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Electrochemical and piezocatalysis properties
Electrochemical and piezocatalysis properties
Ceramics International
journal homepage: www.elsevier.com/locate/ceramint
A R T I C L E I N F O A B S T R A C T
Handling Editor: Dr P. Vincenzini Piezocatalysis activity was examined for poled and unpoled Bi0⋅5(Na0⋅9K0.1)0.5TiO3 (BNKT) ceramic. BNKT was
synthasized using solid state routes and was thoughly characterized using X-ray diffraction, Scanning electron
Keywords: microscopy,and XPS. BNKT was examined for piezocatalysis inder ultrasonication for Rhodamine B (RB) dye.
Electrochemistry Poling was performed using Corona poling setup and piezoelectric nature was evaluated using d33. d33 was found
Piezocatalysis
to be ±45 pC/N for sintered sample. The effect of electric poling was significant in view of dye degradation
Poling effect
performance. Poled BNKT sample degraded ~90% the RB dye solution in 180 min which was segnificanly higher
Piezoelectric
than that of unpoled sample. The influence of electric poling on the oxygen reduction and hydrogen evolution
process in alkaline fuel cells and electrolyzer is also reported.
* Corresponding author.
** Corresponding author. Institute of New Energy on Chemical Storage and Power Sources, School of Chemical and Environmental Engineering, Yancheng Teachers
University, Yancheng, 224000, Jiangsu, PR China.
E-mail addresses: sunyz@yctu.edu.cn (Y. Sun), anuruddh07@hanyang.ac.kr (A. Kumar).
https://doi.org/10.1016/j.ceramint.2023.01.198
Received 22 September 2022; Received in revised form 29 December 2022; Accepted 28 January 2023
Available online 3 February 2023
0272-8842/© 2023 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Y. Sun et al. Ceramics International 49 (2023) 16011–16018
promising piezoelectric applications and energy storage viewpoints and a 1:1 vol ratio of isopropyl alcohol (Sisco Research Laboratories Pvt.
[38–40]. BNKT is solid solution of Bi0⋅5Na0⋅5TiO3 and Bi0⋅5K0⋅5TiO3. Ltd., India): distilled water was added to it, along with 20 μl Nafion as a
BNKT lies near to morphotropic phase boundary (MPB) and superior binder. The ink was sonicated until a homogeneous solution was formed
piezoelectric properties [41]. This composition is not reported for cat and 20 μl (loading = 102 μg cm− 2) dropped cast over RDE to be used as a
alytic application. Hence, BNKT is selected and thoroughly explored in working electrode. Cyclic voltammetry (CV) and linear sweep voltam
electrochemistry and piezocatalysis applications. The results are dis metry (LSV) were performed for characterizing materials for their
cussed in the subsequent sections. electrochemical ability.
Rhodamine B (RB dye) (Loba Chemie Pvt. Ltd.) was selected as a
2. Experimental representative pollutant in the water to investigate piezocatalysis
degradation activities in prepared specimens. In the 15 ml glass vial used
Bi0⋅5(Na0⋅9K0.1)0.5TiO3 (BNKT), piezoelectric material was synthe for the piezocatalysis experiments, RB dye solution with an initial con
sized using a solid-state reaction route method. Powders of high-purity centration of ~5 mg/L was collected, and powder samples were mixed
reagents (AR grade, chemicals) such as Bi2O3 (99% pure), Na2CO3 into it. To further maintain the adsorption-desorption equilibrium be
(98% pure), K2CO3 (98% pure), and TiO2 (99% pure) from Thermo tween the prepared BNKT powder acting as a catalyst and the dye, the
Fisher Scientific in India were used as the raw materials. The mixture glass vial was kept in the dark for 24 h. The piezocatalytic experiment
was calcined at 900◦ C for 5 h to obtain the single-phase BNKT. Powder included continuous sonication (Ultrasonic 40 kHz and 150 W), and test
X-ray diffraction (XRD) technique using Cu-Kα radiation (Smart lab, samples were taken every 15 min. To quantify the degradation in these
Rigaku Tokyo, Japan) was used to characterize the phase formation of samples, a UV–visible spectrophotometer was used. Further, to deter
the calcined sample. 2 wt% PVA was added in BNKT powder sample and mine the most active species during catalysis reactions various scaven
prepared green pellet. These pellets were sintered at ~1150 ◦ C for 2 h. gers Ethylenediaminetetraacetic Acid (EDTA), 3-Indolepropionic acid
Field Emission Scanning Electron Microscope (Nova NanoSEM) with (IPA) and p-Benzoquinone (p-BQ) were used. A 10 ml solution of 0.01 M
tungsten as the source of electrons was used to observe the morphology was prepared for all scavengers. All the catalytic reactions were per
of the material. To determine the surface elemental constitution and formed in same conditions as described in the previous section after
composition, X-Ray Photoelectron Spectroscopy (XPS) was performed adding 1 ml of scavenger solution.
on Thermo Fisher Scientific Nexsa using Al-Kα as a source of X-Rays
(1487 eV). BNKT powder sample was poled with the help of a Corona 3. Results and discussion
poling setup. The Corona poling setup is shown in schematic 1. It con
sists of a copper needle (known as a corona needle) hanging above the The XRD pattern of BNKT powder sample was recorded at the room
powder sample that is set on a hot plate and coupled to a high-power dc temperature is shown Fig. 1. The rhombohedral (JCPDS file No.
supply. The ground is attached to the specimen’s bottom surface where 036–0340) and tetragonal (JCPDS file No. 036–0339) phases, which are
the electrode is located. A Corona needle sprays electric charge onto the well-known, identify the pure Bi0⋅5Na0⋅5TiO3 and Bi0⋅5K0⋅5TiO3 ce
surface of the powder sample, which is resting on a grounded plate, ramics, respectively. The XRD peaks are indexed according to the
when the corona discharge is sparked by the application of a dc high perovskite single phase; no secondary phase was observed in the
voltage. This creates an electric field between the samples. Charges that calcined powder sample.
are still present on the surface create an electric field that is poling be Fig. 2(a and b) shows the surface morphology images of BNKT as
tween the top surface and the ground. We assume that the voltage on the observed under FESEM. It displays irregular-shaped sheet-like particles
powder sample’s upper side is the same as the corona needle’s voltage. with an average diameter of ~500 nm-2μm. Elemental mapping was
The sample can also be heated by the hot plate during poling to a pre performed, and it revealed that all the elements- Bi, K, Na, Ti, and O are
determined temperature. 4 kV/mm electric field was applied at the time present uniformly over the material surface, as shown in Fig. 2(c–h).
of poling. Similarly sintered sample was poled and measured piezo Fig. 2(c) shows the overall element mapping of the BNKT powder sample
electric constant (d33) with the help of d33 m (YE2730A d33 m, APC and the atomic percentage of all the constituents.
international Ltd.). Fig. 3 shows the XPS spectrum of the BNKT. Fig. 3 (a) shows the
The electrochemical properties of the BNKTmaterials were evaluated survey spectrum, revealing that K is abundantly present on the surface of
on Auto Lab, Metrohm using a three-electrode setup. Pt wire and Ag/ BiNaTiO3 as a dopant, apart from Bi, Na, Ti, and O elements. The core
AgCl (3 M KCl) were employed as counter and reference electrodes. A spectrum of Bi 4f was evaluated (Fig. 3 (b)) by deconvoluting into Bi 4f
rotating disk electrode (Glassy carbon, 5 mm diameter) was used as a 7/2 and 4f 5/2 at binding energy, respectively 158.71 eV and 163.99 eV
working electrode, and catalyst ink was drop cast on it. To prepare the belonging to Bi(III) [42]. K 2p dopant core spectrum displayed peaks at
catalyst ink, 1 mg active material was mixed with 4 mg Vulcan carbon binding energy 292.96 eV and 295.42 eV corresponding to 2p 3/2 and 2p
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Y. Sun et al. Ceramics International 49 (2023) 16011–16018
Fig. 1. XRD plot of BNKT powder. 1. Incomplete two-electron pathway, which leads to the formation of
HO−2 ;
1/2respectively, indicating the presence of K+ oxidation state (Fig. 3 (c)) 2. Complete four-electron pathways, which leads to the formation of
[43]. Na 1s displays a peak at 1071.08 eV, indicating the presence of HO− ;
Na+1 in the material (Fig. 3 (d)) [42]. Ti 2p spectrum can be deconvo 3. 2 + 2 electron pathway, involving the formation of intermediate
luted into two peaks at binding energy 457.82 eV and 463.67 eV cor HO−2 , followed by HO− .
responding to Ti+4 2p 3/2 and 2p 1/2 respectively [44]. An additional
peak at 465.92 eV is also visible belonging to Bi 4d 3/2 (Fig. 3 (e)) [42]. The k-L plot follows the K-L equation, which is as follows:
Fig. 3 (f) shows the spectrum of O 1s consisting of three peaks at 532.54
eV, 529.91 eV, and 528.98 eV belonging to M-O-H, M − O, and C–O, 1 1 1
= + (1)
respectively 76.59, 14.13, and 9.28 atomic % respectively [45]. The I IL Ik
peak at 528.98eV could be attributed to C–O bond on the carbon tape
where IL and Ik are Levich current and kinetic current density
used as substrate for powdered BNKT.
respectively.
Fig. 4 shows the electrocatalytic ability of BNKT poled versus
unpoled material. To assess their electrocatalytic activity towards Ik = nFAkO2 CO2 γcatalyst (2)
Fig. 2. Electron microscopic images of BNKT: (a–b) surface morphology of BNKT as observed under FESEM; (c) overall elemental mapping with respect to (b), (d–h)
elemental mapping of Bi, Na, K, Ti, and O.
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Y. Sun et al. Ceramics International 49 (2023) 16011–16018
Fig. 3. XPS revealing the surface atomic composition: (a) Survey spectrum; and core spectrum of (b) Bi4f; (c) K2p; (d) Na1s; (e) Ti2p and (f) O1s.
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Y. Sun et al. Ceramics International 49 (2023) 16011–16018
Fig. 4. ORR capability of BNKT unpoled versus poled collected in O2 saturated 0.1 M KOH electrolyte: (a) LSV at 900 rpm; (b) K-L plot taken at 0.5 V; HER capability
of BNKT unpoled versus poled taken in N2 saturated 0.1 M KOH electrolyte: (c) LSV; (d) Tafel plot.
Fig. 5. OER capability of BNKT unpoled versus poled collected in N2 saturated 0.1 M KOH electrolyte: (a) LSV; (b) Tafel plot.
proton-coupled electron transfer (PCET) pathway. performance with other materials. The rate constant “k” was obtained by
To understand piezocatalysis performance, these unpoled and poled calculating the slope of ln C/C0 vs. time plots (Fig. 6(c). The calculated
powders were submerged in RB dye aqueous solution, and vibration was value of k was 0.0003, 0.0032, and 0.0125 min− 1 for ~5 mg/L RB dye
exposed. Several tests were conducted to rule out any effects (other than using RB dye, unpoled, and poled BNKT powder samples, respectively.
piezocatalysis). Using a predetermined calibration curve and UV–vis Ferroelectric materials have proven piezocatalysis effect due to their
spectroscopy, the catalytic effect was measured. The typical dye piezoelectric nature and semiconductor behavior. Table 1 shows the
degradation behavior signatures can be seen in the absorption plots at comparison of piezocatalytic performance of reported piezocatalysts
different times scales in Fig. 6(a). The enhanced activity in the poled with the BNKT poled sample.
BNKT powder sample is seen in this image. Other standard samples (only Fig. 6(d) depicts the pictorial representation of the piezocatalysis
dye and unpoled powder samples) were also recorded with similar process. Understanding the mechanism of piezocatalysis is necessary in
wavelength scans, however, they are not shown here. The estimated order to effectively discuss the results of experiments using this catalyst.
degradation for all the samples taken into consideration under the same The material must be piezoelectric in nature in order to perform pie
circumstances is shown in Fig. 6(b). Only poled samples have out zocatalysis. If piezoelectric materials are stressed, an internal polariza
performed the unpoled sample, providing an unambiguous interpreta tion field develops [42].
tion possible. The first-order kinetic rate is calculated by using equation The internal polarization forced the electron (e− ) and hole (h+) pairs
(5). to move in the opposite direction, and some of these did so by reacting
C with oxygen species (O2 ) and hydroxyl ions (OH− ) to produce ȮH and ˙
ln = − kt (5) O−2 . These transient radicals target the RB dye right away and break it
C0
down into harmless products. Furthermore, it has been demonstrated in
The plot of rate constants for various understudy experiments is the literature that the local piezoelectricity is adequate to carry out the
shown in Fig. 6(c). These rate constants are needed to compare catalytic piezocatalysis process [2]. This local piezoelectricity induces the
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Y. Sun et al. Ceramics International 49 (2023) 16011–16018
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Y. Sun et al. Ceramics International 49 (2023) 16011–16018
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Declaration of competing interest
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capability of lithium niobate, Adv. Powder Technol. 31 (2020) 1771–1775,
The authors declare that they have no known competing financial https://doi.org/10.1016/j.apt.2020.01.031.
interests or personal relationships that could have appeared to influence [11] S. Verma, M. Sharma, A. Halder, R. Vaish, Effect of poling on piezocatalytic and
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Acknowledgments Ba0.85Ca0.15Zr0.1Ti0.9O3/polyvinylidene difluoride (PVDF) composite film,
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This work was supported by the Opening Project of Jiangsu Province photocatalysis in Ag nanoparticles loaded 0.5(Ba0.7Ca0.3)TiO3–0.5Ba(Zr0.1Ti0.9)
Engineering Research Center of Agricultural Breeding Pollution Control O3 composites towards the degradation of organic pollutants, J. Am. Ceram. Soc.
105 (2022) 3165–3176, https://doi.org/10.1111/jace.18298.
and Resource (2021ABPCR015), the Jiangsu Provincial Key Laboratory [14] R. Djellabi, M.F. Ordonez, F. Conte, E. Falletta, C.L. Bianchi, I. Rossetti, A review of
of Coastal Wetland Bioresources (JKLBS2020004), the Jiangsu Province advances in multifunctional XTiO3 perovskite-type oxides as piezo-photocatalysts
Education Department Major Project (19KJA140003), the Jiangsu for environmental remediation and energy production, J. Hazard Mater. 421
(2022), 126792, https://doi.org/10.1016/j.jhazmat.2021.126792.
Agriculture Sci-ence and Technology Innovation Fund (JASTIF) (CX(20)
[15] X. Cheng, Z. Liu, Q. Jing, P. Mao, K. Guo, J. Lu, B. Xie, H. Fan, Porous (K0.5Na0.5)
3169), and the Innovation and entrepreneurship training program for 0.94Li0.06NbO3-polydimethylsiloxane piezoelectric composites harvesting
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Interface Sci. 629 (2023) 11–21, https://doi.org/10.1016/j.jcis.2022.08.131.
Imed Boukhris extend their appreciation to the Deanship of Scientific
[16] A. Zhang, Z. Liu, B. Xie, J. Lu, K. Guo, S. Ke, L. Shu, H. Fan, Vibration catalysis of
Research at King Khalid University, Saudi Arabia for funding this work eco-friendly Na0.5K0.5NbO3-based piezoelectric: an efficient phase boundary
through Large Research Groups Program under grant number L.R.G.P2/ catalyst, Appl. Catal. B Environ. 279 (2020), 119353, https://doi.org/10.1016/j.
174/43. apcatb.2020.119353.
[17] L. Zhou, L. Zhu, T. Yang, X. Hou, Z. Du, S. Cao, H. Wang, K.C. Chou, Z.L. Wang,
Ultra-stable and durable piezoelectric nanogenerator with all-weather service
Appendix A. Supplementary data capability based on N doped 4H-SiC nanohole arrays, Nano-Micro Lett. 14 (2022)
1–10, https://doi.org/10.1007/s40820-021-00779-0.
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Supplementary data to this article can be found online at https://doi. nanogenerators with high performance against harsh conditions based on tunable
org/10.1016/j.ceramint.2023.01.198. N doped 4H-SiC nanowire arrays, Nano Energy 83 (2021), 105826, https://doi.
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