CN114429866A - Planar filtering electrochemical capacitor and preparation method thereof - Google Patents

Planar filtering electrochemical capacitor and preparation method thereof Download PDF

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CN114429866A
CN114429866A CN202210125591.XA CN202210125591A CN114429866A CN 114429866 A CN114429866 A CN 114429866A CN 202210125591 A CN202210125591 A CN 202210125591A CN 114429866 A CN114429866 A CN 114429866A
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cobalt
manganese
electrochemical capacitor
electrode
nickel
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CN114429866B (en
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汤海潮
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Hangzhou Maoang Technology Co ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/26Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a planar filtering electrochemical capacitor and a preparation method thereof. The filtering electrochemical capacitor sequentially comprises an upper packaging shell, a first electrode, an electrolyte, a diaphragm, a second electrode and a lower packaging shell. The first electrode and the second electrode are two identical symmetrical electrodes, and each electrode comprises an active material layer and a metal layer, wherein the active material layer is preferably a compound containing nickel, cobalt and manganese, and the metal layer is preferably a nickel foil; the electrolyte is preferably KOH or K2SO4An electrolyte; the separator is preferably filter paper or a polypropylene porous membrane. The invention also provides two filtering electrochemical capacitors of cobalt-manganese co-doped nickel telluride and cobalt-manganese co-doped nickel selenate, and provides specific structural characteristics of electrode materials and specific structural characteristics of the electrode materialsA preparation method and a performance index of a corresponding filtering electrochemical capacitor. The filtering electrochemical capacitor provided by the invention can obtain excellent filtering performance at low frequency, and has the advantages of high specific capacitance, simple preparation method, low resistance, low cost and the like.

Description

Planar filtering electrochemical capacitor and preparation method thereof
Technical Field
The invention relates to the field of filter capacitors, in particular to a filter electrochemical capacitor used in the low-frequency field of commercial power and the like.
Background
The filter capacitor is a commonly used circuit energy storage device, is generally arranged at two ends of a rectifying circuit and is used for reducing alternating current ripple coefficients and simultaneously smoothing direct current output efficiently. The filter capacitor is further classified into a low frequency filter capacitor and a high frequency filter capacitor according to its application in different working environments. The low-frequency filter capacitor is mainly applied to circuits under lower frequency, such as commercial power filter and filter after transformer rectification, the working frequency of the low-frequency filter capacitor is consistent with that of commercial power, and the working frequency of the low-frequency filter capacitor is generally 50 Hz domestically; the high frequency filter capacitor is mostly used in the switch circuit, and its working frequency can reach tens of thousands of hertz.
The filter capacitor has the characteristics of low temperature rise, low loss, high safety and the like, and simultaneously requires larger energy storage capacitance, and most of the filter capacitors use aluminum electrolytic capacitors at present. As a filter capacitor generally used at present, the capacity of an electrolytic capacitor is not sufficient, although it is already much larger than that of a conventional ceramic capacitor. In many occasions requiring large-capacity filtering, a plurality of electrolytic capacitors need to be connected in series to meet the filtering requirement, so that the resistance of the whole circuit system is greatly increased, a large amount of energy loss is caused, and a large amount of space is occupied.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention aims to provide a planar Filtering Electrochemical Capacitor (FEC) and a method for manufacturing the same, wherein the Filtering Electrochemical Capacitor (FEC) obtains a high energy storage through a reversible chemical adsorption/desorption or faraday oxidation-reduction process of an active material, has a capacitance which is thousands of times higher than that of a conventional electrolytic capacitor, has the advantages of excellent power characteristics, high safety and the like, is applied to the field of filtering capacitors, has a working frequency which can meet the requirement of 50 hz commercial power in China, and can be used as a low-frequency filtering capacitor device such as the commercial power.
In order to achieve the purpose, the invention adopts the following technical scheme.
The invention provides a planar filtering electrochemical capacitor and a preparation method thereof. The filtering electrochemical capacitor sequentially comprises an upper packaging shell, a first electrode, an electrolyte, a diaphragm, a second electrode and a lower packaging shell; after the packaging is finished, standing for not less than 24 hours at room temperature, then placing the obtained product in a heat treatment furnace, and statically heating for 3-5 hours at the temperature of 50-70 ℃ in an atmospheric environment.
In the filtering electrochemical capacitor, the first electrode and the second electrode are two identical symmetrical electrodes, each of which comprises an active material layer and a metal layer, and the active material layer is coated on the metal layer; the active material layer is preferably a nickel-cobalt-manganese-containing compound; the metal layer is preferably a nickel foil.
In the filtering electrochemical capacitor, the electrolyte is preferably KOH or K2SO4The electrolyte and the separator are preferably filter paper or polypropylene porous membrane.
In the filtering electrochemical capacitor, the nickel-cobalt-manganese-containing compound is preferably cobalt-manganese co-doped nickel telluride (NiTe)2CoMn) or Co-Mn co-doped nickel selenate (NiSeO)3:CoMn)。
The cobalt-manganese codoped nickel telluride (NiTe)2CoMn) is in the shape of a nanocube, the side length of the nanocube is 500-900 nm, the surface of the nanocube is in a two-stage nanosheet structure, and the nanosheets are criss-cross to form a network structure of a three-dimensional nanowall, which is expressed as a porous nanomaterial; in NiTe2The atomic percentage of Ni, Co and Mn in CoMn is about 80:10: 10. The appearance is very beneficial to the infiltration and permeation of electrolyte and the rapid diffusion and transfer of ions and electrons, thereby being beneficial to the rapid response of the filtering performance.
The NiTe2The CoMn nano material is prepared by the following typical preparation process: weighing 0.8mmol of nickel nitrate, 0.1mmol of cobalt nitrate, 0.1mmol of manganese nitrate, 2.0mmol of Te powder and 3.0mL of hydrazine hydrate (80%), dissolving in 40mL of deionized water to form a solution, transferring to a 50mL of polytetrafluoroethylene high-pressure reaction kettle, and magnetically stirring for 12-17 minutes to form a suspension; putting the mixture into a drying oven, heating the mixture to 180 ℃, and reacting for 12 hours; after the reaction is finished, taking out the high-pressure kettle, naturally cooling to room temperature to obtain reaction products, and washing with deionized water and ethanol for 3 times respectively; placing the mixture in a drying oven, and drying the mixture for 5 to 7 hours at the temperature of 60 ℃ to obtain NiTe2Namely a CoMn nano material.
The cobalt and manganese codoped nickel selenate (NiSeO)3CoMn) is a micron granular material with a grain size of 9-15 μm, and each micron grainFrom NiSeO3The CoMn two-dimensional laminated structure is formed by stacking CoMn two-dimensional laminated layers, the thickness of each layer is 30-70 nm, and gaps among the layers are uniform and are of a two-dimensional laminated structure; in NiSeO3The atomic percentage of Ni, Co and Mn in CoMn is about 90:5: 5. The abundant two-dimensional layered structure has high specific surface area, can enable electrolyte to be fully contacted and infiltrated with materials, provides a large number of active sites for ion adsorption/desorption and embedding/desorption, and is also beneficial to rapid diffusion and transfer of ions and electrons, thereby being beneficial to rapid response of filtering performance.
The cobalt and manganese codoped nickel selenate (NiSeO)3CoMn), the typical preparation process is as follows: weighing 0.9mmol of nickel acetate, 0.05mmol of cobalt acetate, 0.05mmol of manganese acetate, 1.0mmol of selenium dioxide and 0.50g of PVP, and dissolving in 40mL of deionized water to form a solution; transferring the mixture into a 50mL polytetrafluoroethylene high-pressure reaction kettle, and magnetically stirring for 13-18 minutes; putting the high-pressure reaction kettle into an oven, heating to 190 ℃, and reacting for 14-16 hours; after the reaction is finished, taking out the high-pressure kettle, and naturally cooling to room temperature; pouring out supernatant, transferring bottom turbid solid into a centrifuge tube, and respectively centrifugally washing 3 times by using deionized water and ethanol as solvents; and drying the obtained precipitate at 50-70 ℃ for 5-7 hours to obtain the nickel selenate powder.
The beneficial results of the invention are as follows:
1) the filtering electrochemical capacitor provided by the invention adopts symmetrical electrodes, has the advantages of simple structure, small volume, compatibility with the existing industrial system, low production cost and low equipment capital investment, and is suitable for large-scale industrial production.
2) The filtering electrochemical capacitor can provide a large specific capacitance which is 3 orders of magnitude larger than that of the existing electrolytic capacitor, so that the application quantity requirement of the capacitor in a circuit can be greatly reduced, the system resistance is reduced, the energy loss is reduced, and the space occupation ratio is obviously saved.
3) Compared with the existing electrolytic capacitor, the filtering electrochemical capacitor has more excellent filtering performance, large capacity, high safety and low leakage current, can replace the electrolytic capacitor in a circuit system with lower frequency, and can be widely applied.
4) The filtering electrochemical capacitor is flat, has a two-dimensional shape and a small volume, can be applied to the field of devices such as solid-state electronics, flexible electronics, transparent electronics and the like, is easy to combine and integrate, and is suitable for products such as miniaturization, portability, intellectualization, mobility and the like.
5) The filtering electrochemical capacitor has filtering performance, high specific capacitance and two advantages of filtering and energy storage, can be applied to the field of green energy such as solar energy, wind energy and tidal energy, provides a composite function of energy storage and filtering in an intermittent or unstable energy power generation system, and is particularly suitable for electric power systems such as mains supply and the like which need high-capacity filtering.
Drawings
Fig. 1 is a schematic diagram of the internal structure of a planar filtering electrochemical capacitor according to the present invention.
FIG. 2 shows cobalt manganese co-doped nickel telluride (NiTe) prepared in example 12CoMn) in the SEM images.
FIG. 3 shows NiTe obtained in example 12The CoMn filtered electrochemical capacitor impedance spectrum Bode curve.
Fig. 4 is a schematic diagram of a rectifying circuit of the planar filtering electrochemical capacitor manufactured by the present invention in practical application.
FIG. 5 is a filter pattern formed by the application of the filtering electrochemical capacitor of the present invention in a rectifier circuit.
FIG. 6 shows Co-Mn-codoped nickel selenate (NiSeO) prepared in example 23CoMn) in the SEM images.
FIG. 7 shows NiSeO obtained in example 23The CoMn filtered electrochemical capacitor impedance spectrum Bode curve.
Detailed Description
The following examples are given by way of illustration.
Example 1
Planar Co-Mn-Co-doped Nickel telluride (NiTe)2CoMn) filtering electrochemical capacitor, which comprises an upper packaging shell, a first electrode, an electrolyte, a diaphragm, a second electrode and a lower packaging shell in sequence; after the encapsulation is finished, standing at room temperatureAnd (3) placing the mixture for not less than 24 hours, then placing the mixture in a heat treatment furnace, and statically heating the mixture for 3 to 5 hours at the temperature of 50 to 70 ℃ in an atmospheric environment. The first electrode and the second electrode are two identical symmetrical electrodes, nanometer NiTe2The CoMn active material is coated on the nickel foil metal layer, the electrolyte is KOH electrolyte, and the diaphragm is filter paper.
The cobalt and manganese codoped nickel telluride (NiTe)2CoMn) in the shape of a nanocube, wherein the side length of the nanocube is 500-900 nm, the surface of the nanocube is in a two-stage nanosheet structure, and the nanosheets are criss-crossed to form a network structure of a three-dimensional nanowall, which is expressed as a porous nanomaterial; in NiTe2The atomic percentage of Ni, Co and Mn in CoMn is about 80:10: 10. The appearance is very beneficial to the infiltration and permeation of electrolyte and the rapid diffusion and transfer of ions and electrons, thereby being beneficial to the rapid response of the filtering performance.
The NiTe2The CoMn nano material is prepared by the following typical preparation process: weighing 0.8mmol of nickel nitrate, 0.1mmol of cobalt nitrate, 0.1mmol of manganese nitrate, 2.0mmol of Te powder and 3.0mL of hydrazine hydrate (80%), dissolving in 40mL of deionized water to form a solution, transferring to a 50mL of polytetrafluoroethylene high-pressure reaction kettle, and magnetically stirring for 12-17 minutes to form a suspension; putting the mixture into a drying oven, heating the mixture to 180 ℃, and reacting for 12 hours; after the reaction is finished, taking out the high-pressure kettle, naturally cooling to room temperature to obtain reaction products, and washing with deionized water and ethanol for 3 times respectively; placing the mixture in a drying oven, and drying the mixture for 5 to 7 hours at the temperature of 60 ℃ to obtain NiTe2Namely a CoMn nano material.
The nickel telluride/nickel screen electrode prepared under the above conditions has substantially consistent physicochemical properties. The sample is subjected to X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and X-ray energy scattering spectroscopy (EDX) tests, and the product is NiTe2The phase structure, Ni, Co, Mn in atomic percent is about 8:1: 1. Fig. 1 is a schematic structural diagram of a planar filtering electrochemical capacitor. FIG. 2 shows the resulting NiTe2Typical SEM images of CoMn nanomaterials.
As shown in FIG. 1, a planar NiTe is assembled2CoMn filter electrochemical capacitorA device. And carrying out electrochemical performance tests on the assembled filtering electrochemical capacitor, wherein the electrochemical performance tests comprise constant current charging and discharging (GCD), Cyclic Voltammetry (CV) and impedance spectroscopy (EIS) tests. Fig. 3 is a typical impedance spectrum Bode curve derived from EIS data, where the larger the corresponding negative phase angle is at a fixed frequency, the stronger the capacitance characteristic is, where 45 ° is a key boundary for distinguishing the capacitance and the resistance of the device, and the negative phase angle corresponding to the filtering electrochemical capacitor is 67.5 ° at 120hz (dual grid frequency, such as 60hz in the united states), and 70.4 ° at 100 hz (dual grid frequency, such as 50 hz in china), which means that the filtering electrochemical capacitor can be fully applied to solve the filtering problem in the actual grid circuit.
The capacitance values under different alternating current frequencies can be calculated according to EIS data, and the specific area capacitance reaches 957 mu F cm under the characteristic frequency of 120Hz-2(much larger than 300. mu.F cm for commercial aluminum electrolytic capacitors-2Specific area capacitance). The relevant performance indexes are shown in attached table 1.
Fig. 4 is a schematic diagram of a rectifier circuit in practical application. NiTe obtained in example 12A CoMn filtering electrochemical capacitor is installed in a rectifying circuit shown in figure 4, a filtering graph shown in figure 5 is obtained through output voltage, a rectifying module consisting of 4 diodes converts a 60Hz bidirectional sine alternating current input signal into a 120Hz unidirectional sine alternating current signal (the voltage drop inherent to the diodes is inevitable, and signals before and after rectification have certain voltage loss), and the rectified unidirectional sine alternating current signal passes through NiTe2The CoMn filtering electrochemical capacitor is converted into a direct current signal to complete the whole alternating current-direct current conversion process.
Example 2
Planar Co-Mn Co-doped Nickel selenate (NiSeO)3CoMn) filtering electrochemical capacitor, which comprises an upper packaging shell, a first electrode, an electrolyte, a diaphragm, a second electrode and a lower packaging shell in sequence; after the packaging is finished, standing for not less than 24 hours at room temperature, then placing the obtained product in a heat treatment furnace, and statically heating for 3-5 hours at the temperature of 50-70 ℃ in an atmospheric environment. The first electrode and the second electrode are two identical symmetrical electrodes of nano NiSeO3CoMn active material is coated on the nickel foil metal layer, and the electrolyte is K2SO4Electrolyte and the diaphragm are polypropylene porous membranes.
The cobalt and manganese codoped nickel selenate (NiSeO)3CoMn) is a micron granular material with the grain size of 9-15 mu m, and each micron grain is made of NiSeO3The CoMn two-dimensional laminated structure is formed by stacking CoMn two-dimensional laminated layers, the thickness of each layer is 30-70 nm, and gaps among the layers are uniform and are of a two-dimensional laminated structure; in NiSeO3The atomic percentage of Ni, Co and Mn in CoMn is about 90:5: 5. The abundant two-dimensional layered structure has high specific surface area, can enable electrolyte to be fully contacted and infiltrated with materials, provides a large number of active sites for ion adsorption/desorption and embedding/desorption, and is also beneficial to rapid diffusion and transfer of ions and electrons, thereby being beneficial to rapid response of filtering performance.
The cobalt and manganese codoped nickel selenate (NiSeO)3CoMn), the typical preparation process is as follows: weighing 0.9mmol of nickel acetate, 0.05mmol of cobalt acetate, 0.05mmol of manganese acetate, 1.0mmol of selenium dioxide and 0.50g of PVP, and dissolving in 40mL of deionized water to form a solution; transferring the mixture into a 50mL polytetrafluoroethylene high-pressure reaction kettle, and magnetically stirring for 13-18 minutes; putting the high-pressure reaction kettle into an oven, heating to 190 ℃, and reacting for 14-16 hours; after the reaction is finished, taking out the high-pressure kettle, and naturally cooling to room temperature; pouring out supernatant, transferring bottom turbid solid into a centrifuge tube, and respectively centrifugally washing 3 times by using deionized water and ethanol as solvents; and drying the obtained precipitate at 50-70 ℃ for 5-7 hours to obtain the nickel selenate powder.
The nickel telluride/nickel screen electrode prepared under the above conditions has substantially consistent physicochemical properties. The sample is subjected to x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS) and x-ray energy scattering spectroscopy (EDX) tests, and the product is NiSeO3The phase structure, Ni, Co, Mn in atomic percent is about 90:5: 5. FIG. 6 shows the resulting NiSeO3Typical SEM image of CoMn nano material.
As shown in FIG. 1, a NiSeO of a flat type was assembled3A CoMn filter electrochemical capacitor. The assembled filtering electrochemical capacitor is carried outAnd electrochemical performance tests comprise constant current charging and discharging (GCD), Cyclic Voltammetry (CV) and impedance spectroscopy (EIS) tests. Fig. 7 is a typical Bode curve of impedance spectrum, derived from EIS data, the larger the corresponding negative phase angle at a fixed frequency, the stronger the capacitance characteristic, where 45 ° is a key boundary for distinguishing the capacitance and the resistance of the device, and the negative phase angle corresponding to the filtering electrochemical capacitor is 70.1 ° at 120hz (dual grid frequency, e.g., 60hz in the united states), and 72.9 ° at 100 hz (dual grid frequency, e.g., 50 hz in china), which means that the filtering electrochemical capacitor can be fully applied to solve the filtering problem in the actual grid circuit.
According to EIS data, the capacitance values under different alternating frequencies can be calculated, and under the characteristic frequency of 120Hz, the specific area capacitance reaches 1215 mu F cm-2(much larger than 300. mu.F cm for commercial aluminum electrolytic capacitors-2Specific area capacitance). The relevant performance indexes are shown in attached table 1.
NiSeO obtained in example 23When the CoMn filter electrochemical capacitor is installed in the rectifying circuit shown in the attached figure 4, a filter pattern similar to that shown in the attached figure 5 can be obtained, and the whole alternating current-direct current conversion process is realized.

Claims (10)

1. A planar filtering electrochemical capacitor, comprising: the filtering electrochemical capacitor sequentially comprises an upper packaging shell, a first electrode, an electrolyte, a diaphragm, a second electrode and a lower packaging shell; the first electrode and the second electrode are two identical symmetrical electrodes, and each electrode consists of an active material layer and a metal layer, and the active material layer is coated on the metal layer; the active material layer is a compound containing nickel, cobalt and manganese; the metal layer is nickel foil.
2. The planar filtering electrochemical capacitor according to claim 1, wherein: the compound containing nickel, cobalt and manganese is cobalt and manganese co-doped nickel telluride (NiTe)2:CoMn。
3. The planar filtering electrochemical capacitor according to claim 2, wherein: the cobalt-manganese co-doped nickel telluride is a porous nano material, the micro appearance of the cobalt-manganese co-doped nickel telluride is nano cube appearance, the side length of the nano cube is 500-900 nm, the surface of the nano cube is of a two-stage nanosheet structure, and the nanosheets are criss-cross to form a network structure of a three-dimensional nanowall.
4. The planar filtering electrochemical capacitor according to claim 3, wherein: in the cobalt-manganese Co-doped nickel telluride, the atomic percentage of Ni to Co to Mn is 80 to 10.
5. The planar filtering electrochemical capacitor according to claim 1, wherein: the compound containing nickel, cobalt and manganese is a cobalt and manganese co-doped nickel selenate (NiSeO)3:CoMn。
6. The planar filtering electrochemical capacitor according to claim 5, wherein: the cobalt-manganese co-doped nickel selenate is a micron granular material, the particle size is 9-15 microns, each micron particle is formed by stacking NiSeO3: CoMn two-dimensional sheets, the thickness of each layer is 30-70 nm, gaps among the layers are uniform, and the two-dimensional layered structure is formed.
7. The planar filtering electrochemical capacitor according to claim 6, wherein: in the cobalt-manganese Co-doped nickel selenate, the atomic percentage of Ni, Co and Mn is 90:5: 5.
8. The planar filtering electrochemical capacitor according to claim 1, wherein: the electrolyte is KOH or K2SO4An electrolyte; the diaphragm is filter paper or a polypropylene porous membrane.
9. The method for preparing the planar filtering electrochemical capacitor according to claim 4, wherein the cobalt-manganese co-doped nickel telluride is prepared by the following steps: 0.8mmol of nickel nitrate, 0.1mmol of cobalt nitrate, 0.1mmol of manganese nitrate, 2.0mmol of Te powder and 3.0mL of 80% hydrazine hydrate are dissolved in 40mL of deionized water to form a solutionTransferring the solution into a polytetrafluoroethylene high-pressure reaction kettle, and stirring to form a suspension; putting the mixture into a drying oven, heating the mixture to 180 ℃, and reacting for 12 hours; after the reaction is finished, taking out, naturally cooling to room temperature to obtain a reaction product, and washing with deionized water and ethanol for multiple times respectively; placing the mixture in a drying oven, and drying the mixture for 5 to 7 hours at the temperature of 60 ℃ to obtain the NiTe2Nano material of CoMn.
10. The planar filtering electrochemical capacitor according to claim 7, wherein the cobalt-manganese co-doped nickel selenate is prepared by the following steps: dissolving 0.9mmol of nickel acetate, 0.05mmol of cobalt acetate, 0.05mmol of manganese acetate, 1.0mmol of selenium dioxide and 0.50g of PVP in 40mL of deionized water to form a solution; transferring the mixture into a polytetrafluoroethylene high-pressure reaction kettle, and stirring; putting the high-pressure reaction kettle into an oven, heating to 190 ℃, and reacting for 14-16 hours; after the reaction is finished, taking out the reaction product, and naturally cooling the reaction product to room temperature; pouring out supernatant liquid, transferring bottom turbid solid into a centrifuge tube, and respectively centrifugally washing for multiple times by using deionized water and ethanol as solvents; and drying the obtained precipitate at 50-70 ℃ for 5-7 hours to obtain the cobalt-manganese co-doped nickel selenate powder.
CN202210125591.XA 2022-02-10 2022-02-10 Planar filter electrochemical capacitor and preparation method thereof Active CN114429866B (en)

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CN1384047A (en) * 2002-06-07 2002-12-11 清华大学 Synthesis of several metal selenides and tellurides as semiconductor material
CN103208373A (en) * 2012-01-16 2013-07-17 清华大学 Grapheme electrode and preparation method and application thereof
CN106910639A (en) * 2017-03-20 2017-06-30 浙江大学 A kind of NiTe for electrode material for super capacitor2Preparation method
CN108292608A (en) * 2015-11-23 2018-07-17 纳米技术仪器公司 Electrode of super capacitor and battery core with high activity mass loading amount
CN110767462A (en) * 2019-11-07 2020-02-07 北京化工大学 Bimetal nickel-cobalt telluride supercapacitor electrode material and preparation method thereof
CN110844946A (en) * 2019-11-19 2020-02-28 上海季丰电子股份有限公司 Metastable crystal material and preparation method thereof
CN111769276A (en) * 2020-06-01 2020-10-13 上海海事大学 Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application
CN113023665A (en) * 2021-03-05 2021-06-25 浙江理工大学 Carbon fiber cloth loaded nano needle-shaped nickel-cobalt double-metal selenide crystal array film and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1384047A (en) * 2002-06-07 2002-12-11 清华大学 Synthesis of several metal selenides and tellurides as semiconductor material
CN103208373A (en) * 2012-01-16 2013-07-17 清华大学 Grapheme electrode and preparation method and application thereof
CN108292608A (en) * 2015-11-23 2018-07-17 纳米技术仪器公司 Electrode of super capacitor and battery core with high activity mass loading amount
CN106910639A (en) * 2017-03-20 2017-06-30 浙江大学 A kind of NiTe for electrode material for super capacitor2Preparation method
CN110767462A (en) * 2019-11-07 2020-02-07 北京化工大学 Bimetal nickel-cobalt telluride supercapacitor electrode material and preparation method thereof
CN110844946A (en) * 2019-11-19 2020-02-28 上海季丰电子股份有限公司 Metastable crystal material and preparation method thereof
CN111769276A (en) * 2020-06-01 2020-10-13 上海海事大学 Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application
CN113023665A (en) * 2021-03-05 2021-06-25 浙江理工大学 Carbon fiber cloth loaded nano needle-shaped nickel-cobalt double-metal selenide crystal array film and preparation method thereof

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