CN104009221A - Method for preparing positive electrode material rich in lithium via sol-gel self-propagating combustion method - Google Patents
Method for preparing positive electrode material rich in lithium via sol-gel self-propagating combustion method Download PDFInfo
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- CN104009221A CN104009221A CN201410247790.3A CN201410247790A CN104009221A CN 104009221 A CN104009221 A CN 104009221A CN 201410247790 A CN201410247790 A CN 201410247790A CN 104009221 A CN104009221 A CN 104009221A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/48—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
- H01—ELECTRIC ELEMENTS
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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
- H01M4/48—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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The invention relates to a method for preparing a positive electrode material rich in lithium via a sol-gel self-propagating combustion method, and belongs to the manufacturing method of a raw material of a lithium battery. The method comprises the following steps: dissolving the salts of lithium, nickel and manganese in an alcohol reagent so as to prepare a solution A; then standing the solution A in a thermostat water bath at a certain temperature and evaporating in a stirring manner so as to obtain a colloidal chelate precursor B; transferring the colloidal chelate precursor B into a crucible, standing in a muffle furnace and carrying out self-propagating combustion at the certain temperature so as to generate an ash material C; grinding the ash material C, then standing in the muffle furnace and calcining for multiple hours at a high temperature and under an oxygen atmosphere; and grinding and screening so as to obtain the anode material rich in lithium. According to the method, the self-propagating combustion reaction can be carried out without a complete gel drying process by adopting the sol-gel method; the synthesized primary particles are in a submicron grade, i.e., the synthesized primary particles are small in particle diameter and short in lithium ion diffusion path, thereby being favorable for deintercalation of lithium ions. Thus, the defects of the material rich in lithium are overcome.
Description
Technical field
The invention belongs to the field of anode material for lithium-ion batteries, be specifically related to that a kind of capacity is high, stoichiometric proportion good, purity is high, the anode material for lithium-ion batteries Li(Li of high rate performance
0.08ni
0.38mn
0.54) O
2preparation method.
Background technology
Along with people are to the growing of energy demand with to the deepening constantly of society and economy sustainable development understanding of importance, the lithium ion battery that environmental protection and efficient high energy is feature of take is more and more subject to people's attention.The application such as big-and-middle-sized electric tool, energy-accumulating power station, electric motor car, intelligent grid have all proposed requirements at the higher level to aspects such as the fail safe of lithium ion battery, energy density, power density, cycle life, price, environmental friendliness.The specific capacity of lithium ion battery negative material is conventionally more than 300mAh/g at present, and the specific capacity of positive electrode is hovered all the time in 150mAh/g left and right.During due to deep charge electrode material to the strong oxidation of organic bath and excessively de-lithium the destruction to material self structure, LiCoO
2reality can utilize capacity only have theoretical capacity half left and right.Although and nickel-cobalt-manganese ternary material has reduced material cost and toxicity, obviously improved the fail safe of material, the actual specific capacity of these layer structure materials (being generally less than 180mAh/g) does not have large breakthrough.Spinel structure positive electrode LiMn2O4 and polyanion positive electrode are (typical in the LiFePO of olivine structural
4) theoretical specific capacity also only have respectively 148mAh/g and 170mAh/g, far can not meet the performance requirement of high specific energy lithium ion battery to positive electrode.Therefore, positive electrode becomes the bottleneck that performance of lithium ion battery further improves.
Rich lithium Layered Structural Positive Electrode Materials Li
1+xm
1-xo
2(M is Ti, Cr, Fe, Co, Ni, Mn etc.) theoretical specific capacity surpass 300mAh/g, reality can utilize capacity to be greater than 200mAh/g, becomes important candidate's positive electrode that development energy density is greater than 300Wh/kg lithium ion battery, gets more and more people's extensive concerning in recent years.
The method of synthetic rich lithium material mainly contains high temperature solid-state method, coprecipitation, sol-gal process, hydro thermal method and spray drying process etc.Coprecipitation is for the synthetic the most frequently used method of composite positive pole presoma, this method can realize the mixing of atom level, but, precipitation when variety classes cation is different in reality, there is sequencing in precipitation, precipitation by metallic ion is incomplete, and stoichiometric proportion is not easy accurate control, precipitate incomplete heavy metal and also cause environmental pollution, and water consumption is large.Sol-gal process not only can be realized the mixing of atom level, and synthetic materials chemistry metering ratio is accurate, distributions of metallic elements is even, purity is high, and self-propagating combustion reaction saves time fast, and particle size distribution is even, and technical process is simple.
Summary of the invention
The object of the present invention is to provide a kind of sol-tgel self-propagating combustion method to prepare the method for lithium-rich anode material, this method technological process is simple, stoichiometric proportion good, purity is high, good rate capability, can improve existing rich lithium material owing to there being Li
2mnO
3component causes material poorly conductive, the deficiency that high rate performance is poor.
Technical scheme of the present invention is as follows:
Sol-tgel self-propagating combustion method is prepared a method for lithium-rich anode material, and described lithium-rich anode material is Li(Li
0.08ni
0.38mn
0.54) O
2, it is characterized in that the method carries out according to the following steps:
(1) salt of lithium, nickel, manganese is dissolved in and in alcohol reagent, is mixed with solution A,
(2) thermostat water bath that then solution A is placed in to uniform temperature is evaporated to gluey chelate precursor B under the condition stirring,
(3) precursor B is transferred in crucible, is placed in Muffle furnace and under uniform temperature, makes its self-propagating combustion generate ashes substance C,
(4) substance C is calcined to a few hours through grinding to be placed in Muffle furnace under high temperature in oxygen atmosphere, grinding obtains lithium-rich anode material Li(Li after sieving
0.08ni
0.38mn
0.54) O
2.
As preferably, described lithium salts is at least one lithium salts in lithium nitrate, lithium acetate; Described nickel salt is at least one nickel salt in nickel nitrate, nickel acetate; Described manganese salt is that at least one in manganese nitrate, manganese acetate is acetate.As preferably, described bath temperature is 50-100 ℃, and agitating mode is mechanical agitation or magnetic agitation.
As preferably, described ignition temperature is 300-500 ℃, and be 0.1-2h burning time.
As preferably, described calcining heat is 750-950 ℃, and calcination time is 6-24h.
The sol-gal process that the present invention adopts can carry out self-propagating combustion reaction without gel bone dry process, easy and simple to handle and save time.Synthetic primary particle is sub-micron grade particle, and particle diameter is little, and lithium ion the evolving path is short, is beneficial to the de-embedding of lithium ion, has improved the deficiency of rich lithium material.
Accompanying drawing explanation
Fig. 1 is the SEM figure of lithium-rich anode material in case study on implementation 1.
Fig. 2 is the first charge-discharge curve chart of lithium-rich anode material in embodiment 1.
Fig. 3 is the cycle performance figure of lithium-rich anode material in embodiment 1.
Embodiment
Below by case study on implementation, further the present invention will be described, but this is not limitation of the present invention, those skilled in the art can, according to basic ideas of the present invention, make corresponding improvement, only otherwise depart from thinking of the present invention, all in scope of the present invention.
Sol-tgel self-propagating combustion method is prepared a method for lithium-rich anode material, and described lithium-rich anode material is Li(Li
0.08ni
0.38mn
0.54) O
2, its feature mainly comprises following steps:
1) salt of lithium, nickel, manganese is dissolved in and in alcohol reagent, is mixed with solution A,
2) thermostat water bath that then solution A is placed in to uniform temperature is evaporated to gluey chelate precursor B under the condition stirring,
3) precursor B is transferred in crucible, is placed in Muffle furnace and under uniform temperature, makes its self-propagating combustion generate ashes substance C,
4) substance C is calcined to a few hours through grinding to be placed in Muffle furnace under high temperature in oxygen atmosphere, grinding obtains lithium-rich anode material Li(Li after sieving
0.08ni
0.38mn
0.54) O
2.
The method of preparing lithium-rich anode material according to described method sol-tgel self-propagating combustion method, is characterized in that, described lithium salts is at least one lithium salts in lithium nitrate, lithium acetate; Described nickel salt is at least one nickel salt in nickel nitrate, nickel acetate; Described manganese salt is that at least one in manganese nitrate, manganese acetate is acetate.
The method of preparing lithium-rich anode material according to described sol-tgel self-propagating combustion method, is characterized in that step 2) described in bath temperature be 50-100 ℃, agitating mode is mechanical agitation or magnetic agitation.
The method of preparing lithium-rich anode material according to described sol-tgel self-propagating combustion method, is characterized in that, the ignition temperature described in step 3) is 300-500 ℃, and be 0.1-2h burning time.
The method of preparing lithium-rich anode material according to described sol-tgel self-propagating combustion method, is characterized in that, the calcining heat described in step 4) is 750-950 ℃, and calcination time is 6-24h.
The present invention adopts first sol-gal process to synthesize the gluey chelate presoma that purity is high, stoichiometric proportion is good, then the method for self-propagating combustion makes it preliminary generate rich lithium material, then obtains evengranular lithium-rich anode material Li(Li through high-temperature process
0.08ni
0.38mn
0.54) O
2.
Case study on implementation 1
Prepare lithium-rich anode material Li(Li
0.08ni
0.38mn
0.54) O
2, according to the stoichiometric proportion of Li, Ni, each element of Mn in target product, accurately take corresponding lithium nitrate, nickel nitrate and manganese acetate, according to slaine gross mass: ethanol quality=1:8, obtain solution, carries out stirring and dissolving and be placed on 80 under normal temperature
oin C thermostat water bath, carry out mechanical agitation evaporation, after becoming gluey transparency material, it is transferred in crucible, crucible is placed in Muffle furnace to calcination 1h at 350 ℃, make it that self-propagating combustion reaction occur, the ashes after burning are placed in Muffle furnace to 850 ℃ of calcining 16h under oxygen atmosphere through grinding.Grind and cross 400 mesh sieves and obtain Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode.
By synthetic Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode, acetylene black, binding agent polyvinylidene fluoride (PVDF) in mass ratio 85:10:5 mix as anodal, take lithium metal as negative pole, 1mol/L LiPF
6-EC/DMC is electrolyte assembling button cell, in 25
oin C environment, in the voltage range of 2.0 – 4.5V, under 0.1C multiplying power, (1C=200mA/g) carries out electro-chemical test, and battery discharge specific capacity is 265mAh/g; After circulating 50 weeks, capability retention is 96%.
Case study on implementation 2
Prepare lithium-rich anode material Li(Li
0.08ni
0.38mn
0.54) O
2, according to the stoichiometric proportion of Li, Ni, each element of Mn in target product, accurately take corresponding lithium acetate, nickel acetate and manganese acetate, according to slaine gross mass: ethanol quality=1:9, obtain solution, carries out under normal temperature adding magneton after stirring and dissolving, is placed in 90
oin C thermostat water bath, carry out magnetic agitation evaporation, after becoming gluey transparency material, it is transferred in crucible, crucible is placed in Muffle furnace to calcination 0.5h at 400 ℃, make it that self-propagating combustion reaction occur, the ashes after burning are placed in Muffle furnace to 900 ℃ of calcining 12h under oxygen atmosphere through grinding.Grind and cross 400 mesh sieves and obtain Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode.
By synthetic Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode, acetylene black, binding agent polyvinylidene fluoride (PVDF) in mass ratio 85:10:5 mix as anodal, take lithium metal as negative pole, 1mol/L LiPF
6-EC/DMC is electrolyte assembling button cell, in 25
oin C environment, in the voltage range of 2.0 – 4.5V, under 0.1C multiplying power, (1C=200mA/g) carries out electro-chemical test, and battery discharge specific capacity is 263mAh/g.
Case study on implementation 3
Prepare lithium-rich anode material Li(Li
0.08ni
0.38mn
0.54) O
2, according to the stoichiometric proportion of Li, Ni, each element of Mn in target product, accurately take corresponding lithium nitrate, nickel acetate and manganese nitrate, according to slaine gross mass: ethanol quality=1:10, obtain solution, carries out stirring and dissolving and be placed on 75 under normal temperature
oin C thermostat water bath, stir evaporation, after becoming gluey transparency material, it is transferred in crucible, crucible is placed in Muffle furnace to calcination 2h at 350 ℃, makes it that self-propagating combustion reaction occur, the ashes after burning are placed in Muffle furnace to 800 ℃ of calcining 24h under oxygen atmosphere through grinding.Grind and cross 400 mesh sieves and obtain Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode.
By synthetic Li(Li
0.08ni
0.38mn
0.54) O
2positive electrode, acetylene black, binding agent polyvinylidene fluoride (PVDF) in mass ratio 85:10:5 mix as anodal, take lithium metal as negative pole, 1mol/L LiPF
6-EC/DMC is electrolyte assembling button cell, in 25
oin C environment, in the voltage range of 2.0 – 4.5V, under 0.1C multiplying power, (1C=200mA/g) carries out electro-chemical test, and battery discharge specific capacity is 260mAh/g.
Claims (5)
1. sol-tgel self-propagating combustion method is prepared a method for lithium-rich anode material, and described lithium-rich anode material is Li(Li
0.08ni
0.38mn
0.54) O
2, its feature mainly comprises following steps:
The salt of lithium, nickel, manganese is dissolved in and in alcohol reagent, is mixed with solution A,
Then the thermostat water bath that solution A is placed in to uniform temperature is evaporated to gluey chelate precursor B under the condition stirring,
Precursor B is transferred in crucible, is placed in Muffle furnace and under uniform temperature, makes its self-propagating combustion generate ashes substance C,
Substance C is calcined to a few hours through grinding to be placed in Muffle furnace under high temperature in oxygen atmosphere, and grinding obtains lithium-rich anode material Li(Li after sieving
0.08ni
0.38mn
0.54) O
2.
2. method sol-tgel self-propagating combustion method according to claim 1 is prepared the method for lithium-rich anode material, it is characterized in that, described lithium salts is at least one lithium salts in lithium nitrate, lithium acetate; Described nickel salt is at least one nickel salt in nickel nitrate, nickel acetate; Described manganese salt is that at least one in manganese nitrate, manganese acetate is acetate.
3. sol-tgel self-propagating combustion method according to claim 1 is prepared the method for lithium-rich anode material, it is characterized in that, described in step (2), bath temperature is 50-100 ℃, and agitating mode is mechanical agitation or magnetic agitation.
4. sol-tgel self-propagating combustion method according to claim 1 is prepared the method for lithium-rich anode material, it is characterized in that, the ignition temperature described in step (3) is 300-500 ℃, and be 0.1-2h burning time.
5. sol-tgel self-propagating combustion method according to claim 1 is prepared the method for lithium-rich anode material, it is characterized in that, the calcining heat described in step (4) is 750-950 ℃, and calcination time is 6-24h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107403903A (en) * | 2017-08-23 | 2017-11-28 | 中国科学院过程工程研究所 | A kind of method that sol-tgel self-propagating combustion method prepares the nickelic positive electrode of ternary |
| CN107863502A (en) * | 2017-10-11 | 2018-03-30 | 苏州宇量电池有限公司 | A kind of fast synthesis method of the lithium-rich manganese-based anode material of uniform nanoparticles |
| CN107910545A (en) * | 2017-11-06 | 2018-04-13 | 西安电子科技大学 | A kind of preparation method of height ratio capacity richness lithium manganese anode material |
| CN112467101A (en) * | 2020-11-04 | 2021-03-09 | 双登集团股份有限公司 | Ternary lithium ion storage battery positive electrode material and preparation method thereof |
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| CN101844817A (en) * | 2008-08-13 | 2010-09-29 | 成都中科来方能源科技有限公司 | Preparation method of spinelle type lithium nickel manganese oxides of positive electrode materials of lithium ion secondary batteries |
| CN103165890A (en) * | 2013-03-26 | 2013-06-19 | 四川大学 | Method for preparing lithium vanadium phosphate through sol-gel self-propagating combustion method |
-
2014
- 2014-06-06 CN CN201410247790.3A patent/CN104009221B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844817A (en) * | 2008-08-13 | 2010-09-29 | 成都中科来方能源科技有限公司 | Preparation method of spinelle type lithium nickel manganese oxides of positive electrode materials of lithium ion secondary batteries |
| CN103165890A (en) * | 2013-03-26 | 2013-06-19 | 四川大学 | Method for preparing lithium vanadium phosphate through sol-gel self-propagating combustion method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107403903A (en) * | 2017-08-23 | 2017-11-28 | 中国科学院过程工程研究所 | A kind of method that sol-tgel self-propagating combustion method prepares the nickelic positive electrode of ternary |
| CN107403903B (en) * | 2017-08-23 | 2019-07-19 | 中国科学院过程工程研究所 | A kind of method of the sol-tgel self-propagating combustion method preparation nickelic positive electrode of ternary |
| CN107863502A (en) * | 2017-10-11 | 2018-03-30 | 苏州宇量电池有限公司 | A kind of fast synthesis method of the lithium-rich manganese-based anode material of uniform nanoparticles |
| CN107910545A (en) * | 2017-11-06 | 2018-04-13 | 西安电子科技大学 | A kind of preparation method of height ratio capacity richness lithium manganese anode material |
| CN112467101A (en) * | 2020-11-04 | 2021-03-09 | 双登集团股份有限公司 | Ternary lithium ion storage battery positive electrode material and preparation method thereof |
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