CN106207169A - A kind of preparation method of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode - Google Patents
A kind of preparation method of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode Download PDFInfo
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- CN106207169A CN106207169A CN201610636120.XA CN201610636120A CN106207169A CN 106207169 A CN106207169 A CN 106207169A CN 201610636120 A CN201610636120 A CN 201610636120A CN 106207169 A CN106207169 A CN 106207169A
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
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- 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
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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
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Abstract
The invention discloses the preparation method of a kind of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode, belong to lithium iron phosphate positive material preparing technical field.The present invention utilizes graphite to be prepared into graphite oxide; reduce to obtain Graphene; and it is dispersed in distilled water to obtain graphene dispersing solution; by the aging carbon gel obtaining doped graphene in itself and resorcinol, formaldehyde addition reactor; and in reactor add LiFePO4 raw material lysate, react under nitrogen protection, obtain reactant; and calcine the most at different temperatures, the method obtaining carbon gel coated LiFePO 4 for lithium ion batteries positive electrode.The invention has the beneficial effects as follows: products obtained therefrom electrical conductivity of the present invention is high, and specific capacity reaches more than 205mAh/g, and cryogenic property is good；Utilizing carbon gel coated LiFePO 4 for lithium ion batteries positive electrode, solve tap density relatively low, the problem that electrode ion diffusion is slow, tap density reaches 1.8～2.3g/mL, and the diffusion coefficient of electrode ion is more than 1.6 × 10‑12cm2/s。
Description
Technical field
The present invention relates to the preparation method of a kind of carbon gel coated LiFePO 4 for lithium ion batteries positive electrode, belong to iron phosphate lithium positive pole material
Material preparing technical field.
Background technology
In recent years, along with resource scarcity, the becoming increasingly conspicuous of problem of environmental pollution, new forms of energy with lithium ion battery are especially
The energy energy storage device represented develops rapidly, constantly replaces NI-G, nickel in fields such as electric automobile, medical apparatus and instruments and communication apparatus
The traditional storage battery such as hydrogen.LiFePO4 because it has plurality of advantages be considered as can replace cobalt acid lithium become lithium of future generation from
The first-selection of sub-cell positive material.But it is slow that LiFePO4 itself has complicated process of preparation, poorly conductive and lithium ion diffusion
Etc. shortcoming.Lithium iron phosphate electrode material is mainly used in various lithium ion battery.The service life of ferric phosphate lithium cell uses with it
Temperature is closely bound up, uses temperature too low or too high all produces very big bad hidden danger at its charge and discharge process and use process.
Especially on north of China electric automobile use, autumn and winter ferric phosphate lithium cell cannot normal power supply or power supply too low,
Its operating ambient temperature need to be regulated and keep its performance.The lithium battery of lithium iron phosphate positive material, it is possible to use big multiplying power charging,
In 1 hour, battery can be full of soon.But poorly conductive, tap density is relatively low.Typically can only achieve 1.3～1.5g/ml, low
Tap density can be described as the disadvantage of LiFePO4.Use coated modified carbon to lithium iron phosphate positive material in electric conductivity
The deficiency of the aspects such as the diffusion of difference, lithium ion is slow is significantly improved.Simple conductive layer cladding means, can only improve material surface
Electron conduction, electron conduction and ion diffusion rates for LiFePO4 crystals the most do not affect, thus right
Limited in the lifting of LiFePO 4 material chemical property.Carbon coating layer limit iron phosphate crystalline lithium growth, shorten lithium from
Son diffusion length in crystal, causes material electric conductivity low, poor performance at low temperatures, and tap density is relatively low, and electrode ion diffusion is slow.
Summary of the invention
The technical problem to be solved: prepare iron phosphate lithium positive pole material for simple conductive layer cladding process
Material, limits the growth of iron phosphate crystalline lithium, shortens lithium ion diffusion length in crystal, cause material electric conductivity low, low
Temperature poor performance, tap density is relatively low, the drawback that electrode ion diffusion is slow, it is provided that one utilizes graphite to prepare oxidation stone
Ink, reduces to obtain Graphene, and is dispersed in distilled water to obtain graphene dispersing solution, and itself and resorcinol, formaldehyde are added reactor
In the carbon gel of aging doped graphene, and in reactor, add Fe (NO3) 3, the lysate of NH4H2PO4, LiNO3,
The lower reaction of nitrogen protection, obtains reactant, and calcines the most at different temperatures, obtain carbon gel coated LiFePO 4 for lithium ion batteries positive electrode
Method.Preparation process of the present invention is simple, and products obtained therefrom electrical conductivity is high, and cryogenic property is good, makes full use of carbon gel cladding and prepares phosphorus
Acid ferrum lithium anode material, efficiently solves material tap density relatively low, the problem that electrode ion diffusion is slow.
For solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) weigh 4～6g graphite powders and put in there-necked flask, flask is put in 0～5 DEG C of ice bath pot, limit stirring in flask
While be slowly added dropwise the mixed acid of 200～300mL, control rate of addition be 5～10mL/min, after completion of dropwise addition, add 20～
30g potassium permanganate, stirring mixing 20～30min after, flask is moved in water-bath, at 55～60 DEG C stirring reaction 12～
18h, reaction raises bath temperature again to 98 DEG C after terminating, insulated and stirred reaction 10～15min；Described mixed acid is that quality is divided
Several 98% sulphuric acid and mass fraction 80% phosphoric acid 10:1 by volume mix；
(2), after above-mentioned reaction terminates, from water-bath, take out flask, and in flask, add the double of 6～8mL mass fractions 30%
Oxygen water, stirring until bubble-free produces, is filtered to obtain filtering residue, is used mass fraction 5% hydrochloric acid and deionized water to its ultrasonic cleaning respectively
5～10min, then centrifugation obtains precipitate, grinds after lyophilization, cross 100～120 mesh sieves, obtains the oxidation stone that structure is fluffy
Powdered ink end, is placed in graphite oxide powder on the quartz boat of tube furnace, is heated to 300～500 DEG C under argon shield, and reduction is anti-
Answer 1～2h, obtain Graphene, by solid-to-liquid ratio 1:10, Graphene is mixed with distilled water, ultrasonic disperse 10～15min, obtain Graphene
Dispersion liquid；
(3) weigh 1.5～2.0g resorcinol, 3～5mL formaldehyde and 35～40mL above-mentioned graphene dispersing solutions respectively, use carbonic acid
Hydrogen sodium regulation pH is 7.0, pours rustless steel autoclave after regulation into, at 60～70 DEG C aging 3～4 days；
(4) after end to be aging, 1:1:1 in molar ratio, weigh 4.82gFe (NO respectively3)3、2.30gNH4H2PO4、
1.38gLiNO3In beaker, and add 15～20mL distilled water, stirring be completely dissolved to solid, lysate is added above-mentioned not
In rust steel autoclave, in reactor, logical nitrogen, under nitrogen protection, is warming up to 80～100 DEG C, is incubated 1～2h, insulation
After with 5～10 DEG C/min ramp to 180～220 DEG C, react 8～10h, reaction terminate after filter, obtain filtering residue, filtering residue divided
Yong not put in vacuum drying oven, at 50～60 DEG C, be dried 5～6h after dehydrated alcohol and water rinses；
(5) by above-mentioned dried solid load porcelain boat, porcelain boat is put in tube furnace, in a nitrogen atmosphere, with 5～8 DEG C/
Min rate program is warming up to 200～300 DEG C of calcinings 2～3h, then is warming up to 400～500 DEG C of calcinings 2～3h, then raises temperature to
600～700 DEG C of calcinings 3～4h, calcining is cooled to room temperature after terminating, obtains carbon gel coated LiFePO 4 for lithium ion batteries positive electrode.
The application process of the present invention: take the 48～55mg carbon gel coated LiFePO 4 for lithium ion batteries positive electrodes prepared, add 6～
7mg politef and 7～9mg acetylene blacks, stirring is allowed to mix homogeneously, is pressed into diameter 4～6mm pole piece, 100～105
It is dried 8～12h at DEG C, is subsequently placed in glove box encapsulation battery, stands 12～15h.This material tap density reach 1.8～
2.3g/mL, electrical conductivity is high, and specific capacity reaches more than 205mAh/g, diffusion coefficient >=1.6 × 10 of electrode ion-12cm2/ s, low temperature
Performance is good, is worthy to be popularized and uses.
The present invention is compared with additive method, and Advantageous Effects is:
(1) preparation process of the present invention is simple, and products obtained therefrom electrical conductivity is high, and specific capacity reaches more than 205mAh/g, and cryogenic property is good；
(2) carbon gel is as the porous carbon materials of a kind of rule, possesses continuous, the high conductivity of structure etc. and is better than other material with carbon elements
Performance, can substitute the simple graphitic carbon covering material of tradition；
(3) make full use of carbon gel cladding and prepare lithium iron phosphate positive material, efficiently solve material tap density relatively low, electrode
The problem that ion diffusion is slow, tap density reaches 1.8～2.3g/mL, diffusion coefficient >=1.6 × 10 of electrode ion-12cm2/s。
Detailed description of the invention
First weigh 4～6g graphite powders and put in there-necked flask, flask is put in 0～5 DEG C of ice bath pot, limit in flask
Stirring limit is slowly added dropwise the mixed acid of 200～300mL, and controlling rate of addition is 5～10mL/min, after completion of dropwise addition, adds
20～30g potassium permanganate, after stirring mixing 20～30min, move into flask in water-bath, stir reaction 12 at 55～60 DEG C
～18h, reaction raises bath temperature again to 98 DEG C after terminating, insulated and stirred reaction 10～15min；Described mixed acid is quality
Mark 98% sulphuric acid and mass fraction 80% phosphoric acid 10:1 by volume mix；After above-mentioned reaction terminates, take from water-bath
Going out flask, and the hydrogen peroxide of addition 6～8mL mass fractions 30% in flask, stirring, until bubble-free produces, filters to obtain filtering residue,
Respectively with mass fraction 5% hydrochloric acid and deionized water to its ultrasonic cleaning 5～10min, then centrifugation obtains precipitate, freezing dry
Grind after dry, cross 100～120 mesh sieves, obtain the graphite oxide powder that structure is fluffy, graphite oxide powder is placed in the stone of tube furnace
On Ying Zhou, under argon shield, it is heated to 300～500 DEG C, reduction reaction 1～2h, obtain Graphene, by solid-to-liquid ratio 1:10, by stone
Ink alkene mixes with distilled water, and ultrasonic disperse 10～15min obtains graphene dispersing solution；Weigh 1.5～2.0g isophthalic two the most respectively
Phenol, 3～5mL formaldehyde and 35～40mL above-mentioned graphene dispersing solutions, be 7.0 with sodium bicarbonate regulation pH, pour into stainless after regulation
Steel autoclave, at 60～70 DEG C aging 3～4 days；After end to be aging, 1:1:1 in molar ratio, weigh respectively
4.82gFe(NO3)3、2.30gNH4H2PO4、1.38gLiNO3In beaker, and adding 15～20mL distilled water, stirring is to solid
It is completely dissolved, lysate is added in above-mentioned rustless steel autoclave, logical nitrogen in reactor, under nitrogen protection, rise
Temperature, to 80～100 DEG C, is incubated 1～2h, with 5～10 DEG C/min ramp to 180～220 DEG C after insulation, and reaction 8～10h, instead
Should filter after terminating, obtain filtering residue, after filtering residue is rinsed with dehydrated alcohol and water respectively, put in vacuum drying oven, 50～60
5～6h it are dried at DEG C；Finally above-mentioned dried solid is loaded porcelain boat, porcelain boat is put in tube furnace, in a nitrogen atmosphere,
It is warming up to 200～300 DEG C of calcinings 2～3h with 5～8 DEG C/min rate program, then is warming up to 400～500 DEG C of calcinings 2～3h, with
After be warming up to 600～700 DEG C calcining 3～4h, calcining terminate after be cooled to room temperature, obtain carbon gel coated LiFePO 4 for lithium ion batteries positive pole material
Material.
Example 1
First weigh 4g graphite powder and put in there-necked flask, flask is put in 0 DEG C of ice bath pot, the slowest in flask
The mixed acid of dropping 200mL, control rate of addition is 5mL/min, after completion of dropwise addition, adds 20g potassium permanganate, stirring mixing
After 20min, being moved into by flask in water-bath, stirring reaction 12h at 55 DEG C, reaction raises bath temperature again to 98 after terminating
DEG C, insulated and stirred reaction 10min；Described mixed acid be mass fraction 98% sulphuric acid and mass fraction 80% phosphoric acid by volume
10:1 mixes；After above-mentioned reaction terminates, from water-bath, take out flask, and in flask, add 6mL mass fraction 30%
Hydrogen peroxide, stirring, until bubble-free produces, filters to obtain filtering residue, ultrasonic clearly to it with mass fraction 5% hydrochloric acid and deionized water respectively
Wash 5min, then centrifugation obtain precipitate, grinds after lyophilization, cross 100 mesh sieves, obtains the graphite oxide powder that structure is fluffy,
Graphite oxide powder is placed on the quartz boat of tube furnace, under argon shield, is heated to 300 DEG C, reduction reaction 1h, obtain graphite
Alkene, by solid-to-liquid ratio 1:10, mixes Graphene with distilled water, and ultrasonic disperse 10min obtains graphene dispersing solution；Weigh the most respectively
1.5g resorcinol, 3mL formaldehyde and the above-mentioned graphene dispersing solution of 35mL, be 7.0 with sodium bicarbonate regulation pH, pour into not after regulation
Rust steel autoclave, at 60 DEG C aging 3 days；After end to be aging, 1:1:1 in molar ratio, weigh 4.82gFe respectively
(NO3)3、2.30gNH4H2PO4、1.38gLiNO3In beaker, and adding 15mL distilled water, stirring to solid is completely dissolved, will
Lysate adds in above-mentioned rustless steel autoclave, and in reactor, logical nitrogen, under nitrogen protection, is warming up to 80 DEG C, protects
Temperature 1h, with 5 DEG C/min ramp to 180 DEG C after insulation, reacts 8h, and reaction is filtered after terminating, and obtains filtering residue, is used respectively by filtering residue
After dehydrated alcohol and water rinse, put in vacuum drying oven, at 50 DEG C, be dried 5h；Finally above-mentioned dried solid is loaded
Porcelain boat, puts into porcelain boat in tube furnace, in a nitrogen atmosphere, is warming up to 200 DEG C of calcining 2h with 5 DEG C/min rate program, then rises
Temperature, to 400 DEG C of calcining 2h, then raises temperature to 600 DEG C of calcining 3h, and calcining is cooled to room temperature after terminating, and obtains carbon gel cladding phosphoric acid
Ferrum lithium anode material.
Take carbon gel coated LiFePO 4 for lithium ion batteries positive electrode prepared by 48mg, add 6mg politef and 7mg acetylene black,
Stirring is allowed to mix homogeneously, is pressed into diameter 4mm pole piece, is dried 8h at 100 DEG C, is subsequently placed in glove box encapsulation battery,
Stand 12h.This material tap density reaches 1.8g/mL, and electrical conductivity is high, and specific capacity reaches 209mAh/g, the diffusion of electrode ion
Coefficient is 1.6 × 10-12cm2/ s, cryogenic property is good, is worthy to be popularized and uses.
Example 2
First weigh 5g graphite powder and put in there-necked flask, flask is put in 3 DEG C of ice bath pots, the slowest in flask
The mixed acid of dropping 250mL, control rate of addition is 8mL/min, after completion of dropwise addition, adds 25g potassium permanganate, stirring mixing
After 25min, being moved into by flask in water-bath, stirring reaction 15h at 58 DEG C, reaction raises bath temperature again to 98 after terminating
DEG C, insulated and stirred reaction 13min；Described mixed acid be mass fraction 98% sulphuric acid and mass fraction 80% phosphoric acid by volume
10:1 mixes；After above-mentioned reaction terminates, from water-bath, take out flask, and in flask, add 7mL mass fraction 30%
Hydrogen peroxide, stirring, until bubble-free produces, filters to obtain filtering residue, ultrasonic clearly to it with mass fraction 5% hydrochloric acid and deionized water respectively
Wash 8min, then centrifugation obtain precipitate, grinds after lyophilization, cross 110 mesh sieves, obtains the graphite oxide powder that structure is fluffy,
Graphite oxide powder is placed on the quartz boat of tube furnace, under argon shield, is heated to 400 DEG C, reduction reaction 2h, obtain graphite
Alkene, by solid-to-liquid ratio 1:10, mixes Graphene with distilled water, and ultrasonic disperse 13min obtains graphene dispersing solution；Weigh the most respectively
1.8g resorcinol, 4mL formaldehyde and the above-mentioned graphene dispersing solution of 38mL, be 7.0 with sodium bicarbonate regulation pH, pour into not after regulation
Rust steel autoclave, at 65 DEG C aging 4 days；After end to be aging, 1:1:1 in molar ratio, weigh 4.82gFe respectively
(NO3)3、2.30gNH4H2PO4、1.38gLiNO3In beaker, and adding 18mL distilled water, stirring to solid is completely dissolved, will
Lysate adds in above-mentioned rustless steel autoclave, and in reactor, logical nitrogen, under nitrogen protection, is warming up to 90 DEG C, protects
Temperature 2h, with 8 DEG C/min ramp to 200 DEG C after insulation, reacts 9h, and reaction is filtered after terminating, and obtains filtering residue, is used respectively by filtering residue
After dehydrated alcohol and water rinse, put in vacuum drying oven, at 55 DEG C, be dried 6h；Finally above-mentioned dried solid is loaded
Porcelain boat, puts into porcelain boat in tube furnace, in a nitrogen atmosphere, is warming up to 250 DEG C of calcining 3h with 7 DEG C/min rate program, then rises
Temperature, to 450 DEG C of calcining 3h, then raises temperature to 650 DEG C of calcining 4h, and calcining is cooled to room temperature after terminating, and obtains carbon gel cladding phosphoric acid
Ferrum lithium anode material.
Take carbon gel coated LiFePO 4 for lithium ion batteries positive electrode prepared by 51mg, add 7mg politef and 8mg acetylene black,
Stirring is allowed to mix homogeneously, is pressed into diameter 5mm pole piece, is dried 10h at 103 DEG C, is subsequently placed in glove box encapsulation battery,
Stand 14h.This material tap density reaches 2.1g/mL, and electrical conductivity is high, and specific capacity reaches 216mAh/g, the diffusion of electrode ion
Coefficient is 1.7 × 10-12cm2/ s, cryogenic property is good, is worthy to be popularized and uses.
Example 3
First weigh 6g graphite powder and put in there-necked flask, flask is put in 5 DEG C of ice bath pots, the slowest in flask
The mixed acid of dropping 300mL, control rate of addition is 10mL/min, after completion of dropwise addition, adds 30g potassium permanganate, and stirring is mixed
After closing 30min, being moved into by flask in water-bath, stirring reaction 18h at 60 DEG C, reaction raises bath temperature again to 98 after terminating
DEG C, insulated and stirred reaction 15min；Described mixed acid be mass fraction 98% sulphuric acid and mass fraction 80% phosphoric acid by volume
10:1 mixes；After above-mentioned reaction terminates, from water-bath, take out flask, and in flask, add 8mL mass fraction 30%
Hydrogen peroxide, stirring, until bubble-free produces, filters to obtain filtering residue, ultrasonic clearly to it with mass fraction 5% hydrochloric acid and deionized water respectively
Wash 10min, then centrifugation obtain precipitate, grinds after lyophilization, cross 120 mesh sieves, obtains the graphite oxide powder that structure is fluffy,
Graphite oxide powder is placed on the quartz boat of tube furnace, under argon shield, is heated to 500 DEG C, reduction reaction 2h, obtain graphite
Alkene, by solid-to-liquid ratio 1:10, mixes Graphene with distilled water, and ultrasonic disperse 15min obtains graphene dispersing solution；Weigh the most respectively
2.0g resorcinol, 5mL formaldehyde and the above-mentioned graphene dispersing solution of 40mL, be 7.0 with sodium bicarbonate regulation pH, pour into not after regulation
Rust steel autoclave, at 70 DEG C aging 4 days；After end to be aging, 1:1:1 in molar ratio, weigh 4.82gFe respectively
(NO3)3、2.30gNH4H2PO4、1.38gLiNO3In beaker, and adding 20mL distilled water, stirring to solid is completely dissolved, will
Lysate adds in above-mentioned rustless steel autoclave, and in reactor, logical nitrogen, under nitrogen protection, is warming up to 100 DEG C, protects
Temperature 2h, with 10 DEG C/min ramp to 220 DEG C after insulation, reacts 10h, and reaction is filtered after terminating, and obtains filtering residue, by filtering residue respectively
After rinsing with dehydrated alcohol and water, put in vacuum drying oven, at 60 DEG C, be dried 6h；Finally above-mentioned dried solid is filled
Enter porcelain boat, porcelain boat is put in tube furnace, in a nitrogen atmosphere, be warming up to 300 DEG C of calcining 3h with 8 DEG C/min rate program, then
Being warming up to 500 DEG C of calcining 3h, then raise temperature to 700 DEG C of calcining 4h, calcining is cooled to room temperature after terminating, and obtains carbon gel cladding phosphorus
Acid ferrum lithium anode material.
Take carbon gel coated LiFePO 4 for lithium ion batteries positive electrode prepared by 55mg, add 7mg politef and 9mg acetylene black,
Stirring is allowed to mix homogeneously, is pressed into diameter 6mm pole piece, is dried 12h at 105 DEG C, is subsequently placed in glove box encapsulation battery,
Stand 15h.This material tap density reaches 2.3g/mL, and electrical conductivity is high, and specific capacity reaches 235mAh/g, the diffusion of electrode ion
Coefficient is 1.8 × 10-12cm2/ s, cryogenic property is good, is worthy to be popularized and uses.
Claims (1)
1. the preparation method of a carbon gel coated LiFePO 4 for lithium ion batteries positive electrode, it is characterised in that concrete preparation process is:
(1) weigh 4～6g graphite powders and put in there-necked flask, flask is put in 0～5 DEG C of ice bath pot, limit stirring in flask
While be slowly added dropwise the mixed acid of 200～300mL, control rate of addition be 5～10mL/min, after completion of dropwise addition, add 20～
30g potassium permanganate, stirring mixing 20～30min after, flask is moved in water-bath, at 55～60 DEG C stirring reaction 12～
18h, reaction raises bath temperature again to 98 DEG C after terminating, insulated and stirred reaction 10～15min；Described mixed acid is that quality is divided
Several 98% sulphuric acid and mass fraction 80% phosphoric acid 10:1 by volume mix；
(2), after above-mentioned reaction terminates, from water-bath, take out flask, and in flask, add the double of 6～8mL mass fractions 30%
Oxygen water, stirring until bubble-free produces, is filtered to obtain filtering residue, is used mass fraction 5% hydrochloric acid and deionized water to its ultrasonic cleaning respectively
5～10min, then centrifugation obtains precipitate, grinds after lyophilization, cross 100～120 mesh sieves, obtains the oxidation stone that structure is fluffy
Powdered ink end, is placed in graphite oxide powder on the quartz boat of tube furnace, is heated to 300～500 DEG C under argon shield, and reduction is anti-
Answer 1～2h, obtain Graphene, by solid-to-liquid ratio 1:10, Graphene is mixed with distilled water, ultrasonic disperse 10～15min, obtain Graphene
Dispersion liquid；
(3) weigh 1.5～2.0g resorcinol, 3～5mL formaldehyde and 35～40mL above-mentioned graphene dispersing solutions respectively, use carbonic acid
Hydrogen sodium regulation pH is 7.0, pours rustless steel autoclave after regulation into, at 60～70 DEG C aging 3～4 days；
(4) after end to be aging, 1:1:1 in molar ratio, weigh 4.82gFe (NO respectively3)3、2.30gNH4H2PO4、
1.38gLiNO3In beaker, and add 15～20mL distilled water, stirring be completely dissolved to solid, lysate is added above-mentioned not
In rust steel autoclave, in reactor, logical nitrogen, under nitrogen protection, is warming up to 80～100 DEG C, is incubated 1～2h, insulation
After with 5～10 DEG C/min ramp to 180～220 DEG C, react 8～10h, reaction terminate after filter, obtain filtering residue, filtering residue divided
Yong not put in vacuum drying oven, at 50～60 DEG C, be dried 5～6h after dehydrated alcohol and water rinses；
(5) by above-mentioned dried solid load porcelain boat, porcelain boat is put in tube furnace, in a nitrogen atmosphere, with 5～8 DEG C/
Min rate program is warming up to 200～300 DEG C of calcinings 2～3h, then is warming up to 400～500 DEG C of calcinings 2～3h, then raises temperature to
600～700 DEG C of calcinings 3～4h, calcining is cooled to room temperature after terminating, obtains carbon gel coated LiFePO 4 for lithium ion batteries positive electrode.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108565409A (en) * | 2018-01-19 | 2018-09-21 | 河北力滔电池材料有限公司 | Composite ferric lithium phosphate material and preparation method |
| CN108899506A (en) * | 2018-07-03 | 2018-11-27 | 广州大学 | A kind of porous nano carbon coating manganate cathode material for lithium and preparation method thereof |
| CN109004207B (en) * | 2018-06-29 | 2021-06-25 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Composite lithium iron phosphate cathode material and preparation method thereof |
| CN114122406A (en) * | 2022-01-25 | 2022-03-01 | 成都特隆美储能技术有限公司 | Preparation method of graphene modified lithium iron phosphate and lithium iron phosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108565409A (en) * | 2018-01-19 | 2018-09-21 | 河北力滔电池材料有限公司 | Composite ferric lithium phosphate material and preparation method |
| CN108565409B (en) * | 2018-01-19 | 2020-06-09 | 河北力滔电池材料有限公司 | Lithium iron phosphate composite material and preparation method thereof |
| CN109004207B (en) * | 2018-06-29 | 2021-06-25 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | Composite lithium iron phosphate cathode material and preparation method thereof |
| CN108899506A (en) * | 2018-07-03 | 2018-11-27 | 广州大学 | A kind of porous nano carbon coating manganate cathode material for lithium and preparation method thereof |
| CN114122406A (en) * | 2022-01-25 | 2022-03-01 | 成都特隆美储能技术有限公司 | Preparation method of graphene modified lithium iron phosphate and lithium iron phosphate |
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