COPPER AT SILICA CORE - SHELL
NANOPARTICLES AS ANTIBACTERIAL
AGENTS BY SOL-GEL CHEMICAL METHODS
Al- Ajeeli, Alaa F. Hashim
Department of Physics, College of Education for Pure Sciences, Tikrit University,
Salahuddin, Iraq
alaa.f.hashim@st.tu.edu.iq - https://orcid.org/0000-0003-3688-0663
Razeg, Khalid Hamdi
Department of Physics, College of Education for Pure Sciences, Tikrit University,
Salahuddin, Iraq
khalid.hr55@tu.edu.iq
Fuad Tariq Ibrahim
Department of Physics, College of Science, University of Baghdad, Baghdad, Iraq
Reception: 24/11/2022 Acceptance: 09/01/2023 Publication: 02/02/2023
Suggested citation:
A. A., Alaa F. Hashim, R., Khalid Hamdi and F. T., Ibrahim, (2023). Copper At
Silica Core - Shell Nanoparticles As Antibacterial Agents By Sol-Gel
Chemical Methods. 3C Tecnología. Glosas de innovación aplicada a la
pyme, 12(1), 337-352. https://doi.org/10.17993/3ctecno.2023.v12n1e43.337-352
https://doi.org/10.17993/3ctecno.2023.v12n1e43.337-352
3C Tecnología. Glosas de innovación aplicadas a la pyme. ISSN: 2254-4143
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ABSTRACT
Core-shell Cu@sio2 nanoparticles were created by a chemical reaction in a sol gel,
and their ability to inhibit S. aureus and E. coli bacteria was tested, when synthesized
and characterized using ultraviolet-visible spectroscopy, a copper band could be seen
before and after encapsulation at wavelengths of 625 nanometers and 635
nanometers, which are surface plasmonic resonant frequency bands, respectively.
The production of Cu @Sio2 core shell nanoparticles was further confirmed using field
emission scanning electron microscope (FESEM) pictures. The core shell
nanoparticles have a mean size of 66 nanometers and a spherical shape, as shown in
TEM. The X-ray diffraction patterns for the nanoparticles, which show face-centered
cubic (FCC) of copper, match the crystal structure of Cu@sio2 we discovered using
fourier transform infrared (FT-IR) spectroscopy, the fourier transform infrared
interaction between the silica and the synthesized copper NPs was investigated. This
revealed the capping of the CuNPs by SiO2. The inhibition zone was evident as a
result of the activities of these compounds (14, 14, 16, and 20) and (24, 24, 28, and
30) against Escherichia coli bacteria and Staphylococcus aureus bacteria,
respectively.
KEYWORDS
Copper Nanoparticle, Silica, Antibacterial, Inhibition Zone.
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ABSTRACT
Core-shell Cu@sio2 nanoparticles were created by a chemical reaction in a sol gel,
and their ability to inhibit S. aureus and E. coli bacteria was tested, when synthesized
and characterized using ultraviolet-visible spectroscopy, a copper band could be seen
before and after encapsulation at wavelengths of 625 nanometers and 635
nanometers, which are surface plasmonic resonant frequency bands, respectively.
The production of Cu @Sio2 core shell nanoparticles was further confirmed using field
emission scanning electron microscope (FESEM) pictures. The core shell
nanoparticles have a mean size of 66 nanometers and a spherical shape, as shown in
TEM. The X-ray diffraction patterns for the nanoparticles, which show face-centered
cubic (FCC) of copper, match the crystal structure of Cu@sio2 we discovered using
fourier transform infrared (FT-IR) spectroscopy, the fourier transform infrared
interaction between the silica and the synthesized copper NPs was investigated. This
revealed the capping of the CuNPs by SiO2. The inhibition zone was evident as a
result of the activities of these compounds (14, 14, 16, and 20) and (24, 24, 28, and
30) against Escherichia coli bacteria and Staphylococcus aureus bacteria,
respectively.
KEYWORDS
Copper Nanoparticle, Silica, Antibacterial, Inhibition Zone.
https://doi.org/10.17993/3ctecno.2023.v12n1e43.337-352
PAPER INDEX
ABSTRACT
KEYWORDS
1. INTRODUCTION
2. EXPERIMENTAL PARTS
2.1. SOL-GEL PROCESS
2.2. CHARACTERIZATION TECHNIQUES
2.3. EQUATIONS USED TO ANALYSIS THE XRAY RESULTS.
2.4. TESTING FOR ANTIMICROBIAL EFFECTIVENESS
3. 3. RESULTS AND DISCUSSION
3.1. X-RAY DIFFRACTION
3.2. UV VISIBLE SPECTROSCOPY
3.3. FTIR
3.4. TEM.
3.5. FeSEM-EDX
4. EVALUATION OF ANTIBACTERIAL
4.1. ACTIVITY OF THE CORE-SHELLS
5. CONCLUSIONS
REFERENCES
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1. INTRODUCTION
The modern concepts for producing nanoparticles with the required size and form
are developing as, science and technology grow more quickly, particularly in the fields
of nanotechnology and material science. [1-4] Metallic nanoparticles are gaining
popularity due to their different physical and chemical characteristics, as well as their
wide variety of applications. There is an increase in interest in working with metals,
polymer particles, metallic nanoparticles, etc. because of they have several
applications in material science due to their tiny size and a huge interaction surface.
surrounding medium affects the features of nanoparticles, and the necessary
attributes can be introduced by changing the ambiance. The scientific discipline of
nanotechnology has enormous promise for use in medicine. Because nanoscience
and biology are comparable to nature, their combination will not only help in the battle
against harmful microbes, but may also lead to a shift in how infectious disease is
treated. [5] [6] Numerous biomedical, and pharmaceutical fields, including diagnostics,
genetic engineering, drug delivery, biomarkers, bioimaging, cosmetics, antibacterial,
cancer, immunology, cardiology, cancer treatment, bioremediation, water treatments,
energy production, and other infectious diseases, can benefit from the use of
nanoparticles. [7-9] Paints typically contain different metals and metal oxides as NPs
because they have antifungal, anti-algal, and antibacterial effects. Exhibiting water
resilience, fewer toxic effects, and antibacterial capabilities through attaching to
bacterial cell proteins. [10]
There are generally two ways to synthesize nanoparticles of Sio2. Since silica has
been widely used as an efficient anticorrosive protective material, numerous attempts
have been made to coat metal nanoparticles with silica shells of customizable
thickness. Due to its excellent compatibility with various materials, great chemical and
thermal stability, and huge surface area, silica is a very important material. SiO2 with
copper exhibited excellent corrosion resistance [11] Multi-infectious bacteria can
produce antimicrobial resistance by adhering to various substrates like medical
equipment or biological surfaces like host organism and forming sticky exopolymeric
substances (EPS) called microbial biofilms [12].
Copper nanoparticles are reported to be more efficient than iron oxide and nickel
nanoparticles in the attack against pathogenic bacteria that produce biofilms and
multidrug resistance. Copper and copper oxide nanoparticles exhibit antibacterial
efficacy against the microorganism's Staph aureus, E. coli, Pseudomonas aerugi, and
B. subtilis the microorganism's Bacillus nosa that produce biofilms. [13-16].
Copper nanoparticles are useful for a variety of purposes, including medicinal,
agricultural, and other industries, and they are inexpensive, these include antifungal,
antiviral, antibiotic, anticancer, and photocatalytic uses[17].
In this study, Cu@Sio2
core-shell nanoparticles are fabricated using the chemical
sol-gel method [18-19]. Ultrasound is used to disperse copper nanoparticles before
mixing them with silica. The final spherical Cu@Sio2
core -shell the spherical shape
was observed as well as measuring the antibacterial activities of Escherichia coli and
Staphylococcus aureus bacteria.
https://doi.org/10.17993/3ctecno.2023.v12n1e43.337-352
3C Tecnología. Glosas de innovación aplicadas a la pyme. ISSN: 2254-4143
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1. INTRODUCTION
The modern concepts for producing nanoparticles with the required size and form
are developing as, science and technology grow more quickly, particularly in the fields
of nanotechnology and material science. [1-4] Metallic nanoparticles are gaining
popularity due to their different physical and chemical characteristics, as well as their
wide variety of applications. There is an increase in interest in working with metals,
polymer particles, metallic nanoparticles, etc. because of they have several
applications in material science due to their tiny size and a huge interaction surface.
surrounding medium affects the features of nanoparticles, and the necessary
attributes can be introduced by changing the ambiance. The scientific discipline of
nanotechnology has enormous promise for use in medicine. Because nanoscience
and biology are comparable to nature, their combination will not only help in the battle
against harmful microbes, but may also lead to a shift in how infectious disease is
treated. [5] [6] Numerous biomedical, and pharmaceutical fields, including diagnostics,
genetic engineering, drug delivery, biomarkers, bioimaging, cosmetics, antibacterial,
cancer, immunology, cardiology, cancer treatment, bioremediation, water treatments,
energy production, and other infectious diseases, can benefit from the use of
nanoparticles. [7-9] Paints typically contain different metals and metal oxides as NPs
because they have antifungal, anti-algal, and antibacterial effects. Exhibiting water
resilience, fewer toxic effects, and antibacterial capabilities through attaching to
bacterial cell proteins. [10]
There are generally two ways to synthesize nanoparticles of Sio2. Since silica has
been widely used as an efficient anticorrosive protective material, numerous attempts
have been made to coat metal nanoparticles with silica shells of customizable
thickness. Due to its excellent compatibility with various materials, great chemical and
thermal stability, and huge surface area, silica is a very important material. SiO2 with
copper exhibited excellent corrosion resistance [11] Multi-infectious bacteria can
produce antimicrobial resistance by adhering to various substrates like medical
equipment or biological surfaces like host organism and forming sticky exopolymeric
substances (EPS) called microbial biofilms [12].
Copper nanoparticles are reported to be more efficient than iron oxide and nickel
nanoparticles in the attack against pathogenic bacteria that produce biofilms and
multidrug resistance. Copper and copper oxide nanoparticles exhibit antibacterial
efficacy against the microorganism's Staph aureus, E. coli, Pseudomonas aerugi, and
B. subtilis the microorganism's Bacillus nosa that produce biofilms. [13-16].
Copper nanoparticles are useful for a variety of purposes, including medicinal,
agricultural, and other industries, and they are inexpensive, these include antifungal,
antiviral, antibiotic, anticancer, and photocatalytic uses[17].
In this study, Cu@Sio2 core-shell nanoparticles are fabricated using the chemical
sol-gel method [18-19]. Ultrasound is used to disperse copper nanoparticles before
mixing them with silica. The final spherical Cu@Sio2 core -shell the spherical shape
was observed as well as measuring the antibacterial activities of Escherichia coli and
Staphylococcus aureus bacteria.
https://doi.org/10.17993/3ctecno.2023.v12n1e43.337-352
2. EXPERIMENTAL PARTS
2.1. SOL-GEL PROCESS
Synthesis of Copper Nanopowder in Chemical Sol Gel (average particle size 30
nanometer ≥
99.9%), (TEOS) tetraethylorthosilicate 98%, 0.5 mol (Merck), ethyl
alcohol (99.9%), ascorbic acid (99%), cetyltrimethylammonium bromide ≥98%, NH3
ammonium hydrate (25%), also utilized was deionized water.
Experiment was carried out 24C° temperature. Shows the composition of core-shell
used in the experiment. The technique of synthesizing core-shell is as follows. First,
the copper solution is made up of 180 mg of Cu nanopowder combined with 10 ml of
distilled water, (0.004 M) cetyltrimethylammonium bromide (CTAB) diluted in 10 ml of
water, and (0.02 M) ascorbic acid mixed in 20 ml of water. and fully dispersed with
ultrasound. Then, while stirring, 32.0 ml of ethanol and 0.5 ml of TEOS were
combined. 1.5 ml of ammonium hydroxide was combined after stirring for around one
hour and the reaction was then completed after another 24 hours of stirring. The core-
shell nanoparticles underwent multiple filtering and washing steps using distilled water
and ethanol.lastlly,80 °C was used to dry powder to produce Cu@sio2 core-shell.
2.2. CHARACTERIZATION TECHNIQUES
Utilizing X-ray diffraction, Cu@SiO2 core-shell peaks were verified. (XRD; Cu, 30
kV, 15 milliampere); Rigaku Corporation), To make specimens, the sol-gel-fabricated
core-shells were disseminated in ethanol. The core-shell shapes were verified using a
transmission electron microscope and fesem. Then, measurements using energy
dispersive X-ray spectroscopy (EDS) produced to confirm the production of the SiO2
shell and Copper nanopowder core. The following techniques were used to
characterize the prepared Cu @Sio2 core shell nanostructures.
2.3. EQUATIONS USED TO ANALYSIS THE XRAY RESULTS.
According to the findings of the XRD examination, the Bragg law Equation (1) was
used to compute the d-spacing (the lattice planes distance between the atoms), and
the Debye-Scherrer Equation was used to calculate the average crystallite size. (2)
(1)
where d is the interplanar distance between atoms, n is an integer (n= 1), and k is
an integer (k= 0.15418 nanometer for Cu Ka).
(2)
where K is a constant number factor (0.89), λ= 0.15418 nanometers for Cu Ka,
FWHM is the full width at half maximum, is the diffraction angle, and ( ) is the lattice
constant, while D is the average crystallite size. ( ) For cubic crystals was calculated
by Equation (3) [17]
2d sinθ=nλ
D=
Kλ
F WHM COSθ
θ
a
a
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(3)
Miller's index (h k l) represents cartesian coordinates for cubic crystals.
2.4. TESTING FOR ANTIMICROBIAL EFFECTIVENESS
The antibacterial capabilities of the composite membrane were tested using the
diffusion method against the gram-positive bacterium. Staphylococcus aureus and
gram-negative bacteria a kind of bacteria called Escherichia coli. [20]. A disk-shaped
test specimen and an untreated control were created with a 10 mm diameter and
sterilized in an autoclave for 15 minutes at 120 °C for the disk diffusion procedure.
After that, they were placed on individual agar media with E. coli and S. aureus
cultures and for 24 hours at 37 °C while the inhibitory zone was monitored.
3. 3. RESULTS AND DISCUSSION
3.1. X-RAY DIFFRACTION
Among the most effective and simple methods for determining out a compound's
crystallite properties is X-ray diffraction (XRD). XRD analysis of synthesized copper
nanopowder using ascorbic acid and CTAB as stabilizing and reduction agents,
confirmed that the finished item is made of metal. The Cu-NPs' XRD patterns are
depicted in Fig. 1, and they are very comparable to those seen in JCPDS Copper.
04-0836 (43.6, 50.8, and 74.4) correspond to the metallic Cu planes (111), (200), and
(220). The outcome of XRD examination shows that the produced Cu-NPs have a
face-centered cubic structure (FCC), in addition to copper peaks, other X-ray
diffraction peaks appear after the process of coating the metal with silica figure 2
depicts the Cu@sio2 core shell's XRD pattern. nanostructure as it was created using
the sol-gel process. Peaks seen at 2θ
values of 21.4, 22.59, 31.8, 45.54, 53.97,
54.55, 56.6, 66.15 and 75.47 correspond to (002), (211), (600), (332), (440),(404),
(620),( 325)and (435) planes of Cu@Sio2
. These peaks were quite comparable to
those of the standard JCPDS Card No. 045-0131 for the sio2 [21].
The JCPDS (Joint Committee on Powder Diffraction Standards) was used to
calculate the broadening of the diffraction peaks matching to the strongest reflections,
which indicates the mean size of nanocrystals. From the XRD diffraction pattern
observed for nanoparticles, the Scherrer equation was applied to calculate the
crystallite size.
The results of the XRD examination show that the Cu-NPs that were created had a
structure with a face-centered cubic (FCC) with a lattice constant of 0.36 nanometers
that matches well with the standard lattice parameter (a = 0.3615 nanometers).
JCPDS card no, 04-0836, the average size of copper crystals and cu@sio2
nanoparticles(D) calculated by using equ.1, the Scherrer equation were about 47.08
and 58.9 respectively [21].
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(3)
Miller's index (h k l) represents cartesian coordinates for cubic crystals.
2.4. TESTING FOR ANTIMICROBIAL EFFECTIVENESS
The antibacterial capabilities of the composite membrane were tested using the
diffusion method against the gram-positive bacterium. Staphylococcus aureus and
gram-negative bacteria a kind of bacteria called Escherichia coli. [20]. A disk-shaped
test specimen and an untreated control were created with a 10 mm diameter and
sterilized in an autoclave for 15 minutes at 120 °C for the disk diffusion procedure.
After that, they were placed on individual agar media with E. coli and S. aureus
cultures and for 24 hours at 37 °C while the inhibitory zone was monitored.
3. 3. RESULTS AND DISCUSSION
3.1. X-RAY DIFFRACTION
Among the most effective and simple methods for determining out a compound's
crystallite properties is X-ray diffraction (XRD). XRD analysis of synthesized copper
nanopowder using ascorbic acid and CTAB as stabilizing and reduction agents,
confirmed that the finished item is made of metal. The Cu-NPs' XRD patterns are
depicted in Fig. 1, and they are very comparable to those seen in JCPDS Copper.
04-0836 (43.6, 50.8, and 74.4) correspond to the metallic Cu planes (111), (200), and
(220). The outcome of XRD examination shows that the produced Cu-NPs have a
face-centered cubic structure (FCC), in addition to copper peaks, other X-ray
diffraction peaks appear after the process of coating the metal with silica figure 2
depicts the Cu@sio2 core shell's XRD pattern. nanostructure as it was created using
the sol-gel process. Peaks seen at 2θ values of 21.4, 22.59, 31.8, 45.54, 53.97,
54.55, 56.6, 66.15 and 75.47 correspond to (002), (211), (600), (332), (440),(404),
(620),( 325)and (435) planes of Cu@Sio2. These peaks were quite comparable to
those of the standard JCPDS Card No. 045-0131 for the sio2 [21].
The JCPDS (Joint Committee on Powder Diffraction Standards) was used to
calculate the broadening of the diffraction peaks matching to the strongest reflections,
which indicates the mean size of nanocrystals. From the XRD diffraction pattern
observed for nanoparticles, the Scherrer equation was applied to calculate the
crystallite size.
The results of the XRD examination show that the Cu-NPs that were created had a
structure with a face-centered cubic (FCC) with a lattice constant of 0.36 nanometers
that matches well with the standard lattice parameter (a = 0.3615 nanometers).
JCPDS card no, 04-0836, the average size of copper crystals and cu@sio2
nanoparticles(D) calculated by using equ.1, the Scherrer equation were about 47.08
and 58.9 respectively [21].
a=d h2+k2+l2
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Figure 1. XRD patterns of CuNps
Figure 2. XRD patterns of silica-coated Cu nanoparticles
3.2. UV VISIBLE SPECTROSCOPY
Small metallic nanoparticles exhibit visible electromagnetic wave absorption
through surface-based collective conduction electron oscillation [18]. The surface
plasmon resonance effect is what's happening here. The advantage of this effect is
that it can be used as a tracer for the presence of metallic nanoparticles with a
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straightforward UV-visible spectrometer, as demonstrated by the size dependence of
the plasmonic resonance of the absorption of copper nanoparticles and core-shell
particles of copper / silica prepared by chemical sol-gel method.The results from UV-
visible demonstrate a red shift in the absorption spectra caused by the increase in
particle size caused by the increased silica coating that the synthesis of Cu@SiO2
nanostructure exhibited in the figure displayed SPR peak at 635 nanometer, when it
was at the wavelength of 630 nanometer for cu nanoparticles. Fig:3
Figure 3. UV-vis absorption spectra for Cu and Cu @Sio2
3.3. FTIR
The FTIR spectra of silica (Sio2) fig:3a and 3b Cu @ Sio2
.The wide band at 3356
cm-1
in the FTIR of Sio2 corresponds to the O-H stretching vibration. of the
condensation of a silanol group (Si-OH) as well as the residual absorbed water in the
FTIR spectra of SiO2 and Cu @ Sio2 in Figure. Water molecules' bending and
vibrations as they absorbed into the surface of the silica particles caused a small peak
at 1666 cm-1. [22].
There were characteristic peaks at 1029 cm-1, 794 cm-1, and 474 cm-1, which
represented, respectively, the bending oscillation of O-Si-O, the asymmetrical
extending vibration of Si-O-Si, and the symmetric stretching vibration of O-Si-O [23].
The vibrations of the silanol groups stretching are connected with the band at 1029
cm-1,while the peak at 1396 cm-1
is connected to the stretching of the Si-O bond [22].
Similar to the Sio2 spectrum, FTIR spectrum of cu @ sio2
nanoparticles in Figure4b
likewise showed typical vibrations, but peaks were displaced to a higher number of
waves, such as peaks of 2916 cm-1 to 2920 cm-1,peaks between 1423 cm-1
and 1458
cm-1 as well as the peaks between 1639 and 1666 cm-1
. This bond can be seen at
1666 cm-1
before to the production of nanoparticles and has since migrated to 1639
cm-1.
The results may confirm that the copper nanoparticles were synthesized and
encapsulated with silica by the Stober's method; The change in wave numbers was
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straightforward UV-visible spectrometer, as demonstrated by the size dependence of
the plasmonic resonance of the absorption of copper nanoparticles and core-shell
particles of copper / silica prepared by chemical sol-gel method.The results from UV-
visible demonstrate a red shift in the absorption spectra caused by the increase in
particle size caused by the increased silica coating that the synthesis of Cu@SiO2
nanostructure exhibited in the figure displayed SPR peak at 635 nanometer, when it
was at the wavelength of 630 nanometer for cu nanoparticles. Fig:3
Figure 3. UV-vis absorption spectra for Cu and Cu @Sio2
3.3. FTIR
The FTIR spectra of silica (Sio2) fig:3a and 3b Cu @ Sio2 .The wide band at 3356
cm-1 in the FTIR of Sio2 corresponds to the O-H stretching vibration. of the
condensation of a silanol group (Si-OH) as well as the residual absorbed water in the
FTIR spectra of SiO2 and Cu @ Sio2 in Figure. Water molecules' bending and
vibrations as they absorbed into the surface of the silica particles caused a small peak
at 1666 cm-1. [22].
There were characteristic peaks at 1029 cm-1, 794 cm-1, and 474 cm-1, which
represented, respectively, the bending oscillation of O-Si-O, the asymmetrical
extending vibration of Si-O-Si, and the symmetric stretching vibration of O-Si-O [23].
The vibrations of the silanol groups stretching are connected with the band at 1029
cm-1,while the peak at 1396 cm-1 is connected to the stretching of the Si-O bond [22].
Similar to the Sio2 spectrum, FTIR spectrum of cu @ sio2 nanoparticles in Figure4b
likewise showed typical vibrations, but peaks were displaced to a higher number of
waves, such as peaks of 2916 cm-1 to 2920 cm-1,peaks between 1423 cm-1 and 1458
cm-1 as well as the peaks between 1639 and 1666 cm-1. This bond can be seen at
1666 cm-1 before to the production of nanoparticles and has since migrated to 1639
cm-1.
The results may confirm that the copper nanoparticles were synthesized and
encapsulated with silica by the Stober's method; The change in wave numbers was
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due to C=C stretching and reveals coordination with Cu nanoparticles. Moreover,
FTIR peak in Fig. 4b indicates that a peak of 624 cm -1
It may refer to copper
nanoparticles [24- 26].
Figure 4. ftir spactra of a- Sio2 b- cu@Sio2
3.4. TEM.
The analyses of the TEM pictures are useful equipment for evaluating the size and
form of the prepared nanoparticles. Fig. 4 displays common TEM pictures of cu@Sio2
NPs, their look is spherical in shape with a cover around them, as in Fig. 5, and they
also offer a wide range of sizes cu @sio2
core shell dimeter is between (35 and 120)
nanometer and rate 66 nanometer as in the fig.6.
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Figure 5. TEM images of Cu@Sio2 core shell NPs
Figure 6. TEM Histograms of Cu@Sio2 core shell NPs
3.5. FESEM-EDX
By using feSEM-EDX analyses, the existence of Cu@sio2
core-shell was
established, and the outcome seems to show a spherical agglomeration in the particle
size distribution, with diameters ranging from 80 to 184 nanometers. High
magnification examination shows more details, though, including the fact that these
copper nanoclusters are made up of smaller nanoparticles with good homogeneity,
whose average diameter is roughly 152 nanometers (figs. 7 and 8 show this). The
copper that was generated and the silica that it was coated in can both be clearly
seen in the EDX analysis in Fig. 9. It should be noted that the copper-metal NPs were
silicate-coated.
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Figure 5. TEM images of Cu@Sio2 core shell NPs
Figure 6. TEM Histograms of Cu@Sio2 core shell NPs
3.5. FESEM-EDX
By using feSEM-EDX analyses, the existence of Cu@sio2 core-shell was
established, and the outcome seems to show a spherical agglomeration in the particle
size distribution, with diameters ranging from 80 to 184 nanometers. High
magnification examination shows more details, though, including the fact that these
copper nanoclusters are made up of smaller nanoparticles with good homogeneity,
whose average diameter is roughly 152 nanometers (figs. 7 and 8 show this). The
copper that was generated and the silica that it was coated in can both be clearly
seen in the EDX analysis in Fig. 9. It should be noted that the copper-metal NPs were
silicate-coated.
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Figure 7. fesem showing the copper nanoparticle capping with silica
Figure 8. fesem Histograms of Cu@Sio2NPs
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Figure 9. EDS Diagram showing the presence of copper Nps and silica
4. EVALUATION OF ANTIBACTERIAL
4.1. ACTIVITY OF THE CORE-SHELLS
Results of the evaluation of the antibacterial activity of the disc diffusion method
prepared from core and shells in Figures (10) and (11) shows the inhibition region
where the rate of bacterial reduction was for samples (14, 14, 16 and 20) for
Escherichia coli and (24, 24, 28 and 30) for Staphylococcus aureus. Samples were
taken with dilute concentrations (12.5, 25, 50, 100) %. They showed a high bacterial
reduction rate for each Escherichia coli and Staphylococcus aureus in particular,
cu @sio2core shell, showed greater action against Staphylococcus aureus than
their action against Escherichia coli, which was observed from the reduction rate after
only 24 hours. The mechanisms by which copper is toxic to bacteria have been
identified as the generation of free radicals [27, 28], which leads to the
permeabilization of cell membranes, and the degradation of DNA and RNA. In the
case of the antibacterial activity of free radicals, interactions with the proteins inside
the bacteria in samples containing copper result in the production of hydroxyl radicals
(OH) and peroxide anions (O2
). The resultant radicals damage DNA and RNA by
degrading intracellular and extracellular components that obstruct the electron
transport system. In addition, the eluted copper affects the bacterial outer membrane,
creating holes in the outer membrane that are atypically formed. Changes in these
membranes alter membrane permeability, leading to a gradual release of
lipopolysaccharide molecules and membrane proteins, leading to the death of the
bacteria [29].
The size, shape, and concentration of copper nanoparticles, as well as the
synthesis procedure, all affect the antibacterial action of cu@sio2 core shell. The
presence of the copper nanopowder coated by SiO2 was verified by TEM
measurements of core shells made using the sol-gel method.Cu@Sio2 nanoparticles
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Figure 9. EDS Diagram showing the presence of copper Nps and silica
4. EVALUATION OF ANTIBACTERIAL
4.1. ACTIVITY OF THE CORE-SHELLS
Results of the evaluation of the antibacterial activity of the disc diffusion method
prepared from core and shells in Figures (10) and (11) shows the inhibition region
where the rate of bacterial reduction was for samples (14, 14, 16 and 20) for
Escherichia coli and (24, 24, 28 and 30) for Staphylococcus aureus. Samples were
taken with dilute concentrations (12.5, 25, 50, 100) %. They showed a high bacterial
reduction rate for each Escherichia coli and Staphylococcus aureus in particular,
cu @sio2core shell, showed greater action against Staphylococcus aureus than
their action against Escherichia coli, which was observed from the reduction rate after
only 24 hours. The mechanisms by which copper is toxic to bacteria have been
identified as the generation of free radicals [27, 28], which leads to the
permeabilization of cell membranes, and the degradation of DNA and RNA. In the
case of the antibacterial activity of free radicals, interactions with the proteins inside
the bacteria in samples containing copper result in the production of hydroxyl radicals
(OH) and peroxide anions (O2). The resultant radicals damage DNA and RNA by
degrading intracellular and extracellular components that obstruct the electron
transport system. In addition, the eluted copper affects the bacterial outer membrane,
creating holes in the outer membrane that are atypically formed. Changes in these
membranes alter membrane permeability, leading to a gradual release of
lipopolysaccharide molecules and membrane proteins, leading to the death of the
bacteria [29].
The size, shape, and concentration of copper nanoparticles, as well as the
synthesis procedure, all affect the antibacterial action of cu@sio2 core shell. The
presence of the copper nanopowder coated by SiO2 was verified by TEM
measurements of core shells made using the sol-gel method.Cu@Sio2 nanoparticles
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core - shell displayed sufficient performance as antibacterial
agent. Although the
presence of the SiO2
shell prevented direct contact with the Cu nano powder, it still
yielded high a reduction rate for bacteria. Thus, it was confirmed that an antibacterial
agent capable of overcoming the disadvantages of using nanopowder could be
manufactured. In addition, by controlling the thickness of the shell, the elution of Cu
can be delayed and antibacterial functions can be maintained for long periods.
Figure 10. antibacterial activity of copper @sio2 core shell vs E.coli and S. aureus
bacteria(the inhibition zone)
Figure 11. Cu@Sio2 core shell inhibition zone of E. coli and S. aureus bacteria at four diluted
concentrations (12.5%, 25%, 50, and 100%)
5. CONCLUSIONS
A chemical sol-gel process was used to create CuSiO2 nanoparticles with a core-
shell structure. A spherical sio2
shell was formed using the sol-gel process, and Cu
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nanopowder was present at the center. The presence of ammonia was also confirmed
as being essential to the process. Using the shaking flask method, the spectra of xrd
confirm the presence of copper nanoparticles, and the Fesem and Tem images
confirm the formation of spherical particles. A red shift was observed in the UV-vis
absorption spectra, indicating an increase in particle size, and it was confirmed that
the core-shells produced through sol-gel method exhibited antibacterial activity.
Cu@sio2
core-shell can be used as a futuristic, effective antibacterial agent in
biomedical applications.
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