CN108832085A - A kind of method that controllable low-temperature combustion method prepares lithium-rich anode material - Google Patents
A kind of method that controllable low-temperature combustion method prepares lithium-rich anode material Download PDFInfo
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Abstract
The invention belongs to the preparation technical fields of anode material for lithium-ion batteries, specifically provide a kind of controllable low-temperature combustion method and prepare lithium-rich anode material 2x/3Li2MnO3·(1‑x)LiMO2, (0 <x< 1, M=Ni, Co, Mn）Method.This method carries out according to the following steps：Nickel cobalt manganese metal salt is dissolved in solvent according to stoichiometric ratio, a certain amount of reducing agent and additive is added, stirs evenly, appropriate ammonium hydroxide is added dropwise and adjusts PH, obtains solution A.After a certain period of time by solution A heating evaporation, it is placed in heating furnace, its burning is made when 300-700 is spent, obtain powder B, B is collected and is ground, be placed in high temperature 700-1100 degree under Muffle furnace and calcine 5-24h, ball milling is sieved to get lithium-rich anode material is arrived after cooling.The preparation method is simple and quick, each element can be reached in the solution to molecular level mixing, ultra-fine nanometer materials can be prepared, and low energy consumption, reaction can be regulated and controled by parameter, the synthesis cost of lithium-rich anode material is greatly reduced, high rate performance and cycle performance are also improved significantly.
Description
Technical field
The invention belongs to the preparation technical fields of anode material for lithium-ion batteries, specifically provide a kind of controllable low-temperature burning
The method that method prepares lithium-rich anode material.
Background technique
As world energy sources crisis and environmental issue become increasingly conspicuous, the background for seeking new energy is national energy security aspect
The needs that increasingly rise of importance.In recent years, to the rush of demand of the new energy materials such as lithium carbonate, new energy revolution will in market
It can break out comprehensively and the impetus has shown.There is an urgent need to develop with high-energy density, high power, long circulating longevity at present in China
The lithium ion battery of life and high security.Positive electrode is the highest material of lithium ion battery cost accounting, accounts for about lithium battery
The 1/3 of core cost.The positive electrode for using and studying at present mainly has the crystal structures such as stratiform, spinelle, olivine
Lithium-containing materials mainly have LiCoO2、LiNiO2、LiMnO2、LiMn2O4、LiFePO4、LiCo1/3Ni1/3Mn1/3O2And it is some other
The positive electrode of series, but be individually present as safety is poor, expensive, the disadvantages of energy density is low, poor circulation, limit
Its development is made.Reach the requirement of 300Wh/Kg to lithium ion battery energy density with country, current commercialized positive electrode
It is unable to meet demand.And novel lithium-rich anode materialxLi2MnO3·(1-x)LiMO2(M=Co, Ni, Mn) theoretical specific capacity is high
Up to 350mAh/g, commercialization is expected to obtain the specific energy of 300Wh/Kg, but the material as made from traditional coprecipitation fills for the first time
Irreversible capacity loss discharge up to 40 ~ 100mAh/g, due to the erosion by electrolyte, the cyclicity of material is bad, Yi Jibei
The problems such as rate discharge performance is poor.Improved method mainly includes ion doping and surface cladding at present, undoubtedly improves electricity in this way
Pond production cost.
Combustion method is a kind of new material preparation method, causes chemical reaction after reactant is ignited, utilizes its own
The heat of releasing is generated high temperature and makes reaction that can voluntarily maintain and be spread in the form of combustion wave to pass through entire reactant, with
The passage of combustion wave, reactant be changed into final product rapidly.Controllable low-temperature combustion method is simple and quick, and each element can exist
Reach molecular level mixing in solution, ultra-fine nanometer materials can be prepared, and low energy consumption, reaction can be carried out by parameter
Regulation, greatly reduces the synthesis cost of lithium-rich anode material, high rate performance and cycle performance are also improved significantly.
Summary of the invention
The purpose of the present invention is to provide a kind of method that controllable low-temperature combustion method prepares lithium-rich anode material, this method
Reaction can be avoided excessively violent, save process and energy consumption, lithium-rich anode material purity obtained by parameter to response regulatory
Height, at low cost, high rate performance and cycle performance are high.
Specific technical solution of the present invention is as follows：
A kind of controllable low-temperature combustion method prepares lithium-rich anode material 2x/3Li2MnO3·(1-x)LiMO2, (0 <x< 1, M=Ni,
Co,Mn）Method, which is characterized in that carry out according to the following steps：Nickel cobalt manganese metal salt is dissolved in solvent according to stoichiometric ratio
In, a certain amount of reducing agent and additive is added, stirs evenly, appropriate ammonium hydroxide is added dropwise and adjusts PH, obtains solution A.By solution A plus
Thermal evaporation after a certain period of time, is placed in heating furnace, its burning is made when 300-700 is spent, heat preservation a period of time, taking-up obtains powder
B grinds B collection, is placed in high temperature 700-1100 degree under Muffle furnace and calcines 5-24h, and ball milling is sieved to get rich lithium is arrived just after cooling
Pole material.
Preferably, which is characterized in that the lithium salts is CH3COOLi or LiNO3Or their hydrate；It is described
Nickel salt be Ni (CH3COO)2Or Ni (NO3)2Or their hydrate；The cobalt salt is Co (CH3COO)2Or Co (NO3)2Or
CoSO4 or their hydrate；The manganese salt is Mn (CH3COO)2Or Mn (NO3)2Or their hydrate.
Preferably, which is characterized in that the solvent is water, ethyl alcohol, ethylene glycol, propyl alcohol, propylene glycol, the third three
Alcohol, n-butanol, NMP single or a variety of mixtures.
Preferably, the reducing agent is carbamide or citric acid or amion acetic acid or carbohydrazide single or a variety of
Mixture, reducing agent：Total metal salt molar ratio is 0.5-2.5 times.
Preferably, the additive is polyethylene glycol or tween or PTEE or PVDF single or a variety of mixing
Body.Additive amount is the 0.1%-10% of liquor capacity.
Preferably, the ammonium hydroxide tune PH range is 4-10.
Preferably, the evaporating temperature is 60-140 degree, time 0.2-12h.
Preferably, the ignition temperature is 300-700 degree, and burning time 0.01-2h, soaking time is
0.05-8h。
Preferably, the high-temperature calcination time is 5-24h, and temperature is 700-1100 degree.
The method that a kind of controllable low-temperature combustion method of the invention prepares lithium-rich anode material, using water, ethyl alcohol, ethylene glycol
Deng for solvent, can abundant dissolved metal salt, using is the reducing agents such as carbamide or citric acid or amion acetic acid or carbohydrazide
Complex system can be formed together with solvent, mixes lithium, nickel, cobalt, manganese ion uniformly in the solution, improving crystal to a certain degree
Purity.
The method that a kind of controllable low-temperature combustion method of the invention prepares lithium-rich anode material, using certain polyethylene glycol
Or tween or PTEE or PVDF additive and plus ammonium hydroxide adjust PH, the temperature of reaction can be regulated and controled to a certain extent, reduced anti-
The severe degree answered makes to react uniform generation, then inhibits segregation and the agglomeration of crystal.
The method that a kind of controllable low-temperature combustion method of the invention prepares lithium-rich anode material, the low-temperature combustion method of use,
The rate of crystallization can be improved, system spontaneous combustion after igniting, energy saving saves the time, saves equipment input cost, fast quickly
It can obtain material precursor.The gas and vapor of generation can provide very high specific surface and aperture to material, make the electricity of material
Chemical property is promoted.
Detailed description of the invention
Fig. 1 is the XRD diagram of the lithium-rich anode material of controllable low-temperature combustion method preparation in case study on implementation 1.
Fig. 2 is the SEM figure of the lithium-rich anode material of controllable low-temperature combustion method preparation in case study on implementation 1.
Fig. 3 is the TEM figure of the lithium-rich anode material of controllable low-temperature combustion method preparation in case study on implementation 1.
Fig. 4 is the first circle charging and discharging curve figure of the lithium-rich anode material of controllable low-temperature combustion method preparation in case study on implementation 1.
Fig. 5 is that the 1C of the lithium-rich anode material of controllable low-temperature combustion method preparation in case study on implementation 1 recycles figure.
Specific embodiment
The present invention provides a kind of method that controllable low-temperature combustion method prepares lithium-rich anode material, and tool is exemplified below
Invention is further explained for body embodiment.
Embodiment 1
This example uses carbamide for reducing agent, in deionized water and alcohol mixed solvent, adds appropriate polyethylene glycol preparation
Obtain lithium-rich anode material 0.4Li2MnO3·0.4Li[Ni1/3Co1/3Mn1/3]O2.The ethanol solution that dose volume score is 50%
100ml stoichiometrically claims the LiNO for preparing 0.5mol/L3、Ni(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO3)2
（50% aqueous solution）The carbamide of 0.14mol is added in metal salt mixed solution A, and 5ml polyethylene glycol stirs evenly, and ammonium hydroxide is added dropwise
PH to 8 is adjusted, solution B is obtained.Solution B is placed in 100 degree of oil baths be stirred to react until solution be concentrated into 50ml, pour into crucible
In, its burning is made at 600 degree, heat preservation 1h takes out to obtain powder C, C is collected and is ground, is placed under Muffle furnace and forges for 900 degree of high temperature
12h is burnt, ball milling is sieved to get lithium-rich anode material 0.4Li is arrived after cooling2MnO3·0.4Li[Ni1/3Co1/3Mn1/3]O2, material
XRD, SEM, TEM test result difference it is as shown in Figure 1, 2, 3, it is known that the material of synthesis has high-crystallinity, and fine and close ball-type is special
Point.
By the drying 3 hours of 120 DEG C of above-mentioned material vacuum, then with acetylene black, Kynoar（PVDF）According to mass ratio
80:10:10 ratio prepares slurry, and coating prepares positive plate on aluminium foil, be then assembled into metal lithium sheet button cell into
Row performance test, wherein electrolyte is 1mol/L LiPF6EC, DMC and EMC mixed liquor（Volume ratio is 1:1:1）, voltage model
It encloses for 2.2V ~ 4.8V, nominal specific capacity is 200mAh/g.The first circle charge-discharge test curve of material is as shown in figure 4, circle electric discharge ratio
Capacity is 332.1mAh/g, and efficiency 76.82%, test results are shown in figure 5 for 1C cycle performance, and 1C specific discharge capacity is 167
MAh/g, 100 circle capacity retention ratios are 95.81%.It is found that this material has very high specific discharge capacity and good cyclicity
Energy.
Embodiment 2
This example uses carbamide and citric acid for reducing agent, in deionized water, adds appropriate polysorbas20 and rich lithium is prepared
Positive electrode 0.5/3Li2MnO3·0.5Li[Ni1/3Co1/3Mn1/3]O2.The propanol solution 100ml that dose volume score is 50%,
Stoichiometrically claim the LiNO for preparing 0.5mol/L3 、Ni(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO3)2（50% water
Solution）The carbamide of 0.1mol and the citric acid of 0.5mol is added in metal salt mixed solution A, and 2ml polysorbas20 stirs evenly, drop
Add ammonium hydroxide to adjust PH to 8, obtains solution B.Solution B is placed in 90 degree of oil baths and is stirred to react until solution is concentrated into 65ml,
Enter in crucible, its burning is made at 550 degree, heat preservation 0.5h takes out to obtain powder C, C is collected and is ground, high temperature under Muffle furnace is placed in
900 degree of calcining 12h, ball milling is sieved to get lithium-rich anode material 0.5/3Li is arrived after cooling2MnO3·0.5Li[Ni1/3Co1/ 3Mn1/3]O2。
By the drying 3 hours of 120 DEG C of above-mentioned material vacuum, then with acetylene black, Kynoar（PVDF）According to mass ratio
80:10:10 ratio prepares slurry, and coating prepares positive plate on aluminium foil, be then assembled into metal lithium sheet button cell into
Row performance test, wherein electrolyte is 1mol/L LiPF6EC, DMC and EMC mixed liquor（Volume ratio is 1:1:1）, voltage model
It encloses for 2.2V ~ 4.8V, nominal specific capacity is 200mAh/g.The first circle specific discharge capacity of material is 293.7 mAh/g, and efficiency is
83.4%, 1C specific discharge capacity are 163.8 mAh/g, and 100 circle capacity retention ratios are 92.6%.
Embodiment 3
This example uses carbohydrazide for reducing agent, in deionized water and ethylene glycol in the mixed solvent, adds appropriate PVDF and is prepared into
To lithium-rich anode material 0.2/3Li2MnO3·0.9Li[Ni0.4Co0.2Mn0.2]O2.The ethylene glycol that dose volume score is 20% is molten
Liquid 100ml stoichiometrically claims the CH for preparing 0.5mol/L3COOLi·2H2O 、Ni(CH3COO)2·4H2O、Co
(CH3COO)2·4H2O and Mn (CH3COO)2·4H2The carbohydrazide of 0.08mol, the PVDF of 2g is added in O metal salt mixed solution A
Powder stirs evenly, and ammonium hydroxide is added dropwise and adjusts PH to 7, obtains solution B.Solution B is placed in 100 degree of oil baths be stirred to react until
Solution is concentrated into 60ml, pours into crucible, its burning is made at 500 degree, and heat preservation 2h takes out to obtain powder C, C is collected and is ground,
900 degree of calcining 12h of high temperature under Muffle furnace are placed in, ball milling is sieved to get lithium-rich anode material 0.2/3Li is arrived after cooling2MnO3·
0.9Li[Ni0.4Co0.2Mn0.2]O2。
By the drying 3 hours of 120 DEG C of above-mentioned material vacuum, then with acetylene black, Kynoar（PVDF）According to mass ratio
80:10:10 ratio prepares slurry, and coating prepares positive plate on aluminium foil, be then assembled into metal lithium sheet button cell into
Row performance test, wherein electrolyte is 1mol/L LiPF6EC, DMC and EMC mixed liquor（Volume ratio is 1:1:1）, voltage model
It encloses for 2.2V ~ 4.8V, nominal specific capacity is 200mAh/g.The first circle specific discharge capacity of material is 311.4 mAh/g, and efficiency is
85.2%, 1C specific discharge capacity are 173.2 mAh/g, and 100 circle capacity retention ratios are 93.3%.
Embodiment 4
This example uses amion acetic acid for reducing agent, in deionized water and NMP in the mixed solvent, adds appropriate PTEE and is prepared
Lithium-rich anode material 0.2Li2MnO3·0.7Li[Ni0.5Co0.2Mn0.3]O2.The nmp solution 100ml that dose volume score is 10%,
Stoichiometrically claim the LiNO for preparing 0.5mol/L3 、Ni(NO3)2·6H2O、Co(NO3)2·6H2O and Mn (NO3)2（50% water
Solution）The amion acetic acid of 0.2mol is added in metal salt mixed solution A, and the PTEE powder of 1g stirs evenly, and ammonium hydroxide is added dropwise and adjusts
PH to 8, obtains solution B.Solution B is placed in the reaction of 70 degree of stirred in water bath until solution is concentrated into 80ml, is poured into crucible,
Making its burning at 600 degree, heat preservation 1h takes out to obtain powder C, C is collected and is ground, 900 degree of calcining 12h of high temperature under Muffle furnace are placed in,
Ball milling is sieved to get lithium-rich anode material 0.2Li is arrived after cooling2MnO3·0.7Li[Ni0.5Co0.2Mn0.3]O2。
By the drying 3 hours of 120 DEG C of above-mentioned material vacuum, then with acetylene black, Kynoar（PVDF）According to mass ratio
80:10:10 ratio prepares slurry, and coating prepares positive plate on aluminium foil, be then assembled into metal lithium sheet button cell into
Row performance test, wherein electrolyte is 1mol/L LiPF6EC, DMC and EMC mixed liquor（Volume ratio is 1:1:1）, voltage model
It encloses for 2.2V ~ 4.8V, nominal specific capacity is 200mAh/g.The first circle specific discharge capacity of material is 307.4 mAh/g, and efficiency is
89.6%, 1C specific discharge capacity are 165.6 mAh/g, and 100 circle capacity retention ratios are 95.3%.
Embodiment 5
This example uses citric acid and carbohydrazide for reducing agent, in n-butanol solvent, adds appropriate polyethylene glycol and is prepared
Lithium-rich anode material is 0.8/3Li2MnO3·0.6Li[Ni0.6Co0.2Mn0.2]O2.The n-butanol that dose volume score is 10% is molten
Liquid 100ml stoichiometrically claims the LiNO for preparing 0.5mol/L3 、Ni(NO3)2·6H2O、Co(NO3)2·6H2O and Mn
(NO3)2（50% aqueous solution）The carbamide of 0.05mol, the citric acid of 0.12mol, the poly- second two of 5ml is added in metal salt mixed solution A
Alcohol stirs evenly, and ammonium hydroxide is added dropwise and adjusts PH to 6, obtains solution B.Solution B is placed in 100 degree of oil baths and is stirred to react until molten
Liquid is concentrated into 50ml, pours into crucible, its burning is made at 550 degree, and heat preservation 2h takes out to obtain powder C, C is collected and is ground, is set
900 degree of calcining 12h of high temperature under Muffle furnace, ball milling is sieved to get lithium-rich anode material 0.8/3Li is arrived after cooling2MnO3·
0.6Li[Ni0.6Co0.2Mn0.2]O2。
By the drying 3 hours of 120 DEG C of above-mentioned material vacuum, then with acetylene black, Kynoar（PVDF）According to mass ratio
80:10:10 ratio prepares slurry, and coating prepares positive plate on aluminium foil, be then assembled into metal lithium sheet button cell into
Row performance test, wherein electrolyte is 1mol/L LiPF6EC, DMC and EMC mixed liquor（Volume ratio is 1:1:1）, voltage model
It encloses for 2.2V ~ 4.8V, nominal specific capacity is 200mAh/g.The first circle specific discharge capacity of material is 322.9 mAh/g, and efficiency is
88.7%, 1C specific discharge capacity are 176.3 mAh/g, and 100 circle capacity retention ratios are 94.5%.
Case recited above is only that preferred embodiment embodiment of the invention is described, and is not defined of the invention
Conception and scope of protection can also make various deformation and improvement without departing from the principle of the present invention, these also fall into
Within the scope of protection scope of the present invention.
Claims (9)
1. a kind of controllable low-temperature combustion method prepares lithium-rich anode material 2x/3Li2MnO3·(1-x)LiMO2, (0 <x< 1, M=
Ni,Co,Mn）Method, which is characterized in that carry out according to the following steps：Nickel cobalt manganese metal salt is dissolved according to stoichiometric ratio
In solvent, a certain amount of reducing agent and additive is added, stirs evenly, appropriate ammonium hydroxide is added dropwise and adjusts PH, obtains solution A, it will be molten
Liquid A heating evaporation after a certain period of time, is placed in heating furnace, its burning is made when 300-700 is spent, heat preservation a period of time, is taken out
To powder B, B is collected and is ground, is placed in high temperature 700-1100 degree under Muffle furnace and calcine 5-24h, ball milling sieving is after cooling to get arriving
Lithium-rich anode material.
2. the preparation method of material according to claim 1, which is characterized in that the lithium salts is CH3COOLi or LiNO3
Or their hydrate；The nickel salt is Ni (CH3COO)2Or Ni (NO3)2Or their hydrate；The cobalt salt is Co
(CH3COO)2Or Co (NO3)2Or CoSO4 or their hydrate；The manganese salt is Mn (CH3COO)2Or Mn (NO3)2Or they
Hydrate.
3. the preparation method of material according to claim 1, which is characterized in that the solvent is water, ethyl alcohol, second two
Alcohol, propyl alcohol, propylene glycol, glycerine, n-butanol, NMP single or a variety of mixtures.
4. the preparation method of material according to claim 1, which is characterized in that the reducing agent is carbamide or lemon
Acid or amion acetic acid or carbohydrazide single or a variety of mixtures, reducing agent：Total metal salt molar ratio is 0.5-2.5 times.
5. the preparation method of material according to claim 1, which is characterized in that the additive is polyethylene glycol or spits
Temperature or PTEE single or a variety of mixtures, additive amount are the 0.1%-10% of liquor capacity.
6. the preparation method of material according to claim 1, which is characterized in that the ammonium hydroxide tune PH range is 4-10.
7. the preparation method of material according to claim 1, which is characterized in that the evaporating temperature is 60-140 degree,
Time is 0.2-12h.
8. the preparation method of material according to claim 1, which is characterized in that the ignition temperature is 300-700 degree,
Burning time is 0.01-2h, soaking time 0.05-8h.
9. the preparation method of material according to claim 1, which is characterized in that the high-temperature calcination time is 5-24h,
Temperature is 700-1100 degree.
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| WO2023184995A1 (en) * | 2022-03-29 | 2023-10-05 | 广东邦普循环科技有限公司 | Ternary positive electrode material having core-shell structure and preparation method therefor and use thereof |
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| CN104112849A (en) * | 2014-07-25 | 2014-10-22 | 江南大学 | Light metal element-doped ternary lithium ion battery positive electrode material and synthesis method thereof |
| CN104241631A (en) * | 2014-09-04 | 2014-12-24 | 中国科学院化学研究所 | High-capacity positive electrode material for lithium ion battery |
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| CN111087029A (en) * | 2019-12-20 | 2020-05-01 | 中国电子科技集团公司第十八研究所 | Method for preparing high-specific-capacity NCM622 material by one-step sol-gel method |
| WO2023184995A1 (en) * | 2022-03-29 | 2023-10-05 | 广东邦普循环科技有限公司 | Ternary positive electrode material having core-shell structure and preparation method therefor and use thereof |
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Application publication date: 20181116 |