J Nanostruct 13(3): 673-684, Summer 2023

RESEARCH PAPER

Synthesis of TiO2 Nanoparticles Using Spin-Coating and Drop-

Casting Techniques for Antibacterial Application
Aseel J. Rahma 1*, Hind F. Oleiwi 2,band Haider A. Abbas 3
1
Middle Technical University, Engineering Technical College, Fuel and Energy Department, Baghdad, Iraq
2
Department of Physics, College of Science for Women, University of Baghdad, Iraq
3
Department of postgraduate Affairs, University of Baghdad, Baghdad, Iraq

ARTICLE INFO ABSTRACT

The “drop casting” and “spin-coating” techniques are frequently utilized
Article History: to manufacture nanostructure materials like TiO2, in which the modifying
Received 19 March 2023
layer comprises nanoparticles (NPs). The study aims to use spin-coating
Accepted 27 May 2023
and drop-casting techniques to deposit highly uniform and good adhesion
Published 01 July 2023
nanoparticles. TiO2 NPs have been successfully deposited using the spin-
Keywords: coating technique which has smoother films with discernible crystallinity
used for antibacterial activity. The structural, morphological, and optical
AFM
properties of TiO2 NPs prepared through drop-casting and spin-coating
Drop-casting
techniques were studied using XRD, SEM, AFM, and UV-Vis, respectively.
Spin-coating XRD patterns of TiO2 NPs which were prepared by drop-casting and
Nanoparticles spin-coating techniques and the solution prepared with concentrations
TiO2 of (60,120) g/L was the monoclinic phase of TiO2 nanoparticle. The
average crystalline size was increased with increasing concentrations.
The films have a smooth surface, a high density, and excellent adhesion
to the glass substrate, according to SEM and AFM’s observation of the
images. Additionally, because of the growth in particle size and increasing
solution concentrations, the surface roughness for synthesized samples
increased. UV-Vis illustrated the allowed direct electronic transition and
the value of band gaps increased with increasing concentrations of TiO2
NPs. Finally, all the modification characterizations via the spin-coating
technique contribute to knowing the effect of TiO2 NPs concentrations
on the antimicrobial activity which was increased with increasing NPs
concentration.

How to cite this article

Rahma A. J., Oleiwi H. F., Abbas H.A. Synthesis of TiO2 Nanoparticles Using Spin-Coating and Drop-Casting Techniques for
Antibacterial Application. J Nanostruct, 2023; 13(3):673-684. DOI: 10.22052/JNS.2023.03.008

INTRODUCTION
Titanium dioxide (TiO2) is a very well-known of 2972°C, melting point of 1843°C, and relative
and well-researched material due to the stability density of 4.26 g/cm3 at 25°C. TiO2 is a poorly
of its chemical structure, biocompatibility, and soluble particulate that has been widely used as a
physical, optical, and electrical properties like white pigment [1]. It has an optical and electrical
white noncombustible and odorless powder with properties like a highly refractive index, optical
a molecular weight of 79.9 g/mol, boiling point band gap of around 3.69 ± 0.10 eV, and exhibits
* Corresponding Author Email: aseel.jabbar@mtu.edu.iq blue shift with respect to the bulk anatase. TiO2

This work is licensed under the Creative Commons Attribution 4.0 International License.
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 Aseel J. Rahma et al. / Synthesis of TiO2 Nanoparticles for Antibacterial Application

exists in three mineral forms: anatase, Rutile, serve as examples of “smart” nanotechnology. It
and Brookite [2]. The Rutile type has a tetragonal follows that it is not unexpected that a significant
crystal structure (with prismatic habit) and portion of modern materials research is focused
exhibits a sufficient light scattering effect without on these nano-scale manufacturing methods. [10].
absorption virtually. With a dipyramidal habit and Given the significance of these two techniques for
a crystalline structure that corresponds to the producing NPs, a comparison of their structural,
tetragonal system, the anatase type is typically morphological, and optical characteristics has
employed as a photocatalyst when exposed been conducted. Nanostructures material has
to UV light [3, 4]. As a semiconductor, it has a been created in recent years using a range of
somewhat smaller energy band gap (3.06eV) synthesis techniques, including hydrothermal and
than anatase (3.23eV). The energy band gap solvothermal [3, 11], direct oxidation method
(~3.06eV), as a semiconductor, is slightly lower [12], chemical vapor deposition (CVD), and
than anatase (~3.23eV) [5]. This particular TiO2 is chemical precipitation [13], green synthesize [14],
mostly utilized as a white paint pigment. Brookite electrodeposition [15], microwave [16], drop-
type has an orthorhombic crystalline structure casting [17],and spin-coating method [18]. Utilizing
[6]. TiO2 is often favored in the anatase form drop-casting and spin-coating, two supposedly
because of its high photocatalytic activity, higher “wet” techniques that are extremely comparable.
specific area, non-toxicity, photochemical stability, In the first process, a spin-coater is required; in
and relative affordability. It also has a stronger the second, it is not. Both techniques are well-
negative conduction band edge potential (higher known and straightforward and both instances
potential energy of photogenerated electrons) employed the same solvent. The morphological
[7]. Today, more than four million tons of TiO2 and structural characteristics of the resultant thin
are manufactured annually, and this chemical is films, however, unambiguously define them. Thin
used in a variety of common products [8]. Fig. 1 films are produced via the widely used, simple, and
illustrates an excipient used in the pharmaceutical affordable drop-casting technique. Additionally,
business for the creation of sunscreen in the the films have simply adhered to corning glass
cosmetics sector as a colorant in white plastics and substrates without the need for a binder. The easy
as a reasonably priced and nontoxic food pigment drop-casting method is also a potential choice for
authorized by the appropriate European Union large-area thin film deposition for technological
authorities for food additive safety [9]. In the applications [19]. The versatile sol-gel technology
past 10 years, researchers in the fields of physics, is used to create a range of ceramic materials. In a
chemistry, and engineering have been more typical sol-gel process, the precursors, which are
interested in the development of self-organized frequently inorganic metal salts or metal organic
nanostructures and nanopatterns, which have a compounds like metal alkoxides, are hydrolyzed
wide range of potential uses. The fundamental and polymerized to produce a colloidal suspension
benefit of these procedures is that they can or solution [20]. The phase change from liquid sol

Fig. 1. Various applications of titanium dioxide/titanium dioxide nanoparticles (TiO2/TiO2 NPs)

674 J Nanostruct 13 (3): 673-684, Summer 2023

 Aseel J. Rahma et al. / Synthesis of TiO2 Nanoparticles for Antibacterial Application

to solid gel is caused by complete polymerization step in creating an effective thin film. Before
and solvent loss. Spin coating or dip coating are the deposition process, the soda Lima glass (20
two methods that may be used to create thin mm× 20 mm ×2 mm) was ultrasonically cleaned
coatings on a substrate. When the solution is in acetone and subsequently with 2-propanol for
poured into a mold, a wet gel will develop, and 20 min, and then rinsed with deionized water.
after additional drying and heating, the wet gel The appropriate TiO2 concentration required to
will harden into a thick ceramic. If the solvent in produce a homogenous coating on the substrate
a wet gel is extracted under a supercritical state, a was determined depending on the literature
very porous and low-density substance known as review and used two different concentrations
an aerogel is created [21]. The spin coating process (60 and 120 g/L). TiO2 solutions with different
is one of the main methods for depositing material concentrations were created by mixing P-25 TiO2
layers onto the flat surface of the substrate. This powder with 200 mL of ethanol. The mixtures
method’s foundation is the dispersion of a solution were aggressively churned until uniform and
onto the substrates and anchoring it to them, white in color.
which accounts for how simple it is. The turntable
of this contraption was rotating at thousands of Drop-Casting
revolutions per minute under the control of the The cleaned soda lime glass was carefully coated
central force. The substrate is dried using this with each produced TiO2 nanoparticle (TiO2NPs)
instrument [22].This study focuses on preparation solution for 30 seconds (Fig. 2). The residual solvent
TiO2 NPs using different concentrations and two was removed by heated the substrates at 100℃ for
different techniques (spin coating and drop- 10 min using the hot-plate device to evaporate all
casting). In addition, study the influence of the residual solvent and repeated this process three
concentration and preparing methods on the times. At this stage, TiO2NPs was obtained by
TiO2NPs properties and examined the performance annealed these substrates inside the furnace for
structure as antibacterial activity. one hour at 300℃. TiO2NPs may be made easily
and affordably by drop casting, the dispersion
MATERIALS AND METHODS volume and concentration have an impact on the
Materials film’s thickness and other characteristics as well.
The materials used in this study include chemical The film structure is influenced by the substrate’s
materials like P-25 TiO2 powder (DIREVO Industrial wetness, the velocity of evaporation, and the
Biotech, Germany). Ethanol (Eth) (99% of purity, drying procedure. This method has a number of
Brazil), Deionized distilled water (University of drawbacks, including difficulty controlling film
Baghdad, Conductivity 10 µs/cm), Glass substrate thickness and non-uniform film formation on large
(Alfa Aesar A Johnson Matthey company. wafers [23].

Sample preparation Spin-Coating

Cleaning the substrate is the first crucial P-25 TiO2 powder was combined with 200

Fig. 2. Drop-Casting technique

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 Aseel J. Rahma et al. / Synthesis of TiO2 Nanoparticles for Antibacterial Application

mL of ethanol to create TiO2 solutions with variety of methods. The first technique employed
concentrations of 60 and 120 g/L, respectively. an X-ray diffraction system with a Cu-Ka x-ray
The mixtures were aggressively churned until tube as the target and a power diffraction system
uniform and white in color. Each prepared TiO2 with a wavelength of 1.5406 A to observe the
nanoparticle solution was carefully deposited crystal structure and identify the phase of the
onto the cleaned soda lime glass (20 mm × 20 mm samples produced. The scan mode is continuous
× 2 mm) for the ideal coating time (30 seconds at with a speed of 5.0000 degrees per minute, the
3000 rpm). After each coating process a heating voltage and current are 40 KV, 30 mA respectively.
process at 100 ºC for 15 min. Then, the coated Atomic force microscopy type (AA3000) was used
glass substrates were annealed. These processes to examine the sample surface topography, to
have a number of benefits, including large scale, determine the grain size of agglomerations on the
low temperature production processing, and the surface and roughness for TiO2 NPs prepared on
use of a wide range of substrates, a wide range of glass substrates by two different method (drop-
structural dimensions, minimal material waste, casting and spin-coating). This technique provides
and cheap cost [24]. information regarding sample surface roughness
at the nanoscale scale. UV-Visible region were
Activation and preparation of the Bacterial isolates recorded using spectrophotometer (SHIMADZU
The bacterial isolates used in this study UV- 1650 PC).
were obtained from the Central Environmental
Laboratory/College of Science/ University of RESULTS AND DISCUSSION
Mustansiriya; it was gram-positive Bacteria Surface coating uniformity is an important
(Staphylococcus. Aureus, Staphylococcus criterion in the present study. The optimal TiO2
epidermidis) and Gram-negative bacteria concentration required to produce a uniform
(Pseudomonas. Klebsiella, Streptococcus sp.). coating on the substrate was identified by
To assess the infection antibacterial activity and depositing two different concentrations using two
fungal type (Candida) to assess the infection different methods of TiO2NPs on glass substrates
antifungal activity of these as-prepared NPs. Lines and by analyzing the properties of the TiO2-coated
of bacterial isolates were placed on brain heart substrates. Analytical results indicated that the
infusion agar and incubated for 18 hours at 37℃. optimal TiO2NPs concentration is 120.0 g/L for two
One colony was then picked from the media plate methods. Fig. 4 shows glass substrates coated with
and inoculated in 5 ml of brain heart infusion broth different TiO2NPs concentrations images of these
and then incubated overnight at 37℃. Fig 5 shows samples. As shown in these images, the surfaces
the antibacterial samples at these conditions. of the substrates coated with 60.0 g/L TiO2 appear
rough and uneven and the roughness of the
Characterization coating surface decreases as TiO2 concentration
The prepared samples were analyzed using a increases.

Fig. 3. Spin coating technique with four stages

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Fig. 4. Images of glass surface coated with TiO2 at two solution concentrations

Fig. 5 shows the XRD patterns of TiO2NPs which expressed in Eq.1, can be used to calculate the
prepared by drop-casting technique and the average crystallite size of TiO2 from the full-width
solution prepared with concentrations of (60 and at half maximum (FWHM).
120 g/L). The anatase phase of TiO2 is represented
by all sharp peaks observed in the XRD patterns. D = Kλ / β cosθ (1)
There are noticeable diffraction peaks located at
2q= 25.35°, 37.90°, 48.10° , 54.49° and 62.92º where D is the crystallite size, K is the form factor,
which is observed on the spectra of drop-casting λ is the X-ray wavelength of Cu Ka (0.154 nm), β
process attribute to (101), (004), (200), (105) and is the full-width at half maximum (FWHM), and θ
(204) orientation plane of anatase-TiO2. These is the Bragg angle. Fig. 5 illustrates the results of
results indicate that the synthesized powders calculating the crystallite size of TiO2 produced by
in monoclinic phase of TiO2 nanoparticle can be the drop-casting procedure using the (101) plane
obtained by double-step drop-casting process diffraction peak. The average crystallite size were
and agreed well with (JCPDS card number 01-084- increased from 6.31nm to 8.01nm for 60g/L and
1285). These results are nearly in agreement with 120g/L, respectively. It noticed that the crystallite
research [25]. The well-known Scherrer’s formula, size of the prepared samples are increased by

Fig. 5. The XRD pattern of the synthesized TiO2NPs via drop-casting method

J Nanostruct 13(3): 673-684, Summer 2023 677

 Fig. 6. The XRD pattern of the synthesized TiO2NPs via spin-coating method

increasing the TiO2 concentration and a good the anatase phase detected around 2q values of
agreement with research [26]. 25.20°, 37.78°, 48.08°,54.66° and 63.01º which is
Fig. 6 explains the phase composition and the observed on the spectra of spin coating process
crystalline size of the two samples that prepared attribute to (101), (004), (200), (105) and (204)
by spin-coating technique and the solution orientation plane, respectively. These findings
prepared with concentrations (60, 120 g/L) in the indicate that spin coating can be used to obtain
2q range from 20º to 80º. The anatase phase of powders of TiO2NPs in the monoclinic phase,
TiO2NPs is represented by all sharp peaks observed which agrees well with previous findings (JCPDS
in the XRD patterns. Five peaks were identified in card number 01-084-1285).The average crystallite

Table 1. The structure properties of TiO2NPs prepared by drop-casting and spin-coating approaches

Concentration 2θ dhkl FWHM C.S. Average

Sample hkl Phase
(g/L) (Deg.) (Ao) (Deg.) (nm) C.S. (nm)

25.357 3.0472 1.2899 (101) 6.16304

37.902 2.6286 1.20121 (004) 6.6197
60 48.103 1.8188 2.90319 (200) 5.9487 6.31 Anatase
54.496 1.596 1.2519 (105) 10.825

TiO2 62.922 1.4822 3.92117 (204) 2.0343

(drop-casting) 25.375 3.1272 0.9899 (101) 8.030
37.902 2.7186 1.2012 (004) 6.619
120 48.103 1.9088 2.9031 (200) 5.948 8.01 Anatase
54.496 1.6259 1.2519 (105) 10.825
62.922 1.5648 0.9211 (204) 8.659
25.2 3.1227 0.9468 (101) 8.396
37.78 2.7276 1.0221 (004) 7.779
60 48.08 1.8188 1.1329 (200) 12.99 9.78 Anatase
54.66 1.5359 1.2319 (105) 11.00

TiO2 63.01 1.6648 0.9117 (204) 8.749

(spin-coating) 25.2 3.2527 0.4846 (101) 16.401
37.78 2.7127 1.1120 (004) 7.150
120 48.08 1.8928 2.0319 (200) 8.499 10.84 Anatase
54.66 1.5129 1.0231 (105) 13.244
63.01 1.6568 0.8911 (204) 8.950

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size of TiO2 can be calculated from the Eq.(1) above surface is well covered with grains that are almost
and increased from 9.78nm to 10.84nm for 60 and consistently dispersed throughout it, according
120g/L, respectively, and this is a good agreement to AFM scans, which also demonstrate that the
to researches [26, 27]. Drop-casting and spin- films are homogenous. The nanocrystalline (TiO2)
coating methods have been used to successfully grains are visible in the surface morphology, and
prepare TiO2 nanoparticle, Top-view FESEM when the concentration is raised, they mix to
images of TiO2 with 200 nm scales are shown in produce noticeably denser films. From the images,
Fig. 7 and 8, respectively. The critical roles of it is observed that the films consist of grain size
preparing method in changing the fundamental 55.05nm and 62.037 nm for 60 g/L and 120 g/L,
characteristics of TiO2 and its antibacterial respectively. The films’ surfaces have some degree
activity were examined in detail. According to of roughness to them. Additional information on
FESEM images which were analyzed using Image the surface morphology of thin films is provided
J software, TiO2 was uniformly distributed on FTO by the surface roughness. In optical coatings,
substrate. Additionally, the figures also display the the variation in surface roughness of thin films is
TiO2 crystalline that forms has a smooth surface significant. It impacts the optical characteristics of
and no agglomeration had developed there. thin films and increases optical absorption. These
Figs. 9 (a and b) show the AFM images and the results are nearly in agreement with research [28].
chart of grain density distribution of the TiO2 NPs Fig. 10 shows the AFM images of the TiO2 NPs films
films at varying solution concentrations (60 and at two different solution concentrations 60 and
120 g/L) via drop-casting method. The substrate 120 g/L. The photos clearly show that the films

Fig. 7. FESEM images of the synthesized TiO2NPs via drop-casting method

Fig. 8. FESEM images of the synthesized TiO2NPs via spin-coating method

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 Aseel J. Rahma et al. / Synthesis of TiO2 Nanoparticles for Antibacterial Application

have a smooth surface, a high density, and good prepared by drop-casting method was determined
adhesion to the glass substrate. Also, the surface by extrapolating the linear portion of (αhυ)2 versus
roughness for synthesizing samples increased photon energy (hυ) at αhυ=0, then the intercept
with the increasing solution concentrations due with x-axis at αhυ=0, give the value of Eg. The
to increasing particle size, which increased from energy gap can be calculated from Eq. 2:
63.61nm to 72.44 nm as shown in (Table 2) when
the solution concentrations increase from 60 g/L to 𝛼𝛼ℎ𝜈𝜈 ∝ (ℎ𝜈𝜈 – Eg)2 (2)
120 g/L. The diameter distribution of the samples
demonstrated that the average particle size As shown in Fig. 10 which illustrate the allowed
increased with increasing solution concentrations, direct electronic transition. The value of band gaps
which might be attributed to an increase in film increased from 2.5 eV to 2.87 eV for (60,120) g/L,
crystallanity [29]. This results agrees well with the respectively. Since the film thickness increased
XRD results. significantly with concentration, the thickness
The optical band gap for the TiO2 films that dependence of the band gap can be referred to

Fig. 9. Atomic force microscopy of the synthesized TiO2 nanoparticles using drop-casting technique at two
solution concentrations.

Fig. 10. Atomic force microscopy of the synthesized TiO2 nanoparticles using spin-coating technique at two
solution concentrations.

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Table 2. Average diameter of TiO2 nanoparticles preparing via two different technique (Drop-
casting and Spin-coating) at two different solution concentrations

Solution Average Average Root Mean

Technique Concentration Roughness Diameter Square
(g/L) (nm) (nm) (nm)

60 7.74 55.05 8.93

Drop-casting
120 7.94 62.037 9.16

60 4.74 63.61 5.7

Spin-Coating
120 4.99 72.44 5.76

as I an increase in barrier in polycrystalline films The tested bacteria were uniformly flushed onto
according to change in grain size, since when the Muller-Hinton agar plates using a sterile cotton
grain size increases the wideness of the electronic swab, then for 6 mm diameter wells were made
levels and the band gap increases. This is because using a sterile well drill. Freshly synthesized TiO2
the pairings of electron hole pairs are significantly NPs solutions of (60 and 120) g/L concentrations
closer to one another, making it impossible to were added to the corresponding wells. The
ignore their Columbic contact, resulting in a larger samples were then incubated overnight at 37 °C.
total kinetic energy. Reduced strain and density After the incubation period, the region of inhibition
of dislocations [28]. At the same way noticed (in mm diameter) was observed and tabulated
the band gap will be increased with increasing as shown in Fig. 13. After the incubation period,
the concentration of TiO2 NPs which prepared by positive test results were recorded when an area
spin-coating technique as seen in Fig. 12, and this of inhibition (in mm diameter) was observed
results were a good agreement to research [30]. around the well as shown in (Table3). TiO2 NPs
Antibacterial Activity of the TiO2 Nanoparticles prepared using a spin-coting process exhibited
(NPs) high antibacterials activity against gram-positive
The antibacterial activity of TiO2 NPs was Bacteria (Staphylococcus. Aureus, Staphylococcus
studied using agar-well diffusion method against epidermidis), Gram-negative bacteria
each of the previously mentioned microorganisms. (Pseudomonas. Klebsiella, Streptococcus sp.), and

Fig. 11. The variation of (αhυ)2 versus photon energy of the synthesized TiO2 nanoparticles prepared by drop-casting at two
solution concentrations.

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 Aseel J. Rahma et al. / Synthesis of TiO2 Nanoparticles for Antibacterial Application

Fig. 12. The variation of (αhυ)2 versus photon energy of the synthesized TiO2 nanoparticles prepared by spin-coating at two
solution concentrations.

fungal type (Candida) for both concentrations 60 have a considerably thinner peptidoglycan coating,
g/L and 120 g/L. The maximum inhibition zone for which plays a critical function in preserving cell
gram-positive Bacteria ( Klebsiella. pneumonia) at integrity. Gram-negative bacteria have more
60 g/L TiO2 NPs, while 120 g/L TiO2 NPs showed complex cell walls than Gram-positive bacteria,
the maximum inhibition zone for gram-positive which acts as a diffusion barrier and makes them
Bacteria (Klebsiella. pneumonia) and gram- less vulnerable to antibacterial agents [31].
negative Bacteria (E. coli). TiO2 NPs (60 g/L) show
excellent antibacterial activity against Gram- CONCLUSION
positive (Klebsiella. Pneumonia with inhabition On glass substrates, TiO2 thin films were created
zone 10 mm) than Gram-negative bacteria (E. coli using the drop-casting and spin-coating techniques.
with inhabition zone 6 mm). When opposed to As a function of the concentration, the structural,
Gram-positive bacteria, Gram-negative bacteria

Fig. 13. Antibacterial activity of the synthesized TiO2 nanoparticles prepared by spin-coating at two
concentrations

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Table 3. Zone of inhibition (mm) of A. hydrophila synthesized TiO2

nanoparticles against various microorganisms.

Diameter of inhibition zone (mm)

Microorganisms
60
120 g/L
g/L
Mean
Mean
Staphylococcus. aureus 6 10

Staphylococcus. epidermidis) 8 13

E. coli 6 15

Klebsiella. pneumonia 10 15

candida 6 9

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