Project Report On TiO2
Project Report On TiO2
Contents
CHAPTER I.................................................................................................................. 1
1.1 Introduction.......................................................................................................................................1
1.2 Emergence of Nanotechnology.........................................................................................................1
1.3 Early Stage of NPs..............................................................................................................................1
1.4 Discovery of Carbon (C), Silver (Ag), Zinc (Zn), Copper (Cu), and Gold (Au) Nanoparticles................2
1.5 Classification of NPs...........................................................................................................................2
1.5.1 Carbon-Based NPs......................................................................................................................2
1.5.2 Metal NPs...................................................................................................................................3
1.5.3 Ceramic NPs................................................................................................................................3
1.5.4 Semiconductor NPs.....................................................................................................................3
1.5.5 Polymeric NPs.............................................................................................................................3
1.6 Approaches for the Synthesis of Metal NPs.......................................................................................3
1.6.1 Top-Down (Physical) Approach...................................................................................................3
1.6.2 Bottom-Up Approach..................................................................................................................4
1.6.3 Green/Biological Synthesis.........................................................................................................4
1.7 Applications of NPs............................................................................................................................5
1.8 Structure of Nanoparticles.................................................................................................................5
1.9 Characterization of Nanoparticles Using XRD....................................................................................7
References:-.............................................................................................................................................9
CHAPTER II................................................................................................................ 13
2.1 Review of Literature........................................................................................................................13
References:-...........................................................................................................................................18
CHAPTER III............................................................................................................... 19
3.1 Proposed Plan of Research Work:...................................................................................................19
3.2 GREEN SYNTHESIS METHOD....................................................................................................19
3.3 Synthesis of Titanium Dioxide Nanoparticles:................................................................................19
References.............................................................................................................................................20
CHAPTER I
1.1 Introduction
Nanoparticles (NPs) and nanostructured materials (NSMs) represent an active area of research
and a techno-economic sector with applications expanding across various domains. NPs and
NSMs have gained prominence due to their tunable physicochemical characteristics, such as
melting point, wettability, electrical and thermal conductivity, catalytic activity, light absorption,
and scattering. These properties result in enhanced performance compared to their bulk
counterparts.
Currently, several pieces of legislation in the European Union (EU) and the USA specifically
reference NMs. However, no single internationally accepted definition for NMs exists. Different
organizations vary in their definitions. According to the Environmental Protection Agency
(EPA), “NMs can exhibit unique properties dissimilar to the equivalent chemical
compound in larger dimensions.” The US Food and Drug Administration (USFDA) defines
NMs as “materials that have at least one dimension in the range of approximately 1–100
nm and exhibit dimension-dependent phenomena.” Similarly, the International Organization
for Standardization (ISO) describes NMs as “materials with any external nanoscale
dimension or having an internal nanoscale surface structure.”
Nanofibers, nanoplates, nanowires, quantum dots, and other related terms have been defined
based on the ISO definition. Additionally, the European Commission describes nanomaterials as
“manufactured or natural materials with unbound, aggregated, or agglomerated particles
with external dimensions between 1–100 nm.”
Nanotechnology emerged in the 1980s due to the convergence of experimental advances such as
the invention of the scanning tunneling microscope in 1981 and the discovery of fullerenes in
1985 (Bayda et al., 2019). The popularization of a conceptual framework for nanotechnology
goals began with the publication of the book Engines of Creation in 1986.
Carbon nanotubes have been discovered in pottery from Keeladi, India, dating back to around
600–300 BC. Cementite nanowires have been discovered in Damascus steel, a material that dates
back to around 900 AD; however, its origin and creation method remain unclear. It is unknown
how these materials developed or whether their use was deliberate.
1.4 Discovery of Carbon (C), Silver (Ag), Zinc (Zn), Copper (Cu), and Gold (Au)
Nanoparticles
Carbon NPs were found in 1991, and Iijima and Ichihashi announced the single-wall carbon
nanotube synthesis with a diameter of 1 nanometer in 1993. Carbon nanotubes (CNTs), also
known as Buckytubes, are nanomaterials made of a two-dimensional hexagonal lattice of carbon
atoms. These lattices are bent and joined to produce hollow cylindrical structures.
Carbon nanotubes are carbon allotropes positioned between fullerene (0-dimensional) and
graphene (2-dimensional) (Chen et al., 2021). Additionally, M. C. Lea reported the synthesis of
citrate-stabilized silver colloids almost 120 years ago. This process produces particles with an
average diameter of 7 to 9 nm. Nanoscale size and citrate stabilization are analogous to recent
findings on nanosilver production using silver nitrate and citrate.
Since 1897, a nanosilver formulation known as "Collargol" has been made commercially and
used for medicinal purposes. Collargol, a type of silver nanoparticle, has a particle size of about
10 nanometers (nm). This size range was determined as early as 1907. In 1953, Moudry
developed a different type of silver nanoparticle called gelatin-stabilized silver nanoparticles,
with diameters ranging from 2–20 nm.
Gold NPs (AuNPs) have a long history in chemistry, dating back to the Roman era when they
were used to decorate glassware. With the work of Michael Faraday, who may have been the
first to observe that colloidal gold solutions possess characteristics different from bulk gold, the
modern era of AuNP synthesis began more than 170 years ago.
Faraday investigated the preparation of colloidal suspensions of “Ruby” gold in 1857. AuNPs
exhibit distinctive optical and electrical characteristics. Faraday demonstrated how gold
nanoparticles could create solutions of varying colors under specific illumination conditions.
Nanoparticles (NPs) are categorized into the following classes based on their shape, size, and
chemical characteristics:
Fullerenes and carbon nanotubes (CNTs) are the two essential subcategories of carbon-based
NPs. Fullerenes feature globular hollow cages with pentagonal and hexagonal carbon units, all
sp²-hybridized. These materials possess high strength, electron affinity, and adaptability,
sparking significant economic interest. CNTs, on the other hand, are elongated, tubular structures
with diameters of 1–2 nm. They are classified as single-walled (SWNTs), double-walled
(DWNTs), or multi-walled (MWNTs) based on the number of walls present.
Metal NPs are composed solely of metals and exhibit distinctive electrical properties due to their
localized surface plasmon resonance (LSPR). Cu, Ag, and Au nanoparticles show broad
absorption bands in the visible region of the solar spectrum. Metal NPs are utilized across
various scientific fields due to their size- and shape-controlled synthesis capabilities.
Ceramic NPs consist of inorganic, non-metallic materials with heat resistance and durability.
They are available in various forms, including amorphous, polycrystalline, dense, porous, and
hollow structures. Ceramic NPs find applications in coatings, catalysts, and batteries.
Semiconductor NPs exhibit properties between those of metals and non-metals, making them
suitable for diverse applications. For example, they can absorb and emit light for use in solar
cells or brighter LEDs, or they can be used in bio-imaging and cancer therapy.
Polymeric NPs, often referred to as polymer nanoparticles (PNPs), consist of organic substances
with active agents either surface-adsorbed onto the polymeric core or entrapped within the
polymer matrix. These NPs resemble nanospheres or nanocapsules and are typically within the
size range of 1 to 1000 nm.
There are three primary approaches for the synthesis of nanoparticles (NPs): physical, chemical,
and biological methods. The physical approach is often referred to as the top-down approach,
while the chemical and biological approaches are collectively termed the bottom-up approach.
The biological approach is also referred to as the green synthesis of NPs. Each of these
approaches is further categorized based on specific methods.
Mechanical Milling:
Mechanical milling involves high-energy impact processes using balls inside containers.
This technique is practical for creating nanoscale materials from bulk materials. It is used
for producing oxide- and carbide-reinforced aluminum alloys, wear-resistant coatings,
and various nanocomposite materials.
Electro spinning:
Electro spinning is used to create nanofibers by drawing charged threads from polymer
solutions or melts. A significant advancement in electrospinning is coaxial electro
spinning, which creates core-shell architectures using two viscous liquids.
Laser Ablation:
Laser ablation vaporizes a material by striking it with a high-intensity laser beam,
producing nanoparticles. This eco-friendly method can generate noble metal
nanoparticles, carbon nanomaterials, oxide composites, and ceramics.
In bottom-up methods, atoms and molecules are combined to form nanostructured particles. Key
techniques include:
Green synthesis is an eco-friendly method involving bioactive agents such as plant extracts,
bacteria, fungi, and algae. Green synthesis is cost-effective and eliminates the need for high
temperature, toxic chemicals, or high pressure. Key advantages include minimal contamination
and stability of nanoparticles.
NPs have unique properties that make them highly valuable in medicine. Applications include:
Diagnostics:
Iron oxide nanoparticles (Fe₃O₄ NPs) serve as MRI contrast agents, while gold
nanoparticles (AuNPs) are used for cancer diagnostics.
Tissue Engineering:
Titanium dioxide (TiO₂) NPs stimulate the growth and repair of bone cells.
Antimicrobials:
Silver (AgNPs) and copper (CuNPs) nanoparticles exhibit antimicrobial properties,
making them suitable for wound dressings and medical devices.
Applications in Agriculture
For each structural state of a nanoparticle, there are specific configurations known as “magic
numbers,” representing optimum stability.
Titanium dioxide is an oxide of titanium metal and is an inorganic compound. The formula for
titanium dioxide is TiO₂, and it is composed of two atoms of oxygen and one atom of titanium.
Titanium is the 9th most common element in the Earth's crust and is generally found in plants
and animals. To form titanium dioxide, titanium metal reacts naturally with oxygen.
This oxide is commonly found in sands, soils, ores, and dust, as well as in indigenous deposits. It
is also referred to as titanium (IV) oxide. The color of titanium dioxide is white, and it is
insoluble in water. However, in some cases, the mineral forms of this solid can appear black.
Titanium dioxide is widely used for various purposes, including as an ingredient in paints, food
coloring, and sunscreen. The properties of titanium dioxide make it valuable in different
industries such as the food and cosmetic industries.
Crystal Structures:
Titanium exhibits octahedral geometry in all three of its main dioxides. The geometry of
the rutile form of titanium dioxide is distorted hexagonal. In contrast, the other two forms
of TiO₂—anatase and brookite—exhibit cubic structures. The structure of rutile is a
general pattern that is also adopted by other difluorides and dioxides of metals, such as
RuO₂ and ZnF₂.
Titanium
Dioxide
X-ray diffraction (XRD) is a versatile, non-destructive analytical technique used to identify and
quantify crystalline forms in powdered or solid samples. Diffraction occurs when X-rays interact
with a crystalline structure, creating constructive interference under specific geometric
conditions.
1. XRD Setup:
o Components: XRD analysis requires a source (X-ray emitter), a detector (to
measure diffracted rays), and a sample.
o Sample Preparation: Thin films of nanoparticles are often prepared via drop-
casting onto a low-background substrate. This ensures minimal interference
during analysis.
2. Analysis Process:
o Sample Orientation:
Specific orientations may require precise placement on a goniometer to
measure reflections.
Randomly oriented samples typically need a quick scan over a range of 2θ
diffraction angles.
o Phase Identification:
The crystal phase of the sample is identified through a search-match
process, focusing on high-intensity diffraction peaks.
o Structural Insights:
Different XRD peak patterns correspond to various atomic arrangements
within the sample.
3. Principle of XRD:
o Based on Bragg's Law:: nλ=2dsinθ
λ: X-ray wavelength
n: Order of diffraction (integer)
d: Spacing between atomic planes
θ: Diffraction angle
o Constructive interference occurs when the wavelength of the X-rays matches the
periodic spacing of the atomic planes.
4. Information Extracted:
o From the width, shape, and position of diffraction peaks, one can deduce:
Crystal defects
Crystal size
Crystalline phase
Shape anisotropy
Strain
Texture
Bragg’s Law
The relationship between X-ray wavelength, atomic spacing, and diffraction angle is given by
Bragg’s law:
Where:
Scherrer’s Formula
Where:
DD = Crystalline size
λ = Wavelength of X-rays (Cu KαK\alpha radiation = 1.54 Å)
β = Full Width at Half Maximum (FWHM) of the diffraction peak
θ = Diffraction angle
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CHAPTER II
2.1 Review of Literature
Abstract 1
K. Ganapathi Rao, CH. Ashok, K. Venkateswara Rao, CH. Shilpa Chakra, Pavani Tambur
Research is focused on applying natural systems in science and technology, particularly in
nanotechnology. Aloe vera, a plant rich in vitamins, minerals, amino acids, and fatty acids, has
been utilized to synthesize Titanium dioxide (TiO₂) nanoparticles using a green synthesis
method.
The TiO₂ nanoparticles were characterized using X-ray diffraction (XRD), Particle Size
Analyzer (PSA), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy
(TEM), and Thermo Gravimetric and Differential Thermal Analyzer (TG/DTA). These
techniques were employed to determine the average crystallite size, particle size, morphology,
structure, and thermal stability of the nanoparticles.
Abstract 2
The study synthesized TiO₂ nanoparticles using Aloe vera extract at varying concentrations (10
mL, 20 mL, 30 mL). Techniques such as XRD, UV-Vis spectroscopy, Raman spectroscopy,
FTIR, and TGA characterized the synthesized nanoparticles. MTT assays assessed cytotoxicity
before and after irradiation. Results demonstrated Aloe vera extract effectively acts as a reducing
agent, influencing the size and bioactivity of TiO₂ nanoparticles.
Abstract 3
ABSTRACT-4
In this present work, Titanium dioxide nanoparticles (TiO2 NPs) were successfully synthesized
using both chemical and green synthesis methods. Ethanol provoked the chemical reduction of
ions. In the green synthesis, jasmine flower extract was used as a reducing and stabilizing agent
because it contains alkaloids, coumarins, and flavonoids. The Rutile phase of TiO2 NPs with an
average crystalline size of 31–42 nm was revealed from the XRD pattern. From UV–Visible
spectroscopy, the optically active region of TiO2 NPs at 385 nm represents the visible region
spectrum. The Ti–O–Ti and Ti–O vibration bond formation confirms the formation of TiO2 NPs.
The SEM image of TiO2 NPs reveals spherical-shaped NPs arranged randomly.
The obtained results revealed that the properties of TiO2 nanoparticles were similar in both
processes. The photodegradation of methylene blue dye was investigated, resulting in a
maximum degradation efficiency of 92% achieved at 120 minutes of irradiation. The
photodegradation study shows that the biosynthesized TiO2 NPs exhibit higher degradation
efficiency compared to chemically synthesized TiO2 NPs. The antibacterial activity of prepared
TiO2 NPs was studied using gram-positive and gram-negative strains. The biological activities
of green-synthesized TiO2 NPs are enhanced compared to chemically synthesized TiO2 NPs.
Hence, the degradation efficiency and zone inhibition layer indicate that the prepared TiO2 NPs
are potential candidates for environmental and biomedical applications.
ABSTRACT-5
Pâmela Cristine Ladwig Muraro, Robson Dias Wouters, Gabriela Pereira Chuy, Bruno Stefanello
Vizzotto, Altevir Rossato Viana, Giovani Pavoski, Denise Crocce Romano Espinosa, Virginia Cielo Rech
& William Leonardo da Silva
This work aims to biosynthesize and characterize titanium dioxide nanoparticles (TiO2-NPs) to
evaluate antimicrobial activity, cytotoxicity, and photocatalytic activity under visible irradiation.
X-ray diffraction (XRD), N2 adsorption/desorption, zeta potential (ZP), field emission gun
scanning electron microscopy (FEG-SEM), and scanning electron microscopy with energy-
dispersive X-ray analysis (SEM–EDX) were used for characterization. The antibacterial potential
was evaluated by minimal inhibitory concentration (MIC) against S. aureus and P. aeruginosa. A
central composite rotational design (CCRD 23) was used for experimental design.
XRD diffractogram and FEG-SEM micrograph showed characteristic peaks of TiO2-NPs (about
32 nm) and spherical shapes, respectively. TiO2-NPs had a negative charge surface (−4.9 mV)
with type V and H1 hysteresis and SBET = 118 m² g⁻¹, Dp = 9.2 nm, and Vp = 0.2 cm³ g⁻¹.
EDX results indicated the presence of TiO2-NPs and the effectiveness of green synthesis. The
antimicrobial activity showed no inhibition of any pathogen. Regarding the safety profile, there
was no reduction in cell viability in the 293 T, MDBK, and HaCat cell lines, and reactive oxygen
species (ROS) generation did not cause significant differences compared to the untreated control,
indicating biocompatibility.
The photocatalytic activity showed a degradation of 90% of RhB dye using the ideal conditions
([RhB] = 10 mg L⁻¹, [TiO2-NPs] = 3.5 g L⁻¹, and pH = 7.0) by CCRD under visible irradiation
with a pseudo-first-order kinetic model (k = 0.0146 min⁻¹). Therefore, TiO2-NPs present
applications as alternative metallic nanoparticles for wastewater treatment and show potential for
antimicrobial activity.
ABSTRACT-6
Green synthesis is an alternative method for obtaining nanoparticles for environmentally friendly
purposes. The present work describes the synthesis and characterization of titanium oxide
nanoparticles, starting from three natural sources: orange peel, Hibiscus rosa-sinensis, and Aloe
vera. Titanium (IV) tetrabutoxide in ethanol solution was used as a precursor. The methodology
was based on the sol-gel technique, through which TiO₂ nanoparticles were obtained in the
anatase phase.
The characterization of the nanoparticles was carried out using X-ray diffraction (XRD),
scanning electron microscopy (SEM), and infrared spectrophotometry (FTIR), which allowed the
identification of a good degree of purity and crystallinity of the samples obtained.
ABSTRACT-7
Jayaram Mari Selvi, Mariappan Murugalakshmi, Ponnusamy Sami, Mariappan Gnanaprakash & R.
Thanalakshmi
Green synthesis is a simple, non-toxic, economical, and eco-friendly approach for the synthesis
of nanoparticles (NPs). The implementation of new technologies has led to the Nano revolution,
highlighting the role of plants in bio- and green synthesis of nanomaterials. Plant extracts
employed include neem, lemongrass, Aloe vera, and Indian gooseberry, among others, focusing
on green chemistry principles.
In the present work, NPs of titanium dioxide (TiO₂) were synthesized using an aqueous extract
of Erythrina variegata leaves as a capping agent. The leaf extract acted as a reducing agent for
the conversion of metal precursors into metal-oxide NPs. The E. variegata-mediated TiO₂ NPs
were characterized using UV–Vis absorption spectroscopy, Fourier transform infrared
spectroscopy (FTIR), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX),
and scanning electron microscopy (SEM).
The UV–Vis absorption spectrum showed an absorption band at 317.6 nm, supporting the
formation of TiO₂ NPs. The optical band-gap energy was determined to be 2.35 eV. Further
characterization by XRD supported the crystallinity and purity of the synthesized TiO₂ NPs.
These NPs demonstrated effective dye degradation ability. The green-synthesized TiO₂ NPs
exhibited significant photocatalytic efficacy on methylene blue dye under UV irradiation (using a
multi-lamp photoreactor) and antibacterial activity against pathogenic organisms like
Streptococcus, Staphylococcus, Escherichia coli, and Pseudomonas aeruginosa.
ABSTRACT-8
Annin K. Shimi, Hiwa M. Ahmed, Muhammad Wahab, Snehlata Katheria, Saikh Mohammad Wabaidur,
Gaber E. Eldesoky, Md Ataul Islam, and Kantilal Pitamber Rane
Metal oxide photocatalyst is one of the promising photocatalysts in the water remediation
process. The present work is aimed at synthesizing the green production of TiO2 (G-TiO2)
nanoparticles from mulberry plant extract. Plant phytochemicals serve a different role to produce
the nanophase particles. The bioreductant is a safer and noxious-free compound for synthesizing
the G-TiO2 nanoparticles.
The synthesized G-TiO2 nanoparticles in anatase phase and their crystallite size of 24 nm were
characterized from X-ray diffraction analysis. The Ti-O bonding and plant derivatives and their
reduction were confirmed from FTIR analysis. The wide bandgap of G-TiO2 nanoparticles (3.16
eV) and their optical characterization were captured from UV-DRS analysis.
The spherical surface morphology and their Ti and O elemental configurations were
characterized from FESEM with EDX technique. The photocatalytic dye degradation was
examined against methylene blue dye, and their pseudo-first-order kinetics were evaluated. The
cyclic experiments declared their catalytic potential.
The bacterial resistance of G-TiO2 nanoparticles was examined against gram-positive and gram-
negative bacteria. Hence, the catalytic potential and bacterial stability of G-TiO2 nanoparticles
make them a powerful candidate for water remediation and biomedical applications.
ABSTRACT-9
The present study deals with the synthesis of titanium dioxide nanoparticles using Azadirachta
indica leaf extract. FTIR study reveals the presence of terpenoids, flavonoids, and proteins
considered responsible for the formation and stabilization of titanium dioxide nanoparticles,
while the XRD studies revealed the crystalline nature of titanium dioxide nanoparticles.
Transmission electron microscopy images showed the spherical shape and size ranged from 15 to
50 nm. SEM study revealed that TiO2 nanoparticles were spherical in shape and their size ranged
from 25 to 87 nm.
The antibacterial activity of synthesized TiO2 nanoparticles and TiO2 compound was assayed
against Escherichia coli, Bacillus subtilis, Salmonella typhi, and Klebsiella pneumoniae.
The results of the present study showed that TiO2 nanoparticles inhibited the growth of all the
tested microorganisms. The antibacterial effect is more pronounced in the case of TiO2
nanoparticles as compared with TiO2 compound. The lowest MIC (minimum inhibitory
concentration) value, i.e., 10.42 μg/mL of nanoparticles, was observed against Salmonella typhi
and Escherichia coli, whereas the lowest MBC (minimum bactericidal concentration) value, i.e.,
83.3 μg/mL, was observed against Klebsiella pneumoniae.
ABSTRACT-10
Vishal Verma, Mawaheb Al-Dossari, Jagpreet Singh, Mohit Rawat, Mohamed G. M. Kordy, and
Mohamed Shaban
The synthesis of titanium dioxide nanoparticles (TiO2 NPs) in a green/sustainable manner has
gotten a lot of interest in the previous quarter. Bioactive components present in organisms such
as plants and bacteria facilitate the bio-reduction and capping processes.
References:-
1. K. Ganapathi Rao, CH. Ashok, K. Venkateswara Rao, CH. Shilpa Chakra, Pavani
Tambur, Centre for Nano Science and Technology, Institute of Science and Technology,
Jawaharlal Nehru Technological University, Hyderabad/Hyderabad-85/Telangana/India,
[email protected]
2. N. K. Ahmed, A. Abbady, Yasmin Abo Elhassan & Alaa Hassan Said
3. Subhapriya S., Gomathipriya P.
4. M. Aravind, M. Amalanathan, M. Sony Michael Mary. Received: 18 September 2020 /
Accepted: 27 January 2021 / Published online: 3 March 2021 © The Author(s) 2021
5. Pâmela Cristine Ladwig Muraro, Robson Dias Wouters, Gabriela Pereira Chuy, Bruno
Stefanello Vizzotto, Altevir Rossato Viana, Giovani Pavoski, Denise Crocce Romano
Espinosa, Virginia Cielo Rech & William Leonardo da Silva
6. Maribel Santiago-Teodoro, Daniela Rivera, Agustín Alfredo Torres-Rodríguez
7. Jayaram Mari Selvi, Mariappan Murugalakshmi, Ponnusamy Sami, Mariappan
Gnanaprakash, and R. Thanalakshmi
8. Annin K. Shimi, Hiwa M. Ahmed, Muhammad Wahab, Snehlata Katheria, Saikh
Mohammad Wabaidur, Gaber E. Eldesoky, Md Ataul Islam, and Kantilal Pitamber Rane
9. B. K. Thakur, A. Kumar, D. Kumar
10. Vishal Verma, Mawaheb Al-Dossari, Jagpreet Singh, Mohit Rawat, Mohamed G. M.
Kordy, and Mohamed Shaban
CHAPTER III
Green synthesis of nanomaterials refers to the synthesis of different metal nanoparticles using
bioactive agents such as plant materials, microorganisms, and various bio wastes, including
vegetable waste, fruit peel waste, eggshells, agricultural waste, etc.
Materials:
To synthesize TiO2 nanoparticles, titanium tetraisopropoxide was purchased (TTIP, Sigma-
Aldrich, AR grade, purity >99%). Fresh Aloe vera leaves were obtained and prepared to be used
as a bio-template. Methylene blue was maintained in a glass bottle in the refrigerator until
needed for photocatalytic activity.
References