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العنوان
Preparation and characterization of TiO2-SiO2
nanocomposites and their analytical applications
/
المؤلف
Raia, Marwa Abdel-haliem Mohammed Abdel-haliem .
هيئة الاعداد
باحث / Marwa Abdel-haliem Mohammed Abdel-haliem Raia
مشرف / Ibrahim El-Sayed Ahmed
مناقش / Mostafa Yassin Nassar
الموضوع
Chemistry.
تاريخ النشر
2021.
عدد الصفحات
187 p. :
اللغة
الإنجليزية
الدرجة
ماجستير
التخصص
Analytical Chemistry
تاريخ الإجازة
1/10/2021
مكان الإجازة
جامعة بنها - كلية العلوم - كيمياء
الفهرس
Only 14 pages are availabe for public view

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from 220

Abstract

English summary
This study consists of three main chapters
Chapter 1: Introduction
Chapter one is the introduction including of the definition of nanomaterials, their preparation technique and their application in different field. This chapter also includes a literature survey on the previous work performed on the simple nanostructure metal oxides along with those performed on the mixed nanosized metal oxides and their various applications.
Chapter 2: Experimental
The secondary chapter is including the complete description of metal oxides, reagent and methods used for the synthesis of nanoparticles silicon oxide (SiO2), titanium oxide (TiO2), and nanocomposite via a hydrothermal route.
Nanoparticles of (SiO2). The pure cristoblite phase silicon oxide was prepared via combustion and sol-gel. Using rice husk (RH) or sodium silicate as precursor of silicon oxide, than calcinations at 800oC for 3hr.
Nanoparticles of (TiO2). The pure anatase phase was prepared by hydrothermal method using titanium tetrachloride for 12h at 200 o C.
SiO2/TiO2 nanocomposite. The pure product of SiO2/TiO2was prepared via sol-gel method using silicon dioxide and titanium tetrachloride mixture, then adding amorphous silica and calcinations for 3hr at 800o.
In addition to description of the structure and characteristics of the used drug (CIP) for the adsorption and (DOX) drug delivery investigation. The adsorption of ciprofloxacin (CIP) antibiotic drug on the synthesis nanoparticles of metal oxide has been described. Many factors affecting the adsorption process was described. The adsorption (DOX) drug delivery on as-prepared nanoparticles has been described.
Chapter 3: Results and discussion
This chapter contains the discussion of the obtained results. It can be divided into four main parts:
Part 1: describes the characterization of the as-prepared nanoparticles silicon dioxide as following:
The synthesis SiO2 nanosizes have been characterized using XRD, FT-IR, FE-SEM, HR-TEM, and thermal analysis. The as-synthesis of RH precursor was produced pure nanoparticles SiO2 (” " ~ " ”14nm) by combustion and sol-gel methods. XRD pattern of silica showed the present of pure cristobalite beta phase. The FT-IR spectra of SiO2showed in the strong absorption band at 1108cm-1 shows asymmetric stretching vibration and shear bands of the Si-O-Si bonds. The FE-SEM micrograph of the SiO2 product exhibited that the product consists of aggregates of two main different morphologies; peanut and irregular shape particles. HR-TEM micrographs of of the as-fabricated SiO2 product exhibited that the product is composed of cubic, spherical, and irregular shape particles with an average size of 14 nm which is compatible with the XRD results. Close inspection of the TEM image revealed the porosity of the silica product.
Part 2: Describes the characterization of the as-synthesis TiO2 nanosizes as following:
The synthesis TiO2 nanosizes have been characterized using XRD, FT-IR, FE-SEM, and HR-TEM. The crystal size of TiO2 was produced via hydrothermal method for tetrachloride at 200oC for 12hr. XRD-pattern of TiO2 nanosizes has been shown, and the pure anatase phase present of crystallite size ” " ~ " ” 20nm. The FT-IR spectrum absorption at 487cm-1 indicated that an attributed to the anatase Ti–O–Ti exhibits vibration bond, the band of a broad band at 3382.83 cm-1 corresponding to the stretching vibrations of hydroxyl groups (-OH). In addition, a shoulder band around 1624-1465.9 cm-1 was observed bending vibrations of adsorbed molecular water. FE-SEM morphology of image is composed of highly spherical particles, irregular and granular surface morphology.
HR-TEM image of TiO2 consisted consisted of hexagon, sphere, and cube-like structures. HR-TEM image also revealed the porous structures of the products, and the average particle size was about 20 nm.
Part 3: Describes the characterization of the as-synthesis SiO2/TiO2 nanocomposite as follows:
The prepared SiO2 nanosizes have been characterized using XRD, FT-IR, FE-SEM, HR-TEM, via sol-gel method. FT-IR spectrum peak assignable to the Si–O–Ti vibration can be seen at ” " ~ " ”940 cm-1 while band at ” " ~ " ”794 cm-1 and ” " ~ " ”1198 -1097cm-1 can be attributed to the symmetric vibration and asymmetric stretching vibration of Si–O–Si, respectively. The peak absorption at487cm-1indicated that an attributedto the anatase Ti–O–Ti exhibits vibration bond. The existence of the hetero linkage Ti–O–Si bond at 935cm-1. FE-SEM image nanocomposite of SiO2/TiO2 has rearranged uniform network structure, due to both SiO2 and TiO2 nanoparticles were collected with each other and covering their surface with diameter size of ca.5μm. HR-TEM images existed as hexagonal and irregularly spherical morphology of composite.
Part 4: Adsorption of ciprofloxacin (CIP) drug on SiO2, TiO2 and SiO2/TiO2nanocomposite
This part includes the result and discussion of the factors affecting the removal of the drug under study from their aqueous solution using SiO2, TiO2 and SiO2/TiO2 nanocomposite as adsorbents, and following remarks can be mentioned:
Regarding to the removal of ciprofloxacin (CIP) drug
• The optimum pH for the adsorption of CIP drug was found to be 8, 9, 8.5 for SiO2, TiO2 and SiO2/TiO2 nanocomposite as adsorbents, respectively.
• On increasing the temperature, the adsorption efficiency enhances for SiO2, TiO2 and SiO2/TiO2 nan-adsorbents.
• The drug removal increases with increasing amount of KCl for silicon oxide and titanium oxide, but decrease in case of SiO2/TiO2 adsorbent nanocomposite.
• The data adsorption well the Langmuir isotherm and pseudo second order.
• The adsorption of CIP founded to be endothermic in all case SiO2 andTiO2 and SiO2/TiO2 nanoadsorbent.

Part 5:
Drug loading of DOX loaded SiO2 /TiO2
• The result revealed that, the loading drug capacity was reach to 25%, which indicated relatively high efficiency of drug loading.
Morphology of (DOX-SiO2/TiO2)
• The morphology of the micelles after drug loading was spherical, with a particle size >50nm.
Drug release of DOX loaded SiO2 /TiO2
• This indicates that DOX could be continuously released in the acidic tumor region.
Cell viability
• Results of the study showed that the mean of the Ehrlich ascites cell lines at 24 h of exposure having higher concentration (100) have shown vitality as 50% compared with lower concentration(10) have shown vitality as 61%. The cells are found to be grown on the surface of composite.
• The results clearly revealed that the prepared composite has better biocompatibility nature on Ehrlich ascites cell lines.