key: cord-0990541-cxvixjvf
authors: Panchal, Priyanka; Meena, Poonam; Nehra, Satya Pal
title: A rapid green synthesis of Ag/AgCl-NC photocatalyst for environmental applications
date: 2021-01-04
journal: Environ Sci Pollut Res Int
DOI: 10.1007/s11356-020-11834-5
sha: 07da02c2a65ce49e3624c11d44a92654aed8fc69
doc_id: 990541
cord_uid: cxvixjvf

The present study focuses on extract-mediated Ag nanoparticles (NPs), AgCl-NPs, and Ag/AgCl nanocomposites (NCs) as photocatalysts along with its antimicrobial and dye degradation activities. The synthesis of these NPs and NCs was performed by using Azadirachta indica plant fruit extract and analyzed using UV-Vis spectroscopy to confirm the synthesis and band gap of these NPs and NCs, X-ray diffraction (XRD) to determine its size and crystalline nature. Fourier transform infrared spectroscopy (FTIR) to discern phytochemicals, responsible for the reduction and capping of the synthesized NCs. Scanning electron microscopy analysis (SEM), transmission electron microscopy analysis (TEM), and energy dispersive X-ray (EDX) spectroscopy analysis were performed to validate the morphology and presence of silver and chloride percentage in the composites. Later, these NPs and NCs were used for their potential role in photocatalytic degradation of methylene blue dye and antibacterial activity against Escherichia coli and Staphylococcus aureus of human pathogen. The prepared Ag/AgCl-NCs exhibited an enhanced photocatalytic and antibacterial activities in comparison with pure Ag and AgCl nanomaterials. However, green-synthesized NPs and NCs played dual roles as a photocatalyst and antibacterial agent in various biomedical and industrial sectors. Moreover, we found that it might be a hot research in many other environmental applications in upcoming days. [Image: see text]

Undoubtedly, semiconductor photocatalyst plays an important role with a good potential for different environmental applications that include mineralization of organic pollutants, water disinfection, hydrogen storage, sensors, photoelectric and biomedical, etc. (Alivisatos 1996; Hoffmann et al. 1995; Khan et al. 2016; Khorrami et al. 2019; Saravanan et al. 2015) . Water contamination has been a huge problem in recent years, only 10% of the contaminated water gets purified, and the remaining contaminated water gets released into water bodies as such. If any action not taken, current water supply will decrease by one-third within a couple of decades (Sushmaand Richa 2015; William and William 2015; Ye et al. 2019) . Pollutants that are released from home, commercial, industries, and agricultural practices are the key sources of water pollution resulting to organic, inorganic, pathogenic, and non-pathogenic microorganisms, which leads to waterborne pathogens such as protozoan, cholera, intestinal flu, and respiratory infectious agents; these are then transmitted by the fecal-oral route. As drinking water is one of the medium for transmission and causes problems to health and can even lead to death (Cui et al. 2017; Theron and Cloete 2002; Sun et al. 2019) , according to the WHO, each year, about 2.2 million populace dies due to diarrhea in which 90% are children, especially in developing countries. For curbing these issues, we are required to provide safe water to everyone (Cui et al. 2017; WHO guidelines 2011; Jin et al. 2014) .

Here, the appearance of color in water release from different industries and other areas are also huge issue for the environment as this effluent waste contains heavy metals, organic toxins, lubricants, nutrients, dye solids, chemicals, nutrients from crop fields, house waste, hospital waste, etc. (Bhatia et al. 2017; Gupta et al. 2015; Moradia et al. 2020; Padhi 2012) . As textile industries consume dyes that are generally Responsible Editor: Sami Rtimi in the concentration range of about 10-200 mg L −1 and approximately more than 10-15% dyes from the textile, paper, carpet, leather, distillery, and printing industries are released into natural streams and rivers, this creates severe problems as their color stops the progress of re-oxygenation in water by cutting off the dissemination of sunlight. This can lead to the environmental changes and the disruption to the natural balance of the ecosystem (Ashbolt 2004; Araújo et al. 2018; Hongyuan et al. 2019; Páez et al. 2018; Ye et al. 2019; Paul and Nehra 2020) . So, it is the responsibility of every person from their respective field to contribute to improve water quality in all possible manners. As new diseases get developed regularly, if we do not get solution on time for older disease, newer one gets to generate and easy to break our immune system. Corona virus is that type of disease which is generally proving deadly on people already infected with medical problems like cardiovascular, respiratory infection, etc. and you know that most of diseases occur due to direct/indirect use of contaminated water (Guan et al. 2020; Shanmugana et al. 2020; WHO guidelines 2020) .

To overcome this major problem, various physical, chemical, and biological methods have been used to investigate the semiconductor photocatalyst. However, these physical and chemical methods require multi-step processing and might prove toxic to the environment (Kumari and Singh 2016; Jamdagni et al. 2018; Malik et al. 2014) . Thus, there is a requirement for developing a procedure which will be able to achieve the synthesis of an innovative photo-catalyst in nano-structured form for removal of contamination from waste water (Alishah et al. 2016; Pattanayak et al. 2015; Rashidi and Islami 2020; Saad et al. 2017) . In recent years, medicinal plant extract-mediated green synthesis of semiconductor-based photocatalyst gained more attention due to their eco-friendly nature and cost effectiveness. It acts as a reducing and stabilizing agent, and there is no requirement of special areas of synthesis as well. Moreover, plants give a more desirable platform for the synthesis of nanoparticles and are claimed to acquire profit such as their broad variety of natural phytochemicals present in plant extract alkaloids, terpenoids, phenols, flavonoids, tannins, and quinines, etc.; they are free from toxicant chemical. Furthermore, as associate simply offered, safe to use (Ahmad et al. 2015; Bhatia et al. 2017; Jamdagni et al. 2018; Kumari and Singh 2016; Malik et al. 2014; Stamplecoskie and Scaiano 2012) .

Nowadays, surface plasmon resonance (SPR) has gained a lot of attention in the field of photocatalysis to enhance the illuminated light reaction of photocatalysts. Several metals like Ag, Au, and Pd have SPR that overlaps with the solar light (Ge et al. 2011; Jiahui and Verma 2012; Zhou et al. 2012; Zada et al. 2020 ). Among the various metallic ions, Ag is widely used as inorganic nanoparticles with huge applications, as silver (Ag) is the most appropriate selection during dopant due to its tremendous chemical stability, electronic, and optical properties. When Ag nanoparticles lie on the surface photocatalyst, it can considerably increase the interfacial charge-migration kinetic due to SPR (Malik et al. 2014; Nguyen et al. 2020; Panchal et al. 2019a ). In the current study, we have reported that the synthesis of Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs has been shown to possess better photocatalytic as well as antibacterial activity potential as compared with the ionic form of the metal, making them one of the most popular metal nanoparticles to be used in photocatalytic and antibacterial applications.

Reagents Silver nitrate and sodium chloride are analytically pure, procured from Merck India and used as it was received without further purification.

The Azadirachta indica plant fruits were brought from herbal garden of South Point College of Pharmacy. To eliminate dirt and contaminants, collected plant fruits were thoroughly washed with distilled water. Washed plant fruits about 20 g were put in Brosile beaker containing 40 mL distilled water. The color changed from transparent to yellow after heating at room temperature (RT) for 30 min. Then, extract was cooled at RT and filtered with filter paper. Then, the collected extract was kept in the refrigerator for further use. The collected plant extract has been shown in Fig. 1 Rashidi and Islami 2020) .

Ag-NP synthesis A total of 0.1 mM AgNO 3 had been used as precursors for green synthesis of Ag-NPs. The solution of precursors was prepared in 250-mL containers by continuously stirring for 1 h using with a magnetic stirrer at RT. Then, 40 mL distilled water was taken and gradually added 10 mL at a time while continuously stirring. The color changed from white to yellowish brown confirming the initial synthesis of Ag-NPs. Then, resultant solutions were cooled at RT and centrifuged at 4000 rpm for 10 min separating the solid particles and washing with alcohol to remove impurities and then kept in hot air oven for drying at 80°C/8 h. A black sample in powder form was obtained at the end of the procedure .

AgCl and Ag-modified AgCl-NC synthesis AgCl-NPs and Ag/ AgCl-NCs were synthesized using 0.1 mM silver nitrate dissolved in 40 mL distilled water and container labeled with A. Then, 0.3 mM silver nitrate was added with 40 mL distilled water in container B, with the addition of 10 mL fruit extracts (Azadirachta indica.) in both containers A and B. Then, the solution in both the containers was continuously stirred for 1 h at RT. After the completion of stirring period, NaCl (0.1 M) was added to both the containers A and B, respectively, again stirred for 1 h. A color change from white to yellowish gray confirmed the initial synthesis of AgCl-NPs and dark grayish color for Ag/AgCl-NCs. Then, resultant solutions were centrifuged at 4000 rpm for 10 min, separated the solid particles, and washed with alcohol to remove contaminants and then kept in hot air oven for dry at 80°C/8 h. For AgCl-NPs, light gray color and dark gray color for Ag/AgCl-NCs in powder form were obtained at the end of the procedure .

Photocatalyst characterizations Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs were characterized by various analytical t e c h n i q u es s uc h a s U V -V i s s p ec t r o p ho t om e t e r (Lambda750 model of Perkin Elmer in the range of 300-800 nm range in reflection mode), X-ray diffraction (Bruker D8 Advance equipped with CuKα radiation (1.5406 A°), 2θ = 20°-80°), FTIR (Perkin Elmer FRONTIER (250-8000 cm −1 ) using the standard KBr disk method), SEM with EDS (EVO LS 10), and TEM (Tecnai 20 G2 300 KV, STWIN). Important techniques used for the characterization of green-synthesized NPs/NCs are summarized in Table 1 . Antibacterial performances Synthesized catalyst was used for antimicrobial activities by a zone of inhibition method. In this experiment, two pathogenic bacteria (s) were used (E. coli and S. aureus); prior to testing, all glass wares were sterilized in an autoclave for 20 min to make it contamination free. A total of 100-μL bacterial suspension was spread on each sterilized agar media plates (E. coli a, b, and c) and (S. aureus a, b, and c) spread equally by sterilized spreader. After that, using of sterilized cork borer makes 5 mm diameter well in each plate and added 10-mg catalyst solution of each prepared sample (E. coli, a-Ag-Nps, b-AgCl-NPs, and c-Ag/AgCl-NCs and S. aureus a-Ag-NPs, b-AgCl-NPs, and c-Ag/AgCl-NCs). Then, plates were left in same condition for 15 min in laminar air flow for proper diffusion of catalyst with agar. Afterward, all plates were kept in an incubator at 37°C/16 h. After completion of incubation time, plates were removed from the incubator and kept in laminar air flow and zone of inhibition calculated by a metric rule method (Dai et al. 2017; Panchal et al. 2019a, b; Trinh et al. 2015; Villanueva et al. 2015) .

Dye degradation performances Methylene Blue (MB) dye decomposition performances were done under direct solar light and confirmed by using UV-Vis spectrophotometer. 10 mg of green-synthesized photocatalysts was added in 100-mL solution having 10 ppm MB dye in three different conical flasks labeled with a-Ag-NPs, b-AgCl-NPs, and c-Ag/AgCl-NC. Prior to exposure under sunlight, all three conical flasks carrying solution of a-Ag-NPs, b-AgCl-NPs, and c-AgCl-NC were stirred without solar light for 30 min to make adsorptiondesorption balance of photocatalyst with dye. After that, all samples were kept under solar light irradiation, and at the same time of gap, 5-mL sample was collected and centrifuged to eliminate the solid substances. The decomposition dye solution spectra were recorded using UV-Vis spectrophotometer. The photocatalytic decomposition ability was measured by the following equation: percentage of degradation = (C 0 − C t ) / C 0 × 100% (Paul and Nehra 2020; Paul et al. 2019a, b; Panchal et al. 2019b Panchal et al. , 2020 .

DRS analysis The UV-visible light DRS were calculated to consider the optical characteristics of Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs as shown in Fig. 2 . Prepared samples of Ag/AgCl-NCs are noticeable absorption band edge at 498 nm (Sun et al. 2014) , respectively, in evaluation to the absorption edge of Ag-NPs and AgCl-NPs at 482 and 460 nm (Ghosh et al. 2012; Hasan and Asmat 2017) . Optical band gap for all samples has been investigated with the equation: α = A (hν − E g ) n / hν, where α = absorption coefficient as shown in the inset of Fig. 2 . The energy band gap identified as 2.53, 2.61, and 2.85 eV for Ag/AgCl-NCs, AgCl-NPs, and Ag-NPs, respectively, as shown in the inset of Fig. 2a , b, and c (Wang et al. 2010; Yingying et al. 2018) . Ag/AgCl-NCs showed the stronger absorption in direct solar light, due to the maximum metallic Ag nanoparticles present on the surface of Ag/AgCl-NCs which enhance the absorption characteristics of surface plasmon resonance (Jiahui and Verma 2012; Wang et al. 2016; Zhou et al. 2012; Zada et al. 2020 ). Thus, the increased absorption region of Ag/AgCl-NCs is indicative of favoring the more production of e − h + pairs, which could enhance its photocatalytic activity (Ghosh et al. 2012; Wang et al. 2016; Ye et al. 2012; Yingying et al. 2018) .

XRD studies The initial synthesis of Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs can be authenticated by observing the color changed. XRD analyses of Ag-NPs, AgCl-NPs, and Ag/ AgCl-NCs were analyzed using X-ray diffractometer. X-ray diffraction peaks were visualized at 2θ value = 38.16°, 44.44°, 64.72°, and 77.52°which corresponded to 111, 200, 220, and 311 which confirmed the synthesis of silver (JCPDS file no 04-0783) as shown in Fig. 3a (Jamdagni et al. 2018; Kumari and Singh 2016) . Another six distinct diffraction peaks at 2θ = 28.13°, 32.10°, 46.50°, 55.06°, 57.75°, and 68.16°c orresponded to 111, 200, 220, 311, 222, and 400 lattice planes, which confirmed that the synthesis of AgCl-NPs (JCPDS file: 31-1238) can be seen in Fig. 3b (Araújo et al. 2018; Alishah et al. 2016; Panchal et al. 2019a ). It can be seen that no Ag peak was noticed here. The reason may be that the quantity of Ag-NPs formed at the surface of the AgCl was low in concentration for detection.

The X-ray diffraction peaks of Ag/AgCl-NCs noticeably showed that the cubic structure of Ag with lattice constant a = 4.0861 A (JCPDS file: 65-2871) similar in the cubic structure of AgCl with lattice constant a = 5.5491 A (JCPDS file: 31-1238) as observed in Fig. 3c (Hasan and Asmat 2017; Sun et al. 2014; Wang et al. 2010) . In Ag/AgCl-NCs, increasing the Ag proportion showed different peaks of Ag, whereas that of Cl decreases (Wang et al. 2016) . No other peak could be recognized here, which proved the purity of Ag/AgCl-NCs. The sharp and fine diffraction peaks expose the well crystalline nature of particles (Anandalakshmi et al. 2016 ; Das et al. FTIR studies FTIR studies were used for identification of possible biomolecules present in plant extract which were important for reducing, capping, and stabilization during synthesis of Ag/AgCl-NPs. As shown in Fig. 4 , peak appeared at 3446 cm −1 which can be recognized to hydrogen bonded O-H functional group of alcohols, phenols, and the occurrence of amines N-H of amide (Anandalakshmi et al. 2016; Shaomin et al. 2017; Wang et al. 2019; Yingying et al. 2018 ). The -OH is derived from water-soluble phenolic compounds in the plant extract. While the peak vibrations at 2923 cm −1 can be attributed to C-H stretching (Anandalakshmi et al. 2016; Wang et al. 2016) , the peak at 1630 cm −1 is related to a C-OH bond of protein arising from plant extract (Yingying et al. 2018 ). In the peak at 1386 cm −1 related to CO, the peak at 1098 cm −1 was recognized to C-O-C bonds in polysaccharides, which are usually found in the region between 1200 and 900 cm −1 (Shaomin et al. 2017; Ye et al. 2012 ). The peak observed at 835.85 cm −1 can be approved to the Ag-Cl Overall, FTIR data indicated that proteins are key components that drive the bioreduction and stabilization of Ag/AgCl-NCs (Anandalakshmi et al. 2016; Das et al. 2010; Shen et al. 2014; Shaomin et al. 2017; Ye et al. 2012) .

SEM and EDX studies Surface morphological study and percentage of elemental composition presented in greensynthesized NPs and NCs were confirmed by SEM and EDX studies. In pure Ag-NPs, a rough aggregated NP surface appeared which may be due to the presence of other elements that may have effects on bioreduction of Ag + ; it can be seen in Fig. 5a . After deposition of Cl, it affects the surface morphology of green-synthesized AgCl-NPs, thus decreases the roughness, and little NPs appeared in a closely packed cubelike structure shown in Fig. 5b. In Fig. 5c , Ag/AgCl-NCs appeared bright cubic in shape (Ghosh et al. 2012; Shen et al. 2014; Wang et al. 2010; Yingying et al. 2018) . Elemental propagation of the synthesized samples was observed by using EDX analysis that can be seen in Fig. 5d . EDX observation proved the occurrence of used elements: Ag and Cl within the Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs, and table shows the weight percentage in inset of Fig.  5d .

The morphological features of prepared samples were explored using TEM analysis. Metallic Ag-NPs can be observed at the surface of Ag/AgCl-NCs with the clear formation of cubic shape NCs with 10 to 15 nm in size. Two different particles can be seen in Fig. 6c , one is small in spherical and other large in cubic shape. The presented images confirmed that Ag-NPs are spherical in shape with 22 to 30 nm in size as shown in Fig. 6a and AgCl-NPs are in cubic shape with 18 to 20 nm in size as seen in Fig. 6b . Interestingly, the boundaries of AgCl-NCs are decorated through Ag-NPs (Kateryna and Matthias 2018; Zhikun et al. 2014; Jianhua et al. 2019) .

Antibacterial studies The antibacterial activities of greensynthesized nanoparticles and nanocomposites were confirmed by the well diffusion method. The pathogenic E. coli and S. aureus strains were used as a test. A zone of inhibition found during an experimental test is mentioned in Table 2 . In presenting work, it was found that bright cubic shape Ag/ AgCl-NCs showed highest antibacterial activities in case of E. coli and S. aureus as compared with pure Ag-NPs and AgCl-NPs as shown in Fig. 7a , b, c. Due to the smaller size, there is a high surface volume ratio and the specific shape of synthesized NCs raised more reactive oxygen species having a greater ability to disturb bacterial cell membrane and directly effect the bacterial metabolism system. After that, bacteria have no ability to further multiply and nanoparticles kill the bacteria (Knuuti et al. 2013; Kabir et al. 2020; Lisdat and Schafer 2008; Nguyen et al. 2020; Panchal et al. 2019b) .

Dye decomposition studies Green-synthesized Ag-NPs, AgCl-NPs, and Ag/AgCl-NCs were used here as a photocatalyst towards organic methylene blue dye decomposition. Experimental test performed under direct solar light irradiation and was confirmed by UV-Visible spectrophotometer. It was found that a bright cubic like nanostructured Ag/ AgCl-NCs showed the greater degradation efficiency of MB dye in 80 min 92.5%, mainly due to the well and definite Ag/AgCl-NCs 10 mg 24 nm 26 nm Fig. 7 Antibacterial studies-E. Coli (a-pure Ag-NPs, b-AgCl-NPs, and c-Ag/AgCl-NCs) and S. aureus (a-pure Ag-NPs, b-AgCl-NPs, and c-Ag/AgCl-NCs) morphology can be seen in Fig. 8c as compared with pure Ag-NPs 77.44% and AgCl-NPs 51.46% in 80 min as shown in Fig. 8a , b. For all samples, MB dye decomposition efficiency, dye decomposition percentage, and apparent rate constant were calculated for a time period of about 80 min and have been compared as shown in Fig. 9a , b, c (Araújo et al. 2018; Dai et al. 2017; Rashidi and Islami 2020) .

Mechanism Antibacterial inactivation and dye decomposition activities totally depend on synthesized nanostructures' size, morphology, crystalline nature, and band gap (Paul and Nehra 2020; Paul et al. 2019a, b; Rashidi and Islami 2020) .

In antibacterial case Bacterial inactivation generally occurred by breaking the cell wall which inhibit the bacterial metabolism system due to which bacteria do not have the capacity to perform any other synthesis like proteins or nucleic acid, which makes changes in membrane permittivity and enzyme formations (Anandalakshmi et al. 2016; Ghosh et al. 2012; Panchal et al. 2019a, b) . In this work, synthesized NPs and NCs produce reactive oxygen species (ROS) in the presence of dissolved oxygen, leading to production of large number free radical . Then, ROS create disturbances in cell membrane due to bacterial internal cell function and formation like (DNA, mitochondria, lipid, protein Table 1 . Due to specific particle morphology, small size and lower band gap proved by XRS, DRS, TEM analysis (Anandalakshmi et al. 2016; Ghosh et al. 2012; Lisdat and Schafer 2008; Panchal et al. 2020; Shen et al. 2014) .

In dye decomposition case Here, Ag/AgCl-NCs showed the excellent dye decomposition efficiency 92.5% in 80 min as shown in Figs. 8c and 9a , b, c as compared with other synthesized NPs as shown in Fig. 8a and Ag-NPs 77.44% and AgCl-NPs = 51.46% shown in Fig. 8b in 80 min. Ag/AgCl-NCs with low band gap 2.53 when comes into contact with illuminated light are activated and attributed to the SPR effect of Ag-NPs then produced electrons, hole pairs. Then, e− might be moved to molecular O 2 to produce ·O 2 − , and photoinduced h + moved to the AgCl surface coincides to the oxidation of Cl − to Cl 0 . Both ·O 2 − and Cl 0 can act as ROS to oxidize MB. At the same time, Cl 0 would be reduced to Cl − again. Consequently, the Ag/ AgCl-NCs showed large and stable photocatalytic efficiency for the degradation of MB (Chung et al. 2014; Hayyan et al. 2016; Knuuti et al. 2013; Paul et al. 2019a, b; Panchal et al. 2020; Sakamoto et al. 2009 ). Ag/AgCl-NCs bacterial inactivation and dye decomposition mechanism are shown in Fig.  10a , b. Antimicrobial activity and photocatalytic potential of green-synthesized Ag/AgCl-NCs against E. coli, Staphylococcus aureus, and MB dye degradation have been in comparison with previous published work in Tables 3 and 4 .

In this work, cubic structure like Ag/AgCl-NCs is successfully synthesized by the use of plant extract. The XRD graph shows the crystalline nature. SEM and TEM morphology showed that spherical shape Ag-NPs properly deposited on the upper surface of Ag/AgCl-NCs. This exhibits huge surface area of Ag/AgCl-NCs and easier partition of e-h+ pairs. Based on the unique structure and size of prepared Ag/AgCl-NCs, they exhibit improved antibacterial as well as photocatalytic activities as compared with Ag-NPs and AgCl-NPs under direct solar light irradiation. This work explores the better antibacterial and photocatalytic performance by good morphology and small size NCs, which could provide not only a simple green method, but also a new approach for designing an effective photocatalyst. Finally, it ought to overcome the restrictions of existing treatment strategies. Moreover, this method will give a secure, solid, and viable treatment towards numerous other environmental applications with excellent efficiency.

Acknowledgments PP is highly thankful to South Point College of Pharmacy, Sonipat for providing antibacterial activity research facilities to do this work. The authors are thankful to Materials Research Center (MRC), Malaviya National Institute of Technology (MNIT), Jaipur for providing characterization facilities.

Authors' contributions P. P. and S. P. Nehra designed the experiment. P. P. and P. M. performed the experiments. P. P. and P.M. analyzed the data. P. P. wrote the draft of manuscript with support from P. M. and S. P. Nehra. S. P. Nehra supervised the project. S. P. Nehra finalized the manuscript.

Funding All India Council for Technical Education, Ministry of Human Resource Development, Govt. of India for provided financial support under Research Promotion Scheme (RPS) reference no. 8-86/RIFD/ RPS/POLICY-1/2016-17.

Data availability The data are available upon request.

Competing interest The authors declare that they have no competing interest.

Ethical approval For this type of study, formal consent is not required.

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