Materials Chemistry and Physics 294 (2023) 127036

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Materials Chemistry and Physics

journal homepage: www.elsevier.com/locate/matchemphys

Synthesis and characterization of MgO nanostructures: A comparative study

on the effect of preparation route
Satti Venu Gopala Kumari a, Kannan Pakshirajan b, G. Pugazhenthi a, *
a
Department of Chemical Engineering, Indian Institute of Technology Guwahati, Guwahati, 781039, Assam, India
b
Department of Biosciences and Bioengineering, Indian Institute of Technology Guwahati, Guwahati, 781039, Assam, India

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• MgO nanostructures were synthesized

by five facile chemical synthesis routes.
• Flake, sphere, natural rose, and mari­
gold flower-like morphology were
obtained.
• Synthesis route influenced surface area
and pore volume of MgO
nanostructures.
• MgO nanostructures exhibited excellent
antibacterial and antioxidant activity.

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, MgO nanostructures were synthesized by five facile and diverse chemical synthesis routes, viz.
MgO nanoflowers precipitation (PT), sonication-precipitation (SPT), microwave combustion (MWC), conventional combustion
Microwave combustion (CC), and solvothermal (ST) processes. The influence of aforementioned synthesis routes on crystallinity, crys­
Antimicrobial activity
tallite size, morphology, optical, and surface traits of MgO nanostructures was evaluated by XRD, BET, FESEM,
Chemical synthesis
MgO synthesis
FETEM, optical absorption, steady-state and time-resolved photoluminescence analyses. Furthermore, antioxi­
dant and antibacterial properties of MgO nanostructures were examined. XRD analysis revealed that crystallite
size and relative crystallinity (%) of MgO varied from 9 to 42 nm and 90.70–99.06%, respectively, depending on
the synthesis route followed. The application of microwave irradiation (MWC) and sonication (ST) reduced
particle size and increased specific surface area of MgO nanostructures compared to nanostructures obtained via
CC and PT methods. This could be due to faster reaction kinetics in MWC and small-scale turbulence generated
during sonication that restricts growth and agglomeration of nuclei during nanostructure synthesis. FESEM
analysis revealed flake, sphere, natural rose, and marigold flower-like morphologies of MgO due to different
methods followed, that can be attributed to the differences in nanostructure formation mechanism involved. The
highest photoluminescence intensity observed with MgO synthesized via MWC is likely to produce a maximum
number of reactive oxygen species. Consequently, MgO synthesized through MWC process showed highest
bactericidal and antioxidant activities compared to MgO synthesized via other routes. Thus, present study
demonstrated that properties of nanostructures required for a particular application could be customized by
proper choice of the synthesis route.

* Corresponding author.
E-mail address: [email protected] (G. Pugazhenthi).

https://doi.org/10.1016/j.matchemphys.2022.127036
Received 30 April 2022; Received in revised form 20 October 2022; Accepted 13 November 2022
Available online 14 November 2022
0254-0584/© 2022 Elsevier B.V. All rights reserved.
S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

1. Introduction nanostructures are not reported thus far. Evaluation of steady-state PL

and TRPL characteristics of MgO nanostructures can establish the po­
Nanostructures exhibit distinctive physicochemical properties tential use of such nanostructures in light-harvesting and optical sensor
compared to their bulk counterparts owing to their nano-size, high applications [5]. On the other hand, screening synthesis routes to
aspect ratio, surface defects, and quantum effects. Among them, MgO customize the MgO nanostructures with the best antimicrobial and
nanostructures are noted for their economical precursors, unique antioxidant performance is essential for their application in food, med­
structural properties such as tunable porosity and high specific surface ical care and packaging industries [24].
area, exceptionally diverse morphology varying from spheres, rods, and To the best of our knowledge, comparative study on the synthesis of
flakes to stars and flowers [1,2]. Besides, nanostructured MgO has high MgO nanostructures by five diverse synthesis routes, viz. precipitation
flame resistance and mechanical strength, high density of catalytically (PT), sonication-precipitation (SPT), microwave combustion (MWC),
active sites, low susceptibility to hydration, surface defects induced conventional combustion (CC), and solvothermal (ST) processes as well
electro and photoluminescence emissions [2,3]. These characteristics as evaluation of their structural, optical absorption, steady-state PL,
make it a versatile material suitable for the fabrication of advanced and TRPL, antioxidant and antimicrobial characteristics is not reported yet
innovative materials [4,5]. MgO nanostructures find application in in the literature. Among the aforementioned routes, PT is a simple and
diverse fields such as catalysis, paints, refractory products, supercon­ cost-effective technique in which the cationic source is homogeneously
ductors, optoelectronic devices like light-emitting diodes, lasers, and dispersed in an alkaline medium and the obtained precipitate is calcined
electrochemical sensors [2,5–7]. Also, porous MgO nanostructures are to get MgO [16]. In the SPT method, sonication aids in deagglomerating
extensively utilized in the sorption of heavy metal ions, nanoparticles by generating strong turbulence and acoustic cavitation in
phosphorus-containing compounds, toxic gases, chlorine, CO2, and HCl solution during the precipitation reaction [25]. Unlike the PT and SPT
[7,8]. In addition, conspicuous features of MgO nanostructures such as methods, in the ST process, the reaction proceeds in a solvent at a point
nontoxicity, biocompatibility, and broad-spectrum antimicrobial action above its normal boiling condition by containing the reaction mixture in
are interesting for application in the food industry, biomedicine, and an autoclave reactor [19]. On the other hand, combustion synthesis
allied fields [4,9]. utilizes a self-sustained exothermic reaction between oxidizer and fuel
Despite the many advantages of MgO nanostructures, certain prop­ [21,23]. Moreover, microwave irradiation in MWC provides volumetric
erties, viz. particle size, morphology, crystallinity, crystallite size, and heating and rapid completion of the reaction. Whereas in the CC process,
surface area are essential for a particular application. For instance, MgO the reaction mixture is heated from the surface to the interior resulting
use as coatings on medical implants usually requires high crystallinity in steep temperature gradients and slow reaction kinetics [21]. There­
for improved physiological stability. On the other hand, the use of MgO fore, the objective of the current study is to synthesize MgO nano­
in photocatalysis and adsorption process demands high specific surface structures via the PT, SPT, MWC, CC and ST routes and compare their
area, low crystallinity, and high concentration of surface defects [10, structural, morphological, optical absorption, PL and TRPL character­
11]. Indeed, the more the surface defects of MgO, the greater the po­ istics. Furthermore, antioxidant and antibacterial properties of MgO
tential of nanostructures to produce reactive oxygen species (ROS), nanostructures were examined. As calcination conditions greatly influ­
resulting in increased antibacterial activity [12,13]. Luminescence, an ence the surface area and activity of MgO, in all the methods adopted in
important characteristic of nanostructures for optoelectronic and the current study, the calcination treatment was performed at 500 ◦ C for
light-harvesting applications, can also be tuned by controlling their 5 h.
surface defects. Concerning the effect of particle size and morphology,
Bindhu et al. (2016) reported an increase in antibacterial activity with a 2. Materials and methods
decrease in particle size of MgO nanostructures [14]. The morphology of
nanostructures also influences their defect-induced properties, such as 2.1. Materials
antioxidant and pro-oxidant activity. Podder et al. (2019) reported
morphology-induced crossover between antioxidant and pro-oxidant Mg(NO3)2⋅6H2O, NaOH, and urea were procured from Merck Spe­
activity of MgO nanostructures [1]. The optical bandgap of nano­ cialties Pvt. Ltd. [India]. Acetone, methanol (99.9%), and ethanol
structures plays a crucial role in optoelectronic device application and (99.9%) were purchased from Finar Ltd. [India]. Nutrient broth was
its porosity greatly influences CO2 capture and photocatalytic activity supplied by Hi-Media Laboratories Pvt. Ltd. [India]. 2,2-diphenyl-1-pic­
[7,8,15]. The extensive literature studies reveal that the synthesis rylhydrazyl hydrate (DPPH) was purchased from Sigma Aldrich Co. Ltd.
methods and conditions adapted significantly impact the aforemen­ [India]. All the chemicals were of analytical grade and used without
tioned characteristics of MgO nanostructures as well as their suitability further purification. Water used in all the experiments was obtained
for a given application. Thus, the interest in synthesizing MgO nano­ from in-house Millipore water synthesis unit (Millipore, ELix-3, USA).
structures with desirable properties is phenomenal.
For the synthesis of MgO nanostructures, diverse approaches were 2.2. Synthesis of MgO nanostructures
reported in the literature. Among them, the chemical routes are simple
and cost-effective, as these require low reaction temperature and pro­ In order to examine the influence of synthesis methods on the
vide a high yield [2,5,7]. The synthesis routes for the production of MgO properties of MgO nanostructures, five simple methods were adopted in
nanostructures include, but are not limited to, precipitation [16], this work and their details are presented below:
sonochemical method [17], sol-gel method [18], hydrothermal [1] and
solvothermal processes [19], pulsed laser deposition method [20], 2.2.1. Precipitation (PT) method
conventional combustion [21], and microwave methods [21]. Literature The synthesis conditions in this approach were adapted from the
on MgO synthesis is mainly focused towards optimizing different literature [16]. Accordingly, 250 ml of NaOH (1 M) solution was first
experimental parameters involved [17,22,23]; however, a comparative added dropwise into 250 ml magnesium nitrate (0.2 M) solution. After
evaluation on the effect of different synthesis routes on MgO charac­ mixing the admixture for 30 min using a magnetic stirrer, the solution
teristics is lacking. Though, Selvam et al. (2011) reported a comparative was filtered, and the resulting precipitate was washed multiple times
study on the synthesis of MgO nanostructures by conventional and mi­ with water followed by acetone to remove any remaining salts. Then, the
crowave combustion methods [21], the study is limited to investigating precipitate was dried for 12 h at 100 ◦ C in a hot air oven and calcined at
their structural, optical absorption, and steady-state photoluminescence 500 ◦ C for 5 h in an air atmosphere.
(PL) properties. Time-resolved photoluminescence (TRPL) characteris­
tics, antioxidant and antibacterial activity of the synthesized MgO

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

2.2.2. Sonication-precipitation (SPT) method taken as positive control in this experiment. Following 24 h of incuba­
In this approach, the admixture consisting of Mg(NO3)2⋅6H2O (250 tion, the optical density of the culture was measured at 600 nm by
ml of 0.2 M solution) and NaOH (250 ml of 1 M solution) was prepared UV–Visible spectrophotometer (Perkin Elmer, Lambda 35, Switzerland),
as described in literature [16] and the solution was sonicated for 30 min. and percentage growth inhibition of bacteria was calculated using
Subsequently, the precipitates collected after sonication were washed Equation (2) [26]. All the experiments were performed in triplicate and
and calcined, following the procedure described in Section 2.2.1. results were presented as mean ± standard deviation.
C0 − Ct
2.2.3. Microwave combustion (MWC) method Growth Inhibition (%) = × 100 (2)
C0
In the current approach, Mg(NO3)2⋅6H2O (oxidizer) and urea (fuel)
were subjected to microwave-induced combustion, adapting the exper­ where Co is the concentration of bacterial culture in control (mg/L), Ct is
imental conditions from the literature [21] with a slight modification. the concentration of bacterial culture in the test sample (mg/L) at the
Accordingly, 0.85 g of Mg(NO3)2⋅6H2O and 0.6 g of urea were separately end of the experiment. The results obtained in this test were further
dissolved in 10 ml of water and mixed until a clear solution was ob­ analyzed statistically by carrying out one-way ANOVA followed by
tained. The obtained solution was then subjected to microwave irradi­ Tukey’s Honest Significance Difference Test using Origin™ Pro 9.0
ation in a conventional microwave oven (Samsung, model: software. Tukey’s test involves in pairwise comparison of means to
MC28h5023AK/TL, frequency: 50 Hz) operated at 900 W for 10 min, assess if two sets of data are statistically significant.
wherein the solution initially boils, undergoes dehydration followed by
decomposition, and becomes solid. The resultant solid was finely 2.4. Analytical methods
ground, washed, dried, and calcined following the procedure described
in Section 2.2.1. The structural characteristics of both calcined and uncalcined sam­
ples synthesized through five different processes were analyzed by an X-
2.2.4. Conventional combustion (CC) method ray powder diffractometer (Rigaku, Micromax-007HF, Japan) operated
In this approach, the combustion reaction of urea (fuel) and Mg at 40 kV and 40 mA using Ni filtered Cu Kα radiation (λ = 0.15418 nm).
(NO3)2⋅6H2O (oxidizer) was performed in a muffle furnace. A homoge­ The analysis was done in the 2θ range of 5◦ –90◦ with a scanning rate of
neous solution of Mg(NO3)2⋅6H2O and urea was prepared as described in 5◦ min− 1. Fourier transform infrared spectroscopy (FTIR) analysis
Section 2.2.3. The solution was then transferred into a silica crucible and (Shimadzu, IR Affinity-1, Japan) was performed for calcined and un­
heated to 500 ◦ C for 5 h in a furnace with a heating rate of 5 ◦ C min− 1 calcined samples in the wavelength range of 400–4000 cm− 1 using KBr
under air atmosphere to get MgO nanostructures. pellet route with an average of 30 scans and spectral resolution of 4
cm− 1. Furthermore, uncalcined samples were analyzed by Thermogra­
2.2.5. Solvothermal (ST) method vimetric Analyzer (Netzsch, TG 209 F1 Libra, Germany) in the temper­
In this approach, synthesis procedure and conditions as described in ature range of 30 ◦ C–700 ◦ C with a heating rate of 5 ◦ C min− 1 in an air
the literature [19] were adopted with a slight modification. Firstly, 15 g atmosphere (flow rate of 40 ml min− 1).
of NaOH was dissolved in 175 ml of 50% (v/v) ethanol/water solution Nitrogen adsorption-desorption analysis was carried out for MgO
and 8.62 g of Mg(NO3)2⋅6H2O was directly added into it and mixed for samples at − 196 ◦ C using an automated gas sorption analyzer (Quan­
30 min using a magnetic stirrer. The admixture was transferred into tachrome, Autosorb-IQ-MP, USA). The samples were outgassed at 200 ◦ C
Teflon-coated stainless steel autoclave reactor of 250 ml capacity, and for 4 h before measurement. The pore size distribution of MgO samples
the reaction was carried out for 12 h at 180 ◦ C. After completion of the synthesized via various routes was evaluated from the desorption branch
reaction, the solution was allowed to cool to room temperature, the of the N2 isotherm by Barrett-Joyner-Halenda (BJH) method, and spe­
precipitate formed was recovered via filtration, and then washed and cific surface area of the nanostructures was derived following Brunauer-
calcined as described in section 2.2.1. Emmet-Teller (BET) method. Morphology of MgO samples was further
analyzed by Field Emission Scanning Electron Microscope (FESEM) and
2.3. Antioxidant and antibacterial activities Field Emission Transmission Electron Microscope (FETEM). For FESEM
analysis, samples were drop cast, dried overnight and placed on a
The antioxidant activity of MgO nanostructures was estimated by stainless steel stub using double-sided carbon tape. The stubs were then
measuring its scavenging ability against DPPH radicals [1]. For this sputtered with gold and observed under FESEM (Sigma 300, Zeiss,
experiment, 200 μL of methanolic DPPH solution (0.1 mM) was mixed Germany). For observation under FETEM, the samples were drop cast on
with 3 ml of MgO nanostructures at various concentrations (10, 50, 100, a copper grid and dried overnight. FETEM images, selected area electron
250 and 500 μg/ml) and incubated in dark at room temperature. After diffraction (SAED) patterns and high-resolution transmission electron
30 min of incubation, the absorbance of the solution was measured at micrographs (HRTEM) were obtained using FETEM (JEOL, JEM 2100F,
517 nm using a UV–Visible spectrophotometer (PerkinElmer, Lambda Japan) operated at 200 kV.
35, Switzerland) and the measured absorbance was recorded as As. A The optical properties of MgO nanostructures were studied by pre­
control experiment was carried out by dissolving 200 μL of DPPH in 3 ml paring samples in colloidal form using Millipore water. The absorption
of water and the absorbance measured after incubation was recorded as measurements were performed using UV–Visible spectrophotometer
Ac. Then, the DPPH radical scavenging activity was calculated using (PerkinElmer, Lambda 950, USA) in the wavelength range of 190–600
Equation (1) [1]. All the experiments were performed in triplicate and nm. Millipore water without nanostructures was used as blank for
results were expressed as mean ± standard deviation. measurement of UV–Vis absorption spectra of samples. Steady-state
photoluminescence spectra (PL) were obtained using a Fluorimeter
Ac − As
DPPH radical scavenging activity (%) = × 100 (1) (Horiaba scientific, FluoroMax-4, Japan) at an excitation wavelength of
Ac
385 nm. Time-resolved PL (TRPL) was recorded by Picosecond time-
The antibacterial property of MgO nanostructures was assessed resolved fluorimeter (Edinburg Instruments, Lifespec II, UK) using a
against Staphylococcus aureus and Escherichia coli. The cultures were picosecond diode laser source at a fixed excitation wavelength of 375
taken in 10 ml of sterile Luria Bertani (LB) broth and added with 20 mg nm.
of MgO nanostructures for determining the antibacterial activity. 10%
(v/v) of freshly grown respective bacterial culture was used as inoculum
and the medium was incubated at 37 ◦ C and 130 rpm in an orbital
shaker. LB broth containing the bacteria but without nanostructures was

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

3. Results and discussion to MgO upon calcination. Furthermore, bands observed in the
3400-3500 cm− 1 and 1500-1650 cm− 1 ranges in Fig. 2a and b can be
3.1. Thermogravimetric analysis assigned to stretching and bending vibrations of –OH group in the sur­
face absorbed water molecules. As evident from Fig. 2a and b, a decrease
TGA and differential thermogravimetric analysis (DTG) of uncal­ in the peak intensity at 3500 cm− 1 is observed for the calcined samples
cined samples obtained via various methods were performed in order to when compared to the uncalcined samples, indicating a gradual reduc­
identify the calcination temperatures to get MgO nanostructures. The tion in the degree of binding of water molecules at the crystallite surface
obtained results are depicted in Fig. 1(a–d). The as-synthesized samples of samples due to transformation of Mg(OH)2 to MgO [30]. In Fig. 2a
(uncalcined) through PT, SPT, and ST methods displayed a total weight and b, two main bands can be noticed for each of Mg(OH)2 and MgO
loss of about 32.67%, 32.53%, and 32.87%, respectively, in two stages samples in the range of 400–1000 cm− 1, in which the high-frequency
(I, II) with a sharp endothermic peak centered at 350 ◦ C. Whereas the bands at 878 and 850 cm− 1 is ascribed to ν1 stretching of Mg–O, and
sample obtained via MWC route showed one additional stage (III) and a the low frequency stretching bands at 500 and 650 cm− 1 are due to ν2
total weight loss of 41.7% (see Fig. 1c). For all the samples, the first stage stretching of Mg–O [29]. Furthermore, the small peak at 2300 cm− 1in
(I) of weight loss observed below 200 ◦ C is attributed to the liberation of Figs. 2b and 1385 cm− 1 in Fig. 2a can be assigned to the bending vi­
physically adsorbed water. The second stage (II) of weight loss observed brations of surface adsorbed CO2 [30]. However, the complete trans­
beyond 270 ◦ C is very close to the theoretical weight loss (30.89%) of formation of Mg(OH)2 to MgO is further confirmed by XRD analysis,
magnesium hydroxide decomposition and consequent formation of MgO which is discussed in the next section.
and water as per the reaction: Mg(OH)2 → < MgO > + < H2O > [12,27].
The third additional stage (III), observed in Fig. 1c, is attributed to the
combustion of remnants of fuel (urea) as reported in the literature [21, 3.3. Structural characteristics
27].
XRD analysis was performed to determine the structural phases of
both calcined and uncalcined samples. The XRD patterns of non-calcined
3.2. Infrared characteristics samples portrayed in Fig. 3a aligned well with that brucite phase, hex­
agonal Mg(OH)2 with unit cell parameters of a = 3.12 Å, b = 3.12 Å, and
FTIR analysis was performed for both uncalcined and calcined c = 4.75 Å, as confirmed from the standard data (JCPDS 00-001-0316).
samples to evaluate the changes in their chemical state during calcina­ Similarly, XRD patterns of the calcined samples depicted in Fig. 3b, well-
tion. The recorded spectra, shown in Fig. 2a and b, well-matched with matched with MgO (JCPDS 00-001-1235) of periclase phase, and cubic
the FTIR patterns of Mg(OH)2 and MgO samples, respectively, as re­ crystal system with a lattice parameter of a = 4.2 Å. Moreover, in Fig. 3b,
ported in the literature [19,28,29]. In Fig. 2a, the sharp intense band there is no evidence of bulk remnants and no shift in peak position as
detected at 3700 cm− 1 for all the samples accounts for the –OH compared to that of standard data (JCPDS 00-001-1235). However,
stretching in Mg(OH)2, which is completely absent in the calcined there is a change in peak broadening in different samples owing to
samples (Fig. 2b), suggesting the complete transformation of Mg(OH)2 variations in crystallite size of MgO nanostructures obtained via various

Fig. 1. TGA and DTG spectra of uncalcined samples synthesized via (a) PT, (b) SPT, (c) MWC, and (d) ST.

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 2. FTIR spectra of (a) uncalcined and (b) calcined samples derived through various processes.

Fig. 3. XRD analysis of samples obtained via different synthesis routes: (a) before calcination and (b) after calcination.

methods. Thus, XRD patterns, together with TGA and FTIR results, crystallite size to peak broadening in the diffraction pattern, whereas the
confirmed the successful transformation of Mg(OH)2 to MgO upon W–H method supposes that peak broadening is affected by both crys­
calcination. tallite size as well as strain in nanostructures. Based on the crystallite
The relative crystallinity of MgO nanostructures was estimated using size (D) obtained in Scherrer and W–H methods, dislocation density (ẟ)
Equation (3) by considering peak intensities reported for MgO in stan­ which is the number of dislocation lines per unit volume of crystal, was
dard data (JCPDS 00-001-1235) as reference [31,32]. The intensity of calculated using Equation (7) [34]. In general, dislocation density af­
peaks in Fig. 3b manifests that the obtained MgO nanostructures are in fects material characteristics, whereas other disruptions connect the
well-crystallized form, and the same can be observed from the per­ activity of disorder [35].
centage relative crystallinity reported in Table 1. In Fig. 3b, the peak ∑
Peak intensities of sample
corresponding to the (2 0 0) plane was most intense compared to other Relative crystallinity (%) = ∑ × 100 (3)
Peak intensities of reference
peaks indicating the preferential orientation of MgO nanostructures
through the (2 0 0) plane. The d-spacing (d) corresponding to (2 0 0)
nλ = 2d sin θ (4)
plane was calculated by Bragg’s law presented in Equation (4). The
d-spacing was obtained to be 0.21 nm for the MgO nanostructures kλ
synthesized through various routes, as no difference was observed in 2θ Ds = (5)
β cos θ
position of the (2 0 0) plane. Furthermore, the average crystallite size of
MgO nanostructures was determined following the Debye-Scherrer kλ
β cos θ = + 4ε sin θ (6)
method and Williamson-Hall (W–H) method with the help of Equa­ Dw
tions (5) and (6), respectively [33]. Scherrer method solely assigns

Table 1
Structural characteristics of MgO nanostructures derived from XRD data.
Synthesis d(2 0 0) Scherrer method Williamson-Hall method Relative crystallinity (%)
Method (nm)
Ds (nm) δ × 103 (nm)− 2
Dw (nm) δ × 103 (nm)− 2
ε × 104
PT 0.21 13.35 5.61 14.49 4.77 4.42 90.70
SPT 0.21 9.00 12.34 10.44 9.17 11.12 99.06
MWC 0.21 10.43 9.19 11.26 7.88 6.25 97.06
CC 0.21 38.08 0.68 42.00 0.66 2.3 92.18
ST 0.21 10.00 10.00 13.73 5.30 1.98 97.76

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

1 Table 2
δ= (7)
D2 Structural properties of MgO nanostructures derived from N2 adsorption-
desorption analysis.
where, n = 1, λ = 0.154 nm, k = 0.9. Ds and Dw are crystallite size
Method BET surface area Average pore diameter Total pore volume
calculated by Scherrer method and W–H method, respectively, β is full (m2 g− 1) (nm) (cm3 g− 1)
width at half maximum, θ is diffraction angle, and ε is microstrain.
PT 23.14 44.94 0.26
As reported in Table 1, the crystallite size of MgO nanostructures SPT 39.70 63.47 0.63
calculated from the Scherrer and W–H method matched well with each MWC 67.32 42.78 0.72
other. Generally, higher the speed of nucleation and growth, the smaller CC 5.21 38.38 0.05
will be the crystallite size [36]. It can be seen from Table 1 that the ST 35.59 16.85 0.15

average crystallite size of MgO nanostructures synthesized via SPT route

is slightly smaller than the nanostructures obtained through PT method. diameter and total pore volume values of MgO demonstrates that the
This can be attributed to faster kinetics and small-scale turbulence synthesis route significantly impacts the pore structure of final MgO
developed during sonication that restricts the growth and agglomeration products (Table 2). More importantly, the nitrogen uptake of MgO
of nuclei in SPT process [25]. Likewise, though the same fuel (urea) and synthesized via MWC increased sharply at high relative pressure (P/Po)
fuel ratio are maintained in MWC and CC methods, larger crystallite size compared to other samples, suggesting its highly porous nature, which is
was obtained in CC owing to slow reaction kinetics. As reported in also evident from its total pore volume (0.72 cm3 g− 1). Compared to
Table 1, microstrain is found to be positive for all the MgO samples, other samples, the MgO sample obtained via CC exhibited very low ni­
which can be ascribed to the influence of tensile forces on crystal trogen adsorption quantity and low total pore volume (0.05 cm3 g− 1)
structures [22]. Also, high values of microstrain and dislocation density [40].
of MgO samples obtained via SPT and MWC processes suggest the ex­ The porous nanostructures with a narrow pore size distribution and
istence of more lattice imperfections and structural defects in the MgO high specific surface area, such as the MgO obtained through MWC in
nanostructures [35]. the current study, are envisaged to be useful for practical adsorption and
The specific surface area and pore characteristics of the prepared catalysis applications [38]. Also, nanostructures with a multimodal pore
MgO nanostructures were evaluated using nitrogen adsorption- size distribution, such as that is MgO obtained via ST method, may find
desorption analysis as these properties influence the performance of promising application in catalysis since the combination of small and
such nanostructures in many applications, such as catalysis and large sized mesopores could reduce transport limitation in catalysis,
adsorption. The isotherm profiles and pore size distribution of MgO resulting in higher activity and controlled selectivity [41].
samples are shown in Fig. 4a and b, respectively, and specific surface
area and pore structure data are summarized in Table 2. It can be seen in Average pore diameter =
4 × Total pore volume
(8)
Fig. 4a that all the MgO samples displayed type III isotherm with H3 type BET surface area
hysteresis loop as per IUPAC categorization. The H3 hysteresis is a
characteristic of slit-shaped pores, with a non-uniform size and/or shape 3.4. Morphological characteristics
in solids consisting of aggregates [21,37,38]. As specific surface area
varies with size and number of particles and agglomerates, the differ­ Morphology is a fascinating aspect of nanomaterials that play a
ence in specific surface area of MgO nanostructures obtained via PT and crucial role in antimicrobial, optoelectronic, and photocatalytic appli­
SPT as well as MWC and CC is due to the decrease in particle size and cations. The growth of materials, i.e., which facets grow and how fast
reduction of agglomeration. The observed results are in good agreement they grow are governed by various factors, viz. nature of raw materials,
with findings in the reported literature [17,39]. alkalinity, temperature of the reaction, driving force of crystallization,
The pore size distribution determined using the BJH method, pre­ energy difference between the surfaces, and the reaction kinetics [42,
sented in Fig. 4b, revealed the existence of mesopores as well as mac­ 43]. In actual, the synthesis route adopted determines the aforemen­
ropores for all the MgO samples. The mesopores exist among small tioned factors, thereby affecting the morphology of the products [42].
primary nanoparticles and the macropores account for the textural pores Therefore, the morphology of MgO nanostructures obtained via different
formed due to the aggregation of small primary nanoparticles with synthesis routes was confirmed by FESEM analysis. As can be seen from
interparticle connections. However, as evident from Fig. 4b, the pore Fig. 5a and b, the MgO nanostructures obtained via PT, and SPT pro­
size distribution is bimodal for MgO nanostructures obtained via ST cesses revealed nanoflake-like morphology with an average thickness of
route and unimodal for the rest of the samples. The average pore 11.3 ± 2.58 nm, and 10.53 ± 2.79 nm, respectively. Furthermore, the
diameter of nanostructures was calculated based on surface area and high-resolution FESEM images shown in Fig. 5a’ and 5b’ revealed that
total pore volume using Equation (8). The difference in average pore the nanoflakes are composed of numerous nanoparticles of diameter

Fig. 4. (a) Nitrogen adsorption-desorption isotherms and (b) pore size distribution of MgO samples.

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 5. Lower and higher magnification FESEM images of MgO nanostructures synthesized via PT (a, a’), SPT (b, b’), MWC (c, c’), CC (d, d’), and ST (e, e’).

4–15 nm each, which is in good agreement with the crystallite size ob­ microwave irradiation in MWC, the fast-changing electric field may lead
tained by XRD analysis. Based on the XRD (Fig. 3a and b), FTIR (Fig. 2a to the oscillation of molecules in polar media, thereby resulting in
and b), and FESEM (Fig. 5a’ and 5b’) analyses results, possible growth volumetric heating of reaction mixture (Fig. 6c). This in turn lead to
mechanism of MgO nanostructures obtained via PT and SPT can be uniform nucleation, fast reaction kinetics, explosion reaction, vigorous
explained as follows: As shown in Fig. 6a and b, firstly, numerous Mg evolution of gases, and formation of Mg(OH)2 precursor [22,23], which
(OH)2 nanoparticles generate in solution, which after attaining the upon calcination transforms into fine porous MgO nanoparticles, as
critical size during Ostwald ripening acts as building blocks for the evident from XRD (Fig. 3a and b), FTIR (Fig. 2a and b) and BET (Fig. 4b)
crystallization through oriented-attachment of structurally similar sur­ analyses. Whereas in the case of CC method, the reaction mixture is
faces at their high-energy interfaces [44]. The orientation of crystallites heated from the surface to the interior resulting in steep temperature
along crystal plane leads to the formation of nanoflake-like architec­ gradients that spread more on the surface (Fig. 6d). The magnesium
tures, which transform into porous MgO nanoflakes during the calci­ nitrate hexahydrate is completely combusted and transformed to MgO in
nation step. However, in the SPT method (Fig. 6b), sonication restricts the CC process, unlike in MWC which necessitates in an additional
the growth and agglomeration of nuclei during MgO synthesis. calcination step. Moreover, prolonged reaction time in CC facilitated the
Fig. 5c and c’ revealed uniform nanosphere-like morphology of the growth of grains into the bulk phase and escape of gaseous products
MgO nanostructures obtained via MWC. Fig. 5d and d’ showed that MgO formed along with MgO, resulting in sheet-like structures on their sur­
nanostructures obtained via CC have nanoflower-like morphology that face, and thereby leading to its nanoflower morphology. The average
closely resembled natural marigold flower (see inset in Fig. 5d’). During thickness of petals (sheet-like structures) of nanoflowers obtained via CC

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 6. Probable formation mechanism of MgO nanostructures synthesized via (a) PT, (b) SPT, (c) MWC, (d) CC and (e) ST routes.

method is 16.19 ± 1.89 nm. In case of MgO nanostructures obtained by high surface energy of the initial crystallites, they aggregate to minimize
MWC and CC methods, the particle size observed through FESEM is their surface energy. The aggregated crystallites orient along a crystal
consistent with that of XRD results, which revealed that the crystallite plane which results in petal morphology. The petals then undergo
size of MgO obtained via CC method is larger than that obtained via random self-assembly and Ostwald ripening process giving rise to
MWC method. flower-like morphology. As reported in the literature [45], ethanol
Fig. 5e shows nanoflower-like morphology of the MgO synthesized (solvent) plays a vital role in providing a favourable environment for the
via ST method that closely resembled natural rose flowers (shown in the nucleation and growth of nanoflowers. High-resolution FESEM image
inset of Fig. 5e’). The high-resolution FESEM image (Fig. 5e’) revealed presented in Fig. 5e’ revealed that the nanoflakes assembled nano­
that nanoflowers obtained via ST were composed of nanoflakes con­ flowers are primarily composed of small nanoparticles of 8–10 nm
structed from fine aggregated nanoparticles, similar to the results diameter, which correlates well with the crystallite size obtained by XRD
described in the literature [44,45]. The average thickness of petals analysis.
(nanoflakes) of nanoflowers obtained via ST method is 8.38 ± 2.84 nm. The morphology and crystal structure of MgO nanostructures were
The mechanism behind nanoflakes-assembled flower-like morphology further analyzed by FETEM, and HRTEM. The FETEM images shown in
in the MgO obtained by ST process can be deduced as follows: as shown Fig. 7 reconfirmed the morphology observed through FESEM analysis.
in Fig. 6d, firstly, hotspots which are potential reaction points originate The HRTEM images shown in Fig. 7 (a’, b’, c’, d’, and e’) along with
in solution due to heating, and these hotspots serve as driving force and Inverse Fast Fourier Transform images (presented as an inset in their
generate a large number of small Mg(OH)2 crystallites [45]. Due to the corresponding images) revealed well-defined lattice fringes of d-spacing

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 7. FETEM (a, b, c, d, e), HRTEM (a’, b’, c’, d’, e’), and particle size distribution (a’’, b’’, c’’, d’’, e’’) of MgO nanostructures synthesized via PT, SP, MWC, CC,
and ST methods, respectively.

0.21 nm corresponding to (2 0 0) plane. The obtained results are in good surface area, numerous active sites, and rapid electron and mass trans­
agreement with the XRD results, confirming the growth direction of port kinetics.
nanostructures along (2 0 0) plane for MgO nanostructures. Further­
more, SAED patterns shown as an inset in Fig. 7 (a, b, c, d, and e) can be 3.5. Optical characteristics
indexed to the Face-centered cubic phase of MgO, which is also in good
agreement with the XRD results. Moreover, the bright spots in the SAED In general, optical transitions ought to occur when a photon is
pattern indicate the high crystallinity of the nanostructures [46]. absorbed or emitted by the defect site. Also, optical investigations open
Furthermore, the particle size distribution of MgO nanostructures was up the prospect of expanding the use of MgO nanostructures in opto­
calculated from FETEM images depicted in Fig. 7 (a, b, c, d, and e). The electronic devices. Therefore, absorbance and PL characteristics were
particle sizes are in the range of 30–110 nm, 25–64 nm, 5–35 nm, investigated to determine the presence of intrinsic point defects,
1129.68–2247.89 nm, and 661.38–1175.81 nm for MgO nanostructures particularly oxygen vacancies in synthesized MgO nanostructures [50].
prepared via PT, SPT, MWC, CC, and ST methods, respectively (see Fig. 7 In the current study, as the samples were analyzed in colloidal form,
(a’’, b’’, c’’, d’’, and e’’)). nanostructures with very small grain sizes are expected to contribute to
As 2D nanomaterials reinforced in polymers can create tortuous path the optical absorption phenomenon [51]. The absorption spectra of
for oxygen and water vapor permeation and extend the shelf-life of food synthesized nanostructures depicted in Fig. 8a revealed that all MgO
[47], the nanoflake-like MgO obtained via PT and SPT methods are samples exhibited strong absorption in the wavelength range of
attractive for loading in polymer matrix for food packaging applications. 190–250 nm due to excitation of four-fold coordinated O2− anions in
The nanosphere morphology with a high specific surface area yielded edges and corners. From the absorption data, the optical band gap of
from MWC route is interesting for catalysis, adsorption and antibacterial synthesized nanostructures was determined using Tauc relation given by
applications [24]. The nanoflakes assembled nanoflower morphology Equation (9) [52].
obtained via ST route could be of great choice for water treatment [48] ( )m
and electrochemical sensor applications [49], as it renders high specific (αhν) = A hν − Eg (9)

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 8. (a) Optical absorption, (b) (αhν)2 vs (hν), (c) PL and, (d) TRPL spectra of MgO samples obtained via different methods.

where, ‘A’ is a constant, α is absorption coefficient, ‘hν’ is incident ∑

i=3
photon energy, Eg corresponds to bandgap energy, m = ½ for direct Ai τi 2
transition. Fig. 8b shows the plot of (αhν)2 vs photon energy (hν), and τavg = i=1 (10)
∑i=3
the bandgap energy of nanostructures was calculated by extrapolating Ai τ i
straight line to (αhν)2 = 0. The estimated bandgap for MgO nano­
i=1

structures synthesized via PT, SPT, MWC, CC, and ST are 5.96, 5.78, τavg was obtained as 3.57, 3.63, 10.86, 4.24, and 3.45 ns for MgO
5.44, 5.88, and 5.78 eV, respectively. The narrow bandgap of the MgO nanostructures prepared via PT, SPT, MWC, CC, and ST, respectively. A
nanostructures can be attributed to the presence of oxygen vacancies similar finding was reported by Jain et al. (2016), in case of MgO
developing new energy levels, resulting in a narrow bandgap as opposed nanostructures synthesized using a wet chemical route, and the
to a perfect MgO surface with 6-coordinated surface anions at its surface, observed decay time was less than 10 ns at 477 nm emission [5]. The
which has a bandgap of 7.8 eV [50]. Besides that, the nanosize effect, authors also proposed the fabrication of white LED by integrating
defect density, and the short-range repulsion energy between atoms may luminescent MgO with blue LED. However, further studies such as
all contribute to the narrow bandgap [1,19]. PL is an optical tool to analysis of colorimetric coordinates and photoluminescence stability are
describe surface defects [12]. PL emissions result from the recombina­ warranted for the applicability of synthesized MgO nanostructures in
tion of photogenerated charge carriers [28]. The PL spectrum obtained solid-state lighting applications.
at room temperature, which is illustrated in Fig. 8c displayed multiple
emission peaks at 420, 444, 460, 524, and 630 nm due to defect band
3.6. Antioxidant property
transition, and the observed results are in well agreement with findings
reported in the literature [12,28]. As MgO is a wide-gap material, sur­
Lipids oxidation is a prominent cause of deterioration of a wide range
face defects resulting from the synthesis process or imperfect oxidation
of food products, next to microbial growth. For limiting the extent of
are considered as the source of PL emission in MgO nanostructures. The
lipid oxidation in packaged food, packaging materials with antioxidant
highest PL intensity observed with MgO synthesized via MWC, is likely
property are being developed by incorporating antioxidant agents in the
to produce a maximum number of ROS [12].
polymer matrix or on their surface [53]. Therefore, to explore the
Furthermore, TRPL analysis was performed to estimate the potential
antioxidant activity of the synthesized MgO nanostructures, its DPPH
of synthesized MgO nanostructures in light-harvesting and optical
radical scavenging ability was measured at different concentrations.
sensor applications. Decay time in the range of nanoseconds to pico­
Fig. 9 shows the results along with the mechanism of antioxidant activity
seconds is essential for these applications. However, the results depicted
[1,54]. A monotonic increase in antioxidant activity was observed with
in Fig. 8d demonstrated a decay time of less than 10 ns for 444 nm
an increase in the dosage of nanostructures. At 500 μg/ml concentration,
emission for all the MgO samples. The PL decay curves were fitted with
MgO nanostructures synthesized via MWC showed 100% scavenging of
tri-exponential decay function (Table S1 of Supplementary Information)
DPPH free radical. The DPPH radical scavenging activity is probably due
and average lifetime (τavg) was obtained using Equation (10) [5].
to the electron transfer from defect sites of MgO nanostructures to free
radicals located at the central nitrogen atom of DPPH. Upon electron
transfer, MgO becomes positively charged, whereas DPPH becomes
negatively charged, leading to the formation of MgO+-DPPH- complex.
The surface area and electron transfer ability of MgO nanostructures are

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

Fig. 9. (a) DPPH radical scavenging activity of MgO nanostructures at various concentrations and (b) mechanistic representation of the interaction between MgO
nanostructures and DPPH free radical.

known to affect the DPPH radical scavenging activity [1,54]. The higher literature [1].
the surface area of nanostructures, their DPPH adsorption capacity and,
therefore, DPPH radical scavenging ability are also higher. Hence, DPPH 3.7. Antibacterial property
radical scavenging activity is proportional to surface area of nano­
structures, and is highest for MgO obtained via MWC method followed Antibacterial agents are of importance in a variety of industries such
by ST, SPT, PT, and CC methods, respectively. A similar observation on as food, medical care, and packaging [55]. Therefore, development of
the antioxidant activity of MgO nanostructures has been reported in the new antibacterial agents has gained attention in parallel to combat

Fig. 10. (a) Antibacterial activity of MgO nanostructures against E. coli and S. aureus (bars with different alphabets indicate that difference of means is significant at
0.05 level according to one away ANOVA followed by Tukey test), and (b) Probable mechanism of antibacterial activity of MgO nanostructures.

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

increased outbreaks of pathogenic infections, new mutations, and 3.8. Comparison of characteristics of MgO nanostructures obtained via
multi-drug resistant bacteria. E. coli belongs to Gram-negative group of various synthesis routes
bacteria and is native to human intestine, whereas the bacterium
S. aureus is Gram-positive and a member of indigenous microbiota on Different characteristics of MgO nanostructures obtained via various
human skin and upper respiratory tract. These bacteria can propagate synthesis routes are presented in Table 3. As discussed earlier in Section
rapidly in food at room temperature [56]. Hence, antibacterial property 3.4, the diverse morphology of MgO nanostructures (nanoflakes, nano­
of the synthesized nanostructures was evaluated against E. coli and spheres, and nanoflowers) is clearly due to the difference in their for­
S. aureus. mation mechanism involved in the various synthesis routes. In
As shown in Fig. 10a, maximum antibacterial activity is due to the particular, novel rose-like morphology observed in ST process is a result
MgO nanostructures obtained via MWC, followed by that due to MgO of modification of surface energies of Mg(OH)2 crystallites during their
nanostructures synthesized via SPT, ST, PT, and CC, respectively. nucleation and growth by the solvent (ethanol) [45].Though the same
Moreover, S. aureus is more susceptible than E. coli to MgO nano­ precursors were used in the PT and SPT methods, MgO nanoflakes ob­
structures, which can be explained by the fact that cell wall of Gram- tained by the SPT process revealed small crystallite, particle size and
positive bacteria, e.g., S. aureus, are devoid of outer membrane and high specific surface area compared to nanostructures obtained via PT.
composed of multilayers of peptidoglycan. In contrast, Gram-negative This can be attributed to small-scale turbulence developed during son­
bacteria, e.g., E. coli are made of complex cell wall structure with a ication that restricts the growth and agglomeration of nuclei in the SPT
layer of peptidoglycan between the outer membrane and cytoplasmic process [25]. Among the five routes employed for the synthesis of MgO
membrane [14]. As a result, the cell membrane of S. aureus can be nanostructures, CC yielded the largest crystallite size as well as particle
damaged easily. size and the least specific surface area due to slow reaction kinetics and
Though antibacterial property of MgO nanostructures are widely steep temperature gradient in the combustion reaction by conventional
reported in literature, the exact underlying mechanism is unclear. heating [21]. On the other hand, MgO obtained via MWC route had the
However, few studies [57,58] suggest that light radiation catalyzes smallest crystallite size as well as particle size, and highest specific
redox reactions in metal oxides, generating electron and hole pairs on surface area and total pore volume compared to MgO obtained via all
conduction band (CB) and valence band (VB), respectively. The resul­ other methods. This is due to volumetric heating of the reaction mixture
tant electron-hole pairs could either recombine or the electrons could be and rapid completion of reaction offered by microwave irradiation.
readily trapped by O2 absorbed on MgO surface (or) dissolved O2 to form Besides, small particle size and high density of surface defects resulting
superoxide radicals (O•-2 ), while the photo-induced holes could be trap­ from the synthesis route contributed to high PL emissions, narrower
ped by surface hydroxyl groups (or) H2O on the MgO surface to form band gap, and excellent antimicrobial and antioxidant characteristics of
hydroxyl radicals (OH•). The superoxide radical successively (O•- 2 ) react the MgO obtained by MWC route.
with H+ to produce (HO•2) radicals, which upon subsequent collision
with electron, produce hydrogen peroxide anions (HO−2 ). These anions 4. Conclusions
react with hydrogen ions to produce H2O2 molecules. The generated
ROS (superoxide, hydrogen peroxide and hydroxyl radical) then interact MgO nanostructures were successfully prepared via five different
with the bacteria cells for efficient killing. As depicted in Fig. 10b, MgO chemical synthesis routes, namely PT, SPT, MWC, CC, and ST. Structural
nanostructures can either directly interact with bacteria leading to characterization by XRD, BET, FESEM, and FETEM analyses revealed
damage of cell wall followed by ROS generation inside the cell, or first that all the obtained nanostructures are in cubic phase, and synthesis
generate ROS outside the cell followed by entry into the cell via damage route has clearly influenced crystallite size, morphology, porosity, par­
of the cell wall. However, both mechanisms ultimately lead to cell death ticle size, and surface area of the obtained nanostructures. MgO nano­
by disintegrating DNA, ribosomes, and proteins present inside the bac­ structures obtained via PT and SPT routes revealed nanoflakes-like
teria due to interaction with ROS. Statistical analysis of the results was morphology, whereas nanosphere-like structures were obtained via
carried out by one-way ANOVA using Tukey’s test, which revealed a MWC process. Nanoflowers resembling natural marigold and rose
significant difference in the percentage growth inhibition of bacteria flowers are obtained through CC, and ST methods, respectively. The
obtained in the experiments with various MgO nanostructures. The very application of microwave irradiation (MWC) and sonication (ST)
high antibacterial activity of MgO nanostructures obtained through resulted in reduced particle size and increased specific surface area of
MWC can be attributed to its high specific surface area, small crystallite MgO nanostructures compared to nanostructures obtained via CC, and
size, and ability to generate numerous ROS. PT methods. The optical characterization confirmed emission peaks that

Table 3
Comparison of characteristics of MgO nanostructures obtained via various synthesis routes.
Property PT SPT MWC CC ST

Crystallite size calculated by Scherrer method, Ds 13.35 9.00 10.43 38.08 10.00
(nm)
Relative crystallinity (%) 90.70 99.06 97.06 92.18 97.76
BET surface area (m2 g− 1) 23.14 39.70 67.32 5.21 35.59
Total pore volume (cm3 g− 1) 0.26 0.63 0.72 0.05 0.15
Morphology nanoflakes nanoflakes nanospheres nanoflowers resembling natural nanoflowers resembling natural
marigold rose
Diameter of particles calculated from FETEM 30–110 25–64 5–35 1129.68–2247.89 661.38–1175.81
images (nm)
Band gap energy (eV) 5.96 5.78 5.44 5.88 5.78
Average lifetime, τavg (ns) 3.57 3.63 10.86 4.24 3.45
DPPH scavenging activity (%) at 500 μg/ml 43.09 ± 67.35 ± 100 18.73 ± 0.06 58.63 ± 1.48
•

concentration 0.03 0.23

Growth inhibition (%) of E. coli 7.82 ± 0.2 27.97 ± 89.86 ± 0.78 0.96 ± 0.56 13.36 ± 0.75
0.07
Growth inhibition (%) of S. aureus 12.31 ± 28.40 ± 94.14 ± 2.12 4.65 ± 0.75 16.66 ± 1.04
0.61 1.53

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S.V.G. Kumari et al. Materials Chemistry and Physics 294 (2023) 127036

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