CN104022283A - Method for improving electrochemical characteristics of lithium iron phosphate by use of graphene/polyaniline - Google Patents
Method for improving electrochemical characteristics of lithium iron phosphate by use of graphene/polyaniline Download PDFInfo
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- CN104022283A CN104022283A CN201410253978.9A CN201410253978A CN104022283A CN 104022283 A CN104022283 A CN 104022283A CN 201410253978 A CN201410253978 A CN 201410253978A CN 104022283 A CN104022283 A CN 104022283A
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention provides a method for improving electrochemical characteristics of lithium iron phosphate by use of graphene/polyaniline, belonging to the technical field of manufacturing of lithium batteries. The method is used for forming a graphene/polyaniline composite layer having electrical conductivity and corrosion resistance on the surface of the lithium iron phosphate powder through once operation in a treating fluid by use of electricity-free auto-polymerization reaction of chemically reducing the graphene and oxidizing aniline, wherein the electricity-free auto-polymerization reaction comprises reducing oxidized graphene into the graphene by the aniline, and meanwhile, oxidizing and polymerizing the aniline into the polyaniline. The method is simple in operation course and process; no organic solvent, surfactant, reducing agent and oxidizing agent are needed in the generation process of the composite layer, and therefore, the production cost is low; meanwhile, compared with simple mechanical mixing, the atomic-scale chemical reduction auto-polymerization reaction attachment of the method is better in combination degree and homogeneity, and therefore, the rate discharge performance and the cyclic stability of the lithium iron phosphate can be obviously improved.
Description
Technical field
What the present invention relates to is the method in a kind of lithium battery manufacturing technology field, and specifically a kind of using mineral carbon alkene/polyaniline improves the method for electrochemical performances of lithium iron phosphate.
Background technology
Lithium ion battery is a kind of high energy green battery that fast development is in recent years got up, compared with other secondary cell, lithium ion battery has that energy density is high, output voltage is high, power output is large, memory-less effect, operating temperature range are wide, good cycle and the advantage such as environmental pollution is little, has a extensive future.But with respect to other lithium ion battery material, the development of its positive electrode is comparatively slow, become the principal element that restriction lithium ion battery overall performance improves.
In recent years, there is the LiFePO4 (LiFePO of olivine structural
4) positive electrode because it is cheap, the advantage such as the high and good high-temperature electrochemical properties of environmental friendliness, specific capacity becomes one of current study hotspot, but still have that the synthetic particle diameter diffusion coefficient wayward, lithium ion of high temperature is little, electronics and the problem such as ionic conductivity is low, high current density charge-discharge performance is poor.Therefore improve LiFePO
4electric conductivity, improve coulombic efficiency, improving high rate during charging-discharging and high rate performance is LiFePO
4the key content of investigation of materials work.
Through the retrieval of prior art is found, Chinese patent literature CN103165898A open (bulletin) day 2013.06.19, a kind of Graphene polyaniline composite material and its preparation method and application is disclosed, this composite material comprises Graphene and polyaniline, described polyaniline is dispersed on described Graphene stratiform structure, and the mass percent of described Graphene in described composite material is 10～80%.But the preparation method of composite material that this technology is addressed, step complexity, raw material is more, and the time is longer, and operating process is wayward; In related lithium ion battery applications, only mix for simple mechanical-physical with positive and negative pole material, Expected Results is limited and to improve performance of lithium ion battery degree not clear.
Chinese patent literature CN102347475A open (bulletin) day 2012.02.08, a kind of high performance lithium ion battery and manufacture craft thereof are disclosed, its electrode material is through Graphene, the nano combined processing of polyaniline, plus plate current-collecting body is aluminium foil, negative current collector is Copper Foil, conductive agent is superconduction carbon black, electrically conductive graphite or acetylene black, binding agent is butadiene-styrene rubber, sodium cellulose glycolate, polytetrafluoroethylene, polyvinylidene fluoride or hydroxypropyl methylcellulose, electrolyte is liquid electrolyte or contains conducting polymer, nano material or containing the polymer dielectric of both compounds, high-temperature insulation porous polymer matrix is processed or directly adopted to barrier film through high-temperature-resistant insulating paint.This technique comprises: batching, apply, dry, roll-in, section, around volume or lamination, assembling, fluid injection, change into, partial volume.But this technology is to the raw-material demand of graphene oxide more (0.025～0.2:1), and need in technique, strictly controls oxidant and add and operating temperature, the enforcement time of this technology is also longer simultaneously.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind of using mineral carbon alkene/polyaniline and improve the method for electrochemical performances of lithium iron phosphate, technique is simple, conjugation and good uniformity.
The present invention is achieved by the following technical solutions, the present invention utilizes reacting without electric auto polymerization of electronation graphene oxide and aniline, in a treatment fluid, forms the graphene/polyaniline composite bed with conductivity and corrosion resistance through once-through operation in iron phosphate powder surface.
Described comprises without electric auto polymerization reaction: graphene oxide is reduced into Graphene by aniline, simultaneously the oxidized polyaniline that aggregates into of aniline.
Described treatment fluid is made up of graphene oxide, aniline, hydrochloric acid and water, and its mass ratio is 0.3～2 × 10
?4: 1～6 × 10
?2: 0.3～3.6 × 10
?2: 1.
Described iron phosphate powder and the mass ratio for the treatment of fluid are 0.01～0.2:1.
Described once-through operation refers to: low whipping speed is to stir 5～60min under the condition of 120～300 turn/min.
Described iron phosphate powder is through once-through operation after washing 2～3 times, and suction filtration forms graphene/polyaniline composite bed to be placed on vacuumize in the vacuum drying chamber of little Yu of pressure ?0.08MPa without water droplet on surface.
The present invention relates to the iron phosphate powder with graphene/polyaniline composite bed that said method prepares, there are graphene layer and coralliform conductive materials in its surface, and has the dual shape characteristic of electronation Graphene and polyaniline oxidation auto polymerization.
The present invention relates to a kind of battery based on the above-mentioned iron phosphate powder with graphene/polyaniline composite bed, prepare in the following manner: taking N ?methyl pyrrolidone (NMP) as solvent, iron phosphate powder, conductive black and the polyvinyladine floride (PVDF) with graphene/polyaniline composite bed are mixed, be stirred into muddy be coated on aluminium foil surface and dry after make positive pole, using lithium metal as with reference to negative pole, taking capillary polypropylene (Celgard2300) film as barrier film, with LiPF
6the mixed liquor of/ethylene carbonate (EC), diethyl carbonate (DEC), carbonic acid Methylethyl ester (EMC) is electrolyte, in the glove box that is full of high-purity argon gas, is assembled into battery.
The mass ratio of the described iron phosphate powder with graphene/polyaniline composite bed, conductive black and polyvinyladine floride (PVDF) is 80:10:10.
Described dryly refer to vacuumize 12 hours.
The component of described electrolyte and content are: 1mol/L LiPF
6/ EC, DEC, EMC mix taking volume ratio as 1:1:1.
Technique effect
Compared with prior art, graphene oxide raw material required for the present invention are few, and graphene oxide and LiFePO4 mass ratio are only 1.5510
?4～0.02:1, far less than 0.025～0.2:1 related in prior art; In addition, the present invention is without interpolation and the control operation temperature of oxidant, and the overall operation time is at most only 60min, having ensured to significantly improve on the basis of LiFePO4 performance, has reduced processing cost, has improved treatment effeciency; The 3rd, the present invention forms the graphene/polyaniline composite bed of high conductivity and corrosion resistance in a treatment fluid in iron phosphate powder surface through once-through operation, operating process and technique are simple, in composite bed generative process, without adding organic solvent, surfactant, reducing agent and oxidant, production cost is low.In addition, the electronation auto polymerization reaction of atom level of the present invention is adhered to compared with simple mechanical mixture, has higher conjugation and homogeneity, thereby can obviously improve multiplying power discharging property and the cyclical stability of LiFePO4.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope figure of commodity carbon-covering lithium iron phosphate powder before and after processing in the embodiment of the present invention 1;
In figure: (a) being untreated commodity carbon-covering lithium iron phosphate powder, is (b) graphene/polyaniline composite surface commodity carbon-covering lithium iron phosphate after treatment powder.
Fig. 2 is the cycle performance curve of commodity carbon-covering lithium iron phosphate electrode before and after processing in the embodiment of the present invention 1;
In figure: (a) being untreated iron phosphate lithium electrode, is (b) graphene/polyaniline composite surface iron phosphate lithium electrode after treatment.
Fig. 3 is commodity carbon-covering lithium iron phosphate rate charge-discharge curve before and after processing in the embodiment of the present invention 1;
In figure: (a) being untreated iron phosphate lithium electrode, is (b) graphene/polyaniline composite surface iron phosphate lithium electrode after treatment.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented under taking technical solution of the present invention as prerequisite, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment comprises the following steps: preparation 200mL is containing the mixed aqueous solution of graphene oxide 0.01g, aniline 6mL, hydrochloric acid 2mL; In above-mentioned mixed solution, add the commercially available carbon-covering lithium iron phosphate powder of 2g, low whipping speed is to stir 30min under 180 turn/min conditions; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?vacuumize in the vacuum drying chamber of 0.08MPa.
As shown in Figure 1, compared with untreated iron phosphate powder (a), there are obvious graphene layer and coralliform conductive materials in graphene/polyaniline composite surface iron phosphate powder after treatment (b) surface, has the dual shape characteristic of electronation Graphene and polyaniline oxidation auto polymerization.
As shown in Figures 2 and 3, taking N ?methyl pyrrolidone (NMP) as solvent, 80:10:10 in mass ratio, iron phosphate powder, conductive black and polyvinyladine floride (PVDF) before and after processing are mixed, be stirred into muddy and be coated on aluminium foil surface, then vacuumize 12 hours, compressing tablet is made the positive plate that diameter is 10mm.Using lithium metal as with reference to negative pole, taking capillary polypropylene (Celgard2300) film as barrier film, with 1mol/L LiPF
6/ EC+DEC+EMC (volume ratio is 1:1:1) is electrolyte.In the glove box that is full of high-purity argon gas, be assembled into CR2032 button cell.Leave standstill and carry out electrochemical property test after 12 hours.
Simulated battery adopts blue electric battery test system (LAND CT ?2001A) to carry out charge-discharge performance test.With different charge-discharge magnifications (0.2,0.5,1,2,5 and 10C), in 2.5～4.2V voltage range, the LiFePO4 sample before and after processing is carried out to charge-discharge performance test.Charge and discharge cycles test result shows: specific capacity when 0.2C and 10C discharge and recharge is about respectively 165 and 110mAh/g.
Embodiment 2
The present embodiment comprises the following steps: preparation 100mL is containing the mixed aqueous solution of graphene oxide 0.2g, aniline 4mL, hydrochloric acid 1.6mL; In above-mentioned mixed solution, add 20g commodity carbon-covering lithium iron phosphate powder, low whipping speed is to stir 60min under 120 turn/min conditions; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?vacuumize in the vacuum drying chamber of 0.08MPa.
LiFePO4 sample before and after processing is carried out to charge-discharge performance test.Charge and discharge cycles test result shows: specific capacity when 0.2C and 10C discharge and recharge is about respectively 157 and 102mAh/g.
Embodiment 3
The present embodiment comprises the following steps: preparation 100mL is containing the mixed aqueous solution of graphene oxide 0.003g, aniline 1mL, hydrochloric acid 0.5mL; In above-mentioned mixed solution, add 1g commodity carbon-covering lithium iron phosphate powder, low whipping speed is to stir 10min under 300 turn/min conditions; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?vacuumize in the vacuum drying chamber of 0.08MPa.
LiFePO4 sample before and after processing is carried out to charge-discharge performance test.Charge and discharge cycles test result shows: specific capacity when 0.2C and 10C discharge and recharge is about respectively 155 and 96mAh/g.
Embodiment 4
The present embodiment comprises the following steps: preparation 100mL is containing the mixed aqueous solution of graphene oxide 0.1g, aniline 6mL, hydrochloric acid 3.6mL; In above-mentioned mixed solution, add 10g commodity carbon-covering lithium iron phosphate powder, low whipping speed is to stir 20min under 240 turn/min conditions; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?vacuumize in the vacuum drying chamber of 0.08MPa.
LiFePO4 sample before and after processing is carried out to charge-discharge performance test.Charge and discharge cycles test result shows: specific capacity when 0.2C and 10C discharge and recharge is about respectively 153 and 100mAh/g.
Embodiment 5
The present embodiment comprises the following steps: preparation 200mL is containing the mixed aqueous solution of graphene oxide 0.025g, aniline 5mL, hydrochloric acid 1.5mL; In above-mentioned mixed solution, add 5g commodity carbon-covering lithium iron phosphate powder, low whipping speed is to stir 5min under 200 turn/min conditions; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?vacuumize in the vacuum drying chamber of 0.08MPa.
LiFePO4 sample before and after processing is carried out to charge-discharge performance test.Charge and discharge cycles test result shows: specific capacity when 0.2C and 10C discharge and recharge is about respectively 147 and 95mAh/g.
Claims (10)
1. a using mineral carbon alkene/polyaniline improves the method for electrochemical performances of lithium iron phosphate, it is characterized in that, utilize reacting without electric auto polymerization of electronation graphene oxide and aniline, in a treatment fluid, form the graphene/polyaniline composite bed with conductivity and corrosion resistance through once-through operation in iron phosphate powder surface;
Described comprises without electric auto polymerization reaction: graphene oxide is reduced into Graphene by aniline, simultaneously the oxidized polyaniline that aggregates into of aniline.
2. method according to claim 1, is characterized in that, described treatment fluid is made up of graphene oxide, aniline, hydrochloric acid and water.
3. method according to claim 1 and 2, is characterized in that, in described treatment fluid: the mass ratio of graphene oxide, aniline, hydrochloric acid and water is 0.3～2 × 10
?4: 1～6 × 10
?2: 0.3～3.6 × 10
?2: 1.
4. method according to claim 1 and 2, is characterized in that, described iron phosphate powder and the mass ratio for the treatment of fluid are 0.01～0.2:1.
5. method according to claim 1, is characterized in that, described once-through operation refers to: low whipping speed is to stir 5～60min under the condition of 120～300 turn/min.
6. the iron phosphate powder with graphene/polyaniline composite bed preparing according to method described in above-mentioned arbitrary claim, it is characterized in that, there are graphene layer and coralliform conductive materials in its surface, and has the dual shape characteristic of electronation Graphene and polyaniline oxidation auto polymerization.
7. the battery of the iron phosphate powder with graphene/polyaniline composite bed based on described in above-mentioned arbitrary claim, it is characterized in that, prepare in the following manner: taking N ?methyl pyrrolidone as solvent, iron phosphate powder, conductive black and the polyvinyladine floride with graphene/polyaniline composite bed are mixed, be stirred into muddy be coated on aluminium foil surface and dry after make positive pole, using lithium metal as with reference to negative pole, taking microporous polypropylene membrane as barrier film, with LiPF
6the mixed liquor of/ethylene carbonate, diethyl carbonate, carbonic acid Methylethyl ester is electrolyte, in the glove box that is full of high-purity argon gas, is assembled into battery.
8. battery according to claim 7, is characterized in that, the mass ratio of the described iron phosphate powder with graphene/polyaniline composite bed, conductive black and polyvinyladine floride is 80:10:10.
9. battery according to claim 7, is characterized in that, described dryly refers to vacuumize 12 hours.
10. battery according to claim 7, is characterized in that, the component of described electrolyte and content are: 1mol/L LiPF
6/ ethylene carbonate, diethyl carbonate, carbonic acid Methylethyl ester mix taking volume ratio as 1:1:1.
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Cited By (7)
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|---|---|---|---|---|
| CN104966836A (en) * | 2015-06-23 | 2015-10-07 | 上海交通大学 | Method for improving electrochemical performance of LiFePO4 through polypyrrole/graphene |
| CN106797018A (en) * | 2014-11-07 | 2017-05-31 | 银旺科技股份有限公司 | Artificial synthesized SEI cathode materials and the lithium secondary battery comprising this artificial synthesized SEI cathode material |
| CN107619032A (en) * | 2017-09-10 | 2018-01-23 | 绵阳梨坪科技有限公司 | A kind of preparation method with uniform-spherical meso-hole structure lithium iron phosphate positive material |
| CN110444740A (en) * | 2018-05-02 | 2019-11-12 | 哈尔滨工业大学 | A method of the small scale nanometer composite material of synthesizing graphite alkene/carbon-coated LiFePO 4 for lithium ion batteries is acted on by aniline polymerization confinement |
| CN111892830A (en) * | 2020-08-28 | 2020-11-06 | 湖州思源颜料有限公司 | Preparation method of iron oxide black pigment with strong acid resistance |
| CN114388800A (en) * | 2021-12-20 | 2022-04-22 | 苏州蔚利昆新能源科技有限公司 | High-power lithium battery for starting and stopping automobile |
| CN115360354A (en) * | 2022-10-20 | 2022-11-18 | 江苏智泰新能源科技有限公司 | Preparation method and application of sodium-ion battery positive electrode material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106797018A (en) * | 2014-11-07 | 2017-05-31 | 银旺科技股份有限公司 | Artificial synthesized SEI cathode materials and the lithium secondary battery comprising this artificial synthesized SEI cathode material |
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| CN110444740A (en) * | 2018-05-02 | 2019-11-12 | 哈尔滨工业大学 | A method of the small scale nanometer composite material of synthesizing graphite alkene/carbon-coated LiFePO 4 for lithium ion batteries is acted on by aniline polymerization confinement |
| CN111892830A (en) * | 2020-08-28 | 2020-11-06 | 湖州思源颜料有限公司 | Preparation method of iron oxide black pigment with strong acid resistance |
| CN114388800A (en) * | 2021-12-20 | 2022-04-22 | 苏州蔚利昆新能源科技有限公司 | High-power lithium battery for starting and stopping automobile |
| CN114388800B (en) * | 2021-12-20 | 2024-04-16 | 苏州蔚利昆新能源科技有限公司 | High-power lithium battery for starting and stopping automobile |
| CN115360354A (en) * | 2022-10-20 | 2022-11-18 | 江苏智泰新能源科技有限公司 | Preparation method and application of sodium-ion battery positive electrode material |
| CN115360354B (en) * | 2022-10-20 | 2023-01-10 | 江苏智泰新能源科技有限公司 | Preparation method and application of sodium-ion battery positive electrode material |
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