CN109786712A - A kind of nickel, bismuth modified manganese dioxide positive electrode and its preparation method and application - Google Patents
A kind of nickel, bismuth modified manganese dioxide positive electrode and its preparation method and application Download PDFInfo
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- CN109786712A CN109786712A CN201910074935.7A CN201910074935A CN109786712A CN 109786712 A CN109786712 A CN 109786712A CN 201910074935 A CN201910074935 A CN 201910074935A CN 109786712 A CN109786712 A CN 109786712A
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- nickel
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- manganese dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a kind of nickel, bismuth modified manganese dioxide positive electrode and its preparation method and application.The material is prepared by following methods: potassium permanganate and hydrochloric acid being stirred evenly in deionized water, a certain amount of nickel nitrate and bismuth nitrate is then added, hydro-thermal reaction is carried out, finally obtains nickel, bismuth modified manganese dioxide powder positive electrode；The nickel, bismuth modified manganese dioxide positive electrode are suitable for Zinc ion battery.Nickel described in the invention, bismuth modified manganese dioxide positive electrode and the Zinc ion battery with the anode have preferable high rate performance, cycle performance and longer cycle life.
Description
Technical field
The invention belongs to Zinc ion battery Material Field, more particularly, to a kind of nickel, bismuth modified manganese dioxide anode
Material and its preparation method and application.
Background technique
Zinc ion battery is using zinc powder or zinc metal sheet as negative electrode material, and manganese base is that one kind of positive electrode is safe and pollution-free
Secondary cell.Manganese dioxide has the advantages that cheap and environmental-friendly, while having because of the variable valence of manganese outstanding
Ion storage performance has performance outstanding as electrode material recently on the chemical cells such as novel Zinc ion battery.
Tetravalence Mn-based material is focused primarily upon to manganese base electrode investigation of materials at present, still, the poor electric conductivity of itself and
Increasing volume change in charge and discharge process causes high rate performance difference and cycle life short, hinders it and further develops.
Summary of the invention
In view of this, the invention is directed to a kind of nickel, bismuth modified manganese dioxide positive electrode and Zinc ion battery,
To improve the high rate performance and cycle performance of manganese dioxide positive pole material, extend electrode life.
In order to achieve the above objectives, the technical solution of the invention is achieved in that
A kind of nickel, bismuth modified manganese dioxide positive electrode, it is characterised in that: the nickel, bismuth modified manganese dioxide anode material
Material is the α phase MnO that nickel element, bismuth element is added2。
Further, 0.005~0.5:0.005 of atomic ratio~0.5:1 of the nickel element, bismuth element and manganese element.
Further, the nickel, bismuth modified manganese dioxide positive electrode pattern be nanometer rods, nano wire or nanobelt.
Further, the draw ratio of the nanometer rods, nano wire or nanobelt be 30~100:1, diameter be 30~
110nm。
The preparation method of nickel, bismuth modified manganese dioxide positive electrode, it is characterised in that: by potassium permanganate and hydrochloric acid go from
It is stirred evenly in sub- water, nickel nitrate and bismuth nitrate is then added, is prepared using hydro-thermal reaction.
Further, in the nickel nitrate and bismuth nitrate in nickel element, bismuth element and potassium permanganate manganese element atomic ratio
For 0.005~0.5:0.005~0.5:1.
Further, the atomic ratio of manganese element is 0.1:0.1:1 in the nickel element, bismuth element and potassium permanganate.
Further, the dosage of the potassium permanganate is 7mmol；Concentration of hydrochloric acid is 36%, dosage 2.5ml；Nickel nitrate
Dosage is 0.7mmol；Deionized water dosage is 70ml.
Further, the reaction temperature of the hydro-thermal reaction is 160 DEG C, and the reaction time is 10 hours.
The nickel, bismuth modified manganese dioxide positive electrode are used for Zinc ion battery.
Compared with the existing technology, nickel described in the invention, bismuth modified manganese dioxide positive electrode and have the anode
Zinc ion battery have the advantage that
Nickel described in the invention, bismuth modified manganese dioxide positive electrode and the Zinc ion battery with the anode have
Preferable high rate performance, cycle performance and longer cycle life.
Detailed description of the invention
Fig. 1 is the X-ray of unmodified made from embodiment 1-4 and comparative example 1 and nickel, bismuth modified manganese dioxide positive electrode
Diffraction (XRD) map；
Fig. 2 is scanning electron microscope (SEM) figure of nickel made from embodiment 1-4, bismuth modified manganese dioxide positive electrode.Wherein,
(a)-(d) respectively corresponds the SEM figure of positive electrode described in embodiment 1-4；
Fig. 3 is the cycle life curve and coulombic efficiency curve of 2 battery of embodiment under 500mA/g current density；
Fig. 4 is the cycle performance that embodiment 1-4 battery and 1 battery of comparative example are crossed under the conditions of current density is 300mA/g
Curve；
Fig. 5 is the cyclic voltammetry curve of 1 battery of 2 battery of embodiment and comparative example under conditions of sweep speed 0.5mV/s.
Specific embodiment
In addition to being defined, technical term used in following embodiment has and the invention one of ordinary skill in the art
The identical meanings being commonly understood by.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；
The experimental method is unless otherwise specified conventional method.
Come that the present invention will be described in detail creates below with reference to embodiment and attached drawing.
Embodiment 1
A kind of nickel, bismuth modified manganese dioxide positive electrode, the material is prepared by following methods: by 7mmol
Potassium permanganate and the hydrochloric acid (concentration 36%) of 2.5ml stirred evenly in 70ml deionized water, 0.035mmol is then added
Nickel nitrate, 0.035mmol bismuth nitrate solution is fallen after being vigorously stirred 30 minutes under conditions of 1000 revs/min of revolving speed
Enter in 100ml polytetrafluoroethylene (PTFE) autoclave, hydro-thermal reaction 10 hours will be reacted wait be cooled to room temperature under the conditions of 160 DEG C
Liquid washs to solution to obtain nickel, bismuth modified manganese dioxide after being dried 12 hours at suction filtration, 80 DEG C, being ground 45 minutes after neutrality
Powder positive electrode, the manganese element and nickel element of positive electrode manufactured in the present embodiment, the atomic ratio of bismuth element are 1:0.005:
0.005, it is labeled as " MnO2: Ni, Bi=1:0.005 ".
Embodiment 2
A kind of nickel, bismuth modified manganese dioxide positive electrode, the material is prepared by following methods: by 7mmol
Potassium permanganate and the hydrochloric acid (concentration 36%) of 2.5ml stirred evenly in 70ml deionized water, be then added 0.7mmol's
The bismuth nitrate of nickel nitrate, 0.7mmol pours into solution after being vigorously stirred 30 minutes under conditions of 1000 revs/min of revolving speed
In 100ml polytetrafluoroethylene (PTFE) autoclave, the hydro-thermal reaction 10 hours under the conditions of 160 DEG C, wait be cooled to room temperature, by reaction solution
Washing obtains nickel, bismuth modified manganese dioxide powder after being dried 12 hours, grinding 45 minutes at suction filtration, 80 DEG C after neutrality to solution
Last positive electrode, the manganese element and nickel element of positive electrode manufactured in the present embodiment, the atomic ratio of bismuth element are 1:0.1:0.1,
Labeled as " MnO2: Ni, Bi=1:0.1 ".
Embodiment 3
A kind of nickel, bismuth modified manganese dioxide positive electrode, the material is prepared by following methods: by 7mmol
Potassium permanganate and the hydrochloric acid (concentration 36%) of 2.5ml stirred evenly in 70ml deionized water, 2.45mmol is then added
Nickel nitrate, 2.45mmol bismuth nitrate solution is fallen after being vigorously stirred 30 minutes under conditions of 1000 revs/min of revolving speed
Enter in 100ml polytetrafluoroethylene (PTFE) autoclave, hydro-thermal reaction 10 hours will be reacted wait be cooled to room temperature under the conditions of 160 DEG C
Liquid washs to solution to obtain nickel, bismuth modified manganese dioxide after being dried 12 hours at suction filtration, 80 DEG C, being ground 45 minutes after neutrality
Powder positive electrode, the manganese element and nickel element of positive electrode manufactured in the present embodiment, the atomic ratio of bismuth element are 1:0.35:
0.35, it is labeled as " MnO2: Ni, Bi=1:0.35 ".
Embodiment 4
A kind of nickel, bismuth modified manganese dioxide positive electrode, the material is prepared by following methods: by 7mmol
Potassium permanganate and the hydrochloric acid (concentration 36%) of 2.5ml stirred evenly in 70ml deionized water, be then added 3.5mmol's
The bismuth nitrate of nickel nitrate, 3.5mmol pours into solution after being vigorously stirred 30 minutes under conditions of 1000 revs/min of revolving speed
In 100ml polytetrafluoroethylene (PTFE) autoclave, the hydro-thermal reaction 10 hours under the conditions of 160 DEG C, wait be cooled to room temperature, by reaction solution
Washing obtains nickel, bismuth modified manganese dioxide powder after being dried 12 hours, grinding 45 minutes at suction filtration, 80 DEG C after neutrality to solution
Last positive electrode, the manganese element and nickel element of positive electrode manufactured in the present embodiment, the atomic ratio of bismuth element are 1:0.5:0.5,
Labeled as " MnO2: Ni, Bi=1:0.5 ".
Embodiment 5
A kind of Zinc ion battery, including manganese dioxide positive pole, zinc load, diaphragm, electrolyte and battery case；The battery case
Specification is 2032 battery cases；The manganese dioxide positive pole is nickel described in embodiment 1-4, in bismuth modified manganese dioxide positive electrode
It is a kind of.
The manganese dioxide positive pole is prepared in the following way: weigh 0.3g manganese dioxide powder, by manganese dioxide powder,
Kynoar and acetylene black mass ratio 7:2:1 ratio weigh, and are then put into togerther the N-Methyl pyrrolidone of itself and 3ml and grind
It is ground to glue in alms bowl in honey state, the glue is coated in the substrate of Thin Stainless Steel, is put in vacuum drying oven
Drying, finally with slicer be cut to the positive sequin of diameter 10mm to get；The manganese dioxide powder is embodiment 1-4
One of the nickel, bismuth modified manganese dioxide positive electrode；
The zinc load is prepared in the following way: 0.5g zinc powder is weighed, by zinc powder, Kynoar and acetylene black quality
It is weighed than 8:1:1 ratio, then the N-Methyl pyrrolidone of itself and 3ml is put into togerther in mortar and are ground to glue in honey shape
The glue is coated in the substrate of Thin Stainless Steel by state, is put in drying in vacuum drying oven, is finally cut to slicer
The cathode sequin of diameter 14mm to get；
The Zinc ion battery manufactures in the following way: at room temperature, assembling electricity according to the sequence that stacks from bottom to top
Electrolyte is simultaneously injected in pond, negative electrode casing > gasket+0.2ml electrolyte > cathode sequin+0.2ml electrolyte > diaphragm+0.2ml electrolysis
Liquid > anode sequin+0.2ml electrolyte > gasket+0.2ml electrolyte > elastic slice > anode cover；Then electricity is encapsulated on sealing machine
Pond.The Zinc ion battery number is named as " 1 battery of embodiment ", " 2 battery of embodiment ", " 3 battery of embodiment ", " embodiment 4
Battery " respectively corresponds the Zinc ion battery that the positive electrode as described in embodiment 1-4 is fabricated.
Comparative example 1
As a comparison case using the Zinc ion battery of unmodified manganese bioxide material and material anode.It is described not change
The manganese bioxide material of property is prepared in the following way: the hydrochloric acid (concentration 36%) of the potassium permanganate of 7mmol and 2.5ml are existed
It is stirred evenly in 70ml deionized water, solution is poured into 100ml polytetrafluoroethylene (PTFE) autoclave, be lauched in 160 DEG C of conditions
Thermal response 10 hours, wait be cooled to room temperature, by reaction solution wash to solution be it is neutral after filtered, dried at 80 DEG C 12 hours,
Grinding obtained unmodified manganese dioxide powder positive electrode after 45 minutes, was labeled as " pure MnO2”。
Zinc ion battery with unmodified manganese dioxide positive pole is identical as 5 structure of embodiment, and only anode uses this reality
Apply the unmodified manganese dioxide positive pole material of example preparation.The Zinc ion battery number is named as " 1 battery of comparative example ".
Fig. 1 is to use X to unmodified and nickel made from embodiment 1-4 and comparative example 1, bismuth modified manganese dioxide positive electrode
The result that x ray diffraction (XRD) instrument is characterized.By changing to the spectrum analysis it is found that testing resulting unmodified and nickel, bismuth
The XRD characteristic peak and α phase MnO of property manganese dioxide positive pole material2Characteristic peak (PDF#44-0141) match, show unmodified
Image structure with nickel, bismuth modified manganese dioxide positive electrode is α phase MnO2。
Fig. 2 is to be carried out to nickel made from embodiment 1-4, bismuth modified manganese dioxide positive electrode using scanning electron microscope (SEM)
The result of characterization.Wherein, (a)-(d) respectively corresponds the SEM figure of positive electrode described in embodiment 1-4；From SEM image (a-d)
It was found that the pattern of product made from embodiment 1-4 is nanometer rods, nanobelt or nanowire structure, nanometer rods, nanobelt or nanometer
Line draw ratio is 30~100:1, and diameter is 30~110nm.
Fig. 3 is the cycle life curve and coulombic efficiency curve of 2 battery of embodiment under 500mA/g current density.By scheming
In it is found that passing through 1000 cycle charge discharge electric process under 500mA/g current density, the specific capacity of 2 battery of embodiment do not drop
It is low, higher level is remained at, furthermore the coulombic efficiency of 2 battery of embodiment is also maintained at 90% or more level, above-mentioned knot
Fruit shows that the cycle performance of 2 battery of embodiment is preferable, and cycle life is longer.
Fig. 4 is the cycle performance that embodiment 1-4 battery and 1 battery of comparative example are crossed under the conditions of current density is 300mA/g
Curve.By in figure it is found that under 300mA/g current density pass through 100 cycle charge discharge electric process, the ratio of the battery of embodiment 2 and 4
Capacity remains at higher level (being greater than 75%) compared with original state, and the specific capacity of 1 battery of comparative example is reduced to original state
22.7%, show 2 battery of embodiment compared with 1 battery of comparative example have preferable cycle performance.
Fig. 5 is the cyclic voltammetry curve of 1 battery of 2 battery of embodiment and comparative example under conditions of sweep speed 0.5mV/s.
The electric current at peak means more greatly better electrode reaction dynamics and preferable high rate performance, and the potential difference at peak is smaller to illustrate material
The polarization of electrode of preparation is smaller.It can be found that the peak current of 2 battery of embodiment is higher from Fig. 5, the potential difference at peak is also more right
The reduction of 1 battery of ratio, show 2 battery of embodiment have preferable electrode reaction dynamics, preferable high rate performance and
Lesser polarization.
The foregoing is merely the preferred embodiments of the invention, are not intended to limit the invention creation, all at this
Within the spirit and principle of innovation and creation, any modification, equivalent replacement, improvement and so on should be included in the invention
Protection scope within.
Claims (10)
1. a kind of nickel, bismuth modified manganese dioxide positive electrode, it is characterised in that: the nickel, bismuth modified manganese dioxide positive electrode
For the α phase MnO that nickel element, bismuth element is added2。
2. nickel bismuth modified manganese dioxide positive electrode according to claim 1, it is characterised in that: the nickel element, bismuth element
With 0.005~0.5:0.005 of atomic ratio~0.5:1 of manganese element.
3. nickel according to claim 1 or 2, bismuth modified manganese dioxide positive electrode, it is characterised in that: the nickel, bismuth change
Property manganese dioxide positive pole material pattern be nanometer rods, nano wire or nanobelt.
4. nickel according to claim 3, bismuth modified manganese dioxide positive electrode, it is characterised in that: nanometer rods, nano wire or
The draw ratio of nanobelt is 30~100:1, and diameter is 30~110nm.
5. the preparation method of nickel described in claim 1, bismuth modified manganese dioxide positive electrode, it is characterised in that: by permanganic acid
Potassium and hydrochloric acid stir evenly in deionized water, and nickel nitrate and bismuth nitrate is then added, is prepared using hydro-thermal reaction.
6. the preparation method of nickel according to claim 5, bismuth modified manganese dioxide positive electrode, it is characterised in that: described
In nickel nitrate and bismuth nitrate in nickel element, bismuth element and potassium permanganate manganese element atomic ratio be 0.005~0.5:0.005~
0.5:1。
7. the preparation method of nickel according to claim 5, bismuth modified manganese dioxide positive electrode, it is characterised in that: described
The atomic ratio of manganese element is 0.1:0.1:1 in nickel element, bismuth element and potassium permanganate.
8. the preparation method of nickel according to claim 5, bismuth modified manganese dioxide positive electrode, it is characterised in that: described
The dosage of potassium permanganate is 7mmol；Concentration of hydrochloric acid is 36%, dosage 2.5ml；Nickel nitrate dosage is 0.7mmol；Bismuth nitrate is used
Amount is 0.7mmol；Deionized water dosage is 70ml.
9. according to the preparation method of nickel described in claim 5-8 any one, bismuth modified manganese dioxide positive electrode, feature
Be: the reaction temperature of the hydro-thermal reaction is 160 DEG C, and the reaction time is 10 hours.
10. nickel, bismuth modified manganese dioxide positive electrode according to claim 1 or 5, it is characterised in that: the nickel, bismuth change
Property manganese dioxide positive pole material be used for Zinc ion battery.
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| CN112886004A (en) * | 2021-01-11 | 2021-06-01 | 北京科技大学 | Cathode material of water-based zinc ion battery and matched electrolyte |
| CN114029067A (en) * | 2021-11-16 | 2022-02-11 | 济南市中两山生态科技中心 | Material for efficiently degrading organic wastewater |
| WO2023273835A1 (en) * | 2021-07-01 | 2023-01-05 | 陈璞 | Positive electrode material of aqueous zinc-ion battery having neutral or slightly acidic system, preparation method therefor, and application thereof |
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