Classifications

• • 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
  • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05D1/00—Processes for applying liquids or other fluent materials
  • B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
  • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
  • B05D3/007—After-treatment
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/20—Graphite
  • C01B32/21—After-treatment
  • C01B32/23—Oxidation
• • 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
  • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
  • H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2204/00—Structure or properties of graphene
  • C01B2204/20—Graphene characterized by its properties
  • C01B2204/22—Electronic properties
• • 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

Definitions

• the invention relates to components for energy storage, in particular capacitors.
• the capacitors concerned are also called “supercapacitors”, characterized by a higher energy density than that of dielectric capacitors and a higher power density than that of batteries.
• Supercapacitors generally comprise two porous electrodes impregnated with an electrolyte (an ionic salt in generally organic solution, a quaternary ammonium salt such as tetraethylammonium tetrafluoroborate in acetonitrile or propylene carbonate, for example). These electrodes are generally separated by an insulating and porous membrane allowing the circulation of the ions of the electrolyte.
• an electrolyte an ionic salt in generally organic solution, a quaternary ammonium salt such as tetraethylammonium tetrafluoroborate in acetonitrile or propylene carbonate, for example.
• the first supercapacitors known as “EDLC” (acronym for “Electrochemical Double Layer Capacitator”) are based on a principle equivalent to that of conventional capacitors with polarizable electrodes and an electrolyte acting as a dielectric. Their capacity comes from the organization of a double layer of ions and electrons at the electrolyte / electrode interface.
• EDLC Electrochemical Double Layer Capacitator
• supercapacitors combine, for the storage of energy, a capacitive component resulting from the electrostatic organization of ions near the electrodes and a pseudocapacitive component due to oxidation-reduction reactions in the capacitor.
• the electrostatic component of the energy storage is effected by a non-homogeneous distribution of the electrolyte ions in the vicinity of the surface of each electrode, under the effect of the potential difference applied between the two electrodes.
• the electrostatic component of the energy storage confers a potentially high specific power and a very good behavior along the charging and discharging cycles.
• Supercapacitors could replace conventional capacitors for applications with high energy demands, including extreme temperatures, vibrations, high acceleration or high salinity. In these environments, the batteries can not operate without their life span being very limited (these conditions apply to radar, motorsport, electrical avionics and military applications for example). Supercapacitors can also be applied to systems that require energy peaks on short times, of the order of a minute, for acceleration phases of vehicles in land transport (automobiles, trams, buses, devices called “ stop and start "in which energy is recovered during deceleration).
• Supercapacitors could also be useful for managing electricity in embedded systems, for securing electrical installations, securing the energy supply of sensitive systems (radio sets, surveillance systems, military field, radio control center). data), in autonomous sensor networks for surveillance applications of industrial sites, complex or sensitive (hospitals, avionics, offshore platform, oil prospecting, submarine applications) and finally in renewable energies (wind turbines, recovery of atmospheric electric energy).
• sensitive systems radio sets, surveillance systems, military field, radio control center. data
• autonomous sensor networks for surveillance applications of industrial sites, complex or sensitive (hospitals, avionics, offshore platform, oil prospecting, submarine applications) and finally in renewable energies (wind turbines, recovery of atmospheric electric energy).
• the energy density and power of supercapacitors must be optimized.
• the internal resistance of a supercapacitor is today too high and poorly controlled.
• the usual supercapacitors consist of activated carbons with inhomogeneous and unoptimized pore size distributions and use a polymeric binder to ensure the mechanical strength of their structure. This binder
• the present invention relates to a process for depositing nano- / microparticles, including at least graphene sheets, on a substrate, comprising the steps of:
• said nanoparticles / microparticles are suspended in a said solution in which said solvent is composed of more than 95% water (H 2 0) by weight and preferably more than 99% by weight water.
• a plurality of said suspensions are sprayed simultaneously on said substrate.
• the nano- / microparticles of the deposition process are chosen from carbon nanotubes, carbon nanowires, carbon nanotypes, carbon nanocornes, carbon onions and a mixture of these nanoparticles / microparticles, in which said nano / microparticles are oxidized prior to spraying and wherein said deposition is annealed after said spraying at a temperature sufficient to deoxidize said nano / microparticles.
• At least one said wet nanoparticle is oxidized with at least one element selected from sulfuric acid, acid and phosphoric acid, sodium nitrate, nitric acid, potassium permanganate and hydrogen peroxide.
• a heating element placed in contact with a support heats said substrate and each said part of said sprayed suspension on said substrate.
• said deposit is annealed at a temperature between 200 degrees Celsius and 400 degrees Celsius.
• the invention also relates to a method for manufacturing an electrode comprising in superposition a deposition of nano- / microparticles and a substrate, said substrate comprising a current collector and said deposition of nano- / microparticles being obtained by a deposition method described. previously.
• the present invention also relates to an electrode of which said nano- / microparticle deposition can be obtained by a method described above.
• said deposition of the electrode comprises at least graphene and a type of said nano- / microparticles chosen from carbon nanotubes, carbon nanowires, carbon nanotubes, carbon nanocornes and carbon onions.
• the present invention also relates to a supercapacitor comprising at least one said electrode described above.
• nanoparticle is understood to mean particles of which at least the smallest of the dimensions is nanometric, that is to say between 0.1 nm and 100 nm.
• microparticle is meant particles of which at least the smallest of the dimensions is micrometric, that is to say between 0.1 ⁇ and 100 ⁇ .
• Nano- / microparticle geometries include nano- / microfilts, nano- / microtiges, nano- / microtubes, nano- / microcornes, nano- / micro onions, and monofilament-type nano- / microfeuilles comprising a layer. crystalline or multifile comprising several stacked leaflets.
• a nano- / microtube is formed of one or more wound nano- / microfossils.
• a nano- / microfil is a one-dimensional object full of massive material.
• a nano- / microtige is a hollow one-dimensional object.
• a sheet is designated by the term “graphene” and is in the form of a two-dimensional carbon crystal of monoatomic thickness and nano- / micrometric size.
• the carbon nanotubes are known and formed of a sheet of graphene wound into a tube (designated by the acronym of "Single Wall Carbon NanoTube", SWCNT) or several stacked sheets of graphene wound into a tube (designated by the acronym for "Multi Wall Carbon NanoTube", MWCNT).
• electrode an assembly comprising a deposition of nanoparticles / microparticles on a substrate (comprising a current collector which leads electrically and optionally a layer or a thick material for the mechanical strength of the electrode).
• FIG. 1 is a schematic representation of an apparatus for producing nano- / microparticle deposition according to a method according to the invention
• Figure 2 is a schematic representation of two deposits of nano- / microparticles and the electrolyte of a supercapacitor;
• Figure 3 is a schematic representation illustrating a particular embodiment of a method according to the invention.
• FIG. 4 is a photograph taken by a scanning electron microscope of the structure of the material of a nanoparticle / microparticle deposit produced by a method according to the invention
• FIG. 5 is a photograph taken by a scanning electron microscope of the material structure of a nano- / microparticle deposit produced according to a process according to the invention.
• FIG. 6 is a photograph taken by a scanning electron microscope of the structure of the material of a nano-microparticle deposit produced according to a method according to the invention.
• FIG. 7 presents cyclic voltammograms obtained from deposits of nanoparticles / microparticles of different compositions
• FIG. 8 illustrates the influence of the cycling rate on the nano- / microparticle deposit capacity of different compositions
• FIG. 9 illustrates the value of the specific capacity and the energy density of an electrode as a function of the proportion of oxidized carbon nanotubes in the pulverized suspension.
• Figure 1 is a schematic representation of an apparatus 3 for producing nano- / microparticle deposition according to a method according to the invention.
• the apparatus 3 comprises a spray nozzle 4, a reservoir 5 containing a suspension of nano / microparticles and a source of spray gas 6.
• the nano- / microparticles comprise oxidized graphene particles and may comprise, in particular embodiments of the invention, oxidized carbon nanotubes, oxidized carbon nanowires, nanotubes oxidized carbon, oxidized carbon nanocornes and oxidized carbon onions. Other nanoparticles are conceivable.
• the solvent used for the suspension may advantageously be composed of more than 95% of water (H 2 O) and even more advantageously of more than 99% water (H 2 O).
• the water may be mixed with other solvents, in proportions that allow them to remain miscible with water, such as methanol (CH 4 0), ethanol (C 2 H 6 O), ethylene chloride (DCE), dichlorobenzidine (DCB), N-methyl-2-pyrrolidone (NMP), dimethylformamide (DMF), hexamethylphosphoramide (HMPA), cyclopentanone (C 5 H 8 O), tetramethylene sulfoxide (TMSO), ⁇ -caprolactone, 1,2-dichlorobenzene, 1,2-dimethylbenzene, bromobenzene, lodobenzene and toluene.
• Other compounds are conceivable.
• the sputtering gas is, for example, air.
• the nozzle 4 is supplied with suspension from the tank 5 and spray gas from the source 6.
• the nozzle 4 is suitable for spraying the suspension, fed at low pressure, in microdroplets using the gas supplied at high pressure.
• the nozzle 4 is of the airbrush type. The drops are created by hydrodynamic instability between the liquid phase, the gaseous phase and the nozzle 4, that is, in a particular embodiment of the invention, sprayed by the effect of the pressure imposed on water, air and water. geometry of the nozzle.
• microdroplets drops of microscopic size, whose diameter is between about 1 and 100 microns.
• the apparatus 3 comprises heating elements 7 of the support 8 in the form of resistive heating elements 9, connected to a power supply circuit (not shown) so that the elements Resistive heating elements 9 emit heat by the Joule effect when an electric current passes through them.
• the apparatus 3 comprises heating elements 7 of the support 8 by induction, comprising for example a plate on which the support 8 is placed with inductors, to induce currents in the plate and generate heat.
• the apparatus 3 comprises a temperature sensor 10 arranged to measure the temperature of the support 8.
• the nozzle 4 In operation, the nozzle 4 generates a spray jet 1 1 formed of suspension microdroplets projected towards the surface 12 to be covered with substrate 15.
• the spray jet 1 1 reaches the surface 12 to be covered in an impact zone 13, the shape and dimensions of which depend in particular on the geometry of the nozzle 4, the adjustment of the nozzle 4 and the position of the nozzle. the nozzle 4 relative to the surface 12 to be covered.
• the shape and the dimensions of the impact zone 13 depend in particular on the angle ⁇ at the apex of the cone formed by the spray jet 1 1 at the outlet of the nozzle 4 and the distance between the outlet of the nozzle 4 and the nozzle. surface 12 of the substrate 15. They also depend on the pressure of the sputtering gas (related to the spraying gas flow rate) and the flow rate of each suspension.
• the spray jet 1 1 is for example conical of revolution, so that it forms an impact zone 13 of generally circular shape.
• the spray jet 1 1 could define an oblong impact zone 13, more elongated in a first direction than in a second direction perpendicular to the first.
• Figure 2 is a schematic representation of two deposits of nano- / microparticles 1 and the electrolyte 2 of a supercapacitor.
• the storage of the energy is carried out by a non-homogeneous distribution of the ions of the electrolyte 2 in the vicinity of the surface of each deposit of nano- / microparticles 1.
• several ionic layers may be formed in the vicinity of the surface of the deposits of nano- / microparticles 1 and have a thickness of the order of a few nanometers, depending on the electrolyte 2 considered and its concentration.
• the origin of these layers is electrostatic. This process does not involve electrochemical transformation of the material as in the case of accumulators.
• Figure 2 illustrates the importance of developing materials with very large specific surfaces and having porosity adapted to ion storage at this scale to increase the storage capacity of supercapacitors.
• the nano- / microparticles used to form a deposit 1 may be graphene sheets and single-walled carbon nanotubes (SWCNT).
• Figure 3 is a schematic representation illustrating a particular embodiment of a method according to the invention. It illustrates the formation of one or more deposits of nanoparticles 1 made on a substrate 15 (having a current collector, conductive and optionally a thick layer for its mechanical strength) superimposed with the support.
• the carbon nanoparticles / nanoparticles are oxidized.
• the carbon nanoparticles / nanoparticles are, for example, SWCNTs.
• SWCNTs are dispersed in an equal volume mixture of sulfuric acid and nitric acid for 30 minutes. The mixture is then refluxed for 3 hours. The SWCNTs are then oxidized. They can be recovered by vacuum filtering the mixture and washing with several hundred milliliters of water until a neutral pH of the filtrate. The product is dried under vacuum at 70 ° C for several days.
• the graphene oxide particles can be obtained commercially.
• a second step it is possible to prepare suspensions of each of the different particles in deionized water by sonication for one hour, at a concentration of between 5 ⁇ g.mL -1 and 50 mg ml -1 and preferably between 50 ⁇ g.mL "1 and 5 mg.mL " 1 .
• the various suspensions can then be combined into a single suspension and the suspension sonicated for one hour.
• the nano- / microparticles are deposited on the current collector of the substrate 15.
• the deposition is carried out by spraying by hydrodynamic instability of the suspension, on a substrate 15 heated to a temperature preferably greater than 100 ° C. and preferentially less than or equal to 200 ° C, or even 150 ° C: the temperature must be sufficient to allow rapid evaporation of drops deposited by spraying and thus avoid the effect "coffee stain", that is to say, a surface distribution nano- / microparticles adsorbed non-homogeneous.
• a temperature too high such as that presented in the method presented by Youn et al.
• the method of Youn et al. requires the use of a high suspension volume for to compensate for the total evaporation induced by a high temperature of a high proportion of the pulverized suspension.
• the deposit 1 is annealed at a temperature above 200 ° C to deploy the accessible surfaces of the electrolyte 2 in the deposition of nano- / microparticles 1, reduce or deoxidize graphene oxide and oxidized nanotubes and increase the conductivity of the deposition of nano- / microparticles 1.
• This step is necessary because the deposition temperature is too low to reduce or deoxidize the nano- / microparticles of the deposit 1.
• This step has two distinct advantages over the process presented by Youn et al .: on the one hand, annealing allows the nano / microparticles to be deoxidized at an effective temperature while keeping a lower temperature during the spraying (and the advantages which are linked to and presented in the previous paragraph).
• annealing can be done in a controlled manner, for example by imposing an equal annealing time for all the particles deposited.
• annealing time for all the particles deposited.
• FIGS. 4, 5 and 6 are photographs taken by a scanning electron microscope of the material structure of a nano-microparticle deposit 1 made according to a method according to the invention. They illustrate the hierarchical structure whose production is described above: the nanotubes of oxidized carbons are interposed between the layers of oxidized graphene. The homogeneous distribution of the two structures is already potentially initiated in the suspension before spraying, via possible esterifications between the hydroxyl and carboxylic groups of each of the two oxidized carbonaceous structures. In a particular and different embodiment of the invention, other oxidized carbonaceous structures may be introduced into the suspension such as carbon nanowires, carbon nanotubes, carbon nanocornes and carbon onions.
• FIG. 7 presents cyclic voltammograms obtained from nanoparticles / microparticle deposits 1 of different compositions.
• the various measurements are carried out at a scanning speed of 20 mV.s -1 , in a three-electrode arrangement: the electrode comprising a nano-microparticle deposit 1, an Ag / AgCl electrode and a LiNO 3 to 3 electrode.
• the curve (a) corresponds to a nano- / microparticle deposit obtained according to a process of the invention using oxidized graphene nanoparticles / microparticles.
• the curve (b) corresponds to a nano-microparticle deposit 1 obtained.
• the curve (c) corresponds to a deposition of nano- / microparticles 1 obtained using nanotubes
• the curve (d) corresponds to a deposition of nano- / microparticles 1 obtained using nano- / microparticles of graphene and pulverized carbon nanotubes (unoxidized materials in the meadow). alable, suspended in an NMP solvent)
• the curve (e) corresponds to a deposition of nano- / microparticles 1 made of disordered carpet or "bucky paper" of carbon nanotubes and graphene in mass proportion of 50% / 50% .
• FIG. 7 The rectangular shape of the various cyclic voltammograms of FIG. 7 illustrates the capacitance of the different electrodes measured.
• Figure 7 further illustrates an increase in measured current density when nano- / microparticle 1 deposits are made from oxidized nano- / microparticles (curves (a), (b) and (c)).
• FIG. 8 illustrates the influence of the cycling speed on the specific capacitance of electrodes covered with a deposit of nano-microparticles 1 of different compositions.
• Curve (f) corresponds to a deposition of nano-microparticles 1 obtained according to a process of the invention using oxidized graphene nanoparticles / microparticles and oxidized SWCNTs, in a mass proportion of 25% / 75% respectively and pulverized. on a substrate heated to 200 ° C. Heating the substrate at 170 ° C gives similar results.
• Curve (g) corresponds to a deposition of nano- / microparticles 1 obtained according to a method of the invention using oxidized nano- / microparticles of graphene
• curve (h) corresponds to a deposition of nano- / microparticles 1 obtained by spraying oxidized SWCNT
• curve (i) corresponds to a deposit of nano- / microparticles 1 based on "bucky paper” with SWCNT
• the curve (j) corresponds to a deposit of nano- / microparticles 1 made from activated carbon paste (as in conventional supercapacitors)
• the curve (k) corresponds to a deposit of nano- / microparticles based on "bucky paper” with a mixture of oxidized nano- / microparticles of graphene and oxidized SWCNTs.
• FIG. 8 illustrates that among the nanoparticle deposits 1 produced by sputtering, the specific capacitances of the electrodes obtained according to a method of the invention are higher than those of the electrode manufactured with deposits 1 of SWCNT. oxidized (alone).
• curve (f) shows the interest of an interaction between oxidized nano- / microparticles of graphene and oxidized SWCNT to keep a high specific capacity even at high cycling speed.
• curve (f) illustrates that the interaction between oxidized graphene nano- / microparticles and oxidized SWCNT makes it possible to keep relatively stationary specific capacitance values.
• FIG. 9 illustrates the value of the specific capacitance and energy density of an electrode as a function of the proportion of oxidized SWCNTs in the pulverized suspension, when using an electrode obtained according to a method of FIG. using oxidized graphene nano- / microparticles and oxidized SWCNTs.
• the specific capacity and the energy density are optimal for a mass proportion of SWCNT between 0 and 25%.

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• 2015
  • 2015-02-06 FR FR1500231A patent/FR3032362B1/fr active Active
• 2016
  • 2016-02-05 JP JP2017541337A patent/JP2018508992A/ja active Pending
  • 2016-02-05 AU AU2016214292A patent/AU2016214292A1/en not_active Abandoned
  • 2016-02-05 EP EP16706982.2A patent/EP3254292A1/fr not_active Withdrawn
  • 2016-02-05 KR KR1020177024642A patent/KR20170116066A/ko not_active Application Discontinuation
  • 2016-02-05 US US15/548,710 patent/US20180025853A1/en not_active Abandoned
  • 2016-02-05 WO PCT/EP2016/052541 patent/WO2016124756A1/fr active Application Filing
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