CN105761942A - Super-capacitor electrode material of sandwiched structure and preparation method - Google Patents
Super-capacitor electrode material of sandwiched structure and preparation method Download PDFInfo
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- CN105761942A CN105761942A CN201610110321.6A CN201610110321A CN105761942A CN 105761942 A CN105761942 A CN 105761942A CN 201610110321 A CN201610110321 A CN 201610110321A CN 105761942 A CN105761942 A CN 105761942A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a super-capacitor electrode material of a sandwiched structure. A graphene sheet layer is inserted into an Ni-MOF interlayer to form a sandwiched structure. The graphene accounts for 6 to 40% of Ni-MOF volume fraction. Also provided is a preparation method for the electrode material, which comprises the steps of adding a nickel nitrate/DMF solution to a terephthalic acid/DMF solution and obtaining a precursor solution after dissolution; and adding a graphene oxide aqueous solution to the precursor solution, transferring to a polytetrafluoroethylene hydrothermal liner kettle after ultrasonic dispersion, conducting a high fire reaction for 6min in a household microwave oven of 600W, suction-filtering the reaction liquid, repeatedly centrifuging, washing and drying a filter cake with absolute ethyl alcohol and DMF, and obtaining a super-capacitor electrode material of a sandwiched structure. The invention can be used in a super-capacitor, with maximum specific capacitance up to 1600Fg-1.
Description
Technical field
The invention belongs to materialogy field, relate to electrode material for super capacitor and the preparation of a kind of sandwich sandwich
Method.
Background technology
Ultracapacitor is also electrochemical capacitor, is a kind of energy storage between battery and conventional electrostatic capacitor
Device, has good reversibility, has extended cycle life.Additionally its to complete the charging interval short, can be as highpowerpulse electricity
Source, can the big instantaneous discharge and recharge of electric current.It is widely used in data accumulating storage system, portable instrument equipment, back-up source, leads to
The fields such as news equipment, computer, electric welding machine, magnet charger, flash lamp, fuel cell, electric vehicle mixed power.Along with green is electronic
The development of automobile, the research of ultracapacitor is also into a brand-new period, but ultracapacitor is because of its weak point: energy
Metric density is on the low side, self-discharge current is big, monomer rated voltage is low, is difficult to meet energy storage requirement, therefore designs efficient, ring
Guarantor, low cost, high-energy-density energy-storage system are most important.Electrode is one important part of ultracapacitor, electrode
Material is to determine the most important factor of ultracapacitor performance, traditional electrode material, can be divided into three major types, i.e. material with carbon element, mistake
Cross metal oxide and conductive organic polymer.The most frequently used material with carbon element: activated carbon, carbon nano-fiber, carbon aerogels, carbon is received
Mitron.Absorbent charcoal material, charge-discharge performance is well improved, but higher than electric capacity is not, at 1 mol/L H2SO4With
6mol/L KOH aqueous solution electrolysis liquid reaches 200 F/g than electric capacity, at 1mol/L (C2H5)4NBF4Electrolyte reaches than electric capacity
To 150 F/g；Carbon nano-fiber materials, its specific surface is big, and good conductivity, the ratio electric capacity after activation is high, but apparent density is usual
Relatively low, therefore its capacitance density is relatively low.Carbon aerogels material, its raw material costliness, complicated process of preparation, production cycle length and rule
Modelling production difficulty is big.CNT, reversible higher than electric capacity, efficiency for charge-discharge is low, and self-discharge phenomenon is serious and easily reunites
Deng the most relatively costly, it is impossible to meet well and be actually needed.With IrO in metal oxide electrode material2Or RhO material work electricity
, there is good electrical conductivity pole, it is possible to obtain higher specific capacity and higher specific energy, but noble metal is expensive, thus limits
Make the practical of it.It is few that conductive polymer electrodes material also exists kind, directly makees electrochemistry electricity with conductive organic polymer
Container electrode material, in capacitor, resistance is bigger.At present, normally used is nanocarbon/metal compound, carbon/ECP, metal compound
The combination electrode materials such as thing/conducting polymer, reach 389F/g than electric capacity.In recent years, metal-organic framework materials was studied
The favor of person, MOF is to be connected, by oxygen-containing or nitrogen organic ligand, the mesh skeleton structure formed with transition metal.Because it has
The features such as orderly honeycomb hole, transiting metal oxidation coordination and high specific surface area, so MOF has high specific density, high ratio
The advantage such as energy and high-specific-power.The every advantage being had due to the architectural feature of MOF, practical has met ultracapacitor
Required high power and density.A kind of Ni-MOF electrode material, this material is disclosed in patent CN201510381600.1
Ratio electric capacity maximum up to 1500F/g, after charge and discharge cycles 3000 times, remain to keep the ratio electric capacity of 90%, and preparation method letter
Single controlled, mild condition, low production cost, but specific surface area and energy density are not the biggest.
Summary of the invention
The invention provides electrode material for super capacitor and the preparation method of a kind of sandwich sandwich, described this
Electrode material for super capacitor and the preparation method of planting sandwich sandwich solve ultracapacitor energy of the prior art
The technical problem that metric density is on the low side, self-discharge current is big, monomer rated voltage is low.
The invention provides the electrode material for super capacitor of a kind of sandwich sandwich, by graphene sheet layer and Ni-
MOF is constituted, and described graphene sheet layer is inserted into described Ni-MOF interlayer, and described Graphene accounts for the volume fraction of Ni-MOF
It is 6～40%.
Present invention also offers the preparation method of the electrode material for super capacitor of above-mentioned a kind of sandwich sandwich,
Comprise the steps:
1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L；
2) nickel nitrate/DMF solution of 0.15mol/l is joined in the terephthalic acid (TPA)/DMF solution of 0.20mol/l, described nitre
The volume ratio of acid nickel/DMF solution and terephthalic acid (TPA)/DMF solution is 2:1, after dissolving stirring 1～2h, it is thus achieved that precursor solution；
3) in 0.1g/L graphene oxide water solution: precursor solution is the ratio of 1.5～10ml:25ml, by graphene oxide
The aqueous solution joins in precursor solution, at 500 ~ 700W ultrasonic disperse 0.5 ~ 2h；
Being transferred to by step 3) gained mixed liquor in polytetrafluoroethylene (PTFE) hydro-thermal lining still, in 500 ~ 700W microwave equipment, high fire is anti-
Answering 5 ~ 7min, gained reactant liquor suction filtration, gained filter cake absolute ethyl alcohol, DMF are centrifugal, washing, 70 ~ 90 DEG C
It is dried, obtains the electrode material for super capacitor of sandwich sandwich.
Concrete, described high fire refers to 700W.
Concrete, described DMF refers to dimethylformamide.
Novelty of the present invention proposes to combine Graphene and Ni-MOF, forms sandwich sandwich Graphene-Ni-MOF
Electrode material, Graphene is the most best known conductive material, and MOF has high specific density, high-energy-density and high-specific-power
Etc. advantage, compound rear graphene sheet layer is inserted into Ni-MOF interlayer, forms sandwich sandwich, thus efficiently utilizes
The specific surface area of Ni-MOF material, improves the electrode material density of specific capacity and energy.
The present invention compares with prior art, and its technological progress is significant.The preparation method of the present invention is controlled, condition temperature
With, low production cost, after assembling, it is more maximum up to 1600Fg than electric capacity-1。
Accompanying drawing explanation
Fig. 1 is the XRD of embodiment 1-4 gained Graphene-Ni-MOF.
Detailed description of the invention
Embodiment 1
The preparation method of the electrode material for super capacitor of the present invention a kind of sandwich sandwich, comprises the steps:
(1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L；
(2) nickel nitrate/DMF solution of 0.15mol/l is joined in the terephthalic acid (TPA)/DMF solution of 0.20mol/l, and nitre
The volume ratio of acid nickel/DMF solution and terephthalic acid (TPA)/DMF solution is 2:1, after dissolving stirring 1～2h, it is thus achieved that precursor solution；
(3) in 0.1g/L graphene oxide water solution: the ratio of precursor solution 1.5ml:25ml, by graphene oxide water solution
Join in precursor solution, at 600W ultrasonic disperse 1h；
(4) by (3) gained mixed liquor, transfer in the water heating kettle of 35mL, in 600W household microwave oven, high fire reaction 6min,
Gained reactant liquor suction filtration, gained filter cake absolute ethyl alcohol, DMF be centrifuged repeatedly, wash, and 80 DEG C are dried,
Obtain the Graphene-Ni-MOF electrode material of sandwich sandwich.
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With cyclic voltammetry (CV) and perseverance
Electric current charging and discharging method is at 0.5Ag-1Under current density, recording than electric capacity is 1550Fg-1, after circulating 1000 times, compare electric capacity
For 1395Fg-1。
Embodiment 2
The preparation method of the electrode material for super capacitor of the present invention a kind of sandwich sandwich, comprises the steps:
(1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L；
(2) nickel nitrate/DMF solution of 0.15mol/l is joined in the terephthalic acid (TPA)/DMF solution of 0.20mol/l, and nitre
The volume ratio of acid nickel/DMF solution and terephthalic acid (TPA)/DMF solution is 2:1, after dissolving stirring 1～2h, it is thus achieved that precursor solution；
(3) in 0.1g/L graphene oxide water solution: the ratio of precursor solution 4.25ml:25ml, graphene oxide is water-soluble
Liquid joins in precursor solution, at 600W ultrasonic disperse 1h；
(4) by (3) gained mixed liquor, transfer in the polytetrafluoroethylene (PTFE) hydro-thermal lining still of 35mL, in 600W household microwave oven, high
Fire reacts 6min, gained reactant liquor suction filtration, and gained filter cake absolute ethyl alcohol, DMF are centrifuged repeatedly, wash, and 80
DEG C it is dried, obtains the Graphene-Ni-MOF electrode material of sandwich sandwich.
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With cyclic voltammetry (CV) and perseverance
Electric current charging and discharging method is at 0.5Ag-1Under current density, recording than electric capacity is 1600Fg-1, after circulating 1000 times, compare electric capacity
For 1440Fg-1。
Embodiment 3
Present invention also offers the preparation method of the electrode material for super capacitor of a kind of sandwich sandwich, including walking as follows
Rapid:
(1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L；
(2) nickel nitrate/DMF solution of 0.15mol/l is joined in the terephthalic acid (TPA)/DMF solution of 0.20mol/l, and nitre
The volume ratio of acid nickel/DMF solution and terephthalic acid (TPA)/DMF solution is 2:1, after dissolving stirring 1～2, it is thus achieved that precursor solution；
(3) in 0.1g/L graphene oxide water solution: the ratio of precursor solution 6.25ml:25ml, graphene oxide is water-soluble
Liquid joins in precursor solution, at 600W ultrasonic disperse 1h；
(4) by (3) gained mixed liquor, transfer in the polytetrafluoroethylene (PTFE) hydro-thermal lining still of 35mL, in 600W household microwave oven, high
Fire reacts 6min, gained reactant liquor suction filtration, and gained filter cake absolute ethyl alcohol, DMF are centrifuged repeatedly, wash, and 80
DEG C it is dried, obtains the Graphene-Ni-MOF electrode material of sandwich sandwich.
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With cyclic voltammetry (CV) and perseverance
Electric current charging and discharging method is at 0.5Ag-1Under current density, recording than electric capacity is 1580Fg-1, after circulating 1000 times, compare electric capacity
For 1422Fg-1。
Embodiment 4
Present invention also offers the preparation method of the electrode material for super capacitor of a kind of sandwich sandwich, including walking as follows
Rapid:
(1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L.
(2) nickel nitrate/DMF solution of 0.15mol/l is joined in the terephthalic acid (TPA)/DMF solution of 0.20mol/l,
And the volume ratio of nickel nitrate/DMF solution and terephthalic acid (TPA)/DMF solution is 2:1, after dissolving stirring 1～2h, it is thus achieved that presoma
Solution.
(3) in 0.1g/L graphene oxide water solution: the ratio of precursor solution 10ml:25ml, by graphene oxide water
Solution joins in precursor solution, at 600W ultrasonic disperse 1h.
(4) by (3) gained mixed liquor, transfer in the polytetrafluoroethylene (PTFE) hydro-thermal lining still of 35mL, at 600W household microwave oven
In, high fire reaction 6min, gained reactant liquor suction filtration, gained filter cake absolute ethyl alcohol, DMF are centrifuged repeatedly, wash
Washing, 80 DEG C are dried, and obtain the Graphene-Ni-MOF electrode material of sandwich sandwich.
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With cyclic voltammetry (CV) and perseverance
Electric current charging and discharging method is at 0.5Ag-1Under current density, recording than electric capacity is 1560Fg-1, after circulating 1000 times, compare electric capacity
For 1404Fg-1。
Claims (2)
1. the electrode material for super capacitor of a sandwich sandwich, it is characterised in that: by graphene sheet layer and Ni-MOF
Constituting, described graphene sheet layer is inserted into described Ni-MOF interlayer, and it is 6 that described Graphene accounts for the volume fraction of Ni-MOF
～40%.
2. the preparation method of the electrode material for super capacitor of a kind of sandwich sandwich described in claim 1, its feature
It is to comprise the steps:
1) Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L, by the nitric acid of 0.15mol/l
Nickel/DMF solution joins in the terephthalic acid (TPA)/DMF solution of 0.20mol/l, described nickel nitrate/DMF solution and to benzene two
The volume ratio of formic acid/DMF solution is 2:1, after dissolving stirring 1～2h, it is thus achieved that precursor solution；
2) in 0.1g/L graphene oxide water solution: precursor solution is the ratio of 1.5～10ml:25ml, by graphene oxide
The aqueous solution joins in precursor solution, at 500 ~ 700W ultrasonic disperse 0.5 ~ 2h；
3) step 3) gained mixed liquor is transferred in polytetrafluoroethylene (PTFE) hydro-thermal lining still, in 500 ~ 700W microwave equipment, Gao Huo
Reaction 5 ~ 7min, gained reactant liquor suction filtration, gained filter cake absolute ethyl alcohol, DMF are centrifugal, washing, and 70 ~ 90
DEG C it is dried, obtains the electrode material for super capacitor of sandwich sandwich.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174187A (en) * | 2018-09-07 | 2019-01-11 | 常州大学 | A kind of preparation of the composite electrocatalyst of nickel based metal organic backbone |
| CN114649116A (en) * | 2022-04-02 | 2022-06-21 | 合肥工业大学 | Preparation method of MXene/MOFs electrode material and preparation method and application of electrochemical driver of MXene/MOFs electrode material |
| CN115360368A (en) * | 2022-09-02 | 2022-11-18 | 华中科技大学 | Method for preparing high-density and ultra-small nanoparticles at high temperature in ligand-assisted transient state |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130026029A1 (en) * | 2010-04-08 | 2013-01-31 | Sam Kayaert | Photo-electrochemical cell |
| CN104538200A (en) * | 2014-12-12 | 2015-04-22 | 上海应用技术学院 | Graphene / Fe-MOFs composite material and preparation method thereof |
| CN104979104A (en) * | 2015-07-02 | 2015-10-14 | 上海应用技术学院 | Preparation method of Ni-MOF electrode material |
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2016
- 2016-02-29 CN CN201610110321.6A patent/CN105761942B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130026029A1 (en) * | 2010-04-08 | 2013-01-31 | Sam Kayaert | Photo-electrochemical cell |
| CN104538200A (en) * | 2014-12-12 | 2015-04-22 | 上海应用技术学院 | Graphene / Fe-MOFs composite material and preparation method thereof |
| CN104979104A (en) * | 2015-07-02 | 2015-10-14 | 上海应用技术学院 | Preparation method of Ni-MOF electrode material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109174187A (en) * | 2018-09-07 | 2019-01-11 | 常州大学 | A kind of preparation of the composite electrocatalyst of nickel based metal organic backbone |
| CN114649116A (en) * | 2022-04-02 | 2022-06-21 | 合肥工业大学 | Preparation method of MXene/MOFs electrode material and preparation method and application of electrochemical driver of MXene/MOFs electrode material |
| CN114649116B (en) * | 2022-04-02 | 2024-01-12 | 合肥工业大学 | Preparation method of electrode material, preparation method of electrochemical driver and application |
| CN115360368A (en) * | 2022-09-02 | 2022-11-18 | 华中科技大学 | Method for preparing high-density and ultra-small nanoparticles at high temperature in ligand-assisted transient state |
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