CN108615874A - A kind of kalium ion battery positive electrode and preparation method thereof based on nickel manganese binary oxide - Google Patents
A kind of kalium ion battery positive electrode and preparation method thereof based on nickel manganese binary oxide Download PDFInfo
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- 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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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention discloses a kind of kalium ion battery positive electrode and preparation method thereof based on nickel manganese binary oxide.This approach includes the following steps：Nickel salt, manganese salt, sylvite and doped chemical salt are dissolved in deionized water and obtain certain density metal ion salt solution；Metal ion salt solution is added to organic acid or salting liquid and is stirred；By organic acid or acylate presoma suspension heating evaporation moisture content until moisture evaporation is complete, the precursor powder of acylate is obtained；Or directly directly mix the organic acid salt containing nickel/manganese/potassium, obtain the presoma of acylate；Precursor powder is ground, is pre-sintered, then grinds again, roasting at high temperature obtains positive electrode.The preparation method operating procedure controllability is high, low production cost, is easier to carry out large-scale production.
Description
Technical field
The present invention relates to kalium ion battery positive electrodes and preparation method thereof, and in particular to one kind is aoxidized based on nickel manganese binary
Kalium ion battery positive electrode of object and preparation method thereof.
Background technology
With the drastically expansion of economic fast development and industry, using coal, oil, three big main energy sources of natural gas as generation
The Fossil fuel consumption amount of table is increased sharply, this excessive exploitation and use to non-renewable resources, exacerbates energy shortage and entirely
Contradiction between ball environmental degradation seriously restricts the development of human economy and society.Therefore, reproducible new energy is cleaned in exploitation
Source is most one of the technical field of decisive influence in world economy from now on.Lithium rechargeable battery is as a kind of novel, clear
Clean, the reproducible energy has the characteristics that open-circuit voltage is high, higher than energy, security performance is superior and environmental-friendly, therefore wide
It is general to be applied to the fields such as portable electronic device and electric vehicle.But since the rare reserves of lithium resource and fancy price are serious
Constrain application of the lithium ion battery in extensive energy storage etc..It is excellent it is therefore desirable to greatly develop next-generation comprehensive effectiveness
Secondary cell new system.
The new secondary batteries such as kalium ion battery, sodium-ion battery, Magnesium ion battery and lithium ion battery are having the same
Chemical principle and the advantages such as resourceful, cheap receive the concern of researcher.Wherein kalium ion battery have with
The closest standard electrode EMF of lithium ion battery, while potassium ion has larger ion mobility in the electrolytic solution.
The preparation of negative material is focused on about the research of kalium ion battery at present more, and the research in terms of positive electrode is less.
Chinese invention patent application CN 107226475 A propose based on Prussian blue kalium ion battery positive electrode, though
Its right capacity recycles 400 times, capacity retention ratio is 90.37% up to 90.7mAh/g；However, there is operation controllably in this material
Property is poor, the problem of being difficult to mass produce.
107093739 A of Chinese invention patent application CN propose the kalium ion battery anode material based on potassium Mn oxide
Material, capacity is up to 83.9mAh/g, but deficiency of this material there are poor circulation, without apparent discharge platform.
105826521 A of Chinese invention patent application CN are proposing the kalium ion battery based on polyanionic compound just
Pole material has apparent discharge platform in 1.6V or so, but this kind of material has that energy density is low；
Kuniko Chihara have found, a kind of KVPO can be obtained by the method for high-temperature roasting4The kalium ion battery anode of F
Material has the discharge platform up to 4V and excellent high rate performance, but there are the low deficiencies of specific capacity for this kind of material；
Since the research of kalium ion battery positive electrode is still in starting stage, the type ten for the positive electrode reported at present
It is point limited, and there is such or such deficiency in these materials, seriously hinder the commercialization process of kalium ion battery, because
This, it would be highly desirable to develop the kalium ion battery positive electrode of novel high-performance.
Invention content
In view of insufficient existing for current material, the present invention provide a kind of novel high-performance based on nickel manganese binary oxide
Kalium ion battery positive electrode and preparation method thereof.
The present invention includes following content：
A kind of kalium ion battery positive electrode based on nickel manganese binary oxide, chemical formula are：KaXmNibMncO2；Wherein
0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1；The X includes Fe, Al, Mg or Li.
A kind of preparation method of the kalium ion battery positive electrode based on nickel manganese binary oxide, includes the following steps：
(1) soluble nickel salt, manganese salt, sylvite and doped chemical salt are dissolved in the mixing of organic solvent and deionized water
Wiring solution-forming A in solvent；
(2) by organic acid or acylate be dissolved in organic solvent obtain with the in the mixed solvent that deionized water is formed it is molten
Liquid B；
(3) solution A is added in solution B under stiring, be uniformly mixed and continuously stirred, obtain suspension C；
(4) precursor powder containing nickel manganese potassium is prepared one of to include the following steps：Heating under vacuum suspension C is until steam
Solid carbon dioxide gets the precursor powder containing nickel manganese potassium；Or suspension C is filtered, is dried to obtain precursor powder；
(5) the acylate precursor powder that step (4) obtains is ground, is pre-sintered, grinding, then high-temperature roasting,
It is K to obtain chemical formulaaXmNibMncO2(0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=
1) positive electrode.
In the above method, in step (1), the nickel salt be nickel nitrate, nickel acetate, nickel sulfate, in nickel chloride it is a kind of with
On；The manganese salt is one or more of manganese nitrate, manganese acetate, manganese sulfate, manganese chloride；The sylvite is potassium hydroxide, acetic acid
One or more of potassium, potassium carbonate, potassium chloride, potassium citrate；The doped chemical salt be soluble ferric iron salt, aluminum soluble salt,
One or more of soluble magnesium salt, soluble lithium salt；The organic acid is one or more of acetic acid, oxalic acid, citric acid；Institute
It is one or more of ethyl alcohol, acetone, ethylene glycol to state organic solvent；In step (1), the body of the organic solvent and deionized water
Product ratio 1:1-4.
In the above method, in step (2), the acylate be acetate, oxalates, in citrate it is a kind of with
On；The organic acid is one or more of acetic acid, oxalic acid, citric acid；The volume ratio of the organic solvent and deionized water is
1:2-6。
In the above method, in step (3), the mixed method be solution A is added drop-wise in solution B, rate of addition be 1~
Solution B is added drop-wise in solution A by 2 drops/s, and rate of addition is 1~2 drop/s；In step (3), the rotating speed of the stirring is
200~500 turns/min, mixing time is 6~12h.
In the above method, in step (4), the temperature of the heating is 60~120 DEG C.
In the above method, the concrete operations of step (5) are：Persursor material after drying is ground, in air gas
In atmosphere 300~500 DEG C pre-sintering 3~6h, then cool to room temperature and be ground, be finally warming up to 700~1000 DEG C roasting 8~
20h。
A kind of preparation method of the kalium ion battery positive electrode based on nickel manganese binary oxide, includes the following steps：It will
Acylate containing nickel manganese potassium is 0.1-0.5 according to nickel manganese potassium molar ratio:0.5-0.9:The ratio ball milling mixing of 0.4-1.2 obtains
To acylate precursor powder；The acylate precursor powder of gained is ground, 300~500 in air atmosphere
DEG C it is pre-sintered 3~6h, then cools to room temperature and be ground, be finally warming up to 700~1000 DEG C of 8~20h of roasting to get to change
Formula is KaXmNibMncO2The anode of (0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1)
Material.
Compared with the prior art, the advantages of the present invention are as follows：
(1) the material K prepared by the present inventionaXmNibMncO2, discharge platform voltage height high with discharge capacity, stability are good
Etc. important advantages, be a kind of there is application value and the novel kalium ion battery positive electrode of foreground.
(2) method of the invention is prepared simple, and production cost is low, and operation controllability is high, can large-scale application it is raw in industry
In production, be of great practical significance.
Description of the drawings
Fig. 1 is the nickel manganese binary kalium ion battery positive electrode XRD diagram；
Fig. 2 is the nickel manganese binary kalium ion battery positive electrode cycle performance figure.
Specific implementation mode
It is described in detail with reference to specific embodiment is further specific to the present invention, but embodiments of the present invention are unlimited
Routine techniques progress can refer to for not specifically specified technological parameter in this.
Embodiment 1
(1) 0.005mol nickel acetates, 0.005mol manganese acetates and 0.013mol potassium acetates (excessive 5%) are dissolved in 20mL
Volume ratio is 1:In 1 ethyl alcohol and deionized water；
(2) by 1.299g acetic acids in 10mL volume ratios be 1:In 2 ethyl alcohol and deionized water；
(3) metal salt solution is added drop-wise to the speed of 1~2 drop/s in acetic acid solution, then with the speed of 200 turns/min into
Row stirring 6h；
(4) 60 DEG C of gained mixed liquor is heated to moisture under vacuum to be evaporated, obtains powder；
(5) gained powder is pre-sintered (heating rate is 3 DEG C/min) for 300 DEG C in air atmosphere, is then cooled to room
It is ground again under temperature, 700 DEG C of high-temperature roasting 8h (heating rate is 5 DEG C/min) obtain kalium ion battery positive electrode
K1.20Ni0.50Mn0.50O2。
The assembling steps of button cell：Positive electrode and binder Kynoar (PVDF), conductive agent acetylene black are pressed
According to mass ratio 8:1:1 ratio mixing, is added solvent N-methyl pyrilidone (NMP) and stirs 4-6h, slurry is applied to totally
Aluminium foil on, it is for use to be put into the drying of 80 DEG C of vacuum drying ovens；With K1.20Ni0.50Mn0.50O2Pole piece is as anode, with potassium piece or stone
Ink is used as cathode, using Whatman GF/D as diaphragm, with 0.8mol/L Potassium Hexafluorophosphates (KPF6)/ethylene carbonate (EC)：
Dimethyl carbonate (DEC) assembles button cell as electrolyte.
Chemical property detects：Assembled button cell is subjected to constant current charge-discharge test, detects the first circle of battery
Capacity and cycle performance, test voltage range is in 2-4.5V；Cyclic voltammetry, electric potential scanning are carried out on electrochemical workstation
Ranging from 2-4.5V, sweep speed 0.1mV/s.
Fig. 1 is the XRD diagram of the material；Fig. 2 is the first circle charging and discharging curve figure of the material.
The basic property of material is shown in Table 1.
Embodiment 2
(1) by 0.001mol nickel nitrates, 0.009mol manganese nitrates, 0.004mol potassium hydroxide (excessive 5%) and
It is 1 that 0.001mol ferrous nitrates, which are dissolved in 50mL volume ratios,:In 4 ethylene glycol and deionized water；
(2) by 1.458g dissolving oxalic acids in 40mL volume ratios be 1:In 6 ethylene glycol and deionized water；
(3) oxalic acid solution is added drop-wise to the speed of 1~2 drop/s in metal salt solution, then with the speed of 500 turns/min into
Row stirring 12h；
(4) 120 DEG C of gained mixed liquor is heated to moisture to be evaporated, obtains powder；
(5) gained powder is pre-sintered (heating rate is 5 DEG C/min) for 500 DEG C in air atmosphere, after being cooled to room temperature
It grinds again, 1000 DEG C of roasting 20h (heating rate is 3 DEG C/min) obtain kalium ion battery positive electrode
K0.40Fe0.10Ni0.10Mn0.90O2。
The basic property of material is shown in Table 1.
Embodiment 3
Except using 0.004mol potassium carbonate substitution 0.013mol potassium acetates, 0.0005mol aluminium chloride replaces ferrous nitrate, etc.
The nickel sulfate of molal quantity, manganese sulfate substitution nickel nitrate, manganese nitrate, acetone replace ethyl alcohol, outside citric acid substituted acetic acid, other compositions
Using completely identical as example 2 with preparation method, positive electrode K is prepared0.40Al0.01Ni0.50Mn0.50O2。
The basic property of material is shown in Table 1.
Embodiment 4
Except using 0.001mol nickel chlorides substitution 0.005mol nickel acetates, 0.009mol manganese chlorides replace 0.005mol acetic acid
Manganese, 0.012mol potassium chloride replace 0.013mol potassium acetates, the magnesium chloride of equimolar number to replace outside ferrous nitrate, and other compositions make
With completely identical as example 2 with preparation method, positive electrode K is prepared1.20Mg0.05Ni0.10Mn0.90O2。
The basic property of material is shown in Table 1.
Embodiment 5
Except using equimolar number potassium citrate, magnesium chloride substitution potassium hydroxide, in addition to ferrous nitrate, other compositions use and
Preparation method is completely identical as example 2, and positive electrode K is prepared1.20Li0.01Ni0.10Mn0.90O2。
The basic property of material is shown in Table 1.
Table 1 is each embodiment main performance table
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention
Embodiment restriction.For those of ordinary skill in the art, it can also make on the basis of the above description
Other various forms of variations or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement etc., should be included in the protection of the claims in the present invention made by within spirit and principle
Within the scope of.
Claims (8)
1. a kind of kalium ion battery positive electrode based on nickel manganese binary oxide, chemical formula are：KaXmNibMncO2；Wherein
0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1；The X includes Fe, Al, Mg or Li.
2. the preparation method of the kalium ion battery positive electrode based on nickel manganese binary oxide described in claim 1, feature exist
In including the following steps：
(1) soluble nickel salt, manganese salt, sylvite and doped chemical salt are dissolved in organic solvent and the mixed solvent of deionized water
Middle wiring solution-forming A；
(2) organic acid or acylate are dissolved in the in the mixed solvent that organic solvent is formed with deionized water and obtain solution B；
(3) solution A is added in solution B under stiring, be uniformly mixed and continuously stirred, obtain suspension C；
(4) precursor powder containing nickel manganese potassium is prepared one of to include the following steps：Heating under vacuum suspension C is until be evaporated water
Get the precursor powder containing nickel manganese potassium；Or suspension C is filtered, is dried to obtain precursor powder；
(5) the acylate precursor powder that step (4) obtains is ground, be pre-sintered, grinding, then high-temperature roasting to get
It is K to chemical formulaaXmNibMncO2(0.4≤a's≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1)
Positive electrode.
3. the preparation method of the kalium ion battery positive electrode according to claim 2 based on nickel manganese binary oxide, special
Sign is：In step (1), the nickel salt is one or more of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride；The manganese salt is nitre
One or more of sour manganese, manganese acetate, manganese sulfate, manganese chloride；The sylvite is potassium hydroxide, potassium acetate, potassium carbonate, chlorination
One or more of potassium, potassium citrate；The doped chemical salt is soluble ferric iron salt, aluminum soluble salt, soluble magnesium salt, solvable
One or more of property lithium salts；The organic acid is one or more of acetic acid, oxalic acid, citric acid；The organic solvent is second
One or more of alcohol, acetone, ethylene glycol；In step (1), the volume ratio 1 of the organic solvent and deionized water:1-4.
4. the preparation method of the kalium ion battery positive electrode according to claim 2 based on nickel manganese binary oxide, special
Sign is：In step (2), the acylate is one or more of acetate, oxalates, citrate；The organic acid is
One or more of acetic acid, oxalic acid, citric acid；The volume ratio of the organic solvent and deionized water is 1:2-6.
5. the preparation method of the kalium ion battery positive electrode according to claim 2 based on nickel manganese binary oxide, special
Sign is：In step (3), the mixed method is that solution A is added drop-wise in solution B, and rate of addition is 1~2 drop/s or will be molten
Liquid B is added drop-wise in solution A, and rate of addition is 1~2 drop/s；In step (3), the rotating speed of the stirring is 200~500 turns/min,
Mixing time is 6~12h.
6. the preparation method of the kalium ion battery positive electrode according to claim 2 based on nickel manganese binary oxide, special
Sign is：In step (4), the temperature of the heating is 60~120 DEG C.
7. the preparation method of the kalium ion battery positive electrode according to claim 2 based on nickel manganese binary oxide, special
Sign is：The concrete operations of step (5) are：Persursor material after drying is ground, 300~500 DEG C in air atmosphere
It is pre-sintered 3~6h, then cools to room temperature and is ground, is finally warming up to 700~1000 DEG C of 8~20h of roasting.
8. the preparation method of the kalium ion battery positive electrode based on nickel manganese binary oxide described in claim 1, including it is as follows
Step：By the acylate containing nickel manganese potassium according to nickel manganese potassium molar ratio be 0.1-0.5:0.5-0.9:The ratio ball of 0.4-1.2
Mill is mixed to get acylate precursor powder；The acylate precursor powder of gained is ground, in air atmosphere
300~500 DEG C of 3~6h of pre-sintering, then cool to room temperature and are ground, and are finally warming up to 700~1000 DEG C of 8~20h of roasting,
It is K to obtain chemical formulaaXmNibMncO2(0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=
1) positive electrode.
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| PCT/CN2018/112825 WO2019192171A1 (en) | 2018-04-03 | 2018-10-30 | Nickel-manganese binary oxide-based potassium ion battery positive electrode material and preparation method therefor |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019192171A1 (en) * | 2018-04-03 | 2019-10-10 | 华南理工大学 | Nickel-manganese binary oxide-based potassium ion battery positive electrode material and preparation method therefor |
| WO2020124507A1 (en) * | 2018-12-20 | 2020-06-25 | 深圳先进技术研究院 | Crystalline material, preparation method therefor and application thereof, positive electrode active material of battery, positive electrode material of battery, battery and electrical equipment |
| WO2020124648A1 (en) * | 2018-12-20 | 2020-06-25 | 中国科学院深圳先进技术研究院 | Application of fluorinated oxalate material, and product containing fluorinated oxalate material and preparation method therefor and use thereof |
| CN111349001A (en) * | 2018-12-20 | 2020-06-30 | 深圳先进技术研究院 | Crystal material, preparation method and application thereof, battery positive electrode active material, battery positive electrode material, battery and electric equipment |
| CN113270581A (en) * | 2021-04-23 | 2021-08-17 | 佛山市天劲新能源科技有限公司 | Potassium ion battery electrode material and preparation method and application thereof |
| CN113871586A (en) * | 2021-09-07 | 2021-12-31 | 武汉理工大学 | Controllable manganese-based layered oxide electrode material and preparation method and application thereof |
| CN115286049A (en) * | 2022-07-26 | 2022-11-04 | 青岛大学 | Preparation method of lithium-doped potassium nickel manganate material, positive electrode material and battery |
| CN115745030A (en) * | 2023-01-09 | 2023-03-07 | 浙江帕瓦新能源股份有限公司 | Positive electrode material of potassium ion battery, precursor of positive electrode material and preparation method of positive electrode material |
| CN117658243A (en) * | 2024-01-31 | 2024-03-08 | 成都大学 | Potassium ion battery anode material and preparation method thereof |
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| CN106784651A (en) * | 2016-11-22 | 2017-05-31 | 武汉理工大学 | Connection nano-material and its preparation method and application in carbon-encapsulated iron potassium manganate |
| CN108615874B (en) * | 2018-04-03 | 2019-08-20 | 华南理工大学 | A kind of kalium ion battery positive electrode and preparation method thereof based on nickel manganese binary oxide |
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| CN106602054A (en) * | 2016-12-26 | 2017-04-26 | 东北大学 | Lithium ion battery positive electrode material and preparation method and application thereof |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019192171A1 (en) * | 2018-04-03 | 2019-10-10 | 华南理工大学 | Nickel-manganese binary oxide-based potassium ion battery positive electrode material and preparation method therefor |
| WO2020124507A1 (en) * | 2018-12-20 | 2020-06-25 | 深圳先进技术研究院 | Crystalline material, preparation method therefor and application thereof, positive electrode active material of battery, positive electrode material of battery, battery and electrical equipment |
| WO2020124648A1 (en) * | 2018-12-20 | 2020-06-25 | 中国科学院深圳先进技术研究院 | Application of fluorinated oxalate material, and product containing fluorinated oxalate material and preparation method therefor and use thereof |
| CN111349001A (en) * | 2018-12-20 | 2020-06-30 | 深圳先进技术研究院 | Crystal material, preparation method and application thereof, battery positive electrode active material, battery positive electrode material, battery and electric equipment |
| CN111354943A (en) * | 2018-12-20 | 2020-06-30 | 中国科学院深圳先进技术研究院 | Use of fluorinated oxalate materials and products comprising fluorinated oxalate materials, methods of making and uses thereof |
| CN111349001B (en) * | 2018-12-20 | 2023-09-19 | 深圳先进技术研究院 | Crystal material, preparation method and application thereof, battery positive electrode active material, battery positive electrode material, battery and electric equipment |
| CN113270581A (en) * | 2021-04-23 | 2021-08-17 | 佛山市天劲新能源科技有限公司 | Potassium ion battery electrode material and preparation method and application thereof |
| CN113871586A (en) * | 2021-09-07 | 2021-12-31 | 武汉理工大学 | Controllable manganese-based layered oxide electrode material and preparation method and application thereof |
| CN115286049A (en) * | 2022-07-26 | 2022-11-04 | 青岛大学 | Preparation method of lithium-doped potassium nickel manganate material, positive electrode material and battery |
| CN115745030A (en) * | 2023-01-09 | 2023-03-07 | 浙江帕瓦新能源股份有限公司 | Positive electrode material of potassium ion battery, precursor of positive electrode material and preparation method of positive electrode material |
| CN117658243A (en) * | 2024-01-31 | 2024-03-08 | 成都大学 | Potassium ion battery anode material and preparation method thereof |
| CN117658243B (en) * | 2024-01-31 | 2024-04-23 | 成都大学 | Potassium ion battery anode material and preparation method thereof |
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| Publication number | Publication date |
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| WO2019192171A1 (en) | 2019-10-10 |
| CN108615874B (en) | 2019-08-20 |
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