Synthesis of magnetite nanocubes ( Fe₃O₄ ) from Iron ( III ) acetylacetonate by removal gas and higher temperature obtained

Introduction

Recently, considerable research has been focused on iron oxides due to their potential uses in  pigments, magnetic drug targeting, magnetic resonance imaging for clinical diagnosis, recording material and catalysts, etc. [1- 6]. The magnetic nanoparticles exhibit super paramagnetic 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 Fe₃O₄ 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- 10].

These methods are  used to prepare magnetite nanoparticles with several controllable particle diameters. However, well-dispersed aqueous Fe₃O₄ nanoparticles have met with very limited success [ 11- 13 ].

In this paper,  preparation of  Fe₃O₄ nanocubes  is reported by  removal  of the gas as well as higher temperature  was used to obtain  Fe₃O₄  nanocubes in powder form under  oven vacuum   at  80 ⁰C temperature .

Experiment

Materials

 Physical parameters of  Iron ( III ) acetylacetonate ( 99 % ,Across ),  4- biphenylcarboxylic  acid , oleic  acid   and Benzyl ether 98 %   are reported in table 1 , 2 ,3 and  4 respectively.

Trade Name	Iron ( III ) acetylacetonate , 99 %
Appearance	Red powder
Molecular weight	353.17
content	25 G R
Company	ACROS ,Organics ,U.S.A

Table 1.  General Characteristics of  Iron ( III ) acetylacetonate ( 99 % ,Across )

 

Trade Name	4- biphenylcarboxylic  a cid, 97  %
Appearance	White  powder
Molecular weight	198.22
density	1.185
Company	Adamas –beta Reagent  Co,Ltd, China

Table 2.  General characteristics of   4- biphenylcarboxylic  acid 97  %

 

Trade Name	Oleic  A cid   ( C18 H34 O2 ) 99.9 %
Appearance	Liquid
Molecular weight	282.46
Density ( 20 0C g/m )	0.870 – 0.90
pH ( 250 g /l ,25 0C	3.0 – 5.0
Company	Sinopharm Chemical  Reagent Co,Ltd, China

Table 3.  General characteristics of  oleic  acid 

 

Trade Name	Benzyl ether  ( C14 H14 O1 ),  98 %
Appearance	Liquid
Molecular weight	198.26
Density ( 25 0C g/m )	1.043 g / ml at 25 0C
pH ( 250 g /l ,25 0C	3.0 – 5.0
Melting point	1.5 – 3.5 0C
Boling point	298  0C
Company	Al-drich  Chemistry

Table 4.  General characteristics of  benzyl ether 98 %   

Notes

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

Synthesis of  Magnetite Nanocubes

Synthesis of ferrimagnetic nanocubes ( Fe₃O₄ )  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 ⁰C  at the rate of 20 ⁰C /min with vigorous magnetic stirring at 290 rpm to get ferrimagnetic nanocubes. where the temperature was held for 30 min when temperature reached  290 ⁰C  .  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 ( CHCl₃ ) . Then after that used   oven vacuum   to obtain  Fe₃O₄  nanocubes in  powder  form at  80 ⁰C temperature [14- 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 chloroform ( CHCl₃ ) 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 300 to 750 nm.

Results and Discussion

Plate  1,2,3 ,4,5,6,7 and 8 ( TEM )  shows the top-view TEM images of the Fe₃O₄   nanocubes  plate  ( TEM ). The surface of  Fe₃O₄ nanocubes  shows several large meandering wrinkles. The size  of  Fe₃O₄  nanocubes  about ( between  39.62 – 48.35 nm )  is  clear from  TEM image . Fig.1. X-ray diffraction  showed the graph all of  Magnetite Fe₃O₄  nanocubes  . Fig .2.  U.V shown the graph all of  Fe₃O₄  nanocubes    respectively dispersed  in chloroform .

Acknowledgements

This work was supported by  UNESCO/People’s Republic of China ( Great wall ) and Al-Baida’a ,University , Republic of  Yemen .

References

1. Maiti.R , Chakraborty .M , J. Alloy and Compod., 2008 , 458 , 450– 456.
2. Riyanto .A, Listiawati .D, Suharyadi .E, Abraha .d. K. Prosiding PertemuanIlmiah XXVI HFI Jateng & DIY, Purworejo , 2012, 14 April, 203-207.
3. Asuhan. S, Wan .H.L, Zhao. S, Deligeer .W, Wu. H.Y, Song.L, Tegus .O. Ceramics Int.  .2012 , 38 , 6579 – 6584.
4. Zhoua .X , Shi.Y,Rena .L, Bao .S , Han.Y, Wu.S, Zhang.H,Zhong.L , Zhang. Q,J. Solid State Chem.  , 2012 , 196 , 138–144.
5. Wang.B ,Wei .Q, Qu. S,Int. J. Electrochem. Sci., 2013 , 8 ,  3786 – 3793.
6. Sun.J, Zhou.S, Hou.P, Yang.Y, Weng.J,Li.X,Li.M,J. Biomed Mater Res 80A : 2007, 333 –341.
7. Jiang.W, Yang.H.C, Yang. S.Y, Horng.H.E ,Hung.J.C,Chene.Y.C , Hong.C.-Y.,J.Mag. Mag. Mater. 2004 , 283 ,  210 – 214.
8. Hu.P, Zhang .S, Wang.H, Pan.D, Tiana.J, Tang.Z, Volinsky.A.A ,J.Alloy. Compd., 2011 , 509 , 2316 – 2319 .
9. J.O. Park, K.Y. Rhee, S.J. Park ,Appl. Surf. Sci., 2010 , 256 , 6945 – 6950.
10. Ur Rahman.O, Mohapatra.S. C, Ahmad. S,Mater. Chem. Phys, 2012,132 ,  196 – 202 .
11. Mukherjee.J, Ramkumar.J ,Chandramouleeswaran. S. ,Shukla.R , Tyagi. A. K.J. Radioanal.Nucl.Chem., 2013 , 22 January .
12. Miyauchi.M,Simmons.T.J, JianjunMiao,Gagner.J.E., Shriver.Z. H.,Aich.U, Dordick .J. S. and Linhardt.R. J, ACS Appl. Mater. Int. 2011, 3, 1958 – 1964.
13. Wang .L.-L. , Jiang. J.-S.Nanoscale Res Lett , 2009, 4 :1439 – 1446 .
14. Nowosielski.R, Babilas.R  ,J.Achievements in Mater. Manuf. Eng., 2011 , 48 / 2 , 153 -160.
15. Mihajlović.G, Xiong. P, and von Molnár. S. Appl. Phys. Lett. 2005 , 87, 112502 -1-3 .
16. Etier. M ,Shvartsman .V. V. , Gao .Y , Landers.J , Wende.H&Lupascu. D.C ,Ferroelectrics, Taylor & Francis ., 2013, 347-177–  355- 185 .
17. Astuti, Claudia.G., Noraida, and Ramadhani .M.,Makara J. Sci, August . 2013, Vol. 17 ,2 ,58- 62 .
18. Kim .D,Lee .N, park .M,Kim.B.H,An.K, and Hyeon .T,J.Am .Chem .Soc. 2009 , 131,  454- 455.

---

This work is licensed under a Creative Commons Attribution 4.0 International License.