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RAPID COMMUNICATION

Flexible nano-paper-based positive

electrodes for Li-ion batteries—Preparation
process and properties
Simon Leijonmarcka,c,n, Ann Cornella,c, Göran Lindbergha,c,
Lars Wågbergb,c

a
Department of Chemical Engineering and Technology, KTH Royal Institute of Technology, SE-100 44
Stockholm, Sweden
b
Department of Fibre and Polymer Technology, KTH Royal Institute of Technology, SE-100 44 Stockholm,
Sweden
c
Wallenberg Wood Science Center, KTH Royal Institute of Technology, SE-100 44 Stockholm, Sweden

Received 4 December 2012; received in revised form 18 February 2013; accepted 18 February 2013

KEYWORDS Abstract
Flexible; Flexible battery solutions is an emerging field due to a demand for bendable electronic devices.
Fibrillated; In this study, a route to make flexible positive electrodes for Li-ion batteries by utilizing nano-
Cellulose; fibrillated cellulose (NFC) as binder material has been examined. These LiFePO4-based
Lithium-ion; electrodes are made by filtration of a water dispersion of NFC, LiFePO4 and Super-P carbon
Battery;
particles, resembling a paper-making process. The resulting electrodes show good mechanical
Electrode
properties both dry as well as when soaked with battery electrolyte with a stress at break of
typically at 5.2 and 2.2 MPa, respectively. The cycling performance was 151 mAh/g at C/10 and
132 mAh/g at 1C for samples dried at 170 1C. The drying temperature, after the filtration step,
was found to be important and to affect both the mechanical properties, rendering the
electrodes more ductile at lower temperatures, as well as the electrochemical properties,
causing a higher coulombic efficiency at higher temperatures.
& 2013 Elsevier Ltd. All rights reserved.

Introduction

Flexible electronics is an emerging field including applica-

n
Corresponding author at: Department of Chemical Engineering
and Technology, KTH Royal Institute of Technology, SE-100 44
Stockholm, Sweden. Tel.: +46 87906557.
E-mail address: simonle@kth.se (S. Leijonmarck).
tions such as wearable devices [1], ink jet-printed radio-
frequency identification (RFID) tags [2,3] and roll-up reading
devices [4]. To power such devices without interfering with
the functionality, a need for flexible battery solutions has

2211-2855/$ - see front matter & 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.nanoen.2013.02.002

Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002
2 S. Leijonmarck et al.
become obvious [5]. Nano-fibrillated cellulose (NFC) with
fibrils of diameters about 1000 times smaller than fibers
from wood allows the production of very thin and mechani-
cally strong papers [6]. The development of such nano-
paper [6] and nanoporous films [7–9] has opened totally new
possibilities for using cellulose-based electrodes since these
materials are flexible and yet mechanically stable. The
renewable cellulose is also inexpensive and has a very
interesting environmental profile [10]. On the way towards
flexible paper batteries, the realization of paper electrodes
is a crucial, not well studied, step. Paper electrodes based
on redox-active polymers have been successfully produced
[11] However, low energy density, low cycling stability and
high self-discharge of such polymers limit their field of
applications [12]. Lithium-ion battery technology could be a
solution for improving these aspects of paper batteries.
Carboxymethyl cellulose (CMC) has been examined as binder
material in various electrode chemistries [13–19] attempt-
ing to implement an environmental friendly manufacturing
process—achieved thanks to a water-based process in contrast to
the well-established, but environmentally questionable [20–22],
polyvinylidene fluoride (PVDF)/N-methyl-2-pyrrolidone (NMP)
process. In spite of the successful use of CMC as electrode binder,
no report on the subject has been found that refers to CMC
electrodes as flexible or bendable. There are, however, routes to
making flexible electrodes with cellulosic binder materials.
Natural cellulose has been used as electrode binder in a few
cases including a silicon electrode [23], a graphite electrode [24]
as well as a LiFePO4 electrode [37] using a paper-making process
and a method using ionic liquids to produce both LiFePO4 and
graphite electrodes [25].
In this work, the aim was to incorporate nano-fibrillated
cellulose (NFC) as binder material in positive electrodes for
lithium ion batteries. NFC, also called MFC—micro-fibril-
lated cellulose, [26] is produced by separating the fibrils of
cellulosic fibers by mechanical shearing forces with the aid
of a high-pressure homogenizer, sometimes with the help of
enzymatic treatment, yielding fibrils 5–30 nm wide and a
few mm long [27,28]. NFC films can be formed without
additives [6,29] or with organic or inorganic fillers [30–32]
added to the NFC to create strong and flexible structures
directly from an aqueous suspension. NFC was utilized as
binder material for Li-ion battery electrodes in a recent
study [33] for a negative electrode based on graphite. In
another study, conductive NFC papers were coated with a
small quantity of silicon as negative electrode material [38]
using chemical vapor deposition. No study has been found
where NFC was incorporated as binder material in a positive
battery electrode, nor any bi-layered electrodes. There-
fore, the work described here is aimed at developing a
method for creating both single- and bi-layered flexible
positive electrodes, based on LiFePO4 chemistry, using an
uncomplicated paper-making type of process.
Experimental
Production of the electrodes
Positive electrodes for lithium-ion batteries were produced
through an aqueous paper-making type process. The materials
used were carbon-coated lithium iron phosphate (LiFePO4) of
Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002
the type Life Power s P2 supplied by Phostech Lithium and
Super-P carbon supplied by Timcal. The nano-fibrillated
cellulose was prepared from a 2,2,6,6-tetramethylpiperidine-
1-oxyl (TEMPO)-oxidized (preparation is described elsewhere
[34]) never-dried, dissolving pulp from Domsjö Fabriker AB,
Örnsköldsvik. The charge density of the pulp was determined
to be 600 meq g 1 using conductometric measurement [35].
Solvents used during solvent exchange were ethanol 96% and
99.5%, both supplied by Solveco, dried acetone 499.9%
provided by Merck KGaA and supplied by VWR International,
and pentane 99.9% provided by Prolabo and supplied by VWR
International.
Lithium iron phosphate, Super-P carbon and NFC were
suspended in water using an Ultra Turrax DI25 Basic
disperser at 8000 rpm for 20 min. The dry weight relations
were 80:9:11 for LiFePO4:Super-P:NFC. The suspension was
vacuum-filtered through a Durapore membrane filter, type
0.22 mm GV provided by Millipore, leaving a water-swollen
film on the filter paper. When no longer any liquid was
visible on the film, 50 ml each of in turn ethanol 96%,
ethanol 99.5%, dried acetone and pentane were added and
passed through the film and filter paper to solvent exchange
and remove the remaining water. Subsequent drying was
performed at 110 1C or 170 1C under vacuum. The resulting
paper electrodes were stored in a glove-box under argon
atmosphere.
A bi-layered electrode was also made by filtration of two
suspensions sequentially. A suspension of 85:15 Super-P:NFC
by dry weight was first filtered until no liquid was visible.
Thereafter, the LiFePO4-containing suspension described
above was filtered on top of the Super-P/NFC film. This
bi-layered film was then solvent exchanged and dried as
described above.
Geometry
The thickness was measured using a micrometer (Mitutoyo)
with a resolution of 1 mm. The porosity was calculated by
dividing the geometrical volume of the paper electrodes by
the volume of the constituents, under the assumption that
the weight relation between the components remains
constant throughout the process. The densities used for
this were: NFC—1.5 g/cm3, LiFePO4—3.6 g/cm3 and Super-
P carbon—2.0 g/cm3.
Scanning electron microscope (SEM)
The electrode materials were examined using
a Hitachi S-4800 field emission SEM.
Electrochemical characterization
The conductivity measurements were performed both with
a four-probe van der Pauw set-up using graphite electrodes
positioned at the corners of a square sample and with a
Swagelok cell, where the sample was pressed between two
stainless-steel plates. The pressure of the steel plates was
increased until a constant value for conductivity was
attained. Both methods measure the apparent conductivity.
However, the direction of the current during testing is
different in the two cases. For the van der Pauw set-up,
Preparation process and properties 3

the current passes in the plane of the paper. In the Swagelok

set-up, on the other hand, the current passes through the
plane of the paper samples. For a uniform sample, the
measured conductivity should essentially be the same,
except for an added contact resistance in the Swagelok
case (since it is only a two-electrode set-up). If the samples
instead were anisotropic, e.g. layered, the apparent con-
ductivities for the two cases would differ.
Batteries were built under argon atmosphere with the
LiFePO4/NFC papers as positive electrode, lithium metal as
negative electrode and a Whatman Glass microfiber GF/A
(260 mm) as separator. The electrolyte used was Selectilyte
LP 40, 1 M LiPF6 in ethylene carbonate (EC):diethyl carbo-
nate (DEC) 1:1 by weight provided by Merck KGaA. The
current collectors, provided by Advent Research Materials,
consisted of aluminum foil, 25 mm thick, and nickel foil, Figure 1 A flexible single-layered LiFePO4 paper electrode.
25 mm thick, for the positive and negative electrode,
respectively. These current collectors were put in contact
with the electrodes without any fixation. The battery was
sealed in a pouch cell. The currents used during discharge
are given in multiples of C — the current needed to charge
the electrode material completely in one hour. The specific
capacity used to calculate C-rate was 170 mAh/g LiFePO4.
The mass of LiFePO4 was calculated by multiplying the
actual electrode mass with the mass ratio between LiFePO4
and the total dry mass of the electrode constituents that
were added into the water dispersion. Thus, assuming that
the mass relation between NFC, LiFePO4 and Super-P carbon
is the same in the electrode paper as it was in the initial
water dispersion.

Tensile testing

Tensile testing was performed by means of an Instron 5944
mechanical testing system using a method adapted from the
ASTM D882 standard. Electrode paper in 5–7 mm wide strips,
dried either at 110 1C or 170 1C, were each stored either at
25 1C and 50%RH in air for 48 h or at 25 1C soaked in
electrolyte (1 M LiPF6 in EC:DEC 1:1 by weight) for 48 h
prior to tensile testing; 4–5 strips were tensile tested for
each set of parameters, with a rate of 10% per minute. The
strength values reported are the stress and strain at break.
Results and discussion
The papermaking method for producing positive electrodes
for lithium-ion batteries yielded thin and flexible free-
standing paper electrodes (Figure 1). The constituents of
the electrode paper, LiFePO4 particles, Super-P carbon and
NFC, appear to be both well dispersed in the water prior to
filtration, as observed visually, and well mixed in the dry film
(Figure 2). The dispersion of the inorganic particles in the
water is believed to be aided by the TEMPO-oxidized NFC,
acting as an analog to the, within the paper industries,
commonly used dispersive agent carboxymethyl cellulose
(CMC) [39]. This, since both the NFC used in this study and
CMC are negatively charged cellulose chains. The formed and
dried electrode surfaces (Figure 2) show a clear web-like
structure caused by the anisotropic NFC particles, which
relates to the binding function of NFC, and interpenetrating
networks of the inorganic particles incorporated into the
Figure 2 SEM image showing the top-side of a LiFePO4 paper
electrode. The web-like structure of NFC is clearly seen, binding
the larger LiFePO4 and smaller Super-P carbon particles.
nano-structure of the NFC network (Figure 2). The two-
layered electrode structure was intended to decrease the
contact resistance between the aluminum current collector
and the paper electrode when built into a battery. The
second layer consisted of a high fraction of Super-P carbon
particles (85%wt) with the outermost surface of this layer
presenting clusters of free carbon particles (Figure 3) toward
the oncoming current collector. This bi-layered electrode
shows a seamless integration of the two layers (Figure 4)
enabling good electrical contact between the two layers.
The single- and bi-layered paper electrodes turned out to
be 120 and 167 mm, respectively, with porosities of around
75% (Table 1). The chosen grammage was 8 mg/cm2 and can
easily be controlled by adjusting the amount of slurry added
in the filtration step.
An advantage with using cellulose as binder is that the
result is a mechanically strong, but still flexible, electrode.
Even though the NFC content in the electrodes was only
11%wt (corresponding to 5%vol considering the estimated
porosity), the electrodes showed good mechanical proper-
ties (Table 2) and continuous films with excellent flexibility
were formed (Figure 1).
The moduli of the single-layered electrodes, dried at
110 1C after filtration and solvent exchange and thereafter

Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002
4 S. Leijonmarck et al.

electrolyte prior to mechanical testing. These results will,

obviously, correlate better to the environment the electro-
des will experience during use in a battery. Compared to the
dry paper, soaking for 48 h in electrolyte led to a lower
stiffness (0.10 GPa), a lower stress at break (2.2 MPa) but
also to a higher strain at break (6.7%) for the samples dried
at 110 1C. The soaking in electrolyte does in fact make the
electrodes more ductile, which is advantageous for an
electrode in a flexible battery. The strength, although
lowered, was still high. A strength of 2.2 MPa means that
an electrode paper, 120 mm thick and 10 cm wide, can lift
up to 2.7 kg without breaking. Drying the samples at 170 1C
instead of 110 1C resulted in a change in mechanical proper-
ties. The main difference appeared in strain at break,
where the higher temperature resulted in lower strains at
break both for samples stored in air (1.4% in contrast to
Figure 3 SEM image showing the carbon (bright particles)/NFC
4.1%) and soaked in electrolyte (2.7% in contrast to 6.7%)
(dark surfaces) side of a bi-layered electrode paper. The Super-
indicating a more brittle material after drying at 170 1C as
P carbon particles are seen protruding through the paper
compared to 110 1C. These reductions in the mechanical
surface, enabling good contact with a current collector.
properties can be compared to the well-described hornifica-
tion processes in cellulose fibers. Evaporation of water from
cellulose fibers commonly causes irreversible structural
changes in the fibers leading to increased fiber stiffness
and reduced strength [36].
The conductivity of the single-layered electrode paper
was 3 S/m, when measured with the four-probe van der
Pauw method. However, when performing the conductiv-
ity measurements in a Swagelok cell, where the paper
electrode is pressed between two stainless steel plates,
the measured conductivity was only 0.02 S/m. This beha-
vior implies that the electrode structure is anisotropic,
likely with partially insulating NFC skins creating high
resistances through the plane of the paper. The bi-layered
electrodes showed higher conductivities for both test
methods (17 S/m and 0.14 S/m respectively), illustrating
that the carbon-rich film aides the electronic interactions
with the stainless steel electrode, as well as the in-plane
Figure 4 SEM image showing the cross-section of the interface
conductivity.
in a bi-layered electrode between the LiFePO4 layer
The electrodes were cycled in pouch cells against a
(larger particles) and the carbon layer (smaller particles).
lithium metal counter-electrode. The results (Figures
5 and 6) show that even though the electrodes were
prepared through water processing including hygroscopic
Table 1 Geometrical and electrical properties of the cellulose, good cycling performance was achieved. The
paper electrodes. one-layered electrode performed rather well both at low
currents, 140 mAh/g LiFePO4 at C/10, and high currents,
Single- Bi-
117 mAh/g LiFePO4 at 1C, as compared to the theoretical
layered layered
specific capacity of lithium iron phosphate at 170 mAh/g
Thickness [mm] 120 167 (Figure 6). The two-layered electrode showed an overall
Total porosity [%] 74 72 better performance, 151 mAh/g LiFePO4 at C/10, and
Loading [g LiFePO4/cm2] 8 8 performed particularly well at higher currents where
Conductivity, 4-probe [S/m] 3 17 the capacity was 132 mAh/g LiFePO4 at 1C (Fig. 6). The
Conductivity, Swagelok cell [S/m] 0.02 0.14 a increase in performance, between the single- and bi-
layered electrodes, most likely stems from the decreased
a
Two same-sized bi-layered electrodes were stacked with contact resistances caused by the added second carbon-
the respective carbon-rich surface facing the stainless steel rich layer.
surface. The coulombic efficiency differed significantly between
the samples dried at 110 1C and the ones stored at 170 1C.
The lower drying temperature resulted in low coulombic
stored at 25 1C and 50%RH, were 0.31 GPa with a stress efficiencies of around 97% during the first ten cycles,
and strain at break of 5.2 MPa and 4.1%, respectively. whereas the higher temperature produced efficiencies
A more useful measure of the mechanical properties is, of around 99%. This difference is believed to be caused by
however, the tensile results from samples soaked in battery water and solvent residues bound onto the NFC surfaces,

Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002
Preparation process and properties 5

Table 2 The mechanical characteristics of the single-layered paper electrode.

Dried at 110 1C, Dried at 170 1C, Dried at 110 1C, Dried at 170 1C,
stored at 50%RH stored at 50%RH soaked in electrolyte soaked in electrolyte

Young’s modulus [GPa] 0.31 0.34 0.10 0.15

Ultimate strength [MPa] 5.2 3.5 2.2 1.8
Strain at break [%] 4.1 1.4 6.7 2.7

Figure 5 Charge/discharge voltage over ten cycles from

a bi-layered electrode measured against a lithium metal
counter electrode at C/10. Figure 7 Coulombic efficiency for the first ten cycles at C/10
for the single- and bi-layered electrodes.

not of great importance. The higher temperature can be used

Figure 6 Rate capabilities for the LiFePO4/NFC electrodes,
dried at 170 1C versus a Li metal electrode. The specific
capacity is given as capacity divided by mass of LiFePO4 in
the electrodes, at the currents C/10, C/4, C/2, 1C and C/10 as
indicated in the figure.
contaminating the battery electrolyte and resulting in para-
sitic side-reactions during delithiation of the LiFePO4 paper
electrode.
An improvement in coulombic efficiency was found on
increasing the drying temperature from 110 1C to 170 1C
(Fig. 7). Drying at 170 1C, however, also affected the mechan-
ical behavior of the electrodes, resulting in a less ductile
material. Based on these results, the choice of drying tempera-
ture is important. A lower temperature is needed whenever a
highly flexible electrode is required and the cycling lifetime is
when the requirements on the cycling are higher but a less
ductile material can be accepted. Regardless of drying tem-
perature, flexible electrodes with good cycling behavior were
produced with the described method. However, an improved
drying process and/or a surface treatment, such as hydropho-
bation, of the fibrils to produce a less hygroscopic material
could possibly increase the coulombic efficiency further without
affecting the mechanical properties. Another important aspect
is that the electrodes showed good mechanical properties when
soaked with battery electrolyte. The mechanical properties also
depended on whether the electrodes were dry or soaked with
electrolyte and it is therefore important to measure such
properties on paper electrodes when soaked to achieve realistic
data applicable for battery use. Avoiding the metal current
collectors used in this study would be favorable for a flexible
battery as the metal sheets are not as stretchable as the
electrode papers. Depending on the size and rate-capability
needed for the battery, one could imagine using the carbon-rich
layer in the bi-layered electrode as current collector (17 S/m in
total conductivity in the plane).
Conclusions
Positive electrodes based on lithium iron phosphate,
LiFePO4, with a binder consisting of TEMPO-oxidized nano-
fibrillated cellulose (NFC) have been successfully produced
in a water-based paper-making type of process. The elec-
trodes were produced both as single- and bi-layered elec-
trodes, where the latter contained a carbon-rich layer that

Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002
6 S. Leijonmarck et al.
enhanced the rate capability. Two-layered electrodes pro-
vided a reversible specific capacity of 132 mAh/g at 1C in a
battery cell against lithium metal. These electrodes were
flexible both in dry condition and when soaked in battery
electrolyte, with Young’s moduli at 0.31 and 0.10 GPa,
respectively, for paper electrodes dried at 110 1C. The
drying temperature was found to be important and to affect
both the mechanical properties, making the electrodes
more ductile at lower temperatures, as well as the electro-
chemical properties, causing a higher coulombic efficiency
at higher temperatures.
Acknowledgments
The Knut and Alice Wallenberg Foundation is much appre-
ciated for financial support. Anna Svensson is much
acknowledged for the making of the TEMPO-oxidized NFC.
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Glossary
NFC: Nano-fibrillated cellulose
RFID: Radio frequency identification
TEMPO: 2,2,6,6-tetramethylpiperidine-1-oxyl
CMC: carboxymethyl cellulose
PVDF: polyvinylidene fluoride
NMP: N-methyl-2-pyrrolidone
EC: Ethylene carbonate
DEC: Diethyl carbonate
SEM: Scanning electron microscope
Simon Leijonmarck is a Ph.D. student at KTH
Royal Institute of Technology at the depart-
ment of Chemical Engineering. The topics of
the Ph.D. work have been functional adhe-
sives and novel Li-ion battery designs.
Simon received his MSc in material chem-
istry from Stockholm University in 2008 and
has performed his Ph.D. studies since.
Preparation process and properties 7

Ann Cornell is an associate professor in Lars Wågberg is professor in Fibre Technol-

Chemical Engineering at KTH Royal Institute ogy at KTH Royal Institute of Technology in
of Technology in Sweden. After receiving Stockholm Sweden. His research team is
her MSc in 1987 she worked for 15 years in focused on using cellulose in new materials
industry (today Akzo Nobel) with R&D and products and to create high value-
mainly related to the development of indus- added products based on renewable cellu-
trial chlorate electrolysis. In 2002 she lose fibres. The team has developed high
received a Ph.D. from KTH in chemical resolution methods for determining mole-
engineering and since 2003 Ann works in cular interactions at cellulose, hemicellu-
the group of Applied Electrochemistry at lose and lignin interfaces by using model
KTH, still conducting research related to films of the respective components and
industrial electrolysis but has also broadened her interests to areas different spectroscopic techniques. Lars holds a Ph.D. from KTH in
as cellulose based Li-ion batteries. applied surface and colloid chemistry and has spent 12 years in the
industry doing research on fundamentals of hygiene products and
Göran Lindbergh is since 2003 professor in fiber based materials.
Chemical Engineering at KTH Royal Institute
of Technology. He received his MSc in 1985
and his Ph.D. in 1991. He is heading the
Applied Electrochemistry group working
with electrochemical power sources and
electrolytic processes within the field of
electrochemical engineering. A common
theme in the ongoing research projects is
the mathematical modeling and electroche-
mical characterization of electrochemical
systems. Of special importance is the development and application
of porous electrode theories for battery electrodes and gas diffu-
sion fuel cells electrodes.

Please cite this article as: S. Leijonmarck, et al., Flexible nano-paper-based positive electrodes for Li-ion batteries—Preparation process
and properties, Nano Energy (2013), http://dx.doi.org/10.1016/j.nanoen.2013.02.002