CN108615874B - 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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- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- 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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- H01M4/525—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.Method includes the following steps: nickel salt, manganese salt, sylvite and doped chemical salt, which are dissolved in deionized water, obtains 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 will directly be mixed containing nickel/manganese/potassium organic acid salt, obtain the presoma of acylate；Precursor powder is ground, is pre-sintered, then grinds again, roasting obtains positive electrode at high temperature.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 technique
With the sharply expansion of economic fast development and industry, using coal, petroleum, the big main energy sources of natural gas three 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 ion secondary battery is as a kind of novel, clear
Clean, the reproducible energy has the characteristics that open-circuit voltage is high, specific energy is high, 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 car.But since the rare reserves of lithium resource and fancy price are serious
Constrain application of lithium ion battery in terms of extensive.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
The concern of chemical principle and the advantages such as resourceful, cheap by researcher.Wherein kalium ion battery have with
The closest standard electrode EMF of lithium ion battery, while potassium ion has biggish ion mobility in the electrolytic solution.
The preparation of negative electrode material is focused on about the research of kalium ion battery at present more, and the research in terms of positive electrode is less.
107226475 A of Chinese invention patent application CN 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, is difficult to the problem of being mass produced.
107093739 A of Chinese invention patent application CN proposes the kalium ion battery anode material based on potassium Mn oxide
Material, capacity is up to 83.9mAh/g, but there are poor circulations, the deficiency without obvious discharge platform for this material.
105826521 A of Chinese invention patent application CN is 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 discovery, can be obtained a kind of KVPO by the method for high-temperature roasting4The kalium ion battery anode of F
Material, discharge platform and excellent high rate performance with reachable 4V, but the deficiency that this kind of material is low there are specific capacity；
Due to kalium ion battery positive electrode research still in its infancy, 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.
Summary of the invention
In view of deficiency 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 as follows: 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 of the preparation containing nickel manganese potassium one of includes 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,
Obtaining chemical formula is KaXmNibMncO2(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 one of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride 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
Stating organic solvent is one or more of ethyl alcohol, acetone, ethylene glycol；In step (1), the body of the organic solvent and deionized water
Product compares 1:1-4.
In the above method, in step (2), the acylate be one of acetate, oxalates, citrate 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 revolving 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 as follows: grind the persursor material after drying, in air gas
300~500 DEG C of 3~6h of pre-sintering, then cool to room temperature and are ground in atmosphere, 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, include the following steps: by
Acylate containing nickel manganese potassium is obtained according to the ratio ball milling mixing that nickel manganese potassium molar ratio is 0.1-0.5:0.5-0.9:0.4-1.2
To acylate precursor powder；Resulting acylate precursor powder is ground, 300~500 in air atmosphere
DEG C be pre-sintered 3~6h, then cool to room temperature and 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 prospect.
(2) method preparation of the invention is 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.
Detailed description of the invention
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 embodiment
It is further specific to the present invention combined with specific embodiments below to be described in detail, 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 acetate, 0.005mol manganese acetate and 0.013mol potassium acetate (excessive 5%) are dissolved in 20mL
Volume ratio is in the ethyl alcohol and deionized water of 1:1；
(2) by 1.299g acetic acid in the ethyl alcohol and deionized water that 10mL volume ratio is 1:2；
(3) metal salt solution is added drop-wise in acetic acid solution with 1~2 drop/s speed, then with the speed of 200 turns/min into
Row stirring 6h；
(4) moisture is heated to by 60 DEG C of gained mixed liquor under vacuum to be evaporated, obtain 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 the ratio mixing of mass ratio 8:1:1, solvent N-methyl pyrilidone (NMP) is added and stirs 4-6h, slurry is applied to completely
Aluminium foil on, it is stand-by 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 Hexafluorophosphate (KPF6)/ethylene carbonate (EC):
Dimethyl carbonate (DEC) assembles button cell as electrolyte.
Chemical property detection: 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
Range is 2-4.5V, scanning 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 nitrate, 0.009mol manganese nitrate, 0.004mol potassium hydroxide (excessive 5%) and
0.001mol ferrous nitrate is dissolved in ethylene glycol and deionized water that 50mL volume ratio is 1:4；
(2) by 1.458g dissolving oxalic acid in the ethylene glycol and deionized water that 40mL volume ratio is 1:6；
(3) oxalic acid solution is added drop-wise in metal salt solution with 1~2 drop/s speed, then with the speed of 500 turns/min into
Row stirring 12h；
(4) moisture is heated to by 120 DEG C of gained mixed liquor to be evaporated, obtain 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 0.013mol potassium acetate is replaced using 0.004mol potassium carbonate, 0.0005mol aluminium chloride replaces ferrous nitrate, etc.
The nickel sulfate of molal quantity, manganese sulfate replace nickel nitrate, manganese nitrate, and acetone replaces 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 0.005mol nickel acetate is replaced using 0.001mol nickel chloride, 0.009mol manganese chloride replaces 0.005mol acetic acid
Manganese, 0.012mol potassium chloride replace 0.013mol potassium acetate, and the magnesium chloride of equimolar number replaces 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
In addition to replacing potassium hydroxide, ferrous nitrate using the potassium citrate of equimolar number, magnesium chloride, 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 of the invention
Made any modifications, equivalent replacements, and improvements etc., should be included in the protection of the claims in the present invention within spirit and principle
Within the scope of.
Claims (6)
1. a kind of kalium ion battery positive electrode based on nickel manganese binary oxide, chemical formula are as follows: 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；
The 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 mixed solvent of organic solvent and deionized water
Middle wiring solution-forming A；
(2) in the mixed solvent that organic acid or acylate are dissolved in organic solvent and deionized water formation is obtained into solution B；
(3) solution A is added in solution B under stiring, be uniformly mixed and continuously stirred, obtain suspension C；
(4) precursor powder of the preparation containing nickel manganese potassium one of includes 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, is pre-sintered, grinding, then roast to get change is arrived
Formula is KaXmNibMncO2The positive material of (0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1)
Material；
The concrete operations of step (5) are as follows: the persursor material after drying is ground, in air atmosphere 300 ~ 500 DEG C it is pre-
It is sintered 3 ~ 6h, then cools to room temperature and is ground, be finally warming up to 700 ~ 1000 DEG C of 8 ~ 20h of roasting.
2. the kalium ion battery positive electrode according to claim 1 based on nickel manganese binary oxide, it is characterized in that: step
(1) in, the nickel salt is one or more of nickel nitrate, nickel acetate, nickel sulfate, nickel chloride；The manganese salt is manganese nitrate, acetic acid
One or more of manganese, manganese sulfate, manganese chloride；The sylvite is potassium hydroxide, potassium acetate, potassium carbonate, potassium chloride, potassium citrate
One or more of；The doped chemical salt is soluble ferric iron salt, in aluminum soluble salt, soluble magnesium salt, soluble lithium salt
More than one；The organic acid is one or more of acetic acid, oxalic acid, citric acid；The organic solvent is ethyl alcohol, acetone, second
One or more of glycol；In step (1), the volume ratio 1:1-4 of the organic solvent and deionized water.
3. the kalium ion battery positive electrode according to claim 1 based on nickel manganese binary oxide, it is characterized in that: step
(2) in, the acylate is one or more of acetate, oxalates, citrate；The organic acid be acetic acid, oxalic acid,
One or more of citric acid；The volume ratio of the organic solvent and deionized water is 1:2-6.
4. the kalium ion battery positive electrode according to claim 1 based on nickel manganese binary oxide, it is characterized in that: step
(3) in, the mixed method is that solution A is added drop-wise in solution B, and rate of addition is 1 ~ 2 drop/s or is added drop-wise to solution B molten
In liquid A, rate of addition is 1 ~ 2 drop/s；In step (3), the revolving speed of the stirring is 200 ~ 500 turns/min, mixing time is 6 ~
12h。
5. the kalium ion battery positive electrode according to claim 1 based on nickel manganese binary oxide, it is characterized in that: step
(4) in, the temperature of the heating is 60 ~ 120 DEG C.
6. based on the kalium ion battery positive electrode preparation method of nickel manganese binary oxide described in claim 1, including it is as follows
Step: the ratio ball for being 0.1-0.5:0.5-0.9:0.4-1.2 according to nickel manganese potassium molar ratio by the acylate containing nickel manganese potassium
Mill is mixed to get acylate precursor powder；Resulting acylate precursor powder is ground, in air atmosphere
300 ~ 500 DEG C of 3 ~ 6h of pre-sintering, then cool to room temperature and are ground, be finally warming up to 700 ~ 1000 DEG C of 8 ~ 20h of roasting to get
It is K to chemical formulaaXmNibMncO2(0.4≤a≤1.2,0≤m≤0.1,0.1≤b≤0.5,0.5≤c≤0.9, b+c=1) just
Pole material.
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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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| 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 |
| 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 |
| 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 |
| CN115745030B (en) * | 2023-01-09 | 2023-05-12 | 浙江帕瓦新能源股份有限公司 | Potassium ion battery anode material, precursor thereof and preparation method |
| 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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