International Journal of Renewable Energy Development
Int. J. Renew. Energy Dev. 2023, 12 (2), 375-380
|375
https://doi.org/10.14710/ijred.2023.49909
ISSN: 2252-4940/© 2022.The Author(s). Published by CBIORE
Contents list available at IJRED website
International Journal of Renewable Energy Development
Journal homepage: https://ijred.undip.ac.id
QPVA-Based Electrospun Anion Exchange Membrane for Fuel Cells
Asep Muhamad Samsudin a,b* and Viktor Hackera
aInstitute of Chemical Engineering and Environmental Technology (CEET), Graz University of Technology, Austria
bDepartment of Chemical Engineering, Diponegoro University, Indonesia
Abstract. The anion exchange membrane is one of the core components that play a crucial and inseparable role in alkaline anion exchange membrane
fuel cells. Anion exchange membranes (AEMs) were prepared from quaternary ammonium poly(vinyl alcohol) (QPVA) by an electrospinning method.
QPVA was used both as material for electrospun fiber mats and as filler for the inter-fiber void matrix. The objective of this work is to investigate the
influence of the inter-fibers void matrix filler concentration on the properties and performance of eQPVA-x AEMs. FTIR spectra were used to identify
the chemical structures of the AEMs. The primary functional groups of PVA and quaternary ammonium-based ion conducting cation were detected.
The surface morphology of QPVA nanofiber mats and eQPVA-x AEMs was observed using SEM. Electrospun nanofiber structures of QPVA with an
average size of 100.96 nm were observed in SEM pictures. The ion exchange capacity, swelling properties, water uptake, and OH− ions conductivity
were determined to evaluate the performance of eQPVA-x AEMs. By incorporating the QPVA matrix of 5 wt.% concentration, the eQPVA-5.0 AEMs
attained the highest ion exchange capacity, water uptake, swelling properties, and OH− conductivity of 0.82 mmol g−1, 25.5%, 19.9%, and 2.26 m⋅s
cm−1, respectively. Electrospun QPVA AEMs have the potential to accelerate the development of alkaline anion exchange membrane fuel cells.
Keywords: anion exchange membranes, fuel cells, QPVA, electrospinning, nanofibers
@ The author(s). Published by CBIORE. This is an open access article under the CC BY-SA license
(http://creativecommons.org/licenses/by-sa/4.0/).
Received: 30th Oct 2022; Revised: 2nd January 2023; Accepted: 29th January 2023; Available online: 11th February 2023
1. Introduction
The decline of energy reserves and the occurrence of ecological
damage encourage researchers to develop renewable energy
sources that are more environmentally friendly, efficient, and
sustainable. Efforts to produce electrical energy from
mechanical, thermal, and chemical energy have continued in
the last few decades (Ayaz et al., 2022).
Among the developed new energy sources, the fuel cell is
regarded as eco-friendly alternative energy that can replace
conventional fossil fuels with high efficiency of energy
conversion and almost no emissions. Anion exchange
membrane fuel cells (AEMFCs), as one fuel cell category, are
getting immense attention because of their advantages. The
advantages include the opportunity to utilize less expensive
transition metals instead of a costly catalyst of platinum group
metals (PGM) and a faster oxygen reduction process. Due to the
counter-direction between the fuel and OH− ions, AEMFCs also
benefit from reduced fuel crossover and reduced corrosion
concerns in alkaline environments (Iravaninia & Rowshanzamir,
2015; Samsudin et al., 2022).
Anion exchange membranes (AEMs) are part of a fuel cell
that has an essential role in hydroxide conduction, electron
inhibition, and gas barrier (Hagesteijn et al., 2018; Ramaswamy
& Mukerjee, 2020). Despite their positive points, the
development of AEMFCs faces several difficulties. Since
hydroxide ions have lower mobility than hydrogen ions, the
ionic conductivity of AEMs tends to be lesser than that of proton
exchange membranes (PEMs) (Das et al., 2022). The toxic and
expensive solvents are also an issue in the synthesis of some
* Corresponding author
Email: asep.samsudinl@live.undip.ac.id (A.M. Samsudin)
AEMs. In addition, complex routes and costly equipment have
also become a concern (Wang et al., 2013).
Polymers are the backbone material used in the
manufacture of AEMs. To date, many types of polymers have
been developed for AEMs, ranging from poly (aryl ether) based
AEMs (e.g., poly (ether sulfone) (Du et al., 2022; Wang et al.,
2022), poly(2,6-dimethyl-1,4-phenylene oxide)(Becerra-
Arciniegas et al., 2019; Mayadevi et al., 2022) and aryl-ether free
AEMs (e.g., polybenzimidazole (Guo et al., 2022; G. Zhang et al.,
2022) and aliphatic-based AEMs (e.g., poly (vinyl alcohol)
(Huang et al., 2022; Samsudin & Hacker, 2019, 2021).
Poly(vinyl alcohol) (PVA) is a synthetic polymer that
possesses scentless, flavorless, biocompatible, and
biodegradable characteristics. Due to its beneficial attributes,
PVA is frequently employed as a backbone polymer for AEMs
development. Due to its hydrophilicity, it exhibits a high water
uptake and possesses exceptional film-forming characteristics.
Furthermore, the availability of reactive functional groups and
lesser fuel crossover are favorable for chemical crosslinking and
other modifications that improve the properties of the
membrane (Aslam et al., 2018; Ding & Qiao, 2022; Samsudin et
al., 2022; Susanto et al., 2016; Zhang et al., 2013).
Various techniques and methods for membrane preparation
of functionalized polymers have been introduced. Solution
casting is a membrane casting technique that has been widely
used because it is simple, easy, and versatile (Samsudin et al.,
2022). Apart from solution casting, another method that is
starting to attract attention is electrospinning. This technique
employs a high-voltage source to induce an electric field from
Research Article
https://doi.org/10.14710/ijred.2023.49909
https://doi.org/10.14710/ijred.2023.49909
mailto:asep.samsudinl@live.undip.ac.id
https://orcid.org/0000-0002-0131-5667
https://orcid.org/0000-0001-5956-7579
http://crossmark.crossref.org/dialog/?doi=10.14710/ijred.2023.49909&domain=pdf
A.M.Samsudin et al Int. J. Renew. Energy Dev 2023, 12(2), 375-380
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the spinneret to the collector. A Taylor cone emerges at the
spinneret's edge at a particular electric field intensity. After
intensity overcomes polymer drop surface tension, an
electrified solution jet is released from the Taylor cone. The
solution jet evaporates and solidifies in the collector, forming
nanofibers (Sood et al., 2016). Electrospinning is favorable
because it facilitates the formation of interlinked structures,
which improves OH− transfer. Additionally, electrospinning is
effective for achieving a uniaxial alignment of nanofiber-formed
polymer chains that has the potential to strengthen the
membrane (Fennessey & Farris, 2004; Sood et al., 2016; Tamura
& Kawakami, 2010).
Despite the many benefits, the fabrication of anion exchange
membranes by electrospinning is still limited. Yang et al.
prepared electrospun AEMs, which utilized a combination of
poly(vinyl alcohol) and chitosan. They investigated the impact
of various crosslinking times on the characteristics of the
membrane (Yang et al., 2018). Gong et al. compared
imidazolium-functionalized polysulfone (IMPSF) AEMs
manufactured by the solution casting and electrospinning
methods. The results depict that electrospun AEMs produce
higher conductivity and lower swelling properties than cast
membranes (Gong et al., 2016). Du et al. fabricated quaternized
poly(2,6-dimethyl-1,4-phenylene oxide) electrospun
(QPPONF)/poly(vinyl alcohol) anion exchange membrane. By
varying the ratio between QPPONF and PVA, it was found that
the addition of the ratio of QPPONF to PVA increased the ion
conductivity of AEMs (Du et al., 2020).
Most developments in the field of electrospun anion
exchange membranes have concentrated on nanofiber mats,
while studies on matrix fillers are still rare. In this work, QPVA-
based electrospun nanofiber AEMs were prepared by an
electrospinning method. A commercially available QPVA,
namely GohsenxTM K-434, was used for both the fibers and the
matrix filler between the fibers. The objective of this work is to
study the influence of different concentrations of QPVA as inter-
fibers void matrix fillers on the AEMs properties.
2. Experimental
2.1 Preparation of Electrospun AEMs
12 wt.% of QPVA solute was prepared by dissolving QPVA
(GohsenxTM K-434, 85.5-88.0% hydrolyzed, 18-22 mPa.s,
obtained from Mitsubishi Chemical Corporation) in ultrapure
water (UPW, resistivity ~18 MΩ.cm) with constant stirring at
80–90 °C overnight. The chemical structure of GohsenxTM K-434
is depicted in Figure 1. A quantity of the QPVA solution was
then inserted into a 10 mL size spinneret needle syringe. A
horizontal movable spinneret and a drum collector which a
distance of 10 cm were used to increase the dimensional
homogeneity of the membrane. Then, 20 kV high voltage was
introduced between the spinneret edge and the aluminium foil-
coated drum collector. The electrospinning was carried out with
a polymer flow rate of 0.5 mL/h at room temperature. The
relative humidity was set in the range of 50−60%. The QPVA
fiber mats were heated at 130 °C for one hour to induce physical
crosslinking between QPVA polymer chains. Subsequently, they
were soaked in a cross-linker solution composed of 2.5 wt.%
glutaraldehyde, 0.2 wt. % hydrochloric acid in acetone to
promote chemical crosslinking. To produce dense AEMs
(QPVA-x), QPVA Fiber mats were then submerged in various
concentration of GohsenxTM QPVA solution at room
temperature. Then, crosslinking was repeated for AEMs to
increase crosslinking degree QPVA chains. The identities of the
QPVA AEMs were determined using Table 1. The AEM's
preparation processes are shown in Figure 2.
Fig. 1 The structure of GOHSENXTM K-434
Table 1
The AEMs samples composition
Membrane
Samples
Fiber (QPVA)
(wt.%)
Matrix Filler Concentration (QPVA)
(wt.%)
cQPVA 12 -
eQPVA-2.5 12 2.5
eQPVA-5.0 12 5.0
eQPVA-7.5 12 7.5
eQPVA-10.0 12 10.0
2.2 FTIR Analysis
An IR-Bruker ALPHA spectrometer was used for the FTIR study
to determine the major functional group of the membranes.
FTIR analysis was conducted at a wavenumber of 400–4000
cm−1 and a resolution of 4 cm−1. The IR spectra of the AEMs
were displayed as absorbance versus wavenumber graphs.
2.3 SEM Analysis
SEM analysis (Zeiss Supra 55VP) was conducted to study the
morphology of the electrospun QPVA AEMs. The measurement
was performed at a voltage of 15 kV. The nanofiber size
distribution of the electrospun mats was determined using
ImageJ software on SEM results.
2.4 Ion Exchange Capacity (IEC)
The IEC of eQPVAx AEMs was measured by back titration.
Firstly, the membranes were weighed and then soaked for 24 h
in 1 M KOH solution to change the AEMs into OH− form. After
removing the KOH residue using ultra-pure water for 24 h, the
AEMs samples were then soaked for 24 h in 0.1 M HCl solution.
The titration was accomplished using 0.1 M KOH solution. IEC
was calculated using Formula 1 (Samsudin et al., 2022) as
follows:
IEC = (𝐕𝐕𝐛𝐛−𝐕𝐕𝐦𝐦).𝐂𝐂𝐇𝐇𝐂𝐂𝐇𝐇
𝐰𝐰𝐝𝐝
(1)
where, Vb, Vm, CHCl, and Wd are the consumed KOH volumes of
the 0.1 HCl solution without membrane samples, the consumed
KOH volumes of AEMs, the HCl concentration, and the dry
weight of AEMs, respectively.
2.5 Swelling Properties
The AEMs' swelling properties were assessed by measuring
water uptake (WU) and swelling degree (SD). The WU was
measured by determining the weight difference of the AEMs
after submerging them in water. On the other hand, the SD was
evaluated by comparing the volume of AEM due to water
immersion for 24 h in RT. Formula 2 and 3 (Movil et al., 2015)
were used for calculating the WU and SD as follows:
WU = Ww − Wd
Wd
x 100% (2)
SD = Vw − Vd
Vd
x 100% (3)
where, Ww, Wd, Vw, and Vd are the wet weight, dry weight, wet
volume, and dry volume of AEMs, respectively.
A.M.Samsudin et al Int. J. Renew. Energy Dev 2023, 12(2), 375-380
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Fig. 2 Schematic of the preparation procedure
2.6 Ion Conductivity
Electrochemical impedance spectroscopy was utilized to
evaluate ionic conductivity (σ). The Gamry Reference 600
potentiostat was used in conjunction with a standard four-probe
conductivity clamp (Scribner Associates, USA). The impedance
of OH− form AEMs was measured between 0.1 Hz and 10 kHz
frequency and with 50 mV voltage. Formula 4 (Feketefoldi &
Cermenek, 2016) was used for calculating the σ as follows:
σ = d
Rm.T.W
(4)
Where d, Rm, T, and W are the distance of electrodes, the
impedance of membranes, the thickness of wet AEMs, and the
width of the membranes, respectively.
3. Results and Discussion
3.1 Chemical structure of AEMs
FTIR spectroscopy was used to verify the chemical composition
of eQPVA-x AEMs. Figure 3 displays the FTIR spectra of
eQPVA-x AEMs. The absorption peaks at 3378 and 1022 cm−1
appear to be caused by the –OH and C–O stretch in the PVA
polymer backbone. The peak in the bending vibration at 2940
cm−1 attributable to the existence of the C–H group. The
stretching vibration of the chemical bond C=O was indicated by
the intensity at the wavenumber of 1734 cm−1. The intensity at
1434 cm−1 and 1376 cm−1 occur on account of the presence of
the CH3 bend and CH2 bend, respectively. A wavenumber of
1240 cm−1 belongs to the C–O–C bond stretching vibration,
which indicates the establishment of covalent bonds between –
OH groups of QPVA and –CHO groups from GA.
Fig. 3 FTIR Spectrum of eQPVA-5.0
Fig. 4 Chemical structure of crosslinked QPVA
The intensities at 1098 cm−1 and 841 cm−1 correspond to the C–
N stretch and N–H bend of ion-conducting cation groups in
QPVA. The chemical structure of crosslinked QPVA is
illustrated in Figure 4.
3.2 Morphology
Figure 5a shows the surface morphology of the eQPVA
nanofiber AEMs from the SEM analysis. It was seen that the
nanofibers formed well with no beads. The size distribution of
the nanofiber mat is presented in Figure 5b. The QPVA mats
fibers possess a size distribution of 69–179 nm and a mean fiber
diameter of 100.96 nm, identifying them as nanofibers (Patel et
al., 2018). Inter-fiber void space, visible as pores between fibers,
is observed in the membranes. This inter-fiber void space of the
membrane should be occupied with a matrix filler in order for it
to be utilized in fuel cells.
Fig. 5 a) SEM Image of QPVA nanofibers, b) QPVA nanofibers size
distribution, c) SEM Image of eQPVA-5 AEM
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This matrix filler can prevents fuel and oxidant gas transport
through the membrane (i.e., gas crossover). The permeability of
fuel through AEMs should be prevented for fuel cells. Since this
crossover process may lead to voltage loss on account of the
mixed potential caused by the penetrated fuel oxidation.
Additionally, fuel crossover could cause peroxide and excess
heat generation, which can degrade the fuel cell (Francia et al.,
2011; T. Huang et al., 2022; Inaba et al., 2006). Figure 5c shows
the eQPVA-5.0 AEMs. Since this membrane is derived from
matrix addition to the eQPVC nanofibers, we can see that the
inter-fiber voids are filled with the matrix while maintaining the
nanofiber structure.
3.3 Ion Exchange Capacity (IEC)
IEC can be described as the capability of the AEMs functional
groups to carry out ions displacement, which is integrated and
loosely attached to its polymer backbone chain structure by
oppositely charged ions in the adjacent solution (Elumalai et al.,
2018). IEC demonstrates the quantity of functional groups or
active sites in an anion exchange membrane that is accountable
for ion exchange or facilitates the transfer of hydroxide (Kumar
et al., 2018). IEC can be expressed as milliequivalent or
millimoles of anionic-exchange groups per gram of the dry
membrane (meq g−1 or mmol g−1).
Figure 6 depicts the ion exchange capacity (IEC) of eQPVA-
x AEMs in hydroxide form of AEMs at 30°C. The IEC of eQPVA-
2.5 AEMs is 0.46 mmol g−1. The ion exchange capacity increases
by around 78% after enhancing the concentration of the QPVA
matrix to 5 wt.% (eQPVA-5.0), which is the highest IEC value.
When the concentration of the QPVA matrix is enhanced to 7.5
and 10 wt.%, the IEC decreases to 0.79 and 0.41 mmol g−1. The
decrease of IEC at higher concentrations of the QPVA matrix is
possibly owing to the QPVA matrix high viscosity, which causes
an impediment for the matrix filler solution to infiltrate the inter-
fiber space of the nanofiber mats. Consequently, the number of
ion-conducting cations in the electrospun QPVA AEMs
decreases, followed by the decline of IEC.
3.4 Swelling Properties
The existence of water in the anion exchange
membranes is significant in the process of conducting
hydroxide ions. The ion movement process in AEMs is
highly reliant on the membrane's hydration level (λ, i.e.,
the water molecules number per OH–), the dispersion and
distribution of water, and the solvation of OH− ions
(Zelovich et al., 2019). Water clusters are able to act as
anion transport channels within the AEMs, improving
hydroxide conductivity (Zhang et al., 2013).
.
Fig. 6 Ion Exchange capacity of eQPVA-x AEMs.
Fig. 7 Sweling properties of eQPVA-x AEMs.
At low water content or low hydration level and in alkaline
conditions, OH− ions can react with side cation charge groups,
which lessen the IEC of AEMs since only free ions play a part in
the conductivity. Furthermore, the degradation of the cation
charge groups will reduce the performance and lifetime of the
AEMs (Tomasino et al., 2022). In addition to the lack of
hydration, excessive water content is also avoided in AEMs.
This excessive water content can induce severe swelling, which
can cause instability in the membrane dimensions causing
mechanical degradation. Moreover, the excessive water content
may dissolve some of the charged cations bound in the polymer
backbone, lowering the IEC and causing the anionic
conductivity to decrease (Vandiver et al., 2014; Zheng et al.,
2018).
The water uptake (WU) and swelling degree (SD) of eQPVA-
x AEMs are depicted in Figure 7. The AEM with the lowest
QPVA matrix concentration (eQPVA-2.5) has a water uptake of
17.6 wt.%. By incorporating QPVA 5 wt.% (eQPVA-5.0), the WU
increases by 45% to 25.5 wt. %. However, by further increasing
the concentration of the matrix to 7.5 (eQPVA-7.5) and 10.0
wt.% (eQPVA-10.0), the WU decrease to 20.3 and 16.9 wt.%.
The results of the WU are in accordance with the IEC values.
Change in water uptake is significantly connected to the amount
of cation groups attached to the AEMs, which in the case of
these eQPVA-x membranes, are quaternary ammonium groups
from QPVA (Samsudin et al., 2021). The swelling degree
measurement demonstrates a similar tendency to water uptake.
The higher the water uptake indicates the higher the water
content in the membrane, which leads to swelling formation and
results in changes in the dimensions of the membrane.
3.5 Hydroxide Conductivity
Hydroxide conductivity is the most crucial characteristic of
AEMs, owing to the principal role of AEMs as OH− ions
conductors. The conductivity of AEMs is very reliant on the WU
and IEC of the AEMs. The high hydrophilicity of the anion
exchange membranes is resulted from the high density of cation
charge groups within the AEMs, which provide sufficient
anionic conductivity (Ayaz et al., 2022). Figure 8 exhibits the
hydroxide conductivity of eQPVA-x AEMs. The eQPVA-x
AEMs demonstrate OH− conductivities in the range of 0.71–2.26
mS cm−1 at 30 °C. Generally, the AEMs with the highest IEC and
WU also possess the highest hydroxide conductivity, which can
also be observed in this work. The eQPVA-5.0 exhibits the
highest value of WU and IEC, which also demonstrates the
highest OH− conductivity of 2.26 mS cm−1. The Grotthuss
mechanism describes how the hydroxide ions migrate along the
water molecules chain via the formation and breaking of
hydrogen bonds (Li et al., 2020). Accordingly, as WU increases,
water content rises as well, improving the conductivity of
hydroxide ions.
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ISSN: 2252-4940/© 2023. The Author(s). Published by CBIORE
Fig. 8 Hydroxide conductivity of eQPVA-x AEMs.
High hydroxide conductivity has a favorable impact on
power density and is accountable for reduced power/ohmic
losses (Cermenek et al., 2018). The higher the ionic conductivity,
the more hydroxide ions are transported through the membrane
so that more hydroxide ions react with the fuel to produce more
electrons. The increase in electrons leads to an increase in the
current density, which follows equation 5 (Kang & Cannon,
2015).
𝐼𝐼 = 𝜎𝜎𝜎𝜎 (5)
Where I is current density, σ is conductivity and E is electric
field.
Since power density (P) is the multiplication of current
density (I) and voltage (V) according to equation 6, an increase
in current density will give a proportional increase in power
density (O’Hayre, 2017).
𝑃𝑃 = 𝑉𝑉𝐼𝐼 (6)
This is consistent with a study conducted by Samsudin et al.
(2021, 2022) that membranes of different conductivity will
produce different power densities in the same fuel cell and
operating conditions.
4. Conclusion
Anion exchange membranes (AEMs) composed of GohsenxTM
K-434 quaternary ammonium poly(vinyl alcohol) (PVA) as
material for electrospun fiber mats and inter-fiber void filler
have been prepared by the electrospinning method. FTIR
spectra recognized the primary functional groups of
membranes. SEM images display the electrospun nanofibers
structures of eQPVA with a mean size of 100.96 nm and the
surface morphology of eQPVA-5.0 dense AEMs. By
incorporating the QPVA matrix of 5 wt.% concentration, the
eQPVA-5.0 membrane achieved the highest IEC, water uptake,
swelling degree, and hydroxide conductivity of 0.82 mmol g−1,
25.5%, 19.9%, and 2.26 ms cm−1, respectively.
Acknowledgments
The authors thank the Austrian Science Fund (FWF) for
providing financial support for the study under project number
I 3871-N37. Additionally, the authors acknowledge Kemdikbud
(Indonesia) and OeAD (Austria) for the IASP scholarship.
Author Contributions: A.M.S.: Conceptualization, methodology,
formal analysis, writing—original draft, writing—review and editing,
V.H.; writing—review and editing, supervision, resources, project
administration. All authors have read and agreed to the published
version of the manuscript.
Funding: This research was funded by Austrian Science Fund (FWF)
under project number I 3871-N37.
Conflicts of Interest: The authors declare no conflict of interest.
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QPVA-Based Electrospun Anion Exchange Membrane for Fuel Cells
Asep Muhamad Samsudin a,b0F and Viktor Hackera
1. Introduction