Arabian Journal of Chemistry 16 (2023) 105231

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Arabian Journal of Chemistry

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Original article

Waste rice noodle-based CQDs/ZnO composite nanorod array on steel

wire mesh: Preparation and photocatalytic capability
Ruijie Che a,b, Biyang Tu b, Yining Zhu b, Jiahe Miao b, Xinyan Jin a, Shuoping Chen a,⇑
a
College of Materials Science and Engineering, Guilin University of Technology, Guilin, Guangxi 541004, China
b
School of Environment, Nanjing Normal University, Nanjing, Jiangsu 210023, China

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

Article history: In order to develop cost-effective photocatalytic devices, a nanorod array-structured carbon quantum
Received 16 May 2023 dot/zinc oxide (CQDs/ZnO) composite was synthesized on a steel wire mesh substrate using waste rice
Accepted 31 August 2023 noodle (WRN) as the raw material. The incorporation of CQDs derived from WRN played a crucial role
Available online 09 September 2023
in controlling the morphology of the ZnO-based array. By optimizing the loading of CQDs, the CQDs/
ZnO composite achieved a regular hexagonal prism nanorod array distribution and exhibited highly effi-
Keywords: cient photocatalytic degradation of various organic pollutants. For instance, in the case of methylene blue,
Waste rice noodle
the CQDs/ZnO composite demonstrated a remarkable degradation rate of 99.4% within 90 min, with a
CQDs/ZnO composite
Array
high degradation rate constant of 0.033 min
1. Moreover, the composite material could be recycled
Steel wire mesh and reused for five photocatalytic cycles without a significant decrease in its degradation performance,
Photocatalytic surpassing the performance of the pure ZnO array. Furthermore, the resulting CQDs/ZnO composite array
exhibited effective photocatalytic degradation for other organic dyes such as malachite green, methyl
violet, basic fuchsin, and rhodamine B. Additionally, this composite material was successfully applied
to real water purification, achieving a high mineralization efficiency of 48% and a low leaching rate of
Zn of 1.2% in a river water sample after a 90-minute photocatalytic process. The introduction of CQDs
derived from WRN into the ZnO array led to efficient electron-hole pair separation, enabling more pho-
togenerated electrons to reduce O2 and more photogenerated holes to oxidize H2O. This resulted in
enhanced radical generation and improved photocatalytic degradation of organic pollutants, showcasing
the superior performance of the CQDs/ZnO composite array.
Ó 2023 The Author(s). Published by Elsevier B.V. on behalf of King Saud University. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction wastewater presents a more promising alternative. Over the past

50 years, semiconductor photocatalysis has been extensively
The global environment is currently facing immense pressure, employed in water treatment (Zhou et al., 2023), encompassing
with water pollution being one of the main sources of environmen- the degradation of various pollutants, hydrogen production, carbon
tal problems (Huang et al., 2022; Sarkar et al., 2017). Commonly dioxide reduction, and nitrogen fixation (Chang et al., 2022; Xue
used methods for wastewater treatment include adsorption, coag- et al., 2022). The key to successful photocatalysis lies in the design
ulation, precipitation, oxidation, and reduction, but these tradi- of efficient and cost-effective photocatalysts (Gangu et al., 2019;
tional approaches are prone to causing secondary pollution to Huszla et al., 2022). Currently, materials like TiO2, CuO, ZnO, and
water bodies and the environment (Chiu et al., 2019; Modrogan V2O5 are widely used as catalysts for photocatalytic reactions due
et al., 2021, 2020). Photocatalytic degradation of pollutants in to their strong and effective ability to combat chemical and biolog-
ical pollution in water (Modrogan et al., 2021). The photocatalytic
activity is largely influenced by catalyst properties, such as mor-
⇑ Corresponding author. phology, composition, specific surface area, and band gap width
E-mail address: [email protected] (S. Chen). (Nicolaescu et al., 2021). Among the various types of catalysts, zinc
Peer review under responsibility of King Saud University. oxide (ZnO) has attracted significant attention for its properties of
high efficiency, nontoxicity, low cost, ease of preparation and
proper conduction band (CB) potential (Jiang et al., 2022b;
Abdollahi et al., 2021; Gao et al., 2021; Senasu et al., 2021). ZnO
Production and hosting by Elsevier is extensively used as a new type of material in various fields such

https://doi.org/10.1016/j.arabjc.2023.105231
1878-5352/Ó 2023 The Author(s). Published by Elsevier B.V. on behalf of King Saud University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

as electronics, textiles, rubber, photocatalysis, and pharmaceuticals good degradation rate of 99.58% within 40 min and a high degrada-
(Purcar et al., 2017). However, ZnO has a large band gap (Eg = 3. tion rate constant of 0.2630 min
1, and could be recycled and
37 eV), resulting in a narrow range of light absorption wave- reused for ten photocatalytic cycles without an appreciable
lengths, mainly concentrated in the UV band. This limitation decrease in the degradation effect, which was much better than
greatly hampers its utilization of solar energy and photocatalytic that of commercial ZnO (Jin et al., 2022b). However, as a powdered
efficiency (Samadi et al., 2016; Shen et al., 2022). Moreover, pris- photocatalyst each recycling step of this CQDs/ZnO composite
tine ZnO suffers from the recombination of photogenerated based on WRN requires careful centrifugation, washing, and dry-
electron-hole pairs (Wang et al., 2020). Numerous strategies have ing. This process posed significant challenges when applied to
been explored to address these drawbacks, such as doping, con- large-scale wastewater treatment in practical settings. In addition,
structing heterojunctions, and incorporating coupled carbon mate- it is challenging to assemble these powdered catalysts into photo-
rials (Abd-Elrahim and Chun, 2021; Jiang et al., 2021; Pan et al., catalytic reaction devices that can be used for an extended period.
2020; Zelekew et al., 2021; Zhang et al., 2023a). In order to meet the demands of large-scale industrial water
The carbon quantum dots (CQDs) have attracted widespread purification, it is essential to address the challenges associated
attention in the field of photocatalytic material design due to their with the difficult recovery and assemble of powdered catalysts
high water dispersibility, high stability, and low toxicity (Jiang et al., 2022a; Marugán et al., 2007; Zhang et al., 2020). One
(Arumugham et al., 2020; Zhao et al., 2022). The high responsive- effective solution is to prepare a photocatalytic device in which
ness to sunlight (Tang et al., 2019), ability to enhance the adsorp- the photocatalytic component could be loaded onto a low-cost
tion performance(Chen et al., 2022; Yu et al., 2022), and high and stable substrate (Misra et al., 2022; Sugita et al., 2020). Zhou
resistance to photogenerated electron-hole pair recombination et al. (Zhou et al., 2020) prepared a three-dimensional artificial
make CQDs a suitable candidate for improving photocatalytic effi- nanoforest by hydrothermally loading n-type polar microporous
ciency (Behnood and Sodeifian, 2020; Que et al., 2017; Zhang et al., modulated wide bandgap ZnO nanodiscs on a copper grid, showing
2023b). Recently, new developments have occurred in the applica- good photocatalytic reduction activity and recyclability for aque-
tion of CQDs in photocatalytic materials. Behnood et al. synthe- ous hexavalent chrome [Cr(VI)]. Misra et al. (Misra et al., 2022)
sized nitrogen-doped carbon quantum dot composite nickel- designed a photocatalytic device utilizing zinc oxide composite
doped zinc oxide (Ni-ZnO/N-CQDs) composites using a hydrother- gypsum loaded with sodium alginate (ZnO/G@alginate) to achieve
mal method. The presence of Ni and N-CQDs could promote the disinfection of Salmonella enterica serovars under visible light.
separation of electron-hole pairs under visible light, and 87% of However, due to the widespread use of expensive synthetic
methylene blue (MB) can be effectively degraded within 120 min reagents in the preparation process of these photocatalytic devices,
(Behnood and Sodeifian, 2020). Mandal et al. prepared nonmetallic their high production costs may hinder practical
nitrogen-doped carbon quantum dots (N-CQDs) hybridized with commercialization.
zinc oxide nanorods (NRs). The degradation performance of rho- Anticipating the incorporation of waste-based raw materials
damine B on ZnO/NCQD reached approximately 90% within and the selection of appropriate low-cost substrates, it becomes
9 min under ultraviolet irradiation (Mandal et al., 2021). To date, feasible to design and synthesize a photocatalytic device that is
most CQDs in CQDs/ZnO composite materials reported by other not only cost-effective but also highly efficient, easy to recycle,
researchers originate from relatively high-cost synthetic raw mate- long-lasting, and environmentally friendly. Building upon previous
rials, such as glucose, sucrose, fructose, ascorbic acids, sodium research, our primary objective is to develop a novel photocatalytic
citrate, and graphite rods(Han et al., 2021; Murali et al., 2021; device comprising a CQDs/ZnO composite based on WRN, which
Tan et al., 2021; Wu et al., 2019; Xu et al., 2019). Unfortunately, offers advantages of lower production costs, convenient assembly,
these raw materials are not conducive to industrial applications, and practical application. Through the utilization of low-cost steel
especially in economically underdeveloped areas. wire mesh as a substrate, we successfully created a budget-friendly
On the other hand, more than 1.3 billion tons of cooking waste photocatalytic device featuring a CQDs/ZnO composite nanorod
are generated worldwide each year (Rojas et al., 2022). Because of array, utilizing WRN as the raw material. This resulted in the
the high levels of water and organic matter in cooking waste, its CQDs/ZnO composite array demonstrating outstanding photocat-
inadequate disposal can easily have several harmful effects on alytic degradation efficiency for various organic pollutants, thereby
the environment (Li et al., 2023), including surface and ground serving as a valuable reference for the design of efficient photocat-
water contamination, virus transmission, and pollutant gas emis- alytic reactors. Our research delves into the morphology, structure,
sions (Barik and Paul, 2017; Chu et al., 2019). Current commercial photocatalytic performance, and photocatalytic mechanism of the
treatments for cooking waste mainly involve methods like anaero- array, with a comprehensive analysis of the effects of CQDs combi-
bic digestion (Yan et al., 2021), aerobic composting (Xie et al., nation on the material’s morphologies and properties.
2023), landfill (Shehzad et al., 2015), incineration (Xiao et al.,
2018), and forage making (Mo et al., 2020). While these strategies
allow for large-scale industrialization of cooking waste treatment, 2. Experiment section
they come with significant drawbacks, including extensive land
use, high equipment investment, low product profit margin, and 2.1. Materials
the potential for secondary pollution such as greenhouse gas emis-
sions and waste leachates (Touze-Foltz et al., 2021). In order to Waste rice noodles (WRN, primary organic constituents: starch
address these issues, our previous investigation proposed a novel 21.65 g/100 g; fat 0.4 g/100 g; protein 1.91 g/100 g) were obtained
approach to utilize cooking waste, specifically waste rice noodle and retrieved from a Guilin-based university canteen. Stainless
(WRN), with starch as the main component. This approach steel wire mesh (material: 304 stainless steel; size: 400 mesh; den-
involved first hydrothermal carbonizing the WRN to create a solu- sity: 7.93 g/cm3), zinc acetate dihydrate (98% purity), ammonia
tion of carbon quantum dots (CQDs), which was then combined (28 wt% in water solution), methylene blue (98.5% purity), mala-
with specific inorganic nano powders like TiO2 or ZnO to produce chite green (98% purity), methyl violet (98% purity), basic fuchsin
CQDs/TiO2 or CQDs/ZnO photocatalytic composites for water pollu- (98% purity), rhodamine B (98% purity), and dimethyl pyridine N-
tion control (Jin et al., 2022b; Jin et al., 2022a). For instance, the oxide (DMPO, 99% purity) were acquired from Maclean’s Reagent
CQDs/ZnO composite based on WRN exhibited a highly efficient (Shanghai, China), and all reagents were used without additional
photocatalytic degradation effect on methylene blue, showing a refinement.
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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

2.2. Synthesis 2.3. General characterization

The schematic illustration of the synthesis and device integra- The scanning electron microscope (SEM) images and energy-
tion of the WRN-based CQDs/ZnO composite nanorod array on dispersive X-ray (EDX) elemental analysis were obtained by using
the steel wire mesh is shown in Fig. 1. At first, the stainless steel an S-4800 field emission scanning electron microscope (Hitachi,
wire mesh was subjected to a cleaning process using acetone and Chiyoda, Tokyo, Japan) with an accelerating voltage of 20 kV. The
anhydrous ethanol with ultrasonic treatment for 30 min, which morphology the CQDs/ZnO composite were characterized using a
was repeated for three times. Subsequently, the steel wire mesh JEM-2100F field emission transmission electron microscope
was dried in a vacuum drying oven at 60 °C. Next, zinc acetate (TEM, JEOL, Akishima, Tokyo, Japan) with an accelerating voltage
was dissolved in anhydrous ethanol to form a 0.005 mol/L ethano- of 200 kV. The powder X-ray diffraction (PXRD) patterns were
lic solution of Zn2+ ions. The cleaned steel wire mesh was obtained using an X’pert PRO X-ray diffractometer (Panalytical,
immersed in the 0.005 mol/L Zn2+ ethanolic solution for approxi- Malvern, Worcestershire, UK) with Cu Ka radiation (k = 0.15418 Å
mately 10 s. and then was removed and quickly dried in a 60 °C ) at 40 kV and 40 mA, and a scan speed of 5° min
1 (2h). The result-
oven for 1 h, which was repeated for four times. The stainless steel ing products’ infrared (IR) spectra were recorded as KBr pellets in
wire mesh then underwent calcination at 350 °C for 20 min using a the range of 400–4000 cm
1 using a Nicolet 5700 FT-IR spectrom-
muffle furnace. eter (Thermo Fisher, Waltham, MA, USA) with a spectral resolution
Simultaneously, following our previously established method of 4.00 cm
1. The X-ray photoelectron spectroscopy (XPS) of the
(Jin et al., 2022a), CQDs solution was prepared via hydrothermal CQDs/ZnO composite and ZnO was carried out using an ESCALAB
treatment of the WRN. Specifically, 150 g of WRN was milled and 250Xi X-ray photoelectron spectrometer (Thermo Fisher, Waltham,
thoroughly mixed with 300 g of deionized water. The mixture MA, USA) with an Al Ka X-ray as the stimulating source.
was placed in a 500 mL hydrothermal reactor (Yitron Instrument, The UV–VIS absorption spectra of the CQDs/ZnO composite and
Xian, China) lined with PTFE and heated at 200 °C for 10 h. The ZnO array were measured using a UV3100 UV–VIS–NIR spec-
upper layer of the reaction product, the CQDs solution, was trophotometer (Shimadzu, Chiyoda, Tokyo, Japan) in diffuse reflec-
obtained by filtration. tion mode, with BaSO4 as the reference material. The photo-
Then, zinc acetate was dissolved in water to form a 0.2 mol/L luminescence spectra of the CQDs/ZnO composite and ZnO array
aqueous solution of Zn2+ ions. The resulting Zn2+ solution were examined using a Cary Eclipse fluorescence spectrophotome-
(0.2 mol/L), ammonia, and CQDs solution were mixed in a ter (Varian, Palo Alto, CA, USA) with a xenon lamp as the excitation
500 mL PTFE-lined hydrothermal reactor (Yitron Instrument, Xian, source. The spectra were recorded in the range of 350 to 650 nm,
China) at a volume ratio of 30: 3: 1  5. Subsequently, the stainless and the excitation wavelength used was 325 nm. For investigating
steel wire mesh that had undergone the previously mentioned the electrochemical properties of the CQDs/ZnO composite and
treatment was placed vertically into the hydrothermal reactor ZnO array, a three-electrode system was employed. This system
and heated at 95 °C for 12 h. The resulting sample was rinsed three included a platinum network counter electrode and an Ag/AgCl
times with deionized water and anhydrous ethanol, followed by (saturated KCl) reference electrode, using a 0.1 mol L–1 Na2SO4
drying at 60 °C for 6 h. This process resulted in the final stainless aqueous electrolyte at 25 °C. To determine the transient photocur-
steel wire mesh with the surface-loaded CQDs/ZnO composite rent response, an electrochemical analyzer was used with a 0.5 V
nanorod array. The synthetic formulation and EDS elemental anal- bias voltage under light irradiation from a 300 W Xe lamp serving
ysis of the CQDs/ZnO composite nanorod arrays on the steel wire as the light source. Moreover, electron spin resonance (ESR) was
mesh are presented in Table 1. employed to evaluate the radical production abilities of the

Fig. 1. Schematic illustration of the synthesis and device integration of WRN-based CQDs/ZnO composite nanorod array on steel wire mesh.

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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Table 1
Synthetic formulation and EDS elemental analysis of CQDs/ZnO composite nanorod array on steel wire mesh.

Serial number Dosage of CQDs solution (mL)* Elemental analysis (wt%)

Zn O C
CQDs/ZnO-1 10 76.90 20.01 3.09
CQDs/ZnO-2 20 72.21 20.91 6.88
CQDs/ZnO-3 30 69.72 20.02 10.26
CQDs/ZnO-4 40 65.29 19.27 15.44
CQDs/ZnO-5 50 62.85 16.43 20.72
*
Dosage of zinc acetate solution and ammonia were 300 mL and 30 mL for all the samples, respectively.

CQDs/ZnO composite array, using an EMXplus X-band electron C0

lnð Þ ¼ K r Kt ¼ K app t ð2Þ
paramagnetic resonance spectrometer (Bruker, Karlsruhe, Baden- C
Württemberg, Germany), while dimethyl pyridine N-oxide (DMPO)
was served as the spin trapping agent for the ESR measurements. where Kapp is the apparent degradation rate constant in min
1, used
as the basic kinetic parameter.
Furthermore, the obtained CQDs/ZnO array on the steel wire
2.4. Photocatalytic performance measurement
mesh was applied to real water purification. We collected actual
river water samples from Nanjing Normal University (NNU) and,
The photocatalytic degradation experiment was conducted in
upon returning to the laboratory, subjected them to filtration to
an opaque, closed-loop photocatalytic degradation system, which
remove impurities. Subsequently, we employed the CQDs/ZnO
includes a core photocatalytic reactor, storage reservoir, pumps,
array on the steel wire mesh for the purification of the river water
and connecting pipes. As shown in Fig. S1, the photocatalytic reac-
sample. To gauge the degradation capacity of photocatalysts
tor had dimensions of 1  0.2  0.2 m. Within the reactor, a blue
towards organic pollutants in the water sample, we utilized the
light tube with a wavelength of 450 nm was installed at the central
mineralization efficiency of total crganic carbon (TOC) as a metric.
axis position as the photocatalytic light source. The stainless steel
This assessment involved passing the river water sample through a
wire mesh with the surface-loaded CQDs/ZnO composite nanorod
photocatalytic reactor containing a steel wire mesh loaded with a
array was installed above and below the light tube in a wavy pat-
CQDs/ZnO composite nanorod array, while employing a pure ZnO
tern, with a ripple spacing of 0.1 m. During operation, the catalytic
array as the control. The mineralization efficiency of TOC of river
dye solution (all with a concentration of 20 mg/L) flows through
water sample was test using a Multi N/C 3100 TOC analyzer (Ana-
the degradation system at a rate of 80 mL/min. Initially, the blue
lytik Jena, Jena, Germany).
light tube was not turned on, allowing the solution to undergo dark
reactions at room temperature for 1 h. Subsequently, the blue light
tube was activated to initiate the photocatalytic process. At specific 3. Results and discussion
time points, a small amount of liquid was extracted from the stor-
age reservoir and subjected to spectrophotometric testing after 3.1. Structural characterization
centrifugation. The concentrations of the organic pollutants in
the samples were measured by UV–VIS spectrophotometry using The microscopic morphology of CQDs/ZnO composite nanorod
a UV3100 UV–VIS–NIR spectrophotometer (Shimadzu, Chiyoda, arrays, as well as the pure ZnO array on the steel wire mesh, was
Tokyo, Japan). Testing wavelengths were as follows: 664 nm investigated using SEM, and the results are presented in Fig. 2.
(methylene blue), 618 nm (malachite green), 582 nm (methyl vio- As shown in Fig. 2a, in the absence of CQDs, the hydrothermal reac-
let), 543 nm (basic fuchsin), and 554 nm (rhodamine B). The pho- tion of zinc acetate and ammonia could still form a pure ZnO array
tocatalytic degradation of organic pollutants was measured with on the surface of the steel wire mesh. However, the resulting ZnO
the value of C/C0. Each of the photocatalytic degradation results array displayed poor regularity, with elongated rod-like clusters
presented in this paper represented the average measurement of and numerous irregularly arranged secondary crystals. In contrast,
three samples having the same composition. the introduction of CQDs significantly altered the morphology of
The photocatalytic degradation efficiency of organic pollutants the ZnO-based array on the steel wire mesh. At relatively low CQDs
is evaluated by calculating the Ct/C0 values and could utilize the loading levels (such as CQDs/ZnO-1 and CQDs/ZnO-2 samples), the
Langmuir-Hinshelwood model to depict the kinetics of photocatal- CQDs/ZnO particles on the stainless steel wire mesh were irregu-
ysis, in which the integral is expressed as: larly distributed in a spherical manner, failing to form a regular
1 C0 C0
C array (See Fig. 2b and 2c). With a moderate loading of CQDs, a reg-
t¼ð Þ lnð Þ þ ð1Þ ular hexagonal prism array distribution was achieved (CQDs/ZnO-3
KrK C Kr
sample, see Fig. 2d) on the stainless steel wire mesh. However,
where t represents the duration of radiation exposure, whose unit is excessive CQDs loading led to the occurrence of clustering phe-
min; Ct indicates the concentration of organic pollutants at time t, nomenon in the array, and the array exhibited a cauliflower-like
whose unit is mg/L, whereas C0 denotes its initial concentration, appearance (CQDs/ZnO-4 sample, Fig. 2e). When the loading
whose unit is mg/L; K indicates the equilibrium constant for the amount of carbon reached 20.72 wt% (CQDs/ZnO-5 sample,
adsorption of organic pollutants on the catalyst, whose unit is Fig. 2f), a layer of CQDs/ZnO composite on the steel wire mesh
mol/L; and Kr is equivalent to the maximum rate of the reaction that was clearly observed, but a well-organized nano array was no
can be achieved under the given conditions at the highest possible longer discernible. In summary, CQDs played a crucial role in mod-
coverage, whose unit is mol/(Ls). ulating the morphology of the ZnO-based array. The addition of an
When the initial level of organic contaminants is low, the sec- appropriate amount of CQDs (e.g., CQDs/ZnO-3 sample, see Fig. 2d)
ond term in Eq. (1) becomes signed and can therefore be ignored. effectively reduced the secondary crystallization of ZnO, resulting
Hence, the kinetic simulations employed for photocatalytic degra- in a more uniform CQDs/ZnO array comprising a large number of
dation in this paper utilize the following equation: relatively thick and short hexagonal crystals. This arrangement
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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Fig. 2. (a-f) SEM images of pure ZnO array (a) and CQDs/ZnO-x arrays [x = 1 (b), 2 (c), 3 (d), 4 (e) and 5 (f)] on steel wire mesh; (g-h) The TEM (g) and HRTEM (h) images of
CQDs/ZnO-3 sample.

was found to be beneficial for achieving excellent photocatalytic bond (3345 cm
1), the CAH bond (2926 cm
1), and the CAO bond
performance. (1049 cm
1). When compared with the IR spectrum of pure ZnO,
Fig. 2g and h depict the TEM images of the CQDs/ZnO-3 com- the incorporation of CQDs caused a redshift and narrowing of the
posite. The CQDs/ZnO composite showed a columnar structure, solid ZnAO vibrations at 445 cm
1. This phenomenon could be
and spheroidal particles of CQDs were uniformly distributed on attributed to the reaction between the carboxyl group present in
the surface of ZnO (Fig. 2g). The HRTEM image (See Fig. 2h) dis- the CQDs and the hydroxyl groups on the surface of ZnO.
played both the lattice interleaving of nano ZnO and CQDs. The lat- Fig. 3c–f and Table 2 display the XPS spectra for the CQDs/ZnO-3
tice stripes of 0.531 nm and 0.304 nm corresponded to the (2 0 4) composite and pure ZnO. The results demonstrated the presence of
and (1 1 0) crystallographic planes of hexagonal ZnO, respectively. Zn, C, and O elements. The distinctive peaks at 1021.78 and
Additionally, the (0 2 0) lattice plane of CQDs was observed with 1044.79 eV in the Zn 2p high-resolution spectra corresponded to
a lattice spacing of 0.281 nm. Furthermore, the element mapping the signals of Zn 2p3/2 and Zn 2p1/2, respectively. In the high-
shows that the distribution of CQDs on the ZnO surface is relatively resolution spectra of the O 1s orbital, ZnAO and CAO bonds were
uniform, with a carbon content of 10.26 wt% in the composite (See observed in the CQDs/ZnO composites with distinctive signals at
Fig. 4f). 531.13 eV and 532.79 eV, respectively. For pure ZnO, the O 1s
Fig. 3a illustrates the PXRD patterns of the CQDs/ZnO composite high-resolution spectra had two characteristic peaks at 530.43 eV
and pure ZnO powder. The two PXRD spectra exhibited similar and 532.18 eV, attributed to ZnAO bonding and the hydroxyl group
peaks, while the diffraction peak of CQDs could not be observed on the surface of ZnO, respectively. Additionally, the characteristic
obviously in the CQDs/ZnO composite, mainly due to its relatively peaks at 284.71 eV in the C 1s high-resolution spectra were asso-
low carbon content (10.26 wt%) and low crystallinity. Intense ciated with CAC bonds of CQDs, and the peaks at 286.06 eV and
diffraction peaks could be observed at 2h = 31.76°, 34.41°, 36.25°, 288.72 eV were attributed to the CAO and C@C bonds, respectively.
47.53°, 56.59°, 62.85°, 66.37°, 69.08°, 72.55°, and 76.95°, corre- Combining the FT-IR analysis, it was speculated that the interac-
sponding to the (1 0 0), (0 0 2), (1 0 1), (1 0 2), (1 1 0), (1 0 3), (2 0 0), tion between the carboxyl group of CQDs and the hydroxyl group
(1 1 2), (2 0 1), (0 0 4), and (2 0 2) crystalline planes of the hexagonal on the surface of ZnO resulted in a closer connection between
fibrous ZnO phase (JCPDS card no. 36–1451), respectively. them. The hydroxyl signal on the surface of ZnO vanished, while
In the IR spectrum of the CQDs/ZnO composite shown in Fig. 3b, a signal for the CAO bond was produced simultaneously. These
the characteristic absorption peaks of CQDs were observed. These observations indicated the successful preparation of the CQDs/
included vibrations related to the stretching of the hydroxyl OAH ZnO composite array.

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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Fig. 3. (a-b) The PXRD spectra (a) and FT-IR spectra (b) of the resulted CQDs/ZnO composite array and pure ZnO array. (c-f) The full XPS spectra (c), high-resolution XPS
spectra of Zn 2p (d), O 1 s (e)and C 1 s (f, CQDs/ZnO composite array only) of the resulted CQDs/ZnO composite array and pure ZnO array.

Table 2
XPS peak assignments of CQDs/ZnO composite array and pure ZnO array.

Photocatalysts Element Peak (eV) Surface Group Identification

CQDs/ZnO composite array Zn 2p 1044.79 ZnAO Zn(2p1/2)
1021.78 ZnAO Zn(2p3/2)
C 1s 284.71 C Graphitic carbon
286.06 CAO Presence of an alcoholic or etheric functional group in CQDs.
288.72 C@C Conjugated p-electrons in the aromatic ring of CQDs.
O 1s 531.13 ZnAO Zinc bonded with oxygen.
532.79 CAO CQDs singly bonded with oxygen.
Pure ZnO array Zn 2p 1044.34 ZnAO Zn(2p1/2)
1021.27 ZnAO Zn(2p3/2)
O 1s 530.43 ZnAO Oxygen bonded to zinc
532.18 OAH Hydroxyl groups on ZnO surfaces

3.2. Photocatalytic performance higher than that of the pure ZnO array. Combining our previous
research findings (Jin et al., 2022b) with the results of microscopic
We investigated the photocatalytic activities of the resulting morphology, we observed that a moderate amount of CQDs loading
CQDs/ZnO composite arrays as well as the pure ZnO array in on (approximately 10 wt%), and a uniform hexagonal crystal cluster
steel wire mesh, using methylene blue as the substrate for degra- array could contribute to the enhancement of photocatalytic effi-
dation under 450 nm visible blue light. As depicted in Fig. 4a-c, ciency. In comparison to the CQDs/ZnO-3 sample, other CQDs/
the photodegradation of methylene blue using pure ZnO arrays ZnO composite arrays with excessive or insufficient CQDs loading
without CQDs was very low, exhibiting a degradation efficiency failed to achieve complete degradation of methylene blue pollu-
of only 10.52% in 90 min and a kinetic constant of 0.963  10-3 tants within 90 min of illumination. This outcome could be attrib-
min
1. However, upon introducing an appropriate amount of CQDs, uted to their insufficiently regular particle arrangement and the
the degradation efficiency of the CQDs/ZnO composite on methy- shielding effect caused by excessive carbon content.
lene blue was significantly improved. Among the CQDs/ZnO com- Compared to other CQDs/ZnO powder catalysts, the CQDs/ZnO
posites with different CQDs loadings, the composite with composite array on the stainless steel wire mesh offered the conve-
approximately 10.26 wt% carbon content (CQDs/ZnO-3 sample) nience of easy processing into photocatalytic devices or compo-
exhibited the highest degradation efficiency and achieved com- nents, capable of stable operation over an extended period and
plete degradation of methylene blue within 90 min, showing a adapting to repeated cyclic degradation processes, without the
degradation efficiency of 99.4% and a high kinetic constant of need for cumbersome recycling and reprocessing procedures.
33.5  10-3 min
1. Notably, this kinetic constant was 37 times Fig. 4d illustrates the outcomes of the photocatalyst reusability test

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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Fig. 4. (a-b): The photocatalytic degradation rate within different irradiation times (a) and apparent degradation rate constant (Kapp, b) of CQDs/ZnO composite arrays (CQDs/
ZnO-x, x = 1, 2, 3, 4 and 5) and pure ZnO array to methylene blue under 450 nm blue light. (c) The photographs showing the photocatalytic degradation effects on methylene
blue of CQDs/ZnO composite arrays (CQDs/ZnO-x, x = 1, 2, 3, 4 and 5) and pure ZnO array. (d) The photocatalytic degradation rate of CQDs/ZnO composite array (CQDs/ZnO-3
sample) of the different photocatalytic cycle with 90 min as a working cycle. (e) The PXRD patterns of CQDs/ZnO-3 sample before photocatalysis and after five photocatalysis
cycles. (f) The elemental content of CQDs/ZnO-3 sample before photocatalysis and after five photocatalysis cycles. (g-h) elemental mapping of CQDs/ZnO-3 sample before
photocatalysis (g) and after five photocatalysis cycles (h).

of CQDs/ZnO array (CQDs/ZnO-3 sample). Remarkably, after under- damine B under visible light irradiation, and showed much better
going five successive cycles, the CQDs/ZnO array demonstrated photocatalytic performance than that of pure ZnO array. Similar
remarkable stability in its degradation rate towards methylene to the photocatalytic degradation of methylene blue, the CQDs/
blue, maintaining an efficiency of over 95%. Moreover, the CQDs/ ZnO-3 sample exhibited the highest degradation efficiency among
ZnO composite array ensured its structural and property stability the CQDs/ZnO composites with different CQDs loadings, and
during the photocatalytic process. As evident from the PXRD pat- achieved high degradation efficiency of 100%, 100%, 96.2 % and
terns in Fig. 4e, the CQDs/ZnO composite array before and after five 83.3% for malachite green, basic magenta, rhodamine B and methyl
photocatalytic cycles remained nearly identical. The EDS mapping violet, respectively (See Table 3 and Fig. S3 in ESI). Compared with
revealed that even after five photocatalytic cycles, the CQDs were other previously reported ZnO-based nanocomposite arrays, the
still evenly distributed on the surface of ZnO within the CQDs/ waste rice noodle-based CQDs/ZnO composite nanorod array on a
ZnO composite array. Simultaneously, the carbon content steel wire mesh exhibited higher catalytic efficiency for multiple
remained at 10.08 wt%, indicating no significant loss compared pollutants, capable of visible-light photocatalytic degradation
to the original sample (see Fig. 4f-h). (See Table 3). Additionally, due to the use of inexpensive waste rice
Apart from methylene blue, the resulted CQDs/ZnO composite noodle-based CQDs as components and a steel wire mesh as the
array (CQDs/ZnO-3 sample) also displayed a high efficient photo- substrate, the fabrication cost was significantly reduced, enabling
catalytic degradation effect on other common water-soluble dyes effective utilization of waste resources and displaying high envi-
such as malachite green, methyl violet, basic fuchsin, and rho- ronmental friendliness. Consequently, this approach showed

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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Table 3
Photocatalytic degradation effect of different ZnO-based nanocomposite arrays.

Composite Substrate Excitation source Pollutant Irradiation Degradation Reference

times (min) rate (%)
CQDs/ZnO PVDF A single-channel peristaltic Tetracycline (TC) 70 39.78 (Wang et al., 2023)
pump (100 rpm/min)
CQDs/ZnO Nanofiber membranes An UV lamp (250 W, 365 nm) MB 180 92.08 (Xu et al., 2023)
and natural sunlight
rGO/ZnO rGO nanosheets A UV lamp Cr(VI) 40 47 (Xia et al., 2020)
CuO NPs/ZnO A clean ITO substrate A Xe lamp (CEL-S500) MO 60 44 (Zhang et al., 2019)
rGO@ZnO NH3 processed chemically A UV light source (100 W) Ofloxacin 300 99 (Sharma et al., 2020)
converted rGO nanosheets
CQDs/ZnO array Stainless steel wire mesh Visible light (k = 450 nm) Methylene Blue 90 99.4 This work
based Malachite Green 100
on WRN Basic Magenta 100
Rhodamine B 96.2
Methyl Violet 83.3

promising potential for large-scale industrial wastewater treat- of CQDs, pure ZnO, and the CQDs/ZnO composite are examined and
ment applications. depicted in Fig. 6a. Pure ZnO displayed strong absorption in the UV
Furthermore, the obtained CQDs/ZnO array on the steel wire range (below 384 nm) but showed low absorption in the visible
mesh was applied to real water purification. The total crganic car- region (beyond 420 nm). However, upon introducing CQDs to form
bon (TOC) refers to the total amount of organic substances in the CQDs/ZnO composite, the absorption strength was significantly
water, including dissolved and particulate organic matter. Photo- elevated within the visible spectrum of 400–800 nm. This demon-
catalysts can oxidize organic pollutants into harmless substances strated that the presence of CQDs greatly enhanced ZnO’s ability to
such as CO2 and H2O. Therefore, the mineralization efficiency of utilize visible light energy, resulting in improved energy capture
TOC can be used to measure the degradation capability of photo- and generation of electron-hole pairs when exposed to visible light.
catalysts towards organic pollutants in natural water bodies. A Furthermore, the band gaps of the CQDs/ZnO composite and the
higher mineralization efficiency indicates that organic pollutants pure ZnO array were determined using the Kubelka-Munk method.
are more effectively decomposed and removed during the photo- As depicted in Fig. 6b, the presence of CQDs in the composite sys-
catalytic process. The mineralization efficiency was assessed by tem resulted in a narrower band gap (1.35 eV) compared to the
passing a river water sample through a photocatalytic reactor con- pure ZnO array with a band gap of approximately 3.15 eV. This
taining steel wire mesh loaded with CQDs/ZnO composite nanorod facilitated electron hopping, leading to enhanced photocatalytic
array, while using pure ZnO array as the control. As shown in degradation performance.
Fig. 5a, after a photocatalytic process of 90 min, the CQDs/ZnO XPS valence band spectroscopy was employed to determine the
composite nanorod array achieved a high mineralization efficiency valence band potentials (VB) of both the CQDs/ZnO composite and
of up to 48%, while the pure ZnO array only reached 11%. Moreover, pure ZnO array. As illustrated in Fig. 6c, for pure ZnO, the VB value
the leaching rate of Zn during the 90 min catalytic process was (2.74 eV) exceeded E0 (OH, H+/H2O) (2.38 eV vs. NHE), while its
only 1.2%, indicating that the CQDs/ZnO composite nanorod array conduction band potential (CB) could reach
0.41 eV (ECB = EVB -
on the steel wire mesh could be applied in practical large-scale Eg), which was more negative than E0(O2/O–2) (
0.33 eV vs. NHE).
water purification projects, demonstrating long-lasting effective- This indicated that the photogenerated holes of the ZnO array
ness in degrading water-soluble pollutants (See Fig. 5b). could oxidize H2O, producing hydroxyl radicals (OH), while its
photogenerated electrons could reduce O2, generating superoxide
radicals (O–
2 ). By contrast, the CQDs/ZnO composite array exhibited
3.3. Photocatalytic mechanism
a valence band potential of 2.98 eV, higher than that of ZnO
(2.74 eV), enabling better oxidation of H2O to form photocatalyti-
The light absorption range is a critical factor that influences the
cally OH radicals. By combining its own band gap (1.35 eV) with
catalytic activity of photocatalysts. The UV–VIS absorption spectra

Fig. 5. (a) The mineralization efficiency of TOC of river water sample using CQDs/ZnO composite array and pure ZnO array as photocatalysts within different irradiation
times; (b) the leaching rate of Zn of CQDs/ZnO composite array within different irradiation times.

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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Fig. 6. (a-b) The UV–VIS absorption spectra (a) and Tauc plots (b) for CQDs/ZnO composite, pure ZnO array and CQDs powder; (c-f) The XPS valence band spectra (c),
photoluminescence spectra (d), photocurrent response (e) and electrochemical impedance spectra (f) for CQDs/ZnO composite and pure ZnO array.

the band gap of CQDs (1.64 eV), its CB potential was calculated to leading to more photogenerated electrons for the reduction of O2
be
0.46 eV, which was lower than E0(O2/O–2) (–0.33 eV vs. NHE). and more photogenerated holes for the oxidation of H2O. The pho-
This indicated that the CQDs/ZnO composite array could reduce togenerated holes initiated a reaction with H2O, resulting in the
oxygen in water, generating photocatalytically active O– 2 radicals. production of OH radicals, while the electrons separated on the
The introduction of CQDs significantly improved the defects in CQDs triggered a reaction with O2 to generate O– 2 radicals. The
ZnO photocatalysis, and this positive effect was further confirmed resulting O– 
2 and OH radicals generated could decompose MB to
through fluorescence spectroscopy tests. As show in Fig. 6d, com- CO2 and H2O, thus resulting in excellent photocatalytic activity.
pared to pure ZnO array, the fluorescence emission intensity of
the CQDs/ZnO composite array was notably lower, indicating the
effective modification of CQDs in reducing the recombination of 4. Conclusions
electron-hole pairs. This advantage of the CQDs/ZnO composite
array was also validated by the photocurrent response under visi- In this work, WRN-based CQDs/ZnO composite nanorod array
ble light irradiation on/off (Fig. 6e). It was evident that the pho- on steel wire mesh was designed and syntheized for the first time,
tocurrent of the array was significantly enhanced after the which resulted in a photocatalytic device which offers advantages
introduction of CQDs, implying a faster charge transfer at the elec- of highly efficient photocatalytic degradation, lower production
tron acceptor interface from CQDs to ZnO, thus leading to a more costs, convenient assembly, good recyclability and environmental
efficient separation of electron-hole pairs. Furthermore, electro- friendliness. The result showed that, the incorporation of CQDs
chemical impedance spectra showed that the half-circle diameter derived from WRN played a crucial role in controlling the morphol-
of CQDs/ZnO composite array was notably smaller than that of ogy of the ZnO-based array. This could potentially serve as a cost-
pure ZnO (Fig. 6f), indicating higher electron migration efficiency effective method for controlling the morphology of nanomaterials.
and lower charge transfer resistance. These results were consistent By optimizing the loading of CQDs, the CQDs/ZnO composite array
with the findings from photoluminescence and photocurrent tests. achieved a regular hexagonal prism nanorod array distribution and
The ability of the CQDs/ZnO composite array to generate radi- exhibited highly efficient photocatalytic degradation of various
cals for photocatalysis under light irradiation was investigated organic pollutants, including methylene blue, malachite green,
via electron spin resonance spectroscopy (ESR) employing 5,5- methyl violet, basic fuchsin, and rhodamine B, which showed bet-
dimethyl-1-pyrrole N-oxide (DMPO) as a spin-trapping reagent. ter photocatalytic performance than pure ZnO array. For instance,
As illustrated in Fig. 7a-b, the CQDs/ZnO composite array could in the case of methylene blue, the CQDs/ZnO composite demon-
produce O– 
2 and OH radicals and therefore could degrade aqueous strated a remarkable degradation rate of 99.4% within 90 min, with
organic pollutants. Fig. 7c illustrated a plausible mechanism for a high degradation rate constant of 0.033 min
1. Moreover, the
methylene blue removal over the CQDs/ZnO composite array on composite material could be recycled and reused for five photocat-
steel wire mesh. Under exposure to visible light, the CQDs/ZnO alytic cycles without a significant decrease in its degradation per-
composite array was more susceptible to excitation through pho- formance. Additionally, this CQDs/ZnO composite array could be
togenerated electrons in the CB, thus leaving holes in the VB. The applied to real water purification with high mineralization effi-
accession of CQDs enhanced the absorption of visible light energy ciency. The introduction of CQDs based on WRN to ZnO array could
and resulted in a more effective separation of electron-hole pairs, result in efficient electron-hole pair separation and enable more
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R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Fig. 7. (a-b) DMPO spin-trapping ESR spectra of CQDs/ZnO composite array in water (a) and methanol (b) under visible light irradiation; (c) a diagrammatic representation of
the photochemical catalysis mechanism for CQDs/ZnO composite array on steel wire mesh.

photogeneration electrons to reduce O2 and more photogeneration in large-scale industrial water treatment projects. Therefore, fur-
holes to oxidize H2O, which could cause stronger abilities in pro- ther research is needed to investigate the material’s long-term
ducing O– 
2 and OH radicals and better photocatalytic activity. photocatalytic performance, stability, and corrosion resistance
Compared with other powdered photocatalysts, the implemen- under extended exposure to light. In addition, the potential appli-
tation of the WRN-based CQDs/ZnO composite nanorod array on cation of the obtained CQDs/ZnO composite array in photocatalytic
steel wire mesh in this study effectively addresses the challenges hydrogen production or carbon dioxide reduction still requires fur-
of recycling and assembling powdered catalysts, which hinder ther validation.
their application in continuous, large-scale industrial water purifi-
cation projects. Due to the relatively low cost of WRN-based CQDs CRediT authorship contribution statement
and steel wire mesh, the photocatalytic degradation efficiency of
the CQDs/ZnO composite nanorod array on steel wire mesh offers Ruijie Che: Conceptualization, Methodology, Data curation,
the advantages of being cost-effective, readily available raw mate- Writing – original draft. Biyang Tu: Methodology, Data curation,
rials, and environmentally friendly, making it a potential candidate Writing – original draft. Yining Zhu: Software, Writing – review
for constructing low-cost photocatalytic water purifier. This array & editing. Jiahe Miao: Data curation, Supervision. Xinyan Jin: Val-
is also expected to be used for photocatalytic hydrogen production idation. Shuoping Chen: Funding acquisition, Project administra-
or carbon dioxide reduction. Furthermore, compared with other tion, Supervision, Writing – review & editing.
recycling methods for catering waste, the conversion strategy of
WRN to CQDs/ZnO composite nanorod array on steel wire mesh Declaration of Competing Interest
can add higher value, presenting promising prospects for industri-
alization and providing a novel approach for the recycling of cook- The authors declare that they have no known competing finan-
ing waste. However, the CQDs/ZnO composite nanorod array on cial interests or personal relationships that could have appeared
steel wire mesh reported in this study has not yet been applied to influence the work reported in this paper.
10
R. Che, B. Tu, Y. Zhu et al. Arabian Journal of Chemistry 16 (2023) 105231

Acknowledgments Jiang, Y., Wang, J., Liu, B., Jiang, W., Zhou, T., Ma, Y., Che, G., Liu, C., 2022a.
Superhydrophilic N, S, O-doped Co/CoO/Co9S8@carbon derived from metal-
organic framework for activating peroxymonosulfate to degrade
This work was supported by grants from the National Nature sulfamethoxazole: Performance, mechanism insight and large-scale
Science Foundation of China (No. 51763007), Guangxi Natural application. Chem. Eng. J. 446,. https://doi.org/10.1016/j.cej.2022.137361
137361.
Science Foundation Program (No. 2015GXNSFBA139033), and the
Jin, X., Che, R., Yang, J., Liu, Y., Chen, X., Jiang, Y., Liang, J., Chen, S., Su, H., 2022a.
Sharing Foundation of Guangxi Key Laboratory of Optical and Elec- Activated carbon and carbon quantum dots/titanium dioxide composite based
tronic Materials and Devices (No. 20 AA-9). on waste rice noodles: simultaneous synthesis and application in water
pollution control. Nanomaterials 12, 472. https://doi.org/
10.3390/nano12030472.
Appendix A. Supplementary material Jin, X.-Y., Ying, W.-Y., Che, R.-J., Xiao, P., Zhou, Y.-Q., Liu, Y., Liu, M.-Y., Chen, S.-P.,
2022b. CQDs/ZnO composites based on waste rice noodles: preparation and
photocatalytic capability. RSC Adv. 12, 23692–23703. https://doi.org/10.1039/
Supplementary data to this article can be found online at D2RA03709B.
https://doi.org/10.1016/j.arabjc.2023.105231. Fig. S1: Schematic Li, L.-H., Li, Y.-L., Hong, Y., 2023. New insights into the microalgal culture using
diagram of the photocatalytic reactor; Fig. S2: Pseudo-first-order kitchen waste: enzyme pretreatment and mixed microalgae self-flocculation.
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