KR101548671B1 - Fabrication method of carbon-metal oxide composite and electrochemical device using intense pulsed light - Google Patents

Fabrication method of carbon-metal oxide composite and electrochemical device using intense pulsed light Download PDF

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KR101548671B1
KR101548671B1 KR1020110131258A KR20110131258A KR101548671B1 KR 101548671 B1 KR101548671 B1 KR 101548671B1 KR 1020110131258 A KR1020110131258 A KR 1020110131258A KR 20110131258 A KR20110131258 A KR 20110131258A KR 101548671 B1 KR101548671 B1 KR 101548671B1
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carbon
current collector
metal
electrode
electrochemical device
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KR20130085487A (en
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김학성
안희준
박성현
장기훈
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한양대학교 산학협력단
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The present invention relates to a carbon-metal oxide composite formed using extreme ultraviolet-white light and a method of manufacturing an electrochemical device using the carbon-metal oxide composite, wherein the super capacitor has high storage capacity and high output characteristics.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a carbon-metal oxide composite and an electrochemical device using the extreme-

The present invention relates to a method for producing a carbon-metal oxide composite and an electrochemical device including the same, and more particularly, to a method for producing a carbon-metal oxide complex under normal atmospheric pressure conditions using extreme ultraviolet And an electrochemical device including the carbon-metal oxide composite.

Supercapacitors are commonly used in solar panels and hydrogen fuel cell batteries for automobiles, and unlike conventional batteries that utilize chemical reactions, they utilize charge phenomena caused by simple ion movements or surface chemical reactions at the electrode and electrolyte interface, It can be used for auxiliary battery or battery replacement due to high charge / discharge efficiency and semi-permanent cycle life.

As a material used for a super capacitor, there are a new electrode material such as a metal oxide including an activated carbon and a conductive polymer which have been conventionally used, and a hybrid type product facility using an asymmetric electrode has been developed and attracts attention. In the case of using the metal oxide as the electrode material, it is much more advantageous than the other materials in terms of the capacity, but it is difficult to synthesize the metal oxide and the carbon carrier which helps the current conduction and accumulation, It is sensitive to environmental conditions and is very difficult to synthesize. In addition, there is a problem in that the production time is long and the process temperature is high due to the synthesis method using an electrochemical method, a thermal process, or the like, which is uneconomical.

The object of the present invention is to provide a method for manufacturing a high-efficiency carbon-metal oxide composite capable of large-scale and large-scale production at a low cost through a simple process at a low temperature, and to provide a carbon- And a supercapacitor including the electrochemical device.

In order to solve the above technical problem,

1) coating a carbon carrier dispersion on a substrate and drying;

2) forming a metal precursor layer by impregnating the substrate coated with the carbon support on an aqueous metal precursor solution containing at least one metal ion selected from Ca, Mg, Fe, Co, Ni, Cu and Zn; And

3) irradiating the substrate on which the metal precursor layer is formed with ultraviolet-white light.

According to an embodiment of the present invention, the carbon carrier includes carbon black, carbon nanotubes (CNT), carbon nanofibers (CNF), carbon nanocoils (CNC), aligned porous carbon (OPC) But are not limited to, beads (MCMB), single wall carbon nanohorns (SWNH), carbon aerogels (CAG), graphene or graphene oxides.

According to another embodiment of the present invention, the metal precursor aqueous solution may include two kinds of metal ions, wherein the ratio of the two kinds of metal ions is preferably 1:10 to 10: 1.

According to another embodiment of the present invention, the extreme ultraviolet white light may be irradiated through a xenon flash lamp. At this time, the pulse width of the xenon flash lamp is 0.1 to 100 ms, the pulse gap is 0.1 to 100 ms, the pulse number is 1 to 1000, the intensity is 0.01 J / Lt; 2 > to 100 J / cm < 2 >.

According to another aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: forming a conductive carbon film on a current collector; Impregnating the current collector with the conductive carbon film in an aqueous metal precursor solution containing a first metal salt, a second metal salt, and a base material and drying the same; And forming a carbon-metal oxide composite active material layer by irradiating ultrafine white light to the current collector coated with the metal precursor.

According to an embodiment of the present invention, the metal precursor aqueous solution may contain a first metal salt of M (X) 2 .mH 2 O, a second metal salt of N (Y) 2 .nH 2 O, and a basic substance, wherein N and M are deulyigo metal of different types selected from the group consisting of Ca, Mg, Fe, Co, Ni, Cu and Zn, X and Y are each independently Cl - the group consisting of -, NO 3 - and CHOO And m and n are integers of 0 to 10. For example, M may be nickel and N may be cobalt and may be included at a mixing ratio of 1: 1.

According to another embodiment of the present invention, there is provided an electrochemical device including a carbon-metal oxide composite active material layer, wherein the electrochemical device includes a first electrode including a current collector and a first active material layer on the current collector; A second electrode including a current collector and a second active material layer on the current collector; A separator interposed between the first electrode and the second electrode; And an electrolyte solution for ion exchange.

The electrode including the carbon-metal oxide composite active material layer produced according to the present invention has high capacitance performance and can be used as a super capacitor.

According to the present invention, an electrochemical device to which an electrode including a carbon-metal oxide active material layer is applied by irradiating ultrafine white light onto a current collector exhibits a high output capacity in addition to a high capacitance, so that it can be used as a supercapacitor electrode.

1 is a schematic cross-sectional view illustrating an electrochemical device according to an embodiment of the present invention.
2 is a schematic view showing a method of coating a carbon material on a current collector according to an embodiment of the present invention.
3 is a flowchart illustrating an electrode manufacturing method according to an embodiment of the present invention.
4 is an electron microscope image of an electrode manufactured according to a method of manufacturing an electrochemical device electrode according to an embodiment of the present invention.
5 is a graph illustrating electrochemical characteristics of a supercapacitor to which an electrode manufactured according to an electrochemical device electrode manufacturing method according to an embodiment of the present invention is applied.

Hereinafter, the present invention will be described in detail.

The method for preparing a carbon-metal oxide composite according to the present invention comprises the steps of: 1) coating a carbon carrier dispersion on a substrate and drying; 2) impregnating the substrate coated with the carbon support to an aqueous solution containing at least one metal precursor selected from Ca, Mg, Fe, Co, Ni, Cu and Zn to form a metal precursor layer; And 3) irradiating the substrate on which the metal precursor layer is formed with extreme ultraviolet light.

Carbon supports that can be used in the present invention include carbon black, carbon nanotubes (CNT), carbon nanofibers (CNF), carbon nanocoils (CNC), aligned porous carbon (OPC), mesocarbon microbeads But are not limited to, single wall carbon nanohorns (SWNH), carbon aerogels (CAG), graphene, or graphene oxides.

In the present invention, when the aqueous solution of the metal precursor contains two kinds of metal ions, the ratio of the two kinds of metal ions is preferably 1:10 to 10: 1.

Also, in the present invention, extreme ultraviolet light is irradiated using a xenon flash lamp. Specifically, the pulse width of the xenon flash lamp is preferably 0.1 to 100 ms. The pulse width of the xenon flash lamp is preferably 0.1 to 100 ms, the number of pulses is 1 to 1000, and the intensity of the xenon flash lamp is preferably 0.01 J / cm 2 to 100 J / cm 2. If the pulse width is less than 0.1 ms, the metal can not be sublimed to form a carbon-metal oxide complex due to irradiation with a very large energy, and if it is greater than 100 ms, the carbon-metal oxide complex can not be formed due to too low energy . Further, when the pulse gap is greater than 100 ms or the number of pulses is larger than 1000, even when the intensity is less than 0.01 J / cm 2, the metal-carbon oxide composite can not be formed due to too low energy and the pulse gap is smaller than 0.1 ms Or strength greater than 100 J / cm 2, equipment and lamps are burdened, which shortens the lifetime of the equipment and lamp rapidly, and it is possible to form carbon-metal oxide complexes well beyond this range.

In addition, when the extreme ultraviolet light is irradiated, the temperature of the contained metal salts (for example, nickel nitrate and cobalt chloride) instantaneously rises, and in the course of the process, The oxidation reaction proceeds due to the contact with the surrounding air and instantaneously forms nickel cobalt oxide. At this time, the metal oxide layer is formed on the surface of CNT according to the shape of CNT, thereby widening the surface area.

According to another aspect of the present invention, there is provided a method of manufacturing an electrochemical device including: forming a conductive carbon film on a current collector; Impregnating the current collector with the conductive carbon film in an aqueous metal precursor solution containing a first metal salt, a second metal salt, and a base material and drying the same; And forming a carbon-metal oxide composite active material layer by irradiating ultrafine white light to the current collector coated with the metal precursor.

According to an embodiment of the present invention, the first metal salt is M (X) 2 .mH 2 O, the second metal salt is N (Y) 2 .nH 2 O and the N and M are Ca, Mg, Fe , Co, Ni, Cu and Zn, X and Y are each independently selected from the group consisting of Cl - , NO 3 - and CHOO - , m and n are each a number of from 0 to Lt; / RTI > For example, M and N may be nickel and cobalt, respectively, and the capacitance performance is particularly good when the mixing ratio is 1: 1.

According to another embodiment of the present invention, there is provided an electrochemical device including a carbon-metal oxide composite active material layer, wherein the electrochemical device includes a first electrode including a current collector and a first active material layer on the current collector; A second electrode including a current collector and a second active material layer on the current collector; A separator interposed between the first electrode and the second electrode; And an electrolyte solution for ion exchange.

The electrode including the carbon-metal oxide composite active material layer produced according to the present invention has high capacitance performance and can be used as a super capacitor.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings.

FIG. 1 is a schematic cross-sectional view illustrating an electrochemical device according to an embodiment of the present invention, and the electrochemical device according to an embodiment of the present invention may be a supercapacitor.

1, an electrochemical device according to an embodiment of the present invention includes a first electrode 10 and a second electrode 20, and a separator (not shown) between the first electrode 10 and the second electrode 20. [ (Not shown in the drawing) between the first electrode 10 and the separator 30, and between the separator 30 and the second electrode 20.

The first electrode 10 is an anode and includes a current collector 11 and a first active material layer 13 on the current collector 11. In addition, it may further include a conductive carbon film 12 interposed between the current collector 11 and the first active material layer 13. 2 is a schematic cross-sectional view of one embodiment of methods for coating conductive carbon on a current collector of the present invention.

At this time, the current collector 11 may be Fe, Cu, Ti, Ni, Pt, Al, Au, or an alloy thereof. The current collector 11 may be any porous or non-porous foam selected from the group consisting of a conductive polymer and a conductive oxide.

In addition, the conductive carbon film 12 may be at least one selected from the group consisting of carbon nanotubes, activated carbon, graphene, and graphene oxide.

Further, the first active material layer 13 contains a metal oxide. These metal oxides include two kinds of metal oxides having different kinds of metals.

When it will be described in more detail, the metal oxide is N x O, M x O, N 1 - x M x O m, N (OH) 2 · mH 2 O, M (OH) 2 · mH 2 O, and [N (OH) 2 ] 1-x [M (OH) 2 ] x mH 2 O. In this case, N and M are different kinds of metals selected from the group consisting of Ca, Mg, Fe, Co, Ni, Cu and Zn, 0 <x <1, and m is an integer of 0 to 10. Preferably, N and M may be Ni and Co, respectively.

The metal oxide of the first active material layer 13 may further include a conductive carbon material for improving the charging capacity of the electrochemical device and improving the electrical conductivity of the electrode according to an embodiment of the present invention. The conductive carbon material may be at least one selected from the group consisting of carbon nanotubes, activated carbon, graphene and graphene oxide.

The second electrode 20 is a negative electrode and includes a current collector 21 and a second active material layer 22 on the current collector 21.

The current collector 21 of the second electrode 20 may be formed of any conductive material. For example, the current collector 21 of the second electrode 20 may be formed of any one of a metal foil, a metal mesh, and a conductive polymer compound.

In addition, the negative electrode active material 22 of the second electrode 20 may be any conductive material. For example, the anode active material 22 of the second electrode 20 may be made of a conductive carbon material, a conductive metal, and a conductive oxide.

The material that can be used for the separator 30 may be a microporous polypropylene or polyethylene membrane, a porous glass fiber tissue, or a combination of polypropylene and polyethylene. The number of the separators 30 to be used may be suitable for the number of electrodes as is well known.

The electrolytic solution may be an alkaline electrolyte such as an aqueous solution of potassium hydroxide (KOH), for example, as an aqueous electrolyte having a basic nature because an inventive electrode is dissolved using an acidic electrolyte.

3 is a flowchart illustrating a method of manufacturing an electrode of an electrochemical device according to an embodiment of the present invention.

Referring to FIG. 3, first, an aqueous metal precursor solution is prepared. (S1) At this time, the metal precursor aqueous solution contains a first metal salt, a second metal salt having a metal different from the first metal salt, and a base material. According to an embodiment of the present invention, the first metal salt may be M (X) 2 · mH 2 O and the second metal salt may be N (Y) 2 · nH 2 O, And X and Y may be independently selected from the group consisting of Cl - , NO 3 -, and CHOO - , and each of X and Y may be independently selected from the group consisting of Mg, Fe, Co, Ni, Cu and Zn. m and n are an integer of 0 to 10; The molar ratio of the second metal salt to the first metal salt, that is, the molar ratio of M to the N in the aqueous metal precursor solution is preferably 10% to 90%.

The metal precursor aqueous solution may further include a conductive carbon material. The conductive carbon material may be at least one selected from the group consisting of carbon nanotubes, activated carbon, graphene and graphene oxide.

After preparing the metal precursor aqueous solution, a current collector is prepared, and a conductive carbon film is formed and coated on the current collector. (S2) The current collector may be Fe, Cu, Ti, Ni, Pt, Al, Au, or an alloy thereof. In addition, the current collector may be any one of porous or non-porous foams selected from the group consisting of a conductive polymer and a conductive oxide.

The conductive carbon film may be at least one selected from the group consisting of carbon nanotubes, activated carbon, graphene and graphene oxide. The conductive carbon film on the current collector can be formed through various methods. For example, the conductive carbon film may be formed on the current collector through a carbonation reaction of the polymer precursor, or may be formed by spreading a carbonaceous material paste containing a dispersant on a current collector.

The current collector formed with the conductive carbon film is impregnated in the metal precursor solution for 10 to 30 minutes to form a conductive carbon film current collector including the metal salt, and then the conductive carbon film current collector including the metal salt is dried at room temperature. (S3) The drying method can be carried out using various methods. For example, it can be left to stand in an ordinary temperature atmosphere and dried, and it is also possible to apply heat to evaporate the solvent of the precursor solution to dry it.

Thereafter, the substrate containing the mixture is irradiated with ultraviolet-white light to prepare a carbon-metal oxide composite. (S4) The extreme ultraviolet radiation irradiation conditions vary depending on the pulse width, the pulse gap, the number of pulses, and the intensity, thereby emitting the total light energy up to 100J. Depending on the type of the substrate, the type of the carbon-based support, and the kind of the metal, the light irradiation condition for forming the carbon-metal oxide complex may be varied.

Hereinafter, the present invention will be described in more detail by way of examples. However, the following examples are provided only for the purpose of understanding the present invention, and the scope of the present invention is not limited by the examples.

Example  One

A carbon nanotube paste well dispersed with a dispersant such as Triton X is spread evenly on a stainless steel substrate using a glass rod and heated at a temperature of 400 ° C to remove impurities.

CoCl 2 and Ni (NO 3 ) 2 .6H 2 O were used as precursors of cobalt and nickel, and 1M CoCl 2 and 1M Ni (NO 3 ) 2 .6H 2 O is dissolved in an aqueous solution to prepare an aqueous solution of cobalt and nickel ions.

A stainless steel substrate, which is a conductive current collector coated with carbon nanotubes, was impregnated in this aqueous solution for 2 hours and then dried at room temperature for 5 hours to prepare a carbon nanotube containing a cobalt-nickel salt aqueous solution.

A carbon nanotube / stainless steel substrate containing a metal salt was irradiated with ultraviolet-white light having the conditions shown in Table 1 below to form nickel cobalt oxide on the carbon nanotubes. The carbon-metal oxide complex can also be further oxidized in a furnace at 500 ° C.

Pulse width Pulse gap Number of pulses burglar 6 ms 5 ms 3 ms 40 J

Example  2

An electrode of an electrochemical device was fabricated in the same manner as in Example 1, except that the intensity of the exposed white light was changed to 10J.

Example  3

An electrode of an electrochemical device was fabricated in the same manner as in Example 1, except that the intensity of the exposed white light was 25J.

Example  4

The electrode of the electrochemical device was fabricated in the same manner as in Example 1, except that the intensity of the exposed white light was 55J.

Example  5

An electrode of an electrochemical device was manufactured in the same manner as in Example 1 except that the molar ratio of nickel and cobalt ions was 2: 1.

Example  6

An electrode of an electrochemical device was manufactured in the same manner as in Example 2 except that the molar ratio of nickel and cobalt ions was 2: 1.

Example  7

An electrode of an electrochemical device was manufactured in the same manner as in Example 3 except that the molar ratio of nickel and cobalt ions was 2: 1.

Example  8

An electrode of an electrochemical device was fabricated in the same manner as in Example 4 except that the molar ratio of nickel and cobalt ions was 2: 1.

Example  9

An electrode of an electrochemical device was fabricated in the same manner as in Example 1, except that the molar ratio of nickel and cobalt ions was 1: 2.

Example  10

Electrode was prepared in the same manner as in Example 2 except that the molar ratio of nickel and cobalt ions was 1: 2.

Example  11

An electrode of an electrochemical device was fabricated in the same manner as in Example 3, except that the molar ratio of nickel and cobalt ions was 1: 2.

Example  12

An electrode of an electrochemical device was manufactured in the same manner as in Example 4 except that the molar ratio of nickel and cobalt ions was 1: 2.

.

The measurement values obtained by applying the electrodes of Examples 1 to 12 to the supercapacitor as an electrochemical device are summarized in Table 2 below.

Capacitance Capacity
(F / g) Energy density
(Wh / kg) Power density
(Kw / kg) NiCo (1: 1) 10J 423.3028 21.16514 5.879206 NiCo (1: 1) 25J 1206.935 60.34675 16.76299 NiCo (1: 1) 40 J 1226.697 61.33485 17.03746 NiCo (1: 1) 55J 437.5939 21.8797 6.077693 NiCo (1: 2) 10J 950.9823 47.54912 13.20809 NiCo (1: 2) 25J 849.7042 42.48521 11.80145 NiCo (1: 2) 40 J 505.3241 25.26621 7.01839 NiCo (1: 2) 55J 608.9336 30.44668 8.457411 NiCo (2: 1) 10J 1076.709 53.83545 14.95429 NiCo (2: 1) 25J 880.0719 44.0036 12.22322 NiCo (2: 1) 40 J 601.825 30.09125 8.358681 NiCo (2: 1) 55J 351.9322 17.59661 4.887947

Referring to Table 2, the electrode exposed to 40 J of white light with a ratio of nickel to cobalt of 1: 1 showed the best performance in terms of specific capacitance, energy density, power density, and the like .

4 is an electron microscope image of an electrode manufactured according to an embodiment of the present invention, and is an image photographed at various magnifications. Referring to FIG. 4, the electrode manufactured according to the embodiment of the present invention has a nickel cobalt oxide layer formed along the surface of the carbon nanotube.

5 is a graph illustrating electrochemical characteristics of a supercapacitor to which an electrode manufactured according to an embodiment of the present invention is applied. Referring to FIG. 5, the supercapacitor to which the electrochemical device electrode according to Example 1 of the present invention is applied has a high redox peak as a result of the measurement of the circulating voltage-ammeter.

Claims (14)

1) coating a carbon carrier dispersion on a substrate and drying;
2) forming a metal precursor layer by impregnating the substrate coated with the carbon support on an aqueous metal precursor solution containing at least one metal ion selected from Ca, Mg, Fe, Co, Ni, Cu and Zn; And
3) irradiating the substrate on which the metal precursor layer is formed with extreme ultraviolet light,
Wherein the metal precursor aqueous solution comprises two kinds of metal ions, and the ratio of the two kinds of metal ions is 1:10 to 10: 1. The method according to claim 1,
The carbon support may be selected from the group consisting of carbon black, carbon nanotubes (CNT), carbon nanofibers (CNF), carbon nanocoils (CNC), aligned porous carbon (OPC), mesocarbon microbeads (MCMB) Wherein the carbon nanotube is selected from the group consisting of horn (SWNH), carbon aerogels (CAG), graphene or graphene oxide. delete The method according to claim 1,
Wherein the extreme ultraviolet light is irradiated through a xenon flash lamp. 5. The method of claim 4,
Wherein the pulse width of the xenon flash lamp is 0.1 to 100 ms. 5. The method of claim 4,
Wherein a pulse gap of the xenon flash lamp is 0.1 to 100 ms. 5. The method of claim 4,
Wherein the pulse number of the xenon flash lamp is 1 to 1000 times. 5. The method of claim 4,
Wherein the intensity of the xenon flash lamp is in the range of 0.01 J / cm2 to 100 J / cm2. Forming a conductive carbon film on the current collector;
Impregnating the current collector with the conductive carbon film in an aqueous metal precursor solution containing a first metal salt, a second metal salt, and a base material and drying the same;
And forming a carbon-metal oxide composite active material layer by irradiating ultrafine white light to the current collector coated with the metal precursor. 10. The method of claim 9,
Wherein the first metal salt is M (X) 2 mH 2 O and the second metal salt is N (Y) 2 .nH 2 O wherein N and M are Ca, Mg, Fe, Co, Ni, Wherein X and Y are each independently selected from the group consisting of Cl - , NO 3 - and CHOO - , and m and n are integers of 0 to 10, / RTI &gt; 11. The method of claim 10,
Wherein M is nickel and N is cobalt. 12. The method of claim 11,
Wherein the mixing ratio of nickel to cobalt is 1: 1. 10. The method of claim 9,
The electrochemical device comprising: a first electrode including a current collector and a first active material layer on the current collector; A second electrode including a current collector and a second active material layer on the current collector; A separator interposed between the first electrode and the second electrode; And an electrolytic solution for ion exchange. 12. A super capacitor comprising the electrochemical device according to claim 9.
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