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Materials Letters
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / m a t l e t
One-step pyrolysis route to C/Fe3O4 hybrids from EDTA ferric sodium salt
Jingchun Zhang a, Wenqing Shen b, Zongwen Zhang b, Dengyu Pan b,⁎, Minghong Wu a,⁎
a
Shanghai Applied Radiation Institute, Shanghai University, Shanghai 200444, PR China
b
Institute of Nanochemistry and Nanobiology, Shanghai University, Shanghai 200444, PR China
a r t i c l e i n f o a b s t r a c t
Article history: C/Fe3O4 hybrid materials have potential applications in sensors and anode materials for lithium-ion batteries.
Received 10 December 2009 In this text, a one-step pyrolysis method was used to prepare C/Fe3O4 hybrid materials from EDTA ferric
Accepted 8 January 2010 sodium salt. The magnetic Fe3O4 nanoparticles can be homogeneously incorporated into carbon materials to
Available online 15 January 2010
form C/Fe3O4 hybrids during the reaction. The morphology and magnetism of the C/Fe3O4 hybrids are strongly
affected by pyrolysis temperature. This method supplies an ideal template to facilely synthesize C/metal-oxide
Keywords:
hybrid materials from EDTA metallic salts.
One-step pyrolysis
EDTA ferric sodium salt
© 2010 Elsevier B.V. All rights reserved.
C/Fe3O4 hybrids
Magnetism
0167-577X/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.matlet.2010.01.023
818 J. Zhang et al. / Materials Letters 64 (2010) 817–819
Scheme 1. Scheme of the preparation process of C/Fe3O4 hybrids. Left: the C/Fe3O4 hybrids dissolved in distilled water. Right: the C/Fe3O4 hybrids dissolved in distilled water under a
magnetic field.
Fig. 1. XRD patterns of C/Fe3O4 hybrids prepared at 300 °C (a) and 400 °C (b).
Scherrer formula [20], the average diameters of Fe3O4 nanocrystals Carbon plays a key role in the formation of C/Fe3O4 hybrids: 1) reduce
increased from 9.1 nm (300 °C) to 14.9 nm (400 °C). Furthermore, the part of Fe3+ to Fe2+ under N2 atmosphere. 2) encapsulate Fe3O4
diffraction peak at 26° indicated the existence of carbon and the nanoparticles in carbon materials simultaneously.
content of carbon decreased as the temperature increased.
The FT-IR spectra of C/Fe3O4 hybrids prepared at 300 °C and 400 °C
are presented in Fig. 2. The strong peaks at about 565 cm−1 are 4. Conclusion
assigned to the vibration of the Fe–O bond of Fe3O4 [13]. The broad
bonds at about 3400 cm−1 are related to the absorbed H2O molecules In summary, we develop a facile and large-scale way to synthesize
on the surface of C/Fe3O4 hybrids. Furthermore, the absorbing peaks at C/Fe3O4 hybrid materials by pyrolysis of EDTA ferric sodium salt. The
about 1633 cm−1 (1616 cm−1) and 1453 cm−1 (1439 cm−1) are formation mechanism of carbon coated Fe3O4 hybrids is also discussed.
assigned to the asymmetric and symmetric stretching vibration of C O The size and ratio of Fe3O4 nanoparticles in C/Fe3O4 hybrids are
(COO−) on the surface of the sample prepared at 300 °C (400 °C). strongly affected by pyrolysis temperature. The saturation magneti-
TEM images of C/Fe3O4 hybrids are shown in Fig. 3 to illuminate zation (Ms) and coercive field (Hc) of the C/Fe3O4 hybrids are also
the morphology of the as-prepared products. As shown in Fig. 3 (a), tuned. This work provides a new insight for the synthesis of C/Fe3O4
most of the Fe3O4 nanoparticles were unattached and encapsulated in hybrids. More importantly, such C/Fe3O4 hybrids show potential
carbon. The statistical average particle size of the product prepared at applications in sensors and anode materials for lithium-ion batteries.
300 °C is about 9.6 nm, which is consistent with that obtained by Additionally, such method supplies an ideal template to facilely
Debye-Scherrer formula. The morphology of the C/Fe3O4 hybrid is synthesize C/metal-oxide hybrid materials such as C/SnO2 for different
strongly affected by the reaction temperature as shown in Fig. 3 (b). applications.
The particle size of Fe3O4 prepared at 400 °C seems inconsistent with
that obtained by Debye-Scherrer formula. Indeed, due to the lower
content of carbon and stronger magnetism (Fig. 4) than that of the
product prepared at 300 °C, the Fe3O4 nanoparticles easily aggregate
into larger ones.
Fig. 4 shows the magnetization hysteresis loops of the C/Fe3O4
hybrids. It can be seen that both of the products prepared at 300 °C and
400 °C are ferromagnetic at room temperature. The saturation
magnetization (Ms) values of the C/Fe3O4 hybrids increased from
12.5 emu/g (300 °C) to 29.5 emu/g (400 °C), which is mainly affected
by particle size, crystallinity and ratio of Fe3O4 nanoparticles in C/Fe3O4
hybrids. Moreover, the coercive field (Hc) ascends from 40 Oe to
360 Oe with the increased size of Fe3O4 nanoparticles.
The formation mechanism of carbon coated Fe3O4 hybrids is
discussed. During the pyrolysis, the part of Fe3+ in the molecular
precursor was broken up. The carbonaceous part of EDTA ferric sodium
salt was carbonized under high temperature and N2 atmosphere. Fig. 2. FT-IR spectra of C/Fe3O4 hybrids prepared at 300 °C and 400 °C.
J. Zhang et al. / Materials Letters 64 (2010) 817–819 819
Fig. 3. TEM images of C/Fe3O4 hybrids prepared at 300 °C (a) and 400 °C (b).
Fig. 4. M–H curves of the C/Fe3O4 hybrids prepared at 300 °C (a) and 400 °C (b).
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