CN109301177A - A kind of stratiform composite ferric lithium phosphate material and preparation method thereof - Google Patents
A kind of stratiform composite ferric lithium phosphate material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of stratiform composite ferric lithium phosphate materials and preparation method thereof, by the LiFePO4 layer structural material being formed by stacking alternate with two-dimensional nano piece；The two-dimensional nano piece is by several combinations of one of graphene and conducting polymer, carbon nanotube, baby's alkene, molybdenum disulfide.It is induced by two-dimensional nano piece, to form the LiFePO4 with lamellar structure.Pass through LiFePO4 piece stratification, layer structure improves Li gan shifting rate, so that contracting has been broken, embedding, the de- channel of Li+, makes Li+ gan move scope of activities and expand, it will make LiFePO4 that there is high reversible capacity and good cyclical stability, greatly promote the cycle performance of battery material；Product is regulated and controled in molecule or atomic level by sol-gal process, by luring into for two-dimensional nano piece, LiFePO4 is made to have the characteristics that monodisperse and two-dimensional.
Description
Technical field
The present invention relates to a kind of battery materials, and in particular to a kind of stratiform LiFePO 4 material and preparation method thereof.
Background technique
Lithium ion battery is a kind of novel secondary energy-storage battery to grow up the 1990s.Due to high energy
Amount, the long-life, low consumption, nuisanceless, memory-less effect and self discharge are small, internal resistance is small, cost performance is high, pollute the advantages that few,
It is widely used in the fields such as mobile phone, laptop, video camera, digital camera, electric car.
In lithium ion battery industrialization promotion, to battery capacity, safety, overall cost more demanding, positive material
Material becomes main bottleneck.Currently, anode material for lithium-ion batteries mainly has cobalt acid lithium, lithium nickelate, LiMn2O4 and LiFePO4 etc.,
Wherein since cobalt and nickel resources are limited, it is only used for small-sized lithium electricity positive electrode；And LiFePO4 (LiFeP04), LiMn2O4
(LiMn204), stratiform manganese oxide lithium (LiMn02) have it is from a wealth of sources, cheap, thermal stability is good, no hygroscopicity, to ring
Border is friendly, and large-scale development is suitble to use, the electric car required more suitable for large capacity.
The LiFePO4 (LiFeP04) of olivine-type structure has stable structure and higher specific capacity, circulating and reversible
Performance is high, is suitable for the positive electrode of lithium battery, however, itself lacking due to olivine-type structure LiFePO4 (LiFeP04)
It falls into, P0 in structure limits the mobile space of L i+, and movable passageway is longer, affects large capacity fast charging and discharging.Although
Improved at present by improving preparation method and doping, but the intrinsic conductivity of LiFePO4 is unable to get changing for essence
Become.In addition, existing preparation method solid phase method has reaction not exclusively, irregular defect is crystallized, there are reaction process for liquid phase method
Complexity, the defect of severe reaction conditions.
In traditional LiFePO4 production technology, ion doping and simple carbon-coated technology are mostly used, is obtained
Lack conductive network connection to spherical LiFeP04 due to carbon-coated incomplete, and between the lithium iron phosphate particles coated, from
And good multiplying power and cycle performance cannot be shown.
Since the graphene with plumbago single slice layer structure is after 2004 are found, constantly about its superior machine
The report of tool performance and superelevation conductivity.Therefore graphene is extremely apparent to electric conductivity is promoted for LiFePO4.But
The power battery required for high rate capability, however it remains the defect that conductive network and conductive channel are not added.Make internal disorder or usurp the reason is that
LiFePO4 pattern is an important influence factor.Common LiFePO4 is spheric granules, and inner conductive network and conduction are logical
There are significant deficiencies in road.Despite the use of the more excellent graphene of electric conductivity, but be difficult to lead in LiFePO4 internal build
Electric channel.
Summary of the invention
It is an object of the invention to: a kind of stratiform LiFePO 4 material and preparation method thereof to solve the above problem,
By the LiFePO4 layer structure being formed by stacking alternate with two-dimensional nano piece, ionic mobility is improved, makes LiFePO4 that there is pole
High reversible capacity and good cyclical stability greatly promotes the cycle performance of battery material.
The technical solution adopted by the present invention is that such:
A kind of stratiform composite ferric lithium phosphate material, by the LiFePO4 layer structural wood being formed by stacking alternate with two-dimensional nano piece
Material；The two-dimensional nano piece is by several combinations of one of graphene and conducting polymer, carbon nanotube, baby's alkene, molybdenum disulfide.
Further, the conducting polymer is one of polypyrrole, polyaniline, polyoxyethylene or a variety of.
Another technical solution of the invention is such that
A kind of preparation method of stratiform composite ferric lithium phosphate material, is induced by two-dimensional nano piece, has lamella to be formed
The LiFePO4 of structure, it is specific the preparation method is as follows:
(1) two-dimensional nano piece is added in dispersing agent, ultrasound 4~15 hours forms the suspension of dispersion, low-speed centrifugal
Biggish two-dimensional nano piece is removed, two-dimensional nano piece suspension is obtained；
(2) source of iron and phosphorus source are dispersed in the mixed solution of ethanol/water according to P:Fe molar ratio=1:1-7 target proportion
In, it is stirred to react 0.5~3 hour, is then added in the two-dimensional nano piece suspension that step (1) obtains and is uniformly dispersed；Pass through ball
Grind the ferric phosphate colloid by two-dimensional nano piece induced synthesis lamella；
(3) using iron and lithium molar ratio Fe:Li=l:1-1.5 as target, lithium source is uniformly added into step (2) colloid,
It is ground and is removed by colloid mill simultaneously, form gel through vacuum distillation removal partial moisture, gel is dry in a vacuum drying oven
Xerogel, xerogel are calcined 5-12 hours at protective atmosphere and 600-75 DEG C, obtain stratiform composite ferric lithium phosphate material.
Further, dispersing agent described in step (1) be trimethyl cetyl ammonium bromide, dodecyl sodium sulfate,
One of polyethylene glycol 400 is a variety of.
Further, protective gas is one of nitrogen, argon gas, nitrogen in high-temperature calcination described in step (3).
Further, colloid mill described in step (3) is that mill is crushed colloid mill, is made by colloid mill in colloid
The piece stratification in shear history of the LiFePO4 of shape.
In conclusion by adopting the above technical scheme, the beneficial effects of the present invention are:
1, suitable two-dimensional nano sheet material is added in LiFePO4 preparation process, to be formed a kind of with sheet
Composite ferric lithium phosphate material, special layer structure improve Li gan shifting rate, so that contracting has been broken, embedding, the de- channel of Li+, makes Li
+ gan moves scope of activities and expands, and has high reversible capacity and good cyclical stability.
2, reaction system is made to reach in initial reaction stage the mixing of molecule or atomic level using sol-gal process, so as to
Product is regulated and controled in molecule or atomic level, compares very advantageous with conventional method.The layer made from the method for the invention
Shape LiFePO4 has the characteristics of high-purity, monodisperse and small size, and lithium ion battery is made to have fine high rate performance, high circulation
Energy and first charge-discharge efficiency.
3, process flow is simple, and high production efficiency, equipment investment be low, continuous operation, easy to implement with control, energy consumption
It is low, be conducive to industrialized production.
Specific embodiment
A kind of stratiform composite ferric lithium phosphate material, by the LiFePO4 layer structural wood being formed by stacking alternate with two-dimensional nano piece
Material；The two-dimensional nano piece is by several combinations of one of graphene and conducting polymer, carbon nanotube, baby's alkene, molybdenum disulfide.
Select the conducting polymer that electro-chemical activity is high, environmental stability is good, conductivity is high；
Carbon nanotube conducting rate is high, and specific surface area utilization rate is big, while having storage lithium performance；
Graphene, silene, molybdenum disulfide have planar structure, there are performances such as many excellent electricity, optics, calorifics,
LiFePO4 forming layer structure is lured into using above-mentioned two-dimensional nano piece；
The conducting polymer is one of polypyrrole, polyaniline, polyoxyethylene or a variety of.
Embodiment 1
A kind of preparation method of stratiform composite ferric lithium phosphate material,
(1) nanometer sheet that graphene and conducting polymer, carbon nanotube are combined into is added to dodecyl sodium sulfate water
Disperse in solution, be ultrasonically treated 15 hours, form the suspension of dispersion, low-speed centrifugal removes biggish two-dimensional nano piece, obtains
Two-dimensional nano piece suspension；
(2) iron hydroxide and ammonium dihydrogen phosphate are dispersed in ethanol/water according to P:Fe molar ratio=1:1-7 target proportion
Mixed solution in, be stirred to react 2 hours, be then added in the two-dimensional nano piece suspension that step (1) obtains and be uniformly dispersed；It is logical
Ball milling is crossed by the ferric phosphate colloid of two-dimensional nano piece induced synthesis lamella；
(3) using iron and lithium molar ratio Fe:L i=l:1.5 as target, lithium nitrate is uniformly added into step (2) colloid,
Mill is crushed colloid mill mill grinding removing, forms gel through vacuum distillation removal partial moisture, gel is done in a vacuum drying oven
It is dry that xerogel, xerogel are calcined 5 hours at protective atmosphere and 600-750 DEG C, obtain stratiform composite ferric lithium phosphate material.
Embodiment 2
A kind of preparation method of stratiform composite ferric lithium phosphate material,
(1) graphene and carbon nanotube, molybdenum disulfide nano sheet will be added in dispersing agent, ultrasound 12 hours is formed
The suspension of dispersion, low-speed centrifugal remove biggish two-dimensional nano piece, obtain two-dimensional nano piece suspension；
(2) ferric sulfate and dibastic sodium phosphate are dispersed in the mixing of ethanol/water according to P:Fe molar ratio=1:6 target proportion
In solution, it is stirred to react 3 hours, is then added in the two-dimensional nano piece suspension that step (1) obtains and is uniformly dispersed；Pass through ball milling
By the ferric phosphate colloid of two-dimensional nano piece induced synthesis lamella；
(3) using iron and lithium molar ratio Fe:L i=l:1 as target, lithium acetate is uniformly added into step (2) colloid, together
It is ground and is removed by colloid mill, form gel through vacuum distillation removal partial moisture, gel is dry solidifyingly dry in a vacuum drying oven
Glue, xerogel are calcined 5-12 hours at protective atmosphere and 600-75 DEG C, obtain stratiform composite ferric lithium phosphate material.
Claims (6)
1. a kind of stratiform composite ferric lithium phosphate material, it is characterised in that: be formed by stacking by LiFePO4 is alternate with two-dimensional nano piece
Layer structural material；The two-dimensional nano piece is by one in graphene and conducting polymer, carbon nanotube, baby's alkene, molybdenum disulfide
Several combinations of kind.
2. a kind of stratiform composite ferric lithium phosphate material according to claim 1, it is characterised in that: the conducting polymer is
One of polypyrrole, polyaniline, polyoxyethylene are a variety of.
3. a kind of preparation method of stratiform composite ferric lithium phosphate material as described in claim 1, it is characterised in that: pass through two dimension
Nanometer sheet induction, to form the LiFePO4 with lamellar structure, it is specific the preparation method is as follows:
(1) two-dimensional nano piece is added in dispersing agent, ultrasound 4~15 hours, forms the suspension of dispersion, low-speed centrifugal removal
Biggish two-dimensional nano piece obtains two-dimensional nano piece suspension；
(2) source of iron and phosphorus source are dispersed in the mixed solution of ethanol/water according to P:Fe molar ratio=1:1-7 target proportion,
It is stirred to react 0.5~3 hour, is then added in the two-dimensional nano piece suspension that step (1) obtains and is uniformly dispersed；By ball milling by
The ferric phosphate colloid of two-dimensional nano piece induced synthesis lamella；
(3) using iron and lithium molar ratio Fe:Li=l:1-1.5 as target, lithium source is uniformly added into step (2) colloid, simultaneously
It is ground and is removed by colloid mill, form gel through vacuum distillation removal partial moisture, gel is dry solidifyingly dry in a vacuum drying oven
Glue, xerogel are calcined 5-12 hours at protective atmosphere and 600-75 DEG C, obtain stratiform composite ferric lithium phosphate material.
4. a kind of preparation method of stratiform composite ferric lithium phosphate material according to claim 3, it is characterised in that: step
(1) dispersing agent described in is one of trimethyl cetyl ammonium bromide, dodecyl sodium sulfate, polyethylene glycol or more
Kind.
5. a kind of preparation method of stratiform composite ferric lithium phosphate material according to claim 3, it is characterised in that: step
(3) protective gas is one of nitrogen, argon gas, nitrogen in the high-temperature calcination described in.
6. a kind of preparation method of stratiform composite ferric lithium phosphate material according to claim 3, it is characterised in that: step
(3) colloid mill described in is that mill is crushed colloid mill, is shearing the LiFePO4 in colloidal by colloid mill
Piece stratification in journey.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148371A (en) * | 2011-03-03 | 2011-08-10 | 上海大学 | Graphene/phosphoric acid iron-lithium composite material with sandwich structure and preparation method thereof |
| CN102544492A (en) * | 2011-03-07 | 2012-07-04 | 南京大学 | Lithium iron phosphate/graphene composite material with interlay sheet structure and preparation method and application thereof |
| CN103094564A (en) * | 2013-01-16 | 2013-05-08 | 天津大学 | Method for preparing composite nano material filled with lithium iron phosphate between graphene layers |
| CN106450214A (en) * | 2016-11-08 | 2017-02-22 | 成都新柯力化工科技有限公司 | Layered lithium iron phosphate composite material and preparation method thereof |
-
2018
- 2018-08-15 CN CN201810931478.4A patent/CN109301177A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102148371A (en) * | 2011-03-03 | 2011-08-10 | 上海大学 | Graphene/phosphoric acid iron-lithium composite material with sandwich structure and preparation method thereof |
| CN102544492A (en) * | 2011-03-07 | 2012-07-04 | 南京大学 | Lithium iron phosphate/graphene composite material with interlay sheet structure and preparation method and application thereof |
| CN103094564A (en) * | 2013-01-16 | 2013-05-08 | 天津大学 | Method for preparing composite nano material filled with lithium iron phosphate between graphene layers |
| CN106450214A (en) * | 2016-11-08 | 2017-02-22 | 成都新柯力化工科技有限公司 | Layered lithium iron phosphate composite material and preparation method thereof |
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