CN105355868A - Preparation method of novel iron-lithium and multi-element battery - Google Patents
Preparation method of novel iron-lithium and multi-element battery Download PDFInfo
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- CN105355868A CN105355868A CN201510682983.6A CN201510682983A CN105355868A CN 105355868 A CN105355868 A CN 105355868A CN 201510682983 A CN201510682983 A CN 201510682983A CN 105355868 A CN105355868 A CN 105355868A
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- Y02E60/10—Energy storage using batteries
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- Crystallography & Structural Chemistry (AREA)
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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention provides a preparation method of a novel iron-lithium and multi-element battery. The combination of LiPO4 material and a three-element composite material is adopted as a positive active material, the cost is low, the safety is high, and the application range of the battery particularly in the aspects of electric automobiles and large-scale storage power supplies is greatly expanded; furthermore, the thermal safety and overcharge tolerance of the battery is extremely high because of incomparable physical and chemical properties, the electrical conductivity of the material, the battery life and a discharge platform are greatly improved after testing, and a high-energy density battery with enhanced high current discharge performance and excellent safety performance can be developed by utilizing the three-element composite material and the LiPO4 material.
Description
technical field:
The present invention relates to technical field of lithium ion, particularly a kind of Novel iron lithium and multielement battery preparation method.
background technology:
Along with the development of economy; the aggravation of the exhaustion of petroleum resources and environmental pollution, greenhouse effect must be caused; people must hold economic growth (Economicgrowth), the equilibrium relation between environmental protection (Environmentprotection) and " three E " of energy resource supply (Energysecurity).The demand in epoch calls the exploitation of the high-efficiency cleaning energy.
With the development of new and high technology and the raising of living standards of the people, the progress of lithium ion battery manufacturing technology and the decline of battery cost, lithium ion battery will become the main flow of chemical power source, and its application prospect is boundless.Since 1992 import market by Japanese Sony company, lightweight with it, capacity is high, operating voltage is high, long service life and the feature such as pollution-free obtains fast development, add that its performance is subject to the affirmative of portable type electronic product producer, extensively used various portable type electronic product, as: mobile phone, notebook computer, video camera, digital camera, MP3, player PDA etc.
From the development of whole both positive and negative polarity electrode material, the key factor that restriction lithium ion battery energy density promotes at present is positive electrode.Positive electrode is in occupation of most important status in lithium ion battery product composition, and its performance and price directly have influence on performance and the price of lithium ion battery.Positive electrode also needs the irreversible capacity loss of added burden negative material.Therefore, the research of positive electrode is the key that lithium ion battery material is studied with improving always.
Since nineteen ninety Japan's Sony Corporation invention lithium ion battery, the lithium and cobalt oxides (LiCoO2) of the maximum positive electrode of current use also mainly layer structure, and the lithium manganese oxide of lithium nickel oxide (LiNiO2), spinel-type (LiMn2O4) and layer structure (LiMnO2).
Lithium and cobalt oxides, its average working voltage is 3.7V, has electric discharge steadily, and the advantages such as applicable heavy-current discharge, specific energy are high, good cycle are most widely used anode material for lithium-ion batteries.But in LixCoO2, x=0.5-1, namely still have 0.5 Li+ electronics not participate in electrode reaction in charge and discharge process, although its theoretical specific capacity is 274mAh/g, actual capacity only has about 140mAh/g.And because cobalt resource is deficient, price is high, and when big current is applied, the fail safe of LiCoO2 is also a problem, thus greatly limit the scope of application of cobalt series lithium ion battery, especially in electric automobile and large-scale redundant electrical power.
The theoretical capacity of lithium nickel oxide LiNiO2 is 274mAh/g, and actual capacity reaches about 110mAh/g, and have good high-temperature stability, self-discharge rate is low, pollution-free, has good compatibility with multiple electrolyte.But due to LiNiO2 synthesis difficulty, and rare to stoichiometric LiNiO2, and its electro-chemical activity is poor, and cycle performance is also poor, away from practical application also.
Lithium manganese oxide is compared with cobalt with nickel, there is cheap, resourceful advantage, the LiMn2O4 having lithium manganate having spinel structure and layer structure of current exploitation, they have the incomparable physics and chemistry character of other positive electrode, its thermal safety and overcharging resisting power fabulous, but LiMn2O4 is in use because the dissolving etc. of Mn easily causes lattice to produce defect, make crystal structure disordering, block embedding and the deintercalation passage of lithium ion, thus the capacity attenuation that result in material is very fast.Especially at high temperature the cycle performance of (more than 45 DEG C) falls sharply and poor storage performance, limits its extensive use.
The theoretical capacity of olivine-type LiFePO_4 is 170mAh/g, thermal stability, and fail safe and cycle life well, but also exist two defects: 1. electronic conductance is very little, is unfavorable for reversible reaction, particularly the carrying out of high-multiplying power discharge; 2. Li+ diffusion is wherein slow.In addition, synthesize desirable LiFePO4 and be also not easy, because Fe2+ will be prevented to be oxidized to Fe3+ when synthesizing.
Other anode material for lithium-ion batteries, as LiNi1/3Mn1/3Co1/3O2, the series compound of vanadium, the research work of the materials such as the compound of organic sulfur, all in process both at home and abroad, although achieve many useful achievements, what have industrially applies, and will industrially applying of having needs to improve further and in-depth.
On battery core preparation method, adopt the method for lamination to reduce the possibility of short circuit generation, improve heavy-current discharge performance and the security performance of battery.
summary of the invention:
Object of the present invention is exactly the deficiency for prior art, and provides a kind of Novel iron lithium and multielement battery preparation method, solves the problem that in prior art, electric conductivity is not enough, battery life is short and discharge platform is little.
Technology solution of the present invention is as follows:
A kind of Novel iron lithium and multielement battery preparation method,
The preparation of a, positive active material within 1 ~ 8 hour, is mixed by the element composite material ball milling of the LiPO4 of 5% ~ 85% and 95% ~ 15%, then within 1 ~ 12 hour, prepares positive active material 100 ~ 600 DEG C of annealing;
B, build up battery core by laminating method.
The present invention adopts LiPO4 material and element composite material combination as positive active material, not only with low cost, and high safety, greatly extend the scope of application of the present invention, especially in electric automobile and large-scale redundant electrical power, more because it has incomparable physics and chemistry character, its thermal safety and overcharging resisting power fabulous, find that the electric conductivity of material and battery life and discharge platform are all improved largely after tested afterwards, element composite material of the present invention and LiPO4 composite material can be utilized, develop the high energy density cells that heavy-current discharge performance strengthens and security performance is superior.
A positive active material for Novel iron lithium and multielement battery, adopts element composite material to be mixed as lithium ion battery novel anode active material by ball milling with LiPO4.
As preferably, element composite material is nickel, cobalt, manganese element complex hydroxide.Nickel, cobalt, manganese element complex hydroxide are a kind of positive electrodes of high power capacity, and the advantage of the acid of set cobalt lithium, lithium nickelate and LiMn2O4, reversible specific capacity can reach more than 160mAh/g, is very promising positive electrode.
As preferably, LiPO4 accounts for 40% ~ 60%, and element composite material accounts for 60% ~ 40%.
As preferably, LiPO4 accounts for 40%, and element composite material accounts for 60%.
As preferably, LiPO4 accounts for 60%, and element composite material accounts for 40%.
As preferably, ball milling carries out ball milling for adopting high-energy ball milling method.The general principle of high-energy ball milling method is the change utilizing mechanical energy to come induced chemical reaction or induced material tissue, stuctures and properties, new material is prepared with this, it has and obviously reduces reaction activity, crystal grain thinning, greatly improves powder activity and improve particle distribution uniformity and the combination at interface between reinforcement and matrix, promote solid state ion diffusivity coefficient, bring out cryochemistry reaction, thus improve the performance such as packing, electricity, calorifics of material, be a kind of energy-conservation, efficient material preparation technology.
As preferably, Ball-milling Time is 1 ~ 4 hour, and annealing temperature is 300 ~ 600 DEG C, and annealing time is 6 ~ 12 hours.
Beneficial effect of the present invention is:
The present invention adopts LiPO4 material and element composite material combination as positive active material, not only with low cost, and high safety, greatly extend the scope of application of the present invention, especially in electric automobile and large-scale redundant electrical power, more because it has incomparable physics and chemistry character, its thermal safety and overcharging resisting power fabulous, find that the electric conductivity of material and battery life and discharge platform are all improved largely after tested afterwards, element composite material of the present invention and LiPO4 composite material can be utilized, develop the high energy density cells that heavy-current discharge performance strengthens and security performance is superior.
accompanying drawing illustrates:
Fig. 1 is the typical charging and discharging curve (0.3C) of novel lithium iron battery of the present invention;
Fig. 2 is the typical recycling characteristic curve (0.3C) of novel lithium iron battery of the present invention.
embodiment:
Embodiment 1: containing 40%LiPO4 and 60% element composite material high-energy ball milling 1 hour in positive active material, then in 600 DEG C of annealing preparation in 12 hours, core adopts the novel lithium iron battery of lamination design.
Following preparation method according to positive active material of the present invention: adopt element composite material and LiPO4 to combine as positive active material, form Novel iron lithium type lithium ion battery with Carbon anode.
The present embodiment adopts the element composite material of content 99%, and according to 60% element composite material in positive pole blending process, 40%LiPO4 high-energy ball milling 1h obtains positive active material.Lithium ion cell positive production technology conveniently, in positive active material: conductive agent: the ratio of PVDF=85:10:5 is mixed into required slurry in de-airing mixer, be coated with through slurry, dry, cut out large stretch of, scraping blade, smear sheet, baking, vacuum pulse is degassed, dust suction, compressing tablet, cut out small pieces, to weigh and pole piece inspection is made into required qualified positive plate, then with negative plate, barrier film adopts lamination to become core, again with electrolyte, battery cases etc. are assembled into 785606 types (overall dimensions 78mm*56mm*6mm) lithium ion battery, novel lithium iron battery of the present invention is obtained after changing into activation.
0.2C electric discharge average size (mAh) of the present embodiment is 6743mAh; 0.5C electric discharge average size (mAh) is 6643mAh; 0.5C electric discharge average size/0.2C electric discharge average size is 98.51%; 0.3C, after 200 circulations, capability retention is 99.21%.
As shown in Figure 1, the typical recycling characteristic curve (0.3C) of the present embodiment as shown in Figure 2 for the typical charging and discharging curve (0.3C) of the present embodiment.
Embodiment 2: only containing 99% element composite material in positive active material, core adopts the lithium iron battery of lamination.
The present embodiment adopts the element composite material of 99%, in positive pole blending process lithium ion cell positive production technology conveniently, in positive active material: conductive agent: the ratio of PVDF=85:10:5 is mixed into required slurry in de-airing mixer, be coated with through slurry, dry, cut out large stretch of, scraping blade, smear sheet, baking, vacuum pulse is degassed, dust suction, compressing tablet, cut out small pieces, to weigh and pole piece inspection is made into required qualified positive plate, then with negative plate, barrier film lamination becomes core, again with electrolyte, battery cases etc. are assembled into 785606 types (overall dimensions 78mm*56mm*6mm) lithium ion battery, conventional lithium iron battery is obtained after changing into activation.
0.2C electric discharge average size (mAh) of the present embodiment is 6640mAh; 0.5C electric discharge average size (mAh) is 6233mAh; 0.5C electric discharge average size/0.2C electric discharge average size is 93.87%; 0.3C, after 200 circulations, capability retention is 95.13%.
Embodiment 3: only containing LiPO4 material in positive active material, core adopts the novel lithium iron battery of back-roll formula design.
Following preparation method according to positive active material of the present invention: adopt LiPO4 as positive active material, form conventional iron lithium type lithium ion battery with Carbon anode.
The present embodiment adopts LiPO4 material, lithium ion cell positive production technology conveniently, in positive active material: conductive agent: the ratio of PVDF=85:10:5 is mixed into required slurry in de-airing mixer, be coated with through slurry, dry, cut out large stretch of, scraping blade, smear sheet, baking, vacuum pulse is degassed, dust suction, compressing tablet, cut out small pieces, to weigh and pole piece inspection is made into required qualified positive plate, then with negative plate, barrier film adopts laminating method to build up core, again with electrolyte, battery cases etc. are assembled into 785606 types (overall dimensions 78mm*56mm*6mm) lithium ion battery, conventional lithium iron battery is obtained after changing into activation.
0.2C electric discharge average size (mAh) of the present embodiment is 6468mAh; 0.5C electric discharge average size (mAh) is 6134mAh; 0.5C electric discharge average size/0.2C electric discharge average size is 94.83%; 0.3C, after 200 circulations, capability retention is 96.25%.
Embodiment 4: in positive active material, (element and LiPO4 are 60%:40% high-energy ball milling 4 hours in mass ratio containing 60%LiPO4 and 40% element composite material, then in 300 DEG C of annealing preparation in 6 hours), the novel lithium iron battery that core adopts lamination process to build up.
The present embodiment is according to 60%LiPO4 and 40% element composite material in positive pole blending process, and ball milling 4h obtains positive active material.Lithium ion cell positive production technology conveniently, in positive active material: conductive agent: the ratio of PVDF=85:10:5 is mixed into required slurry in de-airing mixer, be coated with through slurry, dry, cut out large stretch of, scraping blade, smear sheet, baking, vacuum pulse is degassed, dust suction, compressing tablet, cut out small pieces, to weigh and pole piece inspection is made into required qualified positive plate, then with negative plate, barrier film adopts lamination process to build up battery core, again with electrolyte, battery cases etc. are assembled into 785606 types (overall dimensions 78mm*56mm*6mm) lithium ion battery, novel lithium iron battery of the present invention is obtained after changing into activation.
0.2C electric discharge average size (mAh) of the present embodiment is 6550mAh; 0.5C electric discharge average size (mAh) is 6326mAh; 0.5C electric discharge average size/0.2C electric discharge average size is 96.58%; 0.3C, after 200 circulations, capability retention is 97.77%.
As shown in Figure 1, the typical recycling characteristic curve (0.3C) of the present embodiment as shown in Figure 2 for the typical charging and discharging curve (0.3C) of the present embodiment.
The foregoing is only preferred embodiment of the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, should belong to the scope of protection of the invention.
Claims (8)
1. Novel iron lithium and a multielement battery preparation method, is characterized in that:
The preparation of a, positive active material within 1 ~ 8 hour, is mixed by the element composite material ball milling of the LiPO4 of 5% ~ 85% and 95% ~ 15%, then within 1 ~ 12 hour, prepares positive active material 100 ~ 600 DEG C of annealing;
B, build up battery core by laminating method.
2. a positive active material for Novel iron lithium and multielement battery, is characterized in that: adopt element composite material to be mixed as lithium ion battery novel anode active material by ball milling with LiPO4.
3. a kind of Novel iron lithium according to claim 1 and multielement battery preparation method, is characterized in that: described element composite material is nickel, cobalt, manganese element complex hydroxide.
4. a kind of Novel iron lithium according to claim 1 and multielement battery preparation method, is characterized in that: described LiPO4 accounts for 40% ~ 60%, and described element composite material accounts for 60% ~ 40%.
5. a kind of Novel iron lithium according to claim 4 and multielement battery preparation method, is characterized in that: described LiPO4 accounts for 40%, and described element composite material accounts for 60%.
6. a kind of Novel iron lithium according to claim 4 and multielement battery preparation method, is characterized in that: described LiPO4 accounts for 60%, and described element composite material accounts for 40%.
7. a kind of Novel iron lithium according to claim 1 and multielement battery preparation method, is characterized in that: described ball milling carries out ball milling for adopting high-energy ball milling method.
8. a kind of Novel iron lithium according to claim 1 and multielement battery preparation method, it is characterized in that: described Ball-milling Time is 1 ~ 4 hour, described annealing temperature is 300 ~ 600 DEG C, and described annealing time is 6 ~ 12 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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