CN107226455A - A kind of niobium is modified the preparation method of lithium cobaltate cathode material - Google Patents
A kind of niobium is modified the preparation method of lithium cobaltate cathode material Download PDFInfo
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- 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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Abstract
The present invention relates to the preparation method that a kind of niobium is modified lithium cobaltate cathode material, methods described is simple to operation, cost is low, it is time-consuming short, methods described is adulterated Nb ions in positive electrode, same order elements are carried out to the Co ionic sites in positive pole material lattice, change lattice parameter, the positive electrode of excellent electrochemical performance is obtained；The porosity characteristic that carbon silicon covering material of the present invention has is conducive to the absorption of electrolyte to store, and provide space to volumetric expansion in silicon materials charge and discharge process, porous silicon sized nanostructures level, also the bulk effect effect of alleviation silicon grain is played, therefore it is high with reversible capacity, good cycle, the excellent advantage of high rate performance.
Description
Technical field
The present invention relates to technical field of lithium batteries, and in particular to a kind of niobium is modified the preparation method of lithium cobaltate cathode material.
Background technology
Secondary cell using lead-acid battery, town hydrogen battery and lithium ion battery as representative is used as a kind of height that can be recycled
New energy memory device is imitated, as a kind of important technological approaches for alleviating the energy and environmental problem.With traditional plumbic acid, nickel
The secondary cells such as cadmium, ni-mh are compared, lithium rechargeable battery have operating voltage height, small volume, light weight, capacity density it is high,
The advantages of memory-less effect, pollution-free, self discharge are small and have extended cycle life.
For cathode active material for lithium secondary battery, the cobalt/cobalt oxide (LiCoO containing lithium is widely used2).In addition, can be also
Using the Mn oxide containing lithium as having the LiMnO of layered crystal structure2, LiMn with spinel crystal structure2O4Deng and
Nickel oxide (LiNbO containing lithium2)。
LiCoO2The main positive electrode of current commercial Li-ion battery, but it exist it is expensive, be unfavorable for
Environmental protection, the low shortcoming of specific capacity.LiNbO2The positive electrode of doping Co elements is provided with LiNbO simultaneously2The higher electric discharge ratio of material
Capacity, stabilizes the layer structure of material again, enhances the cyclical stability of material, but there is also overcharging resisting energy for this material
Power is poor, heat endurance is poor, the defect such as irreversible capacity is higher of electric discharge first.
For this problem, researchers mainly using more than people using doping or the method for the Material cladding high with conductance
Modified anode material, and then improve material property.
Coated with carbon silicon materials are also one of current effective ways for improving anode material for lithium-ion batteries deficiency, mesh
Before, Si-C composite material prepares main use：1）Nano silicon material and the compound simultaneously carbon coating of graphite material；2）Thick silicon high-energy ball milling
With the compound simultaneously carbon coating of graphite；3）In graphite particle surface chemistry one layer of silicon materials of vapour deposition cladding and carbon coating.Using upper
The method 1 stated）Due to using nano silicon material, its cost is higher, and because the agglomeration of nano material is difficult dispersed；
Method 2 uses high-energy ball milling, and long preparation period, cost are high；Method 3）The chemical vapor deposition of use is difficult in graphite particle table
Face uniformly coats silicon materials.In addition, above method be difficult overcome capacity play with efficiency first while taking into account.
The content of the invention
The present invention provides the preparation method that a kind of niobium is modified lithium cobaltate cathode material, and methods described is simple to operation, cost
It is low, take short, methods described adulterate Nb ions in positive electrode, to the Co ionic sites progress isomorphous in positive pole material lattice
Substitution, changes lattice parameter, obtains the positive electrode of excellent electrochemical performance；The porous spy that carbon silicon covering material of the present invention has
Property be conducive to the absorption of electrolyte to store, and provide space to volumetric expansion in silicon materials charge and discharge process, porous silicon size is received
Meter level, also plays the bulk effect effect of alleviation silicon grain, therefore high with reversible capacity, and good cycle, high rate performance is excellent
Advantage.
To achieve these goals, the present invention provides the preparation method that a kind of niobium is modified lithium cobaltate cathode material, this method
Comprise the following steps：
（1）Prepare niobium and be modified cobalt acid lithium
The chemical formula that the niobium is modified cobalt acid lithium is LiCo1-x-yFexNbyO2, wherein：X=0.12-0.15, y=0.02-0.03, according to
The mole of Li, Fe, Nb, Co in above-mentioned chemical formula weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, with appropriate water
It is decentralized medium with ethanol, wet ball grinding batch mixing, the slurry mixed is carried out to the raw material weighed；By the slurry mixed
It is spray-dried, obtains cobalt acid lithium precursor；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained
Granular size for 5-10 micron niobium modification positive pole cobalt acid lithium material；The wherein described nozzle diameter 2-5mm for being used to spray；
（2）Prepare carbon silicon covering material
By micron silicon, paraffin, starch, ethylene glycol in mass ratio（15-35）：（30-10）：（15-25）：Ball after the mixing of 100 ratios
Grind as ball-milled mixtures, ball-milled mixtures are dried with granulation and obtains the equally distributed presoma of micron silicon, paraffin, starch；
Gained presoma is heated, paraffin is melted out, the silicon and the equally distributed presoma material of carbon source of loose structure is obtained
Material, the presoma, which heats, controls heat treatment temperature to be 100-150 DEG C, and processing time is 10-15h；
By gained persursor material, the high temperature sintering under inert atmosphere protection obtains carbon silicon covering material；The high temperature sintering is
It is 900-1000 DEG C to control sintering temperature, and the heating rate for controlling temperature during sintering is 5-15 DEG C/min；Sintering time is 10-
20h；
（3）Compound coating
The niobium is modified positive pole cobalt acid lithium material with the carbon silicon covering material according to mass ratio (75-50)：1 in batch mixer
It is well mixed；
In atmospheric conditions, the material mixed is fired, is warming up to 860 DEG C -950 DEG C, be incubated 10-15h, cooling
After obtain product.
The invention has the advantages that and remarkable result：
（1）The plasma high-temperature fusion technology that the present invention is used, is a kind of new technique developed in recent years, and principle is：
Introducing plasma working gas after vacuum system preset vacuum, in melt chamber and cooling chamber, (generally inert gas, lazy
Property gas be one or more in helium, neon and argon gas, the inert gas in melt chamber and cooling chamber can be it is same,
Can also be mixed gas), the inert gas plasma moment heating added between the two poles of the earth in voltage, melt chamber, temperature
Thousands of degree can be reached, the powder in addition feed appliance can be made to be rapidly reached molten condition, plasma high-speed motion, particle
Between can occur material under molten condition required for sharp impacts, in-time generatin, by be ejected come gas take out of
Melt chamber, is entered in cooling chamber, and required lithium cobaltate cathode material is obtained after cooling.This method can make cobalt acid lithium material exist
Moment is formed, and can form continuous production.
（2）Methods described is adulterated Nb ions in positive electrode, the Co ionic sites in positive pole material lattice is carried out same
Crystalline substance substitution, changes lattice parameter, obtains the positive electrode of excellent electrochemical performance.
（3）The porosity characteristic that carbon silicon covering material of the present invention has is conducive to the absorption of electrolyte to store, and to silicon materials
Volumetric expansion provides space in charge and discharge process, and porous silicon sized nanostructures level also plays the bulk effect effect of alleviation silicon grain, because
This has reversible capacity high, good cycle, the excellent advantage of high rate performance.
Embodiment
Embodiment one
The chemical formula that the present embodiment niobium is modified cobalt acid lithium is LiCo0.86Fe0.12Nb0.02O2, according to the Li in above-mentioned chemical formula, Fe,
Nb, Co mole weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, using appropriate water and ethanol as decentralized medium, symmetrically
The raw material taken carries out wet ball grinding batch mixing, the slurry mixed；The slurry mixed is spray-dried, cobalt acid is obtained
Lithium precursor.
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage
20kV, plasma electric arc current 500A；Frit reaction powder is spurted into cooling device with reducibility gas, after cooling to
Grain is crushed and screened, and is sieved obtained granular size and is modified positive pole cobalt acid lithium material for 5 microns of niobium；It is wherein described to be used for what is sprayed
Nozzle diameter 2mm.
By micron silicon, paraffin, starch, ethylene glycol in mass ratio 15：30：15：Ball milling is ball milling mixing after the mixing of 100 ratios
Ball-milled mixtures are dried granulation and obtain the equally distributed presoma of micron silicon, paraffin, starch by thing；By gained presoma
Heat, melt out paraffin, obtain the silicon and the equally distributed persursor material of carbon source of loose structure, the presoma heating
Processing controls heat treatment temperature to be 100 DEG C, and processing time is 10h.
By gained persursor material, the high temperature sintering under inert atmosphere protection obtains carbon silicon covering material；The high temperature burns
Knot is to control sintering temperature to be 900 DEG C, and the heating rate for controlling temperature during sintering is 5 DEG C/min；Sintering time is 10h.
The niobium is modified positive pole cobalt acid lithium material with the carbon silicon covering material according to mass ratio 75：1 in batch mixer
It is well mixed；In atmospheric conditions, the material mixed is fired, is warming up to 860 DEG C DEG C, 10h is incubated, after cooling
Obtain product.
Embodiment two
The chemical formula that the present embodiment niobium is modified cobalt acid lithium is LiCo0.82Fe0.15Nb0.03O2.According to the Li in above-mentioned chemical formula, Fe,
Nb, Co mole weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, using appropriate water and ethanol as decentralized medium, symmetrically
The raw material taken carries out wet ball grinding batch mixing, the slurry mixed；The slurry mixed is spray-dried, cobalt acid is obtained
Lithium precursor.
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage
40kV, plasma electric arc current 1000A；Frit reaction powder is spurted into cooling device with reducibility gas, it is right after cooling
Particle is crushed and screened, and is sieved obtained granular size and is modified positive pole cobalt acid lithium material for 10 microns of niobium；It is wherein described to be used to spray
The nozzle diameter 5mm penetrated.
By micron silicon, paraffin, starch, ethylene glycol in mass ratio 35：10：25：Ball milling is ball milling mixing after the mixing of 100 ratios
Ball-milled mixtures are dried granulation and obtain the equally distributed presoma of micron silicon, paraffin, starch by thing；By gained presoma
Heat, melt out paraffin, obtain the silicon and the equally distributed persursor material of carbon source of loose structure, the presoma heating
Processing controls heat treatment temperature to be 150 DEG C, and processing time is 15h.
By gained persursor material, the high temperature sintering under inert atmosphere protection obtains carbon silicon covering material；The high temperature burns
Knot is to control sintering temperature to be 1000 DEG C, and the heating rate for controlling temperature during sintering is 15 DEG C/min；Sintering time is 20h.
The niobium is modified positive pole cobalt acid lithium material with the carbon silicon covering material according to mass ratio 50：1 in batch mixer
It is well mixed；In atmospheric conditions, the material mixed is fired, is warming up to 950 DEG C, be incubated 15h, after cooling
To product.
Comparative example
Commercially available lithium cobaltate cathode material.
Above-described embodiment one, two and comparative example products therefrom are used into NMP as solvent, by active material: SP: PVDF
Be configured to slurry that solid content be 70% at=90: 5: 5 is evenly applied on Nb paper tinsels, and positive pole is made.Negative pole is from diameter 14mm's
Metal lithium sheet, electrolyte selects 1mol LiFP6 (EC：DMC：EMC=1:1:1, v/v), with negative electrode casing-shell fragment-pad-lithium
Battery is packaged by the order of piece-electrolyte-barrier film-positive plate-pad-anode cover, and whole process is all filled with argon
Completed in the glove box of gas.Electric performance test is carried out in the case where test temperature is 25 DEG C, after tested the material of the embodiment one and two
Compared with the product of comparative example, first charge-discharge reversible capacity improves 15-20%, and service life brings up to more than 15%.
Claims (1)
1. a kind of niobium is modified the preparation method of lithium cobaltate cathode material, this method comprises the following steps：
（1）Prepare niobium and be modified cobalt acid lithium
The chemical formula that the niobium is modified cobalt acid lithium is LiCo1-x-yFexNbyO2, wherein：X=0.12-0.15, y=0.02-0.03, according to
The mole of Li, Fe, Nb, Co in above-mentioned chemical formula weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, with appropriate water
It is decentralized medium with ethanol, wet ball grinding batch mixing, the slurry mixed is carried out to the raw material weighed；By the slurry mixed
It is spray-dried, obtains cobalt acid lithium precursor；
Plasma-arc is imposed under reducing atmosphere to precursor, melts reaction powder, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into cooling device with reducibility gas, particle crushed and screened after cooling, screening is obtained
Granular size for 5-10 micron niobium modification positive pole cobalt acid lithium material；The wherein described nozzle diameter 2-5mm for being used to spray；
（2）Prepare carbon silicon covering material
By micron silicon, paraffin, starch, ethylene glycol in mass ratio（15-35）：（30-10）：（15-25）：Ball after the mixing of 100 ratios
Grind as ball-milled mixtures, ball-milled mixtures are dried with granulation and obtains the equally distributed presoma of micron silicon, paraffin, starch；
Gained presoma is heated, paraffin is melted out, the silicon and the equally distributed presoma material of carbon source of loose structure is obtained
Material, the presoma, which heats, controls heat treatment temperature to be 100-150 DEG C, and processing time is 10-15h；
By gained persursor material, the high temperature sintering under inert atmosphere protection obtains carbon silicon covering material；The high temperature sintering is
It is 900-1000 DEG C to control sintering temperature, and the heating rate for controlling temperature during sintering is 5-15 DEG C/min；Sintering time is 10-
20h；
（3）Compound coating
The niobium is modified positive pole cobalt acid lithium material with the carbon silicon covering material according to mass ratio (75-50)：1 in batch mixer
It is well mixed；
In atmospheric conditions, the material mixed is fired, is warming up to 860 DEG C -950 DEG C, be incubated 10-15h, cooling
After obtain product.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108172809A (en) * | 2018-01-19 | 2018-06-15 | 王顺良 | A kind of preparation method of lithium ion conductor cladding lithium cobaltate cathode material |
| CN108281631A (en) * | 2018-01-19 | 2018-07-13 | 王群华 | A kind of preparation method of nano-particle cladding lithium cobaltate cathode material |
| CN108346820A (en) * | 2018-01-19 | 2018-07-31 | 王群华 | A kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method |
| CN112970141A (en) * | 2018-10-30 | 2021-06-15 | 新强能电池公司 | Silicon-based energy storage device with electrolyte additive containing phosphazene |
| CN113353988A (en) * | 2021-02-18 | 2021-09-07 | 厦门厦钨新能源材料股份有限公司 | Lithium ion battery positive electrode material and preparation method thereof, lithium ion battery positive electrode and all-solid-state lithium battery |
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| CN106784675A (en) * | 2016-12-16 | 2017-05-31 | 无锡晶石新型能源有限公司 | A kind of dry method method for coating of anode material of lithium battery |
| CN106784707A (en) * | 2016-12-28 | 2017-05-31 | 江西正拓新能源科技股份有限公司 | A kind of preparation method of nano-silicone wire/carbon composite lithium ion battery cathode material |
| CN106972169A (en) * | 2017-05-23 | 2017-07-21 | 苏州思创源博电子科技有限公司 | A kind of tungsten coats the preparation method of lithium cobaltate cathode material |
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2017
- 2017-08-05 CN CN201710663443.2A patent/CN107226455A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106784675A (en) * | 2016-12-16 | 2017-05-31 | 无锡晶石新型能源有限公司 | A kind of dry method method for coating of anode material of lithium battery |
| CN106784707A (en) * | 2016-12-28 | 2017-05-31 | 江西正拓新能源科技股份有限公司 | A kind of preparation method of nano-silicone wire/carbon composite lithium ion battery cathode material |
| CN106972169A (en) * | 2017-05-23 | 2017-07-21 | 苏州思创源博电子科技有限公司 | A kind of tungsten coats the preparation method of lithium cobaltate cathode material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108172809A (en) * | 2018-01-19 | 2018-06-15 | 王顺良 | A kind of preparation method of lithium ion conductor cladding lithium cobaltate cathode material |
| CN108281631A (en) * | 2018-01-19 | 2018-07-13 | 王群华 | A kind of preparation method of nano-particle cladding lithium cobaltate cathode material |
| CN108346820A (en) * | 2018-01-19 | 2018-07-31 | 王群华 | A kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method |
| CN112970141A (en) * | 2018-10-30 | 2021-06-15 | 新强能电池公司 | Silicon-based energy storage device with electrolyte additive containing phosphazene |
| CN113353988A (en) * | 2021-02-18 | 2021-09-07 | 厦门厦钨新能源材料股份有限公司 | Lithium ion battery positive electrode material and preparation method thereof, lithium ion battery positive electrode and all-solid-state lithium battery |
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Application publication date: 20171003 |