CN111640589A - Preparation method of flexible symmetrical supercapacitor based on Prussian blue - Google Patents
Preparation method of flexible symmetrical supercapacitor based on Prussian blue Download PDFInfo
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- CN111640589A CN111640589A CN202010528774.7A CN202010528774A CN111640589A CN 111640589 A CN111640589 A CN 111640589A CN 202010528774 A CN202010528774 A CN 202010528774A CN 111640589 A CN111640589 A CN 111640589A
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- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229960003351 prussian blue Drugs 0.000 title claims abstract description 18
- 239000013225 prussian blue Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- -1 polyethylene Polymers 0.000 claims description 12
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 6
- 239000006229 carbon black Substances 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 239000003792 electrolyte Substances 0.000 claims description 6
- 238000004146 energy storage Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 150000003624 transition metals Chemical class 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000011262 electrochemically active material Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- UETZVSHORCDDTH-UHFFFAOYSA-N iron(2+);hexacyanide Chemical compound [Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] UETZVSHORCDDTH-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- GTSHREYGKSITGK-UHFFFAOYSA-N sodium ferrocyanide Chemical compound [Na+].[Na+].[Na+].[Na+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] GTSHREYGKSITGK-UHFFFAOYSA-N 0.000 description 1
- 235000012247 sodium ferrocyanide Nutrition 0.000 description 1
- 239000000264 sodium ferrocyanide Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
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- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
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- Nanotechnology (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a preparation method of a Prussian blue-based flexible symmetrical supercapacitor, which comprises the steps of dispersing GO in distilled water, adding Co-HCF nano particles into the distilled water, violently stirring, transferring a mixture into a high-pressure kettle for hydrothermal reaction, naturally cooling the high-pressure kettle to room temperature, separating the obtained product, drying the product, grinding the product into powder to obtain Co-HCF/GO, and assembling the Co-HCF/GO/NF// Co-HCF/GO/NF flexible symmetrical supercapacitor based on Prussian blue on the basis of Co-HCF/GO.
Description
Technical Field
The invention particularly relates to a preparation method of a Prussian blue-based flexible symmetrical supercapacitor, and belongs to the field of energy storage.
Background
With the rapid increase of energy demand, the development of high performance energy storage devices has become an urgent requirement, and materials with high energy and high power density have become hot spots of interest for researchers. Energy storage materials have numerous applications in hybrid vehicle, portable electronic and wearable device design. The super capacitor has the performance of the combination of an electrolytic capacitor and a traditional battery. In the last few years, sodium ion super capacitors have attracted much attention, have extremely high energy density, ultra-long cycle life, relatively low cost, and have broad application prospects in large-scale electric energy storage systems.
Transition metal-based hydroxides/oxides, sulfides, phosphides, etc. are often compounded with conducting polymers to form composites and used as electrode materials because such composites have multiple oxidation states, large capacity electroactive centers and can thereby initiate redox faradaic reactions, characteristics that make such composites promising electrochemically active materials. The structure of Prussian Blue (PB) is iron hexacyanide (Fe)4[Fe(CN)6]3) Having a Face Centered Cubic (FCC) crystal structure, is considered to be the first example of a synthetic coordination compound or metal organic framework compound. Compared to PB, Prussian Blue Analog (PBA) has a similar crystal structure, with some or all of the iron positions being replaced by other transition metal ions. Such analogs are more widely used in electrolysis, supercapacitors and batteries. Various transition metals such as Mn, Fe, Co, Ni, Cu and Zn are often used to react with sodium ferrocyanide to produce new prussian blue analogues. Among them, the prussian blue analogue Co-HCF containing Co shows great electrochemical activation and high specific capacity. On the other hand, Graphene (GO) is widely used as a dopant for semiconductor materials due to its abundant active centers, stable structure and high conductivity. In recent years, the advantages of graphene and prussian blue analogues are gradually shown, and the requirement of rapid development of supercapacitors is met. Since the symmetrical supercapacitor has excellent rate performance and long-life cycle performance and is easier to assemble, the capacitor is wearableIn energy devices, the research on symmetric supercapacitors is receiving more and more attention.
Disclosure of Invention
The invention aims to provide a preparation method of a Prussian blue-based flexible symmetrical supercapacitor.
The invention adopts the following means:
(1) preparing GO by a conventional improved Hummers method, and synthesizing Co-HCF nanoparticles by a conventional self-coordination method;
(2) 0.1gGO was dispersed in 70mL of distilled water. Afterwards, Co-HCF nanoparticles with different masses were added to the GO dispersion obtained from (1). After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. After the autoclave is naturally cooled to room temperature, separating the product, drying at 50 ℃ and grinding into powder to obtain Co-HCF/GO;
(3) taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto two pieces of 1 × 2cm2Respectively as the cathode and the anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state flexible symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
The invention has the advantages that:
the method comprises the steps of carrying out hydrothermal compounding on Co-HCF and activated GO to prepare a compound Co-HCF/GO of graphene and Prussian blue analogues, and then assembling a flexible symmetrical supercapacitor based on Co-HCF/GO/NF/Co-HCF/GO/NF of Prussian blue on the basis of the Co-HCF/GO, wherein the prepared product is regular in shape and excellent in electrochemical performance; 2. the prepared flexible symmetrical super capacitor has excellent energy storage performance and flexible and wearable characteristics; 3. the product is simple to prepare, low in cost and suitable for large-area popularization and application.
Drawings
FIG. 1 is a scanning electron microscope image of CoHCF/GO, a product of example 2 of the present invention;
FIG. 2 is a FT-IR plot of CoHCF/GO, a product of example 2 of the present invention;
FIG. 3 is a charging and discharging curve of a CoHCF/GO/NF// CoHCF/GO/NF flexible supercapacitor device assembled by the product of example 2 of the invention under different current densities.
Detailed Description
Example 1
Preparing GO by a conventional improved Hummers method, and synthesizing Co-HCF nanoparticles by a conventional self-coordination method;
0.1gGO was sonicated for 2h and dispersed in 70mL of distilled water. Thereafter, 0.05g of co-HCF nanoparticles were added to the ultrasonically dispersed GO solution. After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. And naturally cooling the high-pressure kettle to room temperature, separating the obtained product, drying at 50 ℃, and grinding into powder to obtain the Co-HCF/GO.
Taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto 2 pieces of 1 × 2cm2Respectively as the cathode and the anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
Example 2
Preparing GO by a conventional improved Hummers method, and synthesizing Co-HCF nanoparticles by a conventional self-coordination method;
0.1gGO was sonicated for 2h and dispersed in 70mL of distilled water. Thereafter, 0.1g of co-HCF nanoparticles were added to the ultrasonically dispersed GO solution. After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. And naturally cooling the high-pressure kettle to room temperature, separating the obtained product, drying at 50 ℃, and grinding into powder to obtain the Co-HCF/GO.
Taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto 2 pieces of 1 × 2cm2On foamed nickel of (2), respectively asA cathode and an anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
Example 3
Preparing GO by a conventional improved Hummers method, and synthesizing Co-HCF nanoparticles by a conventional self-coordination method;
0.1gGO was sonicated for 2h and dispersed in 70mL of distilled water. Thereafter, 0.15g of co-HCF nanoparticles were added to the ultrasonically dispersed GO solution. After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. And naturally cooling the high-pressure kettle to room temperature, separating the obtained product, drying at 50 ℃, and grinding into powder to obtain the Co-HCF/GO.
Taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto 2 pieces of 1 × 2cm2Respectively as the cathode and the anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
Example 4
Preparing GO by a conventional improved Hummers method, and synthesizing Co-HCF nanoparticles by a conventional self-coordination method;
0.1gGO was sonicated for 2h and dispersed in 70mL of distilled water. Thereafter, 0.2g of co-HCF nanoparticles were added to the ultrasonically dispersed GO solution. After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. And naturally cooling the high-pressure kettle to room temperature, separating the obtained product, drying at 50 ℃, and grinding into powder to obtain the Co-HCF/GO.
Taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto 2 pieces of 1 × 2cm2Respectively as the cathode and the anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
Without being limited thereto, any changes or substitutions that are not thought of through the inventive work should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (2)
1. A preparation method of a Prussian blue-based flexible symmetrical supercapacitor is characterized by comprising the following steps:
(1) GO was prepared by the conventional modified Hummers method. Synthesizing Co-HCF nano particles by a conventional self-coordination method;
(2) 0.1g GO was dispersed in 70mL distilled water. Afterwards, Co-HCF nanoparticles with different masses were added to the GO dispersion obtained from (1). After vigorous stirring for 2 hours at 60 ℃, the mixture was transferred to an autoclave for hydrothermal reaction. After the autoclave is naturally cooled to room temperature, separating the product, drying at 50 ℃ and grinding into powder to obtain Co-HCF/GO;
(3) taking a polyethylene film as a substrate and foamed nickel as a current collector, and mixing Co-HCF/GO, carbon black and polytetrafluoroethylene powder according to a mass ratio of 8: 1: 1 grinding into uniform slurry, and uniformly coating onto two pieces of 1 × 2cm2Respectively as the cathode and the anode. The battery diaphragm is used as a diaphragm to separate the anode and the cathode, and PVA/Na is used2SO4As an electrolyte, the Prussian blue-based all-solid-state flexible symmetrical supercapacitor Co-HCF/GO/NF// Co-HCF/GO/NF is prepared.
2. The preparation method of the Prussian blue-based flexible symmetrical supercapacitor according to claim 1, which is characterized in that: the flexible symmetrical super capacitor assembled by the obtained product has large energy storage capacity and has the characteristics of flexibility and wearability.
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Citations (4)
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---|---|---|---|---|
US20130130049A1 (en) * | 2009-12-22 | 2013-05-23 | Pasi Moilanen | Fabrication and application of polymer-graphitic material nanocomposites and hybride materials |
CN105017527A (en) * | 2015-07-05 | 2015-11-04 | 桂林电子科技大学 | Preparation method and application of Prussian-blue-nanocrystal-loaded graphene composite material |
CN107799318A (en) * | 2017-10-24 | 2018-03-13 | 上海交通大学 | Prussian blue/reduced graphene composite film material and its preparation method and application |
CN108630446A (en) * | 2017-03-20 | 2018-10-09 | 北京大学深圳研究生院 | Positive plate and water system Asymmetric Supercapacitor for Asymmetric Supercapacitor |
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2020
- 2020-06-11 CN CN202010528774.7A patent/CN111640589A/en active Pending
Patent Citations (4)
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US20130130049A1 (en) * | 2009-12-22 | 2013-05-23 | Pasi Moilanen | Fabrication and application of polymer-graphitic material nanocomposites and hybride materials |
CN105017527A (en) * | 2015-07-05 | 2015-11-04 | 桂林电子科技大学 | Preparation method and application of Prussian-blue-nanocrystal-loaded graphene composite material |
CN108630446A (en) * | 2017-03-20 | 2018-10-09 | 北京大学深圳研究生院 | Positive plate and water system Asymmetric Supercapacitor for Asymmetric Supercapacitor |
CN107799318A (en) * | 2017-10-24 | 2018-03-13 | 上海交通大学 | Prussian blue/reduced graphene composite film material and its preparation method and application |
Non-Patent Citations (2)
Title |
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XU ZHANG等: "A flexible and high voltage symmetric supercapacitor based on hybrid configuration of cobalt hexacyanoferrate/reduced graphene oxide hydrogels", 《CHEMICAL ENGINEERING JOURNAL》 * |
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