CN105047916A - Method for improving electrochemical properties of lithium iron phosphate with copper/graphene - Google Patents
Method for improving electrochemical properties of lithium iron phosphate with copper/graphene Download PDFInfo
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- CN105047916A CN105047916A CN201510350757.8A CN201510350757A CN105047916A CN 105047916 A CN105047916 A CN 105047916A CN 201510350757 A CN201510350757 A CN 201510350757A CN 105047916 A CN105047916 A CN 105047916A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- 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
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- 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
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention provides a method for improving electrochemical properties of lithium iron phosphate with copper/graphene belonging to the technical field of manufacturing of lithium batteries. The chemical replacement reaction of copper and iron ions and the chemical reduction of oxidized graphene comprise : partial iron ions on the surface of the lithium iron phosphate are chemically replaced by copper ions in a copper salt to form a copper film; meanwhile, the oxidized graphene is reduced into the graphene; and a copper/graphene composite layer with electrical conductivity and corrosion resistance is formed on the surface of lithium iron phosphate powder in a treating fluid by once operation. The method is simple in operation process and technology; an organic solvent, a surfactant, a reducing agent and an oxidant does not need to be added in the production process of the composite layer, so that the production cost is low; and meanwhile, compared with simple mechanical mixing, atomic chemical reduction and replacement reaction attachment provided by the invention has higher combination degree and uniformity, so that the rate discharge property and the cycling stability of the lithium iron phosphate can be obviously improved.
Description
Technical field
What the present invention relates to is a kind of method of lithium battery manufacturing technology field, specifically a kind ofly applies the method that copper/Graphene improves electrochemical performances of lithium iron phosphate.
Background technology
In recent years fast-developing get up lithium ion battery because have, power output high compared with high energy density, output voltage greatly, the advantage such as longer useful life, memory-less effect, environmental pollution be little, become research and development and the application focus of current secondary cell.In the application of high-power power battery, LiFePO4 (LiFePO
4) be the anode material for lithium-ion batteries of most prospect, compared with other positive electrode its, LiFePO
4high, the safety and reliability of stability, cheap and environmental protection.But LiFePO
4apply to the problem that there is " conductivity " difference in lithium-ion-power cell, keep height ratio capacity and high speed discharge and recharge to realize simultaneously, when high current charge-discharge, its specific capacity declines obviously, power characteristic can't well meet automobile power demand, therefore its marketization application is caused to having a strong impact on.
Through finding the retrieval of prior art; Chinese patent literature application number CN103779563A; open (bulletin) day 2014.01.20, discloses a kind of method preparing copper carbon-coated LiFePO 4 for lithium ion batteries, lithium source, source of iron, phosphorus source, carbon source and Tong Yuan is carried out ball milling mixing; after carry out spray drying treatment; obtain presoma, then by obtained presoma ball milling 2 ?after 8h, under inert gas shielding; calcining, obtains product after fragmentation.This technology address the preparation method of composite material, step is complicated, energy ezpenditure is large, and the time is longer, and operating process is wayward; In involved lithium ion battery applications, Expected Results is limited and improve the demand that performance of lithium ion battery degree is not enough to meet electrokinetic cell market.
The LiFePO 4 material of Surface coating copper can be regarded as a kind of metal-base composites.Surface clad layer not only improves electrical and thermal conductivity, non-oxidizability, the corrosion resistance of LiFePO4, extends the useful life of material, and drastically increases the electro catalytic activity of LiFePO4.
Summary of the invention
The present invention is directed to prior art above shortcomings, propose a kind ofly to apply the method that copper/Graphene improves electrochemical performances of lithium iron phosphate, by the mode that copper is combined with Graphene, be coated on LiFePO4 surface, utilize the physicochemical properties of copper and Graphene to improve high-rate discharge ability and the stable circulation performance of LiFePO4, simultaneously simple, the conjugation of present invention process and uniformity good.
The present invention is achieved by the following technical solutions:
The present invention utilizes chemical replacement and the chemical reduction reaction graphene oxide of copper iron ion, realizes forming the copper/Graphene composite bed with conductivity and corrosion resistance on iron phosphate powder surface.
Described chemical replacement and chemical reduction reaction, by the treatment fluid of configuration containing graphene oxide, mantoquita and water, fully react with LiFePO4 and be achieved, and the graphene oxide in this treatment fluid, mantoquita and water quality are than being preferably 0.2 ~ 5 × 10
?4: 0.2 ~ 10 × 10
?4: 1.
Described iron phosphate powder and the mass ratio for the treatment of fluid are 0.01 ~ 0.5:1.
Described mantoquita refers to: copper sulphate, copper chloride, copper nitrate or its mixing.
Described abundant reaction refers to: low whipping speed is stir 2 ~ 40min under the condition of 120 ~ 360 turns/min.
Described abundant reaction, takes out after washing 2 ~ 3 times by iron phosphate powder after being preferably reaction, and namely suction filtration forms copper/Graphene composite bed on surface to being placed on vacuumize in the vacuum drying chamber of pressure little Yu ?0.08MPa without water droplet.
The present invention relates to the LiFePO4 with copper/Graphene composite bed that said method prepares, there are graphene layer and granular conductive material in its surface, and has the dual shape characteristic of electronation Graphene and chemical substituting plating copper.
The present invention relates to a kind of ferric phosphate lithium cell, comprise: both positive and negative polarity, barrier film and electrolyte, wherein: positive pole by N ?methyl pyrrolidone (NMP), the powder with the LiFePO4 of copper/Graphene composite bed, conductive black and polyvinyladine floride (PVDF) form.
Described positive pole, with N ?methyl pyrrolidone (NMP) for solvent, to there is the mixing of the iron phosphate powder of copper/Graphene composite bed, conductive black and polyvinyladine floride (PVDF), be stirred into muddy be coated on aluminium foil surface and make after drying, wherein: the mass ratio with the iron phosphate powder of copper/Graphene composite bed, conductive black and polyvinyladine floride (PVDF) is preferably 80:10:10.
Described drying refers to vacuumize 12 hours.
Described negative pole adopts lithium metal.
Described barrier film, adopts capillary polypropylene (Celgard2300) film.
Described electrolyte, by lithium hexafluoro phosphate (LiPF
6)/ethylene carbonate (EC), diethyl carbonate (DEC), methyl ethyl ester (EMC) are mixed, and its component and content are preferably: 1mol/LLiPF
6/ EC, DEC, EMC are that 1:1:1 mixes with volume ratio.
Described battery is assembled and is obtained in the glove box being full of high-purity argon gas.
Technique effect
Compared with prior art, the present invention forms the copper/Graphene 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 simple, without the need to adding surfactant, reducing agent and oxidant in composite bed generative process, production cost is low.Meanwhile, the electronation displacement reaction attachment of atom level of the present invention, compared with simple mechanical mixture, has higher conjugation and homogeneity, thus can significantly improve multiplying power discharging property and the cyclical stability of LiFePO4.
Accompanying drawing explanation
Fig. 1 is field emission scanning electron microscope figure and the electron spectrum of commodity carbon-covering lithium iron phosphate powder before and after process in the embodiment of the present invention 1;
In figure: (a) is untreated commodity carbon-covering lithium iron phosphate powder, (b) is the commodity carbon-covering lithium iron phosphate powder after copper/Graphene compound base amount method.
Fig. 2 is the cycle performance curve of commodity carbon-covering lithium iron phosphate electrode before and after process in the embodiment of the present invention 1;
In figure: (a) is untreated iron phosphate lithium electrode, (b) is the iron phosphate lithium electrode after copper/Graphene compound base amount method.
Fig. 3 is commodity carbon-covering lithium iron phosphate rate charge-discharge curve in process front and back in the embodiment of the present invention 1;
In figure: (a) is untreated iron phosphate lithium electrode, (b) is the iron phosphate lithium electrode after copper/Graphene compound base amount method.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give 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 containing graphene oxide 0.01g, copper sulphate 0.08g, mixed aqueous solution; In above-mentioned mixed solution, add 2g commodity carbon-covering lithium iron phosphate powder, low whipping speed is stir 2min under 180 turns/min condition; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?0.08MPa vacuum drying chamber in vacuumize.
As shown in Figure 1, compared with untreated iron phosphate powder (a), there is obvious graphene layer on iron phosphate powder (b) surface after copper/Graphene compound base amount method, electron spectrum detects the existence of copper, and namely (b) has the dual shape characteristic of electronation Graphene and copper.
As shown in Figures 2 and 3, with N ?methyl pyrrolidone (NMP) for solvent, 80:10:10 in mass ratio, by the mixing of the iron phosphate powder before and after process, conductive black and polyvinyladine floride (PVDF), be stirred into muddy and be coated on aluminium foil surface, then vacuumize 12 hours, the positive plate that diameter is 10mm made by compressing tablet.Using lithium metal as with reference to negative pole, with capillary polypropylene (Celgard2300) film for barrier film, with 1mol/LLiPF
6/ EC+DEC+EMC (volume ratio is 1:1:1) is electrolyte.In the glove box being 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 (LANDCT ?2001A) to carry out charge-discharge performance test.With different charge-discharge magnification (0.2,0.5,1,2,5 and 10C), in 2.5 ~ 4.2V voltage range, charge-discharge performance test is carried out to the LiFePO4 sample before and after process.Charge and discharge cycles test result shows: specific capacity during 0.2C and 20C discharge and recharge is about 175 and 110mAh/g respectively.
Embodiment 2
The present embodiment comprises the following steps: preparation 150mL is containing the mixed aqueous solution of graphene oxide 0.2g, copper chloride 0.02g; In above-mentioned mixed solution, add 10g commodity carbon-covering lithium iron phosphate powder, low whipping speed is stir 40min under 120 turns/min condition; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?0.08MPa vacuum drying chamber in vacuumize.
Charge-discharge performance test is carried out to the LiFePO4 sample before and after process.Charge and discharge cycles test result shows: specific capacity during 0.2C and 20C discharge and recharge is about 147 and 75mAh/g respectively.
Embodiment 3
The present embodiment comprises the following steps: preparation 100mL is containing the mixed aqueous solution of graphene oxide 0.003g, copper nitrate 0.04g; In above-mentioned mixed solution, add 1g commodity carbon-covering lithium iron phosphate powder, low whipping speed is stir 10min under 300 turns/min condition; By above-mentioned reacted iron phosphate powder through washing, suction filtration, Zhi Yu ?0.08MPa vacuum drying chamber in vacuumize.
Charge-discharge performance test is carried out to the LiFePO4 sample before and after process.Charge and discharge cycles test result shows: specific capacity during 0.2C and 20C discharge and recharge is about 155 and 69mAh/g respectively.
Claims (10)
1. one kind has the preparation method of the LiFePO4 of copper/Graphene composite bed, it is characterized in that, utilize chemical replacement and the chemical reduction reaction graphene oxide of copper iron ion, realize forming the copper/Graphene composite bed with conductivity and corrosion resistance on iron phosphate powder surface;
Described chemical replacement and chemical reduction reaction, by the treatment fluid of configuration containing graphene oxide, mantoquita and water, fully react with LiFePO4 and be achieved.
2. method according to claim 1, is characterized in that, described treatment fluid is made up of graphene oxide, mantoquita and water, and wherein graphene oxide, mantoquita and water quality are than being preferably 0.2 ~ 5 × 10
?4: 0.2 ~ 10 × 10
?4: 1.
3. method according to claim 1, is characterized in that, described iron phosphate powder and the mass ratio for the treatment of fluid are 0.01 ~ 0.5:1.
4. method according to claim 1, is characterized in that, described mantoquita refers to: copper sulphate, copper chloride, copper nitrate or its mixing.
5. method according to claim 1, is characterized in that, described abundant reaction refers to: low whipping speed is stir 2 ~ 40min under the condition of 120 ~ 360 turns/min.
6. method according to claim 1 or 5, it is characterized in that, described abundant reaction, takes out after washing 2 ~ 3 times after reaction by iron phosphate powder, namely suction filtration forms copper/Graphene composite bed on surface to being placed on vacuumize in the vacuum drying chamber of pressure little Yu ?0.08MPa without water droplet.
7. one kind has the LiFePO4 of copper/Graphene composite bed, it is characterized in that, according to above-mentioned arbitrary claim, method prepares, and there are graphene layer and granular conductive material in surface, and has the dual shape characteristic of electronation Graphene and chemical substituting plating copper.
8. a ferric phosphate lithium cell, it is characterized in that, comprise: both positive and negative polarity, barrier film and electrolyte, wherein: positive pole by N ?methyl pyrrolidone, form according to the powder with the LiFePO4 of copper/Graphene composite bed, conductive black and the polyvinyladine floride described in above-mentioned arbitrary claim.
9. ferric phosphate lithium cell according to claim 8, it is characterized in that, described positive pole, with N ?methyl pyrrolidone for solvent, to there is the mixing of the iron phosphate powder of copper/Graphene composite bed, conductive black and polyvinyladine floride, be stirred into muddy be coated on aluminium foil surface and make after drying, wherein: the mass ratio with the iron phosphate powder of copper/Graphene composite bed, conductive black and polyvinyladine floride is 80:10:10.
10. ferric phosphate lithium cell according to claim 8, is characterized in that, described electrolyte, is mixed by lithium hexafluoro phosphate/ethylene carbonate, diethyl carbonate, methyl ethyl ester, and its component and content are: 1mol/LLiPF
6/ EC, DEC, EMC are that 1:1:1 mixes with volume ratio.
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| CN201810704060.XA CN108923045A (en) | 2015-06-23 | 2015-06-23 | Improve the method for electrochemical performances of lithium iron phosphate using copper ion/graphene |
| CN201510350757.8A CN105047916A (en) | 2015-06-23 | 2015-06-23 | Method for improving electrochemical properties of lithium iron phosphate with copper/graphene |
| CN201810681993.1A CN108832122A (en) | 2015-06-23 | 2015-06-23 | Improve the method for electrochemical performances of lithium iron phosphate using copper/graphene |
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| CN201810681993.1A Division CN108832122A (en) | 2015-06-23 | 2015-06-23 | Improve the method for electrochemical performances of lithium iron phosphate using copper/graphene |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105489884A (en) * | 2016-02-01 | 2016-04-13 | 上海交通大学 | Method for improving electrochemical performance of nickel-cobalt lithium manganate by chemically reducing oxidized graphene/magnesium |
| CN105633391A (en) * | 2016-02-03 | 2016-06-01 | 上海交通大学 | Preparation method of metal manganese/reduced-oxidized graphene/lithium iron phosphate composite material |
| CN105762351A (en) * | 2016-05-04 | 2016-07-13 | 合肥工业大学 | Lithium titanate/M-graphene composite cathode material for lithium ion battery and preparation method of lithium titanate/M-graphene composite cathode material |
| CN106410207A (en) * | 2016-07-29 | 2017-02-15 | 山东玉皇新能源科技有限公司 | Graphene lithium iron phosphate lithium ion battery with quick charge-discharge function, and manufacturing method therefor |
| CN110280244A (en) * | 2019-07-17 | 2019-09-27 | 肇庆市华师大光电产业研究院 | A kind of carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN112599717A (en) * | 2020-12-17 | 2021-04-02 | 上海交通大学 | Lithium ion battery optimization method based on surface electro-deposition metal/graphene composite layer |
| CN114530594A (en) * | 2021-12-27 | 2022-05-24 | 杭州华宏通信设备有限公司 | High-conductivity long-cycle lithium iron phosphate battery and preparation method thereof |
| CN114744170A (en) * | 2022-04-02 | 2022-07-12 | 楚能新能源股份有限公司 | Preparation method of modified lithium iron phosphate cathode material and lithium ion battery |
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| CN110078042B (en) * | 2019-04-30 | 2022-10-14 | 西南大学 | Lithium-rich lithium iron phosphate material and preparation method and application thereof |
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| CN105489884A (en) * | 2016-02-01 | 2016-04-13 | 上海交通大学 | Method for improving electrochemical performance of nickel-cobalt lithium manganate by chemically reducing oxidized graphene/magnesium |
| CN105489884B (en) * | 2016-02-01 | 2019-01-11 | 上海交通大学 | The method that electronation graphene oxide/magnesium improves nickle cobalt lithium manganate chemical property |
| CN105633391A (en) * | 2016-02-03 | 2016-06-01 | 上海交通大学 | Preparation method of metal manganese/reduced-oxidized graphene/lithium iron phosphate composite material |
| CN105633391B (en) * | 2016-02-03 | 2019-01-11 | 上海交通大学 | Manganese metal/redox graphene/composite ferric lithium phosphate material preparation method |
| CN105762351A (en) * | 2016-05-04 | 2016-07-13 | 合肥工业大学 | Lithium titanate/M-graphene composite cathode material for lithium ion battery and preparation method of lithium titanate/M-graphene composite cathode material |
| CN106410207A (en) * | 2016-07-29 | 2017-02-15 | 山东玉皇新能源科技有限公司 | Graphene lithium iron phosphate lithium ion battery with quick charge-discharge function, and manufacturing method therefor |
| CN110280244A (en) * | 2019-07-17 | 2019-09-27 | 肇庆市华师大光电产业研究院 | A kind of carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN112599717A (en) * | 2020-12-17 | 2021-04-02 | 上海交通大学 | Lithium ion battery optimization method based on surface electro-deposition metal/graphene composite layer |
| CN112599717B (en) * | 2020-12-17 | 2021-11-26 | 上海交通大学 | Lithium ion battery optimization method based on surface electro-deposition metal/graphene composite layer |
| CN114530594A (en) * | 2021-12-27 | 2022-05-24 | 杭州华宏通信设备有限公司 | High-conductivity long-cycle lithium iron phosphate battery and preparation method thereof |
| CN114530594B (en) * | 2021-12-27 | 2023-08-08 | 杭州华宏通信设备有限公司 | High-electric-conductivity long-cycle lithium iron phosphate battery and preparation method thereof |
| CN114744170A (en) * | 2022-04-02 | 2022-07-12 | 楚能新能源股份有限公司 | Preparation method of modified lithium iron phosphate cathode material and lithium ion battery |
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| CN108923045A (en) | 2018-11-30 |
| CN108832122A (en) | 2018-11-16 |
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