CN103515605A - Lithium vanadium phosphate/graphene composite material preparation method - Google Patents
Lithium vanadium phosphate/graphene composite material preparation method Download PDFInfo
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- CN103515605A CN103515605A CN201210212000.9A CN201210212000A CN103515605A CN 103515605 A CN103515605 A CN 103515605A CN 201210212000 A CN201210212000 A CN 201210212000A CN 103515605 A CN103515605 A CN 103515605A
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- lithium
- composite material
- graphene composite
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- graphene
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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
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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides a lithium vanadium phosphate/graphene composite material preparation method, which comprises: taking a graphite oxide and adding to water, and carrying out ultrasonic dispersion to obtain a graphene oxide suspension; taking vanadium pentoxide powder and dissolving in an oxalic acid solution, adding the graphene oxide suspension, uniformly stirring, adding a lithium source and a phosphorus source, stirring for 1-5 h, and carrying out heating drying to obtain dried precursor powder; and in the protection of an inert gas, pre-burning the precursor powder for 0.5-2 h at a temperature of 300-500 DEG C, cooling, grinding, placing in a microwave oven, and carrying out a reaction for 5-60 min to obtain the lithium vanadium phosphate/graphene composite material. According to the present invention, the preparation method has characteristics of simple process and short reaction time, and the prepared lithium vanadium phosphate/graphene composite material has good power density and high capacity, and can be used as the positive electrode material of lithium ion batteries and super capacitors.
Description
Technical field
The present invention relates to electrochemical material preparation field, relate in particular to a kind of preparation method of lithium vanadium phosphate/graphene composite material.
Background technology
The strong competitor that specific energy is large, self discharge is little owing to having for lithium ion battery, have extended cycle life, lightweight and advantages of environment protection becomes electric automobile and hybrid vehicle power supply.
Common power lithium-ion battery positive electrode has spinel lithium manganate (LiMn
2o
4), nickel-cobalt-manganese ternary material (LiNi
1-x-yco
xmn
yo
2) and polyanion type positive electrode (LiMPO
4, M=Mn, Fe, V etc.).Wherein, polyanion type LiFePO4 (LFP) enjoys people to pay close attention to because of the outstanding advantages such as have extended cycle life, safe and cheap; But the critical defect such as it exists electronic and ionic poorly conductive, lithium ion diffusion coefficient is low and heavy-current discharge characteristic is poor.Be all the phosphoric acid vanadium lithium (Li of polyanion type structure
3v
2(PO
4)
3lVP) positive electrode, theoretical energy density reaches 500mWh/g, compare LFP and there is higher electronic and ionic conductivity, theoretical charge/discharge capacity and charging/discharging voltage platform, and under the high charge voltage of 4.8V, still can keep stable frame structure, therefore be considered to a kind of power lithium-ion battery positive electrode that has competitive advantage and application prospect.But due to crystal structure, metal ion relatively far apart, makes the electron mobility in material low, Li
3v
2(PO
4)
3electron mobility be 2 * 10
7s/cm, has limited Li greatly
3v
2(PO
4)
3chemical property.
Graphene is current the thinnest known a kind of material, has extremely strong conductivity, and superhigh intensity and super large specific area get the attention in battery material field.
Summary of the invention
For addressing the above problem, the present invention aims to provide a kind of preparation method of lithium vanadium phosphate/graphene composite material.Preparation method's technological process provided by the invention is simple, and the reaction time is short.Lithium vanadium phosphate/graphene composite material provided by the invention, possesses good power density and higher capacity, can be used as the positive electrode of lithium ion battery and ultracapacitor.
The preparation method who the invention provides a kind of lithium vanadium phosphate/graphene composite material, comprises the following steps:
Get graphite oxide and be added to the water, after ultrasonic dispersion, obtain graphene oxide suspension;
Get vanadium pentoxide powder and be dissolved in oxalic acid solution, add described graphene oxide suspension, stir, add subsequently Li Yuanhelin source, stir 1 ~ 5h, heat drying, obtains dry precursor powder;
By precursor powder under inert gas shielding, pre-burning 0.5 ~ 2h at 300 ~ 550 ℃ of temperature, cooling, grind, then be placed in microwave oven and react 5 ~ 60min, obtain lithium vanadium phosphate/graphene composite material.
Preferably, the time of ultrasonic dispersion is 30 ~ 180min.
What ultrasonic dispersion made that the process of graphene oxide adopts is ultrasonic stripping method, is about to graphite oxide suspension ultrasonic regular hour under certain power.Ultrasonic wave is density interphase eradiation in graphite oxide suspension, make liquid flow and produce the micro-bubble of One's name is legion, these bubbles form at the negative pressuren zone of ultrasonic wave longitudinal propagation, growth, and at zone of positive pressure rapid closing, in the process of this being referred to as " cavitation " effect, bubble closure can form and surpass 1.0 * 10
8pa atmospheric instantaneous pressure, the high pressure successively producing resembles a succession of little " blast " and constantly impacts graphite oxide, oxidized graphite flake is peeled off rapidly and generate mono-layer graphite oxide alkene.Wherein, the size of graphene oxide sheet can regulate by the size of ultrasonic power and the length of ultrasonic time.
Preferably, the mass ratio of graphite oxide and vanadic oxide is 0.2 ~ 1.6:1
Preferably, the mass concentration of oxalic acid solution is 10 ~ 20%.
Preferably ，Li source is lithium hydroxide, lithium acetate or lithium carbonate.
Preferably ，Lin source is ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ammonium phosphate.
Preferably, vanadic oxide ,Li Yuan Yulin source is by vanadium: lithium: the amount that the mol ratio of phosphate radical is 2:3:3 adds.
Preferably, heating-up temperature is 50 ~ 80 ℃.
Low-temperature heat is mainly the moisture of removing in mixed material, makes it become dry into dry precursor powder.
Preferably, inert gas is one or more the combination in nitrogen, argon gas, helium and neon.
Preferably, the power of microwave oven is 600 ~ 3000w.
By dry precursor powder, under inert gas shielding, pre-burning 0.5 ~ 2h at 300 ~ 500 ℃ of temperature, has an oxalic acid charing to become the process of carbon in preheating process, and carbon serves as reducing agent in follow-up microwave reaction.
Preferably, in pre-burning process, add sucrose, citric acid, glucose or starch.
Adding of sucrose, citric acid, glucose or starch, the source that can provide more charings to become carbon, can provide abundanter reducing agent for microwave reaction, thereby makes microwave reaction carry out more completely.
In microwave reaction process, graphene oxide is reduced into Graphene, and chemical reaction occurs in vanadic oxide ,Li Yuan Yulin source, generates phosphoric acid vanadium lithium (Li
3v
2(PO
4)
3) ，Li source take ammonium dihydrogen phosphate as example with lithium hydroxide Wei Li，Lin source, chemical equation is as follows:
3LiOH+V
2O
5+3NH
4H
2PO
4+2C→Li
3V
2(PO4)
3+3NH
3+6H
2O+2CO。
Microwave reaction mechanism: microwave radiation energy can be directly by absorption of sample, and heats fast and equably at short notice reaction raw materials, provides reaction required heat.Microwave reaction generated time is short, pollute little, without the protection of inert gas.
Preferably, in lithium vanadium phosphate/graphene composite material, phosphoric acid vanadium lithium (Li
3v
2(PO
4)
3) mass content be 50 ~ 95%, the mass content of Graphene is 5 ~ 50%.
The lithium vanadium phosphate/graphene composite material that the present invention makes is to consist of the graphene molecules of 2 dimensions and phosphoric acid vanadium lithium, the graphene molecules of the high conduction that phosphoric acid vanadium lithium surface attachment is a large amount of.In lithium vanadium phosphate/graphene composite material, phosphoric acid vanadium lithium (Li
3v
2(PO
4)
3) go out very strong covalent interaction feature with Graphene surface main manifestations.The main contributions of covalent bond comes from the hydridization of the d (x2-y2) of Transition Metals V and the pz track of d (yz) track and carbon atom.
In addition, the present invention also provides the application of lithium vanadium phosphate/graphene composite material in lithium ion battery and super capacitor anode material.
The preparation method of a kind of lithium vanadium phosphate/graphene composite material provided by the invention, has following beneficial effect:
(1) preparation method of lithium vanadium phosphate/graphene composite material provided by the invention is simple and quick, possesses low cost, and energy consumption is little, and the feature such as technique is simple;
(2) lithium vanadium phosphate/graphene composite material provided by the invention possesses good conductivity, and high mechanical performance, has good power density and life-span, has higher capacity;
(3) lithium vanadium phosphate/graphene composite material provided by the invention can be used as good lithium ion battery and super capacitor anode material.
Accompanying drawing explanation
Fig. 1 is the SEM Electronic Speculum picture of gained lithium vanadium phosphate/graphene composite material of the present invention.
Embodiment
The following stated is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Embodiment mono-
The preparation method of lithium vanadium phosphate/graphene composite material, comprises the following steps:
(1) get 3.57g graphite oxide and be added to the water, ultrasonic dispersion 0.5h, obtains graphene oxide suspension;
(2) getting 18.2g vanadic oxide is dissolved in oxalic acid solution, obtain blue solution, add wherein above-mentioned graphene oxide suspension, be uniformly mixed, in mixed solution, add 12.6g lithium hydroxide and 34.5g ammonium dihydrogen phosphate again, stir 1h, then be dried at 50 ℃, obtain dry precursor powder;
(3) by dry precursor powder under inert nitrogen gas protection, pre-burning 0.5h at 300 ℃ of temperature, cooling, grind, then be placed in microwave oven, the power microwave reaction 5min with 600w, obtains lithium vanadium phosphate/graphene composite material.
The present embodiment gained lithium vanadium phosphate/graphene composite material, the mass fraction of phosphoric acid vanadium lithium is 95%.
Fig. 1 is the SEM Electronic Speculum picture of the present embodiment gained lithium vanadium phosphate/graphene composite material.As can be seen from Figure 1, the thickly dotted phosphoric acid vanadium lithium surface that is wrapped in of the graphene molecules of nanostructure.
The present embodiment gained lithium vanadium phosphate/graphene composite material is assembled into lithium ion battery as positive electrode: take 8.5g lithium vanadium phosphate/graphene composite material, 0.5g conductive agent SP and 0.5g PVDF, and add 70g NMP, fully stir and make it to become the slurry mixing.Then by its blade coating on the aluminium foil cleaning through ethanol, under the vacuum of 0.01MPa, 100 ℃ are dried to constant weight, and are pressed into lithium vanadium phosphate/graphene composite material electrode in 10 ~ 15MPa pressure lower roll, and are cut into positive plate.Lithium sheet is as negative pole.By positive plate, barrier film, negative plate in order stack of laminations dress up battery core, then use battery housing seal battery core, subsequently toward by liquid injection port toward the LiPF6/ dimethyl carbonate electrolyte that injects 1mol/L in battery container, sealing liquid injection port, obtains lithium ion battery.In the voltage range of 2.5 ~ 4.2V, utilize charge-discharge test instrument to carry out 0.1C and 5C charge-discharge test to the lithium ion battery assembling in the present embodiment, the specific discharge capacity of 3th is respectively 132mAh/g, 68mAh/g.
Embodiment bis-
The preparation method of lithium vanadium phosphate/graphene composite material, comprises the following steps:
(1) get 29.1g graphite oxide and be added to the water, ultrasonic dispersion 3h, obtains graphene oxide suspension;
(2) getting 18.2g vanadic oxide is dissolved in oxalic acid solution, obtain blue solution, add wherein above-mentioned graphene oxide suspension, be uniformly mixed, in mixed solution, add 19.8g lithium acetate and 39.6g ammonium hydrogen phosphate again, stir 5h, then be dried at 80 ℃, obtain dry precursor powder;
(3) by dry precursor powder under inert gas argon gas protection, pre-burning 2h at 300 ℃ of temperature, cooling, grind, then be placed in microwave oven, the power microwave reaction 60min with 3000w, obtains lithium vanadium phosphate/graphene composite material.
The present embodiment gained lithium vanadium phosphate/graphene composite material, the mass fraction of phosphoric acid vanadium lithium is 70%.
Using the present embodiment gained lithium vanadium phosphate/graphene composite material as positive electrode, be assembled into lithium ion battery (method is with embodiment mono-), in the voltage range of 2.5 ~ 4.2V, utilize charge-discharge test instrument to carry out 0.1C and 5C charge-discharge test to the lithium ion battery assembling in the present embodiment, the specific discharge capacity of 3th is respectively 101mAh/g, 88mAh/g.
Embodiment tri-
The preparation method of lithium vanadium phosphate/graphene composite material, comprises the following steps:
(1) get 17g graphite oxide and be added to the water, ultrasonic dispersion 1h, obtains graphene oxide suspension;
(2) getting 18.2g vanadic oxide is dissolved in oxalic acid solution, obtain blue solution, add wherein above-mentioned graphene oxide suspension, be uniformly mixed, in mixed solution, add 11.1g lithium carbonate and 60.9g ammonium phosphate again, stir 2h, then be dried at 60 ℃, obtain dry precursor powder;
(3) by dry precursor powder under inert gas helium protection, pre-burning 1h at 300 ℃ of temperature, cooling, grind, then be placed in microwave oven, the power microwave reaction 20min with 1000w, obtains lithium vanadium phosphate/graphene composite material.
The present embodiment gained lithium vanadium phosphate/graphene composite material, the mass fraction of phosphoric acid vanadium lithium is 80%.
Using the present embodiment gained lithium vanadium phosphate/graphene composite material as positive electrode, be assembled into lithium ion battery (method is with embodiment mono-), in the voltage range of 2.5 ~ 4.2V, utilize charge-discharge test instrument to carry out 0.1C and 5C charge-discharge test to the lithium ion battery assembling in the present embodiment, the specific discharge capacity of 3th is respectively 116mAh/g, 85mAh/g.
Embodiment tetra-
The preparation method of lithium vanadium phosphate/graphene composite material, comprises the following steps:
(1) get 7.55g graphite oxide and be added to the water, ultrasonic dispersion 2h, obtains graphene oxide suspension;
(2) getting 18.2g vanadic oxide is dissolved in oxalic acid solution, obtain blue solution, add wherein above-mentioned graphene oxide suspension, be uniformly mixed, in mixed solution, add 11.1g lithium carbonate and 39.6g ammonium hydrogen phosphate again, stir 4h, then be dried at 70 ℃, obtain dry precursor powder;
(3) by dry precursor powder under inert gas helium protection, pre-burning 1.5h at 300 ℃ of temperature, cooling, grind, then be placed in microwave oven, the power microwave reaction 40min with 2000w, obtains lithium vanadium phosphate/graphene composite material.
The present embodiment gained lithium vanadium phosphate/graphene composite material, the mass fraction of phosphoric acid vanadium lithium is 90%.
Using the present embodiment gained lithium vanadium phosphate/graphene composite material as positive electrode, be assembled into lithium ion battery (method is with embodiment mono-), in the voltage range of 2.5 ~ 4.2V, utilize charge-discharge test instrument to carry out 0.1C and 5C charge-discharge test to the lithium ion battery assembling in the present embodiment, the specific discharge capacity of 3th is respectively 127mAh/g, 79mAh/g.
The lithium vanadium phosphate/graphene composite material that the embodiment of the present invention makes, by Graphene and phosphoric acid vanadium lithium (Li
3v
2(PO
4)
3) compound mixes, and utilizes the superelevation conductivity of Graphene, greatly improved the conductive capability of material, and improved the chemical property of phosphoric acid vanadium lithium material, is applicable to the positive electrode active materials of electrical source of power.When its positive electrode as lithium ion battery, lithium ion battery also can be brought into play higher capacity under the high magnification of 5C.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a preparation method for lithium vanadium phosphate/graphene composite material, is characterized in that, comprises the following steps:
Get graphite oxide and be added to the water, after ultrasonic dispersion, obtain graphene oxide suspension;
Get vanadium pentoxide powder and be dissolved in oxalic acid solution, then add described graphene oxide suspension, stir, add subsequently Li Yuanhelin source, stir 1 ~ 5h, heat drying, obtains dry precursor powder;
By described precursor powder under inert gas shielding, pre-burning 0.5 ~ 2h at 300 ~ 500 ℃ of temperature, cooling, grind, then be placed in microwave oven and react 5 ~ 60min, obtain lithium vanadium phosphate/graphene composite material.
2. the method for claim 1, is characterized in that, the time of described ultrasonic dispersion is 30 ~ 180min.
3. the method for claim 1, is characterized in that, the mass ratio of described graphite oxide and described vanadic oxide is 0.2 ~ 1.6:1.
4. the method for claim 1, is characterized in that, the mass concentration of described oxalic acid solution is 10 ~ 20%.
5. the method for claim 1, is characterized in that, described lithium source is lithium hydroxide, lithium acetate or lithium carbonate, and described phosphorus source is ammonium hydrogen phosphate, ammonium dihydrogen phosphate or ammonium phosphate.
6. the method for claim 1, is characterized in that, described vanadic oxide, described lithium source and described phosphorus source are by vanadium: lithium: the amount that the mol ratio of phosphate radical is 2:3:3 adds.
7. the method for claim 1, is characterized in that, described inert gas is one or more the combination in nitrogen, argon gas, helium and neon.
8. the method for claim 1, is characterized in that, the power of described microwave oven is 600 ~ 3000w.
9. the method for claim 1, is characterized in that, in described lithium vanadium phosphate/graphene composite material, the mass content of phosphoric acid vanadium lithium is 50 ~ 95%, and the mass content of Graphene is 5 ~ 50%.
10. according to claim 1 ~ 9, select the application in lithium ion battery and super capacitor anode material of lithium vanadium phosphate/graphene composite material that described in one, method prepares.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107799730A (en) * | 2016-08-31 | 2018-03-13 | 苏州艾美得新能源材料有限公司 | Method for preparing anode material, positive electrode and battery |
| CN111883747A (en) * | 2020-06-24 | 2020-11-03 | 华南理工大学 | Method for preparing porous graphene coated lithium vanadium phosphate by recovering graphite cathode material from waste power battery |
| CN115340079A (en) * | 2022-07-27 | 2022-11-15 | 武汉理工大学 | Superfine lithium vanadium phosphate nano-microcrystal integrated chip and preparation method and application thereof |
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| US20120058397A1 (en) * | 2010-09-07 | 2012-03-08 | Aruna Zhamu | Graphene-Enhanced cathode materials for lithium batteries |
| CN102386410A (en) * | 2011-11-05 | 2012-03-21 | 上海大学 | Lithium vanadium phosphate/graphene composite material and preparation method thereof |
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2012
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| CN101651205A (en) * | 2009-08-21 | 2010-02-17 | 常熟理工学院 | Method for preparing lithium vanadium phosphate as lithium ion battery anode material |
| US20120058397A1 (en) * | 2010-09-07 | 2012-03-08 | Aruna Zhamu | Graphene-Enhanced cathode materials for lithium batteries |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107799730A (en) * | 2016-08-31 | 2018-03-13 | 苏州艾美得新能源材料有限公司 | Method for preparing anode material, positive electrode and battery |
| CN111883747A (en) * | 2020-06-24 | 2020-11-03 | 华南理工大学 | Method for preparing porous graphene coated lithium vanadium phosphate by recovering graphite cathode material from waste power battery |
| CN115340079A (en) * | 2022-07-27 | 2022-11-15 | 武汉理工大学 | Superfine lithium vanadium phosphate nano-microcrystal integrated chip and preparation method and application thereof |
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Application publication date: 20140115 |