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Nanomedicine & Nanotechnology Open Access Research Article 22 min read

A Brief Overview of the Morphological Characteristics of Cain2s4- based Photocatalysts and Their Influence on Boosting the Photocatalytic Behavior

Jabbar ZH*
* Corresponding author
ISSN: 2574-187X  10.23880/nnoa-16000303  Received: March 22, 2024  Published: April 02, 2024
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 45 references
 8 figures
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Keywords
CaIn2S4-Based Composites Morphological Characteristics Photocatalytic Reaction Charge Separation Performance
Abstract

CaIn2S4-based heterojunctions have gained significant attention as robust photocatalysts for sustainable environmental applications like organic degradation and H2 production. This study introduces a brief overview of the morphological characteristics of CaIn2S4-based composites and their effects on their catalytic properties. The fabrication of CaIn2S4- based photocatalysts with hierarchical or nanosheet heterostructures could offer an adequate surface area to volume ratio, enhancing the accessibility of pollutants to the catalyst surface and boosting the photodegradation performance. Moreover, the increased active sites reflect positive effects on the visible-light absorption efficiency. The perfect interfacial contact in the CaIn2S4-based composites facilitated the photocarrier transfer, hampered their reunion rate, prolonged their lifetime, and improved their utilization. The morphological durability and stability of CaIn2S4-based composites are also important variables influencing the photoreaction capacity. Finally, the optimization of surface states and morphological defects can modify the electronic structure of CaIn2S4-based semiconductors, improving their optical properties.

Introduction

The photocatalysis process has emerged as an attractive option to solve the challenges related to the energy crisis, offering the opportunity to harvest renewable solar energy for environmental applications and energy conversion [1, 2, 3, 4, 5, 6]. In recent years, various types of ternary metal sulfides like MgIn2S4 [7, 8], ZnIn2S4 [9, 10], CaIn2S4 [11, 12], and CdIn2S4 [13, 14] have been significantly employed for photocatalytic purposes due to their strong visible-light utilization capacity. In particular, typical ternary sulfide-based semiconductors have been considered efficient photocatalysts owing to their excellent light absorption activity, high stability, good catalytic activity, narrow band gap, and appropriate morphology [15, 16]. Unfortunately, the poor surface area, the rapid charge annihilation efficiency, and the intrinsic photocarrier characteristics obstruct further advancement of the pure CaIn2S4 photocatalysts [17].

In this regard, the construction of CaIn2S4-based heterojunctions and modification of their morphologies can be considered a rich strategy for improving the photocatalytic properties, such as stability and durability, visible-light absorption efficiency, charge carrier dynamics, and specific surface area [18, 19]. It was reported that the doping of hierarchical CaIn2S4 with bimetallic Au-Pt alloy nanoparticles can promote the solar-light harvesting of CaIn2S4-based heterojunction. The expanded absorption activity was linked to the strong surface plasmon resonance (SPR) behavior of Au particles and the scattering effect of Pt particles. Besides, the interaction of metal- support exhibited a prominent impact on the morphology of incorporated metals. The poor cooperation between CaIn2S4 and Au produces larger sizes and well-organized structures, while the strong connection between CaIn2S4 and Au results in smaller sizes and disorganized structures [20]. Zhang W, et al. [21] declared that the morphological modification of CaIn2S4-based photocatalysts by loading hierarchical CaIn2S4 films onto conductive glass substrates (ITO) enhanced the photocatalytic stability via three cycles of methyl orange (MO) degradation. Furthermore, it was detected that the construction of CaIn2S4-based heterojunction with flower- like/flower-like morphology recorded upgraded Cr(VI) reduction. The enhanced charge reunion efficiency of type II CaIn2S4/ZnIn2S4 heterojunction was mainly behind the improved photocatalytic activity [22].

This review introduces a comprehensive yet concise overview of the morphological characteristics of CaIn2S4- based photocatalysts and their pivotal role in enhancing the photocatalytic behavior. By collecting all the latest work dealing with CaIn2S4-based photocatalysts, our study offers key advancements in synthesis strategies and structural and morphological characterization techniques. This argument also discusses the influence of morphological characteristics of CaIn2S4-based photocatalysts on their catalytic properties, like pollutant degradation, solar-light response, charge separation, photostability, and surface area. In other words, our overview focuses on the intricate interplay between the morphology of CaIn2S4-based and photocatalytic activity, supported by sophisticated characterization technologies like SEM, TEM, HRTEM, EDS, XRD, FTIR, XPS, PL, TRPL, EIS, DRS, and DFT calculations. Finally, our work may help the researchers design and develop robust CaIn2S4-based heterojunctions with desirable morphology and catalytic capacity.

Fabrication of CaIn2S4-Based Nanomaterials

Nanomaterials have introduced significant efforts in developing the field of photocatalysis due to their unique properties that result from their large surface area-to- volume ratio, providing numerous active sites, enhancing light absorption, accelerating charge mobility, and promoting pollutant selectivity. The nanomaterials recorded crucial significance in medical applications, such as tissue engineering scaffolds, imaging agents for diagnostics, and targeted drug delivery. The small size and high surface area of nanomaterials enable precise drug targeting, which minimizes side effects. Furthermore, these materials enhance contrast in medical imaging and provide structural support for regenerative medicine approaches, advancing treatment options for various diseases. Besides, nanomaterials were intensively employed in many environmental applications and energy conversions, such as organic degradation, CO2 conversion, hydrogen production, and solar cells. In the catalytic sector, nano-photocatalysts offer plenty of active sites and upgrade the adsorption and photoreaction kinetics, resulting in improved pollutant degradation processes. The researchers manifested various outstanding technologies for the synthesis of nanomaterials, like hydrothermal, solvothermal, sol-gel, co-precipitation, and so on [23, 24, 25, 26, 27].

Among them, the hydrothermal strategy is considered the main and most facile method to fabricate pure CaIn2S4 (CIS) photocatalysts. In brief, 8 mmol of thioacetamide, 4 mmol of In(NO3)3•4.5H2O and 2 mmol of CaCl2•2H2O were dissolved in 30 mL of ethanol and 30 mL of deionized water with continuous stirring for 30 min. After that, the mixture was thermally reacted via a 100 mL Teflon-lined-stainless- steel autoclave at 120 °C for 24 h to produce a flower-like CaIn2S4 microsphere. As shown in Figure 1, the same steps were employed to fabricate Co3O4/CaIn2S4 after the addition of Co3O4 nanoparticles, exhibiting strong interconnection between Co3O4 and CaIn2S4 [28]. Moreover, Yuan W, et al. [29] revealed the fabrication of CaIn2S4 nanosheets via modifying the synthesis procedure above by raising the reaction autoclave temperature to 160 °C and reducing the reaction period to 24 h. In another work, very thin CaIn2S4 nanoparticles decorated RGO sheets were fabricated using the hydrothermal method by extending the reaction time to 24 h.

Figure 1: Synthesis procedure of Co3O4/CaIn2S4 heterojunction via hydrothermal method [28].
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Figure 1: Synthesis procedure of Co3O4/CaIn2S4 heterojunction via hydrothermal method [28].

Crystal Structure of CaIn2S4-based

Different powerful and sophisticated technologies were employed to characterize CaIn2S4-based photocatalysts. The crystal structure of CaIn2S4-based photocatalysts was perfectly identified by X-ray diffraction (XRD). For instance, Zhang P, et al. [30] introduced the XRD patterns of CaIn2S4/ TiO2 composites. As revealed in Figure 1a, the CaIn2S4/TiO2 recorded some XRD peaks at 27.43° (311), 33.40° (400), and 47.90° (440), which belonged to cubic CaIn2S4 (JCPDS no. 31–0272), while the other peaks were attributed to crystal planes of anatase TiO2 (JCPDS no. 21–1272). This implies the good crystallinity and high phase purity of CaIn2S4/ TiO2 composites. The functional group and composition of CaIn2S4-based hybrids can be identified via Fourier-transform infrared spectroscopy (FTIR). Figure 2b depicts the FTIR spectra of ZnIn2S4/Er3+:Y3Al5O12@ZnTiO3/CaIn2S4. The FTIR signals at 681.27 cm–1, 599.98 cm–1, 583.98 cm–1, 557.5 cm–1, and 455.52 cm–1, which consistent with the stretching vibrations Ca-S, In-S, Zn-S, Ti-O, Zn-O in CaIn2S4, ZnIn2S4, ZnTiO3, respectively, verifying the perfect composition of ZnIn2S4/Er3+:Y3Al5O12@ZnTiO3/CaIn2S4 [19].

Besides, the chemical state and the charge transfer of CaIn2S4-based heterojunctions can be demonstrated via X-ray photoelectron spectroscopy (XPS). For example, the XPS survey of CaIn2S4/BiOCl-SOVs revealed the presence of S, In, Ca, Cl, O, and Bi in the CaIn2S4/BiOCl-SOVs composite (Figure 2c). In addition, the high-resolution Ca 2p peaks at 347.26 eV and 351.03 eV belonged to Ca 2p1/2 and Ca 2p3/2 in Ca2+ (Figure 2d). As revealed in Figure 2e, the in 3d signals at 452.09 eV and 444.53 eV were in accordance with in 3d3/2 and In 3d5/2, respectively. Furthermore, the XPS peaks of S 2P were not observed due to the overlapping with Bi 4f peaks (Figure 2f). Importantly (Figures 2g-2i), the positive shifting in binding energies of pure BiOCl (Bi 4f, Cl 2p, and O 1s) compared with CaIn2S4/BiOCl-SOVs demonstrates the electron transfer from CaIn2S4 to BiOCl, creating S-scheme heterojunction system [31].

Figure 2: (a) XRD patterns of CaIn2S4/TiO2 [30], (b) ZnIn2S4/Er3+:Y3Al5O12@ZnTiO3/CaIn2S4 [19], (c-i) XPS spectra of the CaIn2S4/BiOCl-SOVs composite [31].
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Figure 2: (a) XRD patterns of CaIn2S4/TiO2 [30], (b) ZnIn2S4/Er3+:Y3Al5O12@ZnTiO3/CaIn2S4 [19], (c-i) XPS spectra of the CaIn2S4/BiOCl-SOVs composite [31].

Morphology of CaIn2S4-based Heterojunctions

Understanding and optimizing the CaIn2S4-based structure is important to developing powerful CaIn2S4-based heterojunctions for environmental applications. In general, the pure CaIn2S4 photocatalyst can be fabricated in 2D structures (nanosheets, nanoplates, and nanoflakes) and 3D morphology (microsphere or flower-like structure). These morphologies enable the CaIn2S4 catalyst to provide an immobilizing framework for other co-catalysts, creating an efficient CaIn2S4-based heterojunction with favorable surface area, strong interfacial contact, excellent charge transfer efficiency, and robust stability [20, 30, 32, 33, 34]. For instance, the morphologies of SrTiO3/CaIn2S4 were analyzed via scanning electron microscope (SEM) technology. For Figure 3a, the pure CaIn2S4 revealed a micro-sphere shape composed of self-assembled nanosheets. According to Figure 3b, the pure SrTiO3 catalyst appeared to have a particle-like morphology with diameters around 150–200 nm. Obviously, the SrTiO3/ CaIn2S4 composites introduced a flower-like structure loaded with SrTiO3 particles, forming a stable heterojunction system (Figure 3c). The intimate contact in the interfaces facilitates the charge transfer between SrTiO3 and CaIn2S4, constructing an S-scheme heterojunction system (Figure 3d) [35].

Figure 3: (a-c) SEM images of CaIn2S4, SrTiO3, and SrTiO3/CaIn2S4 respectively, (d) S-scheme charge transfer route in the SrTiO3/CaIn2S4 heterojunction [35].
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Figure 3: (a-c) SEM images of CaIn2S4, SrTiO3, and SrTiO3/CaIn2S4 respectively, (d) S-scheme charge transfer route in the SrTiO3/CaIn2S4 heterojunction [35].

Transmission electron microscopy (TEM) provides crucial details about the microstructural features of CaIn2S4- based heterojunctions. Bariki R, et al. [36] reported UiO-66(– NH2)/CdIn2S4/CaIn2S4 heterostructure (UN/CDS/CAS) for efficient asulam degradation and H2 production. For Figure 4a & 4b, the TEM images present the epitaxial growth of ultra- thin CaIn2S4 nanosheets and UiO-66(–NH2) nanospecies onto the 3D hierarchical CdIn2S4 nanorods. As exhibited in Figure 4c, the high-resolution TEM (HRTEM) displayed three lattice spacings at 0.32 nm, 0.265 nm, and 0.195 nm. The first two lattice fringes were in accordance with the (311) and (400) planes of CdIn2S4, and the last one belonged to the (440) plane of cubic CaIn2S4. The presence of CdIn2S4 and CaIn2S4 could be further verified by selected area electron diffraction (SAED). The SAED pattern depicted the same d-spacing values as HRTEM, confirming the powerful hybridization of composite semiconductors (Figure 4d). The real heterojunction among three catalysts generates an internal electric field (IEF) at their interfaces, encouraging the recombination between the feeble electrons in the valence band (VB) of UiO-66(–NH2) and the weak holes in the conduction band (CB) of CdIn2S4 and CaIn2S4, forming boosted dual S-scheme charge transfer pathways (Figure 4e).

In another work, the TEM and HRTEM images in Figures 5a-5c showed the formation of pristine CaIn2S4 with lattice spacings at 0.27 nm (400). After immobilization of CoS2, the CaIn2S4 nanosheets were assembled and displayed flower-like morphology to support CoS2 NPs (Figure 5d-5f). Moreover, the elemental mapping images of CoS2/CaIn2S4 displayed the well distribution of Co, S, In, and Ca elements in the binary catalyst, proving the probability of constructing interfacial heterojunction between the two catalysts (Figures 5g-5k). Brunauere-Emmette-Teller (BET) analysis revealed that these regular depositions of CoS2 NPs can significantly influence the texture properties of CaIn2S4. As shown in Figure 6a, the pure CoS2 nanoparticles exhibited a type III isotherm, which indicates their weak interactions with nitrogen molecules. After dispersing the CoS2 nanoparticles onto CaIn2S4 nanosheets, the CoS2/CaIn2S4 composite manifested type IV with a mesoporous texture (Figure 6b).

Besides, the introduction of CoS2 NPs amazingly improved the surface area of CaIn2S4 from 4.08 to 72.63 m2/g [37]. The stronger surface area provides more active sites for adsorption and photoreaction, thereby upgrading catalytic performance [38, 39].

Figure 4: (a-b) TEM images, (c) HRTEM images, (d) SAED pattern, and (e) dual S-scheme mechanism of the ternary UiO-66(– NH2)/CdIn2S4/CaIn2S4 heterojunction [36].
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Figure 4: (a-b) TEM images, (c) HRTEM images, (d) SAED pattern, and (e) dual S-scheme mechanism of the ternary UiO-66(– NH2)/CdIn2S4/CaIn2S4 heterojunction [36].
Figure 5: (a-c) TEM and HRTEM images of pure CaIn2S4, (d-f) SAED, TEM, and HRTEM images of the CoS2/CaIn2S4 composite, (g-k) Elemental mapping of the CoS2/CaIn2S4 hybrid [37].
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Figure 5: (a-c) TEM and HRTEM images of pure CaIn2S4, (d-f) SAED, TEM, and HRTEM images of the CoS2/CaIn2S4 composite, (g-k) Elemental mapping of the CoS2/CaIn2S4 hybrid [37].

Furthermore, it was discovered that the random scattering of CeO2 NPs onto hierarchical CaIn2S4 could increase the BET surface area from 72.75 m2/g to 75.93 m2/g (Figure 6c). This implies that the hybridization of CeO2 NPs with CaIn2S4 can provide excessive active sites to upgrade the photocatalytic degradation performance [40]. On the other hand, the combination of the CaIn2S4 catalyst with other photocatalysts or plasmonic metal NPs can create synergistic efforts, further enhancing the catalytic performance. In other words, the hierarchical and nanosheet morphologies supplied appropriate effective sites to incorporate with other co-catalysts, resulting in improved degradation performance, charge separation efficiency, stability, light harvesting activity, stability and recyclability, and mass transfer and reactant accessibility [41, 42]. For example, Li J, et al. [43] demonstrated that the interfacial contact between the plasmonic Au NPs and CaIn2S4 nanosheets could enhance the methylene blue degradation rate and electron transfer from Au NPs to CaIn2S4 by surface plasmon resonance (SPR) effect (Figure 6d-6f).

Figure 6: (a-b) Nitrogen adsorption isotherm and pore size distribution of the CoS2/CaIn2S4 composite [37], (c) structure of the CeO2/CaIn2S4 composite [40], (d-e) photocatalytic performance, degradation kinetics of plasmonic, and photocatalytic mechanism of MB degradation over Au/ CaIn2S4 composites [43].
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Figure 6: (a-b) Nitrogen adsorption isotherm and pore size distribution of the CoS2/CaIn2S4 composite [37], (c) structure of the CeO2/CaIn2S4 composite [40], (d-e) photocatalytic performance, degradation kinetics of plasmonic, and photocatalytic mechanism of MB degradation over Au/ CaIn2S4 composites [43].

In another investigation, the electrospinning method was employed to fabricate In2O3 fibers with a diameter of approximately 50 nm (Figure 7a). As illustrated in the morphological images of Figure 7b, the CaIn2S4-based nanofibers were developed by growing CaIn2S4 nanofoils onto In2O3 fibers to generate a type II heterojunction system. This strong interaction can stimulate charge migration and separation in the type II heterojunction. The density functional theory (DFT) was employed to identify the electronic structures of In2O3 and CaIn2S4 to demonstrate the boosted photocarrier separation of CaIn2S4-based nanofibers. As revealed in Figures 7c & 7d, the CBs of both semiconductors consist of In 5s orbits, while the VBs are composed of O 2p and S 2p orbits for In2O3 and CaIn2S4 respectively. Although their CBs originated from in atoms, the CBs have distinct band dispersions for In2O3 and CaIn2S4. It can be detected that photoinduced electrons in In2O3 revealed higher mobility than those in CaIn2S4, proving the electron drifting from In2O3 to CaIn2S4 in a type II heterojunction system (Figure 7e) [44].

Figure 7: (a) synthesis procedure of CaIn2S4-based nanofibers, (b) SEM, TEM, and HRTEM images of CaIn2S4/In2O3 nanofibers, (c-d) Electronic structures of In2O3 and CaIn2S4 using DFT calculations, (e) type II heterojunction mechanism of CaIn2S4/In2O3 nanofibers [44].
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Figure 7: (a) synthesis procedure of CaIn2S4-based nanofibers, (b) SEM, TEM, and HRTEM images of CaIn2S4/In2O3 nanofibers, (c-d) Electronic structures of In2O3 and CaIn2S4 using DFT calculations, (e) type II heterojunction mechanism of CaIn2S4/In2O3 nanofibers [44].

The morphological features of hierarchical CaIn2S4- based photocatalysts can promote light utilization activity and scattering effects [12]. For example, diffuse reflectance spectroscopy (DRS) spectra of UiO-66(–NH2)/CdIn2S4/ CaIn2S4 (UN/CDS/CAS) hybrids recorded a dramatic shift in light utilization wavelength compared with pure samples (Figure 8a). Besides, the significant reduction in the photoluminescence (PL) spectra indicates that the hierarchical morphology can also minimize the recombination rate of UN/CDS/CAS (Figure 8b). As exhibited in Figure 8c, the time resolved photoluminescence spectra (TRPL) of UN/CDS/CAS obtained a notable reduction in PL lifetime, recording rapid separation of photocarriers in the flower-like UN/CDS/CAS structure [36]. In another example, the transient photocurrent response (TPR) of CaIn2S4/BiOCl- SOVs offered the strongest TPR emission, indicating that the hierarchical structure facilitates charge carrier separation (Figure 8d). Furthermore, electrochemical impedance spectroscopy (EIS) of the same composite showed the smallest arc radius, implying the limited interfacial resistance of the photocarrier in the CaIn2S4/BiOCl-SOVs hybrid (Figure 8e) [31].

Morphological photostability and structure durability are also additional key parameters that influence catalytic activity. Efficiently constructed hierarchical and nanosheet structures can introduce enhanced durability under photodegradation reactions and enable simple recycling of the catalyst for multiple photoreaction cycles [15]. Gao X, et al. [45] stated that the hierarchical CaIn2S4 can act as a robust immobilizing framework for Sr-SnS2, which reflected excellent stability and reusability in five successive recycling of reduction Cr(VI) (Figure 8f). Furthermore, the authors revealed that the perfect combination of two morphologies can stimulate photocarrier migration in the S-scheme pathways (Figure 8g). In addition, the 3D charge density difference was provided to further investigate the distribution of photocarriers at the interfaces of hierarchical CaIn2S4/Sr-SnS2. As revealed in Figure 8h, the blue area depicts the electron consumption on the surface of Sr-SnS2, while the yellow area indicates the electron accumulation on the surface of CaIn2S4, which suggests the establishment of IEF between CaIn2S4 and Sr-SnS2, improving the S-scheme mechanism.

Figure 8: (a-c) DRS, PL, and TRPL of hierarchical UN/CDS/CAS [36], (d-e) TPR and EIS spectra of flower-like CaIn2S4/BiOCl- SOVs [31], (f-h) cycling experiments, S-scheme diagram, and DFT charge difference density diagram of hierarchical CaIn2S4/ Sr-SnS2 [45].
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Figure 8: (a-c) DRS, PL, and TRPL of hierarchical UN/CDS/CAS [36], (d-e) TPR and EIS spectra of flower-like CaIn2S4/BiOCl- SOVs [31], (f-h) cycling experiments, S-scheme diagram, and DFT charge difference density diagram of hierarchical CaIn2S4/ Sr-SnS2 [45].

Conclusion

This review introduces a novel discussion about the morphological influence of CaIn2S4-based heterojunctions on their catalytic properties. The hydrothermal strategy is considered the main and most facile method to fabricate pure CaIn2S4 and their composites. The crystal structure of CaIn2S4-based photocatalysts was perfectly identified by XRD, which implied the good crystallinity and high phase purity of CaIn2S4/TiO2 composites. The functional group and composition of CaIn2S4-based hybrids can be identified via FTIR analysis. The chemical state and the charge transfer of CaIn2S4-based heterojunctions can be demonstrated via XPS spectra. The positive and negative shifting in binding energies of pure CaIn2S4 compared with composites can give an important hint about the electron transfer in the CaIn2S4- based heterojunctions. In previous studies, the pure CaIn2S4 photocatalysts were fabricated in 2D structures (nanosheets, nanoplates, and nanoflakes) and 3D morphology (microsphere or flower-like structure). The morphological characteristics of CaIn2S4-based heterojunction can play a crucial role in improving the photocatalytic capacity by influencing factors, such as stability and durability, light harvesting efficiency, charge carrier dynamics, and specific surface area. Controlling the morphology of CaIn2S4-based heterojunctions through the synthesis procedures is helpful to optimize the catalytic capacity of CaIn2S4-based nanomaterials for various environmental applications, including energy conversion, pollutant degradation, and water splitting.

Acknowledgements

“The authors are grateful to Al-Mustaqbal University College, Building and Construction Techniques Engineering Department for their support”.

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@article{jabbar2024,
  title   = {A Brief Overview of the Morphological Characteristics of Cain2s4-
based Photocatalysts and Their Influence on Boosting the
Photocatalytic Behavior},
  author  = {Jabbar ZH},
  journal = {Nanomedicine & Nanotechnology Open Access},
  year    = {2024},
  volume  = {9},
  number  = {2},
  doi     = {10.23880/nnoa-16000303}
}
Jabbar ZH (2024). A Brief Overview of the Morphological Characteristics of Cain2s4-
based Photocatalysts and Their Influence on Boosting the
Photocatalytic Behavior. Nanomedicine & Nanotechnology Open Access, 9(2). https://doi.org/10.23880/nnoa-16000303
TY  - JOUR
TI  - A Brief Overview of the Morphological Characteristics of Cain2s4-
based Photocatalysts and Their Influence on Boosting the
Photocatalytic Behavior
AU  - Jabbar ZH
JO  - Nanomedicine & Nanotechnology Open Access
PY  - 2024
VL  - 9
IS  - 2
DO  - 10.23880/nnoa-16000303
ER  -