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Pulsed laser-assisted synthesis of nano nickel(ii) oxide-anchored graphitic carbon nitride: Characterizations and their potential antibacterial/anti-biofilm applications

  • Umair Baig EMAIL logo , Rasha A. AbuMousa , Mohammad Azam Ansari , Muhammad A. Gondal EMAIL logo and Mohamed A. Dastageer
Published/Copyright: November 9, 2022
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Nanotechnology Reviews
From the journal Nanotechnology Reviews Volume 11 Issue 1

Abstract

Nickel(ii) oxide-graphitic carbon nitride (n-NiO@g-C3N4) nanocomposite, in which nickel oxide nanoparticles (n-NiO) are anchored on the polymeric surface of graphitic carbon nitride (g-C3N4), was synthesized using the pulsed laser post processing (PLPP) in liquid medium. In the PLPP method, the precursors (NiO and g-C3N4) were simultaneously subjected to pulsed laser-induced fragmentation, and pulsed laser-induced defect engineering (anchoring of NiO on g-C3N4). To optimize the functionality of the material, n-NiO@g-C3N4 with four different mass contents of n-NiO was synthesized. The synthesized n-NiO@g-C3N4 nanocomposite and its composite partners (n-NiO and g-C3N4) were structurally, morphologically, elementally characterized by X-ray diffraction, filed emission scanning electron microscope, transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analyses. As a first anti-microbial application, n-NiO@g-C3N4 was used to evaluate the minimal inhibitory concentration and minimal bactericidal concentration against the gram-positive Staphylococcus aureus and gram-negative Pseudomonas aeruginosa bacteria. As a second anti-microbial application, the efficacy of n-NiO@g-C3N4 nanocomposite to retard S. aureus and P. aeruginosa biofilms’ growth was evaluated. It was found that for both applications, n-NiO@g-C3N4 nanocomposite exhibited an excellent anti-bacterial activity compared to pure g-C3N4.

Keywords: nanostructured material; nanosecond pulsed laser; characterizations; antibacterial activity; anti-biofilm activity.

1 Introduction

The nanostructured metal and metal oxide are the better antimicrobial agents than their respective bulk counterparts. This is because the nanoparticles of metals and metal oxides are more prone to selectively target the microbial cells than the metal ions of the bulk material [1,2,3,4,5]. For the anti-microbial studies on various gram-positive and gram-negative bacteria, many carbon-based materials such as graphitic carbon nitride (g-C3N4), carbon nanotubes, and grapheme were also used [6,7,8]. In addition to metals, metal oxides, and carbon-based material in their pure forms, the compatible composite of two or more of these materials was found to be more reactive for the antibacterial activity than their individual composite partners [9,10,11]. When two semiconducting materials form a nanocomposite, the formation of the heterojunction between these composite partners perturbs the inherent band structures of the partners, and a modified composite band structure is formed. The new band structure brings about new physical and chemical properties, which can be effectively harnessed for any application like anti-microbial activity.

Gram-positive Staphylococcus aureus is quite harmful, which causes infections in respiratory system, blood stream, skin, and many other common infections, and also, this bacterium is highly adaptive and resistant to many drugs [12,13]. The gram-negative Pseudomonas aeruginosa is also quite harmful and it is the most common cause of ventilator-related pneumonia. One of the main virulence factors of P. aeruginosa is associated with nosocomial infections, and also these bacteria can produce biofilms on a variety of surfaces, including contact lenses, contaminated catheters, and the mucus plugs of cystic fibrosis patients [14]. In the case of metal and metal oxide-based anti-microbial agents, the deactivation is mediated by the reactive oxygen, and also the metal ion nanoparticles penetrate through the cell membrane and disturb DNA replication and cell reproduction and culminate the termination of the microorganism. As the ion penetration into the cell membrane is the major mechanism in the anti-microbial activity of nanomaterial, the particle size and shape are the important parameters that decide the antibacterial efficacy of the nanomaterials. Moreover, the rapid formation of biofilms of the microbes serves as the protective layer for the enclosed bacteria against the antibacterial agent. So, the proper selection of the nature, size, and shape of nanoparticle for the antibacterial activity is the big challenge to reckon with for both the annihilation of bacteria and the prevention of biofilm formation [15,16]. Apart from antibacterial and antibiofilm properties, metal-based nanoparticles have a wide range of potential in pharmaceutical and biomedical applications such as anti-parasitic, antifungal, anti-cancer, disease diagnosis, bio-sensing and bioimaging devices, drug delivery systems, and bone substitute implants [17,18,19].

Many metals and metal oxides were used to study the antibacterial activities of various gram-positive and gram-negative bacteria [20,21,22,23,24]. In many studies, NiO nanoparticles were used as the anti-microbial agents against P. aeruginosa and Escherichia coli (gram-negative bacteria) and S. aureus and Streptococcus pneumonia (gram-positive bacteria) and these studies showed good inhibitory activity of NiO [25,26]. The efficient photo-catalytic deactivation of bacteria using g-C3N4 under visible light is well established, and besides its function as a photo-catalyst, g-C3N4 in its pure form was used for anti-microbial studies, where a mere direct mechanical contact between g-C3N4 nanosheets and cell membranes caused cell rupture [27]. Also, many composites of g-C3N4 were used effectively for studying the antibacterial activity [28,29]. In this work, nano nickel(ii) oxide (n-NiO)-anchored graphitic carbon nitride (g-C3N4) nanocomposite (n-NiO@g-C3N4) was synthesized by pulsed laser processing in liquid medium.

The novelty of this work is the laser-based method used to synthesize n-NiO@g-C3N4 nanocomposite, where the pulsed laser-induced fragmentation and pulsed laser-induced defect engineering (anchoring) are the involved processes. The particle sizes of both the composite partners (NiO and g-C3N4) reduced by pulsed laser-assisted fragmentation process and simultaneously n-NiO was anchored on the polymeric surface of g-C3N4. The high intense laser pulses create local plasma, and the expansion of this plasma results in the formation of cavitation bubbles in the liquid medium. After reaching certain size, these cavitation bubbles implode, and this creates the particle fragmentation and also the anchoring of n-NiO on the g-C3N4 polymeric surface to create n-NiO@g-C3N4 nanocomposite [30]. The advantage of this method is that the size, shape, and the chemical composition of the composite material can be tuned by changing the laser parameters, such as wavelength, pulse duration, repetition rate, pulse energy, and fluence. The efficacy of the antimicrobial agent depends on the size and shape due to the fact that the deactivation of the microbe is carried out by the penetration of nanoparticles into the cell membrane. Hence, pulse laser processing is suitable for the synthesis of antimicrobial agents. Other positive attributes of this method of synthesis are that it is less cumbersome process without the need of heavy equipment, complex chemicals, and post-synthesis purification. Moreover, the n-NiO@g-C3N4 nanocomposite, synthesized by the pulsed laser, resulted in the perfect anchoring of n-NiO on g-C3N4. This method requires only very simple irradiation process and does not need many chemicals and post-purification.

The synthesized n-NiO@g-C3N4 was used as the anti-bacterial agent to study its efficacy to annihilate the harmful S. aureus and P. aeruginosa bacteria by observing the minimal inhibitory concentration (MIC) and minimal bactericidal concentration (MBC) of n-NiO@g-C3N4 that is capable of disinfecting the bacterial growth. MIC is the minimum concentration of the antimicrobial agent required to inhibit the further growth of bacteria, and the MBC is the concentration can completely annihilate the bacteria. As a second, anti-microbial study of the nanocomposite, the capability of n-NiO@g-C3N4 in the process of retarding S. aureus and P. aeruginosa biofilm formation was characterized by the inhibition efficiency of n-NiO@g-C3N4. In addition to the study of antibacterial activity of n-NiO@g-C3N4 on the bulk and biofilm of S. aureus and P. aeruginosa, the morphological filed emission scanning electron microscope (FE-SEM), structural X-ray diffraction (XRD), and elemental X-ray photoelectron spectroscopy (XPS) characterizations of the synthesized n-NiO@g-C3N4 were carried out to elucidate the antibacterial activity of the nanocomposite.

2 Experimental

2.1 Materials

Melamine powder (≥99%; Sigma Aldrich), nickel(ii) oxide powder (≥99%; Sigma Aldrich), and reagents such as ethanol (99%), propanol (99%), and acetone (99%) were commercially procured and used without further purification.

2.2 Synthesis of nanostructured n-NiO@g-C3N4 composites

The nanostructured n-NiO@g-C3N4 composite with varying concentrations of n-NiO in g-C3N4 was synthesized by pulsed laser processing that involves pulsed laser fragmentation and pulsed laser-induced anchoring. For this synthesis, different quantities of n-NiO (2.5, 5, 10, and 20%) are mixed with aqueous dispersion of g-C3N4 sheets, and this dispersion was initially ultra-sonicated for 30 min at room temperature and subsequently irradiated by the second harmonic (532 nm) of pulsed Nd:YAG laser (Quantel Brilliant B) for 60 min with the pulse energy of 150 mJ/pulse. The synthesized n-NiO@g-C3N4 composite with 2.5, 5, 10, and 20% n-NiO loadings are named as 2.5%-n-NiO@g-C3N4, 5%-n-NiO@g-C3N4, 10%-n-NiO@g-C3N4, and 20%-n-NiO@g-C3N4. Schematic diagram for the formation of n-NiO@g-C3N4 nanocomposites using nanosecond pulsed laser ablation in liquid is shown in Figure 1.

Figure 1 Schematic diagram for the synthesis of n-NiO@g-C3N4 nanocomposites by pulsed laser fragmentation and pulse laser-assisted anchoring.
Figure 1

Schematic diagram for the synthesis of n-NiO@g-C3N4 nanocomposites by pulsed laser fragmentation and pulse laser-assisted anchoring.

2.3 Characterizations

The XRD analysis of the pure and composite samples was carried out by using Rigaku MiniFlex 300/600 XRD. X-ray diffractometer is equipped with Cu-Kα radiation source in the 2θ range of 20–80°. The surface morphology of the pure and composite samples was analyzed by Tescan Lyra-3 FE-SEM. The in-depth structure and the morphological analysis of the synthesized samples were characterized by JEOL (JEM-2100F) Transmission Electron Microscope. FE-SEM was performed at an operating voltage of 20 kV and transmission electron microscopy (TEM) at 80 kV.

2.4 Antibacterial activity

Antibacterial activities of pure g-C3N4 and n-NiO@g-C3N4 with four different mass contents of NiO were determined against gram-positive S. aureus ATCC 25923 and gram-negative P. aeruginosa ATCC 27853 bacteria. Bacterial cultures were cultivated in Luria Bertani broth at 37°C for 24 h at a shaking rate of 150 rpm in a shaker incubator.

2.4.1 Minimal inhibitory concentration (MIC)

To determine the MIC values of nanocomposite at varied concentrations (0.125–10 mg/mL) against gram-positive S. aureus and gram-negative P. aeruginosa (108 CFU/mL) in a 96-well microtiter plates, standard broth dilution method M07 A9 of Clinical and Laboratory Standards Institute (2012) was used with slight modification [31]. The negative control contained only inoculated broth without nanocomposites, whereas Gentamicin was used a positive control (Table S1). All the experimental sets were performed in Mueller Hinton broth and were incubated for 24 h at 37°C in a shaker incubator. MIC is the lowest concentration of a tested nanocomposite at which no observable growth was seen [17].

2.4.2 Minimal bactericidal concentration (MBC)

To calculate the MBCs, a 10 µl suspension of bacteria was taken from microtiter plate wells that showed no bacterial growth (i.e., MIC and above MIC values) and spread on an MHA plate for an additional 24 h at 37°C. The MBC values for nanocomposite materials can be defined as the lowest concentration of nanomaterials measured at which no bacterial growth or less than three colony-forming units (CFUs) were identified [17].

2.5 Evaluation of anti-biofilm activity

The anti-biofilm properties of nanocomposite against S. aureus and P. aeruginosa biofilms were investigated using a polystyrene 96-well flat bottom microtiter tissue culture plate, as previously described [1]. In brief, 20 µL of fresh bacterial cultures was added to 180 mL of LB broth with varying concentrations of nanocomposite and incubated for 24 h at 37°C. In the following step, the contents of the plate were discarded, and the plate was washed three times with PBS before being dyed with crystal violet dye (0.1% w/v) for 15 min. The excess dye was washed away, and the samples were rinsed in PBS and allowed to dry completely. The ethanol (95%) was then used to solubilize the dye, and then, the amount of biofilm produced was quantified using an ELISA reader at a wavelength of 595 nm.

3 Results and discussion

3.1 XRD analysis

X-ray powder diffraction study was carried out for pure g-C3N4, pure NiO, and 20%-n-NiO@g-C3N4 nanocomposite, and the results are compiled in Figure 2. The characteristic XRD peaks of g-C3N4 at 13.11 and 27.38° are attributed to (100) diffraction plane of in-plane ordering of tri-s-triazine units and (002) diffraction plane of graphite-like interlayer-stacked structure, respectively (JCPDS 87-1526). It is well known that NiO has the cubic NaCl kind of structure with octahedral Ni2+ and O2− sites, and hence, the diffraction peaks at 37.20, 43.25, 62.83, 74.81, and 79.49° can be indexed as (111), (200), (220), (311), and (222) diffraction planes of face-centered cubic phase of NiO (JCPDS 47-1049) [32]. The XRD pattern of 20%-n-NiO@g-C3N4 nanocomposite shown in Figure 2 shows only the clean merging of all the above characteristic peaks of both g-C3N4 and pure NiO, indicating that the pulsed laser-assisted synthesis of n-NiO@g-C3N4 nanocomposite is a product of the perfect anchoring of nanostructured NiO on the g-C3N4 framework.

Figure 2 XRD of pure g-C3N4, pure NiO, and n-NiO@g-C3N4.
Figure 2

XRD of pure g-C3N4, pure NiO, and n-NiO@g-C3N4.

3.2 FE-SEM and TEM analyses

The FE-SEM images of pure g-C3N4, pure NiO, and n-NiO@g-C3N4 are shown in Figure 3a–c, respectively, where the FE-SEM image of g-C3N4 (Figure 3a) manifests a sheet-like morphology and that of NiO particles (Figure 3b) shows an agglomeration of spherical nanoparticles; finally, it is quite clear in the FE-SEM image of n-NiO@g-C3N4 (Figure 3b), and the spherical NiO nanoparticles are well placed on the g-C3N4 sheets. This change in the surface morphology of n-NiO@g-C3N4, and the molecular level interaction between NiO and the g-C3N4 made this new nanocomposite more efficient in the observed antibacterial activity. This manifestation of the change in the morphology of n-NiO@g-C3N4 is further substantiated by TEM images shown in Figure 4a and b for g-C3N4 and n-NiO@g-C3N4, respectively. The TEM image of g-C3N4 has a flake-like structure and after pulsed laser processing, NiO particles are seen to be robustly adhering to the surface of g-C3N4 and these TEM images clearly validate the anchoring of NiO particles on the g-C3N4 surfaces.

Figure 3 FE-SEM images of pure g-C3N4 (a), pure NiO (b), and n-NiO@g-C3N4 (c).
Figure 3

FE-SEM images of pure g-C3N4 (a), pure NiO (b), and n-NiO@g-C3N4 (c).

Figure 4 TEM images of g-C3N4 (a) and n-NiO@g-C3N4 (b).
Figure 4

TEM images of g-C3N4 (a) and n-NiO@g-C3N4 (b).

3.3 XPS analysis

The elemental compositions of pure g-C3N4 and n-NiO@g-C3N4, and the modified elemental peak positions of carbon (C1s) and nitrogen (N1s), due to the newly developed chemical environment, as a result of the anchoring of n-NiO on g-C3N4, are evaluated using XPS analysis. Figure 5a shows the survey XPS scan of both pure g-C3N4 and n-NiO@g-C3N4, where the carbon (C1s), nitrogen (N1s), nickel (Ni2p), and oxygen (O1s) peaks are present for the latter, compared to only carbon (C1s) and nitrogen (N1s) for the former, which indicates the perfect formation of n-NiO@g-C3N4 nanocomposite due to the pulsed laser-assisted synthesis. Figure 5b and c, respectively, shows the C1s and N1s peaks of pure g-C3N4 in high resolution. The C1s peak in pure g-C3N4 has three-component peaks 283.18, 284.78, and 286.68 eV due to their presence in three different chemical environments of C1s in C−C, (C)3−N, and C−N−C bonding, respectively. Similarly, N1s peak of pristine g-C3N4 consists of two-component peaks at 397.18 and 398.58 eV due to the presence of carbon in C−N−C and N−H bonding, respectively. These original chemical environments of both C1s and N1s are clearly perturbed due to the anchoring of nano NiO on g-C3N4 and these changes are manifested as the shifting of energy positions of C1s and N1s component peaks toward higher energy region, which is clear in Figure 5d and e. The observed shifts in the XPS peak of C1s and N1s due to the presence of NiO in g-C3N4 further confirm the proper loading of NiO on g-C3N4. In addition to these changes, the presence of NiO in g-C3N4 brought the emergence of new nickel (Ni2p) and oxygen (O1s) peaks, which is evident in the survey scan in Figure 5a, whose high-resolution spectra are, respectively, shown in Figure 5f and g. In Figure 5f, the component peaks of Ni2p peak of n-NiO@g-C3N4 at 855.58 and 862.38 eV could be attributed to Ni2p3/2 and the component peaks at 873.08 and 879.68 eV could be attributed to the Ni2p1/2. In Figure 5g, the component peaks of O1s of n-NiO@g-C3N4 at 528.18 and 529.88 eV could be attributed to the Ni–O and O–H bonds, respectively. The slight shifting of C1s and N1s peaks and the appearance of Ni2p and O1s peaks demonstrate the successful formulation of n-NiO@g-C3N4 nanocomposite.

Figure 5 XPS survey scan of g-C3N4 and n-NiO@g-C3N4 (a). High-resolution XPS spectrum of g-C3N4 for C1s peak (b) and N1s peak (c). High-resolution XPS spectrum of n-NiO@g-C3N4 for C1s peak (d), N1s peak (e), Ni2p peak (f), and O1s peak (g).
Figure 5

XPS survey scan of g-C3N4 and n-NiO@g-C3N4 (a). High-resolution XPS spectrum of g-C3N4 for C1s peak (b) and N1s peak (c). High-resolution XPS spectrum of n-NiO@g-C3N4 for C1s peak (d), N1s peak (e), Ni2p peak (f), and O1s peak (g).

3.4 Antibacterial activity

To estimate the relative merits of the antibacterial activities of the five variants of n-NiO@g-C3N4, the following two antibacterial figures of merit are employed: (i) MBC, which is defined as the lowest concentration of the antibacterial agent required for the total annihilation of bacteria with a standard concentration; and (ii) MIC, which is defined as the lowest concentration of antibacterial agent required to inhibit the growth of bacteria. The MBC values obtained from the antibacterial experiments using five different variants of n-NiO@g-C3N4 (pure g-C3N4, 2.5%-n-NiO@g-C3N4, 5%-n-NiO@g-C3N4, 10%-n-NiO@g-C3N4, and 20%-n-NiO@g-C3N4) are summarized in the bar chart in Figure 6a, where it is quite clear that 9.0 mg/mL of pure g-C3N4 is required to completely annihilate the S. aureus bacteria, whereas, where only the half (4.5 mg/mL) or even less than half (4.0 mg/mL) of this concentration of n-NiO@g-C3N4 is required for the complete annihilation of S. aureus bacteria in the given concentration. In the similar way, the estimation of MIC was carried out for the five variants of n-NiO@g-C3N4 and is also summarized in Figure 6a, where we can observe that to inhibit the S. aureus bacterial growth, a concentration of 4.5 mg/mL of pure g-C3N4 is required and only less concentrations of n-NiO@g-C3N4 suspensions are required to inhibit the growth of S. aureus bacteria, where the lowest MIC of 1.0 mg/mL is observed for 20%-n-NiO@g-C3N4. While the MICs/MBC values of pure g-C3N4, and nanocomposites 5%-n-NiO@g-C3N4, 10%-n-NiO@g-C3N4, 10%-n-NiO@g-C3N4, and 20%-n-NiO@g-C3N4 were 4.5/9, 4.5/9, 4/8, 4/8, and 4/8 mg/mL, respectively, against gram-negative P. aeruginosa. Also, as expected, for each variant of n-NiO@g-C3N4, the MIC (minimum concentration required to inhibit) is less than MBC (minimum concentration required for complete annihilation). It is quite obvious from Figure 6, in general, the loading of n-NiO on g-C3N4 enhances the antibacterial activity (both annihilation and inhibition) on S. aureus and P. aeruginosa, and this antibacterial property of n-NiO@g-C3N4 increases with the increasing n-NiO content in the nanocomposite.

Figure 6 MIC and MBC (mg/mL) results of tested nanocomposites/nanomaterials against (a) S. aureus and (b) P. aeruginosa (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4 and E = 20%-n-NiO@g-C3N4).
Figure 6

MIC and MBC (mg/mL) results of tested nanocomposites/nanomaterials against (a) S. aureus and (b) P. aeruginosa (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4 and E = 20%-n-NiO@g-C3N4).

Furthermore, it was observed that the tested compounds were more active against gram-positive S. aureus bacteria than gram-negative P. aeruginosa. It has been reported that size, shape, morphology, surface charge, surface chemistry, and capping agents influence the antimicrobial activity and mechanism of action of nanoparticles [14,17,33,34,35,36]. It has been proposed that the antibacterial activity of most of the inorganic nanoparticles is due to the damage of cell wall and cell membrane that surges the bacterial membrane permeability, production of reactive oxygen species, interaction of nanoparticles with cellular organelles, which results in the leakage of cytoplasmic contents that lead to the cell death of bacteria [17,33,34,35,36].

3.5 Anti-biofilm activity

Microorganism like bacteria and fungus can virtually adhere to any surface and their colonies assemble as a two-dimensional network known as biofilm, and compared to bulk microorganisms, biofilms are more resistant to any antibacterial agent and also serve as a protective shield for the interior microbes against the antibacterial agent. In this work, we studied the inhibition of the growth of S. aureus and P. aeruginosa biofilms mediated by five different variants of n-NiO@g-C3N4 (pure g-C3N4, 2.5%-n-NiO@g-C3N4, 5%-n-NiO@g-C3N4, 10%-n-NiO@g-C3N4, and 20%-n-NiO@g-C3N4) at two different concentrations (0.25 and 0.50 mg/mL), and the results are shown in Figures 7 and 8, respectively, as the percentage of inhibition. For this study, 10 μL of S. aureus and P. aeruginosa bacterial suspension with 1.5 × 108 CFU/mL concentration and the same volume and concentration of the bacterial suspension treated with pure g-C3N4 and n-NiO@g-C3N4 nanocomposites with the respective minimum inhibition concentrations (MIC) were kept in the 96-well enzyme-linked immunosorbent assay plate and these mixtures were simultaneously incubated at 37°C for 24 h. To experimentally quantify the percentage of biofilm growth inhibition, the optical absorption spectra of pure g-C3N4 and n-NiO@g-C3N4 nanocomposites treated and untreated were compared. The incubated biofilm is optically sensitized by an organic dye and this dye-sensitized S. aureus biofilm shows two absorption peaks, one centered at the characteristic wavelength of the dye (465 nm) and another one centered at 595 nm, which is the characteristic absorption of protein molecule of the biofilm, and apparently the intensity of the latter peak proportional to the concentration of bacteria in the biofilm. It is quite clear from Figure 7 that the formation of biofilm was effectively inhibited by the presence of n-NiO@g-C3N4 in general and this inhibiting efficiency increases with increasing n-NiO content in n-NiO@g-C3N4 and the highest biofilm inhibition was observed in the presence of 0.5 mg/mL of 20%-n-NiO@g-C3N4 against S. aureus and P. aeruginosa, i.e., 71.95 and 56.01%, respectively (Figures 7 and 8). Biofilm formed by the bacteria is the complex communities covered by the secretion of exopolysaccharide (EPS), which gets irreversibly attached to the surface. It was stated that the biofilm inhibitory activity of nanoparticles is attributed to the prevention of the formation of EPS. It was also proposed that biosorption may be the major factor responsible for the inactivation of biofilm formation by inorganic nanoparticles. The findings obtained from scanning electron microscopy and confocal laser scanning microscopy images showed that the nanoparticles wrecked the structure of biofilms [14,15,17,33,34,35,36].

Figure 7 (a) Effects of nanocomposites on biofilm formation abilities of S. aureus and (b) 96-well microtiter plate showing biofilm inhibition of S. aureus in the presence of nanocomposites. Negative control (NC): culture media only, without bacteria and nanocomposites; positive control (PC): culture media inoculated with S. aureus, but without nanocomposites: biofilm inhibition in the presence of 0.25 and 0.5 mg/mL of nanocomposites (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4, and E = 20%-n-NiO@g-C3N4).
Figure 7

(a) Effects of nanocomposites on biofilm formation abilities of S. aureus and (b) 96-well microtiter plate showing biofilm inhibition of S. aureus in the presence of nanocomposites. Negative control (NC): culture media only, without bacteria and nanocomposites; positive control (PC): culture media inoculated with S. aureus, but without nanocomposites: biofilm inhibition in the presence of 0.25 and 0.5 mg/mL of nanocomposites (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4, and E = 20%-n-NiO@g-C3N4).

Figure 8 (a) Effects of nanocomposites on biofilm formation abilities of P. aeruginosa; (b) 96-well microtiter plate showing biofilm inhibition of gram-negative P. aeruginosa in the presence of nanocomposites. NC: culture media only, without bacteria and nanocomposites; PC: culture media inoculated with P. aeruginosa, but without nanocomposites: biofilm inhibition in the presence of 0.25 and 0.5 mg/mL of nanocomposites (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4, and E = 20%-n-NiO@g-C3N4).
Figure 8

(a) Effects of nanocomposites on biofilm formation abilities of P. aeruginosa; (b) 96-well microtiter plate showing biofilm inhibition of gram-negative P. aeruginosa in the presence of nanocomposites. NC: culture media only, without bacteria and nanocomposites; PC: culture media inoculated with P. aeruginosa, but without nanocomposites: biofilm inhibition in the presence of 0.25 and 0.5 mg/mL of nanocomposites (A = g-C3N4, B = 2.5%-n-NiO@g-C3N4, C = 5%-n-NiO@g-C3N4, D = 10%-n-NiO@g-C3N4, and E = 20%-n-NiO@g-C3N4).

4 Conclusions

Laser-induced post processing in water medium was used to synthesize n-NiO@g-C3N4 nanocomposites with four different mass contents of NiO (2.5, 5, 10, and 20%). High energy focused laser pulse-created intense plasma, which expands to create a cavitation bubble. This cavitation bubble grows and implodes, resulting in the fragmentation of precursor particles (NiO and g-C3N4), and at the same time anchoring n-NiO on the g-C3N4. n-NiO@g-C3N4 nanocomposites were used as antibacterial agents against gram-positive S. aureus and gram-negative P. aeruginosa bacteria and an optimum performance was observed with 20%-n-NiO@g-C3N4. After 24 h of incubation, MIC and MBC of n-NiO@g-C3N4 antibacterial agent for S. aureus are 1 and 4 mg/mL, respectively, and the same for P. aeruginosa are 4 and 8 mg/mL, respectively. As a second anti-microbial application, n-NiO@g-C3N4 nanocomposites were also used to study the inhibition of biofilm formation of S. aureus and P. aeruginosa, and it was found to be 71.95 and 56.01%, respectively, for these two microbes.

Acknowledgments

R. A. AbuMousa would like to acknowledge the support of Prince Sultan University for paying the Article Processing Charges for this publication.

  1. Funding information: The authors are grateful for the support of Prince Sultan University for paying the Article Processing Charges for this publication.

  2. Author contributions: All authors have accepted responsibility for the entire content of this manuscript and approved its submission.

  3. Conflict of interest: The authors state no conflict of interest.

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Received: 2022-03-15
Revised: 2022-08-14
Accepted: 2022-10-18
Published Online: 2022-11-09

© 2022 Umair Baig et al., published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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https://doi.org/10.1515/ntrev-2022-0492
Keywords for this article
nanostructured material; nanosecond pulsed laser; characterizations; antibacterial activity; anti-biofilm activity.
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Theoretical and experimental investigation of MWCNT dispersion effect on the elastic modulus of flexible PDMS/MWCNT nanocomposites
  3. Mechanical, morphological, and fracture-deformation behavior of MWCNTs-reinforced (Al–Cu–Mg–T351) alloy cast nanocomposites fabricated by optimized mechanical milling and powder metallurgy techniques
  4. Flammability and physical stability of sugar palm crystalline nanocellulose reinforced thermoplastic sugar palm starch/poly(lactic acid) blend bionanocomposites
  5. Glutathione-loaded non-ionic surfactant niosomes: A new approach to improve oral bioavailability and hepatoprotective efficacy of glutathione
  6. Relationship between mechano-bactericidal activity and nanoblades density on chemically strengthened glass
  7. In situ regulation of microstructure and microwave-absorbing properties of FeSiAl through HNO3 oxidation
  8. Research on a mechanical model of magnetorheological fluid different diameter particles
  9. Nanomechanical and dynamic mechanical properties of rubber–wood–plastic composites
  10. Investigative properties of CeO2 doped with niobium: A combined characterization and DFT studies
  11. Miniaturized peptidomimetics and nano-vesiculation in endothelin types through probable nano-disk formation and structure property relationships of endothelins’ fragments
  12. N/S co-doped CoSe/C nanocubes as anode materials for Li-ion batteries
  13. Synergistic effects of halloysite nanotubes with metal and phosphorus additives on the optimal design of eco-friendly sandwich panels with maximum flame resistance and minimum weight
  14. Octreotide-conjugated silver nanoparticles for active targeting of somatostatin receptors and their application in a nebulized rat model
  15. Controllable morphology of Bi2S3 nanostructures formed via hydrothermal vulcanization of Bi2O3 thin-film layer and their photoelectrocatalytic performances
  16. Development of (−)-epigallocatechin-3-gallate-loaded folate receptor-targeted nanoparticles for prostate cancer treatment
  17. Enhancement of the mechanical properties of HDPE mineral nanocomposites by filler particles modulation of the matrix plastic/elastic behavior
  18. Effect of plasticizers on the properties of sugar palm nanocellulose/cinnamon essential oil reinforced starch bionanocomposite films
  19. Optimization of nano coating to reduce the thermal deformation of ball screws
  20. Preparation of efficient piezoelectric PVDF–HFP/Ni composite films by high electric field poling
  21. MHD dissipative Casson nanofluid liquid film flow due to an unsteady stretching sheet with radiation influence and slip velocity phenomenon
  22. Effects of nano-SiO2 modification on rubberised mortar and concrete with recycled coarse aggregates
  23. Mechanical and microscopic properties of fiber-reinforced coal gangue-based geopolymer concrete
  24. Effect of morphology and size on the thermodynamic stability of cerium oxide nanoparticles: Experiment and molecular dynamics calculation
  25. Mechanical performance of a CFRP composite reinforced via gelatin-CNTs: A study on fiber interfacial enhancement and matrix enhancement
  26. A practical review over surface modification, nanopatterns, emerging materials, drug delivery systems, and their biophysiochemical properties for dental implants: Recent progresses and advances
  27. HTR: An ultra-high speed algorithm for cage recognition of clathrate hydrates
  28. Effects of microalloying elements added by in situ synthesis on the microstructure of WCu composites
  29. A highly sensitive nanobiosensor based on aptamer-conjugated graphene-decorated rhodium nanoparticles for detection of HER2-positive circulating tumor cells
  30. Progressive collapse performance of shear strengthened RC frames by nano CFRP
  31. Core–shell heterostructured composites of carbon nanotubes and imine-linked hyperbranched polymers as metal-free Li-ion anodes
  32. A Galerkin strategy for tri-hybridized mixture in ethylene glycol comprising variable diffusion and thermal conductivity using non-Fourier’s theory
  33. Simple models for tensile modulus of shape memory polymer nanocomposites at ambient temperature
  34. Preparation and morphological studies of tin sulfide nanoparticles and use as efficient photocatalysts for the degradation of rhodamine B and phenol
  35. Polyethyleneimine-impregnated activated carbon nanofiber composited graphene-derived rice husk char for efficient post-combustion CO2 capture
  36. Electrospun nanofibers of Co3O4 nanocrystals encapsulated in cyclized-polyacrylonitrile for lithium storage
  37. Pitting corrosion induced on high-strength high carbon steel wire in high alkaline deaerated chloride electrolyte
  38. Formulation of polymeric nanoparticles loaded sorafenib; evaluation of cytotoxicity, molecular evaluation, and gene expression studies in lung and breast cancer cell lines
  39. Engineered nanocomposites in asphalt binders
  40. Influence of loading voltage, domain ratio, and additional load on the actuation of dielectric elastomer
  41. Thermally induced hex-graphene transitions in 2D carbon crystals
  42. The surface modification effect on the interfacial properties of glass fiber-reinforced epoxy: A molecular dynamics study
  43. Molecular dynamics study of deformation mechanism of interfacial microzone of Cu/Al2Cu/Al composites under tension
  44. Nanocolloid simulators of luminescent solar concentrator photovoltaic windows
  45. Compressive strength and anti-chloride ion penetration assessment of geopolymer mortar merging PVA fiber and nano-SiO2 using RBF–BP composite neural network
  46. Effect of 3-mercapto-1-propane sulfonate sulfonic acid and polyvinylpyrrolidone on the growth of cobalt pillar by electrodeposition
  47. Dynamics of convective slippery constraints on hybrid radiative Sutterby nanofluid flow by Galerkin finite element simulation
  48. Preparation of vanadium by the magnesiothermic self-propagating reduction and process control
  49. Microstructure-dependent photoelectrocatalytic activity of heterogeneous ZnO–ZnS nanosheets
  50. Cytotoxic and pro-inflammatory effects of molybdenum and tungsten disulphide on human bronchial cells
  51. Improving recycled aggregate concrete by compression casting and nano-silica
  52. Chemically reactive Maxwell nanoliquid flow by a stretching surface in the frames of Newtonian heating, nonlinear convection and radiative flux: Nanopolymer flow processing simulation
  53. Nonlinear dynamic and crack behaviors of carbon nanotubes-reinforced composites with various geometries
  54. Biosynthesis of copper oxide nanoparticles and its therapeutic efficacy against colon cancer
  55. Synthesis and characterization of smart stimuli-responsive herbal drug-encapsulated nanoniosome particles for efficient treatment of breast cancer
  56. Homotopic simulation for heat transport phenomenon of the Burgers nanofluids flow over a stretching cylinder with thermal convective and zero mass flux conditions
  57. Incorporation of copper and strontium ions in TiO2 nanotubes via dopamine to enhance hemocompatibility and cytocompatibility
  58. Mechanical, thermal, and barrier properties of starch films incorporated with chitosan nanoparticles
  59. Mechanical properties and microstructure of nano-strengthened recycled aggregate concrete
  60. Glucose-responsive nanogels efficiently maintain the stability and activity of therapeutic enzymes
  61. Tunning matrix rheology and mechanical performance of ultra-high performance concrete using cellulose nanofibers
  62. Flexible MXene/copper/cellulose nanofiber heat spreader films with enhanced thermal conductivity
  63. Promoted charge separation and specific surface area via interlacing of N-doped titanium dioxide nanotubes on carbon nitride nanosheets for photocatalytic degradation of Rhodamine B
  64. Elucidating the role of silicon dioxide and titanium dioxide nanoparticles in mitigating the disease of the eggplant caused by Phomopsis vexans, Ralstonia solanacearum, and root-knot nematode Meloidogyne incognita
  65. An implication of magnetic dipole in Carreau Yasuda liquid influenced by engine oil using ternary hybrid nanomaterial
  66. Robust synthesis of a composite phase of copper vanadium oxide with enhanced performance for durable aqueous Zn-ion batteries
  67. Tunning self-assembled phases of bovine serum albumin via hydrothermal process to synthesize novel functional hydrogel for skin protection against UVB
  68. A comparative experimental study on damping properties of epoxy nanocomposite beams reinforced with carbon nanotubes and graphene nanoplatelets
  69. Lightweight and hydrophobic Ni/GO/PVA composite aerogels for ultrahigh performance electromagnetic interference shielding
  70. Research on the auxetic behavior and mechanical properties of periodically rotating graphene nanostructures
  71. Repairing performances of novel cement mortar modified with graphene oxide and polyacrylate polymer
  72. Closed-loop recycling and fabrication of hydrophilic CNT films with high performance
  73. Design of thin-film configuration of SnO2–Ag2O composites for NO2 gas-sensing applications
  74. Study on stress distribution of SiC/Al composites based on microstructure models with microns and nanoparticles
  75. PVDF green nanofibers as potential carriers for improving self-healing and mechanical properties of carbon fiber/epoxy prepregs
  76. Osteogenesis capability of three-dimensionally printed poly(lactic acid)-halloysite nanotube scaffolds containing strontium ranelate
  77. Silver nanoparticles induce mitochondria-dependent apoptosis and late non-canonical autophagy in HT-29 colon cancer cells
  78. Preparation and bonding mechanisms of polymer/metal hybrid composite by nano molding technology
  79. Damage self-sensing and strain monitoring of glass-reinforced epoxy composite impregnated with graphene nanoplatelet and multiwalled carbon nanotubes
  80. Thermal analysis characterisation of solar-powered ship using Oldroyd hybrid nanofluids in parabolic trough solar collector: An optimal thermal application
  81. Pyrene-functionalized halloysite nanotubes for simultaneously detecting and separating Hg(ii) in aqueous media: A comprehensive comparison on interparticle and intraparticle excimers
  82. Fabrication of self-assembly CNT flexible film and its piezoresistive sensing behaviors
  83. Thermal valuation and entropy inspection of second-grade nanoscale fluid flow over a stretching surface by applying Koo–Kleinstreuer–Li relation
  84. Mechanical properties and microstructure of nano-SiO2 and basalt-fiber-reinforced recycled aggregate concrete
  85. Characterization and tribology performance of polyaniline-coated nanodiamond lubricant additives
  86. Combined impact of Marangoni convection and thermophoretic particle deposition on chemically reactive transport of nanofluid flow over a stretching surface
  87. Spark plasma extrusion of binder free hydroxyapatite powder
  88. An investigation on thermo-mechanical performance of graphene-oxide-reinforced shape memory polymer
  89. Effect of nanoadditives on the novel leather fiber/recycled poly(ethylene-vinyl-acetate) polymer composites for multifunctional applications: Fabrication, characterizations, and multiobjective optimization using central composite design
  90. Design selection for a hemispherical dimple core sandwich panel using hybrid multi-criteria decision-making methods
  91. Improving tensile strength and impact toughness of plasticized poly(lactic acid) biocomposites by incorporating nanofibrillated cellulose
  92. Green synthesis of spinel copper ferrite (CuFe2O4) nanoparticles and their toxicity
  93. The effect of TaC and NbC hybrid and mono-nanoparticles on AA2024 nanocomposites: Microstructure, strengthening, and artificial aging
  94. Excited-state geometry relaxation of pyrene-modified cellulose nanocrystals under UV-light excitation for detecting Fe3+
  95. Effect of CNTs and MEA on the creep of face-slab concrete at an early age
  96. Effect of deformation conditions on compression phase transformation of AZ31
  97. Application of MXene as a new generation of highly conductive coating materials for electromembrane-surrounded solid-phase microextraction
  98. A comparative study of the elasto-plastic properties for ceramic nanocomposites filled by graphene or graphene oxide nanoplates
  99. Encapsulation strategies for improving the biological behavior of CdS@ZIF-8 nanocomposites
  100. Biosynthesis of ZnO NPs from pumpkin seeds’ extract and elucidation of its anticancer potential against breast cancer
  101. Preliminary trials of the gold nanoparticles conjugated chrysin: An assessment of anti-oxidant, anti-microbial, and in vitro cytotoxic activities of a nanoformulated flavonoid
  102. Effect of micron-scale pores increased by nano-SiO2 sol modification on the strength of cement mortar
  103. Fractional simulations for thermal flow of hybrid nanofluid with aluminum oxide and titanium oxide nanoparticles with water and blood base fluids
  104. The effect of graphene nano-powder on the viscosity of water: An experimental study and artificial neural network modeling
  105. Development of a novel heat- and shear-resistant nano-silica gelling agent
  106. Characterization, biocompatibility and in vivo of nominal MnO2-containing wollastonite glass-ceramic
  107. Entropy production simulation of second-grade magnetic nanomaterials flowing across an expanding surface with viscidness dissipative flux
  108. Enhancement in structural, morphological, and optical properties of copper oxide for optoelectronic device applications
  109. Aptamer-functionalized chitosan-coated gold nanoparticle complex as a suitable targeted drug carrier for improved breast cancer treatment
  110. Performance and overall evaluation of nano-alumina-modified asphalt mixture
  111. Analysis of pure nanofluid (GO/engine oil) and hybrid nanofluid (GO–Fe3O4/engine oil): Novel thermal and magnetic features
  112. Synthesis of Ag@AgCl modified anatase/rutile/brookite mixed phase TiO2 and their photocatalytic property
  113. Mechanisms and influential variables on the abrasion resistance hydraulic concrete
  114. Synergistic reinforcement mechanism of basalt fiber/cellulose nanocrystals/polypropylene composites
  115. Achieving excellent oxidation resistance and mechanical properties of TiB2–B4C/carbon aerogel composites by quick-gelation and mechanical mixing
  116. Microwave-assisted sol–gel template-free synthesis and characterization of silica nanoparticles obtained from South African coal fly ash
  117. Pulsed laser-assisted synthesis of nano nickel(ii) oxide-anchored graphitic carbon nitride: Characterizations and their potential antibacterial/anti-biofilm applications
  118. Effects of nano-ZrSi2 on thermal stability of phenolic resin and thermal reusability of quartz–phenolic composites
  119. Benzaldehyde derivatives on tin electroplating as corrosion resistance for fabricating copper circuit
  120. Mechanical and heat transfer properties of 4D-printed shape memory graphene oxide/epoxy acrylate composites
  121. Coupling the vanadium-induced amorphous/crystalline NiFe2O4 with phosphide heterojunction toward active oxygen evolution reaction catalysts
  122. Graphene-oxide-reinforced cement composites mechanical and microstructural characteristics at elevated temperatures
  123. Gray correlation analysis of factors influencing compressive strength and durability of nano-SiO2 and PVA fiber reinforced geopolymer mortar
  124. Preparation of layered gradient Cu–Cr–Ti alloy with excellent mechanical properties, thermal stability, and electrical conductivity
  125. Recovery of Cr from chrome-containing leather wastes to develop aluminum-based composite material along with Al2O3 ceramic particles: An ingenious approach
  126. Mechanisms of the improved stiffness of flexible polymers under impact loading
  127. Anticancer potential of gold nanoparticles (AuNPs) using a battery of in vitro tests
  128. Review Articles
  129. Proposed approaches for coronaviruses elimination from wastewater: Membrane techniques and nanotechnology solutions
  130. Application of Pickering emulsion in oil drilling and production
  131. The contribution of microfluidics to the fight against tuberculosis
  132. Graphene-based biosensors for disease theranostics: Development, applications, and recent advancements
  133. Synthesis and encapsulation of iron oxide nanorods for application in magnetic hyperthermia and photothermal therapy
  134. Contemporary nano-architectured drugs and leads for ανβ3 integrin-based chemotherapy: Rationale and retrospect
  135. State-of-the-art review of fabrication, application, and mechanical properties of functionally graded porous nanocomposite materials
  136. Insights on magnetic spinel ferrites for targeted drug delivery and hyperthermia applications
  137. A review on heterogeneous oxidation of acetaminophen based on micro and nanoparticles catalyzed by different activators
  138. Early diagnosis of lung cancer using magnetic nanoparticles-integrated systems
  139. Advances in ZnO: Manipulation of defects for enhancing their technological potentials
  140. Efficacious nanomedicine track toward combating COVID-19
  141. A review of the design, processes, and properties of Mg-based composites
  142. Green synthesis of nanoparticles for varied applications: Green renewable resources and energy-efficient synthetic routes
  143. Two-dimensional nanomaterial-based polymer composites: Fundamentals and applications
  144. Recent progress and challenges in plasmonic nanomaterials
  145. Apoptotic cell-derived micro/nanosized extracellular vesicles in tissue regeneration
  146. Electronic noses based on metal oxide nanowires: A review
  147. Framework materials for supercapacitors
  148. An overview on the reproductive toxicity of graphene derivatives: Highlighting the importance
  149. Antibacterial nanomaterials: Upcoming hope to overcome antibiotic resistance crisis
  150. Research progress of carbon materials in the field of three-dimensional printing polymer nanocomposites
  151. A review of atomic layer deposition modelling and simulation methodologies: Density functional theory and molecular dynamics
  152. Recent advances in the preparation of PVDF-based piezoelectric materials
  153. Recent developments in tensile properties of friction welding of carbon fiber-reinforced composite: A review
  154. Comprehensive review of the properties of fly ash-based geopolymer with additive of nano-SiO2
  155. Perspectives in biopolymer/graphene-based composite application: Advances, challenges, and recommendations
  156. Graphene-based nanocomposite using new modeling molecular dynamic simulations for proposed neutralizing mechanism and real-time sensing of COVID-19
  157. Nanotechnology application on bamboo materials: A review
  158. Recent developments and future perspectives of biorenewable nanocomposites for advanced applications
  159. Nanostructured lipid carrier system: A compendium of their formulation development approaches, optimization strategies by quality by design, and recent applications in drug delivery
  160. 3D printing customized design of human bone tissue implant and its application
  161. Design, preparation, and functionalization of nanobiomaterials for enhanced efficacy in current and future biomedical applications
  162. A brief review of nanoparticles-doped PEDOT:PSS nanocomposite for OLED and OPV
  163. Nanotechnology interventions as a putative tool for the treatment of dental afflictions
  164. Recent advancements in metal–organic frameworks integrating quantum dots (QDs@MOF) and their potential applications
  165. A focused review of short electrospun nanofiber preparation techniques for composite reinforcement
  166. Microstructural characteristics and nano-modification of interfacial transition zone in concrete: A review
  167. Latest developments in the upconversion nanotechnology for the rapid detection of food safety: A review
  168. Strategic applications of nano-fertilizers for sustainable agriculture: Benefits and bottlenecks
  169. Molecular dynamics application of cocrystal energetic materials: A review
  170. Synthesis and application of nanometer hydroxyapatite in biomedicine
  171. Cutting-edge development in waste-recycled nanomaterials for energy storage and conversion applications
  172. Biological applications of ternary quantum dots: A review
  173. Nanotherapeutics for hydrogen sulfide-involved treatment: An emerging approach for cancer therapy
  174. Application of antibacterial nanoparticles in orthodontic materials
  175. Effect of natural-based biological hydrogels combined with growth factors on skin wound healing
  176. Nanozymes – A route to overcome microbial resistance: A viewpoint
  177. Recent developments and applications of smart nanoparticles in biomedicine
  178. Contemporary review on carbon nanotube (CNT) composites and their impact on multifarious applications
  179. Interfacial interactions and reinforcing mechanisms of cellulose and chitin nanomaterials and starch derivatives for cement and concrete strength and durability enhancement: A review
  180. Diamond-like carbon films for tribological modification of rubber
  181. Layered double hydroxides (LDHs) modified cement-based materials: A systematic review
  182. Recent research progress and advanced applications of silica/polymer nanocomposites
  183. Modeling of supramolecular biopolymers: Leading the in silico revolution of tissue engineering and nanomedicine
  184. Recent advances in perovskites-based optoelectronics
  185. Biogenic synthesis of palladium nanoparticles: New production methods and applications
  186. A comprehensive review of nanofluids with fractional derivatives: Modeling and application
  187. Electrospinning of marine polysaccharides: Processing and chemical aspects, challenges, and future prospects
  188. Electrohydrodynamic printing for demanding devices: A review of processing and applications
  189. Rapid Communications
  190. Structural material with designed thermal twist for a simple actuation
  191. Recent advances in photothermal materials for solar-driven crude oil adsorption
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