Synthesis of  Fe₃O₄ nanoparticles from Ironstone from the Republic of Yemen.

Introduction

Recently, a considerable  amount of research  focused on iron oxides , due to their potential uses  in pigments, drug deliverg and resonance imaging for clinical diagnosis, recording material and catalyst, etc[ 1-3]. The magnetic nano particles exhibit superparamagnetic behavior because of the infinitely small coercivity arising from the negligible energy barrier in the hysteresis of the magnetization loop of the particles as predicted [ 4]. There are many ways to prepare Fe₃O₄ nano particles, which have been reported in other papers, such as arc discharge, mechanical grinding, laser ablation, microemulsions, and high temperature decomposition of organic precursors, etc. These methods are used to prepare  magnetice nanoparticle  with controlled  diameters. However, well-dispersed aqueous Fe₃O₄ nano particles have been met with very limited success. Several methods have been published for synthesizing  Fe₃O₄ nano particles, and several research studies have reported the successful preparation of nano- or microscale Fe₃O₄. Using different methods, such as the ultrasonic chemical coprecipitation method and the solvothermal method [2-6] have been for  reported the synthesis of nano particle Fe₃O₄ in organic solvent, and Cupper [ 7] successfully fabricated magnetic Fe₃O₄ covered with a modifiable phospholipid coating . Of these methods, chemical coprecipitation was reported to be the most promising because of its simplicity and productivity [8-10]. The physics of nano scale magnetic materials has been a vivid subject for researchers within the last few decades and the exploration of iron sand from beaches or rivers to prepare magnetic materials on nano scale has been reported in some studies [11]. In this paper, magnetic materials from ironstone mining in Pasaman Barat West Sumatera were investigated, and it was found that ironstone in that area contained 12.462 ppm of iron (Fe), with a susceptibility magnetic value of 888.81 x 10-8 m3/kg by using an atomic absorption spectro photometer and magnetic susceptibility meter.For these reasons, these materials have the potential to be developed and cultivated as raw materials for magnetite (Fe₃O₄). Although there have been many significant developments in the synthesis of magnetic nano particles, the stability of these particles without agglomeration or precipitation is an important issue. It  began with the crushing  of ironstone into powder form and then synthesizing Fe₃O₄ nano particles  by using the coprecipitation method of magnetite ore.

Experiment

Materials

Hydrochloric Acid  ( HCl ) and  Ammonia Solution ( NH₄OH ) were purchased  from Sinopharm chemical reagent Co ,Ltd ,China,and  ironstone was obtained    from Republic of Yemen.

Physical parameters of  Hydrochloric Acid  ( HCl ) ,  Ammonia Solution ( NH₄OH ) and Fe₃O₄  powder  are reported in table 1 , 2 and  3 respectively.

Table 1.  General Characteristics of Hydrochloric Acid  ( HCl )

Molecular  formula	Hydrochloric Acid  ( HCl )
Appearance	liquid
Molecular weight	36 .5
Concentration	36 – 38 %
Company	Sinopharm chemical reagent Co ,Ltd ,China

 

Table 2.  General Characteristics of Ammonia Solution  ( NH₄OH )

Molecular  formula	Ammonia ( NH4OH )
Appearance	liquid
Molecular weight	17.03
Concentration	25 – 28 %
Company	Sinopharm chemical reagent Co ,Ltd ,China

 

Table 3.  General Characteristics of    Fe₃O₄  powder

Molecular  formula	Magentite   oxide powder ( Fe2O3 )
Appearance	Brown     powder
Fe3O4 %	45.31-75
Chorite	37.73-13
Riebeckite	16.95-15
Country	Al-Baida’a ,Yemen.

 

 

Photo1: Fe3O4 Rock Fe3O4 in powder form  Click here to View Photo

 

Experiment

Two  steps of prepararing samples have been reported here . In the first step ironstone was pulverized to obtain a powder . Then a permanent magnet was used to obtain the iron ore.In the second step the iron ore powders were prepared by the chemical coprecitation method .

In typical coprecipitation synthesis procedure , 10 g Fe₃O₄ powder and 20 ml HCl were mixed and heated at 90 ⁰C for one hour . The solutions were filtered and then 25 ml NH4OH (90%) was added to the filtrate .The black precipitate was collected and washed with de-ionized water and pure ethanol three times.

Photo.2 : Equipment Fe3O4 Nano particle ( after dry ) Click here to View Photo

 

Transmission Electron Microscope  ( TEM ) Test

For TEM Test , a small amount of sample was dissolved in  3mL of  deionized water  in test tube and the solution was stirred by ultra-sonication  . Then 10 µ L sample  was transferred to clean Copper Grid  and kept for drying for TEM test.The TEM micro graphs of samples were observed by CM 12 Philips Transmission Electron Microscope .

 

Fig1: XRD for Fe3O4 Iron PowderClick here to View Figure

 

Fig2: Fe3O4 nano particle  Click here to View Figure

 

Results and Discussion

The  Fe₃O₄ nano particle  was synthesized   by  heating to 90 ⁰C of Fe₃O₄ powder . plate  1,2,3 ,4,5,6and 7 ( TEM )  shows the top-view TEM images of the Fe₃O₄   Nano particle plate  ( TEM ) 1  The size of the Fe₃O₄ nano particle  is clear from the  TEM. The surface of Fe₃O₄ nano particle  shows several large meandering wrinkles. The size  of  Fe₃O₄  nanoparticle  can be  clear from  TEM image . Fig (1and 2)  X-ray differaction  shown the graph all of  Magnitite   and Fe₃O₄  nano particle. Fig (3and 4)  U.V shown the graph all of  Magnitite   and Fe₃O₄  nano particle respectively dispersed  in chloroform.

 

Fig3: Magnetite Click here to View figure

 

Fig4: Fe3O4 nano particle  Click here to View Figure

 

Plate1: Fe3O4 nano particle  Click here to View Plate

 

Plate2: Fe3O4 nano particleClick here to View Plate

 

Plate3: Fe3O4 nano particleClick here to View Plate

 

Plate4: Fe3O4 nano particle Click here to View Plate

 

Plate5:  Fe3O4 nano particle Click here to View Plate

 

Plate6: Fe3O4 nano particle Click here to View Plate

 

Plate7: Fe3O4 nano particleClick here to View Plate

 

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