CN105826555A - Preparation method of lithium iron phosphate and positive electrode material - Google Patents

Preparation method of lithium iron phosphate and positive electrode material Download PDF

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Publication number
CN105826555A
CN105826555A CN201610152316.1A CN201610152316A CN105826555A CN 105826555 A CN105826555 A CN 105826555A CN 201610152316 A CN201610152316 A CN 201610152316A CN 105826555 A CN105826555 A CN 105826555A
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fepo
lithium
lifepo4
sintering
pore creating
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CN105826555B (en
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何方勇
先雪峰
陈明
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GUIZHOU ANDA ENERGY TECHNOLOGY Co Ltd
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GUIZHOU ANDA ENERGY TECHNOLOGY Co Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection 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
    • H01M4/5825Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention relates to the field of new energy material preparation, and discloses a preparation method of lithium iron phosphate and a positive electrode material. Lithium iron phosphate is prepared by sintering a raw material containing FePO4, a lithium source, and a carbon source in the presence of a pore forming agent. The preparation method of the positive electrode material comprises the following steps: preparing lithium iron phosphate according to the provided method, and mixing obtained lithium iron phosphate with a conductive agent. The obtained lithium iron phosphate has the characteristics of large specific surface area, large discharge rate, and good low temperature discharge performance.

Description

A kind of method preparing LiFePO4 and positive electrode
Technical field
The present invention relates to new energy materials preparation field, in particular it relates to a kind of method preparing LiFePO4 and positive electrode.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, have that voltage is high, energy density big, the many merits such as life-span length, self discharge are little, memory-less effect and operating temperature range width, at small-sized movable energy field, such as mobile phone, digital camera etc., and Large-scale Mobile energy field, such as plug-in hybrid electric vehicle, pure electric vehicle etc., and fixed sources of energy field, such as energy-accumulating power station, UPS etc., suffer from being widely applied and application prospect.
Positive electrode is the important component part of lithium ion battery, and its performance determines the combination property of battery to a great extent, and positive electrode research and improvement are one of cores of lithium ion battery development.Conventional positive electrode has LiCoO2、LiNiO2、LiMn2O4、LiFePO4And their derived material.Layer structure LiCoO2、LiNiO2Or their derivant is or large-scale commercial is applied, and combination property is preferable, but it exists the shortcomings such as expensive, toxicity is big, heat stability is low, raw material basic unit price is low.The LiMn of spinel structure2O4Low cost, safety is good, but owing to being affected by Mn dissolution, cycle performance particularly high temperature cyclic performance is poor.In general, the LiFePO4 (LiFePO of olivine structural4) positive electrode become study hotspot both domestic and external.
In the various methods preparing LiFePO4, with Orthophosphoric acid Ferrum (FePO4·xH2O) method as precursor has the advantages such as target product specific capacity height, purity height and multiplying power cryogenic property are good.But the technique of existing Orthophosphoric acid Ferrum synthesizing iron lithium phosphate is usually the iron phosphate of two water after pyrolytic, obtains anhydrous iron phosphate, after then mixing with lithium carbonate and glucose, after high temperature sintering, obtains LiFePO4.This technics comparing is complicated, and energy consumption is the highest, and the LiFePO4 primary particle obtained is big, and specific surface area is little, is unfavorable for big multiplying power discharging and the low temperature discharge of LiFePO4.
Summary of the invention
It is an object of the invention to overcome existing technological process complicated, energy consumption is high, the lithium iron phosphate particles obtained is big, specific surface area is little, it is unfavorable for big multiplying power discharging and the defect of low temperature discharge of LiFePO4, it is provided that the method for the LiFePO4 that a kind of synthesis ratio surface area multiplying power discharging big, big is good with low temperature performance.
Therefore, first aspect, the invention provides a kind of method preparing LiFePO4, the method comprises the following steps: in the presence of pore creating material, will be containing FePO4, the raw material of lithium source and carbon source is sintered.
Second aspect, the invention provides a kind of method preparing positive electrode, and the method includes: prepares LiFePO4 according to the inventive method, and is mixed with conductive agent by the LiFePO4 obtained.
The LiFePO4 obtained according to the present invention has the advantage that specific surface area multiplying power discharging big, big is good with low temperature performance.Additionally, using FePO4·xH2When O is as raw material, it is also possible to one-step synthesis LiFePO4, it is not necessary to decomposition and crystallization water in advance, simplifies the synthesis technique of LiFePO4, reduce the energy consumption in building-up process.Especially, the specific surface area of the LiFePO4 obtained according to the preferred embodiment for the present invention can be more than 20m2/g。
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that detailed description of the invention described herein is merely to illustrate and explains the present invention, it is not limited to the present invention.
End points and any value of scope disclosed in this article are not limited to this accurate scope or value, and these scopes or value should be understood to the value comprised close to these scopes or value.For numerical range, between the endpoint value of each scope, between the endpoint value of each scope and single point value, and individually can obtain one or more new numerical range with combination with one another between point value, these numerical rangies should be considered the most specifically to disclose.
In the present invention, in the case of illustrating on the contrary, the FePO related to4, lithium source, carbon source and pore creating material weight all in terms of butt;The term " gram specific capacity " used refers to total electricity that the battery active material of unit mass can be released, and its value is the biggest, illustrates that the electricity that battery material can store is the biggest.
Comprise the following steps according to the method preparing LiFePO4 that the present invention provides: in the presence of pore creating material, will be containing FePO4, the raw material of lithium source and carbon source is sintered.
According to the present invention, kind and consumption to pore creating material have no particular limits, as long as the specific surface area of LiFePO4 can be promoted after distilling to obtain improving.Preferably, with FePO4Butt meter, described pore creating material and FePO4Weight ratio be 0.2-2:10 (arbitrary value as between 0.2:10,0.3:10,0.4:10,0.5:10,0.6:10,0.7:10,0.8:10,0.9:10,1:10,1.1:10,1.2:10,1.3:10,1.4:10,1.5:10,1.6:10,1.7:10,1.8:10,1.9:10,2:10 or aforementioned value).Described pore creating material is boiling point high (more than 150 DEG C) and the material easily distilled at temperature is less than 300 DEG C.Preferably, described pore creating material is provided by one or more in camphor, paracide and naphthalene.Wherein, camphor can be provided by natural camphor ball (commercially available).
According to the present invention, FePO4Can be iron phosphate pressed powder, it is preferable that FePO4By the FePO with water of crystallization4There is provided.
According to the present invention, kind and consumption to lithium source have no particular limits, as long as it can be with FePO4React and obtain LiFePO4.Preferably, in terms of elemental lithium, described lithium source and FePO4Mol ratio be 0.5-2:1 (arbitrary value as between 0.5:1,0.6:1,0.7:1,0.8:1,0.9:1,1:1,1.1:1,1.2:1,1.3:1,1.4:1,1.5:1,1.6:1,1.7:1,1.8:1,1.9:1,2:1 or aforementioned value), more preferably 0.5-1:1.Described lithium source can be various commonly used in the art containing Li+Ionic compound, it is preferable that described lithium source is one or more in lithium carbonate, Lithium hydrate and lithium nitrate.
According to the present invention, kind and consumption to carbon source have no particular limits, as long as can be coated with LiFePO4 is uniform.Preferably, with FePO4Butt meter, described carbon source and FePO4Weight ratio be 1-5:10 (arbitrary value as between 1:10,1.5:10,2:10,2.5:10,3:10,3.5:10,4:10,4.5:10,5:10 or aforementioned value), more preferably 1-2:10.Described carbon source can be one or more in monosaccharide (such as glucose), oligosaccharide (such as disaccharide) and polysaccharide (if molecular weight is the polysaccharide of 150000 to 600000).Preferably, one or more during described carbon source is glucose, sugarcane sugar and starch.
According to the present invention, in order to obtain the LiFePO4 of excellent performance, preferably, described method also includes: control before sintering the particle diameter of raw material below 300 mesh (such as 300-600 mesh), and moisture below 5 weight % (such as 0.1-5 weight %).It can be to pulverize (such as ball milling) and/or be dried (such as microwave drying and/or spray drying) that the particle diameter of control raw material and moisture meet the method for above-mentioned requirements.
According to the present invention, described sintering can be carried out under the normal condition of this area.Preferably, described sintering is carried out under an inert atmosphere, and the temperature of sintering is 300-800 DEG C, and the time of sintering is 2-13h.
It is highly preferred that the mode of sintering is 1-3h at being first placed in 300-400 DEG C, then 1-10h at being placed in 600-800 DEG C.
The method preparing LiFePO4 according to the present invention comprises the following steps:
(1) mixing is with the FePO of water of crystallization4, lithium source, carbon source and pore creating material, wherein, with FePO4Butt meter, described pore creating material and FePO4Weight ratio be 0.2-2:10, described pore creating material by camphor, paracide and naphthalene one or more provide, wherein, camphor can be provided by natural camphor ball (commercially available);In terms of elemental lithium, described lithium source and FePO4Mol ratio be 0.5-2:1, described lithium source is one or more in lithium carbonate, Lithium hydrate and lithium nitrate;Described carbon source and FePO4Weight ratio be 1-5:10, described carbon source is one or more in glucose, sugarcane sugar and starch, wherein FePO4Weight in terms of butt;
(2) carry out pulverizing and/or being dried by the mixing raw material that step (1) obtains so that mixing raw material particle diameter below 300 mesh (such as 300-600 mesh), and moisture below 5 weight % (such as 0.1-5 weight %);
(3) being placed under inert atmosphere be sintered processing, through step (2), the material that obtains, the temperature of sintering is 300-800 DEG C, and the time of sintering is 2-13h.
According to the present invention, the mode of described pulverizing can use the breaking method that this area is conventional, it is preferable that the mode of pulverizing is ball milling.It is highly preferred that described ball milling is carried out in ball grinder (such as planetary ball mill tank).The condition of ball milling can include that rotating speed is 100-200r/min, and the time is 1-10h.
More preferably, the mode of ball milling is wet grinding, and water is 0.5-2:1 (arbitrary value as between 0.5:1,0.6:1,0.7:1,0.8:1,0.9:1,1:1,1.1:1,1.2:1,1.3:1,1.4:1,1.5:1,1.6:1,1.7:1,1.8:1,1.9:1,2:1 or aforementioned value) with the weight ratio mixing raw material.
According to the present invention, described dry mode can use the drying means that this area is conventional, it is preferable that dry method is microwave drying and/or spray drying.In order to before making sintering, the moisture of raw material meets above-mentioned requirements, dry actual conditions can be selected by those skilled in the art, does not repeats them here.
According to the present invention, described in be sintered in atmosphere furnace carrying out.Preferably, atmosphere furnace is tube-type atmosphere furnace.Preferably, it is provided that the noble gas of inert atmosphere is nitrogen and/or argon.
According to the invention, it is further possible to the product obtained after sintering is crushed, be suitable to prepare the LiFePO4 product of positive electrode to obtain.
The method preparing positive electrode of the present invention includes preparing LiFePO4 according to the invention described above method, and is mixed with conductive agent by the LiFePO4 obtained.
According to the present invention, kind and consumption to conductive agent have no particular limits, as long as its weight ratio that can play electric action, conductive agent and LiFePO4 can be 0.5-2:20 (arbitrary value as between 0.5:20,0.6:20,0.7:20,0.8:20,0.9:20,1:20,1.1:20,1.2:20,1.3:20,1.4:20,1.5:20,1.6:20,1.7:20,1.8:20,1.9:20,2:20 or aforementioned value).Preferably, conductive agent is white carbon black.It is highly preferred that conductive agent is little granule conductive black.
According to the present invention, described method can also include mixing the LiFePO4 obtained, conductive agent with binding agent.Described binding agent can be various polymer commonly used in the art, such as polyvinylidene fluoride (pvdf).The weight ratio of described binding agent and LiFePO4 can be 0.5-2:20 (arbitrary value as between 0.5:20,0.6:20,0.7:20,0.8:20,0.9:20,1:20,1.1:20,1.2:20,1.3:20,1.4:20,1.5:20,1.6:20,1.7:20,1.8:20,1.9:20,2:20 or aforementioned value).
According to the present invention it is possible to be further used for preparing battery by the positive electrode that said method prepares.Such as, by the LiFePO4 obtained according to the present invention, little granule conductive black (Super-P) and binding agent (such as polyvinylidene fluoride, pvdf) mixing is as positive pole, Super-P is 0.5-2:20 with the weight ratio of LiFePO4, pvdf is 0.5-2:20 with the weight ratio of LiFePO4, lithium sheet, as negative pole, makes smear button cell.This smear button cell has preferably performance, and the smear button cell prepared by the LiFePO4 prepared according to the preferred embodiment for the present invention is at 2-3.8V, room temperature (23 DEG C) 0.5C, and gram specific capacity is 156-160mAh/g;Room temperature 5C, gram specific capacity is 146-149mAh/g;2-3.8V ,-10 DEG C, 0.5C, gram specific capacity is 124-128mAh/g;Low temperature discharge-10 DEG C/23 DEG C ratio is 77.5-82%.
Hereinafter will be described the present invention by embodiment.
In following example, the method preparing smear button cell is: by LiFePO4, conductive agent Super-P, binding agent pvdf and solvent N-methyl pyrilidone (NMP) according to the proportional arrangement form slurry of 86:7:7:150, single spreading is on smooth aluminium foil, and coated side density is 100g/m2, after drying, (solvent NMP volatilization) is through roll-in, compacted density to 2g/cm3;With special piercer, pole piece is washed into the positive plate of a diameter of 14mm the most again, has weighed the weight of each positive plate with analytical balance, and recorded data;Then by positive plate and a diameter of 16mm lithium sheet and the barrier film of a diameter of 19mm, in glove box, smear button cell it is assembled into.The method of test gram specific capacity is: use the test cabinet (BTS-2) of new Weir, according to multiplying power to be tested, the electric current setting electric discharge makes smear button cell just complete electric discharge (such as in required time, when multiplying power is 5C, required time is 0.2h, when multiplying power is 0.5C, required time is 2h), i.e. can obtain the test data (weight of the electric current × required time/positive plate of gram specific capacity=setting electric discharge) of gram specific capacity.
The natural camphor ball used in following example is song spirit tablet camphor ball (camphor content is 96 weight %);Super-P is purchased from Jitian Chemical Co., Ltd. of Shenzhen;Pvdf is purchased from Xiamen Zhong Wutou Import and Export Co., Ltd.;The method of test specific surface area is: use the JW-004A dynamic adsorption instrument of precise and tiny Gao Bo, Beijing science and technology company limited, it is first turned on computer software and adsorption instrument and preheats 0.5h, then prepared LiFePO4 is added in the sample U-tube of adsorption instrument, the LiFePO4 weight that record adds, then 150 DEG C of process 0.5h in the case of helium is protected, it is cooled to room temperature (25 DEG C), turn off helium, take out sample, the weight of record sample, then U-tube is inserted in adsorption instrument, in Dewar flask, add liquid nitrogen simultaneously, and allow U-tube leaching end in liquid nitrogen, open test software, start test, after having tested, i.e. can obtain specific surface area.
Embodiment 1
Weigh lithium carbonate 24.55g, FePO4·2H2O123.84g, glucose 18.05g, pore creating material (natural camphor ball) 10g, deionized water 135g, they after mix homogeneously, are added in 500mL planetary ball mill tank, with the rotating speed of 150r/min, obtain slurry after ball milling 5h in beaker.
Slurry is placed in microwave oven drying, and dried material moisture is 3 weight %, by dried material through ball mill pulverizing, crosses 300 eye mesh screens and is placed in tube-type atmosphere furnace, nitrogen atmosphere, is first warming up to 700 DEG C of sintering 10h after 350 DEG C of sintering 3h, obtains LiFePO4.
By LiFePO4 after laboratory room small-sized comminution by gas stream crusher machine, obtain LiFePO4 powder (specific surface area is shown in Table 1), be used for carrying out the performance test of material.
After the LiFePO4 powder obtained is made smear button cell, record the parameters such as battery gram specific capacity at different conditions as shown in table 1.
Embodiment 2
Weigh monohydrate lithium hydroxide 27.83g, FePO4·2H2O123.84g, sucrose 19.21g, pore creating material p-dichlorobenzene 6g, deionized water 150g, they after mix homogeneously, are added in 500mL planetary ball mill tank, with the rotating speed of 100r/min, obtain slurry after ball milling 10h in beaker.
Slurry is placed in microwave oven drying, and dried material moisture is 3 weight %, by dried material, through ball mill crushing, crosses 300 eye mesh screens and is placed in tube-type atmosphere furnace, nitrogen atmosphere, is first warming up to 600 DEG C of sintering 8h after 300 DEG C of sintering 2h, obtains LiFePO4.
By LiFePO4 after laboratory room small-sized comminution by gas stream crusher machine, obtain LiFePO4 powder (specific surface area is shown in Table 1), be used for carrying out the performance test of material.
After the LiFePO4 powder obtained is made smear button cell, record the parameters such as battery gram specific capacity at different conditions as shown in table 1.
Embodiment 3
Weigh single water lithium nitrate 58g, FePO4·2H2O123.84g, starch 21.65g, pore creating material naphthalene 17g, deionized water 150g, they after mix homogeneously, are added in 500mL planetary ball mill tank, with the rotating speed of 300r/min, obtain slurry after ball milling 2h in beaker.
Slurry is placed in microwave oven drying, and dried material moisture is 3 weight %, by dried material, through ball mill crushing, crosses 300 eye mesh screens and is placed in tube-type atmosphere furnace, nitrogen atmosphere, is first warming up to 800 DEG C of sintering 6h after 400 DEG C of sintering 1h, obtains LiFePO4.
By LiFePO4 after laboratory room small-sized comminution by gas stream crusher machine, obtain LiFePO4 powder (specific surface area is shown in Table 1), be used for carrying out the performance test of material.
After the LiFePO4 powder obtained is made smear button cell, record the parameters such as battery gram specific capacity at different conditions as shown in table 1.
Embodiment 4
According to the method for embodiment 1, except for the difference that, the pore creating material natural camphor ball of addition is 3g.After tested, the specific surface area of product phosphoric acid ferrum lithium powder is shown in Table 1.Record the parameters such as gram specific capacity under battery different condition as shown in table 1.
Embodiment 5
According to the method for embodiment 1, except for the difference that, the pore creating material natural camphor ball of addition is 1g.After tested, the specific surface area of product phosphoric acid ferrum lithium powder is shown in Table 1.Record the parameters such as gram specific capacity under battery different condition as shown in table 1.
Comparative example 1
According to the method for embodiment 1, except for the difference that, pore creating material is not added.After tested, the specific surface area of product phosphoric acid ferrum lithium powder is shown in Table 1.Record the parameters such as battery gram specific capacity at different conditions as shown in table 1.
Table 1
Comparing embodiment 1 can be seen that with the result of comparative example 1, the LiFePO4 specific surface area multiplying power discharging little, big prepared in comparative example 1 is low with low temperature discharge rate, and the LiFePO4 specific surface area multiplying power discharging big, big prepared in the presence of pore creating material in embodiment 1 is high with low temperature discharge rate, every technique effect will be substantially better than the result of comparative example 1.
Comparing embodiment 1 with the result of embodiment 5 it can be seen that the specific surface area of LiFePO4, the big multiplying power discharging that obtain when the consumption of pore creating material is in the range of preferably are the most excellent with low temperature performance.
The preferred embodiment of the present invention described in detail above; but, the present invention is not limited to the detail in above-mentioned embodiment, in the technology concept of the present invention; technical scheme can be carried out multiple simple variant, these simple variant belong to protection scope of the present invention.
It is further to note that, each concrete technical characteristic described in above-mentioned detailed description of the invention, in the case of reconcilable, can be combined by any suitable means, in order to avoid unnecessary repetition, various possible compound modes are illustrated by the present invention the most separately.
Additionally, can also carry out combination in any between the various different embodiment of the present invention, as long as it is without prejudice to the thought of the present invention, it should be considered as content disclosed in this invention equally.

Claims (10)

1. the method preparing LiFePO4, it is characterised in that the method includes: in the presence of pore creating material, will be containing FePO4, the raw material of lithium source and carbon source is sintered.
Method the most according to claim 1, wherein, with FePO4Butt meter, described pore creating material and FePO4Weight ratio be 0.2-2:10, it is preferable that described pore creating material by camphor, paracide and naphthalene one or more provide.
Method the most according to claim 1 and 2, wherein, FePO4By the FePO with water of crystallization4There is provided.
4. according to the method described in any one in claim 1-3, wherein, in terms of elemental lithium, described lithium source and FePO4Mol ratio be 0.5-2:1, it is preferable that described lithium source is one or more in lithium carbonate, Lithium hydrate and lithium nitrate.
5. according to the method described in any one in claim 1-4, wherein, with FePO4Butt meter, described carbon source and FePO4Weight ratio be 1-5:10, it is preferable that described carbon source is one or more in glucose, sugarcane sugar and starch.
Method the most according to claim 1, wherein, described method also includes: before controlling to sinter, the particle diameter of raw material is below 300 mesh, and moisture is below 5 weight %.
7. according to the method described in claim 1 or 6, wherein, described sintering is carried out under an inert atmosphere, and the temperature of sintering is 300-800 DEG C, and the time of sintering is 2-13h.
8. the method preparing LiFePO4, it is characterised in that the method comprises the following steps:
(1) mixing is with the FePO of water of crystallization4, lithium source, carbon source and pore creating material, wherein, with FePO4Butt meter, described pore creating material and FePO4Weight ratio be 0.2-2:10, described pore creating material by camphor, paracide and naphthalene one or more provide;In terms of elemental lithium, described lithium source and FePO4Mol ratio be 0.5-2:1, described lithium source is one or more in lithium carbonate, Lithium hydrate and lithium nitrate;Described carbon source and FePO4Weight ratio be 1-5:10, described carbon source is one or more in glucose, sugarcane sugar and starch, wherein FePO4Weight in terms of butt;
(2) carry out pulverizing and/or being dried by the mixing raw material that step (1) obtains so that the particle diameter of mixing raw material is below 300 mesh, and moisture is below 5 weight %;
(3) being placed under inert atmosphere be sintered processing, through step (2), the material that obtains, the temperature of sintering is 300-800 DEG C, and the time of sintering is 2-13h.
Method the most according to claim 8, wherein, the mode of described pulverizing is ball milling, and the condition of ball milling includes that rotating speed is 100-300r/min, and the time is 1-10h;
Preferably, described dry mode is microwave drying and/or spray drying;
Preferably, it is provided that the noble gas of inert atmosphere is nitrogen and/or argon.
10. the method preparing positive electrode, it is characterised in that the method includes: prepare LiFePO4 according to the method described in any one in claim 1-9, and the LiFePO4 obtained is mixed with conductive agent.
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CN110931726A (en) * 2019-10-25 2020-03-27 惠州锂威新能源科技有限公司 Lithium titanate negative electrode composite material, preparation method thereof and lithium ion battery
CN111969178A (en) * 2019-05-20 2020-11-20 贵州安达科技能源股份有限公司 Lithium iron phosphate battery positive electrode slurry and preparation method thereof
CN113745481A (en) * 2021-08-30 2021-12-03 大连中比动力电池有限公司 Lithium iron phosphate/carbon composite material, preparation method thereof, positive pole piece and lithium ion battery
CN115084523A (en) * 2022-06-28 2022-09-20 肇庆小鹏汽车有限公司 Electrode slurry and preparation method and application thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101304091A (en) * 2007-05-09 2008-11-12 丰田自动车株式会社 Catalyst powder preparation, catalyst powder and catalyst layer of fuel cell
US20090170003A1 (en) * 2007-12-27 2009-07-02 Industrial Technology Research Institute Cathodal materials for lithium cells
CN102013475A (en) * 2010-10-22 2011-04-13 秦波 Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101304091A (en) * 2007-05-09 2008-11-12 丰田自动车株式会社 Catalyst powder preparation, catalyst powder and catalyst layer of fuel cell
US20090170003A1 (en) * 2007-12-27 2009-07-02 Industrial Technology Research Institute Cathodal materials for lithium cells
CN102013475A (en) * 2010-10-22 2011-04-13 秦波 Method for preparing porous spherical Li(1-x)MxFe(1-y)Ny(PO4)([3+(alpha-1)x+(beta-2) y]/3)/C material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111969178A (en) * 2019-05-20 2020-11-20 贵州安达科技能源股份有限公司 Lithium iron phosphate battery positive electrode slurry and preparation method thereof
CN110931726A (en) * 2019-10-25 2020-03-27 惠州锂威新能源科技有限公司 Lithium titanate negative electrode composite material, preparation method thereof and lithium ion battery
CN113745481A (en) * 2021-08-30 2021-12-03 大连中比动力电池有限公司 Lithium iron phosphate/carbon composite material, preparation method thereof, positive pole piece and lithium ion battery
CN115084523A (en) * 2022-06-28 2022-09-20 肇庆小鹏汽车有限公司 Electrode slurry and preparation method and application thereof

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