CN109273274A - A kind of high-specific surface area NiMnO3Electrode material and its preparation method and application - Google Patents
A kind of high-specific surface area NiMnO3Electrode material and its preparation method and application Download PDFInfo
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- CN109273274A CN109273274A CN201811109904.2A CN201811109904A CN109273274A CN 109273274 A CN109273274 A CN 109273274A CN 201811109904 A CN201811109904 A CN 201811109904A CN 109273274 A CN109273274 A CN 109273274A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 title abstract description 35
- 239000007772 electrode material Substances 0.000 claims abstract description 35
- 239000011259 mixed solution Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 20
- 229910005798 NiMnO3 Inorganic materials 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000003990 capacitor Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical group [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims 1
- 238000003682 fluorination reaction Methods 0.000 claims 1
- WTHDKMILWLGDKL-UHFFFAOYSA-N urea;hydrate Chemical compound O.NC(N)=O WTHDKMILWLGDKL-UHFFFAOYSA-N 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
Classifications
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- 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
- H01G11/22—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
-
- 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
- H01G11/84—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)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention relates to a kind of high-specific surface area NiMnO3Electrode material and its preparation method and application belongs to electrode material field.A kind of high-specific surface area NiMnO3Potassium permanganate, nickel nitrate, urea and ammonium fluoride are dissolved in water and form mixed solution by the preparation method of electrode material；Mixed solution is placed in microwave hydrothermal reaction kettle, 2h~5h is reacted at 120 DEG C~200 DEG C and obtains powder；Powder is heat-treated under air conditions, both.The NiMnO prepared using method of the invention3Electrode material is flower-like nanometer piece, possesses higher specific surface area, containing more crystal defect, increases the effective active site of material, provides more sites for materials from oxidizing reduction, inherently changes and improve its capacitance characteristic.
Description
Technical field
The present invention relates to a kind of high-specific surface area NiMnO3Electrode material and its preparation method and application belongs to electrode material
Field.
Background technique
With weather it is continuous deteriorate, a large amount of uses of the energy, look for a kind of efficient energy storage technology and be subjected to various countries
The great attention of researcher.Supercapacitor has more higher than traditional capacitor as a kind of novel energy storage device
Energy density, power density more higher than battery and cycle life.Main devices one of of the electrode material as supercapacitor,
Research at present is concentrated mainly on three aspects: transition group metallic oxide, carbon material and conducting polymer.Magnesium-yttrium-transition metal oxidation
Object belongs to fake capacitance electrode material, redox reaction occurs by material surface since it stores energy, so relative to carbon
Material, transition group metallic oxide possess higher specific volume；During continuous charge/discharge, transition group metallic oxide shape
It is not susceptible to change, therefore possesses better cycle life relative to conducting polymer.Most study is transition group gold at present
Belong to oxide electrode material.
However NiMnO3As one of super capacitor material, correlative study is less, and the method for promoting material mainly mentions
It rises the electric conductivity of material and increases the specific surface area of material.It is mainly at present NiMnO in these two aspects research3With high conductivity
Material cladding promotes the chemical property of material；It on the other hand is exactly to study NiMnO3Material itself, by adjusting material morphology
Increase specific surface area, effective active site increases, and redox reaction occurs and increases, and storage charge capability increases, and then is promoted
The performance of material.
Summary of the invention
In order to improve NiMnO3The chemical property of material, inherently improves its capacitance characteristic, and the present invention devises one
Kind can simply, quickly prepare the flower-like nanometer piece NiMnO of high-specific surface area3The preparation method of electrode material.Mesh of the present invention
Be the provision of a kind of easy to operate, yield is higher, prepares the flower-shape Ni MnO of supercapacitor high-specific surface area3Electrode material
The preparation method of material.
A kind of high-specific surface area NiMnO3The preparation method of electrode material, by potassium permanganate, nickel nitrate, urea and ammonium fluoride
It is dissolved in water and forms mixed solution；Mixed solution is placed in microwave hydrothermal reaction kettle, 2h~5h is reacted at 120 DEG C~200 DEG C, instead
It is cooling that room temperature should be finished, stood, eccentric cleaning, it is dry, obtain powder；Powder is heat-treated under air conditions, both, institute
State heat treatment condition are as follows: 350 DEG C~650 DEG C are warming up to from room temperature with 2 DEG C/min~5 DEG C/min heating rate, heat preservation 1h~
After 2h, room temperature is cooled to the furnace.
Wherein, the concentration of urea is 0.4mol/L~1.0mol/L in the mixed solution, and the concentration of ammonium fluoride is
0.1mol/L~0.8mol/L, the concentration of potassium permanganate are 2.0g/L~8.5g/L；The molar ratio of potassium permanganate and nickel nitrate is
1:1~3:1.
In above-mentioned technical proposal, potassium permanganate and nickel nitrate are pressed than the original for Ni/Mn=1:1 in the preferably described mixed solution
Sub- proportional arrangement.
In above-mentioned technical proposal, potassium permanganate, nickel nitrate, urea and ammonium fluoride are dissolved in water and form mixed solution；It will mix
It closes solution to be placed in microwave hydrothermal reaction kettle, reacts 2h~5h at 120 DEG C~200 DEG C in microwave hydrothermal reactor.
Preferably, at room temperature, potassium permanganate, nickel nitrate, urea and ammonium fluoride are dissolved in after water in revolving speed is 500~700
30~60min is persistently stirred under rev/min, the mixed solution sufficiently dissolved.
Preferably, it is 30:100 in reaction kettle content volume ratio by mixed solution, it is anti-that mixed solution is placed in 100ml microwave
It answers in kettle, in microwave hydrothermal reactor, microwave heating 1h~5h under the conditions of 120 DEG C~200 DEG C is cooled to room in reactor
Temperature is taken out.
It preferably, the use of deionized water and ethanol solution in revolving speed is respectively 3500 revs/min, under the conditions of time 4min, from
The heart cleans 3 times；Powder dry 12h, taking-up under the conditions of 60 DEG C are ground to required partial size.
Preferably, mixed solution is placed in microwave hydrothermal reaction kettle, reacts 3h at 160 DEG C.
Preferably, 450 DEG C are warming up to from room temperature with the heating rate of 2 DEG C/min, after keeping the temperature 2h, cool to room temperature with the furnace.
Preferably, the concentration of urea is 0.4mol/L in the mixed solution, and the concentration of ammonium fluoride is 0.2mol/L, Gao Meng
The concentration of sour potassium is 5.3g/L；The concentration of nickel nitrate is 9.7g/L.
It is a further object of the present invention to provide high-specific surface area NiMnO prepared by the above method3Electrode material.
NiMnO of the present invention3Electrode material is flower-like nanometer piece.
NiMnO of the present invention3Electrode material is porous material, and aperture is 2~35nm.
NiMnO of the present invention3The specific surface area of electrode material is 74.9m2/ g,
It is yet another object of the invention to provide NiMnO prepared by the above method3Electrode material is as super capacitor electrode
The application of pole material.
The invention has the benefit that the NiMnO prepared using method of the invention3Electrode material is flower-like nanometer piece,
Possess higher specific surface area, containing more crystal defect, increase the effective active site of material, is gone back to be materials from oxidizing
Original provides more sites, inherently changes and improves its capacitance characteristic.Meanwhile having good electric conductivity and circulation steady
It is qualitative, it is a kind of comparatively ideal electrode material for super capacitor.NiMnO3 electrode material prepared by the present invention is easy to operate, substantially
Degree saves time and energy consumption, and process is few, and equipment investment is few, and repeatability is good, convenient for solving the problems, such as that large-scale production is difficult.
Detailed description of the invention
Fig. 1 (a) and (b) are high-specific surface area NiMnO prepared by the embodiment of the present invention 13The SEM photograph of electrode material；
By can be seen that prepared NiMnO under Fig. 1 (a) low power lens3The pattern of electrode material is made of single floriform appearance,
It does not include other patterns；As can be seen that flower-like structure is made of many nanometer sheets under Fig. 1 (b) high power lens, this structure greatly increases
Big material specific surface area.
Fig. 2 (a)~(d) is high-specific surface area NiMnO prepared by the embodiment of the present invention 13The TEM photo of electrode material；
Fig. 2 (a) and (b) further demonstrate NiMnO3Electrode material flower-like nanometer piece pattern；From selective electron diffraction figure (Fig. 2 (c))
It sees, material has good diffraction ring, it was demonstrated that material prepared has good crystallinity；Fig. 2 (d) is after material morphology amplifies
Local diffraction fringe, be respectively that 0.492nm, 0.293nm and 0.208nm correspond to crystal face and be by measuring spacing of lattice
(111), (121) and (- 111) as a result match with XRD result.
Fig. 3 is high-specific surface area NiMnO prepared by the embodiment of the present invention 13The X ray diffracting spectrum of electrode material；From
Fig. 3 can be seen that diffraction maximum mainly corresponds to NiMnO in 28.8 °, 39.5 °, 42.8 °, 49.1 °, 59.6 °, 65.0 °, 78.3 °3
(JCPDS#75-2089) crystal face (110), (121), (- 110), (120), (220), (231), (- 211), illustrate NiMnO3Material
It successfully prepares and has good crystallinity.
Fig. 4 (a) and (b) are high-specific surface area NiMnO prepared by the embodiment of the present invention 13The specific surface area of electrode material
Test result picture；Fig. 4 is NiMnO3The specific surface area test result picture of electrode material.Left figure is the N of material2Absorption/desorption
Curve, material is typical IV type curve as seen from the figure, and H3 type hysteresis loop further demonstrates flaky nanometer structure, compares table
Area is 74.9m2/g；Right figure is the pore-size distribution of material, it can be seen that aperture is mainly distributed on 2.0 between 35nm.
Fig. 5 is high-specific surface area NiMnO prepared by the embodiment of the present invention 13Material is as electrode material different scanning speed
Cyclic voltammetry curve under degree.As seen in Figure 5, material from it is low sweep speed to height sweep speed transformation when, material prepared circulation volt
Pacify curve shape there is no biggish change, shows that material has good high rate performance and higher specific volume, there is oxidation
Reduction peak illustrates that material belongs to fake capacitance material.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
Embodiment 1
1) 1mmol nickel nitrate, 1mmol potassium permanganate, 6mmol ammonium fluoride and 12mmol urea precise are poured into 30ml
It in deionized water, is placed on magnetic stirring apparatus at room temperature, with 700 revs/min of revolving speed, stirs 30min, obtain uniformly mixed molten
Liquid；
2) obtained mixed solution is poured into 100ml microwave hydrothermal reaction kettle, is put into microwave hydrothermal reactor and carries out
Hydro-thermal reaction；Hydrothermal condition is to react 3h, reaction kettle is cooled to room in the reactor after end of reaction at a temperature of 160 DEG C
Temperature is taken out；
3) by the solution left standstill 12h after obtained hydro-thermal reaction, eccentric cleaning is then carried out, is 3500 revs/min in revolving speed,
Under the conditions of time is 4min, it is respectively washed repeatedly with deionized water and ethyl alcohol, by obtained powder in 60 DEG C of freeze-day with constant temperature 12h,
Grinding is taken out, is 100~300nm by powder mull to average grain diameter；
4) powder after grinding is put into Muffle furnace under air conditions and is heat-treated, hot program are as follows: from room temperature with 2
DEG C/heating rate of min is warming up to 450 DEG C, after keeping the temperature 2h, cools to room temperature with the furnace, the high-ratio surface of black is obtained after taking-up
Long-pending flower-like nanometer piece NiMnO3Powder.
Embodiment 2
1) 1mmol nickel nitrate, 2mmol potassium permanganate, 6mmol ammonium fluoride and 12mmol urea precise are poured into 30ml
It in deionized water, is placed on magnetic stirring apparatus at room temperature, with 700 revs/min of revolving speed, stirs 30min, obtain uniformly mixed molten
Liquid；
2) obtained mixed solution is poured into 100ml microwave hydrothermal reaction kettle, is put into microwave hydrothermal reactor and carries out
Hydro-thermal reaction；Hydrothermal condition is to react 3h, reaction kettle is cooled to room in the reactor after end of reaction at a temperature of 160 DEG C
Temperature is taken out；
3) by the solution left standstill 12h after obtained hydro-thermal reaction, eccentric cleaning is then carried out, is 3500 revs/min in revolving speed,
Under the conditions of time is 4min, it is respectively washed repeatedly with deionized water and ethyl alcohol, by obtained powder in 60 DEG C of freeze-day with constant temperature 12h,
Grinding is taken out, is 100~300nm by powder mull to average grain diameter；
4) powder after grinding is put into Muffle furnace under air conditions and is heat-treated, hot program are as follows: from room temperature with 2
DEG C/heating rate of min is warming up to 450 DEG C, after keeping the temperature 2h, cools to room temperature with the furnace, the high-ratio surface of black is obtained after taking-up
Long-pending flower-like nanometer piece NiMnO3Powder.
Embodiment 3
1) 1mmol nickel nitrate, 1mmol potassium permanganate, 6mmol ammonium fluoride and 12mmol urea precise are poured into 30ml
It in deionized water, is placed on magnetic stirring apparatus at room temperature, with 700 revs/min of revolving speed, stirs 30min, obtain uniformly mixed molten
Liquid；
2) obtained mixed solution is poured into 100ml microwave hydrothermal reaction kettle, is put into microwave hydrothermal reactor and carries out
Hydro-thermal reaction；Hydrothermal condition is to react 4h, reaction kettle is cooled to room in the reactor after end of reaction at a temperature of 160 DEG C
Temperature is taken out；
3) by the solution left standstill 12h after obtained hydro-thermal reaction, eccentric cleaning is then carried out, is 3500 revs/min in revolving speed,
Under the conditions of time is 4min, it is respectively washed repeatedly with deionized water and ethyl alcohol, by obtained powder in 60 DEG C of freeze-day with constant temperature 12h,
Grinding is taken out, is 100~300nm by powder mull to average grain diameter；
4) powder after grinding is put into Muffle furnace under air conditions and is heat-treated, hot program are as follows: from room temperature with 2
DEG C/heating rate of min is warming up to 450 DEG C, after keeping the temperature 2h, cools to room temperature with the furnace, the high-ratio surface of black is obtained after taking-up
Long-pending flower-like nanometer piece NiMnO3Powder.
Application examples
Porous nano NiMnO prepared by embodiment 13Material, conductive agent active carbon (XC-72), binder [polyvinylidene fluoride
Alkene (PVDF) and N-Methyl pyrrolidone (NMP) take mass ratio as the mixed liquor of 1:4 formation] be in mass ratio 8:1:1 proportion
Mixing is slurried, and is coated in nickel foam and is prepared into electrode；Electrolyte is 6mol/L KOH solution, using three electrode measurement systems.
Claims (10)
1. a kind of high-specific surface area NiMnO3The preparation method of electrode material, it is characterised in that: by potassium permanganate, nickel nitrate, urea
Water, which is dissolved in, with ammonium fluoride forms mixed solution；Mixed solution is placed in microwave hydrothermal reaction kettle, is reacted at 120 DEG C~200 DEG C
2h~5h, end of reaction room temperature is cooling, stands, eccentric cleaning, dry, obtains powder；Powder is subjected to hot place under air conditions
Reason, both, the heat treatment condition are as follows: be warming up to 350 DEG C~650 from room temperature with 2 DEG C/min~5 DEG C/min heating rate
DEG C, after keeping the temperature 1h~2h, cool to room temperature with the furnace；
Wherein, the concentration of urea is 0.4mol/L~1.0mol/L in the mixed solution, and the concentration of ammonium fluoride is 0.1mol/L
~0.8mol/L, the concentration of potassium permanganate are 2.0g/L~8.5g/L；The molar ratio of potassium permanganate and nickel nitrate is 1:1~3:1.
2. according to the method described in claim 1, it is characterized by: at room temperature, by potassium permanganate, nickel nitrate, urea and fluorination
Ammonium is dissolved in after water be 500~700 revs/min in revolving speed under persistently stir 30~60min, the mixed solution sufficiently dissolved.
3. according to the method described in claim 1, it is characterized by: by mixed solution in reaction kettle content volume ratio be 30:
100, mixed solution is placed in 100ml microwave reaction kettle, in microwave hydrothermal reactor, microwave under the conditions of 120 DEG C~200 DEG C
1h~5h is heated, is cooled to room temperature in reactor, is taken out.
4. according to the method described in claim 1, it is characterized by: being in revolving speed using deionized water and ethanol solution respectively
3500 revs/min, under the conditions of time 4min, eccentric cleaning 3 times；Powder dry 8 under the conditions of 20 DEG C~100 DEG C~for 24 hours, taking-up is ground
It is milled to required partial size.
5. according to the method described in claim 1, it is characterized by: mixed solution is placed in microwave hydrothermal reaction kettle, 160 DEG C
Lower reaction 3h.
6. according to the method described in claim 1, it is characterized by: the heat treatment condition are as follows: from room temperature with the liter of 2 DEG C/min
Warm speed is warming up to 450 DEG C, after keeping the temperature 2h, cools to room temperature with the furnace.
7. according to the method described in claim 1, it is characterized by: in the mixed solution urea concentration be 0.4mol/L,
The concentration of ammonium fluoride is 0.2mol/L, and the concentration of potassium permanganate is 5.3g/L；The concentration of nickel nitrate is 9.7g/L.
8. high-specific surface area NiMnO made from any one of claim 1~7 the method3Electrode material.
9. electrode material according to claim 8, it is characterised in that: the NiMnO3Electrode material is porous material, aperture
For 2~35nm；The NiMnO3The specific surface area of electrode material is 74.9m2/g。
10. NiMnO described in claim 83Application of the electrode material as electrode material for super capacitor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811109904.2A CN109273274B (en) | 2018-09-21 | 2018-09-21 | NiMnO3 electrode material with high specific surface area and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811109904.2A CN109273274B (en) | 2018-09-21 | 2018-09-21 | NiMnO3 electrode material with high specific surface area and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN109273274A true CN109273274A (en) | 2019-01-25 |
| CN109273274B CN109273274B (en) | 2020-07-21 |
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Cited By (5)
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| CN111724996A (en) * | 2020-05-18 | 2020-09-29 | 安徽大学 | Flexible core-shell heterostructure cathode material and preparation method and application thereof |
| CN112875765A (en) * | 2021-01-18 | 2021-06-01 | 欣旺达电动汽车电池有限公司 | NiMnO3Preparation method of bimetal oxide and energy storage device |
| CN113828326A (en) * | 2021-10-20 | 2021-12-24 | 济南市中两山生态科技中心 | Flue gas denitration catalyst and preparation method thereof |
| CN116102088A (en) * | 2022-11-30 | 2023-05-12 | 四川兴储能源科技有限公司 | Negative electrode material of lamellar sodium ion battery and preparation method thereof |
| CN116199277A (en) * | 2023-04-28 | 2023-06-02 | 江苏正力新能电池技术有限公司 | Manganese-nickel bimetallic compound and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111724996A (en) * | 2020-05-18 | 2020-09-29 | 安徽大学 | Flexible core-shell heterostructure cathode material and preparation method and application thereof |
| CN111724996B (en) * | 2020-05-18 | 2023-08-25 | 安徽大学 | Flexible core-shell heterostructure anode material and preparation method and application thereof |
| CN112875765A (en) * | 2021-01-18 | 2021-06-01 | 欣旺达电动汽车电池有限公司 | NiMnO3Preparation method of bimetal oxide and energy storage device |
| CN112875765B (en) * | 2021-01-18 | 2023-05-05 | 欣旺达电动汽车电池有限公司 | NiMnO 3 Preparation method of bimetal oxide and energy storage device |
| CN113828326A (en) * | 2021-10-20 | 2021-12-24 | 济南市中两山生态科技中心 | Flue gas denitration catalyst and preparation method thereof |
| CN113828326B (en) * | 2021-10-20 | 2022-04-01 | 烟台百川汇通科技有限公司 | Flue gas denitration catalyst and preparation method thereof |
| CN116102088A (en) * | 2022-11-30 | 2023-05-12 | 四川兴储能源科技有限公司 | Negative electrode material of lamellar sodium ion battery and preparation method thereof |
| CN116199277A (en) * | 2023-04-28 | 2023-06-02 | 江苏正力新能电池技术有限公司 | Manganese-nickel bimetallic compound and preparation and application thereof |
| CN116199277B (en) * | 2023-04-28 | 2023-08-11 | 江苏正力新能电池技术有限公司 | Manganese-nickel bimetallic compound and preparation and application thereof |
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