sustainability

Article
Activated Carbon Electrodes for Bioenergy Production in
Microbial Fuel Cells Using Synthetic Wastewater as Substrate
Rickelmi Agüero-Quiñones 1 , Zairi Ávila-Sánchez 1 , Segundo Rojas-Flores 2, * , Luis Cabanillas-Chirinos 3 ,
Magaly De La Cruz-Noriega 3 , Renny Nazario-Naveda 4 and Walter Rojas-Villacorta 5

1 Escuela de Ingeniería Ambiental, Facultad de Ingeniería, Universidad Cesar Vallejo, Trujillo 13007, Peru;
[email protected] (R.A.-Q.); [email protected] (Z.Á.-S.)
2 Escuela de Ingeniería Mecánica Eléctrica, Universidad Señor de Sipán, Chiclayo 14000, Peru
3 Instituto de Investigación en Ciencia y Tecnología, Universidad César Vallejo, Trujillo 13001, Peru;
[email protected] (L.C.-C.); [email protected] (M.D.L.C.-N.)
4 Departamento de Ciencias, Universidad Privada del Norte, Trujillo 13007, Peru; [email protected]
5 Programa de Investigación Formativa e Integridad Científica, Universidad César Vallejo, Trujillo 13001, Peru;
[email protected]
* Correspondence: [email protected]

Abstract: The growing global energy demand drives the need to develop new clean energy tech-
nologies. In this context, microbial fuel cells (MFC) are one of the emerging technologies with great
potential for eco-friendly energy generation; however, the correct choice of electrode material is a
significant limitation in the optimal configuration of MFCs. Therefore, this research evaluated the
efficiency of activated carbon (AC) anode electrodes for bioenergy production in MFC using synthetic
wastewater as a substrate. Peak values of voltage (1120 ± 0.050 mV), current (4.64 ± 0.040 mA),
power density (208.14 ± 17.15 mW/cm2 ), and current density (5.03 A/cm2 ) were generated, and
the Rint obtained was 214.52 ± 5.22 Ω. The substrate was operated at pH values from 5.31 to 7.66,
maximum ORP values (858 mV) were reached, and turbidity was reduced to 25.11 NTU. The SEM-
Citation: Agüero-Quiñones, R.; EDS (scanning electron microscopy–energy-dispersive X-ray spectroscopy) analyses allowed us to
Ávila-Sánchez, Z.; Rojas-Flores, S.; observe the morphology and composition of the AC electrodes, revealing a predominance of O, C, Si,
Cabanillas-Chirinos, L.; De La
Al, Fe, K, and Ca. It is concluded that the AC electrodes have the potential to produce bioenergy at a
Cruz-Noriega, M.; Nazario-Naveda,
laboratory by means of MFC.
R.; Rojas-Villacorta, W. Activated
Carbon Electrodes for Bioenergy
Keywords: activated carbon; microbial fuel cells; wastewater; bioenergy
Production in Microbial Fuel Cells
Using Synthetic Wastewater as
Substrate. Sustainability 2023, 15,
13767. https://doi.org/10.3390/
su151813767
1. Introduction
In the growing global demand for energy, the growing dependence on fossil fuels
Academic Editor: Giovanni Esposito
poses a major challenge for modern and developed society [1]. Addressing these problems
Received: 14 August 2023 requires the development of clean technologies that use renewable energy sources that
Revised: 7 September 2023 promote sustainability [2–5]. Recently emerging energy technologies are growing remark-
Accepted: 11 September 2023 ably [6,7]. An emerging technology is microbial fuel cells (MFC) [8]. These MFCs are
Published: 15 September 2023 innovative bioelectrochemical systems with various applications ranging from bioenergy
production to wastewater treatment [9]. The process involves converting chemical energy
within biodegradable organic compounds into renewable bioenergy through exoelectro-
genic microorganisms [10,11]. Microorganisms are in charge of degrading organic matter
Copyright: © 2023 by the authors.
and releasing electrons, which are transferred through an external circuit, reach the cathode,
Licensee MDPI, Basel, Switzerland.
and produce ecological energy [12,13].
This article is an open access article
MFCs have been designed with a dual chamber (dcMFC) and a single chamber
distributed under the terms and
conditions of the Creative Commons
(scMFC) [14]. dcMFCs have certain disadvantages that imply an unadaptable and in-
Attribution (CC BY) license (https://
flexible application since they use an expensive membrane as separator, in addition to the
creativecommons.org/licenses/by/ fact that, in many cases, the ion transfer rate is low [15]. On the other hand, the scMFC is a
4.0/). more prospective option, it is developed without spacers, and at the same time, that they are

Sustainability 2023, 15, 13767. https://doi.org/10.3390/su151813767 https://www.mdpi.com/journal/sustainability

Sustainability 2023, 15, 13767 2 of 14

economical and ecofriendly. Its configuration is relatively simple, consisting of a chamber

where the electrodes (anode and cathode) are located [16]. However, the drawbacks that
they present are the correct choice of materials for the electrodes that allow the performance
of the MFCs to be improved [17,18].
This research focuses on the evaluation of a carbon-based electrode (anode) to improve
the efficiency of electricity production in scMFCs. However, these scMFCs also use a zinc-
based cathode. The cathode is fundamental in MFCs because an electrochemical reduction
reaction occurs in it, where the oxygen taken from the air is reduced with the electrons and
protons that are released from the metabolism of the substrate [19]. On the other hand, the
material of the cathode is also important; zinc is a lower cost material that could replace
platinum in oxidation-reduction reactions, and it could improve the efficiency of bioenergy
production in MFCs, as has been observed in some studies [20,21]. The anode electrode is
an essential component in the configuration of MFCs, since it is the support for the bacterial
biofilm and the conductor of the released electrons [22,23]. The main characteristics that
the anode material must have are biocompatibility, high electrical conductivity, corrosion
resistance, chemical stability, high surface area, non-toxicity, good toughness, low cost, and
being hydrophilic, and they should not decompose in the substrate [24,25]. Taking these
characteristics into account, metal-based and carbon-based materials have been used [26].
The most used metallic materials are platinum, stainless steel, copper, aluminum, cobalt,
titanium, nickel, gold, and silver [12]. These materials are used mainly because they
are highly conductive, which allows the energy efficiency of MFCs to be improved [27].
However, they have significant limitations that prevent their use on a large scale. For
example, titanium, platinum, gold, and silver are costly; cobalt and titanium do not have
good biocompatibility; copper, aluminum, and stainless steel are susceptible to corrosion;
and platinum tends to be toxic when wastewater is used as a substrate and can affect
microorganisms present [19,28,29].
On the other hand, interest in carbon-based electrodes has increased among researchers
due to their chemical, thermal, and electrochemical stability, significantly improving elec-
tricity production and removing contaminants from wastewater in MFCs [28]. These
materials include graphite plate, carbon felt, carbon cloth, reticulated glassy carbon, carbon
rod, carbon paper, carbon-fiber brush, carbon brush, graphite-fiber brush, graphite felt,
granular graphite, graphene [29,30], and granular activated carbon (GAC) [31]. The latter
has not seen many applications as a material for making MFC anode electrodes, but it
has many properties that make it a good candidate [32]. It has a high surface area and
excellent biocompatibility, which facilitates bacterial adhesion and allows the uniform
formation of biofilms; it has high conductivity, chemical stability, corrosion resistance, and
low cost [33–35].
There are studies with results that support the use of activated carbon presented by
Karra et al. [36], which used polyaniline-functionalized activated carbon anodes coated
on stainless steel mesh (SSM—PANi/FAC) to produce a voltage of 0.72 ± 0.010 V and
a power density of 322 mW/m2 using a dcMFC. Likewise, Rojas et al. [37] fabricated
activated carbon cloth anode electrodes to generate a maximum voltage of 0.66 V and
a maximum power density of 272.14 mW/m2 using a double-chamber MFC fed with
municipal wastewater from Yilan County in Taiwan. Using organic sediments from Mirror
Lake at the University of Connecticut as a substrate, Silva et al. [38] achieved maximum
values of 0.56 W/m2 and 0.25 A/m2 using granular activated carbon anodes.
Regarding the substrate, synthetic wastewater obtained from different sources has been
studied in MFCs to generate bioelectricity because they are rich in organic substrates with
high glucose, soluble starch, and sucrose contents, which are metabolized by proteobacteria
that exist in these wastewaters; they have also been reported as electrogenic [39,40].
The main objective of this research was to evaluate the efficiency of activated carbon
anode electrodes for bioenergy production in laboratory-scale single-chamber microbial
fuel cells using a synthetic wastewater sample as substrate. For this, the values of voltage
(mV), electric current (mA), current density (mA/cm2 ), power density (mW/cm2 ), and the
Sustainability 2023, 15, x FOR PEER REVIEW 3 of 14

Sustainability 2023, 15, 13767 3 of 14

fuel cells using a synthetic wastewater sample as substrate. For this, the values of voltage
(mV), electric current (mA), current density (mA/cm2), power density (mW/cm2), and the
internal resistance of the MFCs were monitored, and the oxidation and reduction potential
internal resistance of the MFCs were monitored, and the oxidation and reduction potential
(ORP) (mV), pH and turbidity (NTU) of the substrate for 30 days. This research will con-
(ORP) (mV), pH and turbidity (NTU) of the substrate for 30 days. This research will
tribute to developing MFCs to generate sustainable bioelectricity through economic, eco-
contribute to developing MFCs to generate sustainable bioelectricity through economic,
friendly, and eco-efficient electrodes.
eco-friendly, and eco-efficient electrodes.
2.
2. Materials
Materials and and Methods
Methods
2.1. Manufacture of Granular Activated Carbon (GAC) Electrodes
Seven activated
activatedcarbon
carbonelectrodes
electrodesweighing
weighing25.35
25.35± 2.70 g, 5.2
± 2.70 ± 1 cm
g, 5.2 ± 1incmdiameter, and
in diameter,
0.7
and±0.7
0.1 ±cm0.1thick, connected
cm thick, to a 1 to
connected mm a 1thick
mmcopper wire, were
thick copper wire,manufactured,
were manufactured,for whichfor
200 g GAC
which 200 gwereGACcrushed (NHC-500)
were crushed using ausing
(NHC-500) blender (Oster(Oster
a blender BPST02-BOO
BPST02-BOO600 W,600 Boca
W,
Raton, FL, USA)
Boca Raton, to a fine
FL, USA) to powder, to which
a fine powder, was added
to which a mixture
was added of 60 g of
a mixture of 60
sucrose and 80
g of sucrose
mL
and of
80water
mL of(61° water (61◦The
Brix). solution
Brix). was mixed
The solution until a until
was mixed homogeneous and consistent
a homogeneous paste
and consistent
was obtained.
paste Subsequently,
was obtained. a circular
Subsequently, metallicmetallic
a circular mold ofmold
5.7 cm in diameter
of 5.7 and 1.2and
cm in diameter cm
thick
1.2 cmwas covered
thick with aluminum
was covered foil, andfoil,
with aluminum a circular
and a metallic
circular base of 4.7
metallic cm of
base in 4.7
diameter
cm in
diameterwith
covered covered with commercial
commercial vegetablevegetable oil was
oil was placed (toplaced (to the
facilitate facilitate the extraction
extraction of
of the elec-
the electrode).
trode). Then, aThen,
layera of
layer
15 of 15 the
g of g of mixture
the mixture
waswas added,
added, followed
followed bybya a4.5
4.5cm
cm diameter
diameter
aluminum mesh diagonally intertwined with a copper wire, and finally by another layer
of 15 gg of
of the
themixture,
mixture,to tobebecovered
coveredwith
withanother
anothermetal
metal base.
base. TheThe mold
mold was was placed
placed in
in an
electric stove (Whiteline 220 V/50 Hz/1000 W, Torremolinos, Spain) for 15 min at a tem-a
an electric stove (Whiteline 220 V/50 Hz/1000 W, Torremolinos, Spain) for 15 min at
temperature of °C; ◦ C; then, it was carefully removed and allowed to cool to remove the
300 then,
perature of 300 it was carefully removed and allowed to cool to remove the elec-
electrode
trode (Figure
(Figure 1). 1).

Figure 1. (a) Prototype and (b) structure of the electrodes made with activated carbon.

2.2. Electrode
2.2. Electrode Waterproofing
Waterproofing
For the
For the waterproofing
waterproofing of of the
the electrodes,
electrodes, aa solution
solution of
of 70
70 mL
mL of
of ethanol
ethanol and
and 50
50 gg of
of
pine
pine resin was used, which was previously boiled for 15 min with 100 mL of water to
resin was used, which was previously boiled for 15 min with 100 mL of water to
eliminate the
eliminate volatile substances.
the volatile substances. Then,
Then, the
the electrodes
electrodes were
were immersed
immersed several
several times
times in
in the
the
solution until
solution until they
they were
were completely
completely covered
covered and
and were
were allowed
allowed toto rest
rest at
at room
room temperature
temperature
◦
(27 ±
(27 1.5°C)
± 1.5 C)for
for24
24h.h.

2.3. Construction of MFCs

2.3. Construction of MFCs
Two single-chamber microbial fuel cells (MFC-SC) were constructed from 680 mL
Two single-chamber microbial fuel cells (MFC-SC) were constructed from 680 mL
polypropylene vessels. For the anode, electrodes made of activated carbon were used,
polypropylene vessels. For the anode, electrodes made of activated carbon were used,
which were placed at one end inside the chamber, while for the cathode, a zinc (Zn) plate
which
was were
used placed
that at one end
was attached inside
to the wallthe
of chamber, while
the chamber for the cathode,
at another end of thea zinc (Zn)
cell so thatplate
one
was used that was attached to the wall of the chamber at another end of the
face was in contact with the oxygen. Both electrodes had a surface area of 21.60 cm andcell so2 that
one face
were was in contact
connected to a 1 mmwith the copper
thick oxygen.(Cu)
Bothwire
electrodes had a surface
to the outside, where area
they of 21.60
were cm2
joined
with a 100 Ω resistance to form a closed circuit, as shown in Figure 2.
Sustainability 2023, 15, x FOR PEER REVIEW 4 of 14

Sustainability 2023, 15, 13767 and were connected to a 1 mm thick copper (Cu) wire to the outside, where they were
4 of 14
joined with a 100 Ω resistance to form a closed circuit, as shown in Figure 2.

(a) (b)
Figure 2. (a)2.Prototype
Figure and (b)
(a) Prototype experimental
and setup ofsetup
(b) experimental MFC-SC with activated
of MFC-SC carbon and
with activated zinc elec-
carbon and zinc
trodes.
electrodes.

2.4. 2.4. Substrate

Substrate Preparation
Preparation
The The substrate
substrate waswas prepared
prepared withwith residual
residual waterwater
fromfrom dishwashing
dishwashing and and
foodfood remains
remains
from the Cesar Vallejo University at Trujillo, Peru cafeteria. These residues
from the Cesar Vallejo University at Trujillo, Peru cafeteria. These residues passed through passed through
a processor
a processor (Oster
(Oster BPST02-BOO
BPST02-BOO 600 600 W, USA),
W, USA), obtaining
obtaining 1 Lsynthetic
1 L of of synthetic wastewater
wastewater stored
stored
in sterilized
in sterilized hermetic
hermetic containers
containers forfor use.
use. The The substratehad
substrate hadananinitial
initialpHpHof
of 6.55,
6.55, an
an electrical
elec-
conductivity
trical conductivity ofof
2450.48 ± ±0.1
2450.48 μS/cm,an
0.1µS/cm, anORP 134.5±±11mV,
ORPofof134.5 mV,andanda aturbidity
turbidityofof7575
NTU.
An amount of 500 mL of the substrate was supplied to
NTU. An amount of 500 mL of the substrate was supplied to each well. each well.

2.5. Characterization of MFCs

2.5. Characterization of MFCs
The electrochemical parameters of voltage (mV) and current (mA) were measured
The electrochemical parameters of voltage (mV) and current (mA) were measured
with a calibrated digital multimeter (Truper MUT—830). For the measurement of current
with a calibrated digital multimeter (Truper MUT—830). For the measurement of current
density (DC) and power density (PD) the procedure carried out by Segundo et al. (2022)
density (DC) and power density (PD) the procedure carried out by Segundo et al. (2022)
using external resistances (Rext) with values of 1.92 (±0.08), 10 (±1.81), 50 (±1.2), 100
using external resistances (Rext) with values of 1.92 (±0.08), 10 (±1.81), 50 (±1.2), 100 (±4.3),
(±4.3), 200 (±9.8), 300 (±8), 500 (±15), 750 (±18), 800 (±10), and 1000 (±40) Ω [39]. An
200 (±9.8), 300 (±8), 500 (±15), 750 (±18), 800 (±10), and 1000 (±40) Ω [39]. An energy sensor
energy sensor (Vernier VES-TBA ±30 V and ±1000 mA) was used to measure the internal
(Vernier VES-TBA ±30 V and ±1000 mA) was used to measure the internal resistance (Rint)
resistance (Rint) of the MFCs. The pH values (Digital Meter EZ-9909, Thincol, Guangzhou,
of the MFCs. The pH values (Digital Meter EZ-9909, Thincol, Guangzhou, China), ORP
China), ORP (Portable Meter PT-380, BOECO, Hamburg, Germany), and turbidity (Digital
(Portable Meter PT-380,
Turbidimeter TU-2016,BOECO,
Lutron, Hamburg, Germany),
Taipei, Taiwan) and
of the turbidity
substrate (Digital
were also Turbidime-
monitored. All
ter TU-2016,
measurements were made daily for 30 days at room temperature (21 ± 1.5 ◦measure-
Lutron, Taipei, Taiwan) of the substrate were also monitored. All C). Likewise,
ments were
three made daily for
measurements 30 days
of each at roomwere
parameter temperature
made in (21 ± 1.5
order °C). Likewise,
to report three
the means of the
measurements of each parameter were made in order to report the means of
values. In addition, SEM-EDS analyses were carried out to know the morphology and the values.
In addition,
elemental SEM-EDS analyses
composition of thewere carried
activated out toelectrodes.
carbon know the morphology and elemental
composition of the activated carbon electrodes.
2.6. Electrodes Resistance Test to Synthetic Residual Water
2.6. Electrodes Resistance of
The resistance Test
thetoactivated
Synthetic carbon-based
Residual Waterelectrodes towards the liquid substrate
Theevaluated
was resistancebased
of theon
activated carbon-based
percentage electrodes
weight loss. To see thetowards the liquid
effectiveness of thesubstrate
use of these
waselectrodes,
evaluated based on percentage
a resistance test wasweight loss.
carried outTo
insee the effectiveness
distilled of the use ofelectrodes
water. Waterproofed these
electrodes, a resistance
with pine test waswaterproofing
resin and without carried out in were
distilled water. Waterproofed
manufactured. These wereelectrodes
immersed in
with500
pine
mLresin and without
of distilled waterwaterproofing were
for 15 days, and manufactured.
then Thesefor
dried in an oven were immersed
15 min in
to eliminate
500 moisture
mL of distilled water
content. for 15they
Finally, days,were
and weighed,
then driedandin an
theoven
finalfor 15 min
weight to eliminatewere
percentages
obtained,
moisture obtaining
content. that
Finally, theythewere
electrodes waterproofed
weighed, with
and the final pine resin
weight had lesswere
percentages weight
ob- loss
tained, obtaining that the electrodes waterproofed with pine resin had less weight loss the
compared to those that were not waterproofed. The loss of activated carbon from
electrodes within the substrate with synthetic wastewater was evaluated by performing the
previously described procedure. For this, weight was taken initially and then at the end of
Sustainability 2023, 15, x FOR PEER REVIEW 5 of 14

compared to those that were not waterproofed. The loss of activated carbon from the elec-
Sustainability 2023, 15, 13767 trodes within the substrate with synthetic wastewater was evaluated by performing 5 ofthe
14
previously described procedure. For this, weight was taken initially and then at the end
of the measurement period (30 days). With these values, the percentages of final weight
lossmeasurement
the were obtained.period (30 days). With these values, the percentages of final weight loss
were Through
obtained.the evaluation, it was found that the electrodes covered with pine resin ex-
perienced
Througha significantly lower
the evaluation, decrease
it was in their
found that weight compared
the electrodes covered withto pine
the non-water-
resin expe-
proofed electrode. Therefore, the effectiveness of pine resin as a waterproofing
rienced a significantly lower decrease in their weight compared to the non-waterproofed agent is
validated, thus preventing the detachment of the activated carbon electrodes when
electrode. Therefore, the effectiveness of pine resin as a waterproofing agent is validated,in con-
tact with
thus water, in
preventing thethis way it canofbethe
detachment tested with the
activated substrates.
carbon electrodes when in contact with
water, in this way it can be tested with the substrates.
3. Results and Discussion
3. Results
3.1. and Discussion
Measurement of Electrochemical Parameters of MFCs
3.1. Measurement of
Figure 3a shows Electrochemical
the voltage Parameters of MFCsby the MFCs during the 30 days of
values generated
monitoring. The highest values were recorded duringbythe
Figure 3a shows the voltage values generated the MFCs
first daysduring the 30 with
of operation, daysthe
of
monitoring.
highest voltageThepeak
highest valuesonwere
observed recorded
the first during
day (1120 mV).theInfirst
the days of operation,
following days, thewith
pro-
the highest
duction voltageuntil
decreased peakdayobserved on the
8 (916 mV), first aday
where (1120variable
slightly mV). Ingeneration
the following
was days, the
observed
production
until day 16decreased
(908 mV). until
In theday 8 (916 days,
following mV), there
wherewas a slightly variable
a progressive generation
decrease until was
day
observed
30, when until
789 mVdaywas16 (908 mV). In The
generated. the following
high voltage days, there wasduring
production a progressive
the firstdecrease
days is
until day 30, when 789 mV was generated. The high voltage production
because the bacteria began to proliferate in the MFCs due to the high presence during theoffirst days
organic
is because the bacteria began to proliferate in the MFCs due to the high
substrates in the wastewater that allowed the development of microbial electrogenesis presence of organic
substrates
through redoxin the wastewater
reactions thatAtallowed
[40,41]. the same thetime,
development
the decreaseof microbial
in voltageelectrogenesis
is due to the
through redox reactions [40,41]. At the same time, the decrease
reduction in organic matter in the substrate, consumed by microorganisms in voltage through
is due totheir
the
reduction
metabolic in organic
process to matter
convertinchemical
the substrate,
energyconsumed by microorganisms
into electrical energy [42]. through their
metabolic process to convert chemical energy into electrical energy [42].

1150 5.0

1100 4.5

1050 4.0

1000 3.5
Voltage (mV)

Current (mA)

950 3.0

900 2.5

850 2.0

800 1.5

750 1.0
0 5 10 15 20 25 30 0 5 10 15 20 25 30

Time (days) Time (days)

(a) (b)
Figure 3.
Figure 3. Monitoring
Monitoring of
of values
values of
of (a)
(a) voltage
voltage and
and (b)
(b) electrical
electrical current
current of
of the
the MFCs.
MFCs.

The electrodes used play

The play aacrucial
crucialrole
rolesince,
since,being
beingcarbon-based,
carbon-based,they
theyfacilitate better
facilitate bet-
biocompatibility with the microbes present [43], achieving
ter biocompatibility with the microbes present [43], achieving better better voltage production
production
throughout the
throughout the operation
operation period
period compared
compared to to other
other investigations
investigations where
where electrodes
electrodes were
were
used metals,
used metals, and
and their
their stress
stress production
production was
was markedly reduced in the final days of their their
experiment. The
experiment. Thevoltage
voltagevalues
values obtained
obtained areare higher
higher thanthan
thosethose reported
reported by et
by Bose Bose et al.
al. (2023)
(2023) they
where where they
used used wastewater
wastewater from thefrom the sugarcane
sugarcane industryindustry
in MFC in MFC
with with biomass-
biomass-derived
derived activated
activated carbon ascarbon as theand
the cathode cathode and pretreated
pretreated carbon wire-based
carbon wire-based brush as thebrush
anode asand
the
managed to produce maximum voltage peaks of 870 ± 20 mV [44], and Agüero-Quiñones
et al. (2022), who used municipal wastewater in MFC-SC with aluminum as the cathode and
graphite as the anode, generating maximum values of 220 mV. Compared to our research, it
may be due to the fact that the aluminum electrodes used do not have as good conductive
Sustainability 2023, 15, 13767 6 of 14

properties as the zinc or copper used as connectors [45]. Figure 3b shows the values of
electric current the cells produce during monitoring. High current values were generated
during the first days of operation (4.64 mA on the first day), while in the following days,
the production decreased until day 12 (3.33 mA), where a relatively constant production
was presented until day 24 (3.33 mA). In the following days, the values experienced a
gradual decrease until they produced 1.93 mA on day 30. The peak current values shown
in the first days are attributed to the good formation of the electrogenic biofilm [46], which
depends largely on the measurement of the carbon sources present in the substrates [47],
which act as an energy supply in the biological process of microorganisms to produce
electric current [48]. As the organic compounds decrease, the production of electrons is
reduced, thus generating a lower electrical current in the last few days [49]. The values
shown in this research are higher than those reported by other authors; for example, De La
Cruz-Noriega et al. (2023) managed to generate maximum current values of 0.71 ± 0.02 mA
using MFC-DC from wastewater in the anodic chamber and electrogenic bacteria in the
cathodic chamber [50].
Figure 4a shows the value of the internal resistance of the MFC, showing a peak value
of 214.52 ± 5.22 Ω, calculated with the maximum value of voltage generation and electrical
current. The high value of Rint obtained can be attributed to the characteristics of the
substrate, which contains solids in suspension that hinder electrical conduction, increasing
internal resistance [51,52]. Other authors, such as Du and Shao (2022), reported a peak
internal resistance value of 163.2 Ω in MFC-DC with carbon felt electrodes using solid potato
waste and activated sludge [53]. Figure 4b shows the power density (PD) values as a current
density (DC) function, observing a maximum power density of 208.14 ± 17 mW/cm2 and
a maximum current density of 5.03 A/cm2 . It can be observed in the graphs that the
power density reaches a maximum value and subsequently presents a decrease due to
the operability of the operating time and also due to the reduction in the organic matter
available in the medium [54]. In addition, the values of DP and DC depend on the rate
of degradation of the organic energy of the substrates by the microbial community, on
the external operating conditions [55], as well as on the internal resistance of the MFCs,
due to the fact that a higher Rint hinders the flow of electrons through the system [56].
The values obtained in this research are higher than those shown in other studies, such as
that of Lee et al. (2018), who obtained a power density and maximum current density of
0.0251 mW/m2 and 285.71 mA/m2 , respectively, in MFC-SC with hybrid and conventional
carbon felt bioanodes using municipal wastewater [57], while Rossi et al. (2022) achieved
maximum power density values of 0.135 W/m2 and 0.278 A/m2 current density in 850 L
air cathode MFC of domestic wastewater with carbon-fiber brush anodes and stainless steel
carbon-fiber cathodes [58].

3.2. Monitoring of Physicochemical Parameters of the Substrate

Figure 5a shows the recorded values of the turbidity of the residual water during the
monitoring period. It is observed that the values presented a progressive decrease over
the days, beginning with 75.50 NTU on day one and reaching 25.11 NTU on day 30. The
reduction in turbidity is due to the decrease in organic and suspended material matter
content due to microbial metabolic activity over days [59]. In addition, the anode material
(activated carbon) has adsorption properties that trap suspended wastewater particles
on the electrode surface [60]. Tee et al. (2017) removed 98.00 ± 0.7% of the turbidity of
wastewater generated in a palm oil plant in MFC-SC with graphite-fiber brush electrodes
and granular activated carbon [61].
 Sustainability 2023, 15, x FOR PEER REVIEW 7 of 14
Sustainability 2023, 15, 13767 7 of 14

Figure 4. Characterization of (a) internal resistance and (b) power density concerning the current
density of the MFCs.

3.2. Monitoring of Physicochemical Parameters of the Substrate

Figure 5a shows the recorded values of the turbidity of the residual water during the
monitoring period. It is observed that the values presented a progressive decrease over
the days, beginning with 75.50 NTU on day one and reaching 25.11 NTU on day 30. The
reduction in turbidity is due to the decrease in organic and suspended material matter
content due to microbial metabolic activity over days [59]. In addition, the anode material
(activated carbon) has adsorption properties that trap suspended wastewater particles on
the electrode surface [60]. Tee et al. (2017) removed 98.00 ± 0.7% of the turbidity of
wastewater generated in a palm oil plant in MFC-SC with graphite-fiber brush electrodes
Figure
Figure 4.4. Characterization
Characterization of
of (a)
(a) internal
internal resistance
resistance and
and (b)
(b)power
powerdensity
density concerning
concerning the
the current
current
and granular activated carbon [61].
densityof
density ofthe
theMFCs.
MFCs.

90 3.2. Monitoring of Physicochemical Parameters

1000 of the Substrate
80 Figure 5a shows the recorded values
900 of the turbidity of the residual water during the
monitoring period. It is observed that
800 the values presented a progressive decrease over
70
the days, beginning with 75.50 NTU700 on day one and reaching 25.11 NTU on day 30. The
60
reduction in turbidity is due to the 600
decrease in organic and suspended material matter
Turbidity (NTU)

content due to microbial metabolic activity over days [59]. In addition, the anode material
ORP (mV)

50
500
40 (activated carbon) has adsorption properties that trap suspended wastewater particles on
400
the electrode surface [60]. Tee et al. (2017) removed 98.00 ± 0.7% of the turbidity of
30
wastewater generated in a palm oil plant in MFC-SC with graphite-fiber brush electrodes
300
20
and granular activated carbon [61]. 200
10
100

0 1000
Sustainability
900 2023, 15,
5 x FOR10
PEER REVIEW
15 20 25 30
0 8 of 14
0 5 10 15 20 25 30
Time (days) 900
80 Time (days)
800
70 (a) (b)
700
60 8.0
Turbidity (NTU)

600
ORP (mV)

50
7.5 500
40
400
30 7.0
300
20
200
6.5
pH

10
100

0 0
6.0
0 5 10 15 20 25 30
0 5 10 15 20 25 30
Time (days)
Time (days)
5.5
(a) (b)
5.0
0 5 10 15 20 25 30
Time (days)

(c)
Figure 5. Monitoring of (a) turbidity, (b) ORP, and (c) pH of the MFC substrate.
Figure 5. Monitoring of (a) turbidity, (b) ORP, and (c) pH of the MFC substrate.

On the other hand, the ORP values of the substrate are observed in Figure 5b, pre-
senting an increasing behavior from day 1 (134 mV) to day 7 (858 mV) and then slowly
decreased, presenting decreases and increases until day 13, where a value of 378 mV was
found. High ORP values indicate that there is a more oxidizing environment in the cell
[62,63], which makes it easier for some electroactive bacterial species to thrive in these
Sustainability 2023, 15, 13767 8 of 14

On the other hand, the ORP values of the substrate are observed in Figure 5b, pre-
senting an increasing behavior from day 1 (134 mV) to day 7 (858 mV) and then slowly
decreased, presenting decreases and increases until day 13, where a value of 378 mV
was found. High ORP values indicate that there is a more oxidizing environment in the
cell [62,63], which makes it easier for some electroactive bacterial species to thrive in these
conditions, resulting in increased production of electrons at the anode and favoring the
generation of energy in MFCs [64]. Zhao et al. (2023) reported a peak value of around
325 mV for wastewater ORP in the MFC of sediment coupled with Vallisneria natans [65].
The monitored data of the pH of the substrate are shown in Figure 5c, where it can be seen
that in the first days, the values decreased from 6.55 to slightly acid on day 8 (5.31), and
then in the following days, a significant increase was observed reaching values of 7.66 on
day 30, showing optimal pH values in this period (6–9) for the development of biofilms by
microorganisms [66]. During the oxidation process of the organic compounds in the anode
chamber of the MFC in the first days of operation, the microorganisms, in addition to gen-
erating electrons, also release protons (H+ ions) [67]. If the proton production rate is high
compared to its consumption or transfers to the cathode, there could be an accumulation
of protons at the anode, lowering the pH (5.31) [68]. At the same time, the increase in pH
(7.66) can be attributed to the greater use of protons during microbial and electrochemical
reactions at the anode instead of their release [69]. In other investigations, it has been
observed that the pH values exhibit different variations due to the unique composition
of each substrate; for example, Radeef and Ismail worked with car wash wastewater in
MFCs with graphite electrodes and observed increases in pH from 7.5 to 8.3 after 90 days
of operation [70].

3.3. SEM-EDS Analysis of Activated Carbon Electrodes

Figure 6 shows the micrographs obtained from the SEM analysis of the activated
carbon anode electrodes after the period of operation in the MFCs. Figure 6a shows the
electrode surface (5 mm), evidencing the presence of tiny pores scattered throughout the
area and presenting a relatively smooth texture that favored the adhesion of the bacterial
biofilm. Figure 6b shows a more detailed image of the pores distributed throughout the
surface and with solid activated carbon particles. Figure 6c shows the structure of the
electrode (5 mm), revealing the presence of the aluminum mesh with the copper wire
between the solid layers of activated carbon. Figure 6d shows the integration between
the aluminum mesh, the copper wire, and the layers of activated carbon (1 mm). In other
studies, SEM analyses were also carried out to know the morphology of the electrodes and
to observe the adhered biofilm during their experiments. Nishio, Nguyen, and Taguchi
(2023) used urethane filter electrodes in MFCs with soil and cow dung and obtained SEM
images showing a porous surface with a large amount of activated carbon after their
experiments [71]. Likewise, Li et al. (2023), using their SEM images of their graphite rod
electrodes in their MFCs supplied with anaerobic sludge from a wastewater treatment plant,
observed that the anodic biofilm attached to the electrode was composed of bacilli and
filamentous bacteria [72]. In addition, Li et al. (2017) used carbon cloth electrodes in MFCs
assisted with the effluent from the anode chamber in another previously operating cell
and revealed that the biofilm dissociated from the anode surface, indicating that long-term
operation with inversion voltage could damage the biofilm and ultimately cause the failure
of the MFC [73].
 electrodes in their MFCs supplied with anaerobic sludge from a wastewater treatment
plant, observed that the anodic biofilm attached to the electrode was composed of bacilli
and filamentous bacteria [72]. In addition, Li et al. (2017) used carbon cloth electrodes in
MFCs assisted with the effluent from the anode chamber in another previously operating
cell and revealed that the biofilm dissociated from the anode surface, indicating that long-
Sustainability 2023, 15, 13767 9 of 14
term operation with inversion voltage could damage the biofilm and ultimately cause the
failure of the MFC [73].

Figure 6. SEM
Figure SEMmicrographs
micrographsofofactivated carbon
activated electrodes
carbon (a) (a)
electrodes electrode surface
electrode morphology,
surface (b) acti-
morphology, (b)
activated carbon,
vated carbon, (c) electrode
(c) electrode structure,
structure, and and (d) aluminum
(d) aluminum meshmesh
withwith activated
activated carbon
carbon and carbon
and carbon wire
wire copper.
copper.

Figure
Figure 77 presents
presents the composition
composition spectra
spectra of of the elements
elements in the activated carboncarbon
electrodes obtained from
electrodes obtained fromthe theEDS
EDSanalysis.
analysis.AAmajority
majoritypresence
presenceofof elements
elements such
such as as oxy-
oxygen
(O), (O),
gen carbon (C),(C),
carbon silicon (Si),(Si),
silicon aluminum
aluminum (Al), iron
(Al), (Fe),
iron potassium
(Fe), potassium (K), and
(K), andcalcium
calcium(Ca) is
(Ca)
observed.
is observed.TheThehigh
highpresence
presenceofofoxygen
oxygenreported
reportedin inthe
the spectra
spectra is due to several
several reasons,
reasons,
ranging from
ranging from the
the composition
composition of of the
the electrode
electrode material,
material, which,
which, being
being activated
activated carbon-
carbon-
based, contains a high proportion of oxygen
based, contains a high proportion of oxygen atoms due to atoms due to its activation process,
activation process, to to the
the
surface pollution of the electrode
surface pollution of the electrode that could have been contaminated with compounds
compounds
rich in
rich in oxygen,
oxygen, such
such asas oxides,
oxides, duedue to
to exposure
exposure to to air
air during
during the
the operation
operation process
process of
of the
the
MFC [74].
MFC [74]. At
Atthe
the same
same time,
time, the
the high
high detection
detection of of carbon
carbon is is due
due to
to the
the electrode
electrode material
material
based on
based on activated
activated carbon
carbon [75],
[75], while
while the
the Al
Alisisdue
dueto tothe
thepresence
presenceof ofthe
thealuminum
aluminummesh,mesh,
respectively. The considerable presence of silicon can be attributed
respectively. The considerable presence of silicon can be attributed to the composition of to the composition
of the
the substrate,
substrate, whichwhich
was was
based based on food
on food remainsremains and residual
and residual waterwashing
water from from washing
dishes
dishes using cleaning products [76]. Finally, the low presence of Fe, K, and Ca can be
attributed to the activated carbon material used, which may contain low concentrations of
these elements [77]. Other researchers such as Liu, Lu, and Zhang (2022) performed EDS
analyses on their graphite felt anode electrodes used in MFC with mariculture wastewater,
and the spectra before the operation showed a more significant presence of carbon, oxygen,
platinum, silicon, aluminum, and iron; however, after the operation, the presence of
other additional compounds such as sodium, magnesium, sulfur, potassium, calcium and
titanium were reported; even so, there was a greater predominance of carbon and oxygen
in the electrode sample [78].
 ments [77]. Other researchers such as Liu, Lu, and Zhang (2022) performed EDS analyses
on their graphite felt anode electrodes used in MFC with mariculture wastewater, and the
spectra before the operation showed a more significant presence of carbon, oxygen, plati-
num, silicon, aluminum, and iron; however, after the operation, the presence of other ad-
ditional compounds such as sodium, magnesium, sulfur, potassium, calcium and titanium
Sustainability 2023, 15, 13767 10 of 14
were reported; even so, there was a greater predominance of carbon and oxygen in the
electrode sample [78].

Figure 7.
Figure 7. EDS
EDS analysis
analysis of
of the
the activated
activated carbon
carbon electrodes
electrodes after
after the
the period
period of
of operation.
operation.

3.4.
3.4. Resistance
Resistance Test
Test of
of Activated
Activated Carbon-Based
Carbon-Based Electrode
Electrode in
in Liquid
Liquid Substrate
Substrate
The
The resistance of the activated carbon based electrodes werelow,
resistance of the activated carbon based electrodes were low,asas
shown inin
shown Table 1.
Table
1.
Table 1. Evaluation of the resistance of the activated carbon-based electrodes in synthetic wastewater
contained
Table 1. in MFC for 30
Evaluation ofdays.
the resistance of the activated carbon-based electrodes in synthetic
wastewater contained in MFC for 30 days.
ID Electrode Waterproofing Agent Initial Weight (g) Final Weight (g) Weight Loss Percentage (%)
ID MFC-A
Electrode Waterproofing Agent Initial 27.58
Weight (g) Final Weight
27.18
(g) Weight Loss1.45
Percentage (%)
MFC-A pine resin 27.58 27.18 1.45
MFC-B 27.36 26.99 1.35
pine resin
MFC-B 27.36 26.99 1.35
4. Conclusions
4. Conclusions
The electrodes based on activated carbon and zinc were efficient in terms of pro-
ducingTheelectrical
electrodes basedusing
energy on activated carbon
an scMFC. and zinc
By using were efficient
synthetic wastewater in terms
as aof produc-
substrate,
ing electrical energy using an scMFC. By using synthetic wastewater
it was possible to generate maximum values of voltage (1120 ± 0.050 mV) and current as a substrate, it was
(4.64 ± 0.040 mA), respectively. Another important aspect is the reduction in substrate±
possible to generate maximum values of voltage (1120 ± 0.050 mV) and current (4.64
0.040 mA),
turbidity to respectively.
25.11 NTU and Another important
ORP values of 858aspect
mV. Inisthe
thesame
reduction in substrate
way, values turbidity
of internal resis-
to 25.11 NTU and ORP values of 858 mV. In the same way, values of internal
tance of the cell (214.52 ± 5.22 Ω), power density (208.14 ± 17.15 mW/cm ), and a current 2 resistance of
the cell (214.52 ± 5.22
2 Ω), power density (208.14 ± 17.15 mW/cm 2), and a current density
density (5.03 A/cm ) were obtained. EDS analyses revealed that the most predominant
(5.03 A/cm
elements in )the
2 were obtained. EDS analyses revealed that the most predominant elements
electrodes were oxygen, carbon, silicon, aluminum, iron, potassium, and
in the electrodes
calcium. The potentialwere ofoxygen, carbon,
activated silicon,
carbon anodealuminum,
electrodes iron, potassium, andbioenergy
for laboratory-level calcium.
The potential
production in of
MFCactivated
has been carbon anode electrodes
demonstrated. for laboratory-level
In addition, it has contributed bioenergy produc-
to the develop-
tion inofMFC
ment thesehas been demonstrated.
sustainable technologiesInthrough
addition,theitdevelopment
has contributed to the development
of economical, of
ecological,
and eco-efficient electrodes. Although electrodes are inexpensive, there are still certain
technical challenges for MFCs to increase bioelectricity generation. It is recommended
to optimize MFC designs to improve the electron utilization of substrates for bioenergy
generation.
Sustainability 2023, 15, 13767 11 of 14

Author Contributions: Conceptualization, R.A.-Q., Z.Á.-S. and S.R.-F.; methodology, R.A.-Q., Z.Á.-S.
and S.R.-F.; software, R.A.-Q. and S.R.-F.; validation, Z.Á.-S. and M.D.L.C.-N.; formal analysis, R.A.-Q.
and W.R.-V.; research, R.A.-Q. and Z.Á.-S.; resources, R.A.-Q., Z.Á.-S. and L.C.-C.; data retention, R.A.-
Q., Z.Á.-S. and S.R.-F.; writing—preparing original draft, R.A.-Q. and Z.Á.-S.; Writing—Proofreading
and Editing, S.R.-F., M.D.L.C.-N. and L.C.-C.; visualization, R.A.-Q. and S.R.-F.; supervision, R.A.-Q.,
Z.Á.-S., L.C.-C. and R.N.-N.; project management, R.A.-Q., Z.Á.-S. and W.R.-V. All authors have read
and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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