Bioelectrochemistry 129 (2019) 10–17

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Bioelectrochemistry

journal homepage: www.elsevier.com/locate/bioelechem

Study of the corrosion behavior of Aspergillus niger on 7075-T6 aluminum

alloy in a high salinity environment
Junlei Wang a, Fuping Xiong a, Hongwei Liu a, Tiansui Zhang a, Yanyan Li a, Chenjing Li a, Wu Xia a,
Haitao Wang b, Hongfang Liu a,⁎
a
Key Laboratory of Materials Chemistry for Energy Conversion and Storage, Ministry of Education, Hubei Key Laboratory of Materials Chemistry and Service Failure, School of Chemistry and Chem-
ical Engineering, Huazhong University of Science and Technology, Wuhan 430074, China
b
Key Laboratory for Green Chemical Process of Ministry of Education, School of Chemistry and Environmental Engineering, Wuhan Institute of Technology, Wuhan 430073, China

a r t i c l e i n f o a b s t r a c t

Article history: In this study, the corrosion behavior of 7075-T6 aluminum alloy in a high salinity environment containing Asper-
Received 15 December 2018 gillus niger was investigated using high-performance liquid chromatography tandem mass spectrometry, gas
Received in revised form 25 April 2019 chromatography, surface analysis and electrochemical measurement. Results demonstrated that uniform and lo-
Accepted 25 April 2019
calized corrosion rates of the alloy in the presence of A. niger were approximately 3.7 and 22.4 times, respectively,
Available online 1 May 2019
of that in the absence A. niger. This higher corrosion rate was attributed to accelerated anode and cathode reac-
Keywords:
tions from the actions of A. niger biofilm. Additionally, organic acid corrosion caused by the presence of A. niger
Aluminum alloy was confirmed to be the main cause for the corrosion of aluminum alloy.
Aspergillus Niger © 2019 Elsevier B.V. All rights reserved.
Microbiology
Corrosion
Electrochemistry

1. Introduction
Aluminum alloy is widely used in highway constructions, railway
vehicles and aircraft due to its low density, good machinability, good
corrosion resistance and recyclability [1–4]. Aluminum alloy can suffer
from localized corrosion including pitting corrosion, intergranular cor-
rosion and exfoliation corrosion [5–7]. Localized corrosion is one of
the main reasons causing the failure of aluminum alloy structures in en-
vironments containing chloride ions [8,9].
Aluminum and some of the alloying elements in aluminum alloys
such as Mg and Zn are highly active with very negative standard reduc-
tion potentials for their corresponding ions. They instantly react with O2
to form passivating metal oxide films. The main reason for the localized
corrosion of aluminum alloy is the damage to the passive surface film
[10,11]. Hoyt et al. [12] investigated the roles of the metal elements in
the corrosion behavior of 2024-T3 aluminum alloy and systematically
studied the influence of pH and oxalate concentration on the corrosion.
Aluminum alloys also suffer from microbiologically influenced corro-
sion (MIC). One reason is because microbes can damage their passive
films. Guan et al. [13] found that sulfate reducing bacteria (SRB) could
accelerate both uniform and localized corrosion of 5052 aluminum
alloy due to the formation of an SRB biofilm on its surface. The MIC of
metals and alloys has been investigated for more than one hundred
⁎ Corresponding author.
E-mail address: liuhf@hust.edu.cn (H. Liu).
years, and its awareness is rapidly increasing in recent years [14–20].
Microorganisms including bacteria, fungi, algae and protozoa are com-
monly found in natural environments [21–23]. Most published studies
focus on MIC caused by bacteria, especially SRB [24–30]. Although
there are a few studies related to aluminum alloy corrosion induced
by fungi [31,32], the corrosion behavior and mechanism of MIC on alu-
minum alloys in the presence of fungi are still not clear.
Aspergillus niger is a ubiquitous fungal species in natural environ-
ments, especially in warm and humid environments. The high abun-
dance of A. niger in many environments is attributed to its fast growth
and wide-range temperature and pH tolerances. Previous research has
shown that A. niger can grow in the temperature range 6–47 °C and re-
mains active over an extremely wide pH range of 1.4–9.8 [33,34]. Qu
et al. [32] investigated the corrosion behavior of A. niger on magnesium
alloy and found that A. niger accelerated pitting corrosion. However,
there are few reports on the corrosion process on an aluminum alloy in-
duced by A. niger. U. Jirón-Lazosa et al. [35] found that A. niger can induce
the corrosion on non-anodized and anodized 6061 aluminum alloy.
Moreover, the fungus produced a corrosive environment that led to se-
vere local corrosion. Dai et al. [5] found that A. niger promoted pitting
corrosion when 2024 aluminum alloy was placed on the surface of
solid agar containing medium.
It is known that metabolic activities play a key role in the metallic
biocorrosion process. A. niger primary metabolites have been widely re-
ported. They include citric acid, oxalic acid, succinic acid, malic acid,
gluconic acid, cellulases and pectinases [33–35]. Metabolic products

https://doi.org/10.1016/j.bioelechem.2019.04.020
1567-5394/© 2019 Elsevier B.V. All rights reserved.
 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17
secreted by microorganisms can influence the corrosion process. There-
fore, it is necessary to explore further the role of A. niger in the alumi-
num corrosion process and the influence of the metabolites of A. niger
on the corrosion.
In this work, the corrosion behavior of 7075-T6 aluminum alloy was
investigated in a high salinity environment (3.5% NaCl by mass) solution
inoculated with a 10% (v/v) A. niger seed culture using different
methods, including weight loss, surface analysis, and electrochemical
measurement. High-performance liquid chromatography tandem
mass spectrometry (HPLC-MS) and gas chromatography (GC) were
used, respectively, to analyze the nonvolatile compounds in the test so-
lution and the gas phase compounds in the headspace at the end of the
metallic corrosion process in the presence of A. niger. This work aimed to
provide more details of aluminum alloy corrosion and to reveal the cor-
rosion process in the presence of A. niger.
2. Experimental
2.1. Materials and coupons
Corrosion coupons were cut from a 7075-T6 aluminum alloy sheet
with the following elementary composition (wt%): Fe 0.5, Si 0.4, Mn
0.3, Ti 0.2, Zn 5.1–6.1, Mg 2.1–2.9, Cu 1.2–2.0, Cr 0.18–0.28 and Al bal-
ance. A square-shaped coupon sealed in epoxy resin with an exposed
area of 1 cm2 was used to analyze surface morphology and to measure
weight loss. A cylindrical electrode with an exposed disc area of
0.785 cm2 mounted in epoxy resin was employed for the electrochem-
ical measurements. All coupons were abraded sequentially with 180,
400, 800, 1200 and 2000-grit silicon carbide metallurgical papers.
Then, the coupons were degreased with pure acetone and subsequently
dehydrated with pure ethanol. All specimens were finally dried under a
N2 gas stream and sanitized under an ultraviolet lamp for 20 min.
2.2. Purification and identification of A. niger
A. niger used in this work was obtained from a damp and moldy alu-
minum alloy sheet surface. It was incubated in potato dextrose liquid
culture medium (potato infusion 200 g/L, dextrose 20 g/L) at 37 °C.
The dilution plate method was used for isolation and purification of
A. niger. Potato dextrose culture medium with 2% (w/w) agar was
used as a solid medium. After purification, polymerase chain reaction
(PCR) method was used for DNA sequencing. The obtained sequence in-
dicated that this fungus was A. niger (ATCC 1015), which is a spore-
forming filamentous fungus. In this work, to simulate the marine envi-
ronment, 3.5% (w/w) NaCl solution in 10% (v/v) potato dextrose broth
was used as the test solution. The pH of the test solution was recorded
using a pH meter (Model PHS-3C, Leici, Shanghai, China). The test solu-
tion was sterilized using an autoclave for 20 min at 121 °C before inoc-
ulation [36].
2.3. Growth curve measurement
A. niger was cultured in a 300 mL flask with 150 mL test solution at
37 °C. A single colony was used to inoculate the test solution. This incu-
bation method was applied to all samples in this work. Growth status
was monitored daily for 18 days using the dilution plate method. Prior
to measurement, the flasks were well shaken on a gyratory shaker for
20 min. One mL suspension was diluted in a 10 mL test tube containing
9 mL 0.85% NaCl solution. Then, 1 mL of the diluted suspension was
injected into the next test tube to continue the serial dilution procedure.
One hundred μL of the diluted suspension from each test tube was used
to streak an agar plate. The serial dilution continued until either no or
only a single fungal colony appeared on an agar plate after 14 days of in-
cubation at 37 °C.
11
2.4. HPLC-MS
HPLC-MS was used to analyze the metabolites produced by A. niger
in the broth after 18 days incubation. An HPLC system (Model 1100LC,
Agilent, Palo Alto, USA) was used with an Agilent TC-C18 column
(250 mm × 4.6 mm). The UV detector wavelength was set at 240 nm.
HPLC was coupled with mass spectrometry (MS) (Model MSD Trap,
Agilent, Palo Alto, USA) with an electrospray ionization (ESI) probe in
positive ion mode. The parameters for the MS were: capillary voltage
4.5 kV, end plate offset −500 V, dry temperature 200 °C, and dry gas
flow rate 2.0 L/min. MS results were analyzed using the Bruker data
analysis software.
Elution was performed with a mobile phase containing MeOH, MeCN
and H2O (35:15:50 by volume) at a flow rate of 0.7 mL/min on the HPLC.
Prior to HPLC sampling, the test solution was filtered using a bistratal
gauze to remove fungal mycelia and big particle impurities. Extraction
was carried out three times with dichloromethane (1:1 by volume).
Twenty μL of the organic phase was injected into the HPLC column.
2.5. Gas chromatography
Gas chromatography (GC) (Model GC7900, Techcomp, Beijing,
China) equipped with a SGH-300A hydrogen generator and a WJK-2LB
low noise air pump was used to analyze gas phase products in the head-
space of each flask. Hydrogen evolution testing was performed in three
300 mL flasks sealed with silicone rubber stoppers with 150 mL test so-
lution in each flask. The trapped air in the sealed flasks was initially
available for the aerobic respiration of A. niger. Four disc coupons were
hung in the test solution in each flask. Two sets of three flasks each
were incubated for 18 days with and without A. niger at 37 °C, respec-
tively. Just before the GC sampling, a 500 μL methane gas sample at
room temperature and 1 atm was injected into the headspace of each
flask. Methane is not produced by A. niger and its solubility in water is
negligible. The corresponding methane peak in the GC diagram
corresponded to a fixed amount of methane which was then used as
the relative reference for the calculation of H2 concentration in the
headspace gas samples.
2.6. Weight loss measurement
The corrosion products were removed using a pickling solution after
18 days of incubation as reported [5]. The corrosion rates were calcu-
lated using the equation,
8:76  104  Δm
Corrosion rate ðmm=yÞ ¼ ð1Þ
ρAt
where Δm, ρ, A and t are weight loss (g), coupon density (g/cm3) and
exposed coupon area (cm2) and incubation time (h), respectively.
2.7. Surface analysis
After 18 days of incubation, coupons were retrieved for surface anal-
ysis. Before scanning electron microscope (SEM) (Model Nova
NanoSEM 450, FEI, Eindhoven, Netherlands) observations, coupons
were immersed in a phosphate buffer solution (PBS) mixed with 2.5%
(v/v) glutaraldehyde for 4 h to kill and fix the biofilms [36]. Then, the
biofilms were dehydrated using a series of ethanol solutions (10%,
70%, 90% and 100% by volume) and finally dried under N2 [37]. Three-
dimensional microscopy using a Model VHX-1000E Keyence (Osaka,
Japan) microscope was used to measure the corrosion morphology on
each coupon after removing the biofilm/corrosion products with a pick-
ling solution [5]. The coupons were kept level to avoid anamorphosis of
the 3D results. An X-ray diffractometer (XRD) (Model X'Pert PRO,
PANalytical, Eindhoven, Netherlands) was used to identify the corrosion
products.
12 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17

(a) 12 (b) 6.0

-1
10

logNA. niger/spore· mL
5.5
8

pH
5.0
6
4.5
4

2 4.0
2 4 6 8 10 12 14 16 18 0 2 4 6 8 10 12 14 16 18
t/d t/d

Fig. 1. The growth curve of planktonic A. niger (a) and the changes of broth pH (b) in the test solution at 37 oC. ( Abiotic; A. niger).

2.8. Electrochemical measurements measurements were performed by scanning from −200 mV to

All electrochemical measurements were carried out using an
electrochemical workstation (Model CS350, Corrtest, Wuhan,
China) on a classical three-electrode system with a saturated calomel
electrode (SCE) as the reference electrode, a platinum plate as the
counter electrode and 7075-T6 aluminum alloy (0.785 cm2 exposed
surface) as the working electrode, respectively. The schematic dia-
gram of the electrochemical glass cell setup is shown in Supplemen-
tary Data. When the open circuit potential (OCP) was stable,
electrochemical impedance spectroscopy (EIS) was undertaken by
applying a 10 mV sinusoidal AC voltage at a frequency from
10,000 Hz to 0.01 Hz. Potentiodynamic polarization curve
200 mV vs. OCP at a sweep rate of 0.5 mV/s at the end of the incuba-
tion. As a common practice, the same coupon was not used after-
wards due to possible damages to the biofilm/corrosion product
layer by the wide voltage scan. All tests were repeated three times
to ensure the reproducibility of the test results.
3. Results and discussion
3.1. Growth curve of A. niger and the change of broth pH with time
The growth curve of planktonic A. niger is shown in Fig. 1 (a). A lag
phase is clearly seen in the initial 6 days of incubation, which was

Fig. 2. HPLC-MS results of the test solution containing A. niger after 18 days of incubation.
 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17 13

Fig. 3. Gas chromatogram of the gas phase products (in the headspace) produced during the corrosion process in the presence of A. niger after 18 days of incubation.

consistent with previous reports indicating that A. niger has an initial
period to adapt to a new growth environment in a high salinity test so-
lution [38,39]. After 6 days of incubation, the growth rate of A. niger ac-
celerated rapidly to begin the exponential growth phase. Between days
12 and 18, planktonic A. niger growth slowed down, possibly reaching
the stationary phase. After day 18, the planktonic A. niger cell count
started to decline due to nutrient depletion.
The changes of pH for the test solutions are shown in Fig. 1 (b). It is
seen that the pH of the abiotic shifted only a little with time. The pH of
the test solution in the presence of A. niger changed slightly before day 5
because of the slow growth of A. niger, but this was followed by a sharp
decline afterwards until day 11. The lowest pH in the presence of A. niger
was 4.3. The pH trend was consistent with the growth pattern of A. niger,
because organic acids were among its metabolites.

Fig. 4. SEM images of surface films after 18 days of incubation with and without A. niger: (a) Abiotic, (b) A. niger, and (c) the surface film in the presence of A. niger after removing surface
mycelia with (d) showing an enlarged image of an area (red square) of (c).
14 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17

0.5 3.2. HPLC-MS analysis

0.4 Coupons were taken out from test solutions containing A. niger after
18 days of incubation. The test solutions were analyzed using HPLC-MS.
-1
CR/mm· y

0.3 Fig. 2 shows the HPLC-MS results after an isocratic elution. The MS re-
sults corresponding to the HPLC peak at 3.7 min are shown. In the pos-
0.2 itive ion mode, intense signals at 212 m/z, 213 m/z, and 214 m/z are
seen, which correspond to sodium citrate (its anion or salt). The signals
0.1 at 195 m/z and 196 m/z correspond to gluconic acid and its anion. The
peak at 168 m/z represents gallic acid. There are literature reports that
0.0 A. niger produces weak organic acids such as citric acid, gluconic acid
Abiotic A. niger and oxalic acid [5,35,40,41]. Their accumulation depends on important
factors including pH, aeration, concentration and carbon source variety,
Fig. 5. Corrosion rates calculated based on weight loss with and without A. niger after with pH and aeration of the nutritive medium most influential [40–42].
18 days of incubation. This work failed to detect oxalic acid, Kubicek et al. [43,44] indicated
that oxalic acid biosynthesis is favored by a high, almost alkaline culture
medium pH. Low pH suppressed the formation of oxalic acid but was

Fig. 6. XRD results of corrosion products in the absence (a) and presence (b) of A. niger after 18 days of incubation. ( Al; Al(OH)3; AlO(OH)).

Fig. 7. Surface analysis of specimens after removing corrosion products at the end of 18 days of incubation in the absence (a and b) and presence (c and d) of A. niger.
 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17 15

Fig. 8. Nyquist and Bode plots in the absence (a and b) and presence (c and d) of A. niger during 18 days of incubation, and EIS derived corrosion resistance Rp (= Rf + Rct) vs. with time (c),
and corresponding current density (f) based on 1/Rp. ( 1d; 4d; 7d; 11d; 15d; 18d;\ \Fitted line; Abiotic; A. niger).

(a) -0.72 (b) -0.5

-0.6
-0.76
OCP/V (vs. SCE)

-0.7
E/V (vs. SCE)

-0.80
-0.8

-0.84 -0.9

-1.0
-0.88
0 2 4 6 8 10 12 14 16 18 20 -10 -9 -8 -7 -6 -5 -4 -3 -2 -1
t/d log i /A·cm
-2

Fig. 9. The changes in OCP during the 18-day incubation (a) and potentiodynamic polarization curves at the end of the incubation (b) in the absence and presence of A. niger. (
Abiotic; A. niger).
16 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17
Table 1
Fitted results of potentiodynamic polarization curves in Fig. 9(b).
βa (V∙dec−1) βc (V∙dec−1)
Abiotic 0.054 ± 0.010 −0.860 ± 0.004
A. niger 0.016 ± 0.003 −0.167 ± 0.007
good for the formation of citric acid [45]. Moreover, the citric acid accu-
mulation increased significantly with an increase in dissolved oxygen
concentration [42,46]. On consideration of the above, the low pH in
Fig. 1 (b) was beneficial to citric acid formation, but not to oxalic acid
formation in the pH range between 4.3 and 5.5. Moreover, broth aera-
tion was highly effective from the ambient environment because of
the use of a sterilized sponge plug capping the vessels (Supplementary
Data).
3.3. GC analysis
Gas chromatograms for the gas phase products in the headspace
of A. niger broths after 18 days are shown in Fig. 3. A large H2 peak
(8.16 × 106 mV min of peak area) was observed at 1.21 min retention
time. The large peak (5.99 × 106 mV min of peak area) at 2.81 min in
Fig. 3 corresponds to the nitrogen. The tiny peak (7.35 × 104 mV min
of peak area) at 7.15 min corresponds to the methane reference. The
H2 concentration in the sample was 74.5 mmol/L. This means that a
large amount of H2 was produced due to hydrogen evolution from pro-
ton reduction in organic acid corrosion. This was consistent with the re-
sults of the HPLC-MS indicating organic acid secretion by A. niger.
3.4. Surface analysis
The SEM images of the coupons with or without A. niger incuba-
tion after 18 days are shown in Fig. 4. For the abiotic coupon, the cor-
rosion product appeared compact with some cracks (Fig. 4a). The
coupon surface exhibited a broken passive film after it was sub-
merged in high salinity medium, leading to slight corrosion. After
that, the corrosion products formed a compact film, which usually
inhibited further corrosion [25]. The cracks could be the result of
the coupon surface dehydration process during the sample prepara-
tion for SEM. In the presence of A. niger, mycelium networks
intertwined with corrosion products and the biofilm appeared po-
rous (Fig. 4b). Fig. 4c and Fig. 4d show a biomineralized morphology
after the removal of intertwined mycelia with sterile forceps. More-
over, the biomineralization film was composed of Al(OH)3 and AlO
(OH), according to the XRD results below.
3.5. Weight loss measurement
The corrosion rate calculated based on weight loss at the end of 18 days
with A. niger is compared with that without A. niger in Fig. 5. A. niger led to a
much higher corrosion rate of (0.41 ± 0.07) mm/y compared with (0.11 ±
0.04) mm/y in the absence of A. niger. This indicates that the uniform
biocorrosion rate with A. niger was 3.7 times greater than the abiotic rate.
3.6. XRD analysis
The XRD spectra of corrosion products after 18 days of incubation
are shown in Fig. 6. The full peaks of Al substrate at a high amplification
indicate very little corrosion of the aluminum alloy or the corrosion
products were below detectable levels on the abiotic coupon. In the
presence of A. niger, the peaks of Al(OH)3 and AlO(OH) with a lower am-
plification were broad, suggesting that less protective corrosion prod-
ucts were formed on the biotic coupon surface.
Ecorr (V) vs. SCE icorr (A∙cm−2)
−0.767 ± 0.010 (1.08 ± 0.07) × 10−7
−0.744 ± 0.018 (3.14 ± 0.13) × 10−6
3.7. 3D surface morphology of coupons
Fig. 7 shows the 3D surface morphology of corroded coupons after
removing corrosion products. The deepest corrosion pit depth was
found to be 11 μm in the abiotic (Fig. 7a and b). Some parallel polishing
lines are visible in Fig. 7a, suggesting that the corrosion was localized
pitting corrosion. The deepest pit depth was found to be 247 μm corre-
sponding to a surface diameter of more than 700 μm in Fig. 7c and d.
This pit depth was 22 times greater than that of the abiotic pit. Such se-
rious localized corrosion would be a big threat to aluminum alloy
materials in practical applications.
3.8. Electrochemical measurements
After the analysis of the EIS spectra, the equivalent electrical circuits
and impedance parameters are shown in Supplementary Data. In gen-
eral, the impedance of the abiotic samples showed a steady growth
with time. Log |Z| of day 1 as shown in Fig. 8 (b) is clearly lower than
later values, which could be attributed to the high-salinity substrate
and an increased thickness and compactness of corrosion product
films. Although the biotic impedance was similar with the abiotic ini-
tially, the semi-circle in Fig. 8(c) shows an obvious decrease later on,
which could be attributed to acid corrosion by fungus. In addition to
the two capacitive loops, an inductive loop was also present at the late
stage in the presence of A. niger, which could be due to porous biofilms
on the electrode surface or due to the desorption of Cl−/corrosion prod-
ucts [47]. Fig. 8 (e) shows the change in corrosion resistance (Rp = Rf +
Rct) over time, where the 1/Rp is proportional to the corrosion rate and
was used to calculate current density icorr (B/Rp) with 18 mV for B.
Fig. 8 indicates that the initial values of Rp and icorr were same for the
abiotic and biotic working electrodes, but the biotic values started to
change greatly while the abiotic values did not change much.
The abiotic OCP and the biotic OCP both took off on the first day.
Starting on the second day, they leveled off on remaining days during
the 18 days of incubation period as shown in Fig. 9(a). Fig. 9(a) shows
that the biotic OCP curve is below the abiotic OCP curve, suggesting
that the working electrode in the presence of A. niger had a higher ther-
modynamic tendency to lose electrodes, which could be attributed to
the metabolic activities and metabolic products of A. niger.
Fig. 9(b) shows potentiodynamic polarization curves. The corre-
sponding fitted parameters from Tafel analysis are listed in Table 1.
Table 1 indicated that the biotic icorr was about 29 times of abiotic icorr,
confirming the acceleration of corrosion by A. niger. The icorr trend
here corroborated weight loss and EIS data, all pointing to accelerated
corrosion in the presence of A. niger.
4. Conclusion
The corrosion behavior of 7075-T6 aluminum alloy was studied in
the high salinity solution environment inoculated with A. niger.
A. niger grew well and attached to the surface of aluminum alloy well
after an initial adaptation period. The XRD analysis indicated that the
corrosion products in the presence of A. niger were Al(OH)3 and AlO
(OH). Electrochemical measurements, weight loss and 3D surface anal-
ysis all confirmed that the corrosion of aluminum alloy was accelerated
in the presence of A. niger. Both uniform and localized corrosion were
observed. Organic acid secreted by A. niger was confirmed to be respon-
sible for the corrosion. This study proved the severe biodeterioration by
 J. Wang et al. / Bioelectrochemistry 129 (2019) 10–17
fungus against aluminum alloy can occur. Field operators should be
aware of the importance of materials protection against fungal MIC.
Acknowledgements
This research was supported by National Key Research and Develop-
ment Program of China (2018YFF0215002), the Open Fund of Hubei Key
Laboratory of Materials Chemistry and Service Failure (2017), Key Lab-
oratory of Materials Chemistry for Energy Conversion and Storage, Min-
istry of Education (2018), Graduate Students Innovation Fund of
Huazhong University of Science and Technology (5003013021). We
also acknowledge the support of the Analytical and Testing Center of
the Huazhong University of Science and Technology for SEM and XRD
measurements.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.bioelechem.2019.04.020.
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