Improving ion-exchange membrane

properties by the role of nanoparticles

Cite as: AIP Conference Proceedings 1788, 030003 (2017); https://doi.org/10.1063/1.4968256
Published Online: 03 January 2017

Danu Ariono, and Khoiruddin

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© 2016 Author(s).
 Improving Ion-Exchange Membrane Properties by the Role
of Nanoparticles
Danu Ariono1, a) and Khoiruddin1, b)
1
Department of Chemical Engineering, Institut Teknologi Bandung, Jl. Ganesha 10, Bandung 40132, Indonesia
a)
Corresponding author: danu@che.itb.ac.id
b)
khoiruddin57@yahoo.com

Abstract. Extensive application of synthetic ion-exchange membrane (IEM) in many areas has necessitated the
improvement of their properties. Recently, the introduction of nanoparticles into polymeric membrane has attracted
growing interest since the combination of both materials results in better properties. This well-known mixed-matrix
membrane exhibits superior characteristics compared to an individual polymeric membrane. Properties of the
nanoparticles such as electrical conductivity, hydrophilicity, and adsorption capacity can be utilized to produce the IEM
with better physicochemical, electrochemical, and mechanical characteristics. The nanoparticles may also be used to
achieve a specific characteristic such as an antibacterial property and monovalent ion permselectivity. In this paper,
preparation, the role of inorganic materials and performance of mixed-matrix IEM are reviewed. In addition, challenges
facing mixed-matrix IEM and strategies taken to overcome those challenges and future perspectives are discussed.

INTRODUCTION
Rapid growth in membrane technology development is primarily based on consciousness on the potential and
advantages of this technology allowing a wide range of potential applications in almost every industrial sector [1].
The advantages of membrane technology include energy efficiency, high separation capacity, selective separation,
process intensification or reduction in a number of unit process, and low investment cost [2]. Membrane technology
is now competing with conventional or other technologies in various functions. The membrane can be used as
molecular separation unit, contacting device, diffuser, reactor, catalyst, emulsification unit, hybrid process, etc. [2-
15]. Ion-exchange membrane (IEM) is a charged membrane which is mainly used as a selective separator for ionic
components. IEM has been widely used in a number of different processes and in the various field of applications
such as desalination and seawater pre-concentration, production of chlorine-alkaline, production of organic acids
and organic salts, production of ultrapure water, wastewater treatment, and energy generation [16-23]. With those
various potential applications, IEM-based processes are considered to be the crucial processes in water and energy
supply, chemical industry, and environmental protection.
These extensive applications have necessitated the improvement in IEM properties to achieve better performance
of the processes since the IEM is the key of separation. Recently, development of IEMs has gained much attention
which has been driven by the need to obtain the membranes with better properties, lower production cost, and easier
preparation procedure. Many attempts have been proposed to produce IEMs with improved characteristics, e.g.
selection of appropriate materials, incorporation of additive which has specific properties, membrane surface
modification, and other post-treatments. One of the promising modification methods is by introducing nanoparticles
into a polymeric membrane to combine the advantages of the both materials. These well-known mixed-matrix
membranes are expected to have superior characteristics compared to the individual polymeric membrane. In this
paper, preparation and modification of IEMs using nanoparticles will be introduced, continued with an overview of
characteristics of modified IEMs. In addition, challenges countered for incorporating nanoparticles into polymeric
IEMs are pointed out.

International Conference on Engineering, Science and Nanotechnology 2016 (ICESNANO 2016)

AIP Conf. Proc. 1788, 030003-1–030003-8; doi: 10.1063/1.4968256
Published by AIP Publishing. 978-0-7354-1452-5/$30.00

030003-1
 MODIFICATION OF IEM USING NANOPARTICLES

Preparation of IEM
Most commercial IEMs can be classified into two major categories, namely homogeneous and heterogeneous
membranes with their typical properties and advantages [24]. Homogeneous and heterogeneous IEMS are
distinguished based on the structure of the membrane, particularly on the phases incorporated in the membrane
matrix. The homogeneous membrane has a single polymer which acts as both for a membrane former and for the
ion-exchanger. Meanwhile, the heterogeneous has two different polymers which have different functions. The first
polymer acts as the membrane structural material while the second one is ion-exchange resin particles. Generally,
the heterogeneous IEM has lower conductivity and permselectivity than the homogeneous membrane which are
attributed to their structure. Longer pathway for ionic mobilization and the presence of inert fraction in the
membrane phase contribute to the lower conductivity or the high resistivity while a leakage of co-ions through
solution phase in the membrane results in the lower permselectivity [25, 26]. However, there is growing attention in
the development of heterogeneous IEM since it has simpler fabricating procedure.
Methods for preparation of IEM are reported in literature including the preparation of homogeneous and
heterogeneous IEMs [27-29]. For homogeneous IEM, the methods can be summarized into three different
categories: (1) polymerization or polycondensation of monomers containing anionic or cationic moieties, (2)
introduction of the moieties into polymer film, or (3) preparation of polymer solution using polymer that contains
moieties then followed by casting the solution into a film [28]. Nafion is a typical example of the homogeneous
membrane with excellent characteristics.
For heterogeneous IEM, finely ground ion-exchange resins are commonly embedded into an inert polymer with
two different methods [29]. The first one is by mixing fine ion-exchange particles with a polymer binder. This
mixed product is then pressed in a mold at appropriate temperature and pressure into a flat membrane. For the
second method, fine ion-exchange resin particles are dispersed into a polymer solution, followed by casting the
solution into a sheet. Subsequently, to remove the solvent, the synthesized membrane can be either dried at room
temperature, immersed in a coagulation bath containing non-solvent, or treated through combined method wherein
the drying period is set [24]. This method has also been applied to fabricate hollow fiber IEM [30]. Since the
polymer binder is inert and the cationic or anionic moieties are on the ion-exchange particles, thus these functional
groups are distributed unevenly yet clustered. Therefore, this preparation method results in inhomogeneity of the
membrane structure (Fig. 1).

(a) (b)

FIGURE 1. Heterogeneous IEM. (a) Schematic of heterogeneous IEM and (b) SEM image of polysulfone-based membrane [31].

Introduction of Nanoparticles into IEM

There are several methods possible to introduce nanoparticles into IEMs, such as additive blending, plasma
treatment, in-situ polymerization, sol-gel process, etc. The introduction of the nanoparticles can be conducted during
or after the preparation of the base membrane. Furthermore, the nanoparticles can be introduced into the membrane

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matrix or on the membrane surface (Fig. 2). The introduction of additive into membrane solution or the additive
blending method is a simple method for improving membrane characteristics. Additive blending has been used in
many works to introduce inorganic particles into IEM [31-39]. In this method, nanoparticles are blended with a
polymer and solvent. This solution is then cast into a pre-formed membrane, and the solvent is separated through
solvent evaporation, solution immersion, or combined process. This blending method is also applied in extrusion
technique [40]. In extrusion, additives are mixed with a polymeric binder and ion-exchange resin particles.
Afterward, the mixed product is fed into an extruder and extruded at appropriate temperature and pressure into a flat
sheet membrane.
It is well known that membrane surface and morphology play an important role in the membrane performance.
Modification of membrane surface is one of the most used methods for improving membrane characteristics. In
surface modification using nanoparticles, the nanoparticle can be deposited on the membrane surface by using a
plasma treatment method [41-43]. In a plasma treatment, the base membrane is placed in a vacuum reactor. A
modifier such as a silver plate is placed in the reactor at a certain distance to the membrane. Argon gas is used as
plasma former in a magnetron sputtering system. The deposition rate of the modifier can be adjusted, so desired
coating thickness is obtained. This plasma treatment can produce a nanolayer on the base membrane with a fine
distribution. To improve the stability of the deposited nanoparticle on the membrane surface, plasma treatment could
be combined with thermal treatment [44].
Surface modification is also conducted by incorporating nanoparticles into an additional layer prepared by in-situ
polymerization on the membrane surface [45, 46]. This method is simpler than plasma treatment. The nanoparticles
are blended into a solution containing monomers and then poured onto the base membrane surface. The solution is
then heated in an oven for a period of time. When the polymerization is finished, a new layer containing
nanoparticle is formed on the membrane surface.
The nanoparticles may also be introduced into the membranes through a sol-gel reaction. For example,
tetraethylorthosilicate (TEOS) is mixed with a polymer solution containing catalyst [47]. The resulting gel is then
cast to obtain a film. Furthermore, the synthesized membrane can undergo a reaction for crosslinking formation.
Another technique is by immersing a base membrane into a solution containing TEOS and other compounds which
are involved in the polymerization reaction [48]. During the immersion, the solution is allowed to permeate into the
base membrane. The modified membrane is then dried in an oven to remove excess reactants such as alcohol and
water. By using this method, nanosilica particles are trapped inside the membranes and linked with the base
polymer.

FIGURE 2. Schematic of modified IEMs. Nanoparticles are introduced (A) into the membrane matrix, (B) on the membrane
surface, and (C) inside an additional layer on the membrane surface.

Heidary et al., [49] reported a preparation of composite IEM containing FeOOH nanoparticle via in-situ
formation. In this method, a certain amount of FeCl3.6H2O was added into membrane solution. Subsequently, the
solution pH was adjusted to about 12 by adding NH4OH. When the solution turned from yellow to brown, the
FeOOH nanoparticle was formed. Sonication was employed to obtain a better dispersion of nanoparticle and avoid
aggregation. They reported that nanoparticle with about 14 nm average size could be produced.

CHARACTERISTICS OF MODIFIED IEMs

A simple correlation between parameters of IEM has been explained by Xu et al. [50]. IEM properties such as
water transport number, salt permeation, co-ion diffusion, mechanical strength, the selectivity of ions with the same
charge, counter-ion transport number, conductivity, and degree of swelling are qualitatively dependent on water

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content or water uptake (Wu) and ion-exchange capacity (IEC) of the membrane. For example, conductivity and
degree of swelling are increased with the increase of Wu and IEC. Meanwhile, the selectivity of same charged ion
and the counter-ion transport number are decreased with increasing Wu and they are increased with increasing IEC.
These two main properties are then suggested to be used in predicting the other characteristics of IEM. Therefore,
many attempts are devoted to improve these two properties such as by introducing an additional charge into
membrane matrix, incorporating nanoparticles which contain functional groups, blending of polymer which has
different hydrophilicity, etc. Among them, incorporating nanoparticle is one of the most promising methods.
The properties of the additive such as electrical conductivity, hydrophilicity, and adsorption capacity can be
utilized to produce a membrane with better electrochemical characteristics (Fig. 3). Charged groups provided by the
nanoparticles may improve ion-exchange capacity. The additional functional groups can enhance the ionic transport
and counter-ion permselectiviy [51, 52]. The high electrical conductivity of the nanoparticles, e.g. silver, carbon
nanotube, results in higher conductivity. Nanosilica, which has high hydrophilicity, can entrap water in low
humidity condition and improves the performance of IEMs for fuel cell application [38, 48, 53]. The entrapped
water could enhance proton conductivity thus increases the conductivity. Zeolite nanoparticle showed the same
manner [54]. In addition, in the case of carbon nanotube, additional water channels could be provided [33]. This
additional channel could be due to the diameter of carbon nanotube which is large enough to accommodate water
molecules. This channel increases membrane water uptake and ionic permeability.

FIGURE 3. Properties of some unmodified and modified PVC-based heterogeneous IEMs by nanoparticles. Membranes: (1-4)
Cation-exchange membrane and (5-6) Anion-exchange membrane. Additive: (1) Iron-nickel oxide (0.5 wt.%); (2) Aluminium
oxide (16 wt.%); (3) Ilmenite (16 wt.%); (4) FeOOH (3 wt.%); (5) Titanium dioxide (0.5 wt.%); and (6) Polyaniline/Multi-wall
carbon nanotube (1 wt.%). Data collected from references [37, 49, 52, 55-57].

The addition of nanoparticles in appropriate amount may also result in improvement of mechanical strength.
According to Safronova et al., the improvement could be related to the effect of nanoparticle on the system pores
and channels [58]. When a small amount of nanoparticle is added, an osmotic pressure that attempts to deform pores
from the inside just compensates the elastic deformation forces. As the results, the pore size is increased as well as
the strength of the membrane. A similar result was observed in another work [59]. The improvement of mechanical
strength was also explained as the result of strong interfacial bonding between the polymer and additive particle
[60]. The presence of nanoparticles induces a new bonding. If the bonding is strong enough, it will help in
strengthening the membrane structure.

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 Moreover, by using nanoparticles, a specific characteristic of IEMs could be obtained, e.g. the antibacterial
property, improved monovalent ion permselectivity, oxidative stability, low methanol crossover for a direct
methanol fuel cell (DMFC), etc. (Table 1). These specific properties are required in some applications or in some
conditions. The addition of nanoparticles in several works showed that the particle could provide an antibacterial
property. This antibacterial property, for example, is due the addition of silver nanoparticle which is known as an
inhibitor for microorganism [61]. Modified IEM with the improved antibacterial property was also observed when
ZnO nanoparticle was incorporated [62].

TABLE 1. Typical example of modified IEM with specific property

Membrane Type Modifier Method Features Ref.
PVC/SBR (htr) Fe-Ni nanoparticle Fe-Ni: Additive blending Antibacterial effect (E-Coli [42]
and Ag nanolayer Ag nanolayer: plasma removal)
treatment
PVC (htr) Ag nanoparticle Additive blending Antibacterial effect (E-Coli [61]
(30-50 nm) removal)
PVC (htr) ZnO nanoparticle Additive blending Antibacterial effect (E-Coli [62]
(20 nm) removal)
PVA (htr) Silica (TEOS) Sol-gel method Improved monovalent ion [47]
permselectivity and more
compactness.
PVC (htr) Al2O3 (80 nm size) Additive blending Higher permselectivity of [56]
monovalent ion compared to
bivalent ion.
PVC (htr) Fe3O4 (60 nm) Additive blending Improved monovalent [63]
permselectivity.
SPEEK (hmg) Sulfated zirconia Additive blending Improved oxidative stability [64]
(20 nm)
Nafion (hmg) Na2Ti3O7 nanotube Additive blending Reduced methanol crossover [65]
(d= 4-6 nm; l=
500 nm)
Nafion (hmg) Silica (TEOS) Sol-gel reaction and Reduced methanol crossover [66]
solution casting method
Note: PVA= polyvinyl alcohol; PVC= polyvinyl chloride; SBR= styrene–butadiene–rubber; SPEEK= sulfonated poly(ether
ether) ketone; htr= heterogeneous membrane; hmg= homogeneous membrane;

Meanwhile, a monovalent permselective IEM is produced due to the sieving mechanism of modified IEMs. In
the additive blending method, an additive nanoparticle may contribute to membrane solution viscosity [31]. Since
higher nanoparticle loading results in higher solution viscosity, it produces a membrane with less porosity.
Obviously, the membrane with less porosity possesses excellent pemselectivity while on the other hand, it shows
poor conductivity. Moreover, the less porosity or more dense structure yields in declining permeability of ions with
higher Stoke radius. The ability of IEM to discriminate ion with the same charge was investigated by Nagarale et al.
[47]. To obtain the ability, nanosilica was added into polyvinyl alcohol based heterogeneous IEM via sol-gel
method. It was observed that selective permeation depended on Stokes radius of ions. Furthermore, membrane
compactness was increased with increasing additive content. Consequently, the ability to discriminate between
counter-ions (ions with opposite charge to membrane fixed charge) was also increased. Hosseini et al. investigated
the effect of TiO2 nanoparticle loading on heterogeneous IEM characteristics [67]. They found that TiO2 had a
strong adsorptive affinity toward bivalent (Ba2+) ion attraction compared to the monovalent ion (Na +). The strong
adsorption reduced the permeability of barium compared to natrium.
The addition of nanoparticle is also aimed to obtain a specific characteristic for fuel cell application, for
example, an oxidative stability. It was reported that proton exchange membrane modified with zirconia
nanoparticles exhibits an improvement of the oxidative stability [64]. This improvement was the result of radical
peroxide decomposition which was facilitated by sulfated zirconia. In direct alcohol fuel cell (DAFC), alcohol
crossover is the main drawback [68, 69]. Alcohol crossover leads to fuel loss and declining performance of DAFC
thus requires a membrane with low alcohol permeability. Therefore, a number of works have been conducted to

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synthesize membrane with low alcohol permeability [69-74]. An example of Nafion modified membrane with low
methanol permeability has been prepared by Wei et al. where Na2Ti3O7 nanotubes are used as the modifier [65, 75].
The sodium titanium solution was mixed with Nafion solution. The composite membrane was prepared by solution
casting method. The result of the study indicated the effectiveness of sodium titanium nanotube in hindering
methanol crossover. The nanotube effectively blocks the nano-channels and reduces methanol diffusivity.
Furthermore, this effect was increased with increasing nanotube content.
Many works indicate that the addition of nanoparticle into membrane matrix can improve membrane
characteristics. Nanoparticle plays an important role in increasing the amount of adsorbed water or retaining water
inside the membrane and providing the additional sites to enhance ion-exchange capacity. Moreover, nanoparticle
also contributes to the formation of membrane structure. Nanoparticle may reduce membrane porosity or even
induce additional water channel. In addition, unique properties of nanoparticle can be used to obtain some specific
characteristic.

CHALLENGES AND PERSPECTIVE

The incorporation of nanoparticles is one of the most promising methods for improving the properties of IEMs.
The modification is able to improve electrochemical characteristics of the membranes. It provides the possibility to
produce heterogeneous IEMs with comparable performance to the homogeneous ones [24]. The modified
membranes also exhibit superior characteristics compared to an individual polymeric membrane for many
applications, such fuel cell, electrodialysis, etc. Unfortunately, when the additive loading exceeds a certain
concentration, the properties such as conductivity and permselectivity are decreased. This is attributed to void
fraction occupied by the additive thus results in inaccessibility of functional groups. Consequently, both
conductivity and permselectivity are decreased. The inaccessibility of functional groups could also occur if the
nanoparticles are deposited on the membrane surface. The additional layer introduces an additional resistance for
mass transfer or barrier for ionic migration and penetration. However, the permselectivity could be more enhanced.
The most important part of the mixed-matrix membrane is the compatibility between the nanoparticles and the
polymeric matrix and distribution of the nanoparticles. The compatibility and fine distribution could be achieved by
selecting the appropriate materials, involving a coupling compounds and improving the particles dispersion (highly
ordered particles). In preparation of heterogeneous IEM, an improved distribution of ion exchange resin particle has
been achieved by applying an alternating current field during membrane synthesis [76-78]. The electrical field
induces the ion exchange particle to align and form a long chain which results in a highly ordered particle. The
highly ordered particle yields in the improvement of IEM properties. The improved IEM properties with the
improved particle distribution are also reported as a result of applying magnetic field [79]. In this case, the magnetic
field induces the alignment of a magnetic ion-exchange nanoparticle. Recently, sonication is used in several works
on preparations of heterogeneous IEM [55, 80-85]. They observed that sonication has a significant influence on
resin particle distribution in membrane matrix, can help to break particle aggregation and provide the possibility to
make a uniform phase. In addition, they reported that sonication increased polymer particle interactions and
promoted the compatibility of particles with a polymer binder. Another approach is by functionalizing the inorganic
particle [86]. The inorganic particle is functionalized with functional groups that can interact chemically with the
polymer matrix thus improving the compatibility of the additive particle. By using these techniques, mixed matrix
membrane with a fine distribution of nanoparticle and good compatibility between nanoparticles and polymer can be
produced.

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