Abstract:
The present invention relates to a method of producing iron oxide nanoparticles iron oxide nanoparticles produced by the method and an anode material including same.
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Notices, Deadlines & Correspondence
128, Yeoui- daero,
Yeongdeungpo- gu,
Seoul 150- 721
Inventors
1. LEE, Myung Ki
LG Chem Research Park, 188, Munji-ro, Yuseong-gu,
Daejeon 305-738,
2. PARK, Sung Bin
LG Chem Research Park, 188, Munji-ro, Yuseong-gu,
Daejeon 305-738,
3. KANG, Sung Joong
LG Chem Research Park, 188, Munji-ro, Yuseong-gu,
Daejeon 305-738,
4. JUNG, Wang Mo
LG Chem Research Park, 188, Munji-ro, Yuseong-gu,
Daejeon 305-738,
Specification
BACKGROUND OF THE INVENTION
Field of the Invention
[0001] The present invention relates to a method of preparing iron oxide
nanoparticles, and more particularly, to a method of preparing iron oxide nanoparticles,
iron oxide nanoparticles prepared thereby, and an anode material including the iron
oxide nanoparticles.
Description of the Related Art
[0002] Recently, as issues, such as the depletion of fossil fuels and environmental
destruction, have emerged, many researchers have devoted to develop alternative
energies that may replace fossil fuels. As a kind of such alternative energies, a
significant amount of research into secondary batteries that are applicable to various
fields has been conducted.
[0003] The application fields of secondary batteries have been further expanded to
batteries for vehicles and batteries for power storage as well as typical portable systems.
[0004] A secondary battery may be composed of a cathode, an anode, an electrolyte
solution, and a separator, and among these, components that mostly affect the battery
may be the cathode and the anode in which electrochemical reactions actually occur.
[0005] A graphite material has mainly been used as the anode due to its
competitiveness in terms of stability, lifetime, and price. However, as high-capacity
batteries, which may be used in electric vehicles and batteries for power storage, have
been increasingly required, research into developing a new anode material having high
theoretical capacity has emerged.
[0006] In line with such requirements, metal oxides have recently received attention
as a high-capacity anode active material, and particularly, iron (III) oxide (Fe2O3)
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among these oxides has received attention as an anode material due to its high
theoretical capacity (1007 mAh/g).
[0007] However, since capacity and cycle efficiency may decrease during a
charge/discharge process when a particle diameter of the metal oxide is large (>1 μm),
research into preparing nanometer-sized iron oxide particles by various chemical
syntheses has continued.
[0008] As a synthesis method of the iron oxide nanoparticles, a method has been
known, in which a ferrous hydroxide (Fe(OH)2) aqueous solution, which is prepared by
adding sodium hydroxide to a ferric salt aqueous solution, is irradiated with ultrasonic
waves.
[0009] However, with respect to a typical synthesis method of iron oxide, difficult
synthesis conditions (inert atmosphere) must be maintained and an expensive high
purity raw material must be used. In addition, since the particles obtained by the
irradiation of ultrasonic waves may not be uniform and may have poor crystallinity, the
application range thereof may be narrow. Also, since it takes a long time to irradiate
with ultrasonic waves, mass production may be impossible.
[0010] Furthermore, since iron (III) oxide nanoparticles prepared by a typical
method may be difficult to be prepared as nanoparticles having a fine and uniform
particle size, cracks may occur in an electrode due to volume expansion and shrinkage
of the electrode during a charge/discharge process. Thus, capacity loss is high and
cycle efficiency rapidly decreases.
[0011] Therefore, development of a method of preparing iron oxide nanoparticles is
urgent, in which limitations of a typical preparation method of iron oxide nanoparticles,
such as complex process and long preparation time, may be addressed, particle diameter
and shape of powder may be uniformly controlled, and simultaneously, capacity loss
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may be low even during numerous charge/discharge processes.
SUMMARY OF THE INVENTION
[0012] An aspect of the present invention provides a method of preparing iron oxide
nanoparticles, in which mass production may be possible by a simple process condition
and capacity loss may be low even during numerous charge/discharge processes.
[0013] Another aspect of the present invention provides iron oxide nanoparticles
prepared by the above method and an anode material including the iron oxide
nanoparticles.
[0014] Another aspect of the present invention provides an anode for an
electrochemical device that is formed of the above anode material and an
electrochemical device including the anode.
[0015] According to an aspect of the present invention, there is provided a method
of preparing iron (III) oxide nanoparticles including: preparing a ferric chloride (FeCl3)
aqueous solution; preparing a sodium hydroxide (NaOH) aqueous solution; mixing both
aqueous solutions; adding a sodium sulfate (Na2SO4) aqueous solution while stirring a
mixed aqueous solution prepared by the mixing; and reacting the mixed aqueous
solution having the sodium sulfate aqueous solution added thereto in an electric
convection oven.
[0016] According to a method of the present invention, iron oxide nanoparticles
may be prepared in which particle diameter and particle distribution of the powder may
be controlled by a simple preparation process and capacity loss may be low even during
numerous charge/discharge processes. Also, an anode having excellent capacity and
stability, and an electrochemical device including the anode may be prepared by using
the iron oxide nanoparticles.
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BRIEF DESCRIPTION OF THE DRAWINGS
[0017] FIG. 1 is a scanning electron microscope (SEM) image of iron oxide
nanoparticles prepared by a method of the present invention;
[0018] FIG. 2 is a scanning electron microscope (SEM) image of iron oxide
nanoparticles prepared by a method of the present invention; and
[0019] FIG. 3 is a graph comparing the results of the measurement of capacities of
secondary batteries prepared in Example 1 and Comparative Example 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0020] Hereinafter, the present invention will be described in detail.
[0021] The present invention provides a method of preparing iron (III) oxide
nanoparticles including: preparing a ferric chloride (FeCl3) aqueous solution; preparing
a sodium hydroxide (NaOH) aqueous solution; mixing both aqueous solutions; adding a
sodium sulfate (Na2SO4) aqueous solution while stirring a mixed aqueous solution
prepared by the mixing; and reacting the mixed aqueous solution having the sodium
sulfate aqueous solution added thereto in an electric convection oven.
[0022] Specifically, in the method of the present invention, a concentration of the
FeCl3 aqueous solution may be in a range of 2 M to 3 M and a concentration of the
NaOH aqueous solution may be in a range of 5 M to 6 M. Also, a concentration of the
Na2SO4 aqueous solution may be in a range of 0.5 M to 1 M, and for example, may be
0.6 M.
[0023] In this case, when the concentration of the FeCl3 aqueous solution is 2 M or
less or 3 M or more, metal oxide having a particle diameter of 1 μm or more may be
synthesized. Also, when the concentration of the NaOH aqueous solution is 6 M or
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more, a pH level of the synthesized aqueous solution may be increased and thus, metal
oxide may not be synthesized. Furthermore, when the concentration of the Na2SO4
aqueous solution is 1 M or more, metal oxide having a uniform shape may not be
prepared. In this case, a sodium phosphate (Na2PO4) aqueous solution may be used
instead of the Na2SO4 aqueous solution.
[0024] In the method of the present invention, the ferric chloride aqueous solution,
the sodium hydroxide aqueous solution, and the sodium sulfate aqueous solution may be
mixed in a volume ratio of 10:9:x (where x satisfies 0