CN106654218A - Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and lithium ion battery - Google Patents
Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and lithium ion battery Download PDFInfo
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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
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Abstract
The invention discloses a preparation method of a lithium ion battery positive electrode material lithium vanadium phosphate/carbon. The preparation method comprises the following steps of weighing a lithium source, a vanadium source, a phosphate source and a reducing agent according to a mole ratio of a lithium element, a vanadium element, a phosphate element and the reducing agent being 3.05:2:3:3; placing the vanadium source and the reducing agent in deionized water for dissolving and generating reduction reaction, sequentially adding the lithium source and the phosphate source again, performing heating and stirring to make the lithium source and the phosphate source uniformly mixed, and forming green gel after moisture is evaporated; placing the green gel in a drying box to form dried gel, and then pre-sintering the dried gel to form precursor powder; and adding a dispersing agent for ball grinding and dispersing after the precursor powder and a carbon source are uniformly mixed, and evaporating and sintering the dispersing agent to obtain a lithium vanadium phosphate/carbon composite material, wherein the usage amount of the carbon source is in the way that the percent of carbon in the lithium vanadium phosphate/carbon composite material by weight is 5-10%. Through the preparation method of a sol-gel method and a solid-phase method which are combined, and the lithium ion battery positive electrode material lithium vanadium phosphate/carbon with favorable rate performance and cycle performance can be prepared.
Description
Technical field
The present invention relates to cell art, and in particular to a kind of cathode material lithium vanadium phosphate of lithium ion battery/carbon and its
Preparation method and a kind of lithium ion battery.
Background technology
Lithium ion battery is made up of three parts：Positive pole, negative pole and electrolyte, electrode material can be embedded in/deintercalation for lithium ion
Section bar material.The operation principle of lithium ion battery is that carrying out between positive electrode and negative material of moving in circles of lithium ion is embedding
Enter/deintercalation.In charging process, lithium ion is deviate from from positive electrode, and under electrolyte effect negative pole interlayer is embedded in, and makes negative pole rich
Lithium and positive extreme poverty lithium, at the same the compensation electric charge of electronics via external circuit to negative pole；In contrast, lithium ion is from negative pole for discharge process
Jing electrolyte reaches positive pole, and compensation electric charge reaches positive pole by external circuit.Embedded/the deintercalation of lithium ion is caused in main material skeleton
Distribution of charges change, so as to generate electric current on external circuit.
Electrode material is the key components of lithium ion battery, closely related with battery cost and performance.Cobalt acid lithium electricity
Pond is abandoned for high-power jumbo occasion because material price is expensive, security is poor.Lithium manganate battery have low cost,
High performance advantage, Product Safety is high compared with cobalt acid lithium battery, is the popular alternative positive electrode of batteries of electric automobile, but its
Operating potential is relatively low.LiFePO4 has the more stable state of oxidation, has a safety feature, and high-temperature behavior is good, while and with nothing
Malicious, pollution-free, raw material sources extensively, low price the advantages of, be batteries of electric automobile positive electrode most popular at present it
One.For the lithium ion battery of extensive energy storage, other key technologies also include battery system overall design technique, battery system
Integrated and group technology, battery pack measuring technology etc..
At present, various anode material for lithium-ion batteries have been occurred in that in production practices and scientific research, two can be divided into big
Class：The transition metal salt of lithium, including lamellar compound, spinel type compound etc. (be represented by LixMyOz, M be Co, Ni, Mn,
The transition metal such as V)；Another kind of is polyanionic compound, that is, containing tetrahedron or octahedra anion structure list
Unit (XOm)n-The compound of (X=P, S, As, Mo and W).
With phosphoric acid vanadium lithium (Li3V2(PO4)3Vanadium phosphate compounds to represent have chemical property preferably, Stability Analysis of Structures, security
Can be good, with low cost, environmentally friendly the features such as.Its oxidation-reduction potential is high, and with relatively special three-dimensional ion-transfer passage,
Lithium ion can well carry out deintercalation.
Sol-gal process is the common method for synthesizing phosphoric acid vanadium lithium.Usually said sol-gal process is generally referred to before sintering
All reactions mix with material and carry out in the solution, but the macromolecule carbon such as phenolic resin and Kynoar (PVDF)
Source is water insoluble, it is impossible to mix with the aqueous solution of lithium source, vanadium source, phosphorus source.Therefore, it is to solve to be asked present in prior art
Topic, the present invention proposes a kind of composite preparation process of phosphoric acid vanadium lithium, and the composite preparation process is a kind of sol-gal process and solid phase
The method that method combines, process is simple, applicable surface is extensive.
The content of the invention
In view of this, it is an object of the invention to propose a kind of phosphoric acid vanadium lithium that sol-gal process and solid phase method combine/
The preparation method of carbon positive electrode, by the preparation method can prepare the lithium with good high rate performance and cycle performance from
Sub- battery positive pole material phosphoric acid vanadium lithium/carbon.
A kind of preparation method of the cathode material lithium vanadium phosphate of lithium ion battery/carbon provided based on above-mentioned purpose, the present invention,
Comprise the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium source, vanadium source, phosphorus
Source and reducing agent；
(2) vanadium source and reducing agent are placed in deionized water dissolve and concurrently give birth to reduction reaction, sequentially add lithium source and phosphorus
Source, heating stirring is well mixed it, treats that moisture is evaporated to form green gel；
(3) green gel is dried to be formed after xerogel, xerogel pre-burning is formed into precursor powder；
(4) after precursor powder is well mixed with carbon source, dispersant is added to carry out ball milling dispersion, after dispersant is evaporated
Sintering, obtains vanadium phosphate lithium/carbon composite material；The consumption of the carbon source is the weight for making carbon in vanadium phosphate lithium/carbon composite material
Percentage is 5-10%.
The present invention can be prepared with good high rate performance using the composite-making process of ball milling assisting sol gel method
With the combination electrode material phosphoric acid vanadium lithium/carbon of cycle performance, particle fine uniform, carbon coating works well.
In the present invention, it is preferred to, the lithium source is lithium nitrate, lithium hydroxide, lithium carbonate, lithium fluoride, lithium dihydrogen phosphate
Or the one kind in lithium acetate；The vanadium source is the one kind in vanadic anhydride, sodium vanadate or sodium metavanadate；Phosphorus source is phosphoric acid
One kind in ammonium dihydrogen, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid or pyrophosphoric acid；The reducing agent is citric acid, ascorbic acid, grass
One kind in acid or malic acid.
In the present invention, with high price alum source compound as vanadium source, the cost of synthesis condition and raw material is greatly reduced, also
Pentavalent vanadium ion in vanadium source is reduced to tetravalent vanadium ion by former agent, and in vanadium source reducing agent is added, in normal temperature and pressure or 60 DEG C
Stirred in water bath is reacted, and question response is finished, and obtains clarification blue solution, then sequentially adds lithium source and phosphorus source.The present invention is utilized
Pentavalent vanadium ion is directly reduced to tetravalent vanadium ion by reducing agent, solves the problems, such as that trivalent vanadium ion is oxidized easily.
In the present invention, it is preferred to, the carbon source includes organic carbonaceous material and macromolecule carbonaceous material.
In the present invention, it is further preferred that the organic carbonaceous material is in glucose, sucrose or stearic acid
Kind；The macromolecule carbonaceous material is the one kind in polyvinyl alcohol, epoxy resin, phenolic resin or Kynoar.
In the present invention, it is preferred to, the dispersant is the one kind in acetone, ethanol or ether.
In the present invention, it is preferred to, the temperature of heating stirring described in step (2) is 60-80 DEG C.
In the present invention, it is preferred to, the temperature being dried described in step (3) is 100-120 DEG C；The xerogel pre-burning is
300-450 DEG C of pre-burning 3-5h.
In the present invention, it is preferred to, 700-900 DEG C of sintering 10-20h is sintered to described in step (4)；The ball milling dispersion
Time be 1-10h.
Further, the invention provides a kind of cathode material lithium vanadium phosphate of lithium ion battery/carbon, according to described lithium from
The preparation method of sub- battery positive pole material phosphoric acid vanadium lithium/carbon is prepared.
The Li of phosphoric acid vanadium lithium/carbon system monoclinic structure prepared by the present invention3V2(PO4)3, its space group is P2l/ n, does not go out
The diffraction maximum of existing miscellaneous peak or carbon, carbon is in the form of unformed.Phosphoric acid vanadium lithium/the carbon prepared using said method is combined
Material granule is tiny and even particle size distribution, and electric conductivity is significantly improved, with good charge-discharge performance.
Further, present invention also offers a kind of lithium ion battery, including described anode material for lithium-ion batteries
Phosphoric acid vanadium lithium/carbon.
A kind of lithium ion battery that the present invention is provided, including ion battery anode material vanadium lithium phosphate prepared by said method
Lithium/carbon, the barrier film between negative pole, both positive and negative polarity and electrolyte.
The present invention has investigated the charge-discharge performance of the lithium ion battery by anode material vanadium lithium phosphate/carbon assembling, discharge and recharge
Multiplying power is respectively 0.2C, 0.5C, 1C, 2C, 5C, 10C, 15C, and it is 3.2-4.3V that discharge and recharge is interval.As a result show：Lithium ion battery
Capacity can be maintained at 115mAh/g or so, by what is prepared as carbon source with phenolic resin and Kynoar (PVDF) respectively
The lithium ion battery of phosphoric acid vanadium lithium/carbon assembling to show and be above 90mAh/g under good high rate performance, 15C.And this
Bright lithium ion battery after the circulation of 25 different multiplyings again with 0.2C discharge and recharges once, lithium ion battery shows
Capacity be above circulating first.
The present invention has also investigated the cycle performance of the lithium ion battery by anode material vanadium lithium phosphate/carbon assembling, as a result table
Bright, the lithium ion battery of the present invention is circulated after 50 times under 5C, and the capacity of battery is decayed, good cycling stability,
It is suitable as anode material for lithium-ion batteries.Illustrate the phosphoric acid vanadium lithium/carbon for adopting preparation method of the present invention to obtain as positive electrode
Lithium ion battery there is excellent charge-discharge performance.
The present invention can realize raw material in the other uniform mixing of molecular level using sol-gal process so that reaction is filled
Dividing is carried out, and the sintering temperature of sol-gal process is relatively low, uniform small grains, is more beneficial for improving the chemical property of material.
And the method for adopting ball milling to aid in, various carbon sources, promotion simple and effective can be added to form uniform carbon coating layer, so as to improve
The electronic conductivity of positive electrode.Therefore the preparation method is that one kind effectively improves phosphoric acid vanadium lithium/carbon positive electrode electricity
The method of chemical property.
The present invention prepares the phosphoric acid vanadium lithium presoma with gap structure using sol-gal process, then auxiliary by ball milling
The method for helping adds carbon source, and the cladding of carbon-coating is carried out to material surface by solid-phase sintering.Gained lithium ion cell positive material
Material Li3V2(PO4)3With well-bedded gap, it is conducive to infiltration of the electrolyte to active material, and the expansion of lithium ion
Transmission is dissipated, the surface of active material is coated by carbon-coating, is conducive to improving and improving the electronic conductivity of material.
Compared with prior art, the method for the present invention has the advantages that：
Preparation method of the present invention by sol-gal process in combination with solid phase method, can prepare with good high rate performance
With the cathode material lithium vanadium phosphate of lithium ion battery/carbon of cycle performance, process is simple, applicable surface is extensive；Simultaneously the present invention is with height
Valency alum source compound is vanadium source, greatly reduces the cost of synthesis condition and raw material.
Description of the drawings
Accompanying drawing is to combine specific process embodiment, specifically understands technique trend.
Fig. 1 is the XRD spectrum of the sample obtained in embodiment of the present invention 1-4；
Fig. 2 is the high rate performance figure of the sample obtained in embodiment of the present invention 5-8；
Fig. 3 is the cycle performance figure of the sample obtained in embodiment of the present invention 5-8.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.
The present invention is not particularly limited to the negative material of lithium ion battery, preferable to bear for carbon based negative electrodes material, tinbase
Pole material, alloy type negative material.
The present invention is not particularly limited to diaphragm for lithium ion battery, considers from cost factor, preferably polyethylene diagrams
Or polypropylene diaphragm.
The present invention is not particularly limited to lithium-ion battery electrolytes, the non-water power that can be known to the skilled person
Solution liquid, preferably LiPF6Nonaqueous electrolytic solution.
Embodiment 1
In the present embodiment, the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon is comprised the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium carbonate, five oxygen
Change two vanadium, ammonium dihydrogen phosphate and oxalic acid；
(2) vanadic anhydride and oxalic acid are placed in deionized water dissolve and concurrently give birth to reduction reaction, question response is finished, and obtains clear
Clear blue solution, sequentially adds lithium carbonate and ammonium dihydrogen phosphate, and in 60 DEG C of stirrings it is well mixed, and then vacuum distillation is treated
Moisture is evaporated to form green gel；
(3) green gel is placed in into drying in 100 DEG C of drying boxes to be formed after xerogel, by xerogel in 300 DEG C of pre-burning 4h
Form precursor powder；
(4) after precursor powder is well mixed with sucrose, adding ethanol for dispersant carries out ball milling dispersion 2h, by ethanol
With 800 DEG C of sintering 14h in vacuum tube furnace after being evaporated, vanadium phosphate lithium/carbon composite material is obtained, the consumption of sucrose is to make phosphoric acid
The percentage by weight of carbon is 5% in vanadium lithium/carbon composite material.
Embodiment 2
In the present embodiment, the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon is comprised the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium nitrate, vanadic acid
Sodium, ammonium phosphate and citric acid；
(2) sodium vanadate and citric acid are placed in deionized water dissolve and concurrently give birth to reduction reaction, question response is finished, must clarified
Blue solution, sequentially adds lithium nitrate and ammonium phosphate, makes to be well mixed in 80 DEG C of stirrings, and then vacuum distillation treats that moisture is evaporated
Form green gel；
(3) green gel is placed in into drying in 120 DEG C of drying boxes to be formed after xerogel, by xerogel in 350 DEG C of pre-burning 4h
Form precursor powder；
(4) after precursor powder is well mixed with glucose, adding ether for dispersant carries out ball milling dispersion 5h, by second
Ether sinters 12h in vacuum tube furnace after being evaporated with 750 DEG C, obtains vanadium phosphate lithium/carbon composite material, and the consumption of sucrose is to make phosphorus
The percentage by weight of carbon is 10% in sour vanadium lithium/carbon composite material.
Embodiment 3
In the present embodiment, the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon is comprised the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium hydroxide, partially
Sodium vanadate, phosphoric acid and malic acid；
(2) sodium metavanadate and malic acid are placed in deionized water dissolve and concurrently give birth to reduction reaction, question response is finished, and obtains clear
Clear blue solution, sequentially adds lithium hydroxide and phosphoric acid, makes to be well mixed in 70 DEG C of stirrings, and then vacuum distillation treats that moisture steams
Form is into green gel；
(3) green gel is placed in into drying in 110 DEG C of drying boxes to be formed after xerogel, by xerogel in 350 DEG C of pre-burning 5h
Form precursor powder；
(4) after precursor powder is well mixed with phenolic resin, adding acetone for dispersant carries out ball milling dispersion 8h, will
Acetone sinters 16h in vacuum tube furnace after being evaporated with 750 DEG C, obtains vanadium phosphate lithium/carbon composite material, and the consumption of sucrose is to make
The percentage by weight of carbon is 8% in vanadium phosphate lithium/carbon composite material.
Embodiment 4
In the present embodiment, the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon is comprised the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium acetate, five oxygen
Change two vanadium, pyrophosphoric acid and oxalic acid；
(2) vanadic anhydride and oxalic acid are placed in deionized water dissolve and concurrently give birth to reduction reaction, question response is finished, and obtains clear
Clear blue solution, sequentially adds lithium acetate and pyrophosphoric acid, makes to be well mixed in 70 DEG C of stirrings, and then vacuum distillation treats that moisture steams
Form is into green gel；
(3) green gel is placed in into drying in 110 DEG C of drying boxes to be formed after xerogel, by xerogel in 400 DEG C of pre-burning 4h
Form precursor powder；
(4) after precursor powder is well mixed with Kynoar, ethanol is added to carry out ball milling dispersion for dispersant
10h, vanadium phosphate lithium/carbon composite material, the use of sucrose are obtained after ethanol is evaporated in vacuum tube furnace with 750 DEG C of sintering 18h
The percentage by weight of carbon is 8% in measuring to make vanadium phosphate lithium/carbon composite material.
Sample Jing X-ray diffraction analysis obtained by embodiment 1-4, analysis result are shown in into Fig. 1.From figure 1 it appears that pressing
According to Li in the sample of embodiment 1-4 design route synthesis3V2(PO4)3Each characteristic peak substantially, all diffraction maximums and Li3V2
(PO4)3PDF standard cards (97-016-1335) it is basically identical, it is known that the sample obtained by embodiment 1-4 is monoclinic crystal tying
The Li of structure3V2(PO4)3, its space group is P2l/ n, the diffraction maximum for miscellaneous peak or carbon do not occur, carbon is in the form of unformed.
Embodiment 5
According to mass ratio 8:1:The 1 positive electrode Li for weighing the acquisition of embodiment 13V2(PO4)3, binding agent PVDF and conductive agent
Acetylene black, adds and is coated in aluminum foil current collector after stirring in 1-METHYLPYRROLIDONE (NMP).Coated aluminium foil is existed
120 DEG C are dried after 6h the positive pole diaphragm for going out a diameter of 14mm in vacuum drying chamber.With carbon-based in the glove box of anhydrous and oxygen-free
Material is negative pole, and polypropylene Celgard240 is barrier film, the LiPF of 1mol/L6/EC+DMC+EMC(1:1:1, volume ratio) conduct
Electrolyte, assembles R2016 type button cells.
Embodiment 6
According to mass ratio 8:1:The 1 positive electrode Li for weighing the acquisition of embodiment 23V2(PO4)3, binding agent PVDF and conductive agent
Acetylene black, adds and is coated in aluminum foil current collector after stirring in 1-METHYLPYRROLIDONE (NMP).Coated aluminium foil is existed
120 DEG C are dried after 6h the positive pole diaphragm for going out a diameter of 14mm in vacuum drying chamber.With carbon-based in the glove box of anhydrous and oxygen-free
Material is negative pole, and polypropylene Celgard240 is barrier film, the LiPF of 1mol/L6/EC+DMC+EMC(1:1:1, volume ratio) conduct
Electrolyte, assembles R2016 type button cells.
Embodiment 7
According to mass ratio 8:1:The 1 positive electrode Li for weighing the acquisition of embodiment 33V2(PO4)3, binding agent PVDF and conductive agent
Acetylene black, adds and is coated in aluminum foil current collector after stirring in 1-METHYLPYRROLIDONE (NMP).Coated aluminium foil is existed
120 DEG C are dried after 6h the positive pole diaphragm for going out a diameter of 14mm in vacuum drying chamber.With carbon-based in the glove box of anhydrous and oxygen-free
Material is negative pole, and polypropylene Celgard240 is barrier film, the LiPF of 1mol/L6/EC+DMC+EMC(1:1:1, volume ratio) conduct
Electrolyte, assembles R2016 type button cells.
Embodiment 8
According to mass ratio 8:1:The 1 positive electrode Li for weighing the acquisition of embodiment 43V2(PO4)3, binding agent PVDF and conductive agent
Acetylene black, adds and is coated in aluminum foil current collector after stirring in 1-METHYLPYRROLIDONE (NMP).Coated aluminium foil is existed
120 DEG C are dried after 6h the positive pole diaphragm for going out a diameter of 14mm in vacuum drying chamber.With carbon-based in the glove box of anhydrous and oxygen-free
Material is negative pole, and polypropylene Celgard240 is barrier film, the LiPF of 1mol/L6/EC+DMC+EMC(1:1:1, volume ratio) conduct
Electrolyte, assembles R2016 type button cells.
Fig. 2 describes the charge-discharge performance of the R2016 type button cells of embodiment 5-8 assembling, and charge-discharge magnification is respectively
0.2C, 0.5C, 1C, 2C, 5C, 10C, 15C, it is 3.2-4.3V that discharge and recharge is interval.The R2016 type button cells of the assembling of embodiment 5
Capacity decline most fast, specific capacity is only 71mAh/g under 5C multiplying powers, and the capacity of the R2016 type button cells of the assembling of embodiment 6
The capacity of the R2016 type button cells assembled for 94mAh/g, embodiment 7 and 8 can keep 115mAh/g or so.The He of embodiment 7
8 (i.e. by the R2016 type knobs of the phosphoric acid vanadium lithium/carbon assembling for being prepared as carbon source with phenolic resin and Kynoar (PVDF) respectively
Button battery) to show and be above 90mAh/g under good high rate performance, 15C.After the circulation of 25 different multiplyings
Again with 0.2C discharge and recharges once, the capacity that embodiment 5-6 and the R2016 type button cells of the assembling of embodiment 8 show is above
Circulate first, this should be the reason that the reactivity of lithium ion is enhanced after circulating for several times.
Fig. 3 is the cycle performance of the R2016 type button cells of embodiment 5-8 assembling, and the little figure in Fig. 3 is embodiment 5-8
Charging and discharging curve of the R2016 types button cell of assembling under 5C.As can be seen from Figure 3 circulate under 5C after 50 times, it is real
Apply a capacity for the R2016 type button cells of 5-8 assemblings to decay.
In sum, the present invention can realize raw material in the other uniform mixing of molecular level using sol-gal process so that
Reaction is fully carried out, and the sintering temperature of sol-gal process is relatively low, uniform small grains, is more beneficial for improving the electricity of material
Chemical property.And the method for adopting ball milling to aid in, various carbon sources, promotion simple and effective can be added to form uniform carbon coating
Layer, so as to improve the electronic conductivity of positive electrode.Therefore the preparation method in the present invention be one kind effectively improve phosphoric acid vanadium lithium/
The approach of carbon positive electrode chemical property.
Those of ordinary skill in the art should be understood：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and there is the different aspect of the present invention as above
Many other changes, in order to it is simple and clear they provide without in details.Therefore, it is all within the spirit and principles in the present invention,
Any omission, modification, equivalent, improvement for being made etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon, it is characterised in that comprise the following steps：
(1) it is 3.05 by the mol ratio of elemental lithium, v element, P elements and reducing agent:2:3:3 weigh lithium source, vanadium source, phosphorus source and
Reducing agent；
(2) vanadium source and reducing agent are placed in deionized water dissolve and concurrently give birth to reduction reaction, sequentially add lithium source and phosphorus source, plus
Thermal agitation is well mixed it, treats that moisture is evaporated to form green gel；
(3) green gel is dried to be formed after xerogel, xerogel pre-burning is formed into precursor powder；
(4) after precursor powder is well mixed with carbon source, add dispersant to carry out ball milling dispersion, burn after dispersant is evaporated
Knot, obtains vanadium phosphate lithium/carbon composite material；The consumption of the carbon source is the weight hundred for making carbon in vanadium phosphate lithium/carbon composite material
Divide than being 5-10%.
2. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The lithium source is the one kind in lithium nitrate, lithium hydroxide, lithium carbonate, lithium fluoride, lithium dihydrogen phosphate or lithium acetate；The vanadium source is
One kind in vanadic anhydride, sodium vanadate or sodium metavanadate；Phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphorus
One kind in acid or pyrophosphoric acid；The reducing agent is the one kind in citric acid, ascorbic acid, oxalic acid or malic acid.
3. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The carbon source includes organic carbonaceous material and macromolecule carbonaceous material.
4. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 3, it is characterised in that
The organic carbonaceous material is the one kind in glucose, sucrose or stearic acid；The macromolecule carbonaceous material is polyvinyl alcohol, ring
One kind in oxygen tree fat, phenolic resin or Kynoar.
5. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The dispersant is the one kind in acetone, ethanol or ether.
6. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The temperature of heating stirring described in step (2) is 60-80 DEG C.
7. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The temperature being dried described in step (3) is 100-120 DEG C；The xerogel pre-burning is 300-450 DEG C of pre-burning 3-5h.
8. the preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon according to claim 1, it is characterised in that
The ball milling scattered time described in step (4) is 1-10h, described to be sintered to 700-900 DEG C of sintering 10-20h.
9. a kind of cathode material lithium vanadium phosphate of lithium ion battery/carbon, it is characterised in that according to any one of claim 1-8
The preparation method of cathode material lithium vanadium phosphate of lithium ion battery/carbon prepare.
10. a kind of lithium ion battery, it is characterised in that including the ion battery anode material vanadium lithium phosphate described in claim 9
Lithium/carbon.
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