
rate rolling, rolling,
the and
graintheorientation
grain orientation
is bandedis banded
along
along
the RD the RD orientation.
orientation. After annealing
After annealing for 1 min,for 1 min,
a small a small
amount of amount of fine
fine equiaxed equiaxed
grains (red
grains in
grains (red grains
Figure 3b)inappears
Figure 3b) appears
on the on the
surface, surface,that
indicating indicating
the localthat the local
region of theregion
copper of
the copper foil begins to recrystallize. After annealing for 5 min, a small amount of de-
foil begins to recrystallize. After annealing for 5 min, a small amount of deformed grains
formed
(blue grains
grains (blue grains
in Figure in Figure
3c) remains 3c)surface.
on the remainsAfter
on the surface. After
annealing for 10annealing
min (Figure for3d),
10 min
the
(Figure 3d), the deformed fibrous grains disappear, and complete recrystallization occurs.
deformed fibrous grains disappear, and complete recrystallization occurs. After annealing
After
for annealing
60 min (Figure for3e),
60 the
mingrains
(Figure 3e),into
grow the grains
equiaxedgrow into equiaxed grains.
grains.
The grain boundaries, especially the grain boundaries’ angle of deformed microstruc-
ture, are the basis of analyzing the recovery and recrystallization during the subsequent
annealing process [16]. Because of the symbiotic relationship between annealing twins and
recrystallized structure [17], Σ3 grain boundaries are annealing twin boundaries, which can
be used as the sign to reflect the recrystallization of rolled copper foil during the annealing
process. Figure 4 shows the grain boundary distribution of rolled and annealed copper foil,
in which the green line represents low angle grain boundaries (LAGBs, 2 ≤ θ ≤ 15◦ ), the
black line represents high angle grain boundaries (HAGBs, θ > 15◦ ), and the red line repre-
sents Σ3 grain boundaries. Table 1 shows the fraction of different grain boundary types. It
can be seen that the fraction of LAGBs of the rolled copper foil is 68.5%. After annealing for
1 min, the fraction of LAGBs and HAGBs changes little compared with that of rolled copper
foil, and the fraction of Σ3 grain boundaries increases slightly. After annealing for 5 min,
the fraction of LAGBs decreases sharply, while the fraction of HAGBs increases signifi-
cantly. Meanwhile, the fraction of Σ3 grain boundaries reaches 47.5%, which indicates that
a large number of annealing twins have formed during the annealing process, as shown in
Figure 5. After annealing for 10 min, the fraction of Σ3 grain boundaries increases to 63.3%.
After annealing for 60 min, the fraction of Σ3 grain boundaries decreases slightly. With
the increase in annealing time, the fraction of HAGBs increases. The fraction of Σ3 grain
boundaries increases at the recrystallization stage, while the fraction decreases at the grain
growth stage. When annealed for 10 min, the fraction of Σ3 grain boundaries reaches
the highest.
Figure 6 shows the grain size distribution of the rolled and annealed copper foil. It can
be seen that with the increase in annealing time, the average grain size gradually increases,
and the grain size distribution range gradually widens. When annealed for more than
10 min, the grain size distribution presents a bimodal structure, which is composed of large
recrystallized grains and fine grains. When annealed for 60 min, the percentage of large-
size grains is approximately 65%, indicating that the recrystallized grains have coarsened.
Compared to the average grain size of samples after annealing from 1 min to 60 min, the
coarsening rate of recrystallized grains is more pronounced after annealing from 1 min to
5 min. This difference in the recrystallized grains’ coarsening rate is intimately connected to
the HAGBs and LAGBs during the annealing process [18], as shown in Table 1. Meanwhile,
 Figure 3 exhibits the IPF diagram of the surface of the rolled and annealed copper
foil. It can be seen from Figure 3a that the surface grains of the rolled copper foil are
crushed and refined by large deformation rate rolling, and the grain orientation is banded
along the RD orientation. After annealing for 1 min, a small amount of fine equiaxed
Materials 2022, 15, 2249
grains (red grains in Figure 3b) appears on the surface, indicating that the local region5 ofof17
the copper foil begins to recrystallize. After annealing for 5 min, a small amount of de-
formed grains (blue grains in Figure 3c) remains on the surface. After annealing for 10 min
(Figure 3d),demonstrates
this result the deformedconvincingly
fibrous grains disappear,
that andincomplete
the changes recrystallization
the fraction of HAGBs andoccurs.
LAGBs
After annealing
are closely for 60
related minrecrystallization
to the (Figure 3e), the grains grow into equiaxed grains.
process.

Materials 2022, 15, x FOR PEER REVIEW 5 of 18

3. IPF 3.
FigureFigure diagram of the of
IPF diagram rolled and annealed
the rolled coppercopper
and annealed foil. (a)foil.
Rolled sample;
(a) Rolled (b) 1 min;
sample; (b) 1(c) 5 min;
min; (c) 5 min;
(d) 10 min; (e) 60 min.
(d) 10 min; (e) 60 min.

The grain boundaries, especially the grain boundaries’ angle of deformed microstruc-
ture, are the basis of analyzing the recovery and recrystallization during the subsequent
annealing process [16]. Because of the symbiotic relationship between annealing twins
and recrystallized structure [17], Σ3 grain boundaries are annealing twin boundaries,
which can be used as the sign to reflect the recrystallization of rolled copper foil during
the annealing process. Figure 4 shows the grain boundary distribution of rolled and an-
nealed copper foil, in which the green line represents low angle grain boundaries (LAGBs,
2 ≤ θ ≤ 15°), the black line represents high angle grain boundaries (HAGBs, θ > 15°), and
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FigureFigure 4. Grain
4. Grain boundary
boundary distribution
distribution of rolled
of rolled and annealed
and annealed coppercopper
foil. (a)foil. (a) sample;
Rolled Rolled sample; (b) 1
(b) 1 min;
min; (d)
(c) 5 min; (c) 510min;
min;(d)
(e)10
60min;
min.(e) 60 min.

Table 1. Effect of annealing time on grain boundary fraction of copper foil.

Annealing Time/min Rolled 1 5 10 60

LAGBs 68.5% 61.2% 29.1% 24.1% 16.9%
HAGBs 31.5% 38.8% 70.9% 75.9% 83.1%
Σ3 Grain Boundaries 2.7% 4.2% 47.5% 63.3% 57.7%
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Figure 5. Annealing twins formed during annealing process observed by TEM.

Figure 6 shows the grain size distribution of the rolled and annealed copper foil. It
can be seen that with the increase in annealing time, the average grain size gradually in-
creases, and the grain size distribution range gradually widens. When annealed for more
than 10 min, the grain size distribution presents a bimodal structure, which is composed
of large recrystallized grains and fine grains. When annealed for 60 min, the percentage
of large-size grains is approximately 65%, indicating that the recrystallized grains have
coarsened. Compared to the average grain size of samples after annealing from 1 min to
60 min, the coarsening rate of recrystallized grains is more pronounced after annealing
from 1 min to 5 min. This difference in the recrystallized grains’ coarsening rate is inti-
mately connected to the HAGBs and LAGBs during the annealing process [18], as shown
in Table 1. Meanwhile, this result demonstrates convincingly thatby
theTEM.
changes in the frac-
Figure 5.5.Annealing
Figure Annealing twinsformed
twins formed during
during annealingprocess
annealing processobserved
observedby TEM.
tion of HAGBs and LAGBs are closely related to the recrystallization process.
Figure 6 shows the grain size distribution of the rolled and annealed copper foil. It
can be seen that with the increase in annealing time, the average grain size gradually in-
creases, and the grain size distribution range gradually widens. When annealed for more
than 10 min, the grain size distribution presents a bimodal structure, which is composed
of large recrystallized grains and fine grains. When annealed for 60 min, the percentage
of large-size grains is approximately 65%, indicating that the recrystallized grains have
coarsened. Compared to the average grain size of samples after annealing from 1 min to
60 min, the coarsening rate of recrystallized grains is more pronounced after annealing
from 1 min to 5 min. This difference in the recrystallized grains’ coarsening rate is inti-
mately connected to the HAGBs and LAGBs during the annealing process [18], as shown
in Table 1. Meanwhile, this result demonstrates convincingly that the changes in the frac-
tion of HAGBs and LAGBs are closely related to the recrystallization process.

Materials 2022, 15, x FOR PEER REVIEW 8 of 18

Figure 6.
Figure 6. Effect
Effect of
of annealing
annealing time
time on
on the
the grain
grain size
size of
of rolled
rolled and
and annealed
annealed copper
copper foil.
foil. (a)
(a) Rolled
Rolled
sample; (b)
sample; (b) 11 min;
min; (c)
(c) 55 min;
min; (d)
(d) 10
10 min;
min; (e)
(e) 60
60 min.
min.

The texture type and intensity reflect the softening state of copper foil. Figure 7 shows
the orientation distribution function (ODF) diagram of the rolled and annealed copper
foil. Figure 8 represents texture orientation density along α (0°→90°, 45°, 0°), β (73°, 35°,
45°→90°) and (0°, 0°→45°, 0°) orientation lines, in which, φ1 is the angle between the in-
Materials 2022, 15, x FOR PEER REVIEW 8 of 18
Materials 2022, 15, 2249 8 of 17

The texture type and intensity reflect the softening state of copper foil. Figure 7 shows
the orientation distribution function (ODF) diagram of the rolled and annealed copper
foil. Figure 8 represents texture orientation density along α (0◦ →90◦ , 45◦ , 0◦ ), β (73◦ ,
35◦ , 45◦ →90◦ ) and (0◦ , 0◦ →45◦ , 0◦ ) orientation lines, in which, ϕ1 is the angle between
the intersection of RD-TD plane and [100]-[010] plane and RD orientation, Φ is the angle
between RD-TD plane and [100]-[010] plane, and ϕr2 is the angle between the intersection
of RD-TD plane and [100]-[010] plane and [100] orientation. This [100] orientation-[010]
orientation-[001] orientation is the crystal coordinate system. From Figures 7a and 8b,d, it
can be concluded that the textures of rolled copper foil are copper texture ({112} <111>),
brass texture ({110} <211>), S texture ({123} <634>), Gauss texture ({110} <100>), which are
typical deformed textures [19], and the maximum texture intensity is 14.0. After annealing
for 1 min, the main texture is still deformation texture. Meanwhile, a small amount of cube
textures ({100} <001>) and ({025} <001>) begin to appear, which are annealing textures [20].
Figurethe
With 6. increase
Effect of inannealing
annealingtime on the
time, thegrain size oftexture
annealing rolled and annealed
intensity copperobviously,
increases foil. (a) Rolled
and
sample;
the (b) 1 min;
annealing (c) 5 min;
texture (d) 10reaches
strength min; (e)38.0
60 min.
after annealing for 60 min. Softened annealing
will obviously weaken the deformation texture intensity, while significantly enhancing the
The texture type
recrystallization textureandintensity.
intensity reflect the softening state of copper foil. Figure 7 shows
the orientation
Figure 9 shows distribution function
the textures’ (ODF)
volume diagram
fraction of theof the rolled
rolled andand annealed
annealed coppercopper
foil
foil. Figure
obtained by8the
represents
orientationtexture orientation
density density
integration along The
method. α (0°→90°, 45°, 0°),foil
rolled copper β (73°, 35°,
contains
45°→90°)
1.0% cubicand (0°, 0°→45°,
texture, 1.1% {025}0°) <001>
orientation lines,
texture, andinthe
which,
brassφtexture
1 is the volume
angle between
fractionthe in-
is the
tersection of RD-TD plane and [100]-[010] plane and RD orientation, Φ is the angle be-
highest, at 7.2%. After annealing for 1 min, the brass texture and recrystallization texture
tween RD-TD
volume fraction plane and [100]-[010]
increase. plane, and
After annealing forφ52 is
min,the the
angle between thetexture
deformation intersection
volume of
RD-TD plane
fraction and [100]-[010]
decreases, plane and [100]texture
while the recrystallization orientation.
volume This [100]increases
fraction orientation-[010] ori-
significantly.
entation-[001]
The cubic texture orientation is the crystal
volume fraction coordinate
is 14.8%, and thesystem. Fromtexture
{025} <001> Figuresvolume
7a andfraction
8b,d, it
can
is be concluded
8.0%. After annealingthat thefortextures
10 min,ofthe rolled
cubic copper
texture foil are copper
volume texture
fraction ({112}slightly,
increases <111>),
brass texture ({110} <211>), S texture ({123} <634>), Gauss texture ({110} <100>), which are
the {025} <001> texture volume fraction decreases, and the deformation texture volume
typical deformed
fraction decreases. textures
After [19], and the
annealing formaximum texture
60 min, there is intensity
almost no is deformation
14.0. After annealing
texture.
for 1 min, the main texture is still deformation texture. Meanwhile, a small amount of cube
Meanwhile, the recrystallization texture volume fraction increases significantly, and the
textures
cubic ({100}volume
texture <001>) fraction
and ({025} <001>)the
reaches begin to appear,
highest, at 34.4%. whichWitharethe
annealing
increasetextures [20].
in annealing
With the
time, the increase
copper type in annealing time, the
texture volume annealing
fraction textureand
decreases, intensity increases
the cubic texture obviously,
volume
and the increases.
fraction annealing The texture
mainstrength
texture reaches
of rolled38.0 afterfoil
copper annealing for 60 min.texture,
is the deformation Softened an-
which
transfers to the cubic texture and {025} <001> texture in the recrystallization
nealing will obviously weaken the deformation texture intensity, while significantly stage and grain
en-
growth
hancingstage [21].
the recrystallization texture intensity.

Figure 7. Cont.
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Figure 7. Cont.
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Figure
Figure
Figure 7.
7. ODF
7. ODF ODF diagram
diagram of
of theof
diagram therolled
rolled
the rolled
and andannealed
annealed
and annealed copper
copper foil.
copper foil.
(a) Rolled
foil. (a) Rolled
sample;
(a) Rolled(b) 1sample;
(c) 5(b)
min; (b)
sample; 1 min;
1 min; (c) 5(c) 5
min;
min;
min;
(d) (d)
(d)10
10 10 min;
min;
min; 60(e)
(e) 60
(e) 60 min.
min.
min.

Materials 2022, 15, x FOR PEER REVIEW 11 of 18

◦ ◦ ◦ ◦
Figure 8. Texture
Figure orientation
8. Texture densitydensity
orientation of the copper foil. (a) (0°,0°→45°,0°)
of the copper fiber;
foil. (a) (0 ,0 → (b))β-fiber;
45 ,0 (c) β-fiber;
fiber; (b) Posi- (c) Posi-
tion of β-fiber;
tion (d) α-fiber.
of β-fiber; (d) α-fiber.

Figure 9 shows the textures’ volume fraction of the rolled and annealed copper foil
obtained by the orientation density integration method. The rolled copper foil contains
1.0% cubic texture, 1.1% {025} <001> texture, and the brass texture volume fraction is the
highest, at 7.2%. After annealing for 1 min, the brass texture and recrystallization texture

Materials 2022, 15, 2249
tion decreases. After annealing for 60 min, there is almost no deformation texture. Mean-
while, the recrystallization texture volume fraction increases significantly, and the cubic
texture volume fraction reaches the highest, at 34.4%. With the increase in annealing time,
the copper type texture volume fraction decreases, and the cubic texture volume fraction
increases. The main texture of rolled copper foil is the deformation texture, which trans-
fers to the cubic texture and {025} <001> texture in the recrystallization stage and grain
11 of 17
growth stage [21].

Figure
9. 9.
Figure
Materials 2022, 15, x FOR PEER REVIEW The textures’
The fraction
textures’ of of
fraction thethe
rolled and
rolled annealed
and copper
annealed foil.
copper foil. 12 of 18

3.2. Mechanical Properties

3.2.1. Tensile Properties
3.2. Mechanical Properties
Figure 10 shows the tensile strength and elongation of the rolled and annealed copper
3.2.1. Tensile Properties
foil along the RD orientation. It can be seen that the tensile strength of rolled copper foil is
the Figure
highest.10 shows the tensile strength
After annealing for 1–5 and
min, elongation of the
the tensile rolled and
strength annealed
decreases copper
significantly with
foil along the RD orientation. It can be seen that the tensile strength of rolled copper foil
the increase in annealing time. After annealing for 10 min, the tensile strength tends to be
is the highest. After annealing for 1–5 min, the tensile strength decreases significantly with
stable. The reason why the tensile strength decreases rapidly when annealed for 1–5 min
the increase in annealing time. After annealing for 10 min, the tensile strength tends to be
is that the LAGBs decrease sharply during the annealing time [22]. The interface energy
stable. The reason why the tensile strength decreases rapidly when annealed for 1–5 min
isofthat
thethe
LAGBs
LAGBsisdecrease
lower than thatduring
sharply of thethe HAGBs,
annealingand the[22].
time mobility of the energy
The interface LAGBs is poor,
which
of weakens
the LAGBs the resistance
is lower than that ofofthedislocation
HAGBs, and movement.
the mobilityTherefore,
of the LAGBs theistensile
poor, strength
which weakens
decreases with thethe
resistance
increase of in
dislocation
annealing movement. Therefore,
time. After the tensile
annealing strength
for 5–60 min,de-
the LAGBs
creases
fraction with the increase
changes little, in annealing
and time.strength
the tensile After annealing
tends tofor be5–60 min,When
stable. the LAGBs frac-
the annealing time
tion changesfrom
increases little,1 and
minthe to tensile
30 min,strength tends to be
the elongation stable. When
increases the annealing
gradually. When the timeannealing
increases from 1 from
time increases min to 3030min
min,
tothe
60 elongation increases gradually.
min, the elongation decreasesWhen the On
slightly. annealing
the whole, with
time increases in
the increase from 30 min to
annealing 60 min,
time, the elongation
the elongation decreases
of the copperslightly. On the whole,
foil increases. This is because
with the increase in annealing time, the elongation of the copper foil increases.
with the increase in annealing time, the dislocations obtain enough energy to redistribute. This is
because with the increase in annealing time, the dislocations obtain enough
The structural defects, such as the dislocation density, decrease, thus the hindrance to energy to re-
distribute. The structural defects, such as the dislocation density, decrease, thus the hin-
dislocation movement weakens. Therefore, the deformation resistance decreases, the
drance to dislocation movement weakens. Therefore, the deformation resistance de-
plasticity enhances, and the elongation increases.
creases, the plasticity enhances, and the elongation increases.

Figure
Figure10.10.
Effect of annealing
Effect timetime
of annealing on tensile properties
on tensile of copper
properties foil.
of copper foil.

3.2.2. Bending Resistance Properties

Figure 11 shows the effect of annealing time on the bending resistance properties of
the rolled and annealed copper foil along the RD orientation. It can be seen that the rolled
copper foil has good bending resistance performance, mainly due to the large number of
LAGBs, which can effectively inhibit the crack propagation. With the annealing time in-
Materials 2022, 15, 2249 12 of 17

3.2.2. Bending Resistance Properties

Figure 11 shows the effect of annealing time on the bending resistance properties of
the rolled and annealed copper foil along the RD orientation. It can be seen that the rolled
copper foil has good bending resistance performance, mainly due to the large number
of LAGBs, which can effectively inhibit the crack propagation. With the annealing time
increasing from 1 min to 5 min, the bending times decreases sharply. The LAGBs fraction
decreases sharply with the increase in annealing time. When the annealing time increases
from 5 min to 60 min, the bending resistance performance increases slightly. From the
analysis of texture evolution, it can be seen that with the increase in annealing time, the
deformation texture fraction gradually decreases, while the cubic texture fraction gradually
increases. The grain orientation tends to be concentrated, and the crack is not easy to
expand. At the same time, the increase in grain size leads to the increase in critical value of
Materials 2022, 15, x FOR PEER REVIEW 13 of 18
crack initiation, which slightly improves the bending resistance properties of the copper
foil [23].

Figure 11.
Figure 11. Bending resistance
resistance properties
properties of
of the
the rolled
rolled and
and annealed
annealedcopper
copper foil.
foil.

In
In order
order to
to further
further analyze
analyze the
the fracture
fracture mechanism
mechanism of of the
the copper
copper foil,
foil, the
the surface
surface
morphology and fracture morphology of the longitudinal tensile fracture after
morphology and fracture morphology of the longitudinal tensile fracture after annealing annealing
for
for 10
10 min
min were
were studied.
studied. As
As shown
shown inin Figure
Figure 12,
12, obvious
obvious necking
necking phenomenon
phenomenon occurs occurs
during
during◦ the tensile process. When the copper foil is stretched, there will be
the tensile process. When the copper foil is stretched, there will be slip
slip lines,
lines, which
which
are
are 45 to the
45°to theloading
loadingdirection,
direction,as
aspointed
pointedout
out with
with the
the white
white dotted
dotted line
line in Figure 12a.
in Figure 12a.
The
The results show that the dislocation movement occurs during the tensile process, and the
results show that the dislocation movement occurs during the tensile process, and the
plastic deformation is mainly carried out by dislocation sliding. From Figure 12b, it can be
plastic deformation is mainly carried out by dislocation sliding. From Figure 12b, it can
seen that there are tearing ridges (black dotted line 1) and sliding lines (black dotted line 2)
be seen that there are tearing ridges (black dotted line 1) and sliding lines (black dotted
on the tensile fracture surface, showing good plasticity performance.
line 2) on the tensile fracture surface, showing good plasticity performance.
The fracture surface morphology of the rolled and annealed copper foil after bending
test is shown in Figure 13. From Figure 13a, it can be seen that there are different degrees of
microcracks on the surface of rolled copper foil, and the direction is parallel to the bending
direction. The surface cracks are fine, scattered shallow and flat. After annealing for 1 min,
the surface crack depth increases, and some cracks are connected. After annealing for 3 min,
the width and depth of the crack increase, and the crack trends to being tortuous. The
reason is that there are many LAGBs in the rolled copper foil, and the surface cracks are
not easy to concentrate and connect during the bending process, so the bending resistance
properties of the rolled copper foil are good [24].

Figure 12. Morphological characteristics of the copper foil annealed for 10 min. (a) Surface morphol-
ogy; (b) Fracture morphology.

The fracture surface morphology of the rolled and annealed copper foil after bending
 for 10 min were studied. As shown in Figure 12, obvious necking phenomenon occurs
during the tensile process. When the copper foil is stretched, there will be slip lines, which
are 45°to the loading direction, as pointed out with the white dotted line in Figure 12a.
The results show that the dislocation movement occurs during the tensile process, and the
plastic deformation is mainly carried out by dislocation sliding. From Figure 12b, it can
Materials 2022, 15, 2249 13 of 17
be seen that there are tearing ridges (black dotted line 1) and sliding lines (black dotted
line 2) on the tensile fracture surface, showing good plasticity performance.

Materials 2022, 15, x FOR PEER REVIEW 14 of 18

Figure 12. Morphological characteristics of the copper foil annealed for 10 min. (a) Surface morphol-
Materials 2022, 15, x FOR PEER REVIEW 14 of 18
Figure 12. Morphological characteristics of the copper foil annealed for 10 min. (a) Surface morphol-
ogy; (b) Fracture morphology.
ogy; (b) Fracture morphology.

The fracture surface morphology of the rolled and annealed copper foil after bending
test is shown in Figure 13. From Figure 13a, it can be seen that there are different degrees
of microcracks on the surface of rolled copper foil, and the direction is parallel to the bend-
ing direction. The surface cracks are fine, scattered shallow and flat. After annealing for 1
min, the surface crack depth increases, and some cracks are connected. After annealing
for 3 min, the width and depth of the crack increase, and the crack trends to being tortu-
ous. The reason is that there are many LAGBs in the rolled copper foil, and the surface
cracks are not easy to concentrate and connect during the bending process, so the bending
resistance properties of the rolled copper foil are good [24].
Figure13.
Figure 13. Surface morphology
morphology of the copper foil after bending. (a)(a)
Rolled sample; (b) (b)
1 min; (c) 3(c) 3
Figure 13.Surface
Surface morphologyofofthe
thecopper
copperfoil
foilafter
afterbending.
bending. (a)Rolled sample;
Rolled sample; 1 min;
(b) 1 min;
min.
min.
(c) 3 min.

3.3.
3.3. Electrical
3.3.Electrical Performance
ElectricalPerformance
Performance
Electrical conductivity
conductivity is
Electricalconductivity is one
oneofofthe indicators reflecting the change ofofmicrostructure.
Electrical is one of the
the indicators
indicatorsreflecting
reflectingthethechange
change ofmicrostructure.
microstructure.
Figure
Figure 14
14 shows
shows the
the effect
effect of
of annealing
annealing time
time on
on the
the electrical
electrical conductivity
conductivity of the
of of rolled
thethe
rolled
Figure 14 shows the effect of annealing time on the electrical conductivity rolled
and
and annealed
annealedcopper
copperfoil.
foil.It can be be
It can seen
seenthatthat
withwith
the increase in annealing
the increase time,time,
in annealing the elec-
the
and annealed copper foil. It can be seen that with the increase in annealing time, the elec-
trical conductivity
electrical increases
conductivity increases from 86%
from 86%IACS IACSto to
92%92% IACS.
IACS.During
Duringthe theannealing
annealingprocess,
process,
trical conductivity increases from 86% IACS to 92% IACS. During the annealing process,
the
the lattice
lattice distortion
distortion and
and crystal
crystal defects
defects decrease,
decrease, thethe grain
grain size
size increases,
increases, and
and the
the grain
grain
the lattice distortion
boundaries
boundaries decrease.
and
decrease.So,
crystal
So,thethe
defects
scattering
scattering
decrease,
effect of the
effect
theelectrons
grainweakens,
electrons
of the
size increases,
weakens,
and thede-
the resistivity grain
the resistivity
boundaries
creases
decreases decrease.
gradually
gradually So,
[25], and
[25], the
and scattering
electrical effect
conductivity
electrical of
conductivity the electrons
becomes
becomes weakens,
better.
better. the resistivity de-
creases gradually [25], and electrical conductivity becomes better.

Figure
Figure 14.
14. Influence
Influence of
of annealing
annealing time
time on
on the
the conductivity
conductivity of
of copper
copper foil.
foil.

Figure 14. Influence of annealing time on the conductivity of copper foil.

4. Discussion
4.1. Relationship between the Bending Resistance Properties and Microstructure
4. Discussion
Excellent bending resistance performance is one of the most important properties of
4.1. Relationship between the Bending Resistance Properties and Microstructure
the rolled copper foil, which is also the premise of wide application [26]. During the de-
Excellent
formation bending
process, resistance
the grain performance
size, grain is one
orientation, of the most
dislocation important
configuration properties
and disloca- of
the rolled copper foil, which is also the premise of wide application [26]. During
tion density of the copper foil will change with the deformation rate [27,28]. The bendingthe de-
Materials 2022, 15, 2249 14 of 17

4. Discussion
4.1. Relationship between the Bending Resistance Properties and Microstructure
Excellent bending resistance performance is one of the most important properties
of the rolled copper foil, which is also the premise of wide application [26]. During
the deformation process, the grain size, grain orientation, dislocation configuration and
dislocation density of the copper foil will change with the deformation rate [27,28]. The
bending resistance of the rolled copper foil is obviously better than that of the annealed
copper foil, which is due to the fact that the deformation rate of the rolled copper foil is
more than 95%. The extra high deformation rate of rolled copper foil will result in smaller
grain size and less critical value of bending crack initiation [29]. Meanwhile, the amount
of grain boundaries in the same cross-sectional area increases greatly. As an obstacle to
the movement of dislocation and other defects, the grain boundaries effectively inhibit the
crack propagation and improve the bending resistance performance [30].
It can be seen from Figure 3 that the fraction of <001> oriented grains of the copper foil
after annealing for 60 min is 95.2%, showing relatively consistent grain orientation. Grain
orientation is also one of the important symbols of bending resistance performance [31].
The more concentrated the preferred orientation of the grains, the smaller the orientation
difference between adjacent grains [32,33]. Under certain stress conditions, the difference
of Young’s modulus between adjacent grains decreases, and the slip direction tends to be
the same, which reduces the difference of plastic deformation of different parts. The stress
concentration at the grain boundary will be alleviated, and the initiation and propagation
of cracks will also be reduced [34,35]. Therefore, the occurrence of fracture will be delayed,
and the bending resistance of copper foil will improve.

4.2. Relationship between the Electrical Conductivity and Microstructure

Conductivity, which characterizes the ability of transferring current, is usually related
to the temperature, substitution or interstitial atoms, and crystal defects [36]. Because
the experiment is carried out at a given temperature, the Ag content and the annealing
temperature are also relatively low. The Ag atoms as the replacement atoms would not
change during the annealing process, so the electrical conductivity of the copper foil is only
related to the defect density [37].
The defect density, especially the dislocation density [38], has an important influence
on electrical conductivity. The dislocation density is closely related to the softened annealing
time [39]. With the increase in softened annealing time, the dislocation density decreases
gradually. According to the two fluid models [40], the moving electrons are scattered and
hindered on the dislocations. Meanwhile, the decrease in dislocation density will lead to
not only the increase in effective charge density participating in the conduction, but also the
enhancement of current transmission ability [41]. Therefore, the electrical conductivity of
the copper foil increases with the decrease in dislocation density [42]. The deformation rate
of the rolled copper foil is more than 95%, so a large number of dislocations are accumulated
in the rolled copper foil (as shown in Figure 15). After the softened annealing, the amount
of dislocation defect greatly decreases, and the electrical conductivity increases gradually.
The dislocation density relates to the electrical conductivity and mechanical properties
of the copper foil. The mechanical properties reflect the macroscopic properties of materials,
while the electrical conductivity mainly explains the change of mechanical properties from
the microscopic mechanism [43]. In the past, TEM observation method was often used
to analyze the internal structure of metals. This method is not only difficult in terms of
preparing the samples and being expensive to detect, but it is also difficult to prepare for
quantitative analysis due to the fact that TEM can only observe a small thin area of the
sample. Electrical conductivity can be used as a fast and effective method to analyze the
internal microstructure of metals.
 will lead to not only the increase in effective charge density participating in the conduc-
tion, but also the enhancement of current transmission ability [41]. Therefore, the electrical
conductivity of the copper foil increases with the decrease in dislocation density [42]. The
deformation rate of the rolled copper foil is more than 95%, so a large number of disloca-
tions are accumulated in the rolled copper foil (as shown in Figure 15). After the softened
Materials 2022, 15, 2249 15 of 17
annealing, the amount of dislocation defect greatly decreases, and the electrical conduc-
tivity increases gradually.

Figure15.
Figure 15.High-density
High-densitydislocations
dislocationsof
ofthe
therolled
rolledcopper
copperfoil.
foil.

The dislocation density relates to the electrical conductivity and mechanical proper-
5. Conclusions
ties Based
of the on
copper foil. The
the thermal mechanical
treatment at 180properties reflect times,
◦ C for different the macroscopic
the softenedproperties of
microstruc-
materials,
ture while theofelectrical
and properties 12 µm thickconductivity mainly
rolled copper foilexplains the change of
were systematically mechanical
studied. The
properties
research from
result is the microscopic
of great mechanism
significance [43].
to further In the the
improve past,etching
TEM observation
performance, method
espe-
was often
cially used to analyze
the bending the performance
resistance internal structure of metals.
of rolled This
copper method
foil. is not findings
The main only difficult
are
in terms of preparing
summarized as follows:the samples and being expensive to detect, but it is also difficult to
prepare
(1) When forthe
quantitative analysis
rolled copper due to theatfact
foil is annealed 180 that TEM
◦ C, the can only observe
microstructure changesa small thin
regularly
area with
of thedifferent
sample.annealing
Electrical times.
conductivity can be used as a fast and effective method
After annealing for 1–10 min, the recrystallization of to
analyze the internal microstructure of metals.
copper foil occurs. After annealing for 10–60 min, the grains grow, and the annealing
texture is mainly cubic texture. With the increase in annealing time, the deformation
texture fraction decreases, while the annealing texture fraction increases. When
annealed for 10 min, the Σ3 grain boundaries fraction is the highest. The HAGBs
fraction increases with the increase in annealing time.
(2) When the rolled copper foil is annealed at 180 ◦ C, the mechanical properties change
regularly with different annealing times. After annealing for 1–5 min, the tensile
strength decreases sharply because the LAGBs decrease sharply during the annealing
time. After annealing for 10–60 min, the tensile strength tends to be stable. The
elongation increases with the increase in annealing time. After annealing for 1–
5 min, the bending resistance performance decreases significantly. After annealing for
5–60 min, the bending resistance performance improves slightly.
(3) When the rolled copper foil is annealed at 180 ◦ C, the electrical conductivity changes
regularly with different annealing times. The electrical conductivity increases gradu-
ally with the increase in annealing time. The electrical conductivity of the copper foil
reaches 92% IACS after annealing for 60 min. The electrical conductivity can be used
as a fast and effective method to analyze the microstructure of metals.

Author Contributions: Conceptualization, R.F. and B.G.; data curation, W.Z. and Y.S.; formal analysis,
R.F.; funding acquisition, B.G. and R.F.; investigation B.C. and T.F.; methodology, X.W.; project
administration, B.G. and T.F.; supervision, B.G.; validation, B.G.; visualization, X.W.; writing-original
draft, R.F.; writing-review and editing, B.G. All authors have read and agreed to the published version
of the manuscript.
Funding: This research was funded by the Major Scientific and Technological Innovation Project of
Shandong Province Key R&D Program, grant number 2019TSLH0101, the Natural Science Foundation
of Shandong Province, grant number ZR2021ME082, SDUT & Zhoucun District Integration Develop-
ment Special Plan, grant number 2020ZCXCZH07, SDUT & Yiyuan County Industrial Technology
Research Institute Project.
Institutional Review Board Statement: Not applicable.
Materials 2022, 15, 2249 16 of 17

Informed Consent Statement: Not applicable.

Data Availability Statement: The data presented in this study are available on request from the
corresponding author.
Conflicts of Interest: The authors declare no conflict of interest.

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