CN107619032A - A kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material - Google Patents
A kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material Download PDFInfo
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Abstract
The invention belongs to energy and material technical field of lithium batteries, particularly a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, preparation method comprises the following steps：(1) Li source compound, Fe source compound, P source compound, fullerenes, reducing agent, surfactant and ordered mesopore carbon are weighed, and mixes form mixed liquor in deionized water；By step (1) in obtained mixed liquor in protective atmosphere, reacted products therefrom is filtered, dries, and obtains spherical mesoporous ferric lithium phosphate precursor；By step (2) in obtained spherical mesoporous ferric lithium phosphate precursor in protective atmosphere, in 500 ~ 700 DEG C of 8 ~ 16h of constant temperature, obtain spherical mesoporous lithium iron phosphate positive material.It is provided by the present invention prepare LiFePO4 technological process it is simple, have great application prospect.
Description
Technical field
The invention belongs to energy and material technical field of lithium batteries, particularly one kind to have uniform-spherical meso-hole structure ferric phosphate
The preparation method of lithium anode material.
Background technology
With consuming excessively for fossil energy, seek cleaning, efficient, green, regenerative resource increasingly causes world wide
Extensive concern, and battery be rationally utilize these new energy important medium.Lithium ion battery is the green high-capacity of a new generation
Battery, there is the crowds such as voltage is high, energy density is big, good cycle, self discharge are small, memory-less effect, operating temperature range are wide
More advantages, it is widely used in mobile phone, notebook computer, UPS, video camera, various portable power tools, electronic instrument, force
Installing is standby etc., is also had a good application prospect in electric automobile, it is considered to be in 21st century to national economy and people
The significant new high-tech product of people's livelihood work.
Positive electrode is the important component of lithium ion battery.At present, the positive electrode of most study is LiCoO2、
LiNiO2、LiMn2O4、LiFePO4。LiCoO2Comparative maturity is studied, is the positive electrode of unique large-scale commercial, its is comprehensive
Can be excellent but expensive, capacity is relatively low, and toxicity is larger, and certain safety problem be present, by by the new of high-performance and low-cost
Section bar material is substituted.LiNiO2 costs are relatively low, and capacity is higher, but prepare difficulty, the uniformity and poor reproducibility of material, exist
More serious safety problem.Spinelle LiMn2O4Cost is low, and security is good, but cycle performance, especially high temperature cyclic performance
Difference, there is certain dissolubility in the electrolytic solution, and storge quality is poor.LiFePO4 (the LiFePO of orthogonal olivine structural4) positive pole material
Material has concentrated LiCoO2、LiNiO2、LiMn2O4Deng the respective advantage of material, study hotspot new both at home and abroad is increasingly becoming.Tentatively
Research shows that LiFePO4 is free of precious metal, and raw material is inexpensive, and resource is extremely abundant；Operating voltage is moderate (3.4V)；Platform
Characteristic is good, and voltage is steady (can be matched in excellence or beauty with voltage-stabilized power supply)；Theoretical capacity is big (170mAh/g)；Stability Analysis of Structures, security performance are splendid
(for O and P with strong covalent bond strong bonded, it is difficult analysis oxygen solution to make material)；High-temperature behavior and good cycle；Volume during charging
Reduce, bulk effect when coordinating with carbon negative pole material is good；Good with most of electrolyte system compatibilities, storge quality is good；Nothing
Poison, it is real green material.
But LiFePO4 exist two it is obvious the shortcomings that, first, electrical conductivity is low, cause high magnification charging performance poor, it is actual
Specific capacity is low；Second, bulk density is low, cause volume and capacity ratio low.The two shortcomings hinder the practical application of the material.
At present, the research of people, which focuses on, solves this low field of LiFePO4 electrical conductivity, and achieves certain
Achievement.The corrective measure taken mainly has：
Conductive carbon material or conductive metal particle are mixed inside toward lithium iron phosphate particles, or it is conductive toward LiFePO4 Surface coating
Carbon material, improve the electronic conductivity of material.
A small amount of foreign metal ion, such as Mg are mixed into LiFePO4 lattice2+、Al3+、Ti4+、Zr4+、Nb5+, substitute one
Divide Li+Position so that LiFePO4 assertive evidence semiconductor transition is n-type or p-type semiconductor, significantly improve the electricity of material
Electron conductivity.
The impurity elements such as Mn2+ are mixed into LiFePO4, substitute a part of Fe2+Position, increase the structure cell of LiFePO4
Parameter, the lithium ion conductivity of material is improved, synthesize iron manganese phosphate for lithium（LiFe1-xMnxPO4, 0 ＜ x≤0.4）.
Using new technologies such as sol-gal process, liquid phase synthesizing methods, reduce the size of LiFePO4 crystal grain, or even synthesize nanometer
LiFePO4, shortens Li+ diffusion length as far as possible, it is apparent on improve the lithium ion conductivity and stock utilization of material.
And the research for improving LiFePO4 low bulk density never obtains considerable progress, the reality for hindering material should
With.The solid density of cobalt acid lithium is 5.1g/cm3, and the tap density of commodity cobalt acid lithium is generally 2.0-2.4g/cm3.And ferric phosphate
The solid density of lithium is only 3.6g/cm3, inherently more much lower than cobalt acid lithium.To improve electric conductivity, people mix conductive carbon
Material, the bulk density of material is significantly reduced again so that the tap density of general carbon dope LiFePO4 only has 1.0g/cm3.Such as
This low bulk density so that the volume and capacity ratio of LiFePO4 is more much lower than cobalt acid lithium, and manufactured battery volume will be very huge
Greatly, not only having no advantage can say, and be difficult to apply to reality.Therefore, the bulk density and volume specific volume of LiFePO4 are improved
Measure marginal to the practical tool of LiFePO4.
The bulk density of powder body material and the pattern of powder granule, particles size and distribution are closely related.At present both at home and abroad
The lithium iron phosphate positive material of report is all made up of random sheet or granular solid matter, and bulk density is low.By rule
The LiFePO 4 powder material of spheric granules composition is by with higher bulk density.Moreover, spherical product also has excellent
Different mobility, dispersiveness and machinability, it is advantageous to make the coating of positive electrode slurry and electrode slice, improves electricity
Pole piece quality.And the LiFePO 4 powder material being made up of the spheric granules with meso-hole structure, except by with high accumulation
Outside density, moreover it is possible to increase Li+Diffusion admittance, shorten Li+Diffusion length, it is apparent on improve the lithium ion conductivity of material
And stock utilization.And the LiFePO 4 powder material of spheric granules composition is rarely reported, especially a kind of spherical mesoporous phosphoric acid
The preparation method of iron lithium anode material does not have been reported that before this.
The content of the invention
It is an object of the invention to provide a kind of preparation side with uniform-spherical meso-hole structure lithium iron phosphate positive material
Method, the spherical mesoporous lithium iron phosphate positive material have bulk density high, can increase Li+ diffusion admittance, shorten Li+Expansion
Distance is dissipated, and then improves the lithium ion conductivity and stock utilization of positive electrode.
The present invention is achieved through the following technical solutions：One kind has uniform-spherical meso-hole structure iron phosphate lithium positive pole material
The preparation method of material, the preparation method of the spherical mesoporous lithium iron phosphate positive material are improved by lithium iron phosphate particles spheroidization
Its tap density and volume and capacity ratio；Its lithium ion conductivity is improved by lithium iron phosphate particles mesoporousization, and LiFePO4
Spheroidization with mesoporous chemical industry skill is total to by the soft template effect of surfactant and the hard template effect of ordered mesoporous carbon material
Same-action is realized.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, spherical Jie
The preparation method of hole lithium iron phosphate positive material comprises the following steps：
(1) in molar ratio Li: Fe: P: fullerenes：Reducing agent: surfactant=1: 0.9~1.1: 0.9~1.1: 0.9~1.1:
0.01~0.03: 0.01~0.03 weighs Li source compound, Fe source compound, P source compound, fullerenes, reducing agent and surface
Activating agent, in mass ratio Fe: ordered mesopore carbon=1: 0.1~0.2 weighs ordered mesopore carbon, and mixes in deionized water, formed
Fe concentration is 0.5~3mol/L mixed liquor；
By step (1) in obtained mixed liquor in protective atmosphere, 2~4d, gained are reacted under the conditions of 200~350 DEG C
Product dries 2~24h within the temperature range of 80~200 DEG C after filtering, obtains spherical mesoporous ferric lithium phosphate precursor；
By step (2) in obtained spherical mesoporous ferric lithium phosphate precursor in protective atmosphere, in 500~700 DEG C of constant temperature 8
~16h, obtain spherical mesoporous lithium iron phosphate positive material.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described Li source compound is lithium carbonate, lithium formate, lithium hydroxide, lithium acetate, lithium fluoride, lithium iodide, lithium bromide, lithium chloride
In one or more.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described Fe source compound is ferrous oxalate, ferrous acetate, ferrous carbonate or ferric acetate.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described P source compound is the one or more in phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, triammonium phosphate.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described reducing agent be ascorbic acid, hexanedioic acid, malonic acid, mandelic acid, malic acid, citric acid, lactic acid, formaldehyde, acetaldehyde,
One or more in n-butanal, isobutylaldehyde, tetrem ethyl glycol, isopropanol, ethylene glycol.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described surfactant is trimethyl ammonium phosphate, cetyl trimethyl ammonium phosphate, dodecyltriethylammonium phosphorus
Sour ammonium, cetyl triethyl group ammonium phosphate, DTAB, cetyl trimethylammonium bromide, dodecyl
Triethylammonium bromide, cetyltriethylammonium bromide, DTAC, hexadecyltrimethylammonium chloride,
One or more in dodecyltriethylammonium ammonium chloride, cetyl triethyl ammonium chloride.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (1) in
Described ordered mesoporous carbon material is one kind in CMK-3, C-MTS-9.
In a kind of described preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, step (2),
(3) the protective atmosphere described in uses a kind of protective gas in nitrogen, argon gas, helium or neon.
A kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material of the present invention is with meso-hole structure
Uniform-spherical particle, average pore size 7nm, particle diameter are in standardized normal distribution, and average grain diameter is 3~5um, and tap density is reachable
1.4~1.8g/cm3, first discharge specific capacity is up to 155~165mAh/g at room temperature, 2C specific discharge capacities up to 135~
145mAh/g.It is provided by the present invention prepare spherical mesoporous LiFePO4 technological process it is simple, have great application prospect.
Embodiment
Below by embodiment, to a kind of system with uniform-spherical meso-hole structure lithium iron phosphate positive material of the present invention
Preparation Method, which is made, further to be illustrated.
Embodiment 1
In molar ratio Li: Fe: P: fullerenes: reducing agent: surfactant=1: 0.9: 0.9: 0.9: 0.01: 0.01 weigh lithium carbonate,
Ferrous oxalate, triammonium phosphate, fullerenes, citric acid and cetyl trimethyl ammonium phosphate, Fe in mass ratio: ordered mesopore carbon=1:
0.1 weighs CMK-3, and mixes in deionized water, forms the mixed liquor that Fe concentration is 3mol/L, then this mixed liquor exists
In N2 atmosphere, 30h is reacted under the conditions of 200 DEG C, products therefrom is after filtering in 80 DEG C of dry 24h, obtained ball shaped nano
Ferric lithium phosphate precursor is in N2 atmosphere, after 500 DEG C of constant temperature 16h, obtains spherical mesoporous lithium iron phosphate positive material, is denoted as
LiFePO4-1。
Embodiment 2
In molar ratio Li: Fe: P: fullerenes: reducing agent: surfactant=1: 1.1: 1.1: 1.1: 0.03: 0.03 weigh lithium formate,
Ferrous acetate, ammonium dihydrogen phosphate, fullerenes, formaldehyde and cetyl triethyl group ammonium phosphate, Fe in mass ratio: ordered mesopore carbon=1:
0.2 weighs C-MTS-9, and mixes in deionized water, forms the mixed liquor that Fe concentration is 0.5mol/L, then mixes this
Liquid in an ar atmosphere, reacts 15h, products therefrom is after filtering in 200 DEG C of dry 2h, obtained spherical Jie under the conditions of 350 DEG C
Hole ferric lithium phosphate precursor in an ar atmosphere, after 700 DEG C of constant temperature 8h, obtains spherical mesoporous lithium iron phosphate positive material, is denoted as
LiFePO4-2。
Embodiment 3
In molar ratio Li: Fe: P: fullerenes: reducing agent: surfactant=1: weigh hydroxide at 0.9: 1.1: 0.9: 0.01: 0.03
Lithium, ferrous carbonate, diammonium hydrogen phosphate, fullerenes, ethylene glycol and cetyl trimethylammonium bromide, in mass ratio Fe: order mesoporous
Carbon=1: 0.2 weighs CMK-3, and mixes in deionized water, the mixed liquor that Fe concentration is 0.5mol/L is formed, then mixes this
Liquid is closed in He atmosphere, 30h is reacted under the conditions of 200 DEG C, for products therefrom after filtering in 80 DEG C of dry 24h, what is obtained is spherical
Mesoporous ferric lithium phosphate precursor is in He atmosphere, after 500 DEG C of constant temperature 16h, obtains spherical mesoporous lithium iron phosphate positive material,
It is denoted as LiFePO4-3。
Embodiment 4
In molar ratio Li: Fe: P: fullerenes: reducing agent: surfactant=1: 1.1: 0.9: 1.1: 0.03: 0.01 weigh lithium fluoride,
Ferric acetate, phosphoric acid, fullerenes, ascorbic acid and hexadecyltrimethylammonium chloride, in mass ratio Fe: ordered mesopore carbon=1: 0.1
C-MTS-9 is weighed, and is mixed in deionized water, the mixed liquor that Fe concentration is 0.5mol/L is formed, then this mixed liquor exists
In Ne atmosphere, 30h is reacted under the conditions of 200 DEG C, products therefrom is after filtering in 80 DEG C of dry 24h, obtained spherical mesoporous phosphorus
Sour iron lithium presoma is in Ne atmosphere, after 500 DEG C of constant temperature 16h, obtains spherical mesoporous lithium iron phosphate positive material, is denoted as
LiFePO4-4。
Only illustrated out in embodiment lithium source lithium carbonate, lithium formate, lithium hydroxide and lithium fluoride, due to lithium iodide, lithium bromide,
Lithium chloride has similar chemical property to lithium fluoride, and the chemical reaction type of participation is identical, in the anti-of preparation method of the present invention
Ying Zhongjun can provide the lithium ion of target compound LiFePO4, and then lithium source chemicals are applicable the present invention.
Only illustrated out in embodiment reducing agent ascorbic acid, citric acid, formaldehyde, ethylene glycol, due to hexanedioic acid, malonic acid,
Mandelic acid, malic acid, lactic acid, acetaldehyde, n-butanal, isobutylaldehyde, tetrem ethyl glycol, isopropanol and ascorbic acid, lemon
Acid, formaldehyde, ethylene glycol have similar chemical property, and the chemical reaction type of participation is identical, and then reduce immunomodulator compounds and be applicable
The present invention.
Only illustrated out in embodiment surfactant cetyl trimethyl ammonium phosphate, cetyl triethyl group ammonium phosphate,
Cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, due to trimethyl ammonium phosphate, dodecyl
Triethyl group ammonium phosphate, DTAB, dodecyltriethylammonium ammonium bromide, cetyltriethylammonium bromide,
DTAC, dodecyltriethylammonium ammonium chloride, cetyl triethyl ammonium chloride and cetyl front three
Base ammonium phosphate, cetyl triethyl group ammonium phosphate, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride have
Similar chemical property, the chemical reaction type of participation is identical, and then surfactant compounds are applicable the present invention.
Claims (8)
1. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material, it is characterised in that described is spherical
The preparation method of mesoporous lithium iron phosphate positive material comprises the following steps：
(1) in molar ratio Li: Fe: P: fullerenes: reducing agent: surfactant=1: 0.9~1.1: 0.9~1.1: 0.9~1.1:
0.01~0.03: 0.01~0.03 weighs Li source compound, Fe source compound, P source compound, fullerenes, reducing agent and surface
Activating agent, in mass ratio Fe: ordered mesopore carbon=1: 0.1~0.2 weighs ordered mesopore carbon, and mixes in deionized water, formed
Fe concentration is 0.5~3mol/L mixed liquor；
By step (1) in obtained mixed liquor in protective atmosphere, 2~4d, gained production are reacted under the conditions of 200~350 DEG C
Thing dries 2~24h within the temperature range of 80~200 DEG C after filtering, obtains spherical mesoporous ferric lithium phosphate precursor；
By step (2) in obtained spherical mesoporous ferric lithium phosphate precursor in protective atmosphere, in 500~700 DEG C of constant temperature 8
~16h, obtain spherical mesoporous lithium iron phosphate positive material.
2. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in Li source compound for lithium carbonate, lithium formate, lithium hydroxide, lithium acetate, lithium fluoride, iodine
Change the one or more in lithium, lithium bromide, lithium chloride.
3. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in Fe source compound be ferrous oxalate, ferrous acetate, ferrous carbonate or ferric acetate.
4. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in P source compound be phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, in triammonium phosphate
It is one or more kinds of.
5. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in reducing agent for ascorbic acid, hexanedioic acid, malonic acid, mandelic acid, malic acid, lemon
Acid, lactic acid, formaldehyde, acetaldehyde, n-butanal, isobutylaldehyde, tetrem ethyl glycol, isopropanol, one kind in ethylene glycol or it is a kind of with
On.
6. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in surfactant for trimethyl ammonium phosphate, cetyl trimethyl phosphoric acid
Ammonium, dodecyltriethylammonium ammonium phosphate, cetyl triethyl group ammonium phosphate, DTAB, cetyl three
Methyl bromide ammonium, dodecyltriethylammonium ammonium bromide, cetyltriethylammonium bromide, DTAC, ten
Six alkyl trimethyl ammonium chlorides, dodecyltriethylammonium ammonium chloride, one kind in cetyl triethyl ammonium chloride or it is a kind of with
On.
7. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (1) described in ordered mesoporous carbon material be CMK-3, C-MTS-9 in one kind.
8. a kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material according to claim 1,
It is characterized in that step (2), (3) described in protective atmosphere use nitrogen, argon gas, helium or neon in a kind of protection gas
Body.
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| CN111224103A (en) * | 2020-01-17 | 2020-06-02 | 贝特瑞（天津）纳米材料制造有限公司 | Preparation method of metal ion-doped high-rate mesoporous lithium iron phosphate cathode material |
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