CN106992286B - A kind of preparation method of high capacity trielement composite material - Google Patents
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- H—ELECTRICITY
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- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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 belongs to field of lithium ion battery material preparation, a kind of preparation method of high capacity trielement composite material, the trielement composite material is using ternary material as core, and nitrogenous graphene oxide is shell and is coated with the nucleocapsid trielement composite material of carbonizable substance formation on its surface；Preparation method are as follows: the 1) preparation of nitrogenous graphene oxide: 2) ternary material/graphene preparation: 3) ternary material/graphene coating modification.The present invention by improving the gram volume of graphene to graphene oxide doped nitrogen, while being coated on the gram volume performance that its ternary material is improved on ternary material surface；By the way that its material specific surface area can be greatly lowered to material surface cladding, its first charge discharge efficiency is improved；Since there is density height using the graphene oxide of hydro-thermal method preparation, cause its imbibition ability poor, by adulterating hydrogen peroxide, oxidation pore-creating is carried out to its surface, improves the imbibition liquid-keeping property of its graphene.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, specifically a kind of high capacity trielement composite material and its
Preparation method.
Background technique
The raising that electric car course continuation mileage is required with market, it is desirable that lithium ion battery has higher energy close
Degree, security performance and its high rate performance.And the lithium ion battery of existing market is high with ternary battery energy density, the circulation longevity
It orders the advantages that long and is widely used in the fields such as electric car, bus, but its energy density is relatively low, limits it in some fields
Popularization.Therefore the gram volume and its first charge discharge efficiency for improving ternary used in battery tertiary cathode material become the heat studied at present
Point.And doping techniques are then presently the most one of common, the optimal method of effect, that is, pass through doping metals, oxygen between the materials
Compound and its other materials improve the performance of its gram volume.For example patent (1041578455 A of CN) discloses a kind of graphite oxide
The method that alkene organic solvent prepares graphene complex ternary material, by improving ternary material in ternary material surface coated graphite alkene
The electric conductivity of material, high rate performance, but the biggish specific surface area of its graphene, its first charge discharge efficiency is reduced, and reduce ternary material
The performance of gram volume.And the secondary specific surface area for coating and can then reducing trielement composite material is carried out, and reduce its material surface
With the reactivity of electrolyte and its probability of happening of its side reaction is reduced, and improves its first charge discharge efficiency, and then improve material
Gram volume plays and its energy density.
Summary of the invention
It is played to further increase the gram volume of ternary material, the present invention is prepared by N doping and its carbon coating combination method
The trielement composite material that gram volume is high out, first charge discharge efficiency is high, high rate performance is good.
The technical scheme is that a kind of preparation method of high capacity trielement composite material, the tri compound material
Material is using ternary material as core, and nitrogenous graphene oxide is shell and is coated with the nucleocapsid tri compound of carbonizable substance formation on its surface
Material；Preparation method are as follows: the 1) preparation of nitrogenous graphene oxide: 2) ternary material/graphene preparation: 3) ternary material/
The coating modification of graphene: in parts by weight, it is characterised in that:
1), the preparation of nitrogenous graphene oxide: the graphene oxide solution that 1000ml concentration is 1~10mg/ml is weighed, is surpassed
Addition concentration is 1~30% hydrogen peroxide 10~100mg and 5~50mg nitrogen source after sound is uniformly dispersed, and is contained after being uniformly dispersed
Nitrogen oxidation graphene solution A；
2), ternary material/graphene preparation: weighing the nitrogenous graphene oxide solution A of 1000ml, and add 10~
The ternary material of 100g, and ultrasonic disperse it is uniform after obtain mixed solution B, and be put into autoclave, and dried in air blast
In case, 150~200 DEG C being warming up to, and keep the temperature 2~6h, Temperature fall to room temperature, is obtained by filtration trielement composite material later, it
After be transferred in vacuum oven, and temperature be 40~80 DEG C of progress 24~72h of low temperature drying, finally obtain ternary material/
Graphene composite material C,
3) it, ternary material/graphene coating modification: weighs 10~50g ternary material/graphene composite material and is put into
500ml, concentration filter, and be transferred in tube furnace, to be stirred cladding in 10% hydrocarbon solution in indifferent gas
In atmosphere, it is sintered carbonization, finally obtains ternary material/graphene composite material that external sheath has carbonizable substance.
Nitrogen source is one of aniline, pyrroles, thiophene, melamine, ammonium hydroxide in the step 1)；
In the step 2) during low temperature drying, wherein carrying out moisturizing to ternary material every 4 hours；
Step 3) the Carbonization Conditions are as follows: be warming up to 600~800 DEG C first with 1~10 DEG C/min of heating rate, and protect
1~3h of temperature, later Temperature fall to room temperature.
Step 3) the hydrocarbon is that sucrose, glucose, phenolic resin, epoxy resin, polypropylene be fine, polychlorostyrene second
One of alkene, polyurethane, polypropylene, melamine, pitch, tar, cellulose, lignin, starch, shell, fruit stone carbon contains
Measure high compound.
The present invention by improving the gram volume of graphene to graphene oxide doped nitrogen, while being coated on ternary material table
The gram volume that its ternary material is improved in face plays；It since graphene has biggish specific surface area, causes its side reaction more, leads to
Its material specific surface area can be greatly lowered to material surface cladding by crossing, and improve its first charge discharge efficiency；Due to using hydro-thermal legal system
Standby graphene oxide has density height, causes its imbibition ability poor, by adulterating hydrogen peroxide, carries out oxidation to its surface and makes
The imbibition liquid-keeping property of its graphene is improved in hole.
Detailed description of the invention
Fig. 1 is the SEM picture for the trielement composite material that embodiment 1 is prepared.
Specific embodiment
A kind of preparation method of high capacity trielement composite material, the trielement composite material be using ternary material as core,
Nitrogenous graphene oxide is shell and is coated with the nucleocapsid trielement composite material of carbonizable substance formation on its surface；Preparation method are as follows:
1) preparation of nitrogenous graphene oxide: 2) ternary material/graphene preparation: 3) ternary material/graphene coating modification.
Embodiment 1:
A kind of preparation method of high capacity trielement composite material, step are as follows:
1, the preparation of nitrogenous graphene oxide:
The graphene oxide solution that 1000ml concentration is 5mg/ml is weighed, ultrasonic disperse uniformly adds 70mg hydrogen peroxide afterwards
(concentration 10%) and its 20mg pyrroles, and nitrogenous graphene oxide solution A is obtained after being uniformly dispersed；
2, ternary material/graphene preparation:
The nitrogenous graphene oxide solution A of 1000ml is weighed later, and adds the LiNi of 50g0.6Co0.2Mn0.2O2Ternary material
Material, and ultrasonic disperse it is uniform after obtain mixed solution B, and be put into autoclave, and in convection oven, be warming up to
180 DEG C, and 3h is kept the temperature, Temperature fall to room temperature, is obtained by filtration trielement composite material later later, is transferred to vacuum drying later
In case, and it is 50 DEG C of progress low temperature drying 48h in temperature, finally obtains ternary/graphene composite material C,
3, ternary material/graphene coating modification:
It weighs 30g ternary/graphene composite material and is put into 500ml, in the glucose solution that concentration is 10%, stirred
Cladding is mixed, is filtered later, and is transferred in tube furnace, and in an inert atmosphere, is sintered carbonization (Carbonization Conditions are as follows: first
700 DEG C are warming up to 5 DEG C/min of heating rate, and keeps the temperature 2h), finally obtain ternary material/stone that external sheath has carbonizable substance
Black alkene composite material.
Embodiment 2:
1, the preparation of nitrogenous graphene oxide:
The graphene oxide solution that 1000ml concentration is 1mg/ml is weighed, ultrasonic disperse uniformly adds 10mg hydrogen peroxide afterwards
(concentration 1%) and its 10mg melamine, and nitrogenous graphene oxide solution A is obtained after being uniformly dispersed；
2, ternary material/graphene preparation:
The nitrogenous graphene oxide solution A of 1000ml is weighed later, and adds the LiNi of 10g0.6Co0.2Mn0.2O2Ternary material
Material, and ultrasonic disperse it is uniform after obtain mixed solution B, and be put into autoclave, and in convection oven, be warming up to
150 DEG C, and 1h is kept the temperature, Temperature fall to room temperature, is obtained by filtration trielement composite material later later, is transferred to vacuum drying later
In case, and it is 40 DEG C of progress low temperature drying 72h in temperature, finally obtains ternary/graphene composite material C,
3, ternary material/graphene coating modification:
It weighs 10g ternary/graphene composite material and is put into 500ml, in the sucrose solution that concentration is 10%, be stirred
Cladding, filter later, and be transferred in tube furnace, and in an inert atmosphere, be sintered carbonization (Carbonization Conditions are as follows: first with
1 DEG C/min of heating rate is warming up to 600 DEG C, and keeps the temperature 3h), finally obtain ternary material/graphite that external sheath has carbonizable substance
Alkene composite material.
Embodiment 3:
1, the preparation of nitrogenous graphene oxide:
The graphene oxide solution that 1000ml concentration is 10mg/ml is weighed, ultrasonic disperse uniformly adds 100mg hydrogen peroxide afterwards
(concentration 30%) and its 50mg thiophene, and nitrogenous graphene oxide solution A is obtained after being uniformly dispersed；
2, ternary material/graphene preparation:
The nitrogenous graphene oxide solution A of 1000ml is weighed later, and adds the LiNi of 100g0.6Co0.2Mn0.2O2Ternary
Material, and ultrasonic disperse it is uniform after obtain mixed solution B, and be put into autoclave, and in convection oven, be warming up to
200 DEG C, and 1h is kept the temperature, Temperature fall to room temperature, is obtained by filtration trielement composite material later later, is transferred to vacuum drying later
In case, and temperature be 80 DEG C of progress low temperature dryings for 24 hours, finally obtain ternary/graphene composite material C,
3, ternary material/graphene coating modification:
It weighs 50g ternary/graphene composite material and is put into 500ml, in the phenol resin solution that concentration is 10%, carry out
Stirring cladding, is filtered, and be transferred in tube furnace, and in an inert atmosphere later, is sintered carbonization (Carbonization Conditions are as follows: first
First with 10 DEG C/min of heating rate be warming up to 800 DEG C, and keep the temperature 1h), finally obtain external sheath have the ternary material of carbonizable substance/
Graphene composite material.
Comparative example 1:
The graphene oxide solution for taking 3.6ml concentration to be 8.76 mg/ ml is weighed, is scattered in and fills 50 ml
In the reaction kettle of anhydrous isopropyl alcohol, it is put into magneton, utilizes ultrasonic wave aid dispersion；0.9981g ternary material is added later
LiNi0.5Co0.3Mn0.2O2, point 3 addition reaction kettle natural coolings, obtain graphene oxide/LiNi0.6Co0.2Mn0.2O2
Compound.30g ternary material/graphene composite material is weighed later is put into 500ml, the glucose solution that concentration is 10%
In, it is stirred cladding, is filtered later, and is transferred in tube furnace, and in an inert atmosphere, is sintered carbonization (carbonization item
Part are as follows: be warming up to 700 DEG C first with 5 DEG C/min of heating rate, and keep the temperature 2h), finally obtain external sheath has carbonizable substance three
First material/graphene composite material
1, SEM is tested:
As seen from Figure 1, the trielement composite material presentation that embodiment 1 is prepared is uniform spherical, is reasonably distributed.
2, electrochemical property test:
2.1 production button cell tests.
Button cell is dressed up to the trielement composite material that embodiment 1-3 and comparative example are prepared as follows and is surveyed
Examination:
1) it adds in 220mLN- methyl pyrrolidone, stirs in 95g positive electrode, 1g Kynoar, 4g conductive agent SP
It mixes and uniformly prepares anode sizing agent, be coated on copper foil, drying, roll pressing obtains positive.
Electrolyte uses LiPF6For electrolyte, concentration 1.3mol/L, the EC and DEC that volume ratio is 1:1 are solvent, gold
Belong to lithium piece to be used as to electrode, diaphragm uses polyethylene (PE), polypropylene (PP) or poly- second propylene (PEP) composite membrane, is being flushed with hydrogen gas
Glove box according to existing method assemble button cell A1, A2, A3 and B1.
2) above-mentioned button cell is tested on new prestige 5V/10mA type cell tester, charging/discharging voltage range 2.7-
4.2V, charge-discharge magnification 0.1C, test result are as shown in table 1.
1 button cell test result of table
| Detain electric battery | A1 | A2 | A3 | B1 |
| Discharge capacity (mAh/g) for the first time | 179.9 | 178.1 | 176.3 | 165.1 |
| First charge discharge efficiency (%) | 96.1 | 96.0 | 953.8 | 93.1 |
As can be seen from Table 1, embodiment prepares the gram volume of trielement composite material and its first charge discharge efficiency is better than comparative example,
The reason for this is that the nitrogen-atoms adulterated in ternary material, the gram volume for improving its material is played, while the graphene adulterated improves it
The delivery rate of lithium ion during first charge-discharge, and improve its first charge discharge efficiency.
(2) soft-package battery is tested
Respectively with embodiment 1, embodiment 2, the ternary material that embodiment 3 and comparative example are prepared as positive electrode, and
Anode pole piece is prepared, using artificial graphite as negative electrode material, using LiPF6/ EC+DEC(volume ratio 1: 1) being electrolyte,
2400 film of Celgard is diaphragm, prepares 5Ah soft-package battery C1, C2, C3 and D1, and test the cycle performance of its soft-package battery
And high rate performance；
2.1 high rate performance
It is later that 0.3C charges with multiplying power, is put respectively with multiplying power for the multiplying power of 1.0C, 2.0C, 3.0C, 4.0C
Electricity, test voltage range are 2.7V-4.2V, calculate discharge capacity and discharge capacitance later.
Table 2, embodiment are compared with the multiplying power of comparative example
As can be seen from Table 2, multiplying power discharging ability of embodiment under the conditions of different multiplying is better than comparative example, reason
For trielement composite material is coated with the high grapheme material of conductivity, improves lithium ion under the conditions of its big multiplying power and its electronics
Transmission rate, to improve its high rate performance.
2.2 cycle performance
It is later 1.0C with rate of charge, discharge-rate 1.0C, voltage range 3.0-4.3V test its soft-package battery
Cycle performance (500 times).
3 cycle performance of table compares
| Serial number | Initial capacity (Ah) | Capacity (Ah) after 500 times | Conservation rate (%) |
| Embodiment 1(C1) | 5.22 | 4.87 | 93.4 |
| Embodiment 2(C2) | 5.19 | 4.83 | 93.1 |
| Embodiment 3(C3) | 5.18 | 4.80 | 92.8 |
| Comparative example (D1) | 5.19 | 4.63 | 89.2 |
As can be seen from Table 3, the soft-package battery cycle performance that embodiment is prepared is better than comparative example, the reason for this is that passing through
Hydrogen peroxide improves the imbibition ability of material to material pore-creating, and improves its cycle performance；The nitrogen-atoms tool adulterated in material simultaneously
Play the role of promoting material structure stable and its combine the characteristic of graphene high conductivity, can be further improved following for its material
Ring performance.
Claims (2)
1. a kind of preparation method of high capacity trielement composite material, the trielement composite material is contained using ternary material as core
Nitrogen graphene is shell and is coated with the nucleocapsid trielement composite material of carbonizable substance formation on its surface；Preparation method are as follows: 1) nitrogenous
The preparation of graphene oxide: 2) ternary material/graphene preparation: 3) ternary material/graphene coating modification: with parts by weight
Meter, it is characterised in that:
1) graphene oxide solution that 1000ml concentration is 1~10mg/ml, ultrasound point, the preparation of nitrogenous graphene oxide: are weighed
Addition concentration is 1~30% hydrogen peroxide 10~100mg and 5~50mg nitrogen source after dissipating uniformly, and nitrogenous oxygen is obtained after being uniformly dispersed
Graphite alkene solution A；The nitrogen source is one of aniline, pyrroles, thiophene, melamine, ammonium hydroxide；
2), ternary material/graphene preparation: the nitrogenous graphene oxide solution A of 1000ml is weighed, and adds 10~100g's
Ternary material, and ultrasonic disperse it is uniform after obtain mixed solution B, and be put into autoclave, and in convection oven, rise
Temperature keeps the temperature 2~6h to 150~200 DEG C, and Temperature fall to room temperature, is obtained by filtration trielement composite material, is transferred to later later
In vacuum oven, and it is 40~80 DEG C of progress 24~72h of low temperature drying in temperature, it is multiple finally obtains ternary material/graphene
Condensation material C, during the low temperature drying, wherein carrying out moisturizing to ternary material every 4 hours；
3) it, ternary material/graphene coating modification: weighs 10~50g ternary material/graphene composite material and is put into
500ml, concentration filter, and be transferred in tube furnace, to be stirred cladding in 10% hydrocarbon solution in indifferent gas
In atmosphere, it is sintered carbonization, finally obtains ternary material/graphene composite material that external sheath has carbonizable substance；The carbon
Change condition are as follows: be warming up to 600~800 DEG C first with 1~10 DEG C/min of heating rate, and keep the temperature 1~3h, Temperature fall arrives later
Room temperature.
2. a kind of preparation method of high capacity trielement composite material according to claim 1, it is characterised in that: the step
Rapid 3) hydrocarbon is that sucrose, glucose, phenolic resin, epoxy resin, polypropylene be fine, polyvinyl chloride, polyurethane, poly- third
The high compound of one of alkene, melamine, pitch, tar, cellulose, lignin, starch, shell, fruit stone carbon content.
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| CN107579237B (en) * | 2017-09-13 | 2021-11-05 | 桑顿新能源科技(长沙)有限公司 | Preparation method of ternary cathode material and ternary cathode material |
| CN107512911A (en) * | 2017-09-14 | 2017-12-26 | 原晋波 | A kind of preparation method of energy-storage travelling wave tube composite |
| CN108183039B (en) * | 2017-12-11 | 2020-11-06 | 中国科学院过程工程研究所 | Preparation method of carbon-modified titanium niobate material, lithium ion capacitor and negative electrode slurry thereof |
| CN108899498B (en) * | 2018-06-26 | 2020-10-02 | 上海亿司智能科技有限公司 | Preparation method of environment-friendly flexible lithium ion battery positive electrode framework material |
| CN109728261B (en) * | 2018-11-30 | 2022-03-29 | 宁波容百新能源科技股份有限公司 | Ternary cathode material and preparation method thereof |
| CN111326814A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for repairing anode material of waste ternary battery by ultrasonic hydrothermal method |
| CN115148945B (en) * | 2022-06-24 | 2023-03-07 | 广东墨睿科技有限公司 | Modification method of high-nickel ternary cathode material |
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