CN107369832A - A kind of LiFePO4Positive electrode synthetic method - Google Patents

A kind of LiFePO4Positive electrode synthetic method Download PDF

Info

Publication number
CN107369832A
CN107369832A CN201610318587.XA CN201610318587A CN107369832A CN 107369832 A CN107369832 A CN 107369832A CN 201610318587 A CN201610318587 A CN 201610318587A CN 107369832 A CN107369832 A CN 107369832A
Authority
CN
China
Prior art keywords
source
cnt
lithium
synthetic method
time
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610318587.XA
Other languages
Chinese (zh)
Inventor
刘熙林
钱龙
黎明旭
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen OptimumNano Energy Co Ltd
Original Assignee
Shenzhen OptimumNano Energy Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shenzhen OptimumNano Energy Co Ltd filed Critical Shenzhen OptimumNano Energy Co Ltd
Priority to CN201610318587.XA priority Critical patent/CN107369832A/en
Publication of CN107369832A publication Critical patent/CN107369832A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • H01M4/02—Electrodes composed of, or comprising, active material
    • 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
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Landscapes

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

Abstract

The invention discloses a kind of LiFePO4Positive electrode synthetic method, comprises the following steps：(1) concentrated nitric acid and CNT are mixed, then forms suspension using ultrasonic wave is scattered；Suspension is subjected to oil bath heating under stirring and flowed back, it is standby that grinding is taken out to washing after natural cooling, after being dried after filtering；(2) source of iron and phosphorus source are stoichiometrically weighed, concentration mixed solution is configured to, H2O2 is added in mixed solution；CNT obtained by weighing step (1) is added in mixed solution together to be placed in reactor, stir and heat and reacted, reaction will precipitate scrubbed, filtering and be placed in drying box and be dried after terminating, it is placed in Muffle furnace and is heat-treated after grinding, obtains ferrophosphorus oxide precursor；(3) presoma obtained by step (2) is mixed with lithium source, and adds carbon source and be placed in ball mill, added after dispersant carries out ball milling and be put into after drying, grinding in atmosphere furnace, sintered heat insulating produces LiFePO4Positive electrode.

Description

A kind of LiFePO4Positive electrode synthetic method
Technical field
The invention belongs to technical field of lithium batteries, more particularly to a kind of LiFePO4Positive electrode synthesizes Method.
Background technology
The increasingly rise of new-energy automobile industry has higher and higher requirement for lithium ion battery, Using LiFePO4Have many advantages, such as anode material for lithium-ion batteries：Without precious metal member Element, raw material resources enrich, cheap, and production cost is low；Material crystal structure is stable, peace Full better performances；Good cycle；High-temperature behavior and heat endurance are better than other positive electrodes；Nothing Poison, it is environmentally friendly.LiFePO4Because becoming domestic power battery material with above-mentioned advantage Preferred material；But because its tap density, compacted density and operating voltage are compared to other Positive electrode (such as LiCoO2、LiMn2O4、LiNi1/3Mn1/3Co1/3O2Deng) relatively low so that The energy density of battery is relatively low.In order to meet that user's is easy-to-use, in the market starts to push away in recent years Row quick charging battery, this is for LiFePO4High rate performance propose higher requirement, and positive pole material The electric conductivity of material itself is to influence the principal element of battery high rate performance.Prior art uses single substantially Pure carbon material and LiFePO4Material carries out Surface coating or doping vario-property, simple carbon coating LiFePO4Material lift material conductivity it is limited in one's ability, carbon coating can improve LiFePO4 The electric conductivity of intergranular, but the electric conductivity inside material granule is poor, activity inside particle under big multiplying power Substance migration rate is relatively low, influences the performance of its capacity.
The content of the invention
It is an object of the invention to for the technical problem present on, there is provided one kind causes LiFePO4The better LiFePO of positive electrode electric conductivity4Positive electrode synthetic method.
In order to solve the above technical problems, the present invention provides a kind of LiFePO4Positive electrode synthetic method, Comprise the following steps：
(1) concentrated nitric acid that concentration is 60%-70% is mixed with CNT, then Suspension is formed using ultrasonic wave is scattered；Suspension is carried out into oil bath heating under stirring to go forward side by side Row flows back, and it is 6.5~7.5 suspension to be washed after natural cooling to pH value range, filtering It is standby that grinding is taken out after CNT of the gained after concentrated nitric acid is acidified is dried afterwards；
(2) mole of source of iron and phosphorus source, wherein iron atom and phosphorus atoms is stoichiometrically weighed Than the mixed solution for for 1/1, being configured to 0.5~2.0mol/L of concentration, added in mixed solution with Source of iron 1/1~1/1.3 H2O2 for being in molar ratio；Weigh CNT obtained by step (1) together It is added in mixed solution and mixed solution is placed in reactor after ultrasonic wave is scattered, stirring is simultaneously Heating is reacted, and reaction will precipitate scrubbed, filtering and be placed in drying box and be dried after terminating, It is placed in Muffle furnace and is heat-treated after grinding, obtains the ferrophosphorus oxide using CNT as core Presoma；
(3) presoma obtained by step (2) and lithium source Li/Fe 1.0/1~1.1/1 are entered in molar ratio Row mixing, and adds carbon source and is placed in ball mill, add dispersant carry out after ball milling through drying, It is put into after grinding in atmosphere furnace, is passed through inert gas and carries out being incubated necessarily under certain sintering temperature Time is to be able to LiFePO of the CNT for core and outside carbon coated4Positive electrode.
The beneficial effects of the invention are as follows：The battery electricity of LiFePO 4 material assembling synthesized by the present invention Constant current ratio of the pond under different multiplying charging is higher, and the mean voltage under different multiplying electric discharge is also more Height, shows more preferable high rate performance, and main cause is to use CNT to lithium iron phosphate particles It is doped, while carbon coating is carried out on surface, particle inside and particle surface can be greatly improved Conductive capability, reduce polarization of the battery in different multiplying charge and discharge process, improve times of battery Rate performance.
Brief description of the drawings
Fig. 1 is LiFePO of the present invention4LiFePO prepared by positive electrode synthetic method4Positive electrode Granular model figure.
Fig. 2 is LiFePO of the present invention4LiFePO prepared by positive electrode synthetic method4Positive electrode SEM schemes.
Fig. 3 is LiFePO of the present invention4LiFePO prepared by positive electrode synthetic method4Positive electrode XRD.
Fig. 4 is LiFePO of the present invention4LiFePO prepared by positive electrode synthetic method4Positive electrode institute Assemble LiFePO prepared by battery and existing method comparative example 14The electricity assembled described in positive electrode Cyclic curve figure of the pond under 25 DEG C ± 5 DEG C, 2.0-3.65V, 3C multiplying powers.
Embodiment
In order that the purpose of the present invention, technical scheme and advantageous effects become apparent from understanding, with Lower combination the drawings and specific embodiments, the present invention will be described in further detail.It should be understood that , the embodiment described in this specification is not just for the sake of explaining the present invention In order to limit the present invention.
The present invention provides a kind of LiFePO4Positive electrode synthetic method, specific implementation step are as follows：
(1) concentrated nitric acid that concentration is 60%-70% is mixed with CNT, then Suspension is formed using ultrasonic wave is scattered；Suspension is carried out into oil bath heating under stirring to go forward side by side Row flows back, and it is 6.5~7.5 suspension to be washed after natural cooling to pH value range, filtering It is standby that grinding is taken out after CNT of the gained after concentrated nitric acid is acidified is dried afterwards；
(2) mole of source of iron and phosphorus source, wherein iron atom and phosphorus atoms is stoichiometrically weighed Than the mixed solution for for 1/1, being configured to 0.5~2.0mol/L of concentration, added in mixed solution with Source of iron 1/1~1/1.3 H for being in molar ratio2O2；Weigh CNT obtained by step (1) together It is added in mixed solution and mixed solution is placed in reactor after ultrasonic wave is scattered, stirring is simultaneously Heating is reacted, and reaction will precipitate scrubbed, filtering and be placed in drying box and be dried after terminating, It is placed in Muffle furnace and is heat-treated after grinding, obtains the ferrophosphorus oxide using CNT as core Presoma, it is designated as FPO-C.
(3) by presoma FPO-C obtained by step (2) and lithium source Li/Fe in molar ratio 1.0/1~ 1.1/1 is mixed, and is added carbon source and be placed in ball mill, after adding dispersant progress ball milling It is put into after drying, grinding in atmosphere furnace, is passed through inert gas and is carried out under certain sintering temperature Held for some time is to be able to LiFePO of the CNT for core and outside carbon coated4Positive pole material Material, is designated as LFP/C-C.
Above LiFePO4Positive electrode synthetic method, wherein：
CNT described in step (1) can be in single-walled carbon nanotube or many walls nanotube One or two kinds of combination, CNT accounts for the LiFePO finally synthesized4Positive electrode 0.5%~2.0%；The mixing time is 10~40min (minute), and ultrasonic dispersing time is 10min~30min；Described oil bath temperature is 110~130 DEG C, and return time is 8~12h； Described drying temperature is 70~120 DEG C, and drying time is 8~24h (hour).
Source of iron described in step (2) is ferrous sulfate, ferrous oxalate, frerrous chloride, nitric acid One kind or two kinds and combination of the above in iron, ferric phosphate, di-iron trioxide；Phosphorus source be phosphoric acid, One kind or two kinds and combination of the above in ammonium dihydrogen phosphate, lithium dihydrogen phosphate；Described ultrasonic wavelength-division It is 10~30min to dissipate the time；Reaction temperature in the reactor is 85~100 DEG C, during reaction Between be 8~24h；The drying box temperature is 70~120 DEG C, and drying time is 8~24h；It is described Heat treatment temperature is 400~550 DEG C, and heat treatment time is 3~6h.
Lithium source described in step (3) is lithium carbonate, lithium hydroxide, lithium acetate, biphosphate One kind or two kinds and combination of the above in lithium, lithium oxalate；The carbon source be glucose, polyvinyl alcohol, One kind in phenolic resin, epoxy resin, polystyrene, polyethylene glycol, starch, citric acid or Two kinds and the combination of the above, carbon source ratio are theoretical L iFePO4The 15%~20% of quality；It is described Dispersant be absolute ethyl alcohol, the combination of deionized water, one kind in acetone or two kinds and the above； The Ball-milling Time is 3~6h；Described inert gas is high pure nitrogen or argon gas；The burning Junction temperature is 600 DEG C~800 DEG C, and soaking time is 8~24h.
Embodiment 1：
(1) 4g CNTs are weighed to be added in the concentrated nitric acid solution that 100mL concentration is 65% 25min is mixed, ultrasonic wave is then carried out and disperses 20min, form suspension.By suspension Oil bath heating is carried out under stirring to 110 DEG C and carries out backflow 10h, to outstanding after natural cooling Turbid is washed to pH=7.0, is carried out CNT of the gained after concentrated nitric acid is acidified after filtering It is standby that grinding is taken out after drying；
(2) by FeSO4And H3PO4Stoichiometrically weigh, be configured to 1mol/L FeSO4 And H3PO4Mixed solution, in mixed solution add and FeSO4It is 1 in molar ratio:1.2 H2O2.CNT obtained by step (1) is added in mixed solution together and carries out ultrasonic wavelength-division Mixed solution is placed in reactor after dissipating, stirs and heats mixing liquid temperature in maintenance reaction kettle For 95 DEG C, 10h is reacted, reaction will precipitate scrubbed, filtering and be placed in 100 DEG C of drying boxes after terminating In be dried 8h, take out and 500 DEG C are placed in Muffle furnace after grinding carry out heat treatment 4h, obtain with CNT is the ferrophosphorus oxide precursor of core, is designated as FPO-C.
(3) by presoma FPO-C and Li obtained by step (2)2CO3It is by Li/Fe mol ratios 1.05/1 mixing, and add theoretical L iFePO4The glucose of quality 15% is placed in ball mill, is added Enter suitable alcohols to carry out after ball milling 4h being put into atmosphere furnace after drying, grinding as dispersant, Be passed through the nitrogen of certain throughput, be incubated at 650 DEG C 10h be able to CNT as core and The LiFePO of outside carbon coated4Positive electrode, it is designated as LFP/C-C.
Embodiment 2：
(1) 4g CNTs are weighed to be added in the concentrated nitric acid solution that 100mL concentration is 65% 25min is mixed, ultrasonic wave is then carried out and disperses 20min, form suspension.By suspension Oil bath heating is carried out under stirring to 110 DEG C and carries out backflow 10h, to outstanding after natural cooling Turbid is washed to pH=7.0, is carried out CNT of the gained after concentrated nitric acid is acidified after filtering It is standby that grinding is taken out after drying；
(2) by Fe (NO3)3·9H2O and NH4H2PO4Stoichiometrically weigh, be configured to 1mol/L FeSO4And H3PO4Mixed solution, in mixed solution add with Fe(NO3)3·9H2O is 1 in molar ratio:1.15 H2O2.CNT one obtained by step (1) Rise to be added in mixed solution and mixed solution is placed in reactor after ultrasonic wave is scattered, stir And it is 95 DEG C to heat mixing liquid temperature in maintenance reaction kettle, 12h is reacted, reaction will be heavy after terminating Scrubbed, filtering of forming sediment is placed in 100 DEG C of drying boxes and 8h is dried, and Muffle is placed in after taking out grinding 500 DEG C carry out heat treatment 4h in stove, obtain the ferrophosphorus oxide precursor using CNT as core, It is designated as FPO-C.
(3) by presoma FPO-C and Li obtained by step (2)2CO3It is by Li/Fe mol ratios 1.05/1 mixing, and add theoretical L iFePO4The polyvinyl alcohol of quality 20% is placed in ball mill, Add suitable alcohols carried out as dispersant after ball milling 4h through drying, grind after be put into atmosphere furnace, Be passed through the nitrogen of certain throughput, be incubated at 700 DEG C 12h be able to CNT as core and The LiFePO of outside carbon coated4Positive electrode, it is designated as LFP/C-C.
Comparative example 1：
(1) by FeSO4And H3PO4Stoichiometrically weigh, be configured to 1mol/L FeSO4 And H3PO4Mixed solution, in mixed solution add and FeSO4It is 1 by certain mol proportion:1.2 H2O2.Mixed solution is placed in reactor, stirs and heats mixing liquid in maintenance reaction kettle Temperature is 95 DEG C, reacts 10h, reaction will be precipitated after terminating scrubbed, filtering be placed in 100 DEG C it is dry It is dried 8h in dry case, takes out and 500 DEG C are placed in Muffle furnace after grinding carry out heat treatment 4h, obtain To ferrophosphorus oxide precursor, FPO is designated as.
(2) by presoma FPO-C and Li obtained by step (2)2CO3It is by Li/Fe mol ratios 1.05/1 mixing, and add theoretical L iFePO4The glucose of quality 20% is placed in ball mill, is added Enter suitable alcohols to carry out after ball milling 4h being put into atmosphere furnace after drying, grinding as dispersant, The nitrogen of certain throughput is passed through, 12h is incubated at 700 DEG C and obtains the LiFePO of outside carbon coated4 Positive electrode, it is designated as LFP/C.The LiFePO of the gained of comparative example 14Positive electrode is different from above-mentioned The LiFePO of embodiment 1 and embodiment 2, the i.e. gained of comparative example 14Positive electrode only has outside wrap Carbon is covered, and carbon-free nanoscale pipe is as core.
Using target product prepared in above-described embodiment 1 and comparative example 1 as positive electrode, It is 90 by the mass ratio of Zheng poles Cai Liao ︰ Dao electricity Tan Hei ︰ polyvinylidene fluoride:5:5 are made slurry coating Positive plate is made on aluminium foil, using Delanium as negative material, Shi Mo ︰ conductive blacks are made by people ︰ LA133 mass ratio is 94:3:3 are made slurry coated in negative plate is made on copper foil, with volume Than for 1:1:1 EC/DEC/DMC 1mol/L LiPF6For electrolyte, 32650 are assembled into Full battery carries out high rate performance test and cycle performance test after preliminary filling, high temperature ageing, partial volume.
Table 1 is is assembled discharge and recharge tables of data of the battery under 2.0-3.65V, different multiplying.
Table 1
As can be seen from Table 1, the battery assembled using the LiFePO 4 material synthesized by the present invention is same Comparative example 1 is compared, and constant current ratio of the battery under different multiplying charging is higher, is discharged in different multiplying Under mean voltage it is also higher, show more preferable high rate performance, main cause is to LiFePO4 Particle is doped using CNT, while carries out carbon coating on surface, can be greatly improved Intragranular portion and the conductive capability of particle surface, reduce pole of the battery in different multiplying charge and discharge process Change, improve the high rate performance of battery.
As shown in Figure 1, it with CNT 1 is kernel that material designed by the present invention, which is, LiFePO4 2 homoepitaxials, finally coat one layer of carbon coating layer 3 in the outer surface of LiFePO4 2 and form three with this Rotating fields.
As shown in Figure 2, material primary particle particle diameter prepared by the present invention is at 0.5-1 μm, Duo Geyi Secondary particle agglomeration is into second particle, and the overall dispersiveness of material is preferably.
From the figure 3, it may be seen that the XRD diffraction maximums of material prepared by the present invention match with standard card, Exist without other miscellaneous peaks, show that the material synthesized by the present invention has olivine structural, belong to Pnma space groups.
As seen from Figure 4, had as the battery that the LiFePO 4 material synthesized by the present invention assembles Excellent high rate charge-discharge cycle performance, 500 weeks capability retentions of 3C circulations reach 97.36%, and 500 weeks capability retentions of battery 3C circulations are only 90.33% in comparative example 1.
The beneficial effects of the invention are as follows：
1st, the battery assembled using LiFePO 4 material synthesized by the present invention is had closes than common process Into the more preferable big circulation stability of LiFePO 4 material assembling battery, common process synthesis LiFePO 4 material, which assembles battery 500 weeks capability retentions are circulated under 3C multiplying powers, is only 90.33%, the battery assembled using the LiFePO 4 material synthesized by the present invention is followed under 3C multiplying powers 500 weeks capability retentions of ring reach 97.36%；
2nd, the battery assembled using LiFePO 4 material synthesized by the present invention is synthesized with common process LiFePO 4 material assembling battery is compared, and is had higher charging constant current ratio under equal multiplying power and is put Electric mean voltage, show more preferable high rate performance.
Embodiments of the present invention are the foregoing is only, not thereby limit the patent model of the present invention Enclose, every equivalent structure made using description of the invention and accompanying drawing content or equivalent process are become Change, or be directly or indirectly used in other related technical areas, be similarly included in the present invention's In scope of patent protection.

Claims (8)

  1. A kind of 1. LiFePO4Positive electrode synthetic method, comprises the following steps：
    (1) concentrated nitric acid that concentration is 60%-70% is mixed with CNT, then Suspension is formed using ultrasonic wave is scattered；Suspension is carried out into oil bath heating under stirring to go forward side by side Row flows back, and it is 6.5~7.5 suspension to be washed after natural cooling to pH value range, filtering It is standby that CNT after gained is acidified afterwards takes out grinding after being dried；
    (2) mole of source of iron and phosphorus source, wherein iron atom and phosphorus atoms is stoichiometrically weighed Than the mixed solution for for 1/1, being configured to 0.5~2.0mol/L of concentration, added in mixed solution with Source of iron 1/1~1/1.3 H2O2 for being in molar ratio；Weigh CNT obtained by step (1) together It is added in mixed solution and mixed solution is placed in reactor after ultrasonic wave is scattered, stirring is simultaneously Heating is reacted, and reaction will precipitate scrubbed, filtering and be placed in drying box and be dried after terminating, It is placed in Muffle furnace and is heat-treated after grinding, obtains the ferrophosphorus oxide using CNT as core Presoma；
    (3) presoma obtained by step (2) and lithium source Li/Fe 1.0/1~1.1/1 are entered in molar ratio Row mixing, and adds carbon source and is placed in ball mill, add dispersant carry out after ball milling through drying, It is put into after grinding in atmosphere furnace, is passed through inert gas and carries out being incubated necessarily under certain sintering temperature Time is to be able to LiFePO of the CNT for core and outside carbon coated4Positive electrode.
  2. 2. LiFePO4 positive electrodes synthetic method as claimed in claim 1, it is characterised in that： CNT described in step (1) can be one in single-walled carbon nanotube or many walls nanotube Kind or two kinds of combination, CNT account for the LiFePO finally synthesized4The 0.5% of positive electrode~ 2.0%；The mixing time is 10~40min, and ultrasonic dispersing time is 10min~30min； Described oil bath temperature is 110~130 DEG C, and return time is 8~12h；Described drying temperature For 70~120 DEG C, drying time is 8~24h.
  3. 3. LiFePO4 positive electrodes synthetic method as claimed in claim 2, it is characterised in that： In step (1), concentration of nitric acid 65% mixes 25min, and ultrasonic dispersing time is 20min；Oil bath temperature is 110 DEG C；Return time is 10h；PH=7.0.
  4. 4. LiFePO4 positive electrodes synthetic method as claimed in claim 1, it is characterised in that： Source of iron described in step (2) is ferrous sulfate, ferrous oxalate, frerrous chloride, ferric nitrate, One kind or two kinds and combination of the above in ferric phosphate, di-iron trioxide；Phosphorus source is phosphoric acid, phosphorus One kind or two kinds and combination of the above in acid dihydride ammonium, lithium dihydrogen phosphate；Described ultrasonic wave disperses Time is 10~30min；Reaction temperature in the reactor is 85~100 DEG C, the reaction time For 8~24h；The drying box temperature is 70~120 DEG C, and drying time is 8~24h；The heat Treatment temperature is 400~550 DEG C, and heat treatment time is 3~6h.
  5. 5. LiFePO4 positive electrodes synthetic method as claimed in claim 4, it is characterised in that： The source of iron is ferrous sulfate, and phosphorus source is phosphoric acid.
  6. 6. LiFePO4 positive electrodes synthetic method as claimed in claim 4, it is characterised in that： The source of iron is ferric nitrate, and phosphorus source is ammonium dihydrogen phosphate.
  7. 7. LiFePO4 positive electrodes synthetic method as claimed in claim 1, it is characterised in that： Lithium source described in step (3) is lithium carbonate, lithium hydroxide, lithium acetate, lithium dihydrogen phosphate, One kind or two kinds and combination of the above in lithium oxalate；The carbon source is glucose, polyvinyl alcohol, phenol One kind in urea formaldehyde, epoxy resin, polystyrene, polyethylene glycol, starch, citric acid or two The combination of kind and the above, carbon source ratio is theoretical L iFePO4The 15%~20% of quality；Described Dispersant is the combination of absolute ethyl alcohol, deionized water, one kind in acetone or two kinds and the above；Institute It is 3~6h to state Ball-milling Time；Described inert gas is high pure nitrogen or argon gas；The sintering Temperature is 600 DEG C~800 DEG C, and soaking time is 8~24h.
  8. 8. LiFePO4 positive electrodes synthetic method as claimed in claim 7, it is characterised in that： Lithium source is lithium carbonate.
CN201610318587.XA 2016-05-12 2016-05-12 A kind of LiFePO4Positive electrode synthetic method Pending CN107369832A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610318587.XA CN107369832A (en) 2016-05-12 2016-05-12 A kind of LiFePO4Positive electrode synthetic method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610318587.XA CN107369832A (en) 2016-05-12 2016-05-12 A kind of LiFePO4Positive electrode synthetic method

Publications (1)

Publication Number Publication Date
CN107369832A true CN107369832A (en) 2017-11-21

Family

ID=60304100

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610318587.XA Pending CN107369832A (en) 2016-05-12 2016-05-12 A kind of LiFePO4Positive electrode synthetic method

Country Status (1)

Country Link
CN (1) CN107369832A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109126816A (en) * 2018-09-20 2019-01-04 哈尔滨工业大学 The preparation method and application of order mesoporous perovskite catalyst
CN110021752A (en) * 2019-01-24 2019-07-16 湖北锂诺新能源科技有限公司 A kind of lithium, aluminium and fluorin-doped lithium iron phosphate positive material and preparation method
CN111740113A (en) * 2020-07-01 2020-10-02 中南大学 Preparation method of lithium iron phosphate/carbon nanotube composite positive electrode material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101621121A (en) * 2008-07-04 2010-01-06 合肥国轩高科动力能源有限公司 Method for preparing high-power lithium iron phosphate composite materials
CN101714627A (en) * 2008-10-08 2010-05-26 中国科学院金属研究所 Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof
CN102437334A (en) * 2011-11-23 2012-05-02 陕西科技大学 Microwave hydrothermal synthesizing method for carbon nanotube/LiFePO4 lithium ion battery anode material
CN102569796A (en) * 2012-01-17 2012-07-11 东南大学 Preparation method of lithium iron phosphate/carbon nanotube composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101621121A (en) * 2008-07-04 2010-01-06 合肥国轩高科动力能源有限公司 Method for preparing high-power lithium iron phosphate composite materials
CN101714627A (en) * 2008-10-08 2010-05-26 中国科学院金属研究所 Carbon nanotube/lithium iron phosphate composite positive electrode material and in situ preparation method thereof
CN102437334A (en) * 2011-11-23 2012-05-02 陕西科技大学 Microwave hydrothermal synthesizing method for carbon nanotube/LiFePO4 lithium ion battery anode material
CN102569796A (en) * 2012-01-17 2012-07-11 东南大学 Preparation method of lithium iron phosphate/carbon nanotube composite material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109126816A (en) * 2018-09-20 2019-01-04 哈尔滨工业大学 The preparation method and application of order mesoporous perovskite catalyst
CN110021752A (en) * 2019-01-24 2019-07-16 湖北锂诺新能源科技有限公司 A kind of lithium, aluminium and fluorin-doped lithium iron phosphate positive material and preparation method
CN110021752B (en) * 2019-01-24 2022-10-25 湖北锂诺新能源科技有限公司 Lithium, aluminum and fluorine co-doped lithium iron phosphate cathode material and preparation method thereof
CN111740113A (en) * 2020-07-01 2020-10-02 中南大学 Preparation method of lithium iron phosphate/carbon nanotube composite positive electrode material

Similar Documents

Publication Publication Date Title
CN102244241B (en) Preparation method of lithium iron phosphate composite material modified by lithium pyrophosphate
CN105428648B (en) A kind of preparation method of battery anode material of lithium iron phosphate
CN102623708A (en) Preparation method of lithium vanadium phosphate (Li3V2(PO4)3)/graphene composite material for positive electrode of lithium ion battery
CN106654218A (en) Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and lithium ion battery
CN101237043A (en) Method for making ferrous lithium phosphate/carbon compound material of high active disorderly ferric phosphate
CN101699639A (en) Method for preparing carbon-coated nano-grade lithium iron phosphate composite anode material
CN101339992B (en) Preparation of lithium ionic cell positive electrode material vanadium lithium silicate
CN102842713A (en) Phosphate-coated nano-grade lithium iron phosphate cathode material and preparation method thereof
CN104037413A (en) Preparation method of positive electrode material (carbon-coated iron-manganese-lithium phosphate) of lithium ion battery
CN102013489A (en) Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof
CN108039458A (en) A kind of sodium-ion battery positive material and its preparation method and application
CN103050698A (en) Vanadium lithium iron phosphate anode material and preparation method thereof
CN103956491B (en) A kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium and preparation method thereof
CN107369832A (en) A kind of LiFePO4Positive electrode synthetic method
CN110085862A (en) A kind of sode cell electrode material Na1+xFexTi2-x(PO4)3And its preparation method and application
CN106340620A (en) Preparation method of lithium manganese ferric phosphate/carbon composite positive electrode material for lithium battery
CN105118968A (en) Nested V2O3-cladding lithium vanadium phosphate lithium ion anode material
CN111916703A (en) In-situ synthesis method of lithium iron manganese phosphate/carbon @ graphene composite material
CN104600294B (en) High-capacity microrod lithium manganese iron phosphate material synthesized by hydrothermal process and preparation method thereof
CN105355878B (en) A kind of material as lithium ion cell positive and preparation method thereof
CN107732194B (en) Lithium manganese phosphate-lithium vanadium phosphate/graphene/carbon cathode material and preparation method thereof
CN104332628B (en) The preparation method and its lithium ion battery of anode material for lithium-ion batteries
CN103066286A (en) Vanadium-antimony co-doped lithium iron phosphate used as lithium ion positive pole material and preparation method thereof
CN104078658B (en) Modified manganese-based stratified material, preparation method of material, and lithium ion battery comprising material
CN102544493B (en) Preparation method of lithium ion battery composite positive material compounded by graphene

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20171121