CN110164705A - A kind of novel ferro-cobalt based super capacitor electrode material and preparation method thereof - Google Patents
A kind of novel ferro-cobalt based super capacitor electrode material and preparation method thereof Download PDFInfo
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- CN110164705A CN110164705A CN201910167660.1A CN201910167660A CN110164705A CN 110164705 A CN110164705 A CN 110164705A CN 201910167660 A CN201910167660 A CN 201910167660A CN 110164705 A CN110164705 A CN 110164705A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 59
- 239000003990 capacitor Substances 0.000 title claims abstract description 46
- RIVZIMVWRDTIOQ-UHFFFAOYSA-N cobalt iron Chemical compound [Fe].[Co].[Co].[Co] RIVZIMVWRDTIOQ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 49
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 239000008367 deionised water Substances 0.000 claims description 38
- 229910021641 deionized water Inorganic materials 0.000 claims description 38
- 239000011259 mixed solution Substances 0.000 claims description 37
- 229910021577 Iron(II) chloride Inorganic materials 0.000 claims description 26
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 26
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 20
- 229910020598 Co Fe Inorganic materials 0.000 claims description 20
- 229910002519 Co-Fe Inorganic materials 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 20
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 claims description 20
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 15
- 239000012046 mixed solvent Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 239000002086 nanomaterial Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 230000005611 electricity Effects 0.000 claims description 5
- 229960004756 ethanol Drugs 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 238000004500 asepsis Methods 0.000 abstract description 2
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 2
- 231100000252 nontoxic Toxicity 0.000 abstract description 2
- 230000003000 nontoxic effect Effects 0.000 abstract description 2
- 239000010409 thin film Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 34
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000005406 washing Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000006260 foam Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017709 Ni Co Inorganic materials 0.000 description 1
- 229910003267 Ni-Co Inorganic materials 0.000 description 1
- 229910003262 Ni‐Co Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 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
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention proposes a kind of novel ferro-cobalt based super capacitor electrode material and preparation method thereof, by the resulting novel ultra-thin hexagon electrode material for super capacitor of this method, there is good electrochemical energy storage ability, the performance of high specific capacitance, good cyclical stability and asepsis environment-protecting；It is with a wide range of applications as efficient, lightweight electrode material in Nano-function thin films and electrode material for super capacitor technical field；Prepared combination electrode material has ultralight (active matter quality<2mg), ultra-thin (thickness<100nm), and the characteristic of superelevation specific capacitance (>1000F/g), preparation method provided by the invention has simple process, it is easy to operate, it is reproducible, it is nontoxic environmentally protective, and it is easy to the features such as producing in batches.
Description
Technical field
The present invention relates to materialogy technical field more particularly to a kind of novel ferro-cobalt based super capacitor electrode material and its
Preparation method.
Background technique
Electrochemistry pseudocapacitors, also referred to as supercapacitor, have power density is high, the charging time is short, have extended cycle life,
The advantages that environmentally protective is one of most promising energy storage device in modern electronic product.But due to lack properly at
This high performance electrode material, so that supercapacitor is hindered in practical application.In the past few decades, various electrodes
Material, including carbonaceous material, conducting polymer and transition metal oxide have been used for electrode material for super capacitor.However,
Since the energy density of carbon material is lower, conducting polymer is poor in the cyclicity of long-term charge/discharge, both materials is caused to exist
The application of energy storage device is above subject to certain restrictions；And transition metal oxide can occur quickly because of it at electrode/electrolyte interface
Reversible faraday's redox reaction, therefore can be used as ideal electrode material, but the low conduction of transition metal oxide
Rate also limits their widespread commercial.
Current most of electrode material for super capacitor that prepare are single metal oxides, and there are high rate performance and circulation are steady
The defects of qualitative lower, and bimetallic oxide is due to joined second of metal, so that various metals species composition is complicated
Microstructure and mutual synergistic effect, therefore higher electro-chemical activity can be shown, it avoids existing for single metal oxides
Defect.The common method for currently preparing electrode material for super capacitor is efficient backflow method, and the preparation process is simple, process green
Environmental protection, electrode material capacitive properties are excellent.
Summary of the invention
It is an object of the invention to propose a kind of novel ferro-cobalt with superelevation specific capacitance and good cyclical stability
Based super capacitor electrode material and a kind of simple process, easy to operate and environmentally friendly novel ferro-cobalt based super capacitor electricity
Pole material and preparation method thereof.
In order to achieve the above objectives, the present invention proposes a kind of novel ferro-cobalt based super capacitor electrode material, the novel cobalt
Iron-based electrode material for super capacitor is two-dimensional layered structure, and shape is sheet regular hexagon.
Preferably, the side length of the novel ferro-cobalt based super capacitor electrode material is 1-2um.
Preferably, the active matter quality of the novel ferro-cobalt based super capacitor electrode material is less than 2mg, thickness is less than
100nm and capacitor are greater than 1000F/g, and the active matter is ferro-cobalt bimetallic nano material.
The present invention also proposes a kind of preparation method of novel ferro-cobalt based super capacitor electrode material, comprising the following steps:
Step 1: nitrogen is passed through into deionized water；
Step 2: taking CoCl2·6H2O crystal and FeCl2·4H2O crystal is placed in a part of deionized water and anhydrous second
The in the mixed solvent of alcohol forms the first mixed solution；
Step 3: taking methylimidazole to dissolve in the in the mixed solvent of deionized water and dehydrated alcohol described in another part, formed
Second mixed solution；
Step 4: first mixed solution being placed in a beaker, is flowed back；
Step 5: stirring and heat first mixed solution；
Step 6: second mixed solution is slowly added in first mixed solution, it is molten to form third mixing
Liquid；
Step 7: flowing back to the third mixed solution；
Step 8: it is super that the step that the third mixed solution is successively centrifuged, is washed and is dried obtains novel ferro-cobalt base
Grade capacitor electrode material.
Preferably, in step 1, it takes 100ml deionized water to lead to 30min nitrogen, excludes some CO in water3 2-。
Preferably, in step 2, the CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189g:
0.3168g, mixing are dissolved in the in the mixed solvent of dehydrated alcohol described in deionized water and 10~0ml described in 40~50ml, are sufficiently stirred
It mixes.
Preferably, in step 3, methylimidazole described in 2.46~9.84g is taken to dissolve in deionized water described in 40~50ml
With the in the mixed solvent of dehydrated alcohol described in 10~0ml, it is sufficiently stirred.
Preferably, in step 4, first mixed solution is placed in three-necked flask, is carried out under the atmosphere of nitrogen
Reflux.
Preferably, in steps of 5, it stirs and heats first mixed solution to 90 DEG C.
Preferably, in step 7, the third mixed solution flows back 5~10h under 90 DEG C of nitrogen atmosphere.
Preferably, in step 8, the novel ferro-cobalt based super capacitor electrode material is hexagon Co-Fe nanometers of material
Material.
Compared with prior art, of the invention to be advantageous in that: the above-mentioned resulting novel super electricity of ultra-thin hexagon
Container electrode material has good electrochemical energy storage ability, high specific capacitance, good cyclical stability and asepsis environment-protecting
Performance；As efficient, lightweight electrode material in Nano-function thin films and electrode material for super capacitor technical field
It is with a wide range of applications；Prepared combination electrode material has ultralight (active matter quality < 2mg), ultra-thin (thickness <
100nm) and the characteristic of superelevation specific capacitance (> 1000 F/g), preparation method provided by the invention have simple process, operation side
Just, reproducible, it is nontoxic environmentally protective, and it is easy to the features such as producing in batches.
Detailed description of the invention
Fig. 1 is that the SEM of the resulting novel ferro-cobalt based super capacitor electrode material of embodiment 1 schemes.
Fig. 2 is that the SEM of the resulting novel ferro-cobalt based super capacitor electrode material of embodiment 5 schemes.
Fig. 3 is the cyclic voltammetry curve of Co-Fe electrode material.
Fig. 4 is the constant current charge-discharge curve of Co-Fe electrode material.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be made below into
Illustrate to one step.
The present invention proposes a kind of type ferro-cobalt based super capacitor electrode material, novel ferro-cobalt based super capacitor electrode material
For two-dimensional layered structure, shape is sheet regular hexagon.
Preferably, the side length of novel ferro-cobalt based super capacitor electrode material is 1-2um.
Preferably, the active matter quality of novel ferro-cobalt based super capacitor electrode material is less than 2mg, thickness is less than 100nm
And capacitor is greater than 1000F/g, the active matter is ferro-cobalt bimetallic nano material.
The present invention also proposes a kind of preparation method of novel ferro-cobalt based super capacitor electrode material, comprising the following steps:
Step 1: nitrogen is passed through into deionized water；
Step 2: taking CoCl2·6H2O crystal and FeCl2·4H2O crystal is placed in a part of deionized water and dehydrated alcohol
In the mixed solvent forms the first mixed solution；
Step 3: taking methylimidazole to dissolve in the in the mixed solvent of another part deionized water and dehydrated alcohol, form second
Mixed solution；
Step 4: the first mixed solution being placed in a beaker, is flowed back；
Step 5: stirring and heat the first mixed solution；
Step 6: the second mixed solution being slowly added in the first mixed solution, to form third mixed solution；
Step 7: flowing back to third mixed solution；
Step 8: the step that third mixed solution is successively centrifuged, is washed and is dried obtains the novel super electricity of ferro-cobalt base
Container electrode material.
In the present embodiment, in step 1, it takes 100ml deionized water to lead to 30min nitrogen, excludes some CO in water3 2-。
In the present embodiment, in step 2, CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189g:
0.3168g, mixing are dissolved in the in the mixed solvent of 40~50ml deionized water and 10~0ml dehydrated alcohol, are sufficiently stirred.
In the present embodiment, in step 3, take 2.46~9.84g methylimidazole dissolve in 40~50ml deionized water and
The in the mixed solvent of 10~0ml dehydrated alcohol, is sufficiently stirred.
In the present embodiment, in step 4, the first mixed solution is placed in three-necked flask, under the atmosphere of nitrogen into
Row reflux.
In the present embodiment, in steps of 5, it stirs and heats the first mixed solution to 90 DEG C.
In the present embodiment, in step 7, third mixed solution flows back 5~10 h under 90 DEG C of nitrogen atmosphere.
In the present embodiment, in step 8, novel ferro-cobalt based super capacitor electrode material is hexagon Co-Fe nanometers
Material prepares Co-Fe base two-dimensional nano piece using efficient backflow method, has superelevation specific capacitance, and good cyclical stability etc. is excellent
Point.
The present invention will be made by specific embodiment below further elucidated above:
Embodiment 1
A kind of method of novel novel ferro-cobalt based super capacitor electrode material, comprising the following steps:
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g mixing is added in 50ml deionized water, it is sufficiently stirred, obtains pink solution；
3, it takes 2.46g methylimidazole to be added in 50ml deionized water, is sufficiently stirred to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 5h；
5, to be cooled to room temperature centrifugation after reaction, washing is dried to obtain hexagon Co-Fe based nano-material；Such as Fig. 1
It is shown.
Embodiment 2
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g, mixing are added the in the mixed solvent of 45ml deionized water and 5ml dehydrated alcohol, are sufficiently stirred, obtain powder
Red solution；
3, it takes 2.46g methylimidazole that the in the mixed solvent of 45ml deionized water and 5ml dehydrated alcohol is added, is sufficiently stirred
Obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 5h；
5, it to be cooled to room temperature after reaction, is centrifuged, washing is dried to obtain hexagon Co-Fe based nano-material；
Embodiment 3
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g, mixing are added in the mixed solution of 40ml deionized water and 10ml dehydrated alcohol, are sufficiently stirred, obtain powder
Red solution；
3, it takes 2.46g methylimidazole to be added in the mixed solution of 40ml deionized water and 10ml dehydrated alcohol, sufficiently stirs
It mixes to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 5h；
5, it to be cooled to room temperature after reaction, is centrifuged, washing is dried to obtain hexagon Co-Fe base nanometer plate electrode material
Material；
Embodiment 4
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g mixing is added in 50ml deionized water, it is sufficiently stirred, obtains pink solution；
3, it takes 4.92g methylimidazole to be added in 50ml deionized water, is sufficiently stirred to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 5h；
5, it to be cooled to room temperature after reaction, is centrifuged, washing is dried to obtain hexagon Co-Fe based nano-material；
Embodiment 5
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g mixing is added in 50ml deionized water, it is sufficiently stirred, obtains pink solution；
3, it takes 9.84g methylimidazole to be added in 50ml deionized water, is sufficiently stirred to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 5h；
5, it to be cooled to room temperature after reaction, is centrifuged, washing is dried to obtain hexagon Co-Fe based nano-material；
Embodiment 6
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O crystal and FeCl2·4H2O crystal, CoCl2·6H2O and FeCl2·4H2The material ratio of O is
1.189g:0.3168g mixing is added in 50ml deionized water, it is sufficiently stirred, obtains pink solution；
3, it takes 2.46g methylimidazole to be added in 50ml deionized water, is sufficiently stirred to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, in nitrogen
It flows back under the atmosphere of gas, be vigorously stirred and be heated to 90 DEG C, then methylimidazole solution is added in three-necked flask, at 90 DEG C
Nitrogen atmosphere under efficient backflow 10h；
5, it to be cooled to room temperature after reaction, is centrifuged, washing is dried to obtain hexagon Co-Fe base nanometer plate electrode material
Material；
Embodiment 7
1, it takes 100ml deionized water to be passed through nitrogen 30min, excludes some CO in water3 2-；
2, CoCl is taken2·6H2O and FeCl2·4H2The material ratio of O be 1.189g:0.3168g, mixing be added 50 ml go from
It in sub- water, is sufficiently stirred, obtains pink solution；
3, it takes 4.92g methylimidazole to be added in 50ml deionized water, is sufficiently stirred to obtain white solution；
4, by CoCl2·6H2O and FeCl2·4H2The pink solution that O is mixed to get is transferred in three-necked flask, and is used
The nickel foam of 1*1cm is suspended in solution by rope, is flowed back under the atmosphere of nitrogen, is vigorously stirred and is heated to 90 DEG C, then
Methylimidazole solution is added in three-necked flask, the efficient backflow 5h under 90 DEG C of nitrogen atmosphere；
5, nickel foam is taken out after reacting end and being cooled to room temperature, washing dried foam nickel obtains hexagon Co-Fe base
Nanometer sheet electrode material, as shown in Figure 2；
Embodiment 8
The preparation of Co-Fe electrode slice: Co-Fe based nano-material prepared by embodiment 1, acetylene black, binder are according to matter
For amount than being that 7:2:1 is mixed, mixing wears into the nickel foam on piece that uniform sizing material is applied to 1*2cm after suitable dehydrated alcohol is added,
It takes out after being dried in vacuo 1h at 80 DEG C, and is compacted under 10MPa pressure, continue to be dried in vacuo 12h, Co-Fe electrode slice is made.
The Co-Fe base electrode piece prepared is assembled into standard three electrode and carries out electrochemical property test, wherein platinum electrode
For to electrode, calomel electrode is reference electrode, electrolyte 6MKOH.From figure 3, it can be seen that cyclic voltammetry curve is closed, and have
Have apparent oxidation peak and reduction peak, illustrate that Co-Fe electrode material of the present invention has good fake capacitance, in addition with sweep speed
Increasing, the current potential of oxidation peak towards corrigendum is mobile, and oxidation peak is mobile towards more negative current potential, illustrate under conditions of height sweeps speed,
There are polarization phenomena for Co-Fe electrode material.It is calculated by Fig. 4 constant current charge-discharge curve, the specific volume of Co-Fe electrode material
Amount assigns 1000F/g in 1A/g current density, is significantly higher than the specific capacity of the Ni-Co of conventional hydrothermal method preparation
(CN106057482, specific capacity about 600F/g under 1A/g current density), wherein C=It/mV, C are specific capacity, and I is electric current,
T is discharge time, and m is active material quality, and V is voltage range.
The above is only a preferred embodiment of the present invention, does not play the role of any restrictions to the present invention.Belonging to any
Those skilled in the art, in the range of not departing from technical solution of the present invention, to the invention discloses technical solution and
Technology contents make the variation such as any type of equivalent replacement or modification, belong to the content without departing from technical solution of the present invention, still
Within belonging to the scope of protection of the present invention.
Claims (11)
1. a kind of novel ferro-cobalt based super capacitor electrode material, which is characterized in that the novel ferro-cobalt based super capacitor electricity
Pole material is two-dimensional layered structure, and shape is sheet regular hexagon.
2. novel ferro-cobalt based super capacitor electrode material according to claim 1, which is characterized in that the novel ferro-cobalt
The side length of based super capacitor electrode material is 1-2um.
3. novel ferro-cobalt based super capacitor electrode material according to claim 1, which is characterized in that the novel ferro-cobalt
The active matter quality of based super capacitor electrode material is less than 2mg, thickness is less than 100nm and capacitor is greater than 1000F/g, described
Active matter is ferro-cobalt bimetallic nano material.
4. a kind of preparation method of novel ferro-cobalt based super capacitor electrode material, which comprises the following steps:
Step 1: nitrogen is passed through into deionized water；
Step 2: taking CoCl2·6H2O crystal and FeCl2·4H2O crystal is placed in a part of deionized water and dehydrated alcohol
In the mixed solvent forms the first mixed solution；
Step 3: taking methylimidazole to dissolve in the in the mixed solvent of deionized water and dehydrated alcohol described in another part, form second
Mixed solution；
Step 4: first mixed solution being placed in a beaker, is flowed back；
Step 5: stirring and heat first mixed solution；
Step 6: second mixed solution being slowly added in first mixed solution, to form third mixed solution；
Step 7: flowing back to the third mixed solution；
Step 8: the step that the third mixed solution is successively centrifuged, is washed and is dried obtains the novel super electricity of ferro-cobalt base
Container electrode material.
5. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 1,100ml deionized water is taken to lead to 30min nitrogen, excludes some CO in water3 2-。
6. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 2, the CoCl2·6H2O and FeCl2·4H2The material ratio of O is 1.189g:0.3168g, and 40~50ml is dissolved in mixing
The in the mixed solvent of dehydrated alcohol described in the deionized water and 10~0ml, is sufficiently stirred.
7. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 3, methylimidazole described in 2.46~9.84g is taken to dissolve in anhydrous described in deionized water and 10~0ml described in 40~50ml
The in the mixed solvent of ethyl alcohol, is sufficiently stirred.
8. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 4, first mixed solution is placed in three-necked flask, is flowed back under the atmosphere of nitrogen.
9. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 5, stirs and heat first mixed solution to 90 DEG C.
10. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 7, the third mixed solution flows back 5~10h under 90 DEG C of nitrogen atmosphere.
11. the preparation method of novel ferro-cobalt based super capacitor electrode material according to claim 4, which is characterized in that
In step 8, the novel ferro-cobalt based super capacitor electrode material is hexagon Co-Fe nano material.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150068737A (en) * | 2013-12-12 | 2015-06-22 | 에쓰대시오일 주식회사 | Electorde material containing multi-element metal oxide deposited electrode for supercapacitor and preparation method thereof |
| CN105964257A (en) * | 2016-05-04 | 2016-09-28 | 北京化工大学 | Two-dimensional porous carbon skeletal nano-material and preparation method thereof |
| KR20180102177A (en) * | 2016-06-21 | 2018-09-14 | 산요오도꾸슈세이꼬 가부시키가이샤 | Cathode material for power storage device |
| CN108987121A (en) * | 2018-07-26 | 2018-12-11 | 电子科技大学 | A kind of quick method for preparing NiCo-LDH electrode material for super capacitor |
| CN109065895A (en) * | 2018-07-26 | 2018-12-21 | 北京化工大学常州先进材料研究院 | The preparation of iron cobalt codope carbon nitrogen core-shell particles material and its application in terms of electro-catalysis |
| CN109119250A (en) * | 2018-07-20 | 2019-01-01 | 江苏大学 | CoFe-LDH/ polypyrrole/graphite oxide trielement composite material preparation method |
| CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
-
2019
- 2019-03-06 CN CN201910167660.1A patent/CN110164705B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20150068737A (en) * | 2013-12-12 | 2015-06-22 | 에쓰대시오일 주식회사 | Electorde material containing multi-element metal oxide deposited electrode for supercapacitor and preparation method thereof |
| CN105964257A (en) * | 2016-05-04 | 2016-09-28 | 北京化工大学 | Two-dimensional porous carbon skeletal nano-material and preparation method thereof |
| KR20180102177A (en) * | 2016-06-21 | 2018-09-14 | 산요오도꾸슈세이꼬 가부시키가이샤 | Cathode material for power storage device |
| CN109119250A (en) * | 2018-07-20 | 2019-01-01 | 江苏大学 | CoFe-LDH/ polypyrrole/graphite oxide trielement composite material preparation method |
| CN108987121A (en) * | 2018-07-26 | 2018-12-11 | 电子科技大学 | A kind of quick method for preparing NiCo-LDH electrode material for super capacitor |
| CN109065895A (en) * | 2018-07-26 | 2018-12-21 | 北京化工大学常州先进材料研究院 | The preparation of iron cobalt codope carbon nitrogen core-shell particles material and its application in terms of electro-catalysis |
| CN109289852A (en) * | 2018-10-26 | 2019-02-01 | 天津大学 | Cobalt-iron oxide hollow nano cage material, preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 王婵娜等: "《Co-Fe-Pd纳米粒子的可控制备及其氧还原催化性能》", 《化工学报》 * |
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