CN109671574A - A kind of MnCo2O4Nanometer ball particle and preparation method thereof and the application in supercapacitor - Google Patents
A kind of MnCo2O4Nanometer ball particle and preparation method thereof and the application in supercapacitor Download PDFInfo
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- CN109671574A CN109671574A CN201910088454.1A CN201910088454A CN109671574A CN 109671574 A CN109671574 A CN 109671574A CN 201910088454 A CN201910088454 A CN 201910088454A CN 109671574 A CN109671574 A CN 109671574A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of MnCo2O4Nanometer ball particle, is prepared by four acetate hydrate manganese, four acetate hydrate cobalts, complexing agent and surfactant；Four acetate hydrate manganese and four acetate hydrate cobalt mixing and water addings are formed into homogeneous solution；Polyacrylic acid and peregal O-20 are added, homogeneous mixture solotion is formed；It is then transferred in reaction kettle and reacts, product is filtered, washed, is dried, and MnCo is obtained after calcining2O4Nanometer ball particle, prepared MnCo2O4Nanometer ball particle is used to prepare the positive electrode of supercapacitor, and preparation method of the present invention is simple to operation, and raw material sources are abundant, at low cost, environmentally protective, gained MnCo2O4Nanometer ball particle, partial size is small, and dimensional homogeneity is good, and degree of aggregation is small, is prepared into the positive electrode of supercapacitor, and specific capacitance is high, can satisfy the needs for preparing high-performance super capacitor device.
Description
Technical field
The present invention relates to a kind of MnCo2O4Nanometer ball particle and preparation method thereof and the application in supercapacitor, belong to
Electrode material preparation field.
Background technique
It is largely used as coal, petroleum, natural gas obtain, has resulted in serious global problem of environmental pollution, there is an urgent need to
Invent a kind of energy-storage system device of green high-efficient.Supercapacitor is to utilize the surface of electrode material positive and negative anodes and electrolyte electricity
Chemical process stores a kind of energy-storage travelling wave tube of charge, also referred to as electrochemical capacitor.According to energy storage mechnism difference, mainly there is two
The supercapacitor of seed type, one is double layer capacitor, another kind is Faraday pseudo-capacitance device.Double layer capacitor is logical
Reversible Electrostatic Absorption of the electrolyte ion in surface of active material is crossed to store charge, important is carbon materials；Faraday
Pseudocapacitors are to store energy by quick, the reversible redox reaction on active electrode material surface, and important is lead
Electric high molecular material, transition metal composite material.The performance of ultracapacitor device depends on the preparation of electrode material, electrode
Technology and with the matched electrolyte of electrode material etc., wherein electrode material is the key factor for determining device performance.
In recent years, new electrode material is developed, is the break through direction for improving super capacitor energy density.Relative to carbon materials
Material, transition metal element usually have multiple oxidation state, can be stored by redox reaction in electrochemical energy storage
More energy.Mn, Co metal dual metal oxide have specific capacity height, work as Faraday pseudo-capacitance device positive electrode
The characteristics of voltage range is wide, good cycling stability, and it is at low cost environmental-friendly, promise to be next-generation most potential height
One of performance electrode material for super capacitor.
MnCo2O4It is a kind of bimetallic oxide with spinel structure, the MnCo of different-shape2O4, such as nanometer linear array
Column, nanometer sheet, rodlike etc., have been prepared out, and coprecipitation reaction and subsequent heat treatment are such as carried out at room temperature, in three-dimensional
It grown porous MnCo on Ni foam2O4Nanometer stick array, or nanoscale MnCo is prepared using microwave heating synthetic technology2O4,
And the nanometer MnCo that can be used for super capacitor anode material, but prepared at present2O4Partial size is big, specific surface area
Small, preparation method is cumbersome and reaction condition is not mild.
Summary of the invention
In order to solve deficiency present in existing technology of preparing, the purpose of the present invention is to provide one kind to reach with partial size
7.5nm, and the extraordinary MnCo of diameter uniformity2O4Nanosphere preparation method of granules, it is former using hydro-thermal method simple to operation
Expect abundance, at low cost, environmentally protective, gained MnCo2O4Nanometer ball particle, partial size is small, and dimensional homogeneity is good, and degree of aggregation is small,
It is prepared into the positive electrode of supercapacitor, specific capacitance is high, can satisfy the needs for preparing high-performance super capacitor device.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of MnCo2O4Nanometer ball particle, is prepared: four acetate hydrate manganese (Mn (CH by following raw material3COO)2·
4H2O), four acetate hydrate cobalt (Co (CH3COO)2·4H2O), complexing agent and surfactant, wherein four acetate hydrate manganese, four
The molar ratio of acetate hydrate cobalt, complexing agent and surfactant are as follows: 1-4:2-8:3-15:0.5-4.Preferably, four acetate hydrate
Manganese, four acetate hydrate cobalts, complexing agent and surfactant molar ratio be 2:4:6:1.
MnCo prepared by the present invention2O4Nanosphere grain diameter is small, and up to 7.5nm or so, and dimensional homogeneity is good, reunites
It spends small, is used to prepare the positive electrode of supercapacitor, specific capacitance is high, and stable circulation is good.
Further, complexing agent is the polyacrylic acid (PAA) that molecular weight is 2000-5000；Surfactant is paregal O-
20。
It is surfactant with paregal O -20 using polyacrylic acid as complexing agent, raw material can be effectively ensured and be normally carried out instead
It answers, with processability height, high-quality MnCo2O4Nanometer ball particle.
The present invention also provides a kind of MnCo2O4The preparation method of nanometer ball particle:
1) each raw material is weighed by above-mentioned molar ratio；
2) four acetate hydrate manganese and four acetate hydrate cobalts are taken, add water ultrasonic agitation dispersion 20-25min at homogeneous solution standby
With；
3) complexing agent and surfactant are taken, addition continues ultrasonic agitation dispersion 25- into the homogeneous solution in step 2)
35min forms mixed solution, spare；
4) mixed solution is transferred in reaction kettle, is reacted, after reaction natural cooling, taken out in reaction kettle
Gallbladder removes supernatant, is transferred in centrifuge tube and is centrifugally separating to obtain solid particle, solid particle is used deionized water and nothing respectively
Water-ethanol puts 75-85 DEG C of air dry oven, dry 6h into after respectively washing repeatedly 3-5 times；
5) solid particle after drying is put into quartz boat, in air atmosphere, with the heating rate liter of 3-5 DEG C/min
Natural cooling to calcining 3-5h, preferably 425 DEG C calcining 4h after 400-450 DEG C, after naturally cooling to 20-30 DEG C for temperature to obtain the final product
MnCo2O4Nanometer ball particle.
Abundant raw material needed for preparation process, is conveniently easy to get, and does not generate toxic and harmful gas, environmentally protective；It is easy to operate, instead
Mild condition is answered, is suitble to large-scale production, has a good application prospect.
Further, the additional amount of water is that 15-60mL water is added in every tetra- acetate hydrate manganese of 1mmol in step 2)；Step 4)
Middle reaction kettle is the stainless steel cauldron of polytetrafluoroethylliner liner, and the time reacted in a kettle is 10-18h, preferably
For 14h, reaction temperature is 100-140 DEG C, preferably 125 DEG C, is cooled to be cooled to 20-30 DEG C.
The present invention has accurately selected addition deionization by selection manganese acetate, cobalt acetate, complexing agent and surfactant
The volume of water, it is determined that hydrothermal reaction condition and calcination temperature, to guarantee prepared MnCo2O4Nanosphere grain diameter is small,
Uniform diameter.
The present invention also provides a kind of supercapacitor, positive electrode is by above-mentioned MnCo2O4Nanosphere particle preparation obtains
It arrives.
By MnCo of the invention2O4Nanosphere particle preparation at supercapacitor positive electrode, it is comprehensive by chemical property
Test is closed, under the current density of 1A/g, specific capacitance is high, reaches 765.68F/g, after charge and discharge cycles 4000 times, moreover it is possible to protect
It holds to 87.26%, stable circulation is good.
Detailed description of the invention
Fig. 1 is MnCo in the embodiment of the present invention 12O4Nanometer ball particle X ray diffracting spectrum；
Fig. 2 is MnCo in the embodiment of the present invention 12O4The electron scanning micrograph of nanometer ball particle；
Fig. 3 is MnCo in the embodiment of the present invention 12O4Super capacitor anode material prepared by nanometer ball particle is in 1A/g
Current density under constant current charge-discharge curve graph；
Fig. 4 is MnCo in the embodiment of the present invention 12O4Super capacitor anode material electrochemistry prepared by nanometer ball particle
Stable circulation test curve figure.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Four acetate hydrate cobalt of four acetate hydrate manganese of 0.3721g (2mmol) and 0.9963g (4mmol) accurately is weighed, is put into
In 60mL deionized water, ultrasonic agitation dispersion 25min forms it into homogeneous solution；Add 1.6845g (6mmol) polypropylene
Acid and 1.1995g (1mmol) surfactant paregal O -20 continue ultrasonic agitation dispersion 30min, form it into uniform mixing
Solution；Then naturally cold in 125 DEG C of reaction 14h the stainless steel cauldron of homogeneous mixture solotion transfer polytetrafluoroethylliner liner
But to 20 DEG C.It is filtered, washed, dried, later in 425 DEG C of calcining 4h, obtain MnCo2O4Nanometer ball particle.
To prepared MnCo2O4Nanometer ball particle is detected, X ray diffracting spectrum (XRD) and scanning electron microscopy
Mirror (SEM) photo difference is as depicted in figs. 1 and 2, from fig. 1, it can be seen that the position of map appearance is consistent with JCPDS 23-1237, system
Standby product out is MnCo2O4, and there is no miscellaneous peak, explanation is pure phase, without impurity, as can be seen from Figure 2, MnCo2O4Pattern be
Spherical, partial size is small, reaches 7.5nm, dimensional homogeneity is good, and degree of aggregation is small.
Embodiment 2
Tetra- acetate hydrate cobalt of tetra- acetate hydrate manganese of 0.3721g and 0.9963g accurately is weighed, is put into 60mL deionized water,
Ultrasonic agitation dispersion 25min, forms it into homogeneous solution；It adds 1.6845g polyacrylic acid and 1.1995g surfactant is flat
Flat plus O-20 continues ultrasonic agitation dispersion 30min, forms it into homogeneous mixture solotion；Then homogeneous mixture solotion is shifted poly-
The stainless steel cauldron of tetrafluoroethene liner naturally cools to 20 DEG C in 110 DEG C of reaction 10h.It is filtered, washed, dried, it
Afterwards in 400 DEG C of calcining 3h, MnCo is obtained2O4Nanometer ball particle.
Embodiment 3
Tetra- acetate hydrate cobalt of tetra- acetate hydrate manganese of 0.3721g and 0.9963g accurately is weighed, is put into 60mL deionized water,
Ultrasonic agitation dispersion 25min, forms it into homogeneous solution；It adds 1.6845g polyacrylic acid and 1.1995g surfactant is flat
Flat plus O-20 continues ultrasonic agitation dispersion 30min, forms it into homogeneous mixture solotion；Then homogeneous mixture solotion is shifted poly-
The stainless steel cauldron of tetrafluoroethene liner naturally cools to 30 DEG C in 140 DEG C of reaction 18h.It is filtered, washed, dried, it
Afterwards in 450 DEG C of calcining 5h, MnCo is obtained2O4Nanometer ball particle.
Embodiment 4
Tetra- acetate hydrate cobalt of tetra- acetate hydrate manganese of 0.3721g and 0.9963g accurately is weighed, is put into 60mL deionized water,
Ultrasonic agitation dispersion 25min, forms it into homogeneous solution；It adds 1.6845g polyacrylic acid and 1.1995g surfactant is flat
Flat plus O-20 continues ultrasonic agitation dispersion 30min, forms it into homogeneous mixture solotion；Then homogeneous mixture solotion is shifted poly-
The stainless steel cauldron of tetrafluoroethene liner naturally cools to 25 DEG C in 125 DEG C of reaction 10h.It is filtered, washed, dried, it
Afterwards in 425 DEG C of calcining 5h, MnCo is obtained2O4Nanometer ball particle.
Embodiment 5
Tetra- acetate hydrate cobalt of tetra- acetate hydrate manganese of 0.3721g and 0.9963g accurately is weighed, is put into 60mL deionized water,
Ultrasonic agitation dispersion 25min, forms it into homogeneous solution；It adds 1.6845g polyacrylic acid and 1.1995g surfactant is flat
Flat plus O-20 continues ultrasonic agitation dispersion 30min, forms it into homogeneous mixture solotion；Then homogeneous mixture solotion is shifted poly-
The stainless steel cauldron of tetrafluoroethene liner naturally cools to 28 DEG C in 110 DEG C of reaction 14h.It is filtered, washed, dried, it
Afterwards in 450 DEG C of calcining 3h, MnCo is obtained2O4Nanometer ball particle.
Performance test
By MnCo prepared by embodiment 12O4Nanometer ball particle, acetylene black and polytetrafluoroethylene (PTFE) 85:10:5 in mass ratio
Ratio mixing, be uniformly mixed, be then coated in nickel foam, 12MPa lower sheeting, be dried in vacuo at 80 DEG C, super electricity is made
The anode of container.
Using three-electrode system, platinum electrode is to electrode, and Hg/HgO electrode is as reference electrode, MnCo2O4Nanometer ball particle
Manufactured electrode is working electrode, comprehensive electrochemical test is carried out in 0~0.6V voltage range, and record result.
Constant current charge-discharge curve graph such as Fig. 3 under current density, electrochemical cycle stability test curve figure such as Fig. 4；From
For Fig. 3 it is found that under the current density of 1A/g, specific capacitance is high, reaches 765.68F/g, as can be seen from Figure 4, in charge and discharge cycles 4000
After secondary, moreover it is possible to remain to 87.26%, stable circulation is good.
Claims (10)
1. a kind of MnCo2O4Nanometer ball particle, which is characterized in that be prepared by following raw material: four acetate hydrate manganese, four hydrations
Cobalt acetate, complexing agent and surfactant, the four acetate hydrates manganese, four acetate hydrate cobalts, complexing agent and surfactant
Molar ratio are as follows: 1-4:2-8:3-15:0.5-4.
2. a kind of MnCo according to claim 12O4Nanometer ball particle, which is characterized in that the complexing agent is polypropylene
Acid.
3. a kind of MnCo according to claim 22O4Nanometer ball particle, which is characterized in that the molecular weight of the polyacrylic acid
For 2000-5000.
4. a kind of MnCo according to claim 12O4Nanometer ball particle, which is characterized in that the surfactant is average
Add O-20.
5. a kind of MnCo2O4The preparation method of nanometer ball particle, which is characterized in that be prepared by the following steps to obtain:
1) each raw material is weighed by the described in any item molar ratios of claim 1-3；
2) four acetate hydrate manganese and four acetate hydrate cobalts are taken, are added water and stirred into spare after homogeneous solution；
3) complexing agent and surfactant are taken, addition continues to stir evenly into the homogeneous solution in step 2), and it is molten to form mixing
Liquid, it is spare；
4) mixed solution is transferred in reaction kettle, is reacted, after reaction natural cooling, taken out reaction kettle liner, remove
Supernatant is removed, is transferred in centrifuge tube and is centrifugally separating to obtain solid particle, it is dry after solid particle is washed；
5) by natural cooling after the solid particle calcining after drying up to the MnCo2O4Nanometer ball particle.
6. a kind of MnCo according to claim 52O4The preparation method of nanometer ball particle, which is characterized in that institute in step 2)
The additional amount for stating water is that 15-60mL water is added in every tetra- acetate hydrate manganese of 1mmol.
7. a kind of MnCo according to claim 52O4The preparation method of nanometer ball particle, which is characterized in that institute in step 2)
The operation of stirring is stated as ultrasonic agitation dispersion 25min；The operation of stirring described in step 3) is ultrasonic agitation dispersion 30min.
8. a kind of MnCo according to claim 52O4The preparation method of nanometer ball particle, which is characterized in that institute in step 4)
The stainless steel cauldron that reaction kettle is polytetrafluoroethylliner liner is stated, the time reacted in the reaction kettle is 10-18h, instead
Answering temperature is 100-140 DEG C, described to be cooled to be cooled to 20-30 DEG C.
9. a kind of MnCo according to claim 52O4The preparation method of nanometer ball particle, which is characterized in that institute in step 5)
The operation for stating calcining is to put the solid particle after drying in quartz boat into, in air atmosphere, with the heating rate of 5 DEG C/min
3-5h is calcined after being warming up to 400-450 DEG C, naturally cools to 20-30 DEG C.
10. a kind of supercapacitor, which is characterized in that the positive electrode of the supercapacitor is as described in claim 1-9
MnCo2O4Nanosphere particle preparation obtains.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111223675A (en) * | 2020-01-13 | 2020-06-02 | 龙岩学院 | Porous nano NiFe2O4And preparation method and application thereof |
| CN115430430A (en) * | 2022-07-18 | 2022-12-06 | 西安交通大学 | MnCo 2 O 4 Preparation method of nanosphere-loaded melamine carbon foam composite material |
| CN116855813A (en) * | 2023-08-22 | 2023-10-10 | 吉林省宝利科贸有限公司 | Polyhedral nano high-entropy material and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111223675A (en) * | 2020-01-13 | 2020-06-02 | 龙岩学院 | Porous nano NiFe2O4And preparation method and application thereof |
| CN115430430A (en) * | 2022-07-18 | 2022-12-06 | 西安交通大学 | MnCo 2 O 4 Preparation method of nanosphere-loaded melamine carbon foam composite material |
| CN116855813A (en) * | 2023-08-22 | 2023-10-10 | 吉林省宝利科贸有限公司 | Polyhedral nano high-entropy material and preparation method and application thereof |
| CN116855813B (en) * | 2023-08-22 | 2024-02-09 | 吉林省宝利科贸有限公司 | Polyhedral nano high-entropy material and preparation method and application thereof |
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