CN105845458B - A kind of graphene activated metal organic backbone electrode material and its preparation and application - Google Patents
A kind of graphene activated metal organic backbone electrode material and its preparation and application Download PDFInfo
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- CN105845458B CN105845458B CN201610297027.0A CN201610297027A CN105845458B CN 105845458 B CN105845458 B CN 105845458B CN 201610297027 A CN201610297027 A CN 201610297027A CN 105845458 B CN105845458 B CN 105845458B
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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
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
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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
- H01G11/32—Carbon-based
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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
- H01G11/84—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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/64—Carriers or collectors
- H01M4/70—Carriers or collectors characterised by shape or form
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of graphene activated metal organic backbone electrode material and its preparations and application.Preparation method includes：Soluble-salt containing metal ion and organic ligand are added in solvent, reaction temperature controls and keeps 30h for 24 hours at 100 DEG C 150 DEG C, obtains MOF structural materials；By MOF structural materials in solvent ultrasonic disperse, then add in graphene, react 10 60min, the MOF electrode materials of graphene activation are made.Metal-organic framework materials of the present invention have many advantages, such as that porous, large specific surface area, structure be adjustable, structure diversity, and material preparation process is simple；When using it for electrode material for super capacitor, there is excellent cyclical stability and higher specific discharge capacity, specific capacitance is up to 280F/g, has good stability.
Description
Technical field
The present invention relates to electrochemical material technical fields, and in particular to a kind of graphene activated metal organic frame electrode material
Material and its preparation and application.
Background technology
Ultracapacitor is because it is in high current charge-discharge, and have extended cycle life the outstanding behaviours big etc. with power density,
Become national great scientific and technical innovation, new energy field one of cutting edge technology, be more formulated into《Long-term science in country
Development and technical development plan outline》In, there is important strategic importance and realistic meaning.Ultracapacitor can be applied in electricity
The fields such as son, portable electronics, electric vehicle, space flight and aviation, defence and military.Carbon-based material specific capacity in ultracapacitor research
Smaller, energy density is relatively low, and the metal oxide materials such as ruthenium base are expensive and toxic limit its commercialization.Therefore, compel
Being essential will prepare with height ratio capacity, excellent cyclical stability and environmental-friendly Novel super capacitor electrode material.
Metal-organic framework materials (Metal-Organic-Framework, MOF) are by transition metal ions and organic bridge
Join the crystalline material that ligand is formed, as a kind of novel micropore organometallic polymer, it has higher specific surface area,
Big porosity and modulated aperture.In addition, redox reaction can occur for the metal ion in MOF, generate to method
The contribution of pseudo-capacitance is drawn, therefore it is expected to the electrode material for super capacitor as large capacity.
At present, some reports using MOF materials as electrode material are disclosed, it is public in patent (105047435 A of CN)
A kind of manganese Metal organic backbone electrode material and preparation method thereof is opened, by the way that Mn will be contained2+Soluble-salt, organic acid and two
Tooth containing n-donor ligand is added in deionized water is prepared for manganese Metal organic backbone (Mn-MOF) electrode material using hydro-thermal reaction, tool
There is excellent chemical property, specific capacitance is up to 242F/g.But the materials conductive performance of the system is poor, leads to energy density
It is low, it is therefore necessary to continue to explore new MOF electrode materials.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of graphene activated metal organic backbone electricity
Pole material and its preparation and application.Metal-organic framework materials of the present invention have porous, large specific surface area, structure can
The advantages that tune, structure diversity, material preparation process is simple；When using it for electrode material for super capacitor, have excellent
Cyclical stability and higher specific discharge capacity, specific capacitance are up to 280F/g, have good stability.
The present invention main technical schemes be：
The first object of the present invention is to provide a kind of preparation method of graphene activated metal organic backbone electrode material,
Including：
(1) soluble-salt containing metal ion and organic ligand 2,2'- bipyridyl -4,4'- dioctyl phthalate are added to molten
It in agent, stirs evenly, is transferred in reaction kettle, reaction temperature controls and keeps -30h for 24 hours at 100 DEG C -150 DEG C, through centrifuging, washing
It washs, is dried in vacuo at 80 DEG C -100 DEG C, obtain MOF structural materials；
(2) by MOF structural materials made from step (2), (ultrasonic power and frequency are respectively ultrasonic disperse in solvent
100W and 40kHz), graphene is then added in, reacts 10-60min, it is washed, dry, the MOF electrodes of graphene activation are made
Material.
Further, the metal ion in the step (1) is Cu2+、Co2+、Ni2+、Fe2+Or Mn2+。
Further, the soluble-salt containing metal ion in the step (1) is acetate.
Further, a concentration of 0.02M of the soluble-salt containing metal ion in the step (1) in a solvent；
Preferably, the soluble-salt containing metal ion is nickel acetate, cobalt acetate or copper acetate；Most preferably cobalt acetate.
Further, the solvent in the step (1) is one or two kinds of in DMF, NMP, DMSO, deionized water
Mixing.
Further, the soluble-salt containing metal ion and organic ligand 2 in the step (1), 2'- bipyridyls-
The molar ratio of 4,4'- dioctyl phthalate is 5:1~1:5.
Further, the solvent in the step (2) is deionized water.
Further, the graphene in the step (2) is less than 10 reduced graphene powder for graphene oxide or the number of plies
End.
Further, the mass ratio of the MOF structural materials in the step (2) and graphene is 5:1~200:1；It is preferred that
, the mass ratio of MOF structural materials and graphene is 10:1~100:1.
The second object of the present invention is to provide a kind of organic bone of graphene activated metal for preparing gained by the above method
Frame electrode material.
It is still another object of the present invention to provide above-mentioned graphene activated metal organic backbone electrode material prepare it is super
Application in capacitor.
Electrode material provided by the invention is metal-organic framework materials (MOF), in order to improve the electric conductivity of material, profit
Carrying out activation with graphene reduces electrode material internal resistance.The monomer component of the metal-organic framework material is 2,2'- bipyridyl -4,
4'- dioctyl phthalate, this ligand can be with various metals ion coordination bondings.
Compared with prior art, the graphene activated metal organic backbone electrode material that prepared by the present invention, is provided simultaneously with
The function of MOF materials and graphene, both with larger specific surface area, aperture is adjustable, while electric conductivity is also superior to same type of material,
High specific capacity is shown applied to ultracapacitor, energy density is big, and cyclical stability is good.
Description of the drawings
Fig. 1 is MOF materials N in embodiment 12Adsorption/desorption isotherms；
Fig. 2 is the Ni-MOF crystal structure figures in embodiment 1；
Fig. 3 is ultracapacitor cycle performance figure in embodiment 2.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained without making creative work
Example is applied, shall fall within the protection scope of the present invention.
Embodiment 1
1mmol nickel acetates are weighed respectively, and 1mmol 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL DMF are molten
Liquid stirs evenly, and is transferred in reaction kettle, and reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, vacuum at 85 DEG C
It is dry, Ni-MOF structural materials are obtained, by testing N2Adsorption/desorption isotherms obtain BET as 1869m2/g.As shown in Fig. 2,
Crystal structure figures of the Ni-MOF along [100] direction, it can be seen that 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands are parallel to
(010) crystal face stacked in parallel, and be firmly coordinated with nickel acetate.
It weighs the above-mentioned Ni-MOF structural materials of 2.0g to be put into beaker, adds in 40mL deionized waters and carry out ultrasonic wave dispersion
(ultrasonic power and frequency be respectively 100W and 40kHz), adds 100mg graphenes, and ultrasonic reaction 30min is dry by washing
Dry processing obtains the metal organic framework electrode material GNS--Ni-MOF of graphene activation process.
By GNS--Ni-MOF electrode materials, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in
In NMP, then electrode slurry is coated onto by twin rollers in nickel foam, assembles and detains by the use of the KOH aqueous solutions of 3M as electrolyte
Formula battery, battery performance test equipment are blue electric cell tester, and potential region is 0~1.0V, and specific capacity is 248F/ after tested
g。
Comparative example 1
1mmol nickel acetates are weighed respectively, and 1mmol 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL DMF are molten
Liquid stirs evenly, and is transferred in reaction kettle, and reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, vacuum at 85 DEG C
It is dry, obtain Ni-MOF structural materials.
By Ni-MOF electrode materials obtained, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in
In NMP, then electrode slurry is coated onto by twin rollers in nickel foam, assembles and detains by the use of the KOH aqueous solutions of 3M as electrolyte
Formula battery, battery performance test equipment are blue electric cell tester, and potential region is 0~1.0V, and specific capacity is 224F/ after tested
g。
Embodiment 2
1mmol cobalt acetates are weighed respectively, and 1mmol 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL DMF are molten
Liquid stirs evenly, and is transferred in reaction kettle, and reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, vacuum at 85 DEG C
It is dry, obtain Co-MOF structural materials.
It weighs the above-mentioned Co-MOF structural materials of 2.0g to be put into beaker, adds in 40mL deionized waters and carry out ultrasonic wave dispersion
(ultrasonic power and frequency be respectively 100W and 40kHz) adds 20mg graphenes, ultrasonic reaction 30min, by washing drying
Processing obtains the metal organic framework electrode material GNS--Co-MOF of graphene activation process.
By GNS--Co-MOF electrode materials, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in
In NMP, then electrode slurry is coated onto by twin rollers in nickel foam, assembles and detains by the use of the KOH aqueous solutions of 3M as electrolyte
Formula battery, battery performance test equipment are blue electric cell tester, and potential region is 0~1.0V, and specific capacity can reach after tested
To 280F/g.
Ultracapacitor cycle performance manufactured in the present embodiment is as shown in figure 3, preceding 100 primary current density 0.1A/g, 100 times
Later current density 1.0A/g.
Embodiment 3
1mmol copper acetates are weighed respectively, and 2mmol 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL NMP are molten
Liquid stirs evenly, and is transferred in reaction kettle, and reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, vacuum at 85 DEG C
It is dry, obtain Cu-MOF structural materials.
It weighs the above-mentioned Cu-MOF structural materials of 2.0g to be put into beaker, adds in 40mL deionized waters and carry out ultrasonic wave dispersion
(ultrasonic power and frequency be respectively 100W and 40kHz), adds the 40mg graphene oxides GO (quality of graphene oxide solution
Score is 1.0%) ultrasonic reaction 30min, and the metal organic framework electricity of graphene activation process is obtained by washing and drying treatment
Pole material GO--Cu-MOF.
By GO--Cu-MOF electrode materials, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in NMP
In, then electrode slurry is coated onto by twin rollers in nickel foam, it is electric by the use of the KOH aqueous solutions of 3M as electrolyte assembling button
Pond, battery performance test equipment are blue electric cell tester, and potential region is 0~1.0V, and specific capacity is 232F/g after tested.
Embodiment 4
1mmol manganese acetates are weighed respectively, and 4mmol 2,2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL NMP are molten
Liquid stirs evenly, and is transferred in reaction kettle, and reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, vacuum at 85 DEG C
It is dry, obtain Mn-MOF structural materials.
It weighs the above-mentioned Mn-MOF structural materials of 2.0g to be put into beaker, adds in 40mL deionized waters and carry out ultrasonic wave dispersion
(ultrasonic power and frequency be respectively 100W and 40kHz) adds the 50mg graphene oxides (quality of graphene oxide solution point
Number is 1.0%), ultrasonic reaction 30min obtains the metal organic framework electrode of graphene activation process by washing and drying treatment
Material GO--Mn-MOF.
By GO--Mn-MOF electrode materials, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in NMP
In, then electrode slurry is coated onto by twin rollers in nickel foam, it is electric by the use of the KOH aqueous solutions of 3M as electrolyte assembling button
Pond, battery performance test equipment are blue electric cell tester, and potential region is 0~1.0V, and specific capacity is 253F/g after tested.
By above-mentioned comparative example and embodiment compare it is found that by graphene activation process electrode material conductivity enhance,
Effect in embodiment 2 by the use of cobalt acetate as metal ion is best, and specific capacity can reach 280F/g, and stable circulation is good.
Claims (3)
1. a kind of preparation method of graphene activated metal organic backbone electrode material, including：
(1) by the soluble-salt containing metal ion and organic ligand 2,2'- bipyridyl -4,4'- dioctyl phthalate is added in solvent,
It stirring evenly, is transferred in reaction kettle, reaction temperature controls and keeps -30h for 24 hours at 100 DEG C -150 DEG C, through centrifuging, washing, 80
It is dried in vacuo at DEG C -100 DEG C, obtains MOF structural materials；
(2) by MOF structural materials ultrasonic disperse in solvent made from step (1), graphene is then added in, reacts 10-
60min, it is washed, dry, the MOF electrode materials of graphene activation are made；
1mmol cobalt acetates, 1mmol 2 are weighed respectively, and 2'- bipyridyl -4,4'- dioctyl phthalate organic ligands and 50mL DMF solutions stir
It mixes uniformly, is transferred in reaction kettle, reaction temperature controls to be kept for 24 hours at 120 DEG C, by centrifuge washing, is dried in vacuo at 85 DEG C,
Obtain Co-MOF structural materials；
It weighs the above-mentioned Co-MOF structural materials of 2.0g to be put into beaker, adds in 40mL deionized waters and carry out ultrasonic wave dispersion (ultrasound
Power and frequency are respectively 100W and 40kHz), add 20mg graphenes, ultrasonic reaction 30min, by washing and drying treatment
Obtain the metal organic framework electrode material GNS--Co-MOF of graphene activation process；
By GNS--Co-MOF electrode materials, binding agent and conductive black according to 85：10：5 mass ratio is dispersed in NMP,
Then electrode slurry is coated onto by twin rollers in nickel foam, button cell is assembled by the use of the KOH aqueous solutions of 3M as electrolyte,
Battery performance test equipment is blue electric cell tester, and potential region is 0~1.0V, and specific capacity reaches 280F/g after tested.
2. a kind of graphene activated metal organic backbone electrode material that gained is prepared using method described in claim 1.
3. graphene activated metal organic backbone electrode material according to claim 2 answering in ultracapacitor is prepared
With.
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