CN106992286A - A kind of preparation method of high power capacity trielement composite material - Google Patents
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Abstract
The invention belongs to field of lithium ion battery material preparation, a kind of preparation method of high power capacity trielement composite material, described trielement composite material is that, using ternary material as core, nitrogenous graphene oxide is shell and has the nucleocapsid trielement composite material of carbonizable substance formation in its Surface coating；Its preparation method is：1）The preparation of nitrogenous graphene oxide：2）The preparation of ternary material/graphene：3）The coating modification of ternary material/graphene.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 efficiency first is improved；Because the graphene oxide prepared using hydro-thermal method is had, density is high, cause its imbibition ability poor, by the hydrogen peroxide that adulterates, carries out oxidation pore-creating 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 power capacity trielement composite material and its
Preparation method.
Background technology
The raising required with market electric automobile course continuation mileage, it is desirable to which lithium ion battery has higher energy close
Degree, security performance and its high rate performance.And the lithium ion battery of existing market is with ternary battery energy density height, circulation longevity
The advantages of ordering long and be widely used in the fields such as electric automobile, bus, but its energy density is relatively low, limits it in some fields
Popularization.Therefore improve the gram volume of ternary used in battery tertiary cathode material and its efficiency turns into the heat studied at present first
Point.And doping techniques are then presently the most one of conventional, best results methods, that is, pass through doping metals between the materials, oxygen
Compound and its other materials improve the performance of its gram volume.Such as patent（CN 1041578455 A）Disclose a kind of graphite oxide
The method that alkene organic solvent prepares graphene complex ternary material, by improving ternary material in ternary material Surface coating graphene
The electric conductivity of material, high rate performance, but the larger specific surface area of its graphene, its efficiency first is reduced, and reduce ternary material
The performance of gram volume.And the specific surface area of trielement composite material can then be reduced by carrying out secondary cladding, and reduce its material surface
With the reactivity of electrolyte and its reducing the probability of happening of its side reaction, and its efficiency first is improved, and then improve material
Gram volume is played and its energy density.
The content of the invention
Further to improve the gram volume performance of ternary material, the present invention passes through N doping and its prepared by carbon coating combination method
Go out gram volume height, the first good trielement composite material of efficiency high, high rate performance.
The technical scheme is that：A kind of preparation method of high power capacity trielement composite material, described tri compound material
Material is that, using ternary material as core, nitrogenous graphene oxide is shell and has the nucleocapsid tri compound of carbonizable substance formation in its Surface coating
Material；Its preparation method is：1）The preparation of nitrogenous graphene oxide：2）The preparation of ternary material/graphene：3）Ternary material/
The coating modification of graphene：In parts by weight, it is characterised in that：
1）, nitrogenous graphene oxide preparation：Weigh the graphene oxide solution that 1000ml concentration is 1~10mg/ml, ultrasound point
Dissipate it is uniform after addition concentration be 1~30% hydrogen peroxide 10~100mg and 5~50mg nitrogen source, and obtain nitrogenous oxygen after being uniformly dispersed
Graphite alkene solution A；
2）, ternary material/graphene preparation：1000ml nitrogenous graphene oxide solution A 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 is incubated 2~6h to 150~200 DEG C, and Temperature fall is filtrated to get trielement composite material, be transferred to afterwards to room temperature afterwards
In vacuum drying chamber, and it is 40~80 DEG C of progress 24~72h of low temperature drying in temperature, finally obtains ternary material/graphene multiple
Condensation material C,
3）, ternary material/graphene coating modification：10~50g ternary materials/graphene composite material is weighed to be put into
500ml, concentration filters in 10% hydrocarbon solution, to be stirred cladding, and is transferred in tube furnace, in indifferent gas
In atmosphere, carbonization is sintered, finally obtaining external sheath has ternary material/graphene composite material of carbonizable substance.
Described step 1）Middle nitrogen source is one kind in aniline, pyrroles, thiophene, melamine, ammoniacal liquor；
Described step 2）During middle low temperature drying, wherein carrying out moisturizing to ternary material every 4 hours；
Described step 3）Carbonization Conditions are：600~800 DEG C are warming up to 1~10 DEG C/min of heating rate first, and is incubated 1
~3h, Temperature fall is to room temperature afterwards.
Described step 3）Hydrocarbon is that sucrose, glucose, phenolic resin, epoxy resin, polypropylene be fine, polychlorostyrene second
A kind of carbon in alkene, polyurethane, polypropylene, melamine, pitch, tar, cellulose, lignin, starch, shell, fruit stone contains
The high compound of amount.
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 is played；Because graphene has larger specific surface area, cause its side reaction more, lead to
Its material specific surface area can be greatly lowered to material surface cladding by crossing, and improve its efficiency first；Due to using hydro-thermal legal system
Standby graphene oxide has density height, causes its imbibition ability poor, by the hydrogen peroxide that adulterates, and carries out oxidation to its surface and makes
Hole, improves the imbibition liquid-keeping property of its graphene.
Brief description of the drawings
Fig. 1 is the SEM pictures for the trielement composite material that embodiment 1 is prepared.
Embodiment
A kind of preparation method of high power capacity trielement composite material, described trielement composite material be using ternary material as core,
Nitrogenous graphene oxide is shell and has the nucleocapsid trielement composite material of carbonizable substance formation in its Surface coating；Its preparation method is：
1）The preparation of nitrogenous graphene oxide：2）The preparation of ternary material/graphene：3）The coating modification of ternary material/graphene.
Embodiment 1：
A kind of preparation method of high power capacity trielement composite material, step is：
1st, 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；
2nd, the preparation of ternary material/graphene：
1000ml nitrogenous graphene oxide solution A is weighed afterwards, and adds 50g LiNi0.6Co0.2Mn0.2O2Ternary 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 180
DEG C, and 3h is incubated, Temperature fall is filtrated to get trielement composite material, vacuum drying chamber is transferred to afterwards afterwards to room temperature afterwards
In, and be 50 DEG C of progress low temperature drying 48h in temperature, ternary/graphene composite material C is finally obtained,
3rd, the coating modification of ternary material/graphene：
Weigh 30g ternarys/graphene composite material and be put into 500ml, concentration is in 10% glucose solution, is stirred bag
Cover, filter afterwards, and be transferred in tube furnace, and in an inert atmosphere, be sintered carbonization（Carbonization Conditions are：First with liter
Warm 5 DEG C/min of speed is warming up to 700 DEG C, and is incubated 2h）, finally obtaining external sheath has ternary material/graphene of carbonizable substance
Composite.
Embodiment 2：
1st, 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 melamines, and nitrogenous graphene oxide solution A is obtained after being uniformly dispersed；
2nd, the preparation of ternary material/graphene：
1000ml nitrogenous graphene oxide solution A is weighed afterwards, and adds 10g LiNi0.6Co0.2Mn0.2O2Ternary 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 150
DEG C, and 1h is incubated, Temperature fall is filtrated to get trielement composite material, vacuum drying chamber is transferred to afterwards afterwards to room temperature afterwards
In, and be 40 DEG C of progress low temperature drying 72h in temperature, ternary/graphene composite material C is finally obtained,
3rd, the coating modification of ternary material/graphene：
Weigh 10g ternarys/graphene composite material and be put into 500ml, concentration in 10% sucrose solution, to be stirred cladding,
Filter, and be transferred in tube furnace afterwards, and in an inert atmosphere, be sintered carbonization（Carbonization Conditions are：First with the speed that heats up
1 DEG C/min of rate is warming up to 600 DEG C, and is incubated 3h）, finally obtaining external sheath has ternary material/graphene of carbonizable substance compound
Material.
Embodiment 3：
1st, 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（It is dense
Degree 30%）And its 50mg thiophene, and nitrogenous graphene oxide solution A is obtained after being uniformly dispersed；
2nd, the preparation of ternary material/graphene：
1000ml nitrogenous graphene oxide solution A is weighed afterwards, and adds 100g LiNi0.6Co0.2Mn0.2O2Ternary 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 incubated, Temperature fall is filtrated to get trielement composite material, vacuum drying chamber is transferred to afterwards afterwards to room temperature afterwards
In, and be 80 DEG C of progress low temperature drying 24h in temperature, ternary/graphene composite material C is finally obtained,
3rd, the coating modification of ternary material/graphene：
Weigh 50g ternarys/graphene composite material and be put into 500ml, concentration is in 10% phenol resin solution, is stirred
Cladding, is filtered afterwards, and is transferred in tube furnace, and in an inert atmosphere, is sintered carbonization（Carbonization Conditions are：First with
10 DEG C/min of heating rate is warming up to 800 DEG C, and is incubated 1h）, finally obtaining external sheath has ternary material/graphite of carbonizable substance
Alkene composite.
Comparative example 1：
Weigh take 3.6ml concentration be 8.76 mg/ ml graphene oxide solution, be scattered in fill 50 ml without
In the reactor of water isopropanol, magneton is put into, it is scattered using ultrasonic assistant；0.9981g ternary materials are added afterwards
LiNi0.5Co0.3Mn0.2O2, point 3 addition reactor natural coolings, obtain graphene oxide/LiNi0.6Co0.2Mn0.2O2
Compound.30g ternary materials/graphene composite material is weighed afterwards and is put into 500ml, and concentration is 10% glucose solution
In, cladding is stirred, is filtered afterwards, and be transferred in tube furnace, and in an inert atmosphere, it is sintered carbonization（Be carbonized bar
Part is：700 DEG C are warming up to 5 DEG C/min of heating rate first, and is incubated 2h）, finally obtaining external sheath has the three of carbonizable substance
First material/graphene composite material
1st, SEM is tested：
As seen from Figure 1, the trielement composite material that embodiment 1 is prepared is presented uniform spherical, is reasonably distributed.
2nd, electrochemical property test：
2.1 make button cell test.
Button cell is dressed up as follows to the trielement composite material that embodiment 1-3 and comparative example are prepared and surveyed
Examination：
1）Added in 95g positive electrodes, 1g Kynoar, 4g conductive agents SP in 220mLN- methyl pyrrolidones, stirring is equal
It is even to prepare anode sizing agent, it is coated on copper foil, dries, roll pressing obtains positive pole.
Electrolyte uses LiPF6For electrolyte, concentration is 1.3mol/L, and volume ratio is 1:1 EC and DEC is solvent, gold
Belong to lithium piece as to electrode, barrier film uses polyethylene (PE), polypropylene (PP) or poly- second propylene (PEP) composite membrane, is being flushed with hydrogen gas
Glove box in assemble button cell A1, A2, A3 and B1 according to existing method.
2）Above-mentioned button cell is tested on new prestige 5V/10mA type cell testers, charging/discharging voltage scope 2.7-
4.2V, charge-discharge magnification 0.1C, test result is as shown in table 1.
The button cell test result of table 1
| The electric battery of button | A1 | A2 | A3 | B1 |
| Discharge capacity first（mAh/g） | 179.9 | 178.1 | 176.3 | 165.1 |
| Efficiency first（%） | 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 efficiency is better than comparative example first, and it is former
Because the nitrogen-atoms adulterated in ternary material, the gram volume for improving its material is played, while the graphene of doping improves it first
The transfer rate of lithium ion in charge and discharge process, and improve its efficiency first.
（2）Soft-package battery is tested
Respectively with embodiment 1, embodiment 2, the ternary material that embodiment 3 and comparative example are prepared is prepared as positive electrode
Go out anode pole piece, using Delanium as negative material, using LiPF6/EC+DEC（Volume ratio 1: 1）For electrolyte, Celgard
2400 films are barrier film, prepare 5Ah soft-package battery C1, C2, C3 and D1, and test the cycle performance of its soft-package battery and forthright again
Energy；
2.1 high rate performance
Charged, the multiplying power using multiplying power as 1.0C, 2.0C, 3.0C, 4.0C is discharged respectively, surveyed by 0.3C of multiplying power afterwards
Examination voltage range is 2.7V-4.2V, and discharge capacity and discharge capacitance are calculated afterwards.
Table 2, embodiment are compared with the multiplying power of comparative example
As can be seen from Table 2, multiplying power discharging ability of the embodiment under the conditions of different multiplying is better than comparative example, and its reason is, and three
First composite is coated with the high grapheme material of conductance, improves the transmission speed of lithium ion and its electronics under the conditions of its big multiplying power
Rate, so as to improve its high rate performance.
2.2 cycle performance
Afterwards using rate of charge as 1.0C, discharge-rate is 1.0C, and voltage range is 3.0-4.3V, tests following for its soft-package battery
Ring performance（500 times）.
The cycle performance of table 3 compares
| Sequence number | Initial capacity（Ah） | Capacity after 500 times（Ah） | 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, and its reason is to pass through dioxygen
Water improves the imbibition ability of material to material pore-creating, and improves its cycle performance；The nitrogen-atoms adulterated simultaneously in material, which has, to be promoted
Enter the stable effect of material structure and its combine the characteristic of graphene high conductivity, can further improve the cyclicity of its material
Energy.
Claims (5)
1. a kind of preparation method of high power capacity trielement composite material, described trielement composite material is, using ternary material as core, to contain
Nitrogen oxidation graphene is shell and has the nucleocapsid trielement composite material of carbonizable substance formation in its Surface coating；Its preparation method is：1）
The preparation of nitrogenous graphene oxide：2）The preparation of ternary material/graphene：3）The coating modification of ternary material/graphene：With weight
Measure part meter, it is characterised in that：
1）, nitrogenous graphene oxide preparation：Weigh the graphene oxide solution that 1000ml concentration is 1~10mg/ml, ultrasound point
Dissipate it is uniform after addition concentration be 1~30% hydrogen peroxide 10~100mg and 5~50mg nitrogen source, and obtain nitrogenous oxygen after being uniformly dispersed
Graphite alkene solution A；
2）, ternary material/graphene preparation：1000ml nitrogenous graphene oxide solution A 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 is incubated 2~6h to 150~200 DEG C, and Temperature fall is filtrated to get trielement composite material, be transferred to afterwards to room temperature afterwards
In vacuum drying chamber, and it is 40~80 DEG C of progress 24~72h of low temperature drying in temperature, finally obtains ternary material/graphene multiple
Condensation material C,
3）, ternary material/graphene coating modification：10~50g ternary materials/graphene composite material is weighed to be put into
500ml, concentration filters in 10% hydrocarbon solution, to be stirred cladding, and is transferred in tube furnace, in indifferent gas
In atmosphere, carbonization is sintered, finally obtaining external sheath has ternary material/graphene composite material of carbonizable substance.
2. a kind of N doping trielement composite material according to claim 1 and preparation method thereof, it is characterised in that：Described
Step 1）Middle nitrogen source is one kind in aniline, pyrroles, thiophene, melamine, ammoniacal liquor.
3. a kind of N doping trielement composite material according to claim 1 and preparation method thereof, it is characterised in that：Described
Step 2）During middle low temperature drying, wherein carrying out moisturizing to ternary material every 4 hours.
4. a kind of N doping trielement composite material according to claim 1 and preparation method thereof, it is characterised in that：Described
Step 3）Carbonization Conditions are：600~800 DEG C are warming up to 1~10 DEG C/min of heating rate first, and is incubated 1~3h, afterwards certainly
So cool to room temperature.
5. a kind of N doping trielement composite material according to claim 1 and preparation method thereof, it is characterised in that：Described
Step 3）Hydrocarbon is sucrose, glucose, phenolic resin, epoxy resin, fine polypropylene, polyvinyl chloride, polyurethane, poly- third
A kind of high compound of carbon content in alkene, melamine, pitch, tar, cellulose, lignin, starch, shell, fruit stone.
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| CN107579237A (en) * | 2017-09-13 | 2018-01-12 | 桑顿新能源科技有限公司 | A kind of tertiary cathode material preparation method and tertiary cathode material |
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| CN107512911A (en) * | 2017-09-14 | 2017-12-26 | 原晋波 | A kind of preparation method of energy-storage travelling wave tube composite |
| CN108183039A (en) * | 2017-12-11 | 2018-06-19 | 中国科学院过程工程研究所 | Preparation method, carbon modification titanium niobate material, lithium-ion capacitor and its negative electrode slurry of carbon modification titanium niobate material |
| CN108899498A (en) * | 2018-06-26 | 2018-11-27 | 宁波革创新材料科技有限公司 | The preparation method of environmental protection flexible lithium ion cell positive framework material |
| CN109728261A (en) * | 2018-11-30 | 2019-05-07 | 宁波容百新能源科技股份有限公司 | A kind of tertiary 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 |
| CN115148945A (en) * | 2022-06-24 | 2022-10-04 | 广东墨睿科技有限公司 | Modification method of high-nickel ternary cathode material |
| 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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