Efficient Fabrication of Cu-Doped TiO2 Nanoparticl

Journal of Inorganic and Organometallic Polymers and Materials
https://doi.org/10.1007/s10904-024-03232-y
RESEARCH
Efficient Fabrication of Cu‑Doped TiO2 Nanoparticles for Enhanced

Visible Light Photocatalysis and Antimicrobial Efficacy
Amna Azam1 · Tahir Iqbal1
Received: 12 May 2024 / Accepted: 21 June 2024

© The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2024
Abstract
In order to enhance photocatalytic degradation and antibacterial activities, copper doped titanium dioxide has been synthe-
sized in this work. The samples were analyzed by X-ray diffraction, Energy dispersive X-ray diffraction, Raman spectroscopy,
UV–Vis spectroscopy, Fourier transform infrared spectroscopy and Brunauer–Emmett–Teller (BET) analysis. The rutile
phase tetragonal structure of both pure and Cu/TiO2 has been shown by XRD data. It is discovered that nanoparticle average
crystallite sizes were for pure and Cu-TiO2 is in the range of 8.6–16.50 nm. The band gap decrease trend in this research
is approximately followed from 3.42–2.86 eV. Cu-TiO2 has the best photocatalytic behavior and doping in T iO2 material
changes its structure appears to increase the photocatalytic activity. The SEM images additionally determined the particle
size within the approximately 15.5 nm range. The Tauc plots were utilized to identify the nanoparticles optical band gap.
The surface study of optimized sample has been analyzed using BET analysis. Research on the characterization of copper
doped TiO2 nanoparticles that demonstrate a significant increase in the photocatalytic activity could also be expected to
increase the shelf life of fruit storage. In order to investigate its biological activities for example antimicrobial and antifungal
properties this research has been utilize as the awareness for the fabrication of copper nanoparticles. Due to its exceptional
qualities, the material under study is also thought to present a viable alternative for the creation of intelligent systems that
detect pathogens and act as antimicrobial agents.
* Tahir Iqbal
tahir.awan@uog.edu.pk
Amna Azam
21016110-011@uog.edu.pk
1
Department of Physics, Faculty of Science, University
of Gujrat, Hafiz Hayat Campus, Gujrat 50700, Pakistan
Vol.:(0123456789)
Content courtesy of Springer Nature, terms of use apply. Rights reserved.

Graphical Abstract
Keywords Antimicrobial · Cu-TiO2 · Co-precipitation · Degradation · Organic pollutants · Photocatalysis · TiO2
1 Introduction TiO2 is found in both crystalline forms and amorphous.

TiO2 classified in three crystal structures Anatase, Rutile
The fabrication of metallic nanoparticles has been demon- and Brookite due to its physical properties that conclude
strated from the few decades to enhance the support for the optical bandgap and larger surface area among others. Pho-
advancement of nanomaterial applications across a wide tocatalysts that include both anatase and rutile structures
range of industries. Nanoparticles are now widely used in the are tetragonal forms. When light is exposed with 380 nm
biomedical industry, including electronics, pharmaceuticals, wavelengths or less, T iO2 behave as semiconductor with the
cosmetics, and diagnostics. This is due to advancements in broad bandgap range from (3.0–3.7 eV) and this light expo-
nanoscale [1, 2]. sure results in the creation of electron and hole pairs in the
The most important biological utilization for nanoparti- redox processes respectively [4–6].One especially success-
cles (NPs) includes drug transport and antibacterial therapy. ful method is the introduction of different transition metals,
Nanoparticles (NPs) in biology are extremely significant such as copper (Cu), silver (Ag) nickel (Ni) and iron oxides
and include drug transport, antibacterial therapy, imaging (FeO) [7] is doping approach that give significant results in
and biosensing. Researchers have focused a lot of attention a notable shift in absorption of T
iO2 in the visible light spec-
on metal doped nanoparticles (NPs) from the scientific and trum [8–13]. Copper is a particularly good dopant among
technological standpoint due to their potential uses in nano- these transition metals because of its special electrical char-
electronics, nanosensors, optoelectronics, photo-catalysis, acteristics and capacity to enhance the charge separation and
information storage, nanodevices, antibacterial field and transfer. It can improve the photocatalytic activity of T iO2
environmental remediation [3, 4]. nanoparticles and become the most sensitive to visible light

and copper also has a dual function as a charge carrier trap activity of T iO2 nanoparticles. As a result, T iO2 has the
that makes easier for holes and electrons to move efficiently potential to be an antibacterial agent [22, 23]. When cells
across the materials surface and reduces their recombina- come into direct contact with the nanoparticles, the gener-
tion rate. ated ROS damages the DNA and cell membrane and cause
Copper has an ionic radius about approximately 0.68 Å the cells to die leads the cell cycle to end [25, 26]. Major
that is quite similar to titanium ionic radius is approximate in pathogens including foodborne germs like S. aureus, Bacil-
the range of 0.61 Å. Copper can be easily incorporated into lus subtilis, Staphylococcus aureus, Escherichia coli, and
the TiO2 lattice because of these close ionic sizes [14, 15]. pseudomonas are prevented and destroyed from it. Accord-
The materials band gaps are the electronic density of states ing to numerous studies, the high degree of antibacterial
that is changed by this integration that change the capacity activity attributed to copper dopant is directly related to the
to absorb light. To extend the photocatalytic activity of T iO2 release (Table 1) of ions that results in oxidative stress and
nanoparticles to visible light wavelengths, several research the generation of reactive oxygen species (ROS) in aerobic
groups have utilized the Copper doping to design the nano- conditions [27, 28].
particles with specific light absorption [16, 17]. Copper enters the cell and permeates it and release ions
In this innovative study, Raguram and Rajni synthesized as a result and increase in the volume of intrinsic copper that
pure and Copper doped T iO2 nanoparticles that demonstrate has significant oxidative stress it demonstrated the redox
how this treatment give advantage to Copper electrical prop- cycle among the several forms of Copper includes native
erties for the improvement in the charge transport [18, 19]. Cu, Cu(I) and the Cu(II) [33–35].
Their research elaborated beyond material characterization The current research objective utilized the co-precipita-
and into useful applications, such as photocatalytic degradation approach to create Cu-TiO2 nanoparticles doped with
tion of Rhodamine-B. A significant improvement in perfor- different concentrations of copper. Due to significant effects
mance indicators was noted for copper doped T iO2 nanopar- of copper and T iO2 that may effectively expand the absorp-
ticles in their fundamental work. These dopant nanoparticles tion of light range into the visible region and promote a
were incorporated and the result had significant maximum separation of photo-generated charged particles, the doping
power conversion efficiency (PCE) of 3.90%. Concurrently, of copper into TiO2 has gathered a lot of interest recently.
the Copper doped T iO2 nanoparticles demonstrated the Cu-TiO2 nanoparticles have been synthesized using a variety
97.12% effectiveness in the photocatalytic destruction of of techniques, including co-precipitation, sol–gel and hydro-
Rhodamine-B dye. The fact that copper doped T iO2 can thermal processes. Co-precipitation synthesis is one of these
perform exceptionally well in both energy conversion and approaches and it has the advantage of being simple, scal-
pollution remediation highlights the compounds versatility able, and able to accurately control the dopant concentration.
for tackling problems. Yumatorn et al. looked into the pho- The investigation of significant synthesis factors and
tocatalytic and antibacterial uses of Cu-doped T iO2 nano- their impact on the structural and morphological photocat-
particles in a different study [20]. alytic characteristics of the resultant Cu-TiO2 nanomateri-
Their study concentrated on the adaptable 0.1 weight als constitutes the innovative aspect of this work. It will be
percent copper doped T iO2 verified its superiority over un- possible to optimize photocatalyst design and improve the
doped TiO2 in terms of photocatalytic degradation and anti- performance of dopant concentration, calcination tempera-
bacterial activity against Escherichia coli (E. coli). Copper ture, pH and other synthesis factors. Additionally, the goal
doped TiO2 nanoparticles were recently produced by Majeed of this work is to reveal how Cu and TiO2 work together
Khan and colleagues that examined the photocatalytic to enhance the photocatalytic activity, specifically in the
activity of the particles in the methylene blue dye solution breakdown of organic pollutants exposed to visible light.
degradation [2, 21]. For a 2.5 percent copper doped TiO2 Our latest research has focused on these fields utilizing the
sample results showed a good photocatalytic dye degrada- commonly used minerals TiO2 and also incredibly cheap
tion capability of 95.8%. It has been demonstrated that the
addition of copper to T iO2 nanostructures causes significant
modifications to their optical, morphological, and structural Table 1 Comparison of the antibacterial properties of Cu-TiO2 nano-
characteristics. Among the several synthesis techniques, the particles
co-precipitation method has gained popularity as a flexible Nanoparticles Bacteria Antibacterial effi- References
and affordable way to produce TiO2 nanoparticles and their ciency
doped equivalent [22–24].
Cu-TiO2 S.aureus No activity [29]
The creation of reactive oxygen species (ROS) compris-
Cu-TiO2 S.aureus,E. coli No activity [30]
ing hydroxyl radicals (•OH) and the synthesis of hydrogen
Cu-TiO2 S.aureus,E. coli No activity [31]
peroxide H2O2 under the ultra-visible light that is responsible
Cu-TiO2 B. subtilis,E. coli 90%,80% [32]
for the oxidative stress that is present and the antibacterial

and corrosion resistant, making them ideal for a wide 2 Experimental Methodology
range of applications. Particle size, crystallinity and dop-
ing concentration may all be easily manipulated with this 2.1 Materials
approach's fine control over the reaction circumstances.
The goal of this study is to do a comprehensive analysis Titanium isopropoxide (TTIP (Ti(OC3 H7 )4 ),Copper(II)
of co-precipitation-synthesized pure T iO2 and Cu doped nitrate trihydrate ( Cu ⋅ (NO3 )2 .3H 2 O ), Absolute ethanol
TiO2 nanoparticles. The main goal is to clarify how cop- (C2 H5 OH ) and sodium hydroxide (NaOH), are obtained
per doping affects the TiO 2 morphological, optical and from Gujrat, Pakistan. TTIP is utilized as the primary pre-
structural properties? In order to better understand these cursor for the synthesis of Cu/TiO2. The University of Guja-
interactions between the dopant and the host matrix. This rat's Physics department is the source of this base material.
work is important because it can shed light on the changes The Cu/TiO2 dopant and sodium hydroxide (NaOH) utilized
brought about by Cu doping, which is essential for cus- in this investigation for the modulation of pH were taken
tomizing the nanoparticles to meet the needs of particular from the nano-lab of Physics department in University of
applications. These might involve improved light absorp- Gujrat. All the chemicals (Table 2) and reagents utilized
tion and increased electronic conductivity or increased were of analytical quality. For the stock solutions, water uti-
photocatalytic activity. This study intends to make a sig- lized in this research was either distilled or deionized.
nificant contribution to the expanding field of nanomateri-
als by methodical examining the structural, morphological 2.2 Synthesis Method of Photocatalyst
and optical aspects of pure and Cu doped T iO2 nanopar-
ticles. It is hoped that the research described here will There are several methods for creation of Cu/TiO 2 NPs
direct the design and optimization of TiO2 based materials that include such as sol–gel, hydrothermal, solvothermal,
for a variety of applications, including sophisticated light- co-precipitation and green synthesis. One of the meth-
harvesting devices and environmental cleanup. ods employed in this investigation is the co-precipitation
TiO 2 nanoparticles have promising uses beyond the method. We prepared two different solutions for the fabri-
previously mentioned ones, including as an antimicro- cation of Cu-doped T iO2 nanoparticles: both B and A solu-
bial agent. The most logical approach is the bottom-up tion, 12 ml of titanium isopropoxide (TTIP) were added
approach since atomic-scale precision is attained. In order drop-wise to the 55 ml of ethanol were combined to make
to produce T iO2 nanoparticles, the necessary solvent must Solution A. thereafter, to guarantee homogeneity, stirring
first be added to a titanium precursor solution. Titanium for an hour. To obtain a desirable amount of copper dop-
isopropoxide is the precursor used in this investigation. ing in the TiO2 nanostructure, Solution B was created by
UV–visible spectrophotometry, Raman Spectroscopy, dissolving different weight amounts (from 1 to 5% weight)
Fourier transform infrared spectroscopy, scanning electron of Copper (II) nitrate trihydrate ( Cu ⋅ (NO3 )2 .3H 2 O ) salts
microscopy, X-ray diffraction, Photoluminescence Spec- with specific desirable concentration added into the de-
troscopy and surface study using BET have been utilized ionized water solution. After then, Solution B was precipi-
for analysis of the resulting nanoparticles. tated with a NaOH solution until the pH reached to 10. The
salt solution was mixed for 30 min following precipitation,
and then Solution A was progressively added to ensure
Table 2 Chemicals utilized Chemicals Chemical formula Company Puritya (%)

in this synthesis and their
descriptions Titanium isopropoxide (TTIP) (Ti(OC3 H7 )4 ) Sigma Aldrich ~ 98%
Copper(II) Nitrate Trihydrate Cu ⋅ (NO3 )2 .3H 2 O Sigma Aldrich ~ 99%
Absolute Ethanol C2 H5 OH Sigma Aldrich ~ 98%
Sodium Hydroxide NaOH Sigma Aldrich ~ 98%
Rhodamine (B) C28 H31 CIN2 O3 Sigma Aldrich ~ 95%
Benzoquinone (BQ) C6 H 4 O 4 Merck ~ 98%
Potassium iodate KIO3 Merck –
Methyle Orange C14 H14 N3 NaO3 S Merck ~ 85%
Methyl Blue C16 H18 CN3 S Merck ~ 70%
DPPH C18 H12 N5 O6 Alfa Aesar ~ 95%
a
Declared by the supplier

complete mixing, the resulting mixture had been preserved 3 Characterizations

undisturbed for 15 h. The mechanism of the copper doped
TiO2 consists of three phases. (a) In first the metal ions Cu/TiO2 nanomaterials were characterized utilizing a vari-
reduction and nucleation of the reduced metal ion is the ety of procedures to figure out a number of its attributes.
activation phase occurs, (b) In the growth phase in which The generated material's crystallinity and purity were evalu-
small adjacent nanoparticles combine simultaneously and ated utilizing the X-ray diffraction (XRD) method (Rigaku
form the bigger size leads to the thermodynamic stability Smartlab X-ray Diffractometer X ray source: copper) and
to the nanoparticles (c) Termination phase in which final Raman spectra (Andor SR-500i). The Brunauer -Emmett-
shape is determine to the nanoparticles as shown in the Teller (BET) surface area of the sample was determined
Fig. 1. The solution was then centrifuged and to make based on the nitrogen adsorption–desorption data using a
sure that any remaining contaminants were completely V-sorb 2800S analyzer. Scanning Electron Microscope Jeol
removed. The mixture was then rapidly stirred for an addi- JSM 5910, Japan (SEM) was utilized as well to analyze the
tional hour after solution will be in the centrifugation for targeted samples' morphology. Using UV–Vis spectroscopy
fifteen minutes at 10,000 rpm. After that, the particles Shimadzu, UV–Visible Double Beam Spectrophotometer
were centrifuged once more for ten minutes at 5000 rpm (UV–VIS 1800), we determined the band gap between
after that it has being washed with ethanol. The solution pure TiO2 and the Cu/TiO2 nanoparticles. A fluorescence
was then dried in drying oven for three hours at 30 °C. The (PL: RAMANLOG 6, UOG) spectrometer was also used to
synthesized material was dried and then calcined for two observe PL spectra. FTIR (Thermo Scientific Nicolet iS5
hours at 550 °C. Following the calcination process, the FT-IR Spectrometer) was utilized to determine the chemi-
material was allowed to cool to room temperature before cal characteristics. Energy dispersive X-Ray spectrometer
being finely crushed using a mortar and pestle[24]. The (EDX) INCA200/Oxford instruments, Analysis range is
synthesis yield of copper doped TiO2 was confirmed by Boron to Uranium) ultimately, the degradation of Rhoda-
running the entire process through three replications. The mine (B) dye using produced pure and co-doping titanium
results showed that the synthesis yields of copper doped dioxide nanoparticles with copper was observed through
TiO2 was 47.3 ± 1.33. Figure 2 represents the schematic of activity.
co-precipitation method of copper doped T iO2 and Table 3
shows the components percentage weight ratios of (1%- 3.1 Scanning Electron Microscope (SEM)
5%) concentrations of pure and copper doped TiO2 nano-
particles that are utilized in the synthesis. The composition of the sample and the surface fea-
tures of the pure and Cu/TiO 2 nanopar ticles
Fig. 1 Mechanism for the Cu-

TiO2 nanoparticles

Fig. 2 Schematic dia-

gram of the co-precipita-
tion method for Cu/TiO2
nanoparticles
Table 3 Percentage weight ratio of components utilize for the synthe- emphasize that the dopant concentration in Fig. 3a, b, c, e, f
sis of Cu/ TiO2 composites which is determined using ImageJ software, increases when
Material Cu: TiO2 % weight the concentration of dopant is added. The histogram plots
indicate that the size of nanoparticles spans for pure TiO2
Pure TiO2 0: 4 from 8.74 nm and for 1% Cu/TiO2 for 15.5 nm with the vast
1% Cu/ TiO2 0.048:4
majority of particles being in the16.804 nm range and for
2% Cu/ TiO2 0.096:4
2% Cu/TiO2 for 15.5 nm with the vast majority of particles
3% Cu/ TiO2 0.144: 4
being in the 276.6 nm range and for 3% Cu/TiO2 for 15.5 nm
4% Cu/ TiO2 0.192:4
with the vast majority of particles being in the 718.6 nm
5% Cu/ TiO2 0.24: 4
range and for 4% Cu/TiO2 for 15.5 nm with the vast majority
of particles being in the 76,551.3 nm range and for 5% Cu/
TiO2 for 15.5 nm with the vast majority of particles being
were identified through SEM analysis. At 550 °C, the pre- in the 85.23 nm. Remarkably, there is a strong correlation
pared samples experienced calcination. The spectral resolu- between the average size of NPs and XRD findings.
tion of Fig. 3a shows an irregularly shaped rough nano-rod
at the 200 nm range when pure TiO2 is displayed, Fig. 3b 3.2 Energy Dispersive X‑ray Spectroscopy (EDX)
shows an irregularly shaped rough nano-rod at the 2 µm
range of 1% Cu- TiO2 is displayed, Fig. 3c shows an irregu- To confirm titanium dioxide NP composite's synthesis, EDX
larly shaped rough cube at the 500 nm range of 2% Cu-TiO2 analysis was performed. In the EDX test, multiple areas were
is displayed, Fig. 3d shows an irregularly shaped rough star targeted and the significant peaks can be observed in Fig. 4.
shape, rough spheroid at the 1 µm range of 3% Cu-TiO2 is The generated composite nanostructures exhibit pure,1%, 2%
displayed, Fig. 3e shows an irregularly shaped rough sphe- 3%, 4% and 5% Cu/ T iO2 in the EDX spectrum. In the Pure
roid at the 500 nm range of 4% Cu-TiO2 is displayed but TiO2 spectrum (a), the amounts of Ti, O were 53.67, 46.33
Fig. 3f, g shows 5% Cu-TiO2 results in a distinctive and respectively. In the 1% Cu/ T iO2 spectrum (b), the amounts
the porous nano spheroid of a different at different ranges of O, Na, Ti and Cu were 36.41, 7.12, 56.19 and 0.28 respec-
1 µm 200 nm and 500 nm are displayed respectively. When tively. In the 2% Cu/ T iO2 spectrum (c), the amounts of O,
produced samples are compared at the same magnification Na, Ti and Cu were 44.64, 13.21, 41.83, and 0.32 respec-
and resolution, a doping material difference is observable. tively. In the 3% Cu/ T iO2 spectrum (d), the amounts of O,
Nanoparticles with different lengths, diameters, and mor- Na, Ti and Cu were 35, 30.56, 34.03 and 0.40 respectively.
phologies are determined by the amount of pro- In the 4% Cu/ TiO2 spectrum (e), the amounts of O, Na, Ti
duced dopant and thermodynamic factors (temperat- and Cu were 41.66, 46.67, 11.15 and 0.52 respectively. In the
ure, method, heat treatment, etc.). It is significant to 5% Cu/ T iO2 spectrum (f), the amounts of O, Ti and Cu were

Fig. 3 a SEM image of pure

TiO2 and Histograms plots
represent average size of NPs
b SEM image and Histograms
plots represent average size
of 1% Cu-TiO2 c SEM image
and Histograms plots represent
average size of 2% Cu-TiO2 d
SEM image and Histograms
plots represent average size
of 3% Cu-TiO2 e SEM image
and Histograms plots represent
average size of 4% Cu- T iO2
f SEM image and Histograms
plots represent average size of
5% Cu- T iO2 g SEM image of
5% Cu-TiO2

Fig. 3 (continued)
23.15, 69.78 and 7.06 respectively. The effective production were acquired. The diffraction peaks morphologies and
of Cu-doped T iO2 nanoparticles is confirmed by the pres- being placed are comparable to those of pure T iO2 in Cu-
ence of Cu in the doped T iO2 these results demonstrate that TiO2. The findings show that the majority of rutile and an
with the increase of doping copper concentration become insignificant quantity of anatase are present in both pure
increases and Ti amount become relatively decreases. The and Cu- T iO2.The catalysts XRD patterns, displayed in
EDX spectrum of pure and 1% to 5% Cu/ TiO2 nanoparticles Fig. 5, may be indexed to the planes of the rutile phase
are displayed with the table in which weight percentage and (110) and rutile phase (101), demonstrating the presence
atomic value values are elaborated. of rutile phase in the catalyst. The rutile phase (101) and
rutile phase (110) planes may be referenced to the pri-
3.3 X‑ray Diffraction (XRD) mary diffraction peaks of the XRD patterns for the pure,
which are positioned at 29.4o and 31.8o , respectively. All
X-ray powder diffraction (XRD) was utilized for investi- the indexed peaks correspond to the phase of TiO2 (refer-
gating the pure and Cu- T iO2 nanoparticles. To determine ence pattern 01–078-1508). The lattice parameters were
the size, content and crystallographic orientation concen- calculated from XRD data is as follows. a = 4.5925 A ,
◦
trations of 1% to 5% of copper were dissolved into titanium b = 4.5925 A and c = 2.9578 A and crystal structure is
◦ ◦
dioxide as the evidenced by X-ray diffraction analysis is tetragonal.

displayed in the Fig. 5. To determine the crystallographic Miller indices are calculated for each peak to ascertain
orientation of the generated photocatalysts, XRD patterns stress, unit cell properties, and structural orientation. T
iO2 is

iO2, b EDX spectra of 1% Cu-TiO2, c EDX spectra of 2% Cu-TiO2, d EDX spectra of 3% Cu-TiO2, e EDX spectra
Fig. 4 a EDX spectra of pure T
of 4% Cu-TiO2, f EDX spectra of 5% Cu- T iO2
present in the powdered sample. The Scherrer's formula was where d is the average particle size in meters. The values
used to determine the particles' average size. of k = 0.95–0.98 (shape factor), λ = 0.15406 nm (X-ray
wavelength)m, 𝛽 is the full width half maximum (FWHM)
D = K𝜆∕𝛽cosθ (1) and 𝜃 which stands for the Bragg’s angle of diffraction con-
stant respectively indicate the highest intensity peaks. The
ideal value of k is 0.89. According to SEM measurements,

Table 4 Average crystallite size and d-spacing of pure and copper

doped TiO2
DSpacing
Material Crystal size(nm) (110) (101) (200)
Pure TiO2 8.627281 3.060333 2.982033 3.058341

1% Cu/ TiO2 9.030994 3.514777 3.041925 2.895781
2% Cu/ TiO2 9.150947 3.514777 2.347911 1.875718
3% Cu/ TiO2 13.5854 3.279347 3.397439 2.059599
4% Cu/ TiO2 14.10064 3.514777 2.03805 4.024388
5% Cu/ TiO2 16.50565 2.711275 5.017974 0.807606
3.4 Raman Spectroscopy
The Raman spectra of the pure and the 5% Cu-TiO2 samples

Fig. 5 XRD spectrum of pure and copper doped T
iO2 is shown in Fig. 6. The spectra are characteristic of anatase
phase and no characteristics of any other phase such as rutile
are observable. Considering symmetry suggests that only
the average particle size for the pure T iO2 is 8.74 nm and A1g and B1g modes need to be identified. Due to disorienta-
15.5 nm for Cu/ T iO2. There's a solid association between tions, the tiny structures were assigned to the Eg modes. The
these values. The Debye–Scherrer formula is used to calcu- pure and Cu-TiO2 geometry seem to have the three Eg modes
late the average grain size for pure TiO2 and Cu/ T iO2 for properly resolved. Specifically, the O-Ti-O bending mode
the 1%, 2%, 3%, 4%, 5%, along with is 8.62 nm, 9.03 nm, associated with ʋ = 145c m−1 mode, A1g and B1g modes at
9.15 nm, 13.58, 14.10 and 16.5 respectively. Calculated den- 519 c m−1 and 396 c m−1 respectively can only be assigned
sity for TiO2 is 5.07 g/m3. Furthermore, no additional pollut- using a force constant model since they are resolved at low
ants or Copper related oxides are visible. This implies that temperatures. Interpretation of the variations in the same
perhaps the dopants have been successfully doped into the mode's frequency observed in various geometries should
TiO2 lattice or Cu ions are equally distributed on the surface be based on longitudinal transverse coupling of the modes
of TiO2 in amounts small enough for XRD to detect them. and long-range lattice forces. Additionally, as illustrated in
The rutile (110) and rutile phase (101) stretched XRD Fig. 6, Raman spectroscopy was utilized for pure TiO2 and
peaks are displayed in Fig. 5. After a small quantity of Cu-TiO2 structural analysis in order to discriminate.
Cu2+ doping, XRD peak positions have shifted toward a One of the six fundamental modes that characterizes the
smaller angle. These findings demonstrate the effective- TiO2 anatase phase is represented by the characteristic line
ness of doping Cu2+ into the TiO 2 lattice. Both of these
ways of metal doping into metal oxides are referred to
as interstitial and substitutional doping, respectively.
The doping mode is determined by the ionic radius and
electronegativity of doping ions. The dopant may substi-
tute the lattice ions if its ionic radius its electronegativ-
ity is similar to those of the lattice ions. Although the
electronegativity values of Cu2+ and Ti4+ are compatible,
when considering solely ionic radii, Cu2+ ions are more
likely to be located in the lattice's interstitial places due
to their relatively large size than in individual Ti4+ sites
themselves. Therefore, the doping mechanisms of Cu2+
may be summarized as interstitial doping along with
substitution doping, respectively. Table 4 The d spacing
was calculated using Braggs law, and confirmation was
obtained from the International Center for Diffraction
Data (ICDD).
Fig. 6 The Raman spectrum for pure and 5% Cu-TiO2

that comprises A1g (519 c m−1), B1g (396 c m−1), and Eg(639 charge between metal ions and T iO 2 reduced band gap
c m−1). The active modes peaks at 145 c m−1, 396 c m−1 519 energy increases absorbance in the visible range. This sug-
c m−1, and 639 c m−1 in the TiO2 spectra here are indica- gests that metal doping on T iO2 can produce electron–hole
tive of a pure anatase phase, with no additional rutile phase pairs. The UV–Vis double-beam spectrometer (Double
peaks detected. Cu-TiO2 spectra show weak intensity and a Beam UV–Vis Spectrophotometer SP-IUV&, 2002, UOG)
shift toward high frequency when compared to T iO2. This is has been utilized to examine the UV–Vis spectra for pure
consistent with the documented literatures and clearly veri- TiO2 and Cu/ TiO2. Defects and the optical band gap in
fies the substitution of copper into the TiO2 lattice. these materials are dependent on absorbance. The Fig. 8
represents the direct UV–Vis measurement of band gap
3.5 Fourier Transform Infrared Spectroscopy (FTIR) for pure TiO 2 and Cu/ TiO 2. The pure titanium dioxide
band gap in Tauc plots is 3.34 eV. There is a straight band
This study is utilized in the mid-infrared spectra (500–4000 gap between pure TiO2 and Cu/ TiO2 for the 1%, 2%, 3%,
cm−1) for analysis. Using FTIR spectra analysis for pure and 4%, 5%, along with 3.42 eV, 3.34 eV,3.24 eV, 3.04 eV,
Cu/ TiO2 nanoparticles at different concentrations of 1%, 2.96 eV, and 2.86 eV respectively. The band gap decreased
2%, 3%, 4%, and 5% have been assessed in the 500–4000 when doping was increased to 1%, 2%, 3%, a 4% and 5%
cm−1 range. The unique strong absorption peaks at 3289 and however, the band gap increased once more. This phenom-
2169 cm−1 are responsible for the stretching vibrations of enon is known as the Burstein-Moss effect that explains at
water O–H stretching, water O–H bending and C-O stretch- specific concentration the visible band-gap of semiconduc-
ing. The absorption at 1110 cm−1 and 1632 cm−1 in the TiO2 tor material increases when fermi energy level stretches
spectrum is attributed to Ti–O–Ti stretching vibration and towards valence band which results in color shift. In con-
Ti–O bonds. trast, we can predict that 5% Cu/ T iO2 has been efficient.
These spectra indicate that water molecules are present at According to of the direct band gap, the following formula
the surface of TiO2 as a result of hydrogen holding (O–H). is utilized to calculate the direct band gap:
They also show that bends at 3289 and H–O–H stretching
(𝛼hv)2 = k(hv − Eg ) (2)
suggest the presence of adsorbed water at 1972 cm−1 and C
O2 stretching mode at 2169 cm−1 in the surrounding environ-
The symbol h denotes photon energy there. E g stands
ment. These spectra demonstrate that the Cu/ TiO2 and TiO2
for the sample band gap, while A stands for constant. The
nanoparticles in the Fig. 7.
observed modification of the band gap at absorbance levels
validates the noteworthy enhancing the optical character-
3.6 UV–Visible Spectroscopy istics of the Cu/ T
iO2 nanoparticles and smaller band gap
improve the photo-catalysis efficiency of the target sample.
When Cu was incorporated, the band gap values decreased
from 3.42 eV for pure T
iO 2. Because of the transfer of
Fig. 7 The FTIR spectrum measurements for pure and Cu/TiO2 Fig. 8 The UV–vis spectroscopy measurements for pure and Cu/TiO2

3.7 Photoluminescence Evaluations 3.8 BET analysis
Photoluminescence (PL) measurements employing photolu- The prepared 5% Cu-TiO 2 surface area was determined
minescence spectroscopy (PL: RAMANLOG 6, UOG) have by the BET analysis. The 5% Cu-TiO2 BET spectra were
been used to identify the material's imperfections. When displayed in the Fig. 10. The most important component
photosynthesis occurs at a greater photoluminescence level, critical factor of photocatalytic efficiency is specific sur-
the materials often exhibit the highest rate of e− − h+ pair face area [36]. More active reaction sites are available due
recombination. Cu/ T iO2 samples that have been manufac- to the greater specific surface area that helps to enhance
tured have a wavelength of 370 nm when doped with copper, photocatalytic performance. The 5% Cu-TiO 2 adsorp-
as illustrated in Fig. 9. When pure TiO2 is compared to cop- tion–desorption isotherms determine the 57.30 m2/g sur-
per, this wide emission at the center 452 nm is more intense, face areas. The results describe that with the increase of
suggesting a rate of e− − h+ pairs recombination. The green Cu doping increase the specific surface area. The catalyst's
emission approximately 464 nm is caused by band-to-band wide surface area was thought to have the best antibac-
transitions at a concentration of 5% Cu/ TiO2, which is con- terial and photocatalytic action. The surface area gives
sistent with previous research. the electron–hole pairs the structure they need to actively
But when doping concentration is added, the PL intensity engage in the redox process. Similar results reported with
drops. The band gap begins to expand when pure TiO2 and literature by Ganesh et al.[37] and T Nguyen et al.[38].
3% PL intensity are raised, even at the minimal 5% doping The BET analysis result show the strong correlation with
of copper in T iO2. At 4% Cu/TiO2 band gap is appropri- the literature. In Table 5 BET analysis with literature is
ate for 434 nm wavelength. The wavelength that is suitable compared.
and can create contamination in Tauc plot band gap calcu-
lations, which can result in a 5% decrease in electron and
hole recombination, is well connected to the Cu/TiO2 band
gap of 2.86.
This is because the concentration of dopant creates sites
on surfaces that function as defects that trap electrons; less
electrons are trapped in oxygen vacancies, which lowers
the number of holes created by photo generated light in the
transport chain and smaller energy gap of lower e− − h+ pair
recombination, Cu/TiO2 photo-catalytic activity of 5% is
comparable to that of other doping composites. This recent
work and the UV–Vis spectrum measurements provide suf-
ficient evidence for the necessary PL spectra.
Fig. 10 Adsorption–desorption isotherms of 5% Cu-TiO2
Table 5 BET analysis comparison with literature

Material SBET m2/g References
Pure TiO2 31.3 [36]

1% Cu/TiO2 45.3 [36]
2% Cu/TiO2 41.1 [36]
3% Cu/TiO2 73.9 [36]
4% Cu/TiO2 61.6 [36]
5% Cu/TiO2 57.30 Current study
Fig. 9 The PL spectrum for pure and Cu/TiO2

3.9 Enhanced Photocatalytic Activity copper doped T iO2. This could be explained that band gap
decrease for the ideal 5% copper doped TiO2 nanoparticles.
The effectiveness of synthetic materials in degrading dyes Rho (B) dye was degraded in this experiment by pure
was tested by using a 400 W metal halide lamp in a con- TiO2, 1%, 2%, 3%, 4%, and 5% Cu/TiO2 nanoparticles,
structed photocatalytic reactor. It was basically believed 65%,70%,80%,75%,87% and 92%of the dye, respectively.
that Cu/TiO 2 had a very strong photocatalytic catalyst It was shown that, in Fig. 11g, nearly all the remaining Rh
action. 100 ml of filtered water and 0.1 mg of Rh (B) dye (B) was dissolved in 100 min by 5% Cu/ T iO2. The Fig. 11
are combined for the experiment, stirred, and then allowed shows, the degradation efficiency rises significantly with
to sit in the dark for 20 min. The reactor is filled after exposure time. T iO2 functions as a scavenger and quencher,
the Cu/TiO2 catalyst is added to the 0.01 g dye solution. so slowing down the rate in which electrons and holes
An examination of the UV and Vis twin beam spectrum recombine. The following mathematical formulations are:
was performed with 5 ml sample extracted from solution
Cu∕ TiO2 + hv → Cu∕ TiO2 (e− ) + Cu∕ TiO2 h+ (5)
( )
every 20 min and devoted a hundred minutes using that
approach.
The same procedure is repeated for Cu/TiO2 [39], and Cu∕ TiO2 h+ + MB∕MO∕Rh(B)(dye)
( )
the same procedure has been carried out once more to figure (6)
→ MO∕MB∕Rh(B)+ (dye) + Cu∕ TiO2
out the
( )
Cu∕ TiO2 h+ + H2 O → Cu∕ TiO2 + OH − + H + (7)
( )
C
Degradation Efficiency(%) = 1 − × 100 (3)
Co
Cu∕ TiO2 h+ + OH − → Cu∕ TiO2 + OH . (8)
( )
( )/
Co
Rate constant(k) = ln t (4)
C Cu∕ TiO2 (e− ) + O2 → Cu∕ TiO2 + O2 .− (9)
In this case, C o denotes the initial concentration and
C the dye concentration by time t. For the degradation of O2 .− + e− + 2H + → H2 O2 (10)
Rh (B) dye without nanoparticles results into 4% degrada-
tion. Nevertheless, the degradation efficiency dramatically O2 .− + H2 O2 → OH . + OH − + O2 (11)
increased in with the addition of copper doped nanoparticles
results into 92% degradation for Rh (B) dyes. It becomes
O2 .− ∕OH . + dye → CO2 + H2 O (12)
clear that increased dye degradation is correlated with higher
nanoparticles concentrations. For the reproducible process Utilizing the TiO2 catalyst causes water to produce H +
two more dyes are utilized to check the photodegradation and OH − ions. The Rh (B), a positively charged dye is cre-
of methyl blue (MB) and methyl orange (MO) only for the ated when holes interact with dye.
optimal 5% Cu-TiO2. It shows the maximum degradation as An anion radical known as superoxide is claimed to be
compared to others. The 5% Cu∕ TiO2 is utilized at different produced when electrons and oxygen O2 react. Peroxide
concentrations (10, 27, and 50 mg) in the presence of UV radicals and hydrogen ions are produced by the interaction
light for 60 min allowed for the evaluation of photocatalytic of OH − and radicals. Strong oxidants are produced when
degradation of the MO and MB dyes, It is significant that these hydrogen ions and peroxide radicals mix with the
dyes play most the critical role in the breakdown of the cata- superoxide anion to form hydroxyl radicals. After reacting
lyst UV–visible spectroscopy was utilized to measure the with Rh (B), these oxidants produce water and CO2 as rep-
absorbance of the MO and MB dyes during a 10-min inter- resented in the photocatalysis degradation mechanism. In
mission. Dye degradation is caused by the strong combina- Fig. 11a represents the absorption of the pure and (1–5%)
tions of the oxidizing agents. It is frequently assumed that Cu- TiO2 (b), represents the degradation of pure T iO2 (c),
the substance variety engaged in the photocatalytic reactions represents the degradation of 1% Cu- T iO2 (d), represents
will also contain H + , O2 and OH . ions. The Cu/TiO2 and pure the degradation of 2% Cu- T iO2 (e), represents the degrada-
UV–Vis spectra are shown in Fig. 11. When time interval tion of 3% Cu- TiO2 (f) represents the degradation of 4%
increases absorption peak lowers, indicating the decomposi- Cu- TiO2 represents the degradation of 5% Cu- T iO2 (h)
tion of the Rh (B) dye. The most efficient doping of copper represents Pure and 1–5% Cu-TiO2 degradation efficiency
at all concentrations throughout the process of degradation w.r.t time (i) represents the first-order kinetics for the Pure
is 5% doping in Cu/TiO2, as shown in Fig. 11g. It is impor- and 1–5% Cu-TiO2 nanoparticles (j) demonstrate the out-
tant to keep in mind that the degradation efficiency began comes of the comparison experiment conducted using Rh
to increase and reach the visible light spectrum at about 5%

Fig. 11 a Pure and 1–5% Cu/

TiO2 absorbance UV–Vis spec-
trum b For Pure TiO2 UV–Vis
spectrum for the photocatalytic
activity till 100mint c For 1%
Cu/ TiO2 UV–Vis spectrum
for the photocatalytic activity
till 100mint d For 2% Cu/TiO2
UV–Vis spectrum for the pho-
tocatalytic activity till 100mint
e For 3% Cu/ TiO2 UV–Vis
spectrum for the photocatalytic
activity till 100mint f For 4%
Cu/ TiO2 UV–Vis spectrum
for the photocatalytic activity
till 100mint g For 5% Cu/ TiO2
UV–Vis spectrum for the most
optimized concentration of
the photocatalytic activity till
100mint h For Pure and 1–5%
Cu/TiO2 degradation efficiency
w.r.t time i First-order kinetics
for the Pure and 1–5% Cu/TiO2
nanoparticles j Degradation of
Rh(B) dye in the absence of
nanoparticles. l Degradation of
methyl orange for the 5% Cu/
TiO2 nanoparticles. k Degrada-
tion of methyl blue for the 5%
Cu/TiO2 nanoparticles

Fig. 11 (continued)
Table 6 Degradation value of 5% Cu/TiO2 for MO and MB dyes essential for the practical application of photocatalyst. The
Dye Catalyst Concentrations(mg) Degra-
cyclic stability of 5% Cu-TiO2 was therefore investigated
dation by measuring the catalytic activity over the span of three
(%) cycles of degradation. Throughout three testing cycle 5%
Cu-TiO2 demonstrated a very steady photocatalytic activity
MO 5% Cu-TiO2 10 77
with no evident deactivation. After three testing cycles, it
27 80
was determined that the 5% Cu-TiO2 exhibited remarkable
50 95
stability during multiple reuse cycles, as evidenced by the
MB 5% Cu-TiO2 10 93
degradation stability of 5% Cu-TiO2 for MO and MB dye.
27 95
5% Cu-TiO2 also displayed a very stable photocatalytic effi-
50 96
ciency without any evident deactivation. Table 7 represents
the comparative study of different methods with literature
for degradation of Cu-TiO2.Table 8 represents the compara-
(B) dyes without the nanoparticles, (k) represents the deg- tive study of different dyes degradation of Cu-TiO2. Table 9
radation of Rh (B) dye in the absence of nanoparticles, (l) represents the band gaps and degradation of Rh (B) dye for
represents the degradation of methyl orange for the 5% Cu/ pure and Cu/TiO2 Composites in tabular form and compara-
TiO2 nanoparticles as shown in the Fig. 11. The MO and MB tive study with literature. Table 10 represents the regression
photocatalytic degradation comparison using 5% Cu-TiO2 analysis and first order kinetic constant "k" for pure and Cu/
as the catalyst is demonstrated in the Table 6. It was discov- TiO2 (Fig. 12).
ered that in comparison to pure and 5% Cu-TiO2 results in
more degradation of MB, MO, and Rh(B). Because degra- 3.9.1 Antioxidant Activity
dation results in more active sites and higher oxidation and
reduction rates, it also significantly affects the size, shape, The percentage of scavenging in the samples was determined
and band gap of Cu-TiO2 nanoparticles. Stability is also using the DPPH free radicals assay in order to analyze the

Table 7 Comparative study of prepared sample with previously pub- Table 10 Illustrates the regression analysis and first order kinetic
lished data constant "k" for pure and Cu/ TiO2
Cu/ TiO2 NPs Literature Sr Material 1st Order Correlation Residual
Synthesis Maximum degradation Time Kinetic coefficient, R2 sum of
(%) Constant squares
“k” (min−1)
Sol–gel [40] 99 180 min
1 Pure TiO2 0.00869 0.9978 0.0019
Hydrothermal [41] 90 120 min
2 1% Cu/ TiO2 0.01002 0.9776 0.02575
Sol–gel [42] 98 120 min
3 2% Cu/ TiO2 0.01223 0.98844 0.01957
4 3% Cu/ TiO2 0.01189 0.97419 0.04195
Sol–gel [42] 99 120 min
4% Cu/ T iO2 0.01678 0.97634 0.07643
Solvothermal [37] 70 120 min
5 5% Cu/ TiO2 0.01723 0.99561 0.01223
Sol–gel [44] 99 200 min
Sol–gel [45] 90 180 min
for pure and 5% Cu/ T iO2 and ascorbic acid (for standard)
Microwave-assisted sol–gel 90 350 min
[47] were measured i.e. 27, 50, 100, 200, 300, and 700 g/ml
Hydrothermal [36] 99.4 60 min with 2.0 ml of DPPH methanolic solution. Additionally, the
absorbance of the reaction mixtures was measured at a wave-
length of 517 nm at room temperature using a UV–visible
Table 8 Dyes degradation comparison literature with Cu-TiO2 nano- spectrophotometer (Shimadzu, UV–Visible Double Beam
particles Spectrophotometer (UV–VIS 1800). For standard reference,
Dye Exposure time Percentage removal ascorbic acid was also administered in the same concentra-
tions. The stable radical of DPPH can effectively counteract
RO–4 dye [48] 180 min at 3.5 91.19% the antioxidant activity. Equation was used to measure the
pH
percentage of scavenging of ascorbic acid of Pure and 5%
Methyl orange [49] 150 min 94%
Cu-TiO2 and the results are shown in Table 11.
Methyl orange [49] 150 min 94%
Methyl red [50] 120mint – % Scavenging = Io − I∕Io (13)
Methyl red [51] 60 min 89%,83%
Methylene blue (MB) [52] 45 min 13.3% where Io represents the absorbance for pure DPPH and I
Methylene blue, alizarin red, 6h 86.79%, 76.32%, represents absorbance of samples contains DPPH.
crystal violet, and methyl 77.59%,69.06% Figure 13 illustrates the Pure and 5% Cu-TiO2 scavenges
orange [53] ascorbic acid comparison to ascorbic acid. Table 11 indi-
Rhodamine (B) 60mint 99.4% cates that ascorbic acid exhibited a higher percentage of
scavenging, up to 92%. Additionally, Table 12 represents
the scavenging activity of TiO2 composites comparative lit-
Table 9 Band gaps and degradation of Rhodamine (B) dye for pure erature with the current Pure and 5% Cu-TiO2. They show
and Cu/TiO2 composites in tabular form and comparative study with
literature strong correlations with the literature. These comparisons
resulted in the inhibition of DPPH radicals. It demonstrates
Material % Degradation Band gap Literature that when the bandgap increases with the higher of elec-
100mint matched band
gap tron–hole pairs that amplifies the scavenging activity. The
concentration of pure and 5% Cu- TiO2 improves with an
Pure TiO2 65 3.42 eV [30] increase in the percentage of DPPH free radicals scavenged.
1% Cu/ T iO2 70 3.34 eV [30]
2% Cu/ T iO2 80 3.24 eV [20] 3.9.2 Radical Scavenger Analysis
3% Cu/ T iO2 75 3.04 eV [54]
4% Cu/ T iO2 87 2.96 eV, [55] To determine each active species' specific role in the pho-
5% Cu/ T iO2 92 2.86 eV [56] todegradation, scavenging studies were carried. It was the
standard catalyst. When benzoquinone (BQ) (which can
trap (•O2−), potassium iodate ( KIO3) (which can trap e−)
antioxidant activity [24]. The free radical DPPH assay was or isopropanol (IPA) (which can catch (•OH) is added, as
used to evaluate antioxidant activity for the scavenging illustrated in Fig. 14, the removal efficiency drops just some-
capabilities of Pure and 5% Cu/ T iO2 were examined. After what, suggesting that e−, (•O2−) and •OH are not significant
30 min of dark incubation at 30 °C different concentrations

Fig. 12 Schematic diagram of

photocatalysis mechanism for
the Cu/ TiO2
Table 11 Ascorbic acid % scavenging Value for the Pure and 5% Cu- Table 12 the scavenging activity performance of TiO2 composites
TiO2 nanoparticles with others in literature that had been reported previously
Concentrations % Scavenging Nanoparticles Assay used Scaveng- References
(µL) Ascorbic Pure TiO2 ± 1.25 5% Cu- ing(%)
acid ± 1.5 TiO2 ± 1.25
Sulphur- TiO2 DPPH 90 [57]
27 17 1.3 2 Silver- TiO2 DPPH 70 [58]
50 33 2.4 10 Nitrogen-Neodym- DPPH 93 [59]
63.5 7 27 ium- TiO2
200 82 11.7 49 Nitrogen- TiO2 DPPH 95 [60]
300 90 30 75
800 92 57 90
active species. But ammonium oxalate (AO), which has the
ability to trap h+ significantly affects the reaction rate, indi-
cating that h+ is primary active species in photodegradation.
According to the data, h+ it is still act as catalyst of this
catalysis.
Reactive species such as •OH radicals, superoxide anion
radicals (•O2−) and photogenerated holes h+ can degrade
organic compounds. An approach incorporating different
scavengers was used to investigate the photocatalytic mecha-
nism and to evaluate the role of the principal reactive species
in the dye degradation. The photo-degradation process had
no impact by higher scavenger concentrations. An additional
explanation for such behavior could be higher dye adsorp-
tion onto the photo-catalyst surface, which is enhanced by
increasing amounts of benzoquinone or ammonium oxalate
(AO), Nevertheless, in tests using Rh (B) 10 ppm at scaven-
ger = 1.31 × 10−4 M, the photo-degradation was inhibited.
When ammonium oxalate (AO), h + scavenger, is added
the photodegradation of Rh (B) drops to 44% after 30 min,
whereas it reaches 85% when this scavenger is not present.
Furthermore, benzoquinone, a singlet oxygen scavenger,
inhibited around 80% of the degradation process. Neverthe-
Fig. 13 Scavenging of the ascorbic acid for the pure and 5% Cu-TiO2 less, isopropanol (IPA) a hydroxyl scavenger had no effect
nanoparticles 75% of the time.

Fig. 14 A schematic figure

illustrates how the mecha-
nism of Rh (B) degradation is
affected when specific scaven-
gers are added
Isopropanol (IPA) was found to significantly decrease

the photocatalytic degradation of Rh (B), indicating
that (•OH) acted as an inhibitor of T iO2 photocatalysis.
Additionally, the effects of the superoxide radical anion
•
O2−were investigated with the addition of benzoquinone,
and it was shown that •O2− had no effect on the breakdown
of Rh (B). Furthermore, the role of the holes h + and (•OH)
in the degradation of the Rh (B) dye was investigated by
adding ammonium oxalate (AO).
The results demonstrate that ammonium oxalate (AO)
had the most detrimental effect on the degradation of
the Rh (B) dye, demonstrating that (•OH) is the primary
reactive species and that it plays a significant role in the
dye's degradation. The energy band diagram shown in
Fig. 14 relates to individual T
iO2 pure photocatalysts that
have been treated separately. To develop the correspond-
ing electrical model of the interface between TiO2, more
methodically designed experiments were conducted with Fig. 15 Impact of various radical scavengers on catalytic efficiency
scavengers of the radicals stated above. The photocatalytic for the 5% Cu/ TiO2 nanoparticles
activity sharply drops upon the addition of a specific scav-
enger, suggesting that the trapped radicals are the main
active species in the PS.
It has been observed that when a semiconducting mate- O2−and OH are the primary reactive species in the decom-
rial is activated, these scavengers may absorb holes ( h+), position of Rh (B).
hydroxyl radicals (•OH) and superoxide radicals (•O2−) To examine how the primary active species in degra-
produced in the reaction mixture. The variation in Rh (B) dation of Rh (B) are hydroxyl radical, superoxide radi-
concentration with irradiation duration in the photocatalytic cal anion, and hole. Aqueous solution containing 10 ppm
degradation pathway is depicted in Fig. 15, with and without Rh (B) and 5% Cu/TiO2 photocatalyst was exposed to a
various scavengers like a 5% Cu/TiO2 photocatalyst. The number of quencher species under visible light irradia-
findings show that scavengers such isopropanol (IPA), potas- tion. Figure 15 illustrates that the maximum amount of
sium iodate ( KIO3) and benzoquinone (BQ) are important Rh (B) photodegradation was observed in the absence of
in slowing down the rate of degradation, suggesting that a quencher because all reactive species generated during

illumination contributed to the photodegradation of Rh optimal 5% Cu∕ TiO2 sample is utilized for the pH analy-
(B). sis. The material utilized in this photochemical experiment
was repeatedly washed with ethanol and water to get rid
3.9.3 Recyclability of Optimized Photocatalyst of undesirable ingredients. The results demonstrated that in
each subsequent trial, the photocatalytic degradation rates
Since recyclability is significant from an application stand- of 5% Cu∕TiO2 were however the photocatalytic degradation
point, it was investigated to guarantee the stability of the for PH (6–10) are 30%, 45%, 70%, 75%,, and 88% respec-
photocatalyst. By evaluating its stability, the catalyst with a tively shows the maximum degradation at the pH 10. It has
5% Cu∕ TiO2 mixture was recovered after usage. The mate- been evaluated that in the range of pH 8–10 increases the
rial used in the photochemical experiment was repeatedly hydroxyl radical formation hence increases photocatalytic
washed with ethanol and water to get rid of undesirable efficiency. Figure 17 demonstrate the pH analysis pf optimal
ingredients. 5% Cu∕ TiO2 photocatalyst.
It was dried at 80 °C for three hours before being used in
the following experiment. 3.9.5 Antibacterial Activity
The outcomes demonstrated that in each subsequent trial,
the photocatalytic degradation rates of 5% Cu∕ TiO2 were The disc diffusion method was utilized as test of the antibac-
however the photocatalytic stability for 89%, 87.5%, 84%, terial activity for TiO2 and Cu/TiO2 against four distinct bac-
80%, 77%, 73%, and 67% did not show an obvious decrease terial stains. The results indicated that two strains, namely
in degradation rate. The catalyst did not lessen in contrast. Staphylococcus aureous and Bacillus substilis were gram
The reduction in activity is a consequence of material positive, while Pseudomonas aeruginosa and Escheriachia
depletion with repeated use and considerable degradation coli were gram-negative. After being taken and autoclaved,
of the material's surface photocatalytically active regions. all of the bacterial cultures were renewed and multiplied in
After seven further tests with 5% Cu∕ TiO2 for nutrient broth medium, which was made by mixing 0.64 g of
Rhodamine(B) degradation, the percentage of dye degra- media with 50 ml of distilled water. Four flasks, each hold-
dation can be seen in Fig. 16, demonstrated the material's ing ten milliliters of media, will be used to hold the auto-
enhanced photocatalytic stability by contributing to a slight clave media in order to prevent contamination under LHF
decrease within the catalyst's photocatalytic activity.. (DAIHAN Scientific, MaXtream V12, USA). The 200µL of
the bacterial culture was put under LFH in a flask with NB
3.9.4 pH Analysis medium. After that, the bacterial cultures were kept at 37 °C
for 24 h. Nutrient agar media, which was made by adding
Since pH is crucial factor the for application point of view 2O medium,
2.8 g of neutrient agar to 100 ml of distilled H
it determines the stability of the photocatalyst. For this was well mixed and divided into 4 flasks, each holding 25 ml
of media. The flasks were then autoclaved at 121 °C for
Fig. 16 Highlighting the stability of optimized 5%Cu∕ TiO2 photo-

catalyst for degradation of Rh (B) after seven cycles Fig. 17 The pH analysis of the optimized 5%Cu∕ TiO2 photocatalyst

15–20 min at 15psi for the test. In accordance with LFH, TiO2 zone of inhibition against Gram-positive S. aureus
autoclave media was allowed to cool to a temperature of 30 measured 10 mm, while the 5% Cu/TiO2 zone measured
to 35 °C before being inoculated with freshly made 250µL 30 mm. The pure TiO2 zone of inhibition measured 25 mm,
of the appropriate bacterial culture and allowed to harden whereas the Cu/TiO2 zone measured 18 mm, against the
in petri plates. The paper discs (5 mm in diameter) were Gram-negative Pseudomonas aeruginosa. The outcomes
positioned along the petri plate boundaries with the use of confirmed the antibacterial properties of these antimicrobi-
sterile forceps. In the middle, an efficient gram-positive and als. Because of their smaller size and high surface to vol-
gram-negative antibiotic called Kanamycin was utilized as ume ratio, manufactured nanoparticles have an antibacterial
a control. Samples are added to dimethyl sulfoxide (DMSO) impact. These properties can be used as more functional
and dissolved. The samples are then placed onto the discs compounds with antimicrobial activity. Figure 18 shows the
around the petriplates' perimeter. After letting the solution antibacterial activity of pure TiO2 and 5%Cu TiO2 that are
on the disc dry up for a little while to prevent it from spread- plots against the (a) Grampositive S. aureus (b) Gram nega-
ing, the petriplates are incubated for 24 h at 37 °C. After a tive P.aeruginosa bacteria (c) represents the histogram of the
day, the zone of inhibition (ZOI) surrounding the disc was antimicrobial activity of pure TiO2 and 5%Cu TiO2
calibrated using a vernier caliper. After three iterations of
the experiment, the diameter of the clear ZOI was measured
and determined to be the mean of three replicates. The pure
Fig. 18 Antibacterial activ-

ity (zone of inhibition, mm)
of pure TiO2 and 5%Cu TiO2
plots against a Grampositive
S. aureus b Gram negative
P.aeruginosa represent using
agar well diffusion method. c
histogram plot represent the
antimicrobial activity (zone of
inhibition, mm) of pure TiO2
and 5%Cu TiO2

3.9.6 Antifungal Activity 4 Scope in Future Applications

The antifungal activity for pure TiO2 and 5% Cu TiO2 was TiO2 Became the among the most essential inorganic
determined with minimal changes using the disc diffusion chemicals for commercial purposes after its discovery in
method documented in the literature. Aspergillus fumigatus 1821. titanium dioxide is white, an insoluble, non-flamma-
was the target of the antifungal activity. Potato Dextrose ble and thermally stable material. This element naturally
Agar (PDA) medium, which was made by adding 100 ml occurs in a variety of rocks and sands and ninth most abun-
of water, was used for screening. This served as a prepara- dant element in the crust of Earth. Usually, ilmenite or leu-
tion for Aspergillus fumigatus growth. The media was auto- coxene ores are utilized to obtain it [6].
claved and contains sources of sulfur, nitrogen, magnetism, Copper doped TiO2 nanoparticles have been receiving a
and carbon. The media was added to the petriplates under lot of attention because of their distinctive characteristics
the LFH and left to set. Utilizing a sterile loop, the cor- and utilization in a variety of industries. These are possi-
responding fungal cultures were streaked onto each plast. bilities for copper doped TiO2 nanoparticles in the future
Filter discs were positioned in the middle of the plate using for examples copper antibacterial properties are widely rec-
sterile forceps. The corresponding discs were loaded with ognized. Copper doped TiO2 nanoparticles can be utilized
10µL of the Terbinafine stocks solution (1 mg/1 ml) and pure in antimicrobial textiles, dressings for wounds and surgical
TiO2 and 5%Cu TiO2 nanoparticles samples. Petriplates were instrument coatings. It can be utilized in the cancer treat-
incubated for 48 to 72 h at 28 °C. Following 48–72 h, the ment in the photothermal therapy and for the purification of
antifungal activity of the pure TiO2 and Cu TiO2 solutions water [4]. They can also be utilized in purification systems
put on the corresponding disk was determined by calibrat- and filters. It has also a potential to improve photocatalytic
ing the clear zones of inhibition. According to this method, reaction efficiency, which is crucial for the environment and
an Agar plate had to be prepared for every fungus and the solar energy conversion. Copper doped TiO2 nanoparticles
potato dextrose gar plate had to be sterile. Greater than that can be utilized in the supercapacitors and batteries that
of the resistant strains was the zone of inhibition for the might be increases the longevity and performance. Copper
strains that were susceptible to copper nanoparticles. Fumig- doped TiO2 can be utilized in the medical devices and fur-
atus Aspergillus and Zone of inhibition data as presented in ther bacterial infections. It can be utilized as the Potential
Fig. 19 and further numerical details provided that 5% Cu/ application in biomedical for example in implants dental and
TiO2 zone measured 15 mm, whereas the pure TiO2 zone bones where biocompatibility is essential. It can also be uti-
of inhibition against Aspergillus fumigatus fungi measured lized in the smart drug delivery devices that releases medi-
10 mm. Aspergillus fumigatus exhibited the highest sensitiv- cations in reaction to the particular triggers that includes
ity to copper nanoparticles. changes in pH or light. Copper doped TiO2 nanoparticles
have anti-bacterial qualities that can be utilized as an active
Fig. 19 a Antifungal activity (zone of inhibition, mm) for pure TiO2 and 5% Cu TiO2 b histogram, plots represents the (zone of inhibition, mm)
for pure TiO2 and 5% Cu TiO2

component in pesticides that possibly lowers the need for Availability of Data and Materials All data generated or analyzed dur-
conventional chemical pesticides and lower environmental ing this study are included in this published article.
impact. Improving photocatalysis selectivity and efficiency
Declarations
is still a major challenge. The most significant difficulties
to be addressed involve handling rapid recombination of Competing Interests The authors declare no competing interests.
charges and devising approaches to efficiently harvest vis-
ible light. Ethical Approval Not applicable.
Consent to Participate Not applicable.
5 Conclusion
Pure and (1 to 5%) Cu/TiO2 concentrations are synthesized References

through the coprecipitation method. It has been determined
that doping has significant effects on these synthesized nano- 1. A.A. Saraev et al., Cu/TiO2 photocatalysts for CO2 reduction:
particles morphological and structural characteristics. XRD structure and evolution of the cocatalyst active form. Trans. Tian-
jin Univ. 30, 1–12 (2024)
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Journal of Inorganic and Organometallic Polymers and Materials

Efficient Fabrication of Cu‑Doped ­TiO2 Nanoparticles for Enhanced

Received: 12 May 2024 / Accepted: 21 June 2024

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Keywords Antimicrobial · Cu-TiO2 · Co-precipitation · Degradation · Organic pollutants · Photocatalysis · TiO2

1 Introduction TiO2 is found in both crystalline forms and amorphous.

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Table 2 Chemicals utilized Chemicals Chemical formula Company Puritya (%)

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complete mixing, the resulting mixture had been preserved 3 Characterizations

Fig. 1 Mechanism for the Cu-

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Fig. 2 Schematic dia-

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Fig. 3 a SEM image of pure

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dioxide as the evidenced by X-ray diffraction analysis is tetragonal.

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Table 4 Average crystallite size and d-spacing of pure and copper

Pure ­TiO2 8.627281 3.060333 2.982033 3.058341

The Raman spectra of the pure and the 5% Cu-TiO2 samples

Fig. 6 The Raman spectrum for pure and 5% Cu-TiO2

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3.7 Photoluminescence Evaluations 3.8 BET analysis

Fig. 10 Adsorption–desorption isotherms of 5% Cu-TiO2

Table 5 BET analysis comparison with literature

Pure ­TiO2 31.3 [36]

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Fig. 11 a Pure and 1–5% Cu/

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Fig. 12 Schematic diagram of

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Fig. 14 A schematic figure

Isopropanol (IPA) was found to significantly decrease

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Fig. 16 Highlighting the stability of optimized 5%Cu∕ TiO2 photo-

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Fig. 18 Antibacterial activ-

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3.9.6 Antifungal Activity 4 Scope in Future Applications

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Consent to Participate Not applicable.

Pure and (1 to 5%) Cu/TiO2 concentrations are synthesized References

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Efficient Fabrication of Cu‑Doped TiO2 Nanoparticles for Enhanced

complete mixing, the resulting mixture had been preserved 3 Characterizations

Pure TiO2 8.627281 3.060333 2.982033 3.058341

3.7 Photoluminescence Evaluations 3.8 BET analysis

Pure TiO2 31.3 [36]

3.9.6 Antifungal Activity 4 Scope in Future Applications