Synthesis of Magnetite Nanocubes ( Fe 3 O 4 ) from Iron ( III ) Acetylacetonate by Removal Gas and Higher Temperature Obtained

Fe3O4 nanocubes were synthesized from Iron ( III ) acetylacetonate ( 99 % ,Across ), 4biphenylcarboxylic acid , oleic acid and benzyl ether 98 % at higher temperature with drying under vacuum. Fe3O4 nanocubes were obtained in powder form . The Fe3O4 nanocubes structures, nanoparticles size, chemical composition, and magnetic properties were characterized by TEM, U.V and XRD .

The magnetic nanopar ticles 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 .
There are many various ways to prepare Fe 3 O 4 nanoparticles, which have been reported in other papers, such as arc discharge, mechanical grinding, laser ablation, microemulsions, and high temperature decomposition of organic precursors, etc [7][8][9][10] .These methods are used to prepare magnetite nanoparticles with several controllable particle diameters.However, well-dispersed aqueous Fe 3 O 4 nanoparticles have met with very limited success [11][12][13] .
In this paper, preparation of Fe 3 O 4 nanocubes is reported by removal of the gas as well as higher temperature was used to obtain Fe 3 O 4 nanocubes in powder form under oven vacuum at 80 0 C temperature.

EXPERIMENTAL Materials
P hy s i c a l p a r a m e t e r s o f I r o n ( I I ) acetylacetonate (99 %, Across), 4-biphenylcarboxylic acid , oleic acid and Benzyl ether 98 % are reported in table 1 , 2 ,3 and 4 respectively.

Notes
Molecular sieves type 4 A 98.5% ,d = 0.69 -0.75 heated them in oven at temperature at 400 0 C for 2-3 hrs and then put them in 50 ml Benzyl ether 98 % in flash to remove water before starting the experimen.

Synthesis of Magnetite Nanocubes
Synthesis of ferrimagnetic nanocubes ( Fe 3 O 4 ) was carried out under nitrogen (N 2 ).Typical synthesis of mangntic nanocubes ( 0.71g,2 mmol ) Iron ( III ) acetylacetonate ( Fe ( acac) 3 mixed with ( 0.41 g,2.1 mmol ) 4-biphenylacarboxylic a cid added to mixture ( 1.129 g , 4 mmol ) oleic acid and ( 10.40 g ,10 ml ) benzyl ether .The mixture solution was degassed at room temperature for 1 hour .The solution was then heated to 290 0 C at the rate of 20 0 C /min with vigorous magnetic stirring at 290 rpm to get ferrimagnetic nanocubes.where the temperature was held for 30 min when temperature reached 290 0 C .After cooling the solution to room temperature , a mixture of ( 40 ml ) toluene and ( 10 ml ) hexane was added to solution .The solution was then centrifuged at 5000 rpm for minutes to precipitate the magnetite nanocubes .The precipitate was washed using ( 10 ml ) chloroform ( CHCl 3 ) .Then after that used oven vacuum to obtain Fe 3 O 4 nanocubes in powder form at 80 0 C temperature [14][15][16][17][18] .

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 micrographs of samples were observed by CM 12 Philips Transmission Electron Microscope.

UV Results
For UV results, a small amount of sample in test tube and then was dissolved in 3mL ethanol or chloroform (CHCl 3 ) into the sample and the solution was stirred by ultra-sonication to make sure the sample was uniform .Then solution was transferred to cavity of spectrophotometer to get the test.Spectra were recorded at 400 to 750 nm.