Magnetic Properties and Characterization of Spinel Xfe O (X MN, Co, Ni, Cu Yzn) Obtained by Molten Salt Synthesis

Magnetic properties and characterization of spinel XFe2O4
2+
2+
2+
2+
2+
(X=Mn , Co , Ni , Cu y Zn ) obtained by molten salt synthesis
G.A. Covarrubias-Corts 1, J.A. Herrera-Pedroza 1, A. Snchez Martnez 3, C. Ostos-Ortz 4, A. Durn-Hernndez 5, M.L Garca-Guaderrema 2
1
Centro universitario de Tonal (CUTONALA), Av. Nuevo Perifrico No. 555, ejido San Jos Tatepozco, 48525 Tonal, Jal, Mxico.
2
Departamento de Ingeniera de Proyectos, Centro universitario de Ciencias Exactas e Ingeniera (CUCEI), Universidad de Guadalajara, Zapopan, Jalisco. CP. 45100.
3
Catedrtica CONACYT-Centro universitario de Ciencias Exactas e Ingenieras (CUCEI), Universidad de Guadalajara, Zapopan, Jalisco. CP. 45100.
4
Instituto de Qumica, Universidad de Antioquia, AA 12-26, Medelln, Colombia.
5
Universidad Nacional Autnoma de Mxico, Centro de Nanociecias y Nanotecnologa, Ensenada, B.C., Mxico
Key words: Spinel, Molten Salt-Synthesis, Magnetism
e-mail: covarrubias.cga@outlook.com; anthonyhpdz@hotmail.com
Abstract:
Spinel ferrites with XFe2O4 structure where X represents a X2+ cation of Mn, Co, Ni, Cu or Zn, these were synthesized by molt en salt in relation 4:1 of salt
a n d o x i d e s a n d c a l c i n e d a t t e m p e r a t u r e s o f 8 5 0 , 9 0 0 a n d 9 5 0 C , a f t e r w a r d s w e r e c h a r a c t e r i z e d w i t h X - r a y d i ff r a c t o m e t e r, t h e n i n a Vi b r a n t S a m p l e M a g n e t o m eter (VSM) in a physical properties measure system, magnetic hysteresis (M vs H), magnetic properties respect to type of meta l ion with temperature variations
and finally scanning electron microscopy (SEM).
Methodology:
Molten Salt Synthesis
Mixture of precursor oxides

with KCl / NaCl salts
Melting salts process: to 850C 900C950C

Grinding to homogeneity
XO + Fe2O3
4(KCl 1M/NaCl 1M) + (XO + Fe2O3)
XFe2O4
Dry at 150C
Desalting Washes
Analysis
Heating Ramps
1.- 10C/min
100C before final temp.
2.- 5C/min
to final temp
3.- 8hrs. in final temp
4.- Cooling
10C/min to 24C
Results Y Discussions
X-Ray Diffraction
Scanning Electron Microscopy (SEM)

The morphology of the materials has many similarities
between them, indicating that the synthesis method used will
result in the growth of "crystals , on the other hand, the EDS
spectrum indicates that the materials are in the appropriate
atomic distribution for spinel structure.
The result of the X-ray Diffraction shows the presence of the crystalline phase in the spinels cations of nickel (trevorite), Copper
(copper ferrite) and Zinc (franklinite), presenting sizes of crystallite up to 29nm for copper, 104nm for cobalt, 85nm for nickel and
103nm for zinc according to the Scherrer Equation (formula 1), affirming that the phases presented the optimum magnetic
properties at the highest temperature of reaction (image 11 and 12), as it is presented in the case of manganese (Image 4) the
Iwakiite (MnFe2O4) phase is only present at 950C of heating reaction, however this phase is not pure and shows hematite
(Fe2O3) and manganese-iron oxide ((Mn0.983Fe0.017)2O3) like impurities.
Formula 1: Scherrer Equation
Element
Unn (wt.%) Norm (wt.%)
Atom (at.%) Comp.C (wt.%)
3 Sigma (wt. %)
Oxygen
17.82
21.99
50.00
0.00
6.64
Iron
42.12
51.98
33.86
66.87
3.47
Nickel
21.1
26.06
16.14
33.13
1.83
Magnetic Properties
(Hysteresis)
Image 1: X ray parameters for the material X= Ni
Image 6: S.E.M. photography of

NiFe2O4 spinel.
Image 11: Magnetization versus field at a temperature of
300K for different samples synthetized at 950C and those
obtained pure phase.
Molecular weight (g/mol)
Saturation magnetization s
40
1.6786
CoFe2O4 234.6208
63.2
2.6549
CuFe2O4 239.2336
25
1.0708
NiFe2O4
234.3810
Table 1: Experimental Calculated magnetization of TMFe2O4

(TM = Co,Ni & Cu) Samples at 300K.
Image 2: X ray parameters for the material X= Cu

CuFe2O4 spinel.
The results show that all samples have magtetic response at

300K with ferromagnetic order,
except nickel spinel. This last
exhibits antiferromagnetic property (Image 11). At 10K the
magnetic order is maintained,
no significant changes were observed preserving their magnitudes at this temperature. The
thermal effects not take precedence
on
magnetoelastic
energy. About zinc spinels increases are observed in the
magnetization assicuated with
possible paramagnetic property
(Image 12).
Table 3: EDS quantitative analysis for ZnFe2O4 spinel.

Acquisition: 787
Image 14: EDS spectrum NiFe2O4 spinel

Element
3 Sigma (wt. %)
Oxygen
21.38
21.32
50.00
0.00
8.39
Iron
46.67
49.53
33.27
63.71
4.07
Zinc
29.24
29.15
16.73
36.29
2.55
Table 4: EDS quantitative analysis for ZnFe2O4 spinel.

Acquisition: 789
Image 15: EDS spectrum ZnFe2O4 spinel

Element
3 Sigma (wt. %)
Oxygen
18.60
16.30
41.43
0.00
7.72
Iron
64.93
56.91
41.43
73.21
5.28
Copper
30.57
26.79
17.14
26.79
2.62
Table 5: EDS quantitative analysis for CuFe2O4 spinel.

Acquisition: 791
Magnetic Properties
(Type metal ion)
Image 3: X ray parameters for the material X= Co

CoFe2O4 spinel.
Image 12: Magnetization versus field at a temperature of

10K for different samples synthetized at 950C and those
obtained pure phase.
Molecular weight (g/mol)
Saturation magnetization s
43
1.8171
CoFe2O4 234.6208
72.8
3.0582
CuFe2O4 239.2336
28
1.1993
NiFe2O4
234.3810
Table 2: Experimental Calculated magnetization of TMFe2O4

(TM = Co,Ni & Cu) Samples at 10K.
Image 4: X ray parameters for the material X= Mn
Image 5: X ray parameters for the material X= Zn

MnFe2O4 spinel.

ZnFe2O4 spinel.
Image 13 shows the tendency

of saturation magnetization
(Ms) with respect to type metal
ion. At room temperature and at
low temperatures the Ms remains the same, Ms starts above of 0.5T. This property it can
attributed of type spinel formed
according to site A. considering
the spinel formula (AB2O4) where A is= metalic ion located in
tetrahedral sites and B = ion located in Octahedral site. About
this can determine that the
Magnetization may decrease
depending on the location of
metal ion of different subnets
( A and B)
Image 13: Ms, Hc vs metal ion of samples synthetized at

950C and those obtained pure phase and magnetic properties.
a) Temperature at 300K
b) Temperature at 10K
Image 16: EDS spectrum CuFe2O4 spinel

Element
3 Sigma (wt. %)
Oxygen
15.73
15.47
39.43
0.00
6.19
Iron
54.91
53.99
39.43
69.45
4.49
Cobalt
31.07
30.55
21.14
30.55
2.61
Table 6: EDS quantitative analysis for CoFe2O4 spinel.

Acquisition: 794
Image 17: EDS spectrum CoFe2O4 spinel
Conclusion:
The X-Ray Diffraction show how the highest temperatures
presents the purest phases of material, with a morphology of
polydisperse crystals by the synthesis method used. In the
EDS analysis we can see how the atomic distribution is according to the AB2O4 spinel formula in all cases. The magnetic measurements by vibrant sample magnetometer (VSM)
denote a high magnetic response to the samples with Co, Ni
and Cu (3.05, 1.81 and 1.19 Bohr Magnetons respectively),
all the samples has been measured under the same conditions.
Acknowledgements

Magnetic Properties and Characterization of Spinel Xfe O (X MN, Co, Ni, Cu Yzn) Obtained by Molten Salt Synthesis

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Magnetic properties and characterization of spinel XFe2O4

e-mail: covarrubias.cga@outlook.com; anthonyhpdz@hotmail.com

Mixture of precursor oxides

Melting salts process: to 850C 900C950C

4(KCl 1M/NaCl 1M) + (XO + Fe2O3)

Scanning Electron Microscopy (SEM)

Formula 1: Scherrer Equation

Unn (wt.%) Norm (wt.%)

Atom (at.%) Comp.C (wt.%)

Image 1: X ray parameters for the material X= Ni

Image 6: S.E.M. photography of

Molecular weight (g/mol)

Table 1: Experimental Calculated magnetization of TMFe2O4

Image 2: X ray parameters for the material X= Cu

Image 7: S.E.M. photography of

The results show that all samples have magtetic response at

Table 3: EDS quantitative analysis for ZnFe2O4 spinel.

Image 14: EDS spectrum NiFe2O4 spinel

Unn (wt.%) Norm (wt.%)

Atom (at.%) Comp.C (wt.%)

Table 4: EDS quantitative analysis for ZnFe2O4 spinel.

Image 15: EDS spectrum ZnFe2O4 spinel

Unn (wt.%) Norm (wt.%)

Atom (at.%) Comp.C (wt.%)

Table 5: EDS quantitative analysis for CuFe2O4 spinel.

Image 3: X ray parameters for the material X= Co

Image 8: S.E.M. photography of

Image 12: Magnetization versus field at a temperature of

Molecular weight (g/mol)

Table 2: Experimental Calculated magnetization of TMFe2O4

Image 4: X ray parameters for the material X= Mn

Image 5: X ray parameters for the material X= Zn

Image 9: S.E.M. photography of

Image 10: S.E.M. photography of

Image 13 shows the tendency

Image 13: Ms, Hc vs metal ion of samples synthetized at

Image 16: EDS spectrum CuFe2O4 spinel

Unn (wt.%) Norm (wt.%)

Atom (at.%) Comp.C (wt.%)

Table 6: EDS quantitative analysis for CoFe2O4 spinel.

Image 17: EDS spectrum CoFe2O4 spinel

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