CN108133834A - A kind of nickel foam is the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor - Google Patents
A kind of nickel foam is the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor Download PDFInfo
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- CN108133834A CN108133834A CN201711450252.4A CN201711450252A CN108133834A CN 108133834 A CN108133834 A CN 108133834A CN 201711450252 A CN201711450252 A CN 201711450252A CN 108133834 A CN108133834 A CN 108133834A
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- super capacitor
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000003990 capacitor Substances 0.000 title claims abstract description 47
- 239000007772 electrode material Substances 0.000 title claims abstract description 43
- 239000006260 foam Substances 0.000 title claims abstract description 43
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 36
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 24
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 24
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019253 formic acid Nutrition 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- CNFDGXZLMLFIJV-UHFFFAOYSA-L manganese(II) chloride tetrahydrate Chemical compound O.O.O.O.[Cl-].[Cl-].[Mn+2] CNFDGXZLMLFIJV-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 1
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000001291 vacuum drying Methods 0.000 claims 1
- 239000011572 manganese Substances 0.000 abstract description 18
- 239000012621 metal-organic framework Substances 0.000 abstract description 6
- 238000007306 functionalization reaction Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 17
- 239000000243 solution Substances 0.000 description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000008151 electrolyte solution Substances 0.000 description 5
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000004134 energy conservation Methods 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000033001 locomotion Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000009329 sexual behaviour Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
-
- 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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of using nickel foam as the MOFs Mn of substrate2O3The preparation method of electrode material for super capacitor, includes the following steps：(1) tetrahydrate manganese chloride, ammonium chloride, acetonitrile, formic acid and acetic acid are configured to precursor solution in proportion；(2) precursor solution obtained by step (1) is added in reaction kettle liner, stirred and evenly mixed；(3) nickel foam is put into the reaction kettle liner of step (2), seals, then carry out hydro-thermal reaction；(4) natural cooling after the completion of hydro-thermal reaction takes out product, washs, dry；(5) it in tube furnace, is heat-treated in air atmosphere to obtain the final product.Easy to operate, the capacitor electrode material that the shorter time can be made structural integrity, have excellent performance of the invention；The MOFs Mn of synthesis2O3For electrode material for super capacitor, large specific surface area is evenly distributed, have higher specific capacitance, programmable skeleton structure, high-specific surface area, high-sequential porous structure and can some unique properties of the hole space etc. of functionalization, stable electrochemical property has extended cycle life.
Description
Technical field
It is specially a kind of using nickel foam as the MOFs- of substrate the present invention relates to the preparation field of capacitor electrode material
Mn2O3The preparation method of electrode material for super capacitor.
Background technology
In the contemporary society that non-renewable energy resources reserves are becoming tight, how efficiently energy conservation and environmental protection has become the theme in epoch,
Ground utilizes the energy, is that modern scientific research primarily solves the problems, such as.Ultracapacitor is as a kind of novel energy storage device, at it
It is not chemically reacted in thermal energy storage process, and this process is reversible, also just determines ultracapacitor compared to general
Logical electrochmical power source can be with the hundreds thousand of secondary advantages of repeated charge[1].This experiment inserts three simultaneously in electrolyte solution
Electrode, and apply the voltage that will not decompose electrolyte solution between its working electrode and reference electrode.At this point, electrolyte
In positive and negative ion can form electric double layer in two electrode surfaces rapidly to two polar motions under the action of electric field.Due to close electricity
Lotus interlamellar spacing is more much smaller than ordinary capacitor charge interlamellar spacing, therefore can accommodate more electricity than ordinary capacitor.Meanwhile
Double layer capacitor inherently has larger internal resistance, therefore can plug in an unloaded situation.When overvoltage charges,
Double layer capacitor can voluntarily without damaging device, this point be different from the voltage breakdown of traditional aluminium electrolutic capacitor for open circuit.
Ultracapacitor isGenerallyIt is numerous applied to portable electronic device, electric vehicle, data accumulating storage and accumulation power supply etc.
Field, and determine that the key element of super capacitor function is then its electrode material.
MOFs materials have attracted more and more concerns, since it is with programmable skeleton structure, high-specific surface area, height
Spend orderly porous structure and can some unique properties of the hole space etc. of functionalization, as novel inorganic-organic hybridization work(
Energy material, there is the unrivaled advantage of traditional inorganic material.So in many field extensive uses, such as energy storage and turn
It changes, catalyst, chemical sensor etc..
A kind of therefore it provides MOFs materials --- Mn2O3, and applied in ultracapacitor, to reduce cost, raising is imitated
For the purpose of rate, design synthesizes more outstanding metal nanometer composite material or finds a kind of more ideal MOFs for super
Capacitor emerges from the various advantage performances of MOFs in the energy or environmental area, is a good problem to study.
Invention content
At low cost the present invention provides a kind of preparation method is simple in order to solve deficiency of the prior art, yield is high,
Electrode material obtained has higher specific capacitance and good stability, and service life is long, while also has good electrification
Learn activity using nickel foam as the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor.
The object of the present invention is achieved like this：
It is a kind of using nickel foam as the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor, includes the following steps：
(1) tetrahydrate manganese chloride, ammonium chloride, acetonitrile, formic acid and acetic acid are configured to precursor solution in proportion；
(2) precursor solution obtained by step (1) is added in reaction kettle liner, stirred and evenly mixed；
(3) nickel foam is put into the reaction kettle liner of step (2), seals, then carry out hydro-thermal reaction.
(4) natural cooling after the completion of hydro-thermal reaction takes out product, washs, dry；
(5) in tube furnace, in air atmosphere be heat-treated to get.
Further：
(1) tetrahydrate manganese chloride and sal-ammoniac molar ratio are 3 in the step (1):8；Acetonitrile, formic acid, acetic acid volume ratio be
15:7:7；Specially：The four water nickel chlorides of 3.75 mM, the ammonium chloride of 10 mM, 37.5 ml acetonitriles, 17.5ml formic acid, 17.5ml
Acetic acid；
(2) in step (1) precursor solution, the concentration of tetrahydrate manganese chloride and sal-ammoniac is 1 mM-10 mM；
(3) nickel foam is in the step (3)：Nickel foam after cleaning, wherein cleaning is successively with acetone, dilute hydrochloric acid, ethyl alcohol
It is cleaned by ultrasonic with deionized water；
(4) hydro-thermal reaction is in the step (3)：It is placed in baking oven, heating carries out hydro-thermal reaction, and hydrothermal temperature is
100-120 DEG C, the time is 24 h；
(5) to be washed 3-5 times with absolute ethyl alcohol, drying temperature is 50 DEG C -70 DEG C for washing in the step (4), drying time
For 3-5 h；
(6) air atmosphere is 750 DEG C of annealing 3-5 h in step (5).
Positive beneficial effect：MOFs-Mn prepared by the present invention2O3Preparation method for electrode material for super capacitor operates
Simply, the capacitor electrode material that the shorter time can be made structural integrity, have excellent performance only is needed, does not need to complex device,
It is of low cost.The MOFs-Mn of synthesis2O3For electrode material for super capacitor, large specific surface area is evenly distributed, cube structure tool
There are higher surface area, obtained MOFs-Mn2O3Electrode material for super capacitor has higher specific capacitance, programmable bone
Frame structure, high-specific surface area, high-sequential porous structure and can some unique properties of the hole space etc. of functionalization, electrochemistry
Performance is stablized, and has extended cycle life, possibility is provided for industrialized production, be a kind of excellent electrode material for super capacitor, has
There is good development prospect.The preparation method of the present invention is simple, effective, of low cost, energy conservation and environmental protection.
Description of the drawings
Fig. 1 is the MOFs-Mn using nickel foam as substrate prepared by the embodiment of the present invention 12O3SEM figure；
Fig. 2 is the MOFs-Mn using nickel foam as substrate prepared in the embodiment of the present invention 12O3Electrode material for super capacitor exists
Difference sweeps the cyclic voltammetry curve figure under speed；
Fig. 3 is the MOFs-Mn using nickel foam as substrate prepared in the embodiment of the present invention 12O3Electrode material for super capacitor exists
Charging and discharging curve figure under different current densities；
Fig. 4 is the MOFs-Mn using nickel foam as substrate prepared in the embodiment of the present invention 12O3Electrode material for super capacitor is 2
A g-1Cyclical stability curve graph under current density；
Fig. 5 is the MOFs-Mn using nickel foam as substrate prepared by the embodiment of the present invention 12O3The electrochemical impedance figure of nano material；
Fig. 6 is the MOFs-Mn using nickel foam as substrate prepared by the embodiment of the present invention 12O3The XRD diagram of nano material.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is described further：
It is a kind of using nickel foam as the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor, includes the following steps：
(1) tetrahydrate manganese chloride, ammonium chloride, acetonitrile, formic acid and acetic acid are configured to precursor solution in proportion；
(2) precursor solution obtained by step (1) is added in reaction kettle liner, stirred and evenly mixed；
(3) nickel foam is put into the reaction kettle liner of step (2), seals, then carry out hydro-thermal reaction；
(4) natural cooling after the completion of hydro-thermal reaction takes out product, washs, dry；
(5) in tube furnace, in air atmosphere be heat-treated to get.
Further：
(1) tetrahydrate manganese chloride and sal-ammoniac molar ratio are 3 in the step (1):8；Acetonitrile, formic acid, acetic acid volume ratio be
15:7:7；Specially：The four water nickel chlorides of 3.75 mM, the ammonium chloride of 10 mM, 37.5 ml acetonitriles, 17.5ml formic acid, 17.5ml
Acetic acid.
(2) in step (1) precursor solution, the concentration of tetrahydrate manganese chloride and sal-ammoniac is 1 mM-10 mM；
(3) nickel foam is in the step (3)：Nickel foam after cleaning, wherein cleaning is successively with acetone, dilute hydrochloric acid, ethyl alcohol
It is cleaned by ultrasonic with deionized water；
(4) hydro-thermal reaction is in the step (3)：It is placed in baking oven, heating carries out hydro-thermal reaction, and hydrothermal temperature is
100-120 DEG C, the time is 24 h；
(5) to be washed 3-5 times with absolute ethyl alcohol, drying temperature is 50 DEG C -70 DEG C for washing in the step (4), drying time
For 3-5 h；
(6) air atmosphere is 750 DEG C of annealing 3-5 h in step (5).
Embodiment 1
After nickel foam is cleaned by ultrasonic 15 min with acetone, the hydrochloric acid of a concentration of 1 M, ethyl alcohol and deionized water successively, 60 DEG C
It is dry.Utilize the four water nickel chlorides of 3.75 mM, the ammonium chloride of 10 mM, 37.5 ml acetonitriles, 17.5ml formic acid, 17.5ml acetic acid
Formed precursor solution, stirring 30 min at room temperature is uniformly mixed precursor solution, be packed into liner for polytetrafluoroethylene (PTFE) not
It becomes rusty in steel autoclave；Dried nickel foam is put into reaction kettle liner, is sealed, is placed in 100 DEG C of baking oven anti-
24 h are answered, cooled to room temperature after the completion of reaction is collected product, is washed several times with ethanol, 60 DEG C of dry 4h.After dry
Nickel foam be placed in tube furnace, 750 DEG C of 4 h of annealing are to get to the MOFs- using nickel foam as substrate in air atmosphere
Mn2O3Electrode material for super capacitor.
Embodiment 2
After nickel foam is cleaned by ultrasonic 15 min with acetone, the hydrochloric acid of a concentration of 1 M, ethyl alcohol and deionized water successively, 60 DEG C
It is dry.Utilize the four water nickel chlorides of 3.75 mM, the ammonium chloride of 10 mM, 37.5 ml acetonitriles, 17.5ml formic acid, 17.5ml acetic acid
Formed precursor solution, stirring 30 min at room temperature is uniformly mixed precursor solution, be packed into liner for polytetrafluoroethylene (PTFE) not
It becomes rusty in steel autoclave；Dried nickel foam is put into reaction kettle liner, is sealed, is placed in 110 DEG C of baking oven anti-
24 h are answered, cooled to room temperature after the completion of reaction is collected product, is washed several times with ethanol, 60 DEG C of dry 4h.After dry
Nickel foam be placed in tube furnace, 750 DEG C of 4 h of annealing are to get to the MOFs- using nickel foam as substrate in air atmosphere
Mn2O3Electrode material for super capacitor.
Embodiment 3
After nickel foam is cleaned by ultrasonic 15 min with acetone, the hydrochloric acid of a concentration of 1 M, ethyl alcohol and deionized water successively, 60 DEG C
It is dry.Utilize the four water nickel chlorides of 3.75 mM, the ammonium chloride of 10 mM, 37.5 ml acetonitriles, 17.5ml formic acid, 17.5ml acetic acid
Formed precursor solution, stirring 30 min at room temperature is uniformly mixed precursor solution, be packed into liner for polytetrafluoroethylene (PTFE) not
It becomes rusty in steel autoclave；Dried nickel foam is put into reaction kettle liner, is sealed, is placed in 120 DEG C of baking oven anti-
24 h are answered, cooled to room temperature after the completion of reaction is collected product, is washed several times with ethanol, 60 DEG C of dry 4h.After dry
Nickel foam be placed in tube furnace, 750 DEG C of 4 h of annealing are to get to the MOFs- using nickel foam as substrate in air atmosphere
Mn2O3Electrode material for super capacitor.
To MOFs-Mn in the embodiment of the present invention 12O3Electrode material for super capacitor makees performance test, the result is shown in Figure 1-5：
As shown in Figure 1, MOFs-Mn2O3Foam nickel surface is attached to electrode material for super capacitor even compact, passes through high power
Microscope can be seen that MOFs-Mn2O3For the bulk of hole, it is conducive to provide larger specific surface area and cyclical stability；
It is illustrated in figure 2 MOFs-Mn2O3Electrode material for super capacitor is under the sweep speed of 10-100 mV/s, with 6M KOH
For the cyclic voltammetry curve of electrolyte solution, the redox peaks in cyclic curve figure are symmetrical, show as typical farad
Fake capacitance model；
It is illustrated in figure 3 MOFs-Mn2O3Electrode material for super capacitor under the current density of 1-25 A/g, using 6M KOH as
The charge-discharge performance test curve of electrolyte solution, curve deviate from the curve model of symmetrical triangle, with reference to Fig. 2, explanation
MOFs-Mn2O3Energy storage mechnism be Faraday pseudo-capacitance model；With the increase of current density, material specific capacitance reduces, but under
Drop trend is gentle, meanwhile, curve can illustrate it with good capacitance sexual behaviour to a certain extent about axial symmetry；
It is illustrated in figure 4 MOFs-Mn2O3Electrode material for super capacitor is under the current density of 1A/g, using 6M KOH as electrolysis
The cyclical stability test curve of matter solution, by the charge-discharge test of 1000 circles, MOFs-Mn2O3Electrode material is still shown
Larger specific capacitance, fall is smaller, illustrates it with good electrochemical stability；
It is illustrated in figure 5 MOFs-Mn2O3Electrochemical impedance of the electrode material for super capacitor using 6M KOH as electrolyte solution is surveyed
Examination.As shown in Figure 5, MOFs-Mn2O3The resistance of electrode material for super capacitor is smaller, is conducive to the transmission of electronics, shows
Good chemical property；
If Fig. 6 is the MOFs-Mn that in the present invention prepared by case study on implementation 12O3The X-ray diffractogram of composite material.It will be appreciated from fig. 6 that
Product diffraction maximum and MOFs-Mn after annealing2O3Standard card diffraction maximum is consistent, illustrates that product has preferable crystallinity.
MOFs-Mn prepared by the present invention2O3Preparation method for electrode material for super capacitor is easy to operate, only needs shorter
Time structural integrity can be made, have excellent performance capacitor electrode material, do not need to complex device, it is of low cost.Synthesis
MOFs-Mn2O3For electrode material for super capacitor, large specific surface area is evenly distributed, and cube structure has higher surface
Product, obtained MOFs-Mn2O3Electrode material for super capacitor has higher specific capacitance, programmable skeleton structure, high ratio
Surface area, high-sequential porous structure and can some unique properties, the stable electrochemical property such as hole space of functionalization follow
Ring long lifespan provides possibility for industrialized production, is a kind of excellent electrode material for super capacitor, has good development
Prospect.The preparation method of the present invention is simple, effective, of low cost, energy conservation and environmental protection.
The foregoing is merely the schematical specific embodiments of the present invention, are not limited to the scope of the present invention, any
The equivalent variations and modification that those skilled in the art is made under the premise of present inventive concept and principle is not departed from, should all belong to
In the scope of protection of the invention.
Claims (7)
- It is 1. a kind of using nickel foam as the preparation method of the MOFs-NiS electrode material for super capacitor of substrate, which is characterized in that packet Include following steps：(1) tetrahydrate manganese chloride, ammonium chloride, acetonitrile, formic acid and acetic acid are configured to precursor solution in proportion；(2) Precursor solution obtained by step (1) is added in reaction kettle liner, is stirred and evenly mixed；(3) nickel foam is put into the reaction kettle liner of step (2), seals, then carry out hydro-thermal reaction；(4) natural cooling after the completion of hydro-thermal reaction takes out product, washs, dry；(5) in tube furnace, in air atmosphere be heat-treated to get.
- 2. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, which is characterized in that tetrahydrate manganese chloride and sal-ammoniac molar ratio are 3 in the step (1):8；Acetonitrile, formic acid, acetic acid volume Than being 15:7:7；.
- 3. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, it is characterised in that：In the step (1) in precursor solution, the concentration of tetrahydrate manganese chloride and sal-ammoniac is 1 mM-10 mM。
- 4. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, it is characterised in that：Hydrothermal temperature is 100-120 DEG C in the step (3), and the time is 24 h.
- 5. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, it is characterised in that：Nickel foam is in the step (3)：Nickel foam after cleaning, wherein cleaning is successively with acetone, dilute salt Acid, ethyl alcohol and deionized water are cleaned by ultrasonic.
- 6. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, it is characterised in that：To be washed 3-5 times with absolute ethyl alcohol, vacuum drying temperature is 50 DEG C -70 DEG C for washing in the step (4), Drying time is 3-5 h.
- 7. a kind of preparation side of the nickel foam according to claim 1 for the MOFs-NiS electrode material for super capacitor of substrate Method, it is characterised in that：Nitrogen atmosphere is 700-750 DEG C of annealing 3-5 h in the step (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711450252.4A CN108133834A (en) | 2017-12-27 | 2017-12-27 | A kind of nickel foam is the MOFs-Mn of substrate2O3The preparation method of electrode material for super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN109192981A (en) * | 2018-09-03 | 2019-01-11 | 南京大学深圳研究院 | A kind of three nickel positive electrode of foam curing and the preparation method and application thereof |
| CN110918103A (en) * | 2019-12-24 | 2020-03-27 | 济南大学 | Composite electrocatalyst and preparation method and application thereof |
| CN113711390A (en) * | 2019-03-25 | 2021-11-26 | 赛莫必乐公司 | Metal foam capacitor and super capacitor |
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| CN106395908A (en) * | 2016-09-06 | 2017-02-15 | 上海应用技术大学 | Preparation method of bamboo joint structure Mn2O3 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109192981A (en) * | 2018-09-03 | 2019-01-11 | 南京大学深圳研究院 | A kind of three nickel positive electrode of foam curing and the preparation method and application thereof |
| CN113711390A (en) * | 2019-03-25 | 2021-11-26 | 赛莫必乐公司 | Metal foam capacitor and super capacitor |
| CN110918103A (en) * | 2019-12-24 | 2020-03-27 | 济南大学 | Composite electrocatalyst and preparation method and application thereof |
| CN110918103B (en) * | 2019-12-24 | 2022-07-01 | 济南大学 | Composite electrocatalyst and preparation method and application thereof |
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