CN107492634A - A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof - Google Patents
A kind of binder free Li3V2(PO4)3/ C compound potassium ion battery plus plates and preparation method thereof Download PDFInfo
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- CN107492634A CN107492634A CN201710556602.9A CN201710556602A CN107492634A CN 107492634 A CN107492634 A CN 107492634A CN 201710556602 A CN201710556602 A CN 201710556602A CN 107492634 A CN107492634 A CN 107492634A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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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
- 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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- 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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- 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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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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Abstract
The present invention provides a kind of middle liquid phase process and prepares carbon compound phosphoric acid vanadium lithium binder free positive pole, comprise the concrete steps that weigh lithium source, vanadium is come from small beaker, add deionized water, stirring 20min is completely dissolved to it, transfer them in hydro-thermal inner bag, deionized water is added to the 80% of inner bag volume, 12 ~ 48h of hydro-thermal in 100 ~ 180 DEG C of convection oven.Phosphorus source and organic carbon source are weighed in beaker, deionized water is added, stirring 20min is completely dissolved to it, the interphase liquid after natural cooling is slowly dropped to dissolved with the beaker of phosphorus source and organic carbon source afterwards, stirring 20min becomes orange-yellow to solution, and heating is concentrated into certain volume.Carbon base body is immersed in liquid phase presoma 14 hours afterwards, and dried in 60 DEG C of convection oven in 24 ~ 36h.By the 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere of the carbon base body after drying, 6 ~ 12h is calcined at 650 ~ 850 DEG C, binder free Li is obtained after natural cooling3V2(PO4)3/ C electrodes, preferable chemical property is shown using it as lithium ion cell positive.
Description
Technical field
The present invention relates to a kind of high-performance binder free lithium ion cell positive, more particularly to a kind of Li3V2(PO4)3/ C is multiple
Condensation material electrode preparation method, belongs to field of electrochemical power source.
Technical background
Lithium ion battery is because having the advantages that high-energy-density, high safety performance, low self-discharge, long-life, memoryless, mesh
Before become the main power source of mancarried electronic aid.Meanwhile it is also regarded as following electric automobile, field operation communication, large-scale energy storage electricity
The ideal source stood.The research and development of high performance lithium ion battery are always the important topic of domestic and international battery enterprise and institute,
Determine that the key of its success or failure is the research and application of high-performance lithium ion electrode.
Traditional electrode preparation technology is by mixing, and being coated in metal collector active material, conductive agent, binding agent
On.The introducing of conductive agent, binding agent will increase battery weight, reduce the energy density of battery.And active material and conductive afflux
By conductive agent mediate contact between body, electronic transmission process in electrode will be directly affected, so as to limit battery high rate performance.Pass through
Electrode material is grown directly upon in conductive current collector by growth in situ mode, can not only be remarkably reinforced active material and collector
Electrical contact, and conductive agent, the capacitance loss caused by binding agent can be effectively reduced, so as to be obviously improved the property of battery
Energy.At present, in conductive current collector growth in situ lithium ion battery negative material report it is more, but on direct growth
The report of positive electrode is actually rare.Existing positive electrode is mainly multicomponent system, including cobalt acid lithium, LiMn2O4, LiFePO4
And ternary material etc., preparation method are mostly solid phase reaction method, course of reaction is complex.On the one hand, multicomponent material is difficult
Good contact is kept with conducting base, realizes growth in situ；On the other hand, it is difficult to realize uniform anti-between a variety of reaction raw materials
Should, so as to obtain uniform positive electrode.
Li3V2(PO4)3It is a kind of novel anode material, there is higher charge and discharge platform and reversible capacity（Voltage is in 3-
Theoretical capacity is 133 mAh g during 4.3V-1）, and there is preferable heat endurance and cost advantage, there is stronger practical valency
Value.A kind of middle liquid phase process of invention, prepare Li3V2(PO4)3/ C binder free positive poles.On the one hand, middle liquid phase tool
There is higher toughness, be advantageous to its uniform adsorption on carbon base body；On the other hand, middle liquid phase can be realized between reactant
Uniform mixing, obtain the Li of size uniform3V2(PO4)3Particle；Meanwhile middle liquid phase is advantageous to carbon source introducing, drying course
Middle interphase liquid crystallization can induce organic carbon source molecule to be carbonized in its surface uniform adsorption and in subsequent solid phase reaction situ,
Realize Li3V2(PO4)3It is uniformly multiple in micro-scale with C.Finally, prepared binder free Li3V2(PO4)3/ C electrodes are as lithium
Ion battery positive pole shows excellent chemical property.
The content of the invention
The present invention relates to a kind of preparation method of lithium ion cell positive, electrode Li3V2(PO4)3/ C growth in situ is in carbon
Composite construction on matrix.Active material is Li3V2(PO4)3/ C composite, it is made up of average-size about 100nm particle.
Specific preparation method step is as follows：A certain amount of lithium source, vanadium source, hexamethylenetetramine are dissolved in deionized water, stir 30min
Fully dissolved to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water to the 80% of inner bag volume, it
12 ~ 48h of hydro-thermal in 100 ~ 180 DEG C of convection oven, natural cooling obtain interphase liquid afterwards.Weigh a certain amount of carbon source and
Phosphorus source is dissolved in deionized water, and stirring 20min fully dissolves to it, and the interphase liquid after cooling is slowly added dropwise afterwards, is added dropwise
After stir 30min to color in orange-yellow.Liquid is dried to different volumes concentration in 60 DEG C of convection oven afterwards；Will
1-4 hours in liquid obtained by carbon base body immersion after concentration, and dried in 60 DEG C of convection oven in 24 ~ 36h.After drying
Carbon base body 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere, 6 ~ 12h is calcined at 650 ~ 850 DEG C, soap-free emulsion polymeization is obtained after natural cooling
Agent Li3V2(PO4)3/ C electrodes.
Described lithium, vanadium, the mol ratio of phosphorus and hexamethylenetetramine are 3：2：3：2~10.Described carbon source accounts for gross mass
0~10%.Described lithium source is lithium carbonate, lithium hydroxide, lithium acetate or lithium oxalate, and vanadium source is vanadic anhydride or inclined alum acid ammonium,
Phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate, and carbon source is citric acid, glucose, sucrose or ascorbic acid.
Binder free Li involved in the present invention3V2(PO4)3Preparation method, structure and the performance of/C electrodes have following several
Individual outstanding feature：
（1）Electrode synthesis technique is simple, easily operated, reproducible；
（2）Li3V2(PO4)3/ C and carbon-based bluk recombination are uniform, and contact is good；
（3）Prepared Li3V2(PO4)3/ C is granule-morphology, average-size about 200nm；
（4）Li obtained by the present invention3V2(PO4)3/ C binder frees electrode can be directly used as lithium ion cell positive, show
Preferable cycle performance and higher specific capacity.
Brief description of the drawings
The SEM figures of sample prepared by Fig. 1 embodiments 1.
The preceding charging and discharging curve figure three times of sample prepared by Fig. 2 embodiments 1（a）And cycle performance figure（b）.
The cycle performance figure of sample prepared by Fig. 3 embodiments 2.
The cycle performance figure of sample prepared by Fig. 4 embodiments 3.
Embodiment
Embodiment 1
3mmol lithium carbonates, 2mmol vanadic anhydrides, 5mmol hexamethylenetetramines is weighed to be dissolved in equipped with the small of 20mL deionized waters
In beaker, stirring 30min fully dissolves to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water is extremely
The 80% of inner bag volume, the hydro-thermal 24h in 120 DEG C of convection oven, natural cooling obtain interphase liquid afterwards.Weigh 0.05g
Citric acid and 6mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, it
The interphase liquid after cooling is slowly added dropwise into beaker afterwards, 30min is stirred after being added dropwise to color in orange-yellow.Afterwards will
It is original half that liquid is dried to volume concentration in 60 DEG C of convection oven in beaker, by grapheme foam immersion after concentration
2 hours in gained liquid, and dried in 60 DEG C of convection oven in 30h.By the grapheme foam after drying in nitrogen atmosphere
Lower 350 DEG C of pre-burning 4h, and 8h is calcined at 750 DEG C, binder free Li is obtained after natural cooling3V2(PO4)3/ C electrodes.To sample
SEM signs, as seen from Figure 1, Li are carried out3V2(PO4)3/ C homoepitaxials are in graphenic surface, by size about 100nm's
Particle forms.Above-mentioned electrode is cut into 1 × 1 cm sizes, 12h is dried in vacuo at 120 DEG C.Using metal lithium sheet as to electrode,
Celgard films are barrier film, dissolved with LiPF6EC+DEC (the volume ratios 1 of (1mol/L):1) solution is electrolyte,
CR2025 type batteries are assembled into the glove box of argon gas protection.Battery pack stands 8h after installing, then with CT2001A battery testings system
System carries out constant current charge and discharge test, test voltage 3-4.3V.Fig. 2 shows, the Li prepared by embodiment 13V2(PO4)3/C
Charge and discharge capacity is respectively 134.6 and 109.3 mAh/g to binder free electrode first, charge and discharge capacity after 100 circulations
Respectively 109.8 and 109 mAh/g, it is shown that preferable chemical property.
Embodiment 2
3mmol lithium oxalates, 2mmol vanadic anhydrides, 5mmol hexamethylenetetramines is weighed to be dissolved in equipped with the small of 20mL deionized waters
In beaker, stirring 30min fully dissolves to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water is extremely
The 80% of inner bag volume, the hydro-thermal 24h in 120 DEG C of convection oven, natural cooling obtain interphase liquid afterwards.Weigh 0.05g
Glucose and 6mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, it
The interphase liquid after cooling is slowly added dropwise into beaker afterwards, 30min is stirred after being added dropwise to color in orange-yellow.Afterwards will
It is original half that liquid is dried to volume concentration in 60 DEG C of convection oven in beaker, by liquid obtained by carbon cloth immersion after concentration
2 hours in body, and dried in 60 DEG C of convection oven in 30h.By the 350 DEG C of pre-burnings in a nitrogen atmosphere of the carbon cloth after drying
4h, and 8h is calcined at 750 DEG C, binder free Li is obtained after natural cooling3V2(PO4)3/ C electrodes.In the way of embodiment 1
Assembled battery.Fig. 3 shows, the Li prepared by embodiment 23V2(PO4)3Charge and discharge capacity is respectively/C binder frees electrode first
133.3 and 121.3 mAh/g, charge and discharge capacity is respectively 119 and 119.1 mAh/g after 90 circulations, it is shown that preferably
Chemical property.
Embodiment 3
3mmol lithium hydroxides, 2mmol ammonium metavanadates, 5mmol hexamethylenetetramines is weighed to be dissolved in equipped with the small of 20mL deionized waters
In beaker, stirring 30min fully dissolves to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water is extremely
The 80% of inner bag volume, the hydro-thermal 24h in 120 DEG C of convection oven, natural cooling obtain interphase liquid afterwards.Weigh 0.03g
Citric acid and 3mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, it
The interphase liquid after cooling is slowly added dropwise into beaker afterwards, 30min is stirred after being added dropwise to color in orange-yellow.Afterwards will
It is original half that liquid is dried to volume concentration in 60 DEG C of convection oven in beaker, by liquid obtained by carbon paper immersion after concentration
2 hours in body, and dried in 60 DEG C of convection oven in 30h.By the 350 DEG C of pre-burnings in a nitrogen atmosphere of the carbon paper after drying
4h, and 8h is calcined at 750 DEG C, binder free Li is obtained after natural cooling3V2(PO4)3/ C electrodes.In the way of embodiment 1
Assembled battery.Fig. 3 shows, the Li prepared by embodiment 33V2(PO4)3/ C binder frees electrode first distinguish by charge and discharge capacity
For 142.1 and 111.7 mAh/g, charge and discharge capacity is respectively 93.5 and 92.1 mAh/g after 90 circulations, it is shown that preferably
Chemical property.
Claims (4)
- A kind of 1. binder free lithium ion battery Li3V2(PO4)3/ C combination electrodes, its pattern are compound pattern, are by grain fraction Li3V2(PO4)3/ C homoepitaxials are on carbon base body, it is characterised in that the preparation technology of the binder free electrode is as follows：（1）Lithium source, vanadium source, hexamethylenetetramine are weighed in container, deionized water is added, it is complete to its to be sufficiently stirred 20min Dissolving, the solution dissolved is transferred in hydro-thermal inner bag, and addition deionized water is to the 80% of inner bag volume, afterwards 100 ~ 180 DEG C convection oven in 12 ~ 48h of hydro-thermal；（2）Phosphorus source and carbon source are weighed in container, adds deionized water, 20min is sufficiently stirred and is completely dissolved to it, by step （1）Interphase liquid after hydro-thermal cooling is added dropwise in the mixed solution of phosphorus source and carbon source, and 30min is stirred after dripping to liquid In orange-yellow, liquid is dried to different volumes concentration in 60 DEG C of convection oven；（3）Carbon base body is immersed in step（2）1-4 hours in middle gained liquid, and in 24 ~ 36h in 60 DEG C of convection oven Drying, by the 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere of the carbon base body after immersion, 6 ~ 12h is calcined at 650 ~ 850 DEG C, it is naturally cold But binder free Li is obtained afterwards3V2(PO4)3/ C electrodes.
- 2. binder free lithium ion battery Li according to claim 13V2(PO4)3The preparation method of/C combination electrodes, it is specialSign is, lithium, vanadium, the mol ratio of phosphorus and hexamethylenetetramine are 3：2：3：2 ~ 10, described carbon source account for gross mass 0 ~ 10%。
- 3. binder free lithium ion battery Li according to claim 13V2(PO4)3The preparation method of/C combination electrodes, it is special SignIt is, described lithium source is lithium carbonate, lithium hydroxide, lithium acetate or lithium oxalate, and vanadium source is vanadic anhydride or inclined alum acid Ammonium, phosphorus source are ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate, and carbon source is citric acid, glucose, sucrose or ascorbic acid.
- 4. binder free lithium ion battery Li according to claim 13V2(PO4)3The preparation method of/C combination electrodes, it is special Sign is that described carbon base body can be：Grapheme foam, carbon cloth or carbon paper.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102386412A (en) * | 2011-11-11 | 2012-03-21 | 中南大学 | Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof |
| CN104779393A (en) * | 2015-04-15 | 2015-07-15 | 河北民族师范学院 | Method for preparing lithium-vanadium-phosphate lithium ion battery positive material by means of liquid phase reduction |
| CN104868119A (en) * | 2015-04-16 | 2015-08-26 | 三峡大学 | Binder-free Li3VO4/C lithium ion battery cathode material and preparation method thereof |
| CN106654218A (en) * | 2017-01-11 | 2017-05-10 | 湖南文理学院 | Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and lithium ion battery |
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- 2017-07-10 CN CN201710556602.9A patent/CN107492634B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102386412A (en) * | 2011-11-11 | 2012-03-21 | 中南大学 | Lithium ion battery anode Li3V2(PO4)3/C composite material and preparation method thereof |
| CN104779393A (en) * | 2015-04-15 | 2015-07-15 | 河北民族师范学院 | Method for preparing lithium-vanadium-phosphate lithium ion battery positive material by means of liquid phase reduction |
| CN104868119A (en) * | 2015-04-16 | 2015-08-26 | 三峡大学 | Binder-free Li3VO4/C lithium ion battery cathode material and preparation method thereof |
| CN106654218A (en) * | 2017-01-11 | 2017-05-10 | 湖南文理学院 | Lithium ion battery positive electrode material lithium vanadium phosphate/carbon, preparation method thereof and lithium ion battery |
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