Journal of Inorganic and Organometallic Polymers and Materials

https://doi.org/10.1007/s10904-022-02525-4

RESEARCH

Nanoarchitectonics of Silver/Poly (Methyl Methacrylate)

Films: Structure, Optical Characteristics, Antibacterial Activity,
and Wettability
Asmaa N. Mohammed Ali1 · Nadia A. Ali1 · Seenaa I. Hussein1 · A. Hakamy2 · Bahaaudin Raffah3 · Ayman S. Alofi4 ·
Alaa M. Abd‑Elnaiem5

Received: 19 December 2022 / Accepted: 29 December 2022

© The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2023

Abstract
Functionalizing organic–inorganic materials for use in packaging technologies, such as polymers wrapped in thin metal,
has proven to be one of the more successful strategies. In this study, the direct current (DC) sputtering technique under a
vacuum of 3 × ­10−5 Torr was used to deposit silver (Ag) films of thicknesses of 100 and 300 nm on poly (methyl methacrylate)
(PMMA) polymer. The structural, optical, antibacterial activity, and wettability properties of Ag/PMMA were carried out
using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), field emission scanning electron micro-
scope (FE-SEM), atomic force microscopy (AFM), UV spectrophotometer, and contact angle. The cubic crystal structure
phase of Ag was confirmed by the XRD. The Ag coating layer has consistent nanomorphology, according to AFM, and
the PMMA substrate surface was well coated with Ag nanoparticles. As the Ag film thickness rose, the optical band gap
values of Ag/PMMA slightly increased. In addition, it has been found that these optical characteristics such as extension
coefficient, optical density, and optical surface resistance essentially depend on the thickness of the Ag layers. Both samples
of pure PMMA and Ag/PMMA polymers show no activity against E. coli. In the meantime, S. aureus activity is detected
in the Ag/PMMA samples, and the antibacterial activity is slightly influenced by the Ag thickness. The contact angle rose
as the Ag film thickness grew over the PMMA, resulting in a decrease in the wettability of the liquid which is required for
food packaging technology.

Keywords  Nanosilver · PMMA · DC sputtering · Antibacterial activity · Optical · Wettability

1 Introduction

The polymer needs to be combined with other materials to

make polymer composites and/or covered with a metal thin
* Alaa M. Abd‑Elnaiem layer for a range of potential applications, such as optoelec-
abd-elnaiem@aun.edu.eg
tronic ones, food packaging, building, etc. [1–4]. Surface
A. Hakamy coating and engineering improve the performance of poly-
amhakamy@uqu.edu.sa
mers by using functionalized thin film coatings, making it
1
Department of Physics, College of Science, University suitable for applications such as energy harvesting, water
of Baghdad, Baghdad, Iraq purification, and dielectric layers, among others. The fol-
2
Department of Physics, Umm Al-Qura University, Mecca, lowing factors contribute to the importance of metal thin
Saudi Arabia layer fabrication over polymeric materials: lightweight, high
3
Department of Physics, Faculty of Sciences, King Abdulaziz shock resistance, and scalable roll-to-roll preparation tech-
University, Jidda 21589, Kingdom of Saudi Arabia niques [5]. Two common techniques can be used for incor-
4
Physics Department, College of Science, Taibah University, porating metallic nanoparticles into a polymer matrix, such
Medina, Saudi Arabia as the chemical synthesis approaches which mostly apply
5
Physics Department, Faculty of Science, Assiut University, to colloidal and metal–organic synthesis [6]. Another tech-
Assiut 71516, Egypt nique is the agglomeration of metal atoms over a substrate

13
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surface such as thermal evaporation, DC magnetron sputter-
ing, and pulsed laser deposition (PLD) [7]. The latter tech-
nique has been employed to form metal nanoparticles over
poly (methyl methacrylate) (PMMA) and Teflon [8]. The
PMMA is a thermoplastic polymer with good mechanical,
optical, and processability properties [9]. The PMMA is a
very translucent plastic with strong mechanical strength that
is utilized in a variety of applications ranging from com-
modities to industrial [10]. In addition, the PMMA is a pos-
sible substrate for medical nanotechnology including bone
cement, scaffolds for tissue engineering, etc. [11, 12]. The
PMMA surface may be modified using atomic layer deposi-
tion (ALD), layer-by-layer assembly, and a chemical depo-
sition process that allows for atomic-level control [12, 13].
Meanwhile, the PMMA is a problem for the ALD method as
its lacks active surface sites, which are required for gas pre-
cursor reactivity, nucleation, and subsequent development.
The PMMA composites, like other polymer composites, fre-
quently display superior mechanical and physical properties
when compared to pure PMMA [4]. Recently, the physical
and mechanical properties of certain polymer composites
have been improved by the oil palm fibers' cellulose com-
ponent [14].
Such a technique, i.e. DC sputtering is a thin film physi-
cal vapor deposition (PVD) coating technology, is applied
to produce various metal films due to its ease of use and
suitable speed [15]. In addition to DC sputtering, there are
various ways for producing metals nanostructured such as
Ag, Ni, and Au such as the sol–gel method, ALD, radio-
frequency (RF) magnetron sputtering, chemical vapor depo-
sition, spray pyrolysis, thermal evaporation and PLD [16,
17]. The PLD technique involves heating a solid material
to a specific temperature that creates some vapor pressure
and inside a high vacuum chamber to avoid the oxidation
process [18, 19]. Such an approach is utilized for coating
polymeric materials, but the poor thermal conductivity of
polymers limits thermal evaporation via resistive heating.
In addition, the breakdown of the molecule limits electron
beam evaporation of organic materials [20]. There are sev-
eral coatings of the thin layer were performed effectively
by thermal evaporation on polymeric substances including
polytetrafluoroethylene and nylon in the metal–polymer
nanocomposite [21].
Amongst the above-mentioned techniques, DC sputter-
ing was used to prepare the Ag-PMMA nanocomposites to
protect the PMMA against moisture, flavor, aroma, oxygen,
and oil [22]. Ag nanoparticles have played an essential role
in medicine nanotechnology due to their excellent antibacte-
rial activity against bacteria and eukaryotic microorganisms
[23]. Apart from its chemical stability, Ag is particularly
essential due to its unique features such as high conductiv-
ity, and antibacterial and catalytic activity. Ag nanoparticles
have been effectively employed in catalysis, electronics, and
13
Journal of Inorganic and Organometallic Polymers and Materials
optics depending on their particle size [24]. Currently, Ag
nanoparticles are used primarily as antibacterial and anti-
fungal agents in a variety of applications including bioen-
gineering, biotechnology, textiles, and water treatment, as
well as numerous consumer items using Ag [25]. Micro and
nanotechnologies based on novel systems that associate met-
als such as Ag nanoparticles with polymer matrices such as
PMMA qualify the new products to be applied as optoelec-
tronics devices [8]. The physical and chemical character-
istics of the formed composite materials can be controlled
by varying dopant particle size, particle distribution, and
particle form and shape [14, 26–28].
In most previous studies, Ag was doped or incorporated
into the PMMA polymer to improve its physical proper-
ties [1, 29–43]. The incorporation of Ag into the PMMA
polymer results in an excellent photoluminescence property,
making it suitable for nanophotonic devices [44]. The addi-
tion of Ag to PMMA reduced the polymer’s glass transition
temperature and altered its electrical properties [45, 46]. The
main problem with incorporating the Ag inside the polymer
material is that couldn’t be suitable to use for food packing
as the Ag nanomaterials could interact with food and unde-
sirable results could happen. Additionally, nanotechnologies
are used in food packaging to enhance packaging processes
by enhancing the properties of gas-leaking casings as well
as resistance to temperature and humidity during packaging
[47]. In general, Ag coatings on one side of the polymer
could offer antimicrobial qualities through the creation of
smart packaging to detect pathogens and sense biochemical
or microbial changes in food. This would allow for the moni-
toring of the product's safety concerning food [48].
Therefore, in the present study, we proposed covering
one side of the PMMA by the Ag layer using the DC sput-
tering technique. The structural characteristics, morphology,
optical properties, antibacterial activity, and wettability of
Ag films of thicknesses of 100 and 300 nm prepared by the
DC sputtering method on the PMMA substrates were inves-
tigated. The samples were evaluated utilizing a variety of
methodologies and data analysis to optimize the composites
for use in food packaging technologies, among other uses.
2 Experimental Procedures
PMMA was prepared by solving 1 g of PMMA in Chloro-
form ­(CHCl3) at 40 °C. The PMMA substrates then were
cleaned from impurities using acetone at 25 °C and agitated
with moderate ultrasonic power for 10 min. The estimated
thickness of the PMMA films is 110 ± 5 μm and was cut into
small square pieces with dimensions of 3 mm × 20 mm. The
fabrication of the PMMA substrate is shown schematically
in Fig. 1a.
Journal of Inorganic and Organometallic Polymers and Materials
Fig. 1  Schematic figures show
the fabrication of a PMMA
substrate and b DC magnetron
sputtering of Ag layer on the
PMMA substrate
The magnetron sputtering deposition of Ag on the
PMMA substrate is shown schematically in Fig. 1b. First,
the Ag metal ingots (diameter of 5 cm and a thickness of
1 mm) were placed in an inert crucible and the vacuum of
the chamber was adjusted to ­10–6 to 1­ 0–7 Torr. The distance
between the Ag target and PMMA substrates was kept con-
stant at 10 cm. The deposition of Ag was carried out at a
constant Ar pressure of 5 × ­10–3 mbar. To obtain different
thicknesses of Ag films, the deposition power was performed
at two different powers (50 and 100 W) for 2 h.
The thickness (t) of Ag films on PMMA substrates was
determined using the optical interferometer method and esti-
mated from t = 𝜆Δx2x
 , where x is the fringe width, Δx is the
distance between two fringes, and λ is the wavelength of
laser light (He–Ne laser 632 nm).
The XRD patterns of the deposited Ag films were
performed using a Shimadzu XRD-6000 diffractometer
equipped with Cu-Kα radiation in the diffraction angle
(2θ) range of 20–60°. The FTIR spectra for the Ag/PMMA
samples were recorded using a Shimadzu FTIR spectrom-
eter (Kyoto, Japan). A field emission scanning electron
microscope (FE-SEM) was used at an operating voltage of
20–30 kV, and the roughness behavior was scanned using
Gwyddion 2.45 software. Ultraviolet–Visible spectroscopy
(UV–Vis) model Shimadzu UV-1700 PharmaSpec Instru-
ment (Kyoto, Japan) was used to record the optical absorb-
ance through the Ag/PMMA samples. The analyzed Ag/
PMMA samples were examined using the model AA3000
atomic force microscope from Angstrom Advanced Inc.
in the United States. The contact angles were measured,
at room temperature, by a drop of water on an Ag/PMMA
substrate using a syringe pump device. During the meas-
urement, the pictures of the dropped water were taken at a
fixed time interval using a charge-coupled device camera.
The contact angles were measured on both view sides (left
and right) of the water drops, and then the average value
was considered.
The antibacterial effectiveness of the Ag/PMMA sam-
ples against the Staphylococcus aureus (S. aureus) and
Escherichia coli (E. coli) was evaluated using the diffusion
technique on the Mueller–Hinton agar. The micro-organism
unfolds on the surface of the agar. The agar plates were then
incubated at 37 °C for 24 h with 100 μl of the examination
samples placed in wells measuring 6 mm in diameter.
3 Results and Discussion
3.1 Structural Parameters
The thickness of Ag films was determined using: t = 𝜆Δx 2x
 ,
and found to be 100 ± 5 nm and 300 ± 10 nm at the DC sput-
tering deposition power of 50, and 100 W for 2 h, respec-
tively. Higher deposition power results in a greater deposited
thickness of Ag, which can be attributed to higher charged
particle concentration, and more high-energy reactants are
produced.
The chemical relationships and possible physical inter-
actions between Ag nanoparticles and PMMA polymer
were investigated using FTIR. Figure 2 shows the FTIR
for PMMA and Ag/PMMA with various Ag thicknesses.
In general, it is seen that the FTIR for pure PMMA and
Ag/PMMA samples are similar except one peak was
observed at 2000–2200  ­cm–1 for Ag/PMMA only. Pure
PMMA has a strong absorption at 1731  ­cm–1, which is
associated with C=O [49]. The C–H deformations are
responsible for the peaks at 1149 and 1192 ­cm–1. C–C–O
paired with C–O stretch is accompanied by those peaks
at 1242 and 1269 ­cm–1, respectively. Another bending and
stretching modes were observed such as bending modes at
1500–1350 ­cm–1, and the C–O stretching mode (1728 ­cm–1)
[50]. There are three bands in the 1350–1100 ­cm–1 region of
the spectrum, which have been belonging to the ester group
stretching [51]. The band that was observed at 843 ­cm–1 is
13
 Journal of Inorganic and Organometallic Polymers and Materials

Ag/PMMA_300nm
Ag/PMMA_300nm 294

196

98
Transmittance (arb. units)

Ag/PMMA_100nm 0
372
Ag/PMMA_100nm
279

Intensity
186

93
PMMA
0

180
PMMA

120

60
4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm–1) 0
0 5 10 15 20 25 30 35 40 45 50 55 60 65

Fig. 2  FTIR spectra of pure PMMA and Ag/PMMA of Ag thick- 2θ

nesses of 100 nm and 300 nm
belonging to the methylene rocking mode, whereas there
are some bands at 827 and 809 ­cm–1 associated with the
vibrations of the ester group, possibly the C–O–C symmetric
stretching mode [52]. In another hand, for the FTIR of Ag/
PMMA films observed peaks at 1240 ­cm–1 can be explained
owing to the C–O (ester bond) stretching vibration, and
peaks at 1641 ­cm–1 and 3307 ­cm–1 are assigned to C=C
stretching and O–H broadening stretching peak, respectively
[53]. The detected peak at 2000–2200 ­cm–1 was not present
in pure PMMA; it is possible that this peak was drawn to
the Ag nanoparticle rather than the PMMA polymer [54].
Generally, the FTIR spectra of pure PMMA and Ag/PMMA
exhibit comparable behavior. This finding is consistent with
other research and suggests that the contact between the Ag
nanoparticles and the PMMA polymer is most likely medi-
ated by a weak physical force as opposed to a strong chemi-
cal bond [55].
Figure 3 shows the XRD patterns of the PMMA and Ag/
PMMA samples. It is generally observed from the XRD
charts that the PMMA polymer is classified as a partially
amorphous polymer material that possesses no crystalline
structure. The observation of small peaks at 2θ equals 13°
and 23.7° agrees with other work elsewhere [56]. It is clear
that all the peaks in the XRD patterns of the Ag/PMMA
θ (°)
Fig. 3  XRD patterns of PMMA and Ag/PMMA samples of Ag thick-
nesses of 100 nm and 300 nm
samples interview similar patterns compared to the pure Ag
with a cubic crystal structure. The main observed diffrac-
tion peaks were provided by three main peaks located at 2θ
equals 38°, 44°, and 61° which are assigned to the Miller
indices or lattice planes of (111), (200), and (220), respec-
tively, which are well agreed with other work [57]. As the
thickness of the films increased from 100 to 300 nm, the
diffraction peaks shifted to a lower position. This observa-
tion is attributed to changes in the crystal structure's lattice
parameters, such as the lattice edge and unit cell volume.
The average crystallite size (D) was calculated using the
well-known Scherrer equation [58]: D = 𝛽cos(𝜃) K𝜆
 , as well as
𝜆
−𝛽
the microstrain (μ) [59]: 𝜇 = Dcos(𝜃)
 , and dislocation density
tan(𝜃)
(δ) [60]: 𝛿 = D12  , were estimated, where K is a constant close
to unity and 𝛽 is the full width of the peak at half maximum.
The numerical values for D, μ, and δ are determined to be
equal 11.65 nm, 0.87, and 7.4 × ­10−3 ­nm−2 for Ag/PMMA
films of a thickness of 100 nm, meanwhile equals 16.5, 0.37,
and 3.7 × ­10−3 ­nm−2 for Ag/PMMA films of a thickness of
300 nm, respectively. Furthermore, the crystallites number
for each unit area (Nc) is determined using the following

13
Journal of Inorganic and Organometallic Polymers and Materials
equation [60]: Nc = Dd3  , where d is the film thickness and D
is the average crystallite size. The value of Nc is equal to
6.3 × ­10−2 ­nm−2 and 6.7 × ­10−2 ­nm−2 for Ag/PMMA films of
thickness 100 nm, and 300 nm, respectively.
Figure 4 shows the top-view FE-SEM images for pure
PMMA polymer and Ag/PMMA films. The FE-SEM image
for pure PMMA polymer (Fig. 4a) shows a smooth and uni-
form surface without any morphology indicating the purity
of the PMMA substrate. The FE-SEM images presented in
Fig. 4b and c indicated that Ag film disperses in the PMMA
polymer with uniform distribution and formed mostly spher-
ical and slightly agglomerate. The surface morphology of
the Ag/PMMA samples reveals numerous clusters or chunks
that are randomly distributed.
Figure  5 shows the two-dimensional (2D) and three-
dimensional (3D) AFM images over 8.5 × 8.5 μm2 and
3.5 × 3.5 μm2 areas of the Ag layer over PMMA substrates of
a thickness of 100 nm and 300 nm, respectively. The image
has light and dark regions, where the light region represents
the highest points and the dark points are the depressions.
2D and 3D AFM images indicating that the nano-thin film
coating layer is uniform, and the substrate surface is well-
covered with nearly uniformly distributed. The average par-
ticle size was evaluated to be about 60 nm for the deposited
Ag nanoparticles and slightly affected by the Ag thickness.
The AFM scans show flat surfaces with few surface features,
such as root means square (RMS) roughness measurements
of 3.8 nm for Ag with a thickness of 100 nm and 3.9 nm
for Ag with a thickness of 300 nm, respectively. AFM soft-
ware was used to determine the sample's mean particle
size, roughness, surface area ratio, grain density, and height
profile. For Ag/PMMA with a layer thickness of 100 nm,
the estimated values of mean roughness, root mean square
roughness, surface area fraction, grain density, and height
profile equal 3.25 nm, 3.9 nm, 0.597, 31.9 μm2, and 21.8 nm,
Fig. 4  FE-SEM images of a PMMA, and Ag/PMMA samples of Ag thickness of b 100 nm and (c) 300 nm
respectively. Additionally, for Ag/PMMA with a layer thick-
ness of 300 nm, the values of mean particle size, roughness,
surface area, grain density, and height profile equal 3.2 nm,
3.82 nm, 0.555, 31.9 μm2, and 20.2, respectively.
In general, the AFM image in Fig. 5a shows a minimal
definition of cluster size for 100 nm film layers because
of the mobility of Ag atoms on the surface of the PMMA
polymer. The sample with the thin coating of Ag has a very
distinct surface morphology. The AFM picture in Fig. 5b
shows the 300 nm Ag's morphology and illustrates the pres-
ence of larger clusters that are more clearly defined as a
result of the significant Ag deposition. After deposition for
10 min, the homogenous structure the Ag coating layer was
obtained. The different particles gather on a small island
after 25 min of deposition to form a new sheet. The granules
enlarge with increasing thickness and may finally cluster to
form big grains, suggesting that the thickness rises with ris-
ing sputtering voltage and causes an increase in roughness.
3.2 Optical Properties
The UV–Vis absorbance spectra for pure PMMA and Ag/
PMMA samples in the range of 200–800  nm are illus-
trated in Fig. 6a. The absorption spectra for all investigated
samples were significantly decreased as the photon wave-
length was increased for a low wavelength (λ < 450 nm).
The decrease in the absorption has become a smaller for a
further increase in the wavelength. Meanwhile, the absorp-
tion was increased with an increase in the Ag film thickness
from 100 to 300 nm. The value of the observed absorption
shifted to higher values as an increase in the Ag thickness
which with well agrees with other work [24]. This observa-
tion is concluded as the Ag nanoparticle ions are combined
with the polymer chains, at the Ag and PMMA interface,
which absorb the incident radiation at the shortest wave-
lengths greater than 250  nm by the free electrons [61].
13

Fig. 5  2D and 3D AFM images of Ag layer over PMMA substrates of Ag thickness of a 100 nm and b 300 nm
The presence of the Ag layer or Ag coating on the PMMA
raised the absorption by ~ 21%. Additionally, the absorbance
increases with increased Ag layer thickness over PMMA,
which required for the application of food packaging.
Figure 6b shows the transmittance (T) as a function of
the wavelength (λ) for PMMA and Ag/PMMA films with
thicknesses of Ag equal to 100 nm and 300 nm. It can be
observed that the transmittance of the pure PMMA closed
to 100%, especially with an increased wavelength greater
than 425 nm. The existence of the Ag layer over the PMAA
polymer reduces the value of the transmittance through Ag/
PMMA, and its value was decreased with increasing Ag
layer thickness above the PMMA polymer. The transmit-
tance of the incident light especially at the shortest wave-
lengths decreases for Ag/PMMA. The presence of covalent
bonds between polymer chains and Ag additives in the Ag/
PMMA interface could explain the decrease in transmit-
tance [62]. Since the electrons in the external orbits have
traveled to higher energies and occupied vacant positions in
energy bands, some incident light doesn't transfer through
it. However, pure PMMA contains no free electrons, and the
conduction band requires high-energy photons.
13
Journal of Inorganic and Organometallic Polymers and Materials
The absorption coefficient, α, ­(cm–1) was estimated from
the following equation: 𝛼 = 2.303At
 , where A is the absorb-
ance and t is the thickness of the matter. Figure 6c shows
α ­(cm–1) versus λ for pure PMMA and Ag/PMMA films
with thicknesses of Ag equal to 100 nm and 300 nm. At low
energies (longer wavelengths), the ability of electron transi-
tion is limited because the energy is insufficient to assist
this electron in transferring from the valence band to the
conduction band, or less than the optical bandgap ( Eg ). On
the other hand, absorption is high for high photon energies,
which means that there is a high possibility of electron tran-
sitions from the valence band to the conduction band. In
such cases, the energy of the incident photon is sufficient to
help the electron travel from the valence band to the conduc-
tion band, or the energy of the incident photon is greater than
the energy gap. It thus demonstrates that the absorption coef-
ficient aids in determining the nature of electron transitions,
as the coefficient of absorption for the Ag/PMMA film less
than ­104 ­cm−1 indicates that transitions are indirect.
Figure 7 shows the plots between (αhυ)1/2 and photon
energy (hυ) for Ag/PMMA film. The plots are fitted to
straight lines from the upper part of the curve toward the (x)
Journal of Inorganic and Organometallic Polymers and Materials

(a) 3.2
(b)
PMMA 98.8
3.0 Ag/PMMA_100nm
98.6
2.8 Ag/PMMA_300nm
98.4
2.6

Transmittance (%)
98.2
2.4
Absorption

98.0
2.2
97.8
2.0
97.6
1.8
97.4
1.6
97.2
PMMA
1.4
97.0 Ag/PMMA_100nm
1.2 Ag/PMMA_300nm
96.8
300 400 500 600 700 800 300 400 500 600 700 800

λ (nm) λ (nm)

(c)
PMMA
0.07
Ag/PMMA_100nm
Ag/PMMA_300nm

0.06
α (cm–1)

0.05

0.04

0.03

300 400 500 600 700 800

λ (nm)

Fig. 6  a Absorption (A), b transmittance (T), and (c) Absorption coefficient (α) versus wavelength (λ) for PMMA and Ag/PMMA samples

axis that is calculated using: 𝛼h𝜐 = k(h𝜐 − Eg )1∕2 , where h

is the Planck constant, ν is the radiation frequency, and k is
a constant. According to the excellent linear fitting observed
in Fig. 7, the photon transition from the valence band to
the conduction band obeyed the allowed indirect transition
mode. At the value (αhυ)1/2 = 0, the value of Eg for the inves-
tigated polymers can be determined. The value of Eg was
found to increase from 2.3 ± 0.1 eV for the pure PMMA
polymer to 2.7 ± 0.1 and 2.8 ± 0.1 eV for Ag/PMMA sam-
ples of Ag thickness of 100 nm, and 300 nm, respectively.
The observed increase in Eg could be attributed to the crea-
tion of the interface region between the Ag layer and PMMA
substrate. The values of optical band gaps were typically
found to be lower in Ag-PMMA nanocomposites than in
pure PMMA polymer, and this was explained by the devel-
opment of local states inside the optical band gap [51, 61].
Fig. 7  (𝛼h𝜐)2 versus h𝜐 for PMMA, and Ag/PMMA samples

13

Contrarily, the optical band gap in this investigation was
larger for the Ag/PMMA samples than for the pure PMMA
polymer, and this finding may be related to the development
of an interface layer between the Ag layer and PMMA sub-
strate. The average crystallite size is well known to be highly
dependent on the thickness of the coated layer. If charges
accumulate at grain boundaries and interfaces, the band gap
of metal films is expected to increase. The decrease in the
band gap as Ag thickness increases indicates that there is
no charge accumulation at grain boundaries in Ag/PMMA
interface. The change in the optical band gap matches the
estimated crystallite size from the XRD analysis perfectly.
In other words, the smaller crystallite sizes observed for
100 nm Ag demonstrate a smaller optical band gap.
Further discussion of optical properties is conducted
using the computation of optical density (O.D), which
(a)
(c)
Fig. 8  a optical density (O.D), b extension coefficient ­(kex), and c optical surface resistance ­(Rs) values versus the wavelength (λ) for PMMA and
Ag/PMMA samples
13
Journal of Inorganic and Organometallic Polymers and Materials
describes the transmission of photons through matter. The
processes of absorption and emission are created when inci-
dent electromagnetic waves interact with particles such as
electrons, ions, and atoms. To determine the values of O.D
for produced thin films of a thickness (d), utilize equation
[63]: O.D = −log10 (T(𝜆)) = 0.434 × 𝛼(𝜆) × d  . It should be
noted that, as shown in Fig. 8a, the T(λ) of the produced thin
film has a significant impact on the value of O.D. The gener-
ated data show that optical density decreases as wavelength
increases. The value of O.D drops when Ag is deposited
with a thickness of 100 nm; nevertheless, it increases when
the thickness reaches 300 nm. Other optical characteristics,
including extension coefficients (­ kex), are essential for inves-
tigating optical materials and their performance. The values
of ­kex (λ) can be roughly determined using the following
equation [64]:kex = 𝜀0 × 𝛼(𝜆) × 𝜆 = 𝛼(𝜆)×𝜆 4𝜋
 , where 𝜀0 is the
(b)
Journal of Inorganic and Organometallic Polymers and Materials

permittivity of free space. The dependence of k­ ex on the λ of

incident electromagnetic (EM) waves was shown in Fig. 8b
for investigated samples. One can see that the value of k­ ex
decreases as the thickness of the Ag layer increases from 100
to 300 nm and increases when the λ incident EM wave inten-
sity increases. The static refractive index (n), another sig-
nificant optical property, can be calculated from ­Eg using the
empirical√ method developed by Ravindra and Srivastava
[64]: n = 4 108
Eg
 . The estimated values of n for PMMA and
Ag/PMMA samples are 2.6, 2.5, and 2.49, respectively. It is
observed that films with a wide optical band gap have a
lower static refractive index. The static refractive index is
almost exactly twice as high as the refractive index of glasses
made of silicon oxide. The estimated n can be used to evalu-
ate the optical surface resistance ­(R s ) using [65]:
Rs = −4𝜋
c
1
× nln(T)  , where c is the speed of light in a vacuum,
and n is the static refractive index. The deposition of Ag on
PMMA causes enhancement in the R ­ s value, while the
increase in Ag thickness causes a reduction in the R ­ s value
as shown in Fig. 8c. The Ag/PMMA samples' behaviors in
terms of optical parameters including extension coefficient, Fig. 9  Contact angle for a PMMA and Ag/PMMA samples of Ag
optical density, and optical resistivity follow similar trends thickness of b 100 nm, and c 300 nm
to those of other materials such as chalcogenide glasses
semiconductors [63, 64].
increases its hydrophobicity. The mean contact angle with
3.3 Wettability Ag particles was greater than the borderline value, indicating
that water behaved as a poor wetting liquid on the PMMA
It is generally known that the word "hydrophobicity" is surface covered by larger Ag particles. The hydrophilicity of
used in physics to characterize a molecule's physical char- Ag surface molecules hydrophilic molecules forms ionic or
acteristic that causes it to be pushed away (repelled) from hydrogen bonds with water molecules. Therefore, when Ag
water. Water molecules have a wide angle of contact with nanoparticles are exposed to the environment, they oxidize
hydrophobic surfaces, but most hydrophobic compounds and become contaminated. Such oxides are susceptible to
are nonpolar [66]. One industry where these hydrophobic hydrogen bonding with environmental moisture. Accord-
overlays are useful is packaging, whether it be for the food ingly, the bonds have become stronger, and hence water
or industrial sectors [67]. In addition, water is one of the prefers to wet the surface, making Ag more hydrophilic.
conditions that is considered to be the most important for The PMMA surface is hydrophilic based on the values
the growth of bacteria [68]. To stop bacterial development, of the contact angle, but after coating with Ag, it became
the coatings with metallic materials could change the surface hydrophobic which is helpful when applying coatings. Mois-
from hydrophilic to hydrophobic [69]. ture and dampness have been eradicated using the coating
Wettability was determined through the evaluation of the process. This technique eliminates moisture, which when
contact angle and surface free energy estimation using the packaging creates an ideal habitat for the growth of mold
contact angle hysteresis approach [70]. Figure 9 presents the and bacteria as we discussed in the next section.
water contact angle values measured for the PMMA poly-
mer with a contact angle is 58.5° ± 0.4° (intrinsic contact 3.4 Evolution of Antibacterial Activity
angle below 90°) which means a hydrophilic surface [70].
In addition, when the PMMA polymer was coated with Ag In this section, samples of pure PMMA and Ag/PMMA were
led for obtaining a more hydrophobic property of the formed tested for antibacterial activity using the pour plate method.
films. The contact angle was increased from 76 ± 0.1° to Figure 10 displays the results of the evaluation of the zones
83.4 ± 0.6° as the thickness of the Ag layer was increased of inhibition of the generated PMMA and Ag/PMMA sam-
from 100 to 300 nm for Ag/PMMA samples. ples toward E. coli and S. aureus bacteria. These bacteria
The mean contact angles were estimated to be less are chosen over others because of how they affect food and
than 90°, indicating that the addition of Ag to the PMMA cause food poisoning. Figure 10 displays that pure PMMA

13
 Journal of Inorganic and Organometallic Polymers and Materials

Fig. 10  Photograph images
showing Escherichia coli (E.
coli) and Staphylococcus aureus
(S. aureus) bacteria inhibition in
the presence of a pure PMMA,
and Ag/PMMA samples with
Ag thickness of b 100 nm, and
c 300 nm

membranes did not show any antibacterial activity against of the results attained in the present investigation. The thick-
the tested bacteria. ness of the Ag layer over the PMMA substrate is typically
E. coli and S. aureus exhibit no inhibitory zones on pure found to have a significant impact on the structural char-
PMMA polymer. Similar to this, neither of the Ag/PMMA acteristics, optical parameters, wettability, and ultimately
samples exhibits an inhibitory zone for E. coli, whereas S. bacterial activity. The size of the crystallites increases as
aureus does. For Ag thicknesses of 100 nm and 300 nm, the Ag thickness increases. Additionally, the greater absorption,
inhibition zone sizes for Ag/PMMA are 11 mm ± 0.5 mm optical density, lesser transmittance, and extension coeffi-
and 12 mm ± 0.5 mm, respectively. The PMMA membrane cient were seen when the Ag thickness increased. Moreo-
covered by 100 and 300 nm of Ag layer had shown anti- ver, as the thickness of the Ag increases, the wettability
bacterial activity against S. aureus only. Similar to prior decreases, boosting bacterial activity.
research using Ag/PVA/PMMA nanofiber, the Ag/PMMA
films exhibit high biocidal activity against the Gram-positive
bacterium S. aureus [37]. The Ag targets bacterial metabo- 4 Conclusion
lism by binding to its DNA, proteins, and enzymes; resulting
in bacteriostatic effects. The presence of the Ag layer over The DC sputtering technique was used to form Ag films of
the PMMA destabilizes and disrupts both the outer and cyto- thicknesses of 100 and 300 nm on PMMA polymer sub-
plasmic membranes. In addition, the Ag layer inhibits the strates. The PMMA's crystal structure was somewhat amor-
respiratory chain enzymes and can stimulate the production phous, whereas Ag/PMMA films formed a cubic crystal
of reactive oxygen species. In addition, the ­Ag+ ions released structure. The AFM shows the creation of homogenous Ag
from Ag nanoparticles can attach directly to cell surfaces nanoparticles over the PMMA with an average particle size
and change the membrane permeability resulting in attack-
ing the bacterial cells. Ag nanoparticles have low toxicity as
compared to other metal nanoparticles which makes them a
suitable choice for commercial food packages. Moreover, Ag
has antimicrobial properties and can be easily incorporated
into polymers that are used for packaging [71]. It is evident
that as compared to pure PMMA, both Ag/PMMA mixtures
exhibit enhanced antibacterial activity against the two tested
pathogens. In the literature, the bacterial activity of polymer/
metal nanocomposites to demonstrate antibacterial activities
and their underlying processes based on Cu and Ag metal
nanoparticles was reported [72]. Another study showed how
Escherichia coli bacteria were affected by the insertion of
Ag in the PMMA matrix [73].
Figure 11 shows the impact of Ag thickness on the exam- Fig. 11  Dependent trend of structure, optical, wettability and bacteria
ined properties and parameters and summarizes the majority activity on the thickness of the Ag layer in the Ag/PMMA samples

13
Journal of Inorganic and Organometallic Polymers and Materials
of around 60 nm, and the substrate surface is thoroughly
covered with nearly equally dispersed nanoparticles, espe-
cially for thicker films. As the film thickness rose, the optical
band gap values of Ag films declined and were smaller than
the optical band gap of pure PMMA polymer. The pres-
ence and thickness of the Ag layer over the PMMA polymer
are affected by optical transmittance, absorbance, extension
coefficient, optical density, surface resistance, and absorp-
tion coefficient. Ag/PMMA and pure PMMA polymer sam-
ples both exhibit no action against E. coli. The antibacterial
activity is marginally impacted by the Ag thickness while S.
aureus activity is found in the Ag/PMMA samples. The wet-
tability, bacterial activity test, and contact angle demonstrate
that the Ag/PMMA film grew more hydrophobic, indicating
that it might be utilized for food packaging.
Acknowledgements  The authors would like to thank the Deanship of
Scientific Research at Umm Al-Qura University for supporting this
work by Grant Code (22UQU4250045DSR27).
Author Contributions  ANMA: Data curation; methodology; writing
the original draft. NAA: Investigation; methodology; writing the origi-
nal draft. SIH: Investigation, Formal analysis; resources, writing the
original draft. AH: Data curation; formal analysis; investigation, writ-
ing the original draft. AMA‑E: Data curation; methodology; writing
the original draft. All authors have read, revised, and agreed to the
published version of the manuscript.
Funding  This work is funded by the Deanship of Scientific Research
at Umm Al-Qura University Grant Code (22UQU4250045DSR27).
Data Availability  Not applicable.
Declarations  laser ablation (PLAL). Nano Biomed. Eng 14, 15–22 (2022)
Competing Interests  The authors declare that they have no conflict
of interest.
Ethical Approval  Not applicable.
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