CN102386412A - Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof - Google Patents
Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof Download PDFInfo
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- CN102386412A CN102386412A CN2011103566563A CN201110356656A CN102386412A CN 102386412 A CN102386412 A CN 102386412A CN 2011103566563 A CN2011103566563 A CN 2011103566563A CN 201110356656 A CN201110356656 A CN 201110356656A CN 102386412 A CN102386412 A CN 102386412A
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Abstract
The invention relates to a lithium ion battery anode Li3V2(PO4)3/C composite material and a preparation method thereof. In the method, a precursor solution of Li3V2(PO4)3/C can penetrate into a porous structure of a Ketjen Black (KB) porous carbon and then the porous structure is roasted to obtain the product. The Li3V2(PO4)3 particles in the Li3V2(PO4)3/C composite material prepared by the method in the invention has small size, meanwhile, the reaction temperature is low, the reaction time is short and the cost is low. The Li3V2(PO4)3 and carbon nano composite material can be used as an anode for the lithium ion battery, thus having better electrochemical performance.
Description
Technical field
The present invention relates to a kind of lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material and preparation method thereof.
Background technology
Rechargeable lithium ion batteries has extended cycle life because its energy density is high, is widely used in the various portable electronic products, and like notebook computer, mobile phone etc.Be applied in electric automobile and the energy storage device at present.The performance of lithium ion battery largely depends on the material property of battery, like positive electrode, negative material etc.Lithium and cobalt oxides is successfully commercially produced, but cost is higher, the cobalt resource shortage, and bigger toxicity is arranged.Develop new anode material of lithium battery and become necessary.China's vanadium resource is abundant, accounts for 1/5th of world's vanadium reserves.The synthetic good Li of chemical property
3V
2(PO
4)
3Positive electrode has important society and economic benefit.
Recently, lithium transition metal phosphates is like LiFePO
4, LiMnPO
4And Li
3V
2(PO
4)
3Deng because their excellent electrochemistry and thermal stability, caused researchers' interest greatly as the positive electrode of lithium ion battery.Li
3V
2(PO
4)
3Three-dimensional structure is by the VO of slight distortion
6Octahedron and PO
4Tetrahedron, and the Li composition that is positioned at position, big space.Because PO
4Big space has been created in the unit, allows the three-dimensional rapid diffusion of ion, and this structure has good ion ducting capacity.(reference is in Li/Li 3.0 to 4.8V
+) the interior charging of voltage range, 3 reversible lithium ions can be deviate from completely, and theoretical capacity can reach 197mAh g
-1, this value is the highest in lithium transition metal phosphates.But Li
3V
2(PO
4)
3The conductive capability of material itself is relatively poor, has seriously influenced its high rate performance.Metal-doped, charcoal coating etc. is used to improve the combination property of material.The synthetic material of these methods has all shown higher specific capacity and better cyclical stability.But the performance of these materials also has certain distance from practical application.According to Fick ' s law, square be directly proportional with the diffusion distance diffusion time.The distance that the size that reduces particle shortens lithium ion diffusion and electric transmission can improve the high rate performance of material.Therefore, adopt a kind of easier, and the Li of method synthesis of nano size that can large-scale production
3V
2(PO
4)
3The composite material of particle and charcoal has research and is worth and using value.
Summary of the invention
The purpose of this invention is to provide a kind of lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material and preparation method thereof.
A kind of lithium ion cell positive Li
3V
2(PO
4)
3The preparation method of/C composite material: according to stoichiometric proportion, adopt vanadium oxalate, the lithium source, the phosphorus source is a raw material, in the aqueous solution, fully stirs; Add the Ketjen Black porous carbon material that accounts for composite material weight 5%-40% then, heating (temperature is no more than 900 ℃) is fully stirred and is obtained viscous mixture; This mixture (grinds up to can't see tangible blocky-shaped particle) after the grinding through drying, roasting, and take out the cooling back, grinds and obtain lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material, Li in the described composite material
3V
2(PO
4)
3Particle is not more than 300 nanometers.
Described lithium source comprises lithium hydroxide, lithium acetate, lithium carbonate, lithium fluoride, the mixing of one or more in lithium nitrate, lithium iodide, lithium bromide, LiBF4, the lithium oxalate.
Described phosphorus source comprises one or more the mixing in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, the phosphorus pentoxide.
The roasting in protective atmosphere of described mixture, protective atmosphere are nitrogen or argon gas, or the mist of hydrogen and argon gas.
Described grinding all is on stirring ball mill, circulating agitating ball mill, sand mill, planetary ball mill, high energy mechanical ball mill or mortar, to carry out.
Adopt vanadium oxalate in the said method, lithium source, phosphorus source are raw material, and wherein, the mol ratio of Li/V/P is 3: 2: 3.
Mixture is dry in the said method, after the grinding, and compressing tablet; Predecomposition 1～8 hour under 300～400 ℃ of temperature protection property atmosphere earlier, again 650～900 ℃ of temperature, roasting is 2～16 hours under the protective atmosphere; Take out the cooling back, grinds, and obtains lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material.
A kind of lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material is to be prepared from above-mentioned method.
Ketjen Black porous charcoal (being called for short the KB charcoal) is a kind of conduction charcoal, and good dispersive property is arranged in the solution of aqueous systems, and specific area is high, and the aperture is bigger, at Li
3V
2(PO
4)
3In/C the composite material, must not be application.Can be good in the KB charcoal aqueous systems separately, with the solution absorption of presoma in porous charcoal.In the preparation process of material, can well the limits particle reunion grow up, also can improve the electron transport ability of electrode material simultaneously.This method is synthesized Li
3V
2(PO
4)
3/ C nano composite material has good high-rate discharge ability and cyclical stability.While KB charcoal low price, this method is synthetic easy, is fit to large-scale production.
Description of drawings
Synthetic Li among Fig. 1 embodiment 1
3V
2(PO
4)
3XRD figure spectrum with Ketjen Black carbon composite;
The Li that synthesizes among Fig. 2 embodiment 1
3V
2(PO
4)
3TEM collection of illustrative plates with Ketjen Black carbon composite;
The Li that synthesizes among Fig. 3 embodiment 1
3V
2(PO
4)
3With the cyclic voltammetry curve of Ketjen Black carbon composite, voltage range is 3-4.3Vvs.Li/Li
+, sweep speed is 0.1mV s
-1
The Li that synthesizes among Fig. 4 embodiment 1
3V
2(PO
4)
3With the cycle performance curve of Ketjen Black carbon composite, the voltage tester scope is 3-4.3V vs.Li/Li
+, 1C=140mA g
-1
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1
With VOC
2O
4Join in the deionized water, magnetic agitation is up to forming blue solution; Then, NH
4H
2PO
4, Li
2CO
3Join in the above-mentioned solution and stirred one hour, the mol ratio of Li/V/P is 3: 2: 3; The KB charcoal adds in the above-mentioned mixed solution then.Form up to slimy mixture 80 ℃ of heated and stirred, obtain dry solid 80 ℃ of dried overnight afterwards.The KB charcoal adds according to the ratio that it in the end accounts for 20% in the composite material.The particle process that obtains is milled, compressing tablet, and at 96%Ar, 4%H
2Mixed gas protected following 350 ℃ of calcinings 4 hours.The sample of the gained compressing tablet of milling again more afterwards, calcining is 8 hours under 800 ℃ of same atmosphere, the cooling back grind (grinding) up to can't see tangible blocky-shaped particle Li to the end
3V
2(PO
4)
3/ C composite material.Li
3V
2(PO
4)
3/ C composite material and PVDF bonding agent mix according to 90: 10 weight ratio, in N-crassitude ketone solvent, disperse to obtain starchy mixture then.Active material (Li in this mixture
3V
2(PO
4)
3The ratio of)/charcoal/bonding agent is 72: 18: 10.Paste mixture is coated on the aluminium foil, vacuumizes dried overnight at 100 ℃.The tap density of composite material is approximately 0.6g ml
-1, the quality of unit are is loaded as 1-2mgcm on the aluminium foil
-2((MBraun Inc.) carries out the glove box of having filled high-purity argon gas that is assembled in Canada) half-cell for 2325 button cells, National Research council.Polypropylene screen (Celgard 3501) is as barrier film, and the lithium metal is as negative pole, 1M LiPF
6Be dissolved in ethyl carbonate and the dimethyl carbonate of 1: 1 volume mixture as electrolyte.(Arbin Instruments, College Station carry out on TX) the Arbin cell tester BT-2000 that is evaluated at of chemical property.At room temperature, the test of half-cell high rate performance is carried out in 3 to 4.3V voltage ranges.The specific capacity of supposing the 1C discharge is 140mAh g
-1
That Fig. 1 shows is Li
3V
2(PO
4)
3The XRD figure spectrum of/C composite material, main XRD diffraction maximum index marks, and coincide Li with card 01-072-7074
3V
2(PO
4)
3Be monocline, belong to the P21/n space group.The XRD figure spectrum does not show the peak of other phases, explains that the charcoal in the composite material exists with unbodied state.Fig. 2 has provided these nano particles and has been embedded in TEM image in the KB carbon matrix.Particle diameter is approximately 20nm, and these nano particles contact fine with carbon matrix simultaneously.The structure of this novelty means and is penetrated into precursor solution in the matrix of porous charcoal, and in the synthetic process of high temperature, porous charcoal is growing up of limits particle effectively, thereby obtain Li
3V
2(PO
4)
3/ C nano composite material.
Fig. 3 is Li
3V
2(PO
4)
3The cyclic voltammetry curve of/C composite material.Can see be positioned at 3.62,3.70 and 4.12V (reference is in Li/Li
+) three oxidation peak, this has reflected Li
+Ion is from Li
3V
2(PO
4)
3Deviate to have passed through a plurality of steps in the basis material, simultaneously Li
xV
2(PO
4)
3Experienced from x=3.0 to 2.5 2.0 and 1.0 transformation.First lithium ion take off Li
+Process has experienced two steps, and this is because the centre exists an orderly Li
2.5V
2(PO
4) phase, the valence state of V is V
3+/ V
4+Mixed valence.Take off the lithium process at the observed platform of 4.12V corresponding to the single step of second lithium ion subsequently.Corresponding V
3+Also become V fully
4+Corresponding seeing is positioned at 4.0V, the reduction peak of 3.63V and 3.55V, Li
xV
2(PO
4)
3Also be transformed into 2,2.5 and 3.0 mutually by x=1.
Fig. 4 is that combination electrode arrives cycle performance curve in the voltage range of 4.3V 3, and the ratio discharge capacity of first week circulation is 122mAh g
-1This numeric ratio bibliographical information do not introduce porous KB charcoal synthetic material in the precursor solution, (the 110mA h g of the capacity under the C/5 multiplying power
-1) want high.After 1C circulated for 22 weeks, still can obtain 120mA h g
-1The ratio discharge capacity.In the 2C discharge, the 1C charging does not reduce than discharge capacity then.When under 4C and 8C multiplying power, discharging, their ratio discharge capacity is respectively 118,115mA h g
-1We find that from 1C to the 8C multiplying power discharging, the difference of the ratio discharge capacity of composite material has only 5mAh g
-1Even in 16C and 32C discharge, still can obtain respectively 105 with 83mA h g
-1The ratio discharge capacity.In the 80th week, in the 1C discharge, the ratio discharge capacity of composite material is 119mAh g again
-1, ratio discharge capacity (the 120mAh g that this numerical value obtains when discharging and recharging with the 22nd all 1C
-1) be more or less the same.
Embodiment 2
Lithium source Li among the embodiment 1
2CO
3Use CH
3The COOLi replacement, other conditions remain unchanged, and the composite property of preparation is still fine.
Embodiment 3
Protective atmosphere among the embodiment 1 is replaced with pure Ar, and other conditions remain unchanged, and the composite property of preparation is still fine.
Claims (8)
1. lithium ion cell positive Li
3V
2(PO
4)
3The preparation method of/C composite material is characterized in that, according to stoichiometric proportion, adopts vanadium oxalate, the lithium source, and the phosphorus source is a raw material, in the aqueous solution, fully stirs; Add the Ketjen Black porous carbon material that accounts for composite material weight 5%-40% then, heating is fully stirred and is obtained viscous mixture; This mixture is through drying, and after the grinding, roasting is taken out after the cooling, grinds and obtains lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material, Li in the described composite material
3V
2(PO
4)
3Particle be not more than 300 nanometers.
2. according to the described preparation method of claim 1, it is characterized in that described lithium source comprises lithium hydroxide, lithium acetate, lithium carbonate, lithium fluoride, the mixing of one or more in lithium nitrate, lithium iodide, lithium bromide, LiBF4, the lithium oxalate.
3. preparation method according to claim 1 is characterized in that, described phosphorus source comprises one or more the mixing in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, the phosphorus pentoxide.
4. preparation method according to claim 1 is characterized in that, the roasting in protective atmosphere of described mixture, and protective atmosphere is nitrogen or argon gas, or the mist of hydrogen and argon gas.
5. preparation method according to claim 1 is characterized in that, described grinding all is on stirring ball mill, circulating agitating ball mill, sand mill, planetary ball mill, high energy mechanical ball mill or mortar, to carry out.
6. preparation method according to claim 1 is characterized in that, adopts vanadium oxalate, and lithium source, phosphorus source are raw material, and wherein, the mol ratio of Li/V/P is 3: 2: 3.
7. preparation method according to claim 1 is characterized in that, mixture is dry; After the grinding, compressing tablet, predecomposition 1～8 hour under 300～400 ℃ of temperature protection property atmosphere earlier; 650～900 ℃ of temperature, roasting is 2～16 hours under the protective atmosphere again, and take out the cooling back; Grind, obtain lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material.
8. lithium ion cell positive Li
3V
2(PO
4)
3/ C composite material is characterized in that, is prepared from any described method of claim 1-7.
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| CN2011103566563A CN102386412A (en) | 2011-11-11 | 2011-11-11 | Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104466181A (en) * | 2014-12-05 | 2015-03-25 | 福建师范大学 | Preparation method of high-performance lithium ion power battery/porous carbon composite positive electrode material |
| CN105036104A (en) * | 2015-08-18 | 2015-11-11 | 东南大学 | Preparation method of lithium vanadium phosphate by high-energy ball milling |
| CN106684353A (en) * | 2016-12-27 | 2017-05-17 | 深圳市川马电子股份有限公司 | Preparation method for carbon-coated potassium vanadium phosphate and application of carbon-coated potassium vanadium phosphate |
| CN106876707A (en) * | 2017-04-05 | 2017-06-20 | 宁波力赛康新材料科技有限公司 | A kind of solid lithium battery |
| CN106935821A (en) * | 2017-03-16 | 2017-07-07 | 湖南工业大学 | A kind of phosphoric acid vanadium lithium composite positive pole with porous foam and preparation method thereof |
| CN107482181A (en) * | 2017-07-10 | 2017-12-15 | 三峡大学 | A kind of anode material for compound lithium ion battery Li3V2(PO4)3/ C and preparation method thereof |
| CN107492634A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof |
| CN107706412A (en) * | 2017-10-18 | 2018-02-16 | 青海民族大学 | A kind of method of the zeolite imidazole ester skeletal porous carbon coating vanadium phosphate cathode materials of ZIF 8 |
| CN110649263A (en) * | 2019-10-22 | 2020-01-03 | 华南理工大学 | Nickel-ion battery lithium vanadium phosphate positive electrode material, sol-gel preparation method and application |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104466181A (en) * | 2014-12-05 | 2015-03-25 | 福建师范大学 | Preparation method of high-performance lithium ion power battery/porous carbon composite positive electrode material |
| CN105036104A (en) * | 2015-08-18 | 2015-11-11 | 东南大学 | Preparation method of lithium vanadium phosphate by high-energy ball milling |
| CN106684353A (en) * | 2016-12-27 | 2017-05-17 | 深圳市川马电子股份有限公司 | Preparation method for carbon-coated potassium vanadium phosphate and application of carbon-coated potassium vanadium phosphate |
| CN106935821A (en) * | 2017-03-16 | 2017-07-07 | 湖南工业大学 | A kind of phosphoric acid vanadium lithium composite positive pole with porous foam and preparation method thereof |
| CN106935821B (en) * | 2017-03-16 | 2019-12-06 | 湖南工业大学 | lithium vanadium phosphate composite cathode material with porous foam and preparation method thereof |
| CN106876707A (en) * | 2017-04-05 | 2017-06-20 | 宁波力赛康新材料科技有限公司 | A kind of solid lithium battery |
| CN107482181A (en) * | 2017-07-10 | 2017-12-15 | 三峡大学 | A kind of anode material for compound lithium ion battery Li3V2(PO4)3/ C and preparation method thereof |
| CN107492634A (en) * | 2017-07-10 | 2017-12-19 | 三峡大学 | A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof |
| CN107492634B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | binder-free Li3V2(PO4)3/C composite lithium ion battery anode and preparation method thereof |
| CN107482181B (en) * | 2017-07-10 | 2019-12-06 | 三峡大学 | Composite lithium ion battery anode material Li3V2(PO4)3/C and preparation method thereof |
| CN107706412A (en) * | 2017-10-18 | 2018-02-16 | 青海民族大学 | A kind of method of the zeolite imidazole ester skeletal porous carbon coating vanadium phosphate cathode materials of ZIF 8 |
| CN110649263A (en) * | 2019-10-22 | 2020-01-03 | 华南理工大学 | Nickel-ion battery lithium vanadium phosphate positive electrode material, sol-gel preparation method and application |
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Application publication date: 20120321 |