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لقطة شاشة 2022-01-06 في 10.08.40 ص
لقطة شاشة 2022-01-06 في 10.08.40 ص
Supervised By
Assistant Professor Dr. Sarmed salih mehdi
Alawadi
2021 AD 1443 AH
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Chapter One Theoretical Part
Abstract
Then many techniques have been done to test the samples and study their
optical properties and internal structure, such as Atomic force
microscopic , Scanning electron microscopic , Energy dispersion x-ray,
X-ray diffraction ,Fourier transfer Infrared ,ultraviolet visible
spectroscopic tests. Finally , many conclusions and suggested future
works are listed.
Chapter One Theoretical Part
List of Terms
AFM Atomic force microscope
AuNP Gold nanoparticles
EDX Energy-dispersive X-ray spectroscopy
FTIR Fourior Transformation at Infrared region
FWHM Full Width Half Maximum
HAuCl4 Gold hydrochloric Acid
NP Nano Particles
PVA Poly Vinyle Alcohol
SEM Scanning electron microscope
SPR Surface Plasmon resonance
TiO2 Titanium dioxide
UV Ultra Violet
V Volume of the solvent
V1 Volume before dilution
V2 Total volume after dilution
W Weight
XRD X-ray diffraction
wavelength
abs wavelength of peak absorbance maximum
Chapter One Theoretical Part
Contents :
Title Page
Chapter one: Introduction and Theoretical Part
1-1 Introduction
1-2 The Importance of Nanoscale
1-3 Nobel Metals Nanoparticles
1-5-1 Reduction 10
Chapter One
Chapter One Theoretical Part
1-1 Introductions:
9
Chapter One Theoretical Part
10
Chapter One Theoretical Part
1- Synthesis of Nanoparticles
12
Chapter One Theoretical Part
13
Chapter One Theoretical Part
Figure 1-3: The top-down approach vs. the bottom-up approach [18].
Figure (1-4) The different strategies & method to synthesis Nanoparticles[ 19]
14
Chapter One Theoretical Part
1-4-2-1Turkevich method
One of the most well-known techniques for synthesising of AuNPs
is based on the reduction of HAuCl4 by citrate in water, was first
designed by Turkevich in 1951.
In this method, the HAuCl4 solution is boiled, and the trisodium citrate
dihydrate is then rapidly added into the boiling solution under vigorous
stirring. After a few minutes, the color of the solution changes from light
yellow to wine red. This method results in AuNPs measuring about 20
nm in diameter. In this technique, citrate ions play a double role , as both
stabilizing and reducing agents.[106]
15
Chapter One Theoretical Part
have been generated in gold, silver and platinum with various reduction
techniques and capping materials [23].
16
Chapter One Theoretical Part
1-5-1Reduction :-
17
Chapter One Theoretical Part
19
Chapter One Theoretical Part
20
Chapter One Theoretical Part
Gold is one of the most noble metal nanoparticales and the most
extensively investigated one due to its unique tunable optical properties,
which can be applied in various applications such as sensing, detecting,
and imaging applications . In the research filed , developing new
protocols for preparing functionalized gold nanoparticles and using them
for biosensing is presently an active research area. The synthesis
techniques of gold nanoparticles have been continuously evolving,
leading to improvements in the control over their size and shape. In
addition to sensing, gold nanoparticles are an attractive candidate for
photothermal therapeutic, diagnostic, and drug delivery applications [107,
108].
Au NPs are being used in biomedical applications, cellular imaging,
molecular diagnosis, targeted therapy, and as contrast agents, photo
thermal agents, and radio sensitizers. Their usefulness is because of their
stability and unique optical, electronic, magnetic, oxidation resistance,
and structural properties, in addition to their structure, composite, and
shape [28]. Noble metal NPs such as Au NPs have been a source of great
interest to their unusual physical properties, especially because of their
sharp Plasmon absorption peak on the visible region. The resonance
frequencies depend on particle shape and size , and are stable for a long
period of months.
1-7-1Properties of Au NPs
22
Chapter One Theoretical Part
23
Chapter One Theoretical Part
Figure 1-6 show the collective oscillation of free electrons under the effect of an
electromagnetic wave [21]
26
Chapter One Theoretical Part
result, the absorption cross- section, which scales with their volume, can
reach values several orders of magnitude larger than common organic
dye molecules. Such collective oscillation is known as surface Plasmon
resonance [65]. In general, the term cross-section is used in physics to
quantify the probability of interactions between particular particles, A
larger extinction cross- section means a higher probability of light being
absorbed or scattered by an optical species [8].
Figure 1-7 Plot of the ratio between the extinction and physical cross- sections versus
the physical size of optical species.[105]
Two aspects are notable from Figure (1- 7) First, the sizes of the four
types of optical species are all smaller than the wavelength of visible
light. Second, only plasmonic nanocrystals have extinction cross- sections
larger than their physical cross-sections. With the ratio between the
extinction and physical cross sections being larger than 1, plasmonic
nanocrystals can strongly concentrate electromagnetic fields in the
vicinity of their physical boundary. This feature enables them to function
as an intermediary to enhance the interactions between other optical
species and far-field light [65]. The metal nanoparticles have a much
stronger interaction with light than the fluorophore [9].
27
Chapter One Theoretical Part
28
Chapter One Theoretical Part
other advantages [68, 69-70]. Because its high refractive index, it is used
as an anti-reflection coating in silicon solar cells and many thin-film
optical devices.
Titanium dioxide is considered an n-type semiconductor due to the
presence of oxygen vacancies in the lattice. These vacancies are formed
upon the release of two electrons and molecular oxygen, leaving a
positive (+2) oxide ion vacancy [71].
contact with eight neighbours (four sharing an edge and four sharing a
corner) [76].
Figure (1-7): Crystalline structures of titanium dioxide: (a) Anatase, (b) Rutile and (c)
Brookite [77]
1-11Photocatalysis
Photocatalysis is defined as (the acceleration of a photoreaction by
the presence of a catalyst). A catalyst does not change in itself or is
consumed in the chemical reaction [78].
The chlorophyll of plants is a type of photocatalyst. Photocatalysis
compared to photosynthesis, in which chlorophyll captures sunlight to
turn water and carbon dioxide into oxygen and glucose , as shown in the
figure (1-8). Photocatalysis creates a strong oxidation agent to breakdown
any organic material to carbon dioxide and water in the presence of
photocatalyst, light and water [78].
30
Chapter One Theoretical Part
31
Chapter One Theoretical Part
1-11-1TiO2 as photocatalyst
32
Chapter One Theoretical Part
Figure (1-9): Band positions of various semiconductors and relevant redox couples
[80]
33
Chapter One Theoretical Part
1-11-3Photocatalytic degradation
Photo-induced holes have been proposed to directly oxidize
adsorbed molecules or react with surface hydroxyl groups to produce
(OH·) radicals. The (OH·) radicals are strong oxidizing species reacting
with almost any organic compounds. They can react with organic
compounds by hydrogen abstraction, electrophilic addition and electron
transfer [81].
The rate of degradation was found to obey (pseudo) first- order kinetics
and hence the rate constant for degradation, (k), was obtained from the
first-order plot of kinetic analysis according to (Langmuir Hinshelwood)
equation [83]:
Ln(A0/A)=kt (1-7)
Where (A0) is the initial absorbance, (A) is the absorbance after a time (t)
of dye degradation under UV irradiation, and (k) is the pseudo first- order
decay rate constant in (min.-1).
1-11-4 Oxidation-Reduction Reactions
35
Chapter One Theoretical Part
36
Chapter One Theoretical Part
1-12Congo red:
Congo red is the sodium salt 3,3 -([1,1 -biphenyl]-4,4 -diyl)bis(4-
aminonaphthalene-1-sulfonic acid), its formula is (C32H22N6Na2O6S2) and
its molecular weight is (696.66 g/mole) and it is considered a secondary
diazo dye because it contains two azo groups (-N=N-) figure(1-14), and
is highly soluble in water resulting from a colloidal solution, but its
solubility is better in the organic solvents such as ethanol, and it absorbs
max=497nm [84,85] . It has a strong
affinity to cellulose fibers. However, Congo red in the cellulose industries
(cotton textile, wood pulp & paper) was used for a long time as a textile
dye , It is an anionic acid dye used as a laboratory aid in testing for free
hydrochloric acid in gastric contents, in the diagnosis of amyloidosis[86].
1-13Antibacterial Activity
1-13-1Escherichia coli
38
Chapter One Theoretical Part
The work aims to synthesis the Au NPs and study the structures
and spectroscopic properties of Au NPs doped photo catalyst materials ,
such asTiO2 NP Analysis of result to identify the prepared samples in
suitable photocatalyst applications such as antibacterial activity and
Water Purification .
Colloidal gold has been used since Ancient Roman times to colour glass
of intense shades of red, or mauve, depending on the concentration of
the metal. A fine example is the famous Lycurgus Cup in the British
Museum, dated 4th century AD[97]. Au colloids have been used in
medicine for all the middle ages believing in their curative properties for
various diseases [98].
39
Chapter One Theoretical Part
40
Chapter One Theoretical Part
41
Chapter One Theoretical Part
42
Chapter Two Experimental part
Chapter Two
43
Chapter Two Experimental part
Introduction
44
Chapter Two Experimental part
The precursors, solvents ,and other chemicals used in this work are
listed in the table (2-1).
258.06 (g/mol)
46.07 (g/mol)
18 (g/mol)
45
Chapter Two Experimental part
W=Mw -1)
C1 V1 =C2 V2 -2)
46
Chapter Two Experimental part
(pale purple). After 5 minutes from the boiling point , the solution was
removed from the heater and continued to stir until it was cooled to room
temperature. All the above procedures have been repeated by variation
the reduction period from 4 minutes to 15 minutes ,that shown in figures
(2-2a)and (2-2b).
of HNO3), then added the first solution to the second solution and mixed
on the stirrer, until the color of the solution changed to white that is a
AuNP TiO2
Figure (2-3): Schematic diagram showing the preparation of Au+ TiO2 nanoparticles
via sol-gel method
48
Chapter Two Experimental part
49
Chapter Two Experimental part
And then exposing the mixture (gold with titanium dioxide and E. coli
bacteria) to radiation (green laser ) for one hour it is important to motion
that the distance between the source and the ray is 15 cm ,Then activated
in a bacterial medium N_ Agar, The same process had been done by using
a UV lamp .
50
Chapter Two Experimental part
51
Chapter Two Experimental part
The data obtained from the XRD measurements can be used to calculate
the crystallite size (C.S.) of the prepared samples according to Debye-
Scherer's formula [102]:
D= -4 )
53
Chapter Two Experimental part
the sample surface can be achieved based on the interactions between the
tip and the surface of the sample. It is characterized by imaging almost any
surface type, including polymers, ceramics, composites, glass, and
biological samples. AFM provides several advantages compared to
traditional microscopy techniques. AFMs probe the sample and perform
measurements in three dimensions on the surface of the sample, and hence
can present a three-dimensional image of the sample surface . This
provides a significant advantage over any microscope available
previously , as shows in the figure (2-9).
55
Chapter Two Experimental part
56
Chapter Two Experimental part
57
Chapter Three Results and Discussion
Chapter Three
58
Chapter Three Results and Discussion
3-1 Introduction
In this chapter, the characterizations of the prepared samples were
determined by different parametric tests, such as X-ray diffraction (XRD)
patterns, Fourier-transform infrared spectroscopy (FTIR), scanning
electron microscopy (SEM), Energy-Dispersive X-ray (EDX)
Spectroscopy ,UV-Visible spectroscopy and Atomic Force Microscopic
(AFM). The spectroscopic studies for AuNPs are prepared by chemical
reduction method and study the absorption and fluorescence spectra. Also
, Preparation of Titanium dioxide by sol-gel technique and adding it to
gold colloidal and using it in applications as an anti-bacterial and water
purification.
From the image, it is clear that the prepared AuNp has a red color.
It is clear from the image that the color of colloidal is red which is the
59
Chapter Three Results and Discussion
60
Chapter Three Results and Discussion
61
Chapter Three Results and Discussion
The FTIR spectrum shown in figure (3-5) is recorded for Au/ TiO2
62
Chapter Three Results and Discussion
63
Chapter Three Results and Discussion
The results of AFM test for AuNP 5min sample was produced with
average roughness of 9.312nm and root mean square value of 15.7nm, as
shown in figure (3-7).
The results of AFM test for AuNP 6min sample was produced with
average roughness of 7.441 nm and root mean square value of 10.99nm,
as shown in figure (3-8).
64
Chapter Three Results and Discussion
The results of AFM test for AuNP 8min sample was produced with
average roughness of 6.603 nm and root mean square value of 12.56nm,
as shown in figure (3-9).
The results of AFM test for AuNP 10min sample was produced with
average roughness of 6.224 nm and root mean square value of 12.983nm,
as shown in figure (3-10).
65
Chapter Three Results and Discussion
The results of AFM test for AuNP 12min sample was produced with
average roughness of 7.639 nm and root mean square value of 13.77nm,
as shown in figure (3-11).
The results of AFM test for AuNP 15min sample was produced with
average roughness of 9.514 nm and root mean square value of 13.64nm,
as shown in figure (3-12).
66
Chapter Three Results and Discussion
8 75.25
The results in a table (3-1) show that when the reduction time increases,
the grain size increases.
67
Chapter Three Results and Discussion
The results of AFM test for TiO2 sample was produced with average
roughness of 4.328 nm and a root mean square value of 9.041nm, as
shown in figure (3-13).
The results of AFM test for AuNP+TiO2 sample was produced with
average roughness of 8.828 nm and root mean square value of 13.266nm,
as shown in figure (3-14).
A cursory glance at the images shows that the gold nanoparticles tend to
aggregate in the form spherical with a semi-uniform distribution and that
the particle diffusion within this pool is uniform and the particle size is
approximately constant within the 20-30 nm range.
69
Chapter Three Results and Discussion
Figure(3-15) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 4 minutes as a reduction period
Figure(3-16) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 5minutes as a reduction period
70
Chapter Three Results and Discussion
Figure(3-17) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 6 minutes as a reduction period
Figure(3-18) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 8 minutes as a reduction period
71
Chapter Three Results and Discussion
Figure(3-19) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 10 minutes as a reduction period
Figure(3-20) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using12 minutes as a reduction period
72
Chapter Three Results and Discussion
Figure(3-21) show the SEM image with magnification force = 50 kx of AuNP which
had been prepared using 15minutes as a reduction period
4min
5min
6min
8min 22.1-23.6
10min 22.4-23.8
15min 24.2-26.8
The results in table (3-3) show that when the reduction time increases, the
particle size increases.
73
Chapter Three Results and Discussion
Figure(3-22) show the SEM image with magnification force = 50 kx of TiO2NP which
had been prepared using the sol- gel technique
74
Chapter Three Results and Discussion
Figure(3-23) The SEM picture for Au/TiO2NP prepared by chemical reduction method and sol-gel
techniques.
TiO2 23.8-26.3
Au/TiO2 30.8-47.3
The results in table (3-4) show that when the reduction time increases, the
particle size increases.
Figure(3-24) shows the EDX results for Au+TiO2NP, mixture . From the
EDX spectrum, the existence of gold with 26.88% percentage was
75
Chapter Three Results and Discussion
Figure (3-24)shows the EDX result of Au+TiO2NP which had been prepared by
chemical reduction method and sol gel method
Table (3-5) Percentages of each element as recorded by the EDX
76
Chapter Three Results and Discussion
77
Chapter Three Results and Discussion
Figure(3-25) The total absorption spectra of AuNP prepared by the hot reduction
method
Table (3-6)The values of the peak position of AuNP which had been prepared by
variation the reduction periods
1day
7day
day
30day
78
Chapter Three Results and Discussion
Figure (3-26): shows the absorption spectrum for TiO2 nanoparticles prepared by
sol- gel techniques , the maximum peak absorbance occurred at 369.5 nm.
Figure 3-27 gives an approximation of the energy for this direct allowed
band gap which is determined and equal to 3ev .
79
Chapter Three Results and Discussion
Figure (3-28): shows the absorption spectrum for Au +Tio2 nanoparticles prepared by
hot chemical reduction method and sol- gel techniques
Figure 3-29 gives an approximation of the energy for this direct allowed
band gap which is determined and equal to 2.9ev .
Figure (3-29): shows the absorption spectrum for Au +TiO2 nanoparticles prepared by
3-9Antibacterial effect
same way of processing but used green laser and combined source
between UV lamp and green laser. When using a green laser, notice the
growth of few groups of bacteria ,but when used a combined source
between UV lamp and the green laser does not lead to the growth of
bacteria in the dish .We note the activity of the material against
bacteria.That lead us to important conclusion that the TiO2 and Au must
be effect us to an important conclusion that the TiO2 and Au must be
affected together to get a high anti-bacterial effect because using a
combined source leads to complete absorption inside Au/TiO2 mixture .
UV will be absorbed from TiO2 and green laser will be absorbed from
AuNP .Guide to the health of our conclusion , when green laser had been
used as a single exposure irradiation source, no anti bicameral effect was
observed.
82
Chapter Three Results and Discussion
83
Chapter Three Results and Discussion
84
Chapter Three Results and Discussion
Figure ( 4) The peaks of absorbance with wave length for Combined source between UV lamp and green
laser
85
Chapter Three Results and Discussion
Figure (3-35) The peak of absorbance intensity for Combined source between UV lamp and green laser
Figure (3-36) The dye during the purification stage of Combined source between UV lamp and green
laser
86
Chapter Three Results and Discussion
0 0.3 1
10 0.125 0.41
20 0.11 0.36
30 0.08 0.26
40 0.07 0.23
50 0.06 0.2
60 0.04 0.13
70 0.01 0.03
Figure (3-37) The peaks absorbance with wave length of the sunlight source
87
Chapter Three Results and Discussion
Figure (3-39) The dye during the purification stage of the sun light source
88
Chapter Three Results and Discussion
0 0.3 1
30
0.124 0.41
60
0.118 0.39
90
0.11 0.36
120
0.1 0.33
150
0.074 0.24
180
0.05 0.16
Figure (3-40) The peaks absorbance with wave length of UV lamp source
89
Chapter Three Results and Discussion
Figure (3-42) The dye during the purification stage of the UVlamp source
90
Chapter Three Results and Discussion
Table (3-9)The absorbance and intensity peaks of the UVlamp source
0 0.3 1
30
0.25 0.83
60
0.24 0.8
90
0.23 0.76
120
0.22 0.73
135
0.19 0.63
180
0.15 0.5
Figure (3-43) The peak absorbance with wave length of the blue laser source
91
Chapter Three Results and Discussion
Figure (3-44) The peak of absorbance intensity for the blue laser source
Figure (3-45) The dye during the purification stage blue laser source
92
Chapter Three Results and Discussion
Table (3- )The absorbance and intensity peaks of blue laser source
30
0.295 0.98
60
0.24 0.8
90
0.22 0.73
120
0.21 0.7
150
0.19 0.63
180
0.17 0.56
Figure (3-46) The peaks absorbance with wave length of the green laser source
93
Chapter Three Results and Discussion
Figure (3-47) The peak absorbance intensity of the green laser source
Figure (3-48) The dye during the purification stage of the green Laser Source
94
Chapter Three Results and Discussion
Table (3- )The absorbance and intensity peaks of the green laser source
0 0.3 1
30
0.29 0.96
60
0.25 0.83
90
0.21 0.7
120
0.15 0.5
150
0.14 0.46
180
0.06 0.2
95
Chapter Three Results and Discussion
3-11 Conclusions
96
Chapter Three Results and Discussion
97
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AuNP sol-gel TiO2
PVA
AuNP / TiO 2
E. coli
114
115
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