Synthesis And Characterizations Of Iron Oxide Nanoparticle

1180 Kanza Ijaz, Muhammad Ali, Rabia Hameed, Muntasir Ahmed, Gull Zarin, Muhammad Ajmal, Naima Rubab, Muhammad Adnan, Ali https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) ISSN Online: 3007-1941 ISSN Print: 3007-1933 Synthesis And Characterizations Of Iron Oxide Nanoparticle Article Details A B S T R A C T *Kanza Ijaz Institute of Chemistry, University of Sargodha, Pakistan Email: [email protected] Muhammad Ali Department of Physics, University of Agriculture, Faisalabad, Pakistan Email: [email protected] Rabia Hameed Department of Botany, Government college university Faisalabad, Pakistan Email: [email protected] Muntasir Ahmed Department of Chemistry, Govt Degree college Lal Qilla Maidan Dir lower, University of Malakand,Pakistan Email: [email protected] Gull Zarin Department of Physics, University of Agriculture Faisalabad, Pakistan, Email: zari[email protected]m Muhammad Ajmal Department of Physics Khawaja Fareed University of Engineering and Technology Rahimyarkhan, Pakistan Email: Ajmalkhan25243[email protected] Naima Rubab Department of Biochemistry, University of Agriculture, Faisalabad, Pakistan. [email protected] Muhammad Adnan Department of Chemistry, Govt Degree college Lal Qilla Maidan Dir lower, University of Malakand , Pakistan Email: [email protected] Ali Department of biochemistry, University of Agriculture, Faisalabad, Pakistan ali7622[email protected]m Corresponding Author: *Kanza Ijaz Nanotechnology is well-known area of research since the last century. Nanotechnology has attained a lot of attraction over time. The basic component of nanotechnology is the nanomaterial. These are the particles that lie between the ranges of 1 to 100nm in size and are buildup of carbon, organic matter, metals or metal oxide. In the past decade, magnetic nanomaterials have attracted much attention due to their physical properties and technological applications. In this research work, Fe2O3 nanoparticles were first synthesized via a simple coprecipitation method using iron chloride hexahydrate (FeCl3.6H2O) as precursor and ammonia solution as precipitator. The samples were then characterized by, scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive X rays and UVVis spectrophotometer. XRD pattern showed that the iron oxide nanoparticles. The Fe2O3 nano-powders with uniform size were prepared when the samples calcined at 450°C, and the lowest particle size was found to be 30 nm by XRD technique. The surface morphological studies from SEM micrography that the iron oxide nanoparticles where not in same size. In microghraphy confirmed that the particles are irregular in size and shape. The EDX spectrum showed peaks of iron and oxygen free of impurity with fewer elements. Keywords: Synthesis, Characterization, Iron oxide nanoparticles, https://msra.online/index.php/Journal/about https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 11 81 Introduction Nanotechnology Nanotechnology deals with various structures of matter having dimensions of the order of a billionth of a meter. While the word nanotechnology is relatively new, the existence of functional devices and structures of nanometer dimensions is not new, and in fact such structures have existed Soon Earth as long as life itself. The abalone, a mollusk, constructs very strong shells having iridescent inner surfaces by organizing calcium carbonate into strong nanostructured bricks held together by a glue made of a carbohydrate-protein mix. Cracks initiated on the outside are unable to move through the shell because of the nanostructured bricks. The shells represent a natural demonstration that a structure fabricated from nanoparticles can be much strong [1]. Nanotechnology is the cluster of techniques involved in design, synthesis, characterization and application of structures, materials, devices and systems by manipulating shape and size at nanometer scale. At nanometer level, individual molecules and interaction between them becomes important in comparison with the macroscopic properties of the material or device. Control at nanometer scale and manipulation of fundamental molecular structure permits to regulate the bulk macroscopic chemical and physical properties of the material and device [2]. The term nanotechnology, while describing how the dimensional accuracy has improved with elapsing time. He was the first one to study development and advancements in machine technologies over three decades from 1940s to 1970s. He had foreseen the development of dimensional accuracies better than 100 nm by the era of late 1980s. He employed the term nanotechnology for these future developments [3]. Nanotechnology is the study of the controlling the matter on an atom and molecular scale. Generally nanotechnology deals with structures sized between 1-100 nanometers in at least one dimension, and involve modifying or developing materials within that size. It makes the material lighter, stronger, faster, smaller and more durable. Nanotechnology obligates the ability to frame components of molecular size and precise machine. In other words, ‘nanotechnology’ refers to the contrived ability to construct items from the bottom up, using tools and techniques that are being defined to make high performance products. In 1959, a physicist R. Feynman envisioned this theoretical capability. According to National science Foundation, Nanotechnology is the capability to understand, manipulate and control matter at the level of individual atoms and molecules [4]. Nanotechnology has great potential in improving air, water, and soil quality in the environment. It can improve detection and sensing of pollutants and help in the development of new technologies for remediation. Understanding the formation and growth dynamic processes of nanoparticles (e.g., in the combustion system) allows the development of efficient methodologies for minimizing the formation of pollutants in the first place and for reducing their emissions. Although nanotechnology has the potential to improve environmental quality, there are concerns that it can also lead to a new class of environmental hazards [5]. Nanoparticles Nanoparticles (NPs) are at the forefront of rapid development in nanotechnology. Their exclusive size-dependent properties make these materials indispensable and superior in many areas of human activities [6]. Being the most current transition metal in the Earth’s crust, iron stands as the backbone of current infrastructure [7]. However in comparison to group elements such as cobalt, nickel, gold, and platinum, iron oxides are somewhat https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 11 82 neglected. Nanoparticles (NPs) are wide class of materials that include particulate substances which have one dimension less than 100 nm at least [8]. The importance of these materials realized when researchers found that size can influence the physiochemical properties of a substance e.g. the optical properties. A 20nm gold (Au), platinum (Pt), silver (Ag), and palladium (Pd) NPs have characteristic wine red color, yellowish gray, black and dark black colors, in which Au NPs synthesized with different sizes. These NPs showed characteristic colors and properties with the variation of size and shape, which can be utilized in bio imaging applications [9]. A nanoparticle is the most fundamental component in the fabrication of a nanostructure, and is far smaller than the world of everyday objects that are described by Newton’s laws of motion, but bigger than an atom or a simple molecule that are governed by quantum mechanics [10]. In general, the size of a nanoparticle spans the range between 1 and 100 nm. Metallic nanoparticles have different physical and chemical properties from bulk metals (e.g., lower melting points, higher specific surface areas, specific optical properties, mechanical strengths, and specific magnetizations), properties that might prove attractive in various industrial applications. However, how a nanoparticle is viewed and is defined depends very much on the specific application. These properties of nanoparticles have led to its use various applications. The nanoparticles differ from various dimensions, to shapes and sizes apart from their material [11]. A nanoparticle can be either a zero dimensional where the length, breadth and height is fixed at a single point for example nano dots, one dimensional where it can possess only one parameter for example graphene, two dimensional where it has length and breadth for example carbon nanotubes or three dimensional where it has all the parameters such as length, breadth and height for example gold nanoparticles. The nanoparticles are of different shape, size and structure. It be spherical, cylindrical, tubular, conical, hollow core, spiral, flat, etc. or irregular and differ from 1 nm to 100 nm in size. The surface can be a uniform or irregular with surface variations. Some nanoparticles are crystalline or amorphous with single or multi crystal solids either loose or agglomerated [12]. Numerous synthesis methods are either being developed or improved to enhance the properties and reduce the production costs. Some methods are modified to achieve process specific nanoparticles to increase their optical, mechanical, physical and chemical properties [13]. Classification of nanoparticles The nanoparticles are generally classified into the organic, inorganic and carbon based. Organic nanoparticles Dendrimers, micelles, liposomes and ferritin, etc. are commonly knows the organic nanoparticles or polymers. These nanoparticles are biodegradable, non-toxic, and some particles such as micelles and liposomes has a hollow core also known as nano capsules and are sensitive to thermal and electromagnetic radiation such as heat and light [14]. These unique characteristics makes them an ideal choice for drug delivery. The drug carrying capacity, its stability and delivery systems, either entrapped drug or adsorbed drug system determines their field of applications and their efficiency apart from their normal characteristics such as the size, composition, surface morphology, etc. The organic nanoparticles are most widely used in the biomedical field for example drug delivery system as they are efficient and also can be injected on specific parts of the body that is also known as targeted drug delivery [15]. Inorganic nanoparticles Inorganic nanoparticles are particles that are not made up of carbon. Metal and metal oxide based nanoparticles are generally categorized as inorganic nanoparticles [16]. https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 11 83 Metal based nanoparticles That are synthesized from metals to nonmetric sizes either by destructive or constructive methods are metal based nanoparticles. Almost all the metals can be synthesized into their nanoparticles [17]. The commonly used metals for nanoparticle synthesis are aluminium (Al), cadmium (Cd), cobalt (Co), copper (Cu), gold (Au), iron (Fe), lead (Pb), silver (Ag) and zinc (Zn). The nanoparticles have distinctive properties such sizes as low as 10 to 100nm, surface characteristics like high surface area to volume ratio, pore size, surface charge and surface charge density,crystalline and amorphous structures, shapes like spherical and cylindrical and colour, reactivity and sensitivity to environmental factors such as air, moisture, heat and sunlight etc. [18]. Metal oxides based The metal oxide based nanoparticles are synthesized to modify the properties of their respective metal based nanoparticles, for example nanoparticles of iron (Fe) instantly oxidizes to iron oxide (Fe2O3) in the presence of oxygen at room temperature that increases its reactivity compared to iron nanoparticles. The commonly synthesized are Aluminium oxide (Al2O3), Cerium oxide (CeO2), Iron oxide (Fe2O3), Magnetite (Fe3O4), Silicon dioxide (SiO2), Titanium oxide (TiO2), Zinc oxide (ZnO). These nanoparticles have possess an exceptional properties when compared to their metal counterparts [19]. Carbon based The nanoparticles made completely of carbon are knows as carbon based [20]. They can be classified into fullerenes, graphene, carbon nano tubes (CNT), carbon nanofibers and carbon black and sometimes activated carbon in nano size and are presented in Figure1. Figure 1: Carbon based nanoparticles: (a) fullerenes, (b) graphene, (c) carbon nanotubes, (d) carbon nanofibers and (c) carbon black. https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 1184 Fullerenes Fullerenes (C60) is a carbon molecule that is spherical in shape and made up of carbon atoms held together by sp2 hybridization. About 28 to 1500 carbon atoms forms the spherical structure with diameters up to 8.2 nm for a single layer and 4 to 36 nm for multi-layered fullerenes [21]. Graphene Graphene is an allotrope of carbon. Graphene is a hexagonal network of honeycomb lattice made up of carbon atoms in a two dimensional planar surface. Generally the thickness of the graphene sheet is around 1 nm. Carbon Nano Tubes (CNT) Carbon Nano Tubes (CNT), a graphene nanofoil with a honeycomb lattice of carbon atoms is wound into hollow cylinders to form nanotubes of diameters as low as 0.7 nm for a single layered and 100 nm for multi-layered CNT and length varying from a few micrometres to several millimetres. The ends can either be hollow or closed by a half fullerene molecule [22]. Carbon Nanofiber The same graphene nanofoils are used to produce carbon nanofiber as CNT but wound into a cone or cup shape instead of a regular cylindrical tubes. Carbon black An amorphous material made up of carbon, generally spherical in shape with diameters from 20 to 70 nm. The interaction between the particles is so high that they bound in aggregates and around 500 nm agglomerates are formed [23]. Methods for the preparations of nanoparticles Chemical Methods Sol–Gel Sol–gel processing and a wet chemical-synthesis approach are widely used to synthesize magnetic nanoparticles. In this method, the process starts with a chemical solution as precursor undertake different forms of hydrolysis and polycondensation reactions. The solution is then stirring to make a sol. The sol is then dried to form a gel by using chemical reaction. The basic catalysis leads to producing a colloidal gel, while a polymeric form of the gel is produced by means of acid catalysis. The particles produced in this method are significantly influenced by the rate of condensation and hydrolysis. The set of solvent parameters, namely, concentration, pH, and temperature, have impact on the size of the particles too [24, 25]. Hydrothermal Synthesis The hydrothermal synthesis methods can be described as any heterogeneous reactions for synthesizing inorganic materials. The process is carried out by using aqueous solution above ambient temperature above 200°C and higher pressure more than 2000 psi [26] in this method, the experimental procedure involves dissolving the reactants in the water. Then, the solvent will be heated above the boiling point for the desired duration the nanoparticle size increases, when both the amount of water and the time of reaction increase [27]. Co-Precipitation The co-precipitation method is the most commonly used as promising route for generating https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 1185 iron oxide nanoparticles. This method has many advantages such as simplicity, productivity, requires less procedures and hazardous materials, and, therefore, become widely employed for biomedical applications. The production of the iron oxide nanoparticles is undertaken by an ageing of stoichiometric mixture of ferric salts and ferrous in aqueous media [28]. Nanoparticle size, shape, and composition influence significantly on the used salts, the pH of the solution, the temperature, the ratio of Fe2+ and Fe3+, and the media ionic strength. Generally, this method is low cost and becomes much convenient for a very high production rate. However, the great challenge is in the nano-particles involving their aggregation and large size distribution [29]. Microwave Method Microwave method has gain much interesting due to simpler, low cost, a shorter crystallization time, and more energy efficient technique to synthesize new improved nanostructural materials and short crystallization time comparing with the conventional heating methods [28] Therefore, microwave method is a convenient technique for preparing nanocrystalline oxides with possible formation of new metastable phases and rapid heating to reach the required temperature [30]. For preparing iron oxide nano-particles. In this method, the experimental reaction happens by mixing a solution of starting materials Fe (NO3) 2.9H2O and urea. Then, the irradiation process for the mixed solution takes place under 540 W micro-waves for 6 min. Finally, the calcination process undertakes for the pre-pared sample at 800°C for 4 hours to obtain the Fe2O3 nanoparticles [31]. Physical Method The nanoparticles can be generated by using a number of physical methods including laser ablation, chemical vapour decomposition, plasma synthesis, and combustion synthesis. However, the most important challenge with this method is the inability for controlling the particle size in the nanometer range [32]. Applications Medicine Nanotechnology has improved the medical field by use of nanoparticles in drug delivery. The drug can be delivered to specific cells using nanoparticles [33].The total drug consumption and side effects are significantly lowered by placing the drug in the required area in required dosage. This method reduces the cost and side effects. The reproduction and repair of damaged tissue (Tissue engineering) can be carried out with the help nanotechnology. The traditional treatments such as artificial implants and organ transplants can be replaced by tissue engineering. One such example is the growth of bones carbon nanotube scaffolds [34].The use of gold in medicine is not new. In Ayurveda an Indian medical system, gold is used in several practices. One common prescription is the use of gold formemory enhancement. To enhance the mental fitness of a baby gold is included in certain medical preparations [35]. Food The improvement in production, processing, protection and packaging of food is achieved by incorporating nanotechnology. For example a nanocomposite coating in a food packaging process can directly introduce the anti-microbial substances on the coated film surface. One of the example is the canola oil production industry includes nanodrops, an additive designed to transfer the vitamins and minerals in the food [36]. https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 1186 Properties of nanoparticles Physical properties Surface area It has been found that properties vary with particle size. In sub-micrometre particles, forces that govern the atomic or molecular universe dominate to the detriment of statistical aspects, which are revealed at the macroscale. Optical properties Nanoparticles often have particular optical properties, as they are small enough to limit the thickness of the common electron layer of metals; this phenomenon generates quantum effects. Although it is common knowledge that gold is yellow and silicon is grey, gold and silicon nanoparticles are bright red to black. Moreover, gold nanoparticles melt at a much lower temperature (300ºC, 2.5 nm size) than gold slabs that melt at 1064ºC. Solar energy absorption in photovoltaic cells made of silicon-based nanomaterials is much higher than in thin films of the same materials. The smaller the particles, the higher the absorption efficiency [37]. Uniformity Clusters, aggregates or filaments, in other words, the molecular or atomic assemblies that form nanoparticles, are defined by the interaction of forces among the molecules or atoms of a particle and the interaction forces among particles. Functionalization. Nanoparticles of any type can be linked to microbiological entities randomly, through natural processes occurring in atmosphere, water or at the surface of the Earth. Nanoparticles are then directed to living organisms, organelles within the cells and individual protein or RNA molecules. This property is related both to the harmful effects of nanoparticles on the living kingdom and the pharmaceutical or biochemical studies conducted voluntarily, to the level of peptide molecules. Quantum confinement Changes in size-dependent properties also include quantum confinement, a phenomenon which causes spontaneous properties of semiconductivity, conductivity or electric insulation for neighbouring particles less than 10 nm in diameter [38]. Magnetic properties Magnetic NPs are of great curiosity for investigators from an eclectic range of disciplines, which include heterogeneous and homogenous catalysis, biomedicine, magnetic fluids, data storage magnetic resonance imaging (MRI), and environmental remediation such as water decontamination. The literature revealed that NPs perform best when the size is <critical value i.e. 10–20 nm [39].At such low scale the magnetic properties of NPs dominated effectively, which make. The uneven electronic distribution in NPs leads to magnetic property [40]. Experimental work Chemicals The chemicals used in the research work were received and used (FeCl3.6H2O) Hydrochloric Acid HCl (Riedel-de Haen), Sodium Hydro Oxide (NaOH) (Riedel-de Haen), (Scharlau), Copper Sulphate, Zinc Sulphate and Hydrogen per oxide were used. https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 1187 Instruments PH Meter (Bante instruments), UV-Visible spectrophotometer (ModelSP-300 plus, Optima, Japan), Digital balance, Centrifuge Machine(C.F 10, wetig) Magnetic Stirrer hot plate, Mechanical Shaker (Model OS-340C, Taiwan), UV-Light source ( 254 nm, 15 w) scanning electron microscope (JSM 5910, Jeol, Japan), energy dispersive X-rays spectrometer (INCA200/ Oxford instruments) and X-ray diffractometer (Model: JDX-3532, Make: JEOL, Japan) were used. Synthesis of Iron Oxide In the synthesis of iron oxide nanoparticles Fe2O3 first the molar solution of (FeCl3.6H2O) and Sodium hydroxide were prepared at 1:2. We Take 100ml from (FeCl3.6H2O) solution in a plask and add Sodium Hydroxide solution drop wise until the nanoparticles of Fe2O3 take place. Purified nanoparticles were washed many times in distilled water before being dried overnight at 100°C in a Wise oven (Ven oven). The dried particles were ground into powder. Characterization of nanoparticles Scanning electron microscopy: Through SEM we determined the surface morphology of the nanoparticles X rays diffraction. XRD show the crystallinity of nanoparticle. Energy dispersive X rays. Show the elemental composition of nanoparticle. Results and Discussion Characterization of iron oxide The prepared iron oxide were characterized using SEM, EDX, and XRD techniques to determine different properties of iron oxide nanoparticle. Scanning electron microscopy The surface morphology of iron oxide was investigated by SEM scanning electron microscopy. The SEM micrographs of iron oxide nanoparticles are shown in fig 2.the micrographs obtained for the iron oxide nanoparticles show that the particles where not of same size. The SEM image obtained for the particles synthesized by co-precipitation method show that the nanoparticles are irregular in size and shape and very from 10 to 90 nm with aggregation. Figure 2: SEM images of the Fe2O3 nanoparticles X-ray diffraction The XRD data of iron oxide magnetic nanoparticles are in agreement with the standard https://msra.online/index.php/Journal/about Volume 3, Issue 4 (2025) 1188 value of Fe2O3. XRD analysis of the particles (Figure 3) shows well defined Bragg reflection characteristics of Fe2O3. The data shows diffraction peaks at 2θ = 30.103°, 35.451°, 43.088°, 53.516°, 56.998°,62.657° and 74.098°, which can be indexed to the (220), (311), (400), (422), (511), (440) and (533) planes of Fe2O3 in a cubic phase, respectively. Figure 3: X-ray diffraction pattern of iron oxide nanoparticles Energy dispersive X-rays EDX analysis reported in Fig. 4 showed that the respective percent weight of oxygen and iron on the surface of iron oxide nanoparticles was found to be 22.07 and 77.93 %. The EDX data displayed only the peaks for Fe and O atoms which thus confirmed the absence of any impurities during the preparation of desired material. Figure 4: EXD Spectrum of Iron oxide Conclusion Nanotechnology the matter on an atom and molecular scale. Nanotechnology obligates the ability to frame components of molecular size and precise machine. The nanomaterials have attracted much attention due to their physical properties and technological applications. In this research work, Fe2O3 nanoparticles were first synthesized via a simple co-precipitation method using (FeCl3.6H2O) as precursor and Sodium hydroxide NaOH solution as precipitator. The samples were then characterized by, scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive X rays (EDX) and UVVis spectrophotometer. XRD pattern showed that the iron oxide nanoparticles. The Fe2O3