CN108899536A - A kind of pulse battery NixAlyMnzO2The preparation method and application of tertiary cathode material - Google Patents
A kind of pulse battery NixAlyMnzO2The preparation method and application of tertiary cathode material Download PDFInfo
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- CN108899536A CN108899536A CN201810719741.3A CN201810719741A CN108899536A CN 108899536 A CN108899536 A CN 108899536A CN 201810719741 A CN201810719741 A CN 201810719741A CN 108899536 A CN108899536 A CN 108899536A
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- mixed solution
- sodium carbonate
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- aluminum nitrate
- tertiary cathode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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Abstract
A kind of pulse battery NixAlyMnzO2Nickel sulfate, aluminum nitrate, manganese sulfate are configured to nickel sulfate-aluminum nitrate-manganese sulfate mixed solution by the preparation method and application of tertiary cathode material；Sodium carbonate is matched into sodium carbonate liquor, ammonium hydroxide is added, is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；Sodium carbonate-ammonium hydroxide mixed solution is added in nickel sulfate-aluminum nitrate-manganese sulfate mixed solution, stands after mixing evenly, discards supernatant liquor, centrifugal treating, supernatant is removed again, and sediment is put into container, it is dry, after grinding, it places in Muffle furnace, after 200-300 DEG C of pre-sintering and 700-850 DEG C of high temperature sintering, furnace cooling, after being ground up, sieved, tertiary cathode material is obtained.Preparation method is simple, easy to operate, and tertiary cathode material is applied in pulse battery, can effectively improve the voltage platform of pulse battery charging and discharging, and pulse battery is made to have excellent cyclical stability under high-multiplying power discharge system.
Description
Technical field
The present invention relates to a kind of pulse battery NixAlyMnzO2The preparation method and application of tertiary cathode material.
Background technique
Pulse battery is a kind of mechanism of new electrochemical power sources for capableing of fast charging and discharging, and ternary material is the hot spot studied now,
It is applied in pulse battery, can be improved voltage platform, makes it have higher specific capacity, and realizes heavy-current discharge.
Currently, the positive electrode of most enterprise selection nickel, cobalt, manganese ternary material as pulse battery, but the electric discharge of nickel
Current potential is lower, poorly conductive, and the price of cobalt is relatively high, the practicability is poor.In order to improve disadvantages mentioned above, nickel, aluminium, manganese preparation three are selected
First metal oxide, one side aluminium have good electric conductivity, metallicity good, aluminium doped with the charge being conducive between ion turn
It moves, increases insertion/embedding invertibity out of ion；On the other hand its price is cheap, and the capacity of metal oxide is than traditional carbon
Material is high, is able to ascend voltage platform, therefore aluminium replaces cobalt to have good researching value.
Summary of the invention
The present invention is to prepare a kind of pulse battery NixAlyMnzO2The preparation method and application of tertiary cathode material, preparation
Method is simple, easy to operate, by NixAlyMnzO2Tertiary cathode material is applied in pulse battery, can effectively improve pulse electricity
The voltage platform of pond charge and discharge makes pulse battery have excellent cyclical stability under high-multiplying power discharge system.
The technical solution of the invention is as follows：
A kind of pulse battery NixAlyMnzO2The preparation method of tertiary cathode material, specific step is as follows：
(1) by nickel sulfate, aluminum nitrate, manganese sulfate according to molar ratio 1:1:1 is configured to concentration as 0.02mol/L-0.04mol/L's
Nickel sulfate-aluminum nitrate-manganese sulfate mixed solution；
(2) sodium carbonate is configured to the sodium carbonate liquor that concentration is 0.1mol/L-0.2mol/L, and is added and accounts for sodium carbonate liquor matter
The ammonium hydroxide of 5%-8% is measured, is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；
(3) sodium carbonate-ammonium hydroxide mixed solution is added in nickel sulfate-aluminum nitrate-manganese sulfate mixed solution, the sodium carbonate-ammonia
Water mixed solution and nickel sulfate-aluminum nitrate-manganese sulfate mixed solution volume ratio are 1:1, it stands after mixing evenly, discards upper layer
Clear liquid, centrifugal treating remove supernatant again, retain sediment；
(4) sediment that centrifugation obtains is put into container, it is -15 hours 10 hours dry under conditions of 100 DEG C -130 DEG C,
After grinding, places in Muffle furnace, be pre-sintered 2 hours at 200 DEG C -300 DEG C, then through high temperature sintering 15-25 at 700 DEG C -900 DEG C
Hour, furnace cooling after being ground up, sieved, obtains NixAlyMnZO2Ternary material.
A kind of NixAlyMnzO2Application of the tertiary cathode material in preparation pulse positive electrode for battery, specific steps are such as
Under：By NixAlyMnzO2Ternary material, Super-P and PVDF are according to mass ratio 7:2:1 is mixed and made into paste, and single side is coated in aluminium
On foil, coating thickness 0.05-0.08mm, after drying 12 hours in a vacuum drying oven at 60 DEG C -80 DEG C, diameter, which is made, is
The electrode of 10mm.
Further, it when sodium carbonate-ammonium hydroxide mixed solution is added in nickel sulfate-aluminum nitrate-manganese sulfate mixed solution, adopts
It is added dropwise with peristaltic pump with the speed of 20mL/min-50mL/min.
Further, when step (3) centrifugal treating, centrifugal speed 4000r/min-8000r/min, centrifugation time 5
- 15 minutes minutes.
Beneficial effects of the present invention：
Preparation method is simple, easy to operate, NixAlyMnzO2In tertiary cathode material Al doped be conducive to ion between electricity
Lotus transfer increases insertion/embedding invertibity out of ion, to guarantee under heavy-current discharge system, the stable circulation of battery
Property is promoted；By NixAlyMnzO2Tertiary cathode material is applied in pulse battery, can effectively improve pulse battery charge and discharge
The voltage platform of electricity, while pulse battery has excellent cyclical stability under high-multiplying power discharge system.
Detailed description of the invention
Fig. 1 is Ni of the present inventionxAlyMnzO2The energy spectrum diagram of positive electrode；
Fig. 4 is Ni of the present inventionxAlyMnzO2Scanning electron microscope (SEM) photograph of the positive electrode under 90.0k multiplying power；
Fig. 2 is Ni of the present inventionxAlyMnzO2The cycle performance curve of positive electrode；
Fig. 3 is Ni of the present inventionxAlyMnzO2Discharge capacity curve under positive electrode difference current density.
Specific embodiment
Embodiment 1
(1) by nickel sulfate, aluminum nitrate, manganese sulfate according to molar ratio 1:1:1 is configured to nickel sulfate-nitre that concentration is 0.02mol/L
Sour aluminium-manganese sulfate mixed solution；
(2) sodium carbonate is configured to the sodium carbonate liquor that concentration is 0.1mol/L, and the ammonia for accounting for sodium carbonate liquor quality 5% is added
Water is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；
(3) sodium carbonate-ammonium hydroxide mixed solution is added drop-wise to by nickel sulfate-aluminum nitrate-sulfuric acid with the speed of 50mL/min with peristaltic pump
In manganese mixed solution, the sodium carbonate-ammonium hydroxide mixed solution and nickel sulfate-aluminum nitrate-manganese sulfate mixed solution volume ratio are
1:1, it stands after mixing evenly, discards supernatant liquor, 15min is then centrifuged with 4000r/min revolving speed, removed again after centrifugation
Clear liquid retains sediment；
(4) sediment that centrifugation obtains is put into culture dish drying 15 hours under conditions of 100 DEG C, after grinding, placed
It in Muffle furnace, is pre-sintered 2 hours at 200 DEG C, then through high temperature sintering 25 hours at 700 DEG C, furnace cooling, after being ground up, sieved,
Ni is madexAlyMnZO2Ternary material.
NixAlyMnzO2Tertiary cathode material prepares pulse positive electrode for battery
By NixAlyMnzO2Ternary material, Super-P and PVDF are according to mass ratio 7:2:1 mixes and is made paste, single side coating
On aluminium foil, coating thickness 0.05mm, after drying 12 hours in a vacuum drying oven at 60 DEG C, it is 10mm that diameter, which is made,
Electrode.The pulse battery being assembled into is stablized circulation 500 times or more under the discharge system of 1000mAh/g.
Embodiment 2
(1) by nickel sulfate, aluminum nitrate, manganese sulfate according to molar ratio 1:1:1 is configured to nickel sulfate-nitre that concentration is 0.04mol/L
Sour aluminium-manganese sulfate mixed solution；
(2) sodium carbonate is configured to the sodium carbonate liquor that concentration is 0.2mol/L, and the ammonia for accounting for sodium carbonate liquor quality 8% is added
Water is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；
(3) 100mL sodium carbonate-ammonium hydroxide mixed solution is added drop-wise to by 100mL nickel sulfate-nitre with the speed of 20mL/min with peristaltic pump
It in sour aluminium-manganese sulfate mixed solution, stands after mixing evenly, discards supernatant liquor, then with the centrifugation of 8000r/min revolving speed
5min removes supernatant again after centrifugation, retain sediment；
(4) sediment that centrifugation obtains is put into culture dish drying 10 hours under conditions of 130 DEG C, after grinding, placed
It in Muffle furnace, is pre-sintered 2 hours at 250 DEG C, then through high temperature sintering 15 hours at 900 DEG C, furnace cooling, after being ground up, sieved,
Ni is madexAlyMnZO2Ternary material.
NixAlyMnzO2Tertiary cathode material prepares pulse positive electrode for battery
By NixAlyMnzO2Ternary material, Super-P and PVDF are according to mass ratio 7:2:1 mixes and is made paste, single side coating
On aluminium foil, coating thickness 0.08mm, after drying 12 hours in a vacuum drying oven at 80 DEG C, it is 10mm that diameter, which is made,
Electrode.The pulse battery being assembled into is stablized circulation 500 times or more under the discharge system of 1000mAh/g.
Embodiment 3
(1) 0.01mol nickel sulfate, 0.01mol aluminum nitrate and 0.01mol manganese sulfate are dissolved in and are configured to concentration in 1L water and are
Nickel sulfate-aluminum nitrate-manganese sulfate mixed solution of 0.03mol/L；
(2) sodium carbonate is configured to the sodium carbonate liquor that concentration is 0.15mol/L, and is added and accounts for sodium carbonate liquor quality 6%
Ammonium hydroxide is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；
(3) sodium carbonate-ammonium hydroxide mixed solution is added drop-wise to by nickel sulfate-aluminum nitrate-sulfuric acid with the speed of 30mL/min with peristaltic pump
In manganese mixed solution, the sodium carbonate-ammonium hydroxide mixed solution and nickel sulfate-aluminum nitrate-manganese sulfate mixed solution volume ratio are
1:1, it stands after mixing evenly, discards supernatant liquor, 10min is then centrifuged with 5000r/min revolving speed, removed again after centrifugation
Clear liquid retains sediment；
(4) sediment that centrifugation obtains is put into culture dish drying 12 hours under conditions of 120 DEG C, after grinding, placed
It in Muffle furnace, is pre-sintered 2 hours at 300 DEG C, then through high temperature sintering 20 hours at 850 DEG C, furnace cooling, after being ground up, sieved,
Ni is madexAlyMnZO2Ternary material.The NixAlyMnZO2The energy spectrum diagram of ternary material is as shown in Figure 1, can be with according to gamma-spectrometric data
Know, ratio shared by Ni, Al, Mn, O is 18.31%, 11.36%, 13.87% and 45.92% respectively in gained sample.Cause
This, the chemical formula of the sample should be Ni0.78Al0.48Mn0.61O2.The NixAlyMnzO2Scanning of the electrode material under 90.0k multiplying power
Electron microscope is as shown in Fig. 2, particle is in cubic structure as can be seen from Figure 2, and particle size is between 60nm-80nm, particle point
Cloth is uniform, and it can be ion by providing channel, so that after material assembling that surface is smooth and more rule and stable structure
Circulating battery stability is good, electric conductivity is promoted, battery performance makes moderate progress.
NixAlyMnzO2Tertiary cathode material prepares pulse positive electrode for battery
By NixAlyMnzO2Ternary material, conductive black (Super-P) and Kynoar (PVDF) are according to mass ratio 7:2:1 is mixed
Paste is closed and is made, single side is coated on aluminium foil, and coating thickness 0.06mm dries 12 in a vacuum drying oven at 70 DEG C
After hour, the electrode that diameter is 10mm is made.
The assembling of pulse battery：
Use NixAlyMnzO2Pulse battery of the ternary material as anode, which includes lithium an- ode, diaphragm, electrolyte
(solute：1mol/LLiPF6, solvent：EC/EMC/DMC, 1:1:1vol.%), NixAlyMnZO2Tertiary cathode, battery case.Electricity
Pond assembling process is as follows：
By NixAlyMnzO2Tertiary cathode is placed in battery case；2. two panels polypropylene diaphragm is taken uniformly to dip electricity in weighing bottle
Solution liquid is sequentially placed on pole piece；3. drawing a small amount of electrolyte in volumetric flask, 2mL, then, at two layers with disposable dropper
0.3mL electrolyte is dripped on diaphragm；4. lithium piece is placed on diaphragm；5. by with a thickness of the gasket of 1mm and elastic slice elder generation postposition
On lithium piece；6. covering battery case.
According to data such as Fig. 3 and Fig. 4 institute measured by aforesaid operations electrode assembling pulse battery prepared with embodiment 3
Show, as can be seen from figs. 3 and 4, when current density is respectively 100mAh/g, 200mAh/g, 500mAh/g and 1000mAh/g,
Battery specific capacity can achieve 66mAh/g, 45mAh/g, 40mAh/g and 20mAh/g, especially be in current densities
When 1000mAh/g, battery can stablize circulation 500 times.This is because the doping of Al is able to ascend leading for battery in electrode material
Electrically, be conducive to the electric charge transfer between ion, increase insertion/embedding invertibity out of ion, to guarantee to put in high current
Under electric system, the cyclical stability of battery is promoted.
Ni of the inventionxAlyMnzO2Anode is made in tertiary cathode material, and the pulse battery being assembled into is 1000mAh/g's
Under discharge system, stablize circulation 500 times or more.
The above is only specific embodiments of the present invention, are not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of pulse battery NixAlyMnzO2The preparation method of tertiary cathode material, it is characterized in that：
Specific step is as follows：
(1) by nickel sulfate, aluminum nitrate, manganese sulfate according to molar ratio 1:1:1 is configured to concentration as 0.02mol/L-0.04mol/L's
Nickel sulfate-aluminum nitrate-manganese sulfate mixed solution；
(2) sodium carbonate is configured to the sodium carbonate liquor that concentration is 0.1mol/L-0.2mol/L, and is added and accounts for sodium carbonate liquor matter
The ammonium hydroxide of 5%-8% is measured, is uniformly mixed, obtains sodium carbonate-ammonium hydroxide mixed solution；
(3) sodium carbonate-ammonium hydroxide mixed solution is added in nickel sulfate-aluminum nitrate-manganese sulfate mixed solution, the sodium carbonate-ammonia
Water mixed solution and nickel sulfate-aluminum nitrate-manganese sulfate mixed solution volume ratio are 1:1, it stands after mixing evenly, discards upper layer
Clear liquid, centrifugal treating remove supernatant again, retain sediment；
(4) sediment that centrifugation obtains is put into container, it is -15 hours 10 hours dry under conditions of 100 DEG C -130 DEG C,
After grinding, places in Muffle furnace, be pre-sintered 2 hours at 200 DEG C -300 DEG C, then through high temperature sintering 15-25 at 700 DEG C -900 DEG C
Hour, furnace cooling after being ground up, sieved, obtains NixAlyMnZO2Ternary material.
2. pulse battery Ni according to claim 1xAlyMnzO2The preparation method of tertiary cathode material, it is characterized in that：
When sodium carbonate-ammonium hydroxide mixed solution is added in nickel sulfate-aluminum nitrate-manganese sulfate mixed solution, use peristaltic pump with 20mL/
The speed of min-50mL/min is added dropwise.
3. pulse battery Ni according to claim 1xAlyMnzO2The preparation method of tertiary cathode material, it is characterized in that：
When step (3) centrifugal treating, centrifugal speed 4000r/min-8000r/min, centrifugation time is -15 minutes 5 minutes.
4. a kind of Ni as described in claim 1xAlyMnzO2Application of the tertiary cathode material in preparation pulse positive electrode for battery,
It is characterized in that：
Specific step is as follows：
By NixAlyMnzO2Ternary material, Super-P and PVDF are according to mass ratio 7:2:1 mixes and paste is made, and single side is coated in
On aluminium foil, coating thickness 0.05mm-0.08mm after drying 12 hours in a vacuum drying oven at 60 DEG C -80 DEG C, is made straight
Diameter is the electrode of 10mm.
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| CN201810719741.3A CN108899536B (en) | 2018-06-30 | 2018-06-30 | Ni for pulse batteryxAlyMnzO2Preparation method and application of ternary cathode material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112185710A (en) * | 2020-01-23 | 2021-01-05 | 渤海大学 | Na of sodium ion capacitor batteryxMnyAlzO2@Na3V2(PO4)3Composite electrode material and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284684A (en) * | 2008-05-29 | 2008-10-15 | 金川集团有限公司 | Preparing method for nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material |
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- 2018-06-30 CN CN201810719741.3A patent/CN108899536B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101284684A (en) * | 2008-05-29 | 2008-10-15 | 金川集团有限公司 | Preparing method for nickel-cobalt-lithium manganate precursor of lithium ionic cell positive material |
Non-Patent Citations (1)
| Title |
|---|
| JIAN ZENG等: ""Al and/or Ni-doped nanomanganese dioxide with anisotropic expansion and their electrochemical characterization in primary Li–MnO2 batteries"", 《JOURNAL OF SOLID STATE ELECTROCHEMISTRY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112185710A (en) * | 2020-01-23 | 2021-01-05 | 渤海大学 | Na of sodium ion capacitor batteryxMnyAlzO2@Na3V2(PO4)3Composite electrode material and application |
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