KR20140087393A - Method for manufacturing a porous carbon black and its applications - Google Patents
Method for manufacturing a porous carbon black and its applications Download PDFInfo
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- KR20140087393A KR20140087393A KR1020120157595A KR20120157595A KR20140087393A KR 20140087393 A KR20140087393 A KR 20140087393A KR 1020120157595 A KR1020120157595 A KR 1020120157595A KR 20120157595 A KR20120157595 A KR 20120157595A KR 20140087393 A KR20140087393 A KR 20140087393A
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- carbon black
- porous carbon
- electrode
- aqueous solution
- energy storage
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- 239000006229 carbon black Substances 0.000 title claims abstract description 65
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000007772 electrode material Substances 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 27
- 238000004146 energy storage Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 5
- 241000872198 Serjania polyphylla Species 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 2
- 229920005830 Polyurethane Foam Polymers 0.000 claims 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims 1
- 239000004327 boric acid Substances 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 239000011496 polyurethane foam Substances 0.000 claims 1
- 239000003990 capacitor Substances 0.000 abstract description 15
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000003575 carbonaceous material Substances 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 235000019241 carbon black Nutrition 0.000 description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 230000004913 activation Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 238000007600 charging Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 239000002482 conductive additive Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010325 electrochemical charging Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J6/00—Heat treatments such as Calcining; Fusing ; Pyrolysis
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B1/00—Nanostructures formed by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B1/008—Nanostructures not provided for in groups B82B1/001 - B82B1/007
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
Abstract
The present invention relates to a capacitor additive and a method for producing carbon black for an electrode active material. More particularly, the present invention relates to a method for manufacturing a carbon material capable of simultaneously achieving prevention of energy density reduction and improvement of power density by performing chemically- ≪ / RTI >
Description
BACKGROUND OF THE
High-performance portable energy storage devices are a key component of devices that are essential for all portable information and communications devices, electronic devices, and electric vehicles. The next-generation energy storage systems that have been recently developed are all based on electrochemical principles, and are representative of lithium-based secondary batteries and electrochemical capacitors. An electrochemical capacitor is an energy storage device that stores and supplies electric energy by using a capacitor behavior caused by an electrochemical reaction between an electrode and an electrolyte. As compared with a conventional electrolytic capacitor and a secondary battery, an energy density and an output density are superior Is a new concept of energy storage power source capable of quickly storing or supplying energy of various kinds. Electrochemical capacitors are expected to be used as back-up power sources for electronic devices, pulse power sources for portable mobile communication devices, and high output power sources for hybrid electric vehicles due to their ability to supply a large amount of current in a short time . The development of a supercapacitor whose energy density is larger than that of a conventional capacitor is of interest in such an electrochemical capacitor. An electric double layer capacitor (hereinafter referred to as an " electric double layer capacitor " : EDLC) and pseudo-capacitors generated in the faradaic reaction accompanied by the charge transfer between the electrode and the electrolyte such as the adsorption reaction on the electrode surface of the electrolyte or the oxidation / reduction reaction of the electrode It is a supercapacitor. Among them, the pseudo capacitor is a super capacitor which exhibits a super high capacitance with a
The lithium secondary battery and the electric double layer capacitor are very similar in the structure and the operating principle of the unit cell, but show a difference in the charge storing mechanism. That is, in the lithium secondary battery, electrons and ions are transferred to the bulk of the electrode material depending on charge and discharge, and depend on the reaction involving the movement of electrons, so that the phase change of the electrode material is accompanied by the phase change. There is a characteristic that charging and discharging occurs only at the interface between the electrode and the electrolyte.
In general, a method of manufacturing an electrode is a coating method in which a binder is a mixture of a binder and a conductive material such as carbon black, which is prepared by dissolving a certain amount of active carbon powder or fiber in a solvent, Can be divided into a sheet form in paste state together with a binder and a rolling method in which the sheet is adhered to a current collector or is adhered to a current collector through a conductive adhesive. Because the activated carbon used here is very resistant to the reaction, carbon black is used as a conductive additive to control the resistance of the entire cell. However, carbon black has a very small specific surface area compared to activated carbon and low density, .
SUMMARY OF THE INVENTION It is an object of the present invention to solve the above problems by providing a method of forming a pore by performing a chemical activation treatment on a surface of a carbon black to increase the amount of energy storage while maintaining conductivity by introducing a mixed secondary structure between the carbon black .
In order to achieve the above-mentioned object, carbon black having different diameters of 18 nm and 95 nm were selected to confirm the activation behavior according to the diameter of the primary structure of carbon black. Carbon black exists in various sizes and various structures, and carbon black having a diameter of 10 nm to 130 nm is commercially available.
When carbon black is used as an active material to replace activated carbon, differences in generation of pores depending on the diameter and difference in electrochemical charging amount can be considered as important characteristics in selection.
Carbon black has a secondary structure in which the primary structure is aggregated and also has a great influence on the properties such as electrical conductivity and the penetration degree of the chemical during chemical activation also changes depending on the secondary structure.
Preferred activation methods include heat treatment in an inert atmosphere by mixing a powdered or boiled aqueous solution of either sodium hydroxide or potassium hydroxide with carbon black, and an instantaneous heat treatment at high temperature for removal of the functional groups.
The present invention is characterized by using low-cost carbon black, which has been considered only as a conductive additive in an energy storage device, directly as an electrode material of a supercapacitor or improving the energy density to be lowered due to the low specific surface area of carbon black to be added do.
1 is a graph showing the results of measurement of carbon content of 18 nm carbon activated at respective heat treatment temperatures (600 ° C. (HTT 600), 700 ° C. (HTT 700), 800 ° C. (HTT 800) and 900 ° C. To the adsorption isotherms of black (CB-18) and 95 nm carbon black (CB-95).
Figure 2 relates to the BET value according to the heat treatment temperature calculated from the adsorption isotherm of Figure 1.
Fig. 3 relates to the capacitance per unit weight measured by the constant-voltage / constant-current method of carbon black activated at each heat treatment temperature.
Figure 4 relates to capacity per volume calculated using the density of the electrode using the capacitance of Figure 3;
Fig. 5 relates to the capacity change of carbon black activated at each heat treatment temperature and the behavior according to the discharge current density.
FIG. 6 is a Rangone plot showing the correlation between energy density and power density calculated from the charge / discharge results using activated CB-18 at each heat treatment temperature.
7 is a Rangone plot showing the correlation between energy density and power density calculated from the results of charging and discharging using CB-95 activated at each heat treatment temperature.
The differences in the pore structure and the electrochemical energy storage characteristics depending on the diameter of the carbon black when activating the chemical (KOH) of the present invention will be described in detail below with reference to the accompanying drawings.
In a first embodiment of the present invention, there is provided a process for producing a porous carbon black comprising the steps of mixing carbon black with an alkaline aqueous solution or a boiling aqueous solution, heat-treating the mixture in the mixing step, washing the heat-treated carbon black with water, Followed by washing and drying. The present invention also relates to a method for producing the porous carbon black.
A second embodiment of the present invention relates to a process for producing a porous carbon black according to the first embodiment, wherein the carbon black has a diameter of 10 to 130 nm.
A third embodiment of the present invention relates to a method for producing a porous carbon black according to the first embodiment, wherein the aqueous alkaline solution is sodium hydroxide or potassium hydroxide aqueous solution.
A fourth embodiment of the present invention relates to a method for producing a porous carbon black according to the first embodiment, wherein the aqueous alkaline solution is mixed at 2 to 5 times the weight of the carbon black.
In a fifth embodiment of the present invention, in the first embodiment, the heat treatment is performed at 600 to 900 ° C in an inert atmosphere.
A sixth embodiment of the present invention relates to a porous carbon black having mesopore type pores having a BET value of 100 to 800 m 2 / g, produced by the manufacturing method of the first embodiment.
A seventh embodiment of the present invention relates to an electrode comprising the porous carbon black of the sixth embodiment as an electrode active material.
An eighth embodiment of the invention relates to an energy storage device comprising an electrode of the seventh embodiment.
A ninth embodiment of the present invention relates to an energy storage device according to the eighth embodiment, wherein the energy storage device is a supercapacitor.
Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples.
Example
Carbon black, which is the starting material of the present invention, was selected from Tokai Corporation and Asahi Corp. carbon blacks (9H SAF-HS, SP SRF-LS and Sunblack- series) in Japan among thermal blacks generated during incomplete combustion. Two samples with large diameters of 18 nm and 95 nm were selected to confirm the activation tendency and the electrochemical characteristics according to the diameter of carbon black. The KOH was mixed with 4 times the weight ratio and heat treated to 600 ~ 900 ° C. Respectively. After activating KOH, it was neutralized with water and dilute acid to remove chemicals inside the pores, and the surface was washed and dried, and then applied as an electrode material.
The conditions for electrode production were a coin type having a diameter of 1.2 cm and molded using a molder to form an electrode having a thickness of about 300 micrometers. The composition ratio at the time of electrode molding was made without using a conductive agent in the ratio of the active material 90 and the
The prepared electrode was impregnated in the used organic solvent, and the internal gas was removed for about 3 hours in a vacuum state, and the first charge / discharge capacity was measured after 10 charge / discharge cycles.
1 is an adsorption isotherm showing changes in pores obtained by activating carbon black at 18 nm and carbon black at 95 nm by adding KOH at 4 times KOH at 600, 700, 800 and 900 ° C, respectively. All the samples had a structure similar to that of Type II and IV, confirming that mesopore was predominant rather than micropores. As the temperature increased, the amount of pores on the surface of the carbon black increased further. Under the same conditions, CB-95 with larger diameter shows more pore structure, which seems to be related to the accessibility of KOH solution.
FIG. 2 shows the result of checking how the BET value calculated from the adsorption isotherm of FIG. 1 changes with the treatment temperature. Contrary to the tendency of the adsorption amount, it was confirmed that CB-18 having a small diameter had a specific surface area of about 1/2 at the same temperature as that of CB-95. This is due to the influence of micropores formed in CB-18 . Small-diameter carbon black confirmed that small pores were predominantly formed by chemical activation.
Fig. 3 shows the results of comparing the electrostatic capacity per unit weight of the electrochemical charged amount measured by the constant voltage / constant current method. In the case of CB-18, continuous increase in capacity was observed with increasing heat treatment. However, in case of CB-95, no increase in capacity was observed at temperatures above 700 ° C., .
FIG. 4 is a graph showing the capacitance per volume by using the density of the electrode using the capacitance of FIG. 3; In the case of small-sized CB-18, the capacity of CB-95 was increased after heat treatment. However, CB-95, which has larger capacity than CB-95, And correlated with the pore structure of the highly formed CB-18.
FIG. 5 is a graph illustrating the behavior of the CB-18 according to the change of the capacity according to the temperature and the discharge current density. As the temperature increases with the temperature, the capacity is about 25 F / g at a slow discharge rate of 1 mA. It can be seen that even if the speed is increased, the deviation is not large. CB-95 shows a slight decrease in capacity after 700 ° C and a larger capacity deviation due to the discharge current density. This tendency has similar results in volume capacity. Small-diameter carbon black allows quick charging and discharging with a small capacity variation according to the current density. However, large-diameter carbon black has a large capacity deviation and has advantages in capacity per volume .
6 and 7 are Rangone plots showing the correlation between the energy density and the power density calculated from the charge / discharge results. Small diameter CB-18 has an energy density of 10 ~ 20Wh / kg and a power density of 15 ~ 1000W / kg with continuous increase in capacity as the activation temperature increases. In the case of large diameter CB-95, The energy density at the treatment temperature is saturated and has a value higher than that of CB-18 at the energy density per volume. That is, it is possible to propose various possibilities to control energy and power by controlling the size of the carbon black and the condition of the chemical activation treatment.
Claims (9)
Mixing the carbon black with an alkaline aqueous solution or a boric acid aqueous solution;
Heat-treating the mixture in the mixing step; And
Washing the heat-treated carbon black with water, neutralizing and then washing and drying.
A method for producing porous carbon black.
Characterized in that the carbon black has a diameter of 10 to 130 nm.
A method for producing porous carbon black.
Wherein the alkali aqueous solution is sodium hydroxide or potassium hydroxide aqueous solution.
A method for producing porous carbon black.
Characterized in that the alkali aqueous solution is mixed at 2 to 5 times the weight of the carbon black.
A method for producing porous carbon black.
Characterized in that the heat treatment is carried out at 600-900 < 0 > C in an inert atmosphere.
A method for producing porous carbon black.
A porous carbon black having mesopore type pores having a BET value of 100 to 800 m 2 / g.
Characterized in that the energy storage device is a supercapacitor.
Energy storage device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020120157595A KR20140087393A (en) | 2012-12-28 | 2012-12-28 | Method for manufacturing a porous carbon black and its applications |
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| Application Number | Priority Date | Filing Date | Title |
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| KR1020120157595A KR20140087393A (en) | 2012-12-28 | 2012-12-28 | Method for manufacturing a porous carbon black and its applications |
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| KR20140087393A true KR20140087393A (en) | 2014-07-09 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102153241B1 (en) | 2019-12-19 | 2020-09-07 | 금오공과대학교 산학협력단 | Hollow carbon black having micro-porosity and manufacturing method thereof |
| KR20210094443A (en) | 2020-01-21 | 2021-07-29 | 금오공과대학교 산학협력단 | Hollow carbon black assembly having micro-porosity and manufacturing method thereof |
| KR20210130642A (en) | 2020-04-22 | 2021-11-01 | 금오공과대학교 산학협력단 | cathode material for metal-air bettery and manufacturing method thereof |
| KR20210130641A (en) | 2020-04-22 | 2021-11-01 | 금오공과대학교 산학협력단 | anode material for lithium ion bettery and manufacturing method thereof |
| KR20210143104A (en) | 2020-05-19 | 2021-11-26 | 금오공과대학교 산학협력단 | cathode material for metal-air bettery and manufacturing method thereof |
| KR20210143091A (en) | 2020-05-19 | 2021-11-26 | 금오공과대학교 산학협력단 | Hollow carbon black assembly having micro-porosity and manufacturing method thereof |
-
2012
- 2012-12-28 KR KR1020120157595A patent/KR20140087393A/en not_active Application Discontinuation
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102153241B1 (en) | 2019-12-19 | 2020-09-07 | 금오공과대학교 산학협력단 | Hollow carbon black having micro-porosity and manufacturing method thereof |
| WO2021125782A1 (en) * | 2019-12-19 | 2021-06-24 | 금오공과대학교 산학협력단 | Microporous hollow carbon black and manufacturing method therefor |
| KR20210094443A (en) | 2020-01-21 | 2021-07-29 | 금오공과대학교 산학협력단 | Hollow carbon black assembly having micro-porosity and manufacturing method thereof |
| KR20210130642A (en) | 2020-04-22 | 2021-11-01 | 금오공과대학교 산학협력단 | cathode material for metal-air bettery and manufacturing method thereof |
| KR20210130641A (en) | 2020-04-22 | 2021-11-01 | 금오공과대학교 산학협력단 | anode material for lithium ion bettery and manufacturing method thereof |
| KR20210143104A (en) | 2020-05-19 | 2021-11-26 | 금오공과대학교 산학협력단 | cathode material for metal-air bettery and manufacturing method thereof |
| KR20210143091A (en) | 2020-05-19 | 2021-11-26 | 금오공과대학교 산학협력단 | Hollow carbon black assembly having micro-porosity and manufacturing method thereof |
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