U.S. patent application number 14/897012 was filed with the patent office on 2016-05-12 for device for preparing core-shell particles and method for preparing core-shell particles by using same.
The applicant listed for this patent is LAMINAR CO., LTD., POSCO, RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY. Invention is credited to Gyeong Rye CHOI, Jong Pal HONG, Geun HWANGBO, Jung Hoon SONG.
Application Number | 20160133924 14/897012 |
Document ID | / |
Family ID | 51748988 |
Filed Date | 2016-05-12 |
United States Patent
Application |
20160133924 |
Kind Code |
A1 |
HONG; Jong Pal ; et
al. |
May 12, 2016 |
DEVICE FOR PREPARING CORE-SHELL PARTICLES AND METHOD FOR PREPARING
CORE-SHELL PARTICLES BY USING SAME
Abstract
A method of manufacturing core-shell particles comprises:
filling a buffer into a rotor, which is extended in a longitudinal
direction, and is accommodated so as to be spaced apart from an
inner wall side of an irrotational hollow cylinder extended in a
longitudinal direction and then discharging air to outside;
rotating the rotor after terminating the filling; forming a
core-shell precursor by supplying raw materials from a first
storage and a second storage, which comprise a material forming a
core, into an interior of the cylinder in which the rotor rotates;
supplying a shell material for coating the core to the interior of
the cylinder in which a core-type precursor is formed; separating a
liquid comprising core-shell particles formed through the supplying
into a solid and a liquid; and drying the core-shell particles
obtained through the separating. An apparatus for manufacturing the
core-shell particles is provided.
Inventors: |
HONG; Jong Pal;
(Seongnam-si, KR) ; SONG; Jung Hoon; (Seoul,
KR) ; HWANGBO; Geun; (Incheon, KR) ; CHOI;
Gyeong Rye; (Seongnam-si, KR) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
LAMINAR CO., LTD.
POSCO
RESEARCH INSTITUTE OF INDUSTRIAL SCIENCE & TECHNOLOGY |
Gyeonggi-do
Gyeongsangbuk-do
Gyeongsangbuk-do |
|
KR
KR
KR |
|
|
Family ID: |
51748988 |
Appl. No.: |
14/897012 |
Filed: |
June 13, 2014 |
PCT Filed: |
June 13, 2014 |
PCT NO: |
PCT/KR2014/005201 |
371 Date: |
December 9, 2015 |
Current U.S.
Class: |
427/123 ; 118/58;
427/58 |
Current CPC
Class: |
B01J 19/28 20130101;
H01M 4/5825 20130101; C01G 3/006 20130101; Y02E 60/10 20130101;
B01J 2219/00894 20130101; H01M 4/525 20130101; B01J 8/10 20130101;
H01M 2220/30 20130101; B01J 19/1806 20130101; B01J 8/085 20130101;
B01J 2219/00094 20130101; H01M 4/485 20130101; H01M 4/602 20130101;
B01J 2208/00584 20130101; B05C 3/08 20130101; H01M 4/38 20130101;
B01J 2219/00905 20130101; C01P 2004/84 20130101; B01J 8/087
20130101; B01J 2219/1943 20130101; B01J 2219/00889 20130101; B01J
19/18 20130101; B01J 2208/00212 20130101; B01J 2219/00189 20130101;
H01M 4/366 20130101 |
International
Class: |
H01M 4/36 20060101
H01M004/36; H01M 4/38 20060101 H01M004/38; H01M 4/60 20060101
H01M004/60; B05C 3/08 20060101 B05C003/08; H01M 4/58 20060101
H01M004/58 |
Foreign Application Data
Date |
Code |
Application Number |
Jun 14, 2013 |
KR |
10-2013-0068434 |
Claims
1. An apparatus for manufacturing core-shell particles, the
apparatus comprising: a reactor comprising an irrotational hollow
cylinder extended in a longitudinal direction, a rotor accommodated
so as to be spaced apart from an inner wall side of the cylinder
and extended in a longitudinal direction, a driving part connected
to one end of the rotor and rotating the rotor, a first raw
material inlet and a second raw material inlet respectively formed
so as to be connected to the interior of the cylinder at an
external circumferential side of one end of the cylinder with
respect to a longitudinal direction of the cylinder, an outlet
formed at another end of the cylinder so as to be connected to the
interior of the cylinder in an opposite direction from the first
raw material inlet and the second raw material inlet, at least one
shell material inlet formed at an external circumferential side of
the cylinder and supplying a shell material to the interior of the
cylinder, a heat exchange material moving path formed between an
external circumferential side and an interior circumference of the
cylinder and providing a moving path of a heat exchange material, a
heat exchange material inlet connected to the heat exchange
material moving path and serving to inject a heat exchange
material, and a heat exchange material outlet connected to the heat
exchange material moving path and discharging a heat exchange
material; a first storage connected to the first raw material inlet
of the reactor; a second storage connected to the second raw
material inlet of the reactor; a solid-liquid separator connected
to the outlet of the reactor and separating a product discharged
from the outlet into solid particles and a liquid; and a drier
connected to the solid-liquid separator and drying solid particles
separated by the solid-liquid separator.
2. The apparatus according to claim 1, further comprising a
circulation pump for circulating the heat exchange material,
connected between the heat exchange material inlet and the heat
exchange material outlet.
3. The apparatus according to claim 1, wherein a first pump and a
second pump are respectively connected between the first storage
and the first raw material inlet and between the second storage and
the second raw material inlet.
4. The apparatus according to claim 1, wherein the driving part is
a variable speed stirrer motor for controlling a rotation speed to
1 rpm or more.
5. A method of manufacturing core-shell particles, the method
comprising: filling a buffer into a rotor, which is extended in a
longitudinal direction, and is accommodated so as to be spaced
apart from an inner wall side of an irrotational hollow cylinder
extended in a longitudinal direction and then discharging air to
outside; rotating the rotor after terminating the filling; forming
a core-shell precursor by supplying raw materials from a first
storage and a second storage, which comprise a material forming a
core, into an interior of the cylinder in which the rotor rotates;
supplying a shell material for coating the core to the interior of
the cylinder in which a core-type precursor is formed; separating a
liquid comprising core-shell particles formed through the supplying
into a solid and a liquid; and drying the core-shell particles
obtained through the separating.
6. The method according to claim 5, wherein as the liquid
comprising the core-shell particles separated at the separating, a
reactant in a normal state within the reactor is used.
7. The method according to claim 5, wherein lithium chloride and
sodium carbonate; or lithium hydroxide and carbon dioxide; or
aluminum carbonate and copper sulfate, as a pair of raw materials,
are respectively stored in the first storage and the second
storage.
8. The method according to claim 5, wherein the shell material is
an inorganic metal comprising copper, cobalt, or manganese; or is a
polymer or an oligomer selected from the group consisting of
polyethylene glycol, polyethylene oxide, polyethylene glycol methyl
ether, polyethylene glycol dimethyl ether, polypropylene oxide,
polyethylene, polypropylene, polyisobutylene, and polyvinylidene
chloride.
Description
BACKGROUND OF THE INVENTION
[0001] (a) Field of the Invention
[0002] The present invention relates to an apparatus for
manufacturing core-shell particles, particularly core-shell
particles used in a positive electrode active material of lithium
rechargeable batteries, in order to form a shell on a core by
injecting a gas, liquid, and/or solid material in the presence of a
liquid-type solvent, and a method of manufacturing the core-shell
particles using the same.
[0003] (b) Description of the Related Art
[0004] As mobile device technology continues to develop and demand
therefor continues to increase, demand for rechargeable batteries
as energy sources is rapidly increasing. Among these rechargeable
batteries, lithium rechargeable batteries, which exhibit high
energy density and operating electrical potential, and have long
cycle lifespan and a low self-discharge rate, are commercially
available and widely used.
[0005] As positive electrode active materials of such lithium
rechargeable batteries, lithium-containing cobalt oxides such as
LiCoO.sub.2 are mainly used. In addition thereto, use of
LiMnO.sub.2 with a layered crystal structure, lithium-containing
manganese oxides such as LiMn.sub.2O.sub.4 with a spinel crystal
structure, lithium-containing nickel oxides such as LiNiO.sub.2, or
ternary LiNixMnyCO(1-x-y)O.sub.2 is also under consideration.
[0006] In general, positive electrode active materials of lithium
rechargeable batteries are prepared through solid-state reaction at
a high temperature of 700.degree. C. or more.
[0007] However, when positive electrode active materials are
prepared through solid-state reaction, the positive electrode
active materials are subjected to physical mixing and grinding,
thus resulting in a non-uniform mixed state. Accordingly, the
mixing and grinding should be repeated several times, whereby time
taken for manufacturing the same is greatly increased and
preparation costs increase.
[0008] Accordingly, a sol-gel method including hydrolysis and
condensation and a wet process including a co-precipitation method
as representative examples were developed.
[0009] Thereamong, through the co-precipitation method, a chloride,
a nitride, a sulfide, or the like containing a raw material is
precipitated with a hydroxide in an alkaline co-precipitation
solution and then calcined to prepare an oxide powder. When
positive electrode active materials are prepared through
co-precipitation, the pH, temperature, and stirring conditions of a
co-precipitation solution should be controlled.
[0010] In an existing co-precipitation method, positive electrode
active materials are prepared using a continuous stirred-tank
reactor (CSTR). However, when positive electrode active materials
are prepared using the CSTR reactor, it is not easy to increase
reaction scale, a force generating a vortex varies depending upon a
distance from the inner turbine of the reactor, used devices are
expensive, an energy dissipation rate is high, and it is difficult
to apply the method to a continuous process.
[0011] In order to address the problems of a CSTR reactor, a
reaction device using a Taylor vortex was considered (Korean Patent
Application Pub. No. 2010-0112843). However, the device can be used
in general mixing, extraction, chemical reaction, etc., but cannot
be used in manufacturing positive electrode active materials.
[0012] In addition, in the case of general positive electrode
active materials, a precursor is prepared and then an external
circumferential side of a core composed of an active material is
coated through a separate process to form a shell.
[0013] The above information disclosed in this Background section
is only for enhancement of understanding of the background of the
invention and therefore it may contain information that does not
form the prior art that is already known in this country to a
person of ordinary skill in the art.
SUMMARY OF THE INVENTION
[0014] The present invention has been made to address the problems
described above and provides an apparatus for manufacturing
core-shell particles, particularly core-shell particles used in a
positive electrode active material of lithium rechargeable
batteries, in order to form a shell on a core by injecting a gas,
liquid, and/or solid material in the presence of a liquid-type
solvent.
[0015] In accordance with an aspect of the present invention, the
above and other objects can be accomplished by the provision of an
apparatus for manufacturing core-shell particles including: a
reactor including an irrotational hollow cylinder extended in a
longitudinal direction, a rotor accommodated so as to be spaced
apart from an inner wall side of the cylinder and extended in a
longitudinal direction, a driving part connected to one end of the
rotor and rotating the rotor, a first raw material inlet and a
second raw material inlet respectively formed so as to be connected
to the interior of the cylinder at an external circumferential side
of one end of the cylinder with respect to a longitudinal direction
of the cylinder, an outlet formed at another end of the cylinder so
as to be connected to the interior of the cylinder in an opposite
direction from the first raw material inlet and the second raw
material inlet, at least one shell material inlet formed at an
external circumferential side of the cylinder and supplying a shell
material to the interior of the cylinder, a heat exchange material
moving path formed between an external circumferential side and an
interior circumference of the cylinder and providing a moving path
of a heat exchange material, a heat exchange material inlet
connected to the heat exchange material moving path and serving to
inject a heat exchange material, and a heat exchange material
outlet connected to the heat exchange material moving path and
discharging a heat exchange material;
[0016] a first storage connected to the first raw material inlet of
the reactor;
[0017] a second storage connected to the second raw material inlet
of the reactor;
[0018] a solid-liquid separator connected to the outlet of the
reactor and separating a product discharged from the outlet into
solid particles and a liquid; and
[0019] a drier connected to the solid-liquid separator and drying
solid particles separated by the solid-liquid separator.
[0020] In accordance with another aspect of the present invention,
a method of manufacturing core-shell particles is provided,
including: filling a buffer into a rotor, which is extended in a
longitudinal direction, and is accommodated so as to be spaced
apart from an inner wall side of an irrotational hollow cylinder
extended in a longitudinal direction and then discharging air to
the outside;
[0021] rotating the rotor after terminating the filling;
[0022] forming a core-shell precursor by supplying raw materials
from a first storage and a second storage, which include a material
forming a core, into an interior of the cylinder in which the rotor
rotates;
[0023] supplying a shell material for coating the core to the
interior of the cylinder in which a core-type precursor is
formed;
[0024] separating a liquid including core-shell particles formed
through the supplying into a solid and a liquid; and
[0025] drying the core-shell particles obtained through the
separating.
[0026] In accordance with yet another aspect of the present
invention, an apparatus for manufacturing core-shell particles,
particularly core-shell particles used in a positive electrode
active material of lithium rechargeable batteries, is provided, in
order to form a shell on a core by injecting a gas, liquid, and/or
solid material in the presence of a liquid-type solvent.
[0027] In particular, according to the present invention, the
core-shell particles may be prepared by manufacturing a positive
electrode active material precursor as a core type and then coating
the same in one reactor without a separate coating process.
BRIEF DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 is a view illustrating an overall configuration of an
apparatus for manufacturing core-shell particles according to the
present invention.
[0029] FIG. 2 is a cross-sectional view illustrating a reactor
included in an apparatus for manufacturing core-shell particles
according to the present invention.
DESCRIPTION OF SYMBOLS
TABLE-US-00001 [0030] 10: FIRST STORAGE 20: SECOND STORAGE 30:
FIRST PUMP 40: SECOND PUMP 50: DRIVING PART 60: REACTOR 61: FIRST
RAW MATERIAL INLET 62: SECOND RAW MATERIAL INLET 63: OUTLET 64:
SHELL MATERIAL INLET 65: HEAT EXCHANGE MATERIAL INLET 66: HEAT
EXCHANGE MATERIAL OUTLET 67: HEAT EXCHANGE MATERIAL MOVING PATH 68:
CYLINDER 69: ROTOR 70: SHELL MATERIAL STORAGE 80: CIRCULATION PUMP
90: SOLID-LIQUID SEPARATION PART 92: DRYER 100: PRECURSOR FORMATION
PART 110: CORE-SHELL FORMATION PART
DETAILED DESCRIPTION
[0031] Hereinafter, the present invention is described in more
detail
[0032] In an embodiment, the present invention provides an
apparatus for manufacturing core-shell particles, including: a
reactor including an irrotational hollow cylinder extended in a
longitudinal direction, a rotor accommodated so as to be spaced
apart from an inner wall side of the cylinder and extended in a
longitudinal direction, a driving part connected to one end of the
rotor and rotating the rotor, a first raw material inlet and a
second raw material inlet respectively formed so as to be connected
to the interior of the cylinder at an external circumferential side
of one end of the cylinder with respect to a longitudinal direction
of the cylinder, an outlet formed at another end of the cylinder so
as to be connected to the interior of the cylinder in an opposite
direction from the first raw material inlet and the second raw
material inlet, at least one shell material inlet formed at an
external circumferential side of the cylinder and supplying a shell
material to the interior of the cylinder, a heat exchange material
moving path formed between an external circumferential side and an
interior circumference of the cylinder and providing a moving path
of a heat exchange material, a heat exchange material inlet
connected to the heat exchange material moving path and serving to
inject a heat exchange material, and a heat exchange material
outlet connected to the heat exchange material moving path and
discharging a heat exchange material; a first storage connected to
the first raw material inlet of the reactor; a second storage
connected to the second raw material inlet of the reactor; a
solid-liquid separator connected to the outlet of the reactor and
separating a product discharged from the outlet into solid
particles and a liquid; and a drier connected to the solid-liquid
separator and drying solid particles separated by the solid-liquid
separator.
[0033] In another embodiment, the present invention provides a
method of manufacturing core-shell particles including filling a
buffer into a rotor, which is extended in a longitudinal direction,
and is accommodated so as to be spaced apart from an inner wall
side of an irrotational hollow cylinder extended in a longitudinal
direction and then discharging air to the outside, rotating the
rotor after terminating the filling, forming a core-shell precursor
by supplying raw materials from a first storage and a second
storage, which include a material forming a core, into an interior
of the cylinder in which the rotor rotates, supplying a shell
material for coating the core to the interior of the cylinder in
which a core-type precursor is formed, separating a liquid
including core-shell particles formed through the supplying into a
solid and a liquid, and drying the core-shell particles obtained
through the separating.
[0034] Hereinafter, the present invention is described in detail
with reference to the accompanying drawings. However, it should be
understand that the following descriptions are merely to concretely
explain the spirit of the invention, and therefore there is no
intent to limit the invention to the descriptions.
[0035] FIG. 1 is a view illustrating an overall configuration of an
apparatus for manufacturing core-shell particles according to the
present invention, and FIG. 2 is a cross-sectional view
illustrating a reactor included in an apparatus for manufacturing
core-shell particles according to the present invention.
Hereinafter, the present invention is described with reference to
FIGS. 1 and 2.
[0036] As shown in FIGS. 1 and 2, the apparatus for manufacturing
core-shell particles according to the present invention includes: a
reactor 60 including an irrotational hollow cylinder 68 extended in
a longitudinal direction, a rotor 69 accommodated so as to be
spaced apart from an inner wall side of the cylinder 68 and
extended in a longitudinal direction, a driving part 50 connected
to one end of the rotor 69 and rotating the rotor 69, a first raw
material inlet 61 and a second raw material inlet 62 respectively
formed so as to be connected to the interior of the cylinder 68 at
an external circumferential side of one end of the cylinder 68 with
respect to a longitudinal direction of the cylinder 68, an outlet
63 formed at another end of the cylinder 68 so as to be connected
to the interior of the cylinder 68 in an opposite direction from
the first raw material inlet 61 and the second raw material inlet
62, at least one shell material inlet 64 formed at an external
circumferential side of the cylinder 68 and supplying a shell
material to the interior of the cylinder 68, a heat exchange
material moving path 67 formed between an external circumferential
side and an interior circumference of the cylinder 68 and providing
a moving path of a heat exchange material, a heat exchange material
inlet 65 connected to the heat exchange material moving path 67 and
serving to inject a heat exchange material, and a heat exchange
material outlet 66 connected to the heat exchange material moving
path 67 and discharging a heat exchange material; a first storage
10 connected to the first raw material inlet 61 of the reactor 60;
a second storage 20 connected to the second raw material inlet 62
of the reactor 60; a solid-liquid separator 90 connected to the
outlet 63 of the reactor 60 and separating a product discharged
from the outlet 63 into solid particles and a liquid; and a drier
92 connected to the solid-liquid separator 90 and drying solid
particles separated by the solid-liquid separator 90.
[0037] The reactor 60 forms a Taylor vortex and basically includes
the cylinder 68 and the rotor 69, which have the same central axis
and are extended in a longitudinal direction, the raw material
inlets 61 and 62, the outlet 63, and the driving part 50
accommodated in the cylinder 68 and determining rotation of the
rotor 69.
[0038] Here, each of materials to be reacted are input between the
cylinder 68 and the rotor 69 via the first raw material inlet 61
and the second raw material inlet 62. The rotor 69 is rotated by
operating the driving part 50, thereby generating a rotational
flow.
[0039] In this case, as the driving part, a variable speed stirrer
motor able to control a rotation speed to 1 rpm or more is
recommended.
[0040] Meanwhile, when an angular speed of the rotor 69 is low,
laminar Couette flow occurs. On the other hand, as the angular
speed is increased, fluids tend to move in an outer direction of
the cylinder. Accordingly, the fluid becomes unstable and a Taylor
vortex occurs at a specific threshold speed or more.
[0041] A Taylor vortex is arranged in a very regular ring shape in
an axis direction and rotates in opposite directions. Accordingly,
mixing does not occur in an axis direction, and thus uniform mixing
is induced to mix raw materials. Accordingly, a core as a precursor
for manufacturing core-shell particles may be generated.
[0042] In this case, when a shell material is injected into the
interior of the cylinder 68 via one side of the reactor 60,
particularly the at least one shell material inlet 64 formed at the
cylinder 68 of the reactor 60, an external circumferential side of
the core is coated to form core-shell-type double particles.
[0043] Here, the reactor 60 includes a precursor formation part
100, in which a precursor is formed, located at the first raw
material inlet 61 and second raw material inlet 62 to which a raw
material, preferably a raw material used to prepare positive
electrode active materials of lithium rechargeable batteries, is
injected, with respect to a longitudinal direction of the reactor
60. A core-shell formation part 110 is present from a rear part of
the precursor formation part 100 to a part to which a shell
material is injected.
[0044] Meanwhile, the raw material forming a core as a precursor
according to the present invention is not specifically limited so
long as it is one generally used in the art.
[0045] In particular, the raw material may form a precursor as a
core through injection of a gas, liquid, and/or solid material in
the presence of a liquid-type solvent.
[0046] As an embodiment, a core composed of lithium carbonate may
be formed through liquid-liquid reaction using lithium chloride and
sodium carbonate as in Formula 1.
LiCl+Na.sub.2CO.sub.3(l).fwdarw.Li.sub.2CO.sub.3 [Formula 1]
[0047] As another embodiment, a core composed of lithium carbonate
may be formed through gas-liquid reaction using lithium hydroxide
and carbon dioxide as in Formula 2.
2LiOH+3CO.sub.2(g).fwdarw.Li.sub.2CO.sub.3 [Formula 2]
[0048] As another embodiment, a core composed of copper aluminum
carbonate may be formed through solid-liquid reaction using
aluminum carbonate and copper sulfate as in Formula 3.
Al.sub.2CO.sub.3(S)+CuSO.sub.4.fwdarw.Cu--Al.sub.2CO.sub.3 [Formula
3]
[0049] Here, lithium chloride and sodium carbonate; lithium
hydroxide and carbon dioxide; or aluminum carbonate and copper
sulfate, as a pair of raw materials, may be respectively stored in
the first storage 10 and the second storage 20 connected to the
first raw material inlet 61 and the second raw material inlet
62.
[0050] Meanwhile, a shell material used to prepare core-shell
particles through coating of the core is not specifically limited
so long as the material may coat the core. Particularly, the
material may be a polymer, a metal, a metal oxide, etc., more
particularly an inorganic metal including copper, cobalt, or
manganese, or a polymer or an oligomer selected from the group
consisting of polyethylene glycol, polyethylene oxide, polyethylene
glycol methyl ether, polyethylene glycol dimethyl ether,
polypropylene oxide, polyethylene, polypropylene, polyisobutylene,
and polyvinylidene chloride.
[0051] In addition, the shell material may be stored in a separate
storage unit, e.g., a shell material storage 70, and then,
according to selection of a user, supplied to the reactor 60 by
connecting the shell material storage 70 to the at least one shell
material inlet 64.
[0052] The at least one shell material inlet 64 is provided at the
reactor 60 such that a shell is formed on a core. The location and
the number of the at least one shell material inlet 64 are
determined according to users' selection, and preferably, the at
least one shell material inlet 64 is formed between the raw
material inlets 61 and 62 and the outlet 63 provided at the
cylinder 68 of the reactor 60 extended in a longitudinal
direction.
[0053] The reactor 60 according to the present invention may
control core-shell particle formation reaction through temperature
control.
[0054] In this case, the reactor 60 includes the heat exchange
material moving path 67, in which a heat exchange material moves to
heat and cool the reactor 60, between an external circumferential
side and an interior circumference of the cylinder 68. The heat
exchange material moving path 67 may include the heat exchange
material inlet 65 and the heat exchange material outlet 66 for
injecting or discharging the heat exchange material.
[0055] Here, the heat exchange material may be a material, e.g., a
coolant, generally used in the art.
[0056] As a specific embodiment, the heat exchange material moving
path 67 according to the present invention may be formed in plural
or in a radial structure between an interior circumference side and
an external circumferential side of the cylinder 68 so as to more
rapidly control the temperature of the reactor 60.
[0057] As another specific embodiment, the apparatus for
manufacturing core-shell particles according to the present
invention may further include a circulation pump 80 for circulating
a heat exchange material connected between the heat exchange
material inlet 65 and the heat exchange material outlet 66 to
continuously circulate the heat exchange material.
[0058] Meanwhile, a first pump 30 is connected between the first
storage 10 including the raw material according to the present
invention and the first raw material inlet 61, which supplies the
raw material, connected to the first storage 10, and a second pump
40 is connected between the second storage 20 including the other
raw material and the second raw material inlet 62, which supplies
the other raw material, connected to the second storage 20, to
quantitatively control the amount of the raw material supplied.
[0059] In this case, the first pump 30 and the second pump 40 are
not specifically limited, but particularly, a metering pump may be
used.
[0060] The solid-liquid separator 90 according to the present
invention is connected to the outlet 63 of the reactor 60 and
separates a product discharged from the outlet 63, e.g., a liquid
including core-shell particles, into a solid and a liquid. As the
solid-liquid separator 90, any general solid-liquid separation
apparatuses used in the art performing such function may be used,
and particularly, a centrifuge or a dehydrator may be used.
[0061] The drier 92 according to the present invention is connected
to the solid-liquid separator 90 and dries solid particles,
particularly core-shell particles, separated from the solid-liquid
separator 90.
[0062] In the drier 92, drying is performed using a method
generally used in the art.
[0063] As a specific embodiment, the apparatus for manufacturing
core-shell particles according to the present invention may further
include a scanning electron microscope which is connected to a rear
part of the drier 92, to analyze uniformity of the shape and size
of dried core-shell particles, preferably positive electrode active
material particles composed of core-shell particles.
[0064] As another specific embodiment, the apparatus for
manufacturing core-shell particles according to the present
invention may further include a densitometer for measuring the
density of a positive electrode active material composed of
core-shell particles at a rear part of the scanning electron
microscope.
[0065] Hereinafter, a method of manufacturing core-shell particles
is described using the apparatus for manufacturing core-shell
particles having such a configuration according to the present
invention.
[0066] First, the method includes: a buffer solution filling step
of filling a buffer into the rotor 69, which is extended in a
longitudinal direction, and is accommodated so as to be spaced
apart from an inner wall side of the cylinder 68 included in the
irrotational hollow reactor 60 extended in a longitudinal direction
and then discharging air to the outside; a rotor rotation step of
rotating the rotor 69 after terminating the buffer solution filling
step; a precursor formation step of forming a core-shell precursor
by supplying raw materials from the first storage 10 and the second
storage 20, which include a material forming a core, into the
interior of the cylinder 68 in which the rotor 69 rotates; a shell
material injection step of supplying a shell material for coating
the core to the interior of the cylinder 68 in which the core-type
precursor is formed; a solid-liquid separation step of separating a
liquid including core-shell particles formed through the shell
material injection into a solid and a liquid; and a drying step of
drying the core-shell particles obtained through the solid-liquid
separation step.
[0067] Here, a rotation speed of the rotor 69 may be 1 rpm or
more.
[0068] In addition, any buffer generally used in the art may be
used.
[0069] Meanwhile, as the liquid including the core-shell particles
separated in the solid-liquid separation step, a reactant in a
normal state within the reactor is used. In each of the first
storage 10 and the second storage 20, a pair of lithium chloride
and sodium carbonate, a pair of lithium hydroxide and carbon
dioxide, or a pair of aluminum carbonate and copper sulfate is
stored.
[0070] However, raw materials stored in the first storage 10 and
the second storage 20 are not limited to the materials described
above.
[0071] In addition, as the shell material, an inorganic metal
including copper, cobalt, or manganese; or a polymer or an oligomer
selected from the group consisting of polyethylene glycol,
polyethylene oxide, polyethylene glycol methyl ether, polyethylene
glycol dimethyl ether, polypropylene oxide, polyethylene,
polypropylene, polyisobutylene, and polyvinylidene chloride may be
used.
[0072] Core-shell particles prepared according to the present
invention preferably have diameters of several nanometers to
micrometers, but are not limited thereto.
[0073] Hereinafter, the present invention is described in more
detail by way of examples. However, it should be understand that
the following examples are merely to concretely explain the spirit
of the invention, and therefore there is no intent to limit the
invention to the examples.
Example
[0074] First, the interior of a reactor was filled with a buffer,
and air remaining in the reactor was discharged to the outside.
[0075] Subsequently, a motor was operated to rotate a rotor of the
reactor connected to the motor at 1000 rpm.
[0076] Lithium chloride stored in a first storage and sodium
carbonate stored in a second storage were then injected into the
reactor by means of a metering pump to form a core.
[0077] Next, copper ions were injected into a shell material inlet
to coat an external circumferential side of a core with a shell
material. As a result, core-shell particles were formed.
[0078] Liquid including core-shell particles were then separated
into solid particles and a liquid by means of a centrifuge and the
core-shell particles were dried. Finally, core-shell positive
electrode active material particles were prepared.
Example 2
[0079] An experiment was carried out in the same manner as in
Example 1, except that, instead of the lithium chloride stored in
the first storage and the sodium carbonate stored in the second
storage, lithium hydroxide was stored in the first storage and
carbon dioxide was stored in the second storage.
Example 3
[0080] An experiment was carried out in the same manner as in
Example 1, except that, instead of the lithium chloride stored in a
first storage and the sodium carbonate stored in a second storage,
aluminum carbonate was stored in the first storage and copper
sulfate was stored in the second storage.
[0081] As described above, those skilled in the art will appreciate
that the present invention may be carried out in specific ways
other than those set forth herein without departing from the spirit
and essential characteristics of the present invention. Therefore,
the present invention is not limited to the examples described
above, and covers modifications of the technical spirit
substantially equivalent thereto. The scope of the invention is
defined not by the detailed description of the invention but by the
appended claims, and all differences within the scope will be
construed as within the scope of the present invention.
* * * * *