CN107293722A - A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof - Google Patents
A kind of self-supporting NaVPO4F/C compound potassium ion battery plus plates and preparation method thereof Download PDFInfo
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- CN107293722A CN107293722A CN201710557110.1A CN201710557110A CN107293722A CN 107293722 A CN107293722 A CN 107293722A CN 201710557110 A CN201710557110 A CN 201710557110A CN 107293722 A CN107293722 A CN 107293722A
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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
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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
- 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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
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- 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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Abstract
The present invention provides a kind of middle liquid phase process and prepares the compound fluorophosphoric acid vanadium sodium self-supporting positive pole of carbon, comprise the concrete steps that weighing sodium source, vanadium comes 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 in the beaker dissolved with 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 36h.By the 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere of the carbon base body after immersion, self-supporting NaVPO is obtained after calcining 6 ~ 12h, natural cooling at 650 ~ 850 DEG C4F/C electrodes, preferable chemical property is shown using it as lithium ion cell positive.
Description
Technical field
The present invention relates to a class high-performance self-supporting lithium ion cell positive, more particularly to a kind of NaVPO4F/C composite woods
Expect electrode preparation method, belong to field of electrochemical power source.
Technical background
The research and development of high performance lithium ion battery are always the important topic of domestic and international battery enterprise and institute, determine it
The key of success or failure is the research and application of high-performance lithium ion electrode.On the one hand, lithium ion battery is on the basis of existing structure
Develop towards high-energy-density with high power density direction, be used as following electric vehicle and large-scale energy-accumulating power station, intelligence electricity
The power supply of net；On the other hand, lithium ion battery extends towards flexibility, lightening direction, is set mainly as following wearableization
Standby power supply.Traditional electrode is by mixing, and being coated in metal collector active material, conductive agent, binding agent.It is conductive
Agent, the introducing of binding agent will increase battery weight, reduce the energy density of battery.Simultaneously as active material and conductive afflux
Pass through binding agent physical bond between body, it is impossible to ensure the stability in the case of bending.Therefore, exploitation have it is flexible from
Support electrode is the key for developing high-performance flexible lithium ion battery.At present, the research report of self-supporting negative pole is more, main collection
In in two-spot（Two kinds of elements）Compound such as oxide, sulfide etc..And positive electrode is generally ternary（Three kinds of elements）And more than
Compound, it is difficult to realize the growth in situ of active positive electrode material on a current collector, and the uniformity of active material is difficult to control to.
The content of the invention
NaVPO4F is a kind of Olivine-type Cathode Material in Li-ion Batteries, there is higher charge and discharge platform and reversible capacity,
With stronger practical value.The present invention provides a kind of middle liquid phase process, prepares NaVPO4F/C self-supporting positive poles.On the one hand,
There is special toughness using middle liquid phase, by interphase uniform adsorption to carbon base body；On the other hand, middle liquid phase is favourable
Uniform mixing between reactant, so as to obtain the NaVPO of size uniform in solid phase reaction4F particles；In addition, middle interstitial fluid
Carbon source is mutually conducive to introduce and uniformly mix, interphase liquid crystalization can induce organic carbon source molecule in crystal table in drying course
Adsorb and in the charing of subsequent solid phase reaction situ, realize NaVPO in face4F and C is uniformly multiple in micro-scale.Finally, it is prepared
Self-supporting NaVPO4F/C electrodes show excellent chemical property as lithium ion cell positive.
The present invention relates to a kind of preparation method of lithium ion cell positive, electrode is NaVPO4F/C growth in situ is carbon-based
Composite construction on body.Active material is NaVPO4F/C composites, are made up of average-size about 300nm particle.Specific system
Preparation Method step is as follows：A certain amount of sodium fluoride, vanadium source, hexamethylenetetramine are dissolved in the small beaker of deionized water, stirred
30min fully dissolves to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water to inner bag volume
80%, 12 ~ 48h of hydro-thermal in 100 ~ 180 DEG C of convection oven afterwards, natural cooling obtain interphase liquid.Weigh a certain amount of
Carbon source and phosphorus source are dissolved in deionized water, and stirring 20min fully dissolves to it, and the interphase liquid after cooling is slowly added dropwise afterwards
30min is stirred after body, completion of dropping to color in orange-yellow.Liquid is dried to different volumes in 60 DEG C of convection oven afterwards
Concentration；Carbon base body is soaked in gained liquid after concentration 1-4 hours, and is dried in 60 DEG C of convection oven in 36h.It will dry
Carbon base body after dry 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere, calcined at 650 ~ 850 DEG C obtained after 6 ~ 12h, natural cooling from
Support NaVPO4F/C electrodes.
Described sodium, vanadium, the mol ratio of phosphorus and hexamethylenetetramine are 1:1:1:1~5.Described carbon source accounts for the 0 of gross mass
~10%.Described sodium source is that sodium fluoride, vanadium source are vanadic anhydride or the sour ammonium of inclined alum, and phosphorus source is ammonium dihydrogen phosphate, phosphoric acid hydrogen two
Ammonium or ammonium phosphate, carbon source are citric acid, glucose, sucrose or anti-ascorbic acid.
Self-supporting NaVPO involved in the present invention4Preparation method, structure and the performance of F/C electrodes have following aobvious
The characteristics of work：
（1）Electrode synthesis technique is simple, it is easy to operate, reproducible；
（2）NaVPO4F/C is uniform with carbon-based bluk recombination, and contact is good；
（3）Prepared NaVPO4F/C is granule-morphology, average-size about 300nm；
（4）NaVPO obtained by the present invention4F/C self-supportings electrode can be directly used as lithium ion cell positive, show preferably
Cycle performance and higher specific capacity.
Brief description of the drawings
The SEM figures of sample prepared by Fig. 1 embodiments 1.
First three charging and discharging curve figure 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
4mmol sodium fluorides, 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 afterwards, natural cooling obtains interphase liquid.Weigh 0.04g
Citric acid and 4mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, it
Slow be added dropwise into beaker after the interphase liquid after cooling, completion of dropping stirs 30min to color in orange-yellow afterwards.Afterwards will
Liquid is dried to volume concentration for original half 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 36h.By the grapheme foam after drying in nitrogen atmosphere
Lower 350 DEG C of pre-burning 4h, and calcined at 750 DEG C self-supporting NaVPO is obtained after 9h, natural cooling4F/C electrodes.Sample is carried out
SEM signs, as seen from Figure 1, NaVPO4F/C homoepitaxials are in graphenic surface, by the particle group that size is 200nm
Into.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, are dissolved with LiPF6(volume ratio is 1 to the EC+DEC 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, and test voltage is 2.5-4.2V.Fig. 2 shows, the NaVPO prepared by embodiment 14F/C is certainly
Charge and discharge capacity is respectively 132.1 and 111 mAh/g to support electrode first, and charge and discharge capacity is respectively after 100 circulations
94.9 and 93.7 mAh/g, it is shown that preferable chemical property.
Embodiment 2
4mmol sodium fluorides, 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 afterwards, natural cooling obtains interphase liquid.Weigh 0.04g
Glucose and 4mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, it
Slow be added dropwise into beaker after the interphase liquid after cooling, completion of dropping stirs 30min to color in orange-yellow afterwards.Afterwards will
Liquid is dried to volume concentration for original half 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 calcined at 750 DEG C self-supporting NaVPO is obtained after 9h, natural cooling4F/C electrodes.Assembled in the way of embodiment 1
Battery.Fig. 3 shows, the NaVPO prepared by embodiment 14Charge and discharge capacity is respectively 117.6 Hes to F/C self-supportings electrode first
102.5 mAh/g, charge and discharge capacity is respectively 107.7 and 105.9mAh/g after 100 circulations, it is shown that preferably electrochemical
Learn performance.
Embodiment 3
Weigh 2mmol sodium fluorides, 2mmol ammonium metavanadates, 5mmol hexamethylenetetramines and be dissolved in the small burning equipped with 20mL deionized waters
In cup, stirring 30min fully dissolves to it；Obtained mixed solution is transferred in hydro-thermal inner bag, addition deionized water is to interior
The 80% of courage volume, the hydro-thermal 24h in 120 DEG C of convection oven afterwards, natural cooling obtains interphase liquid.Weigh 0.02g lemons
Lemon acid and 2mmol ammonium dihydrogen phosphates are dissolved in the beaker equipped with 20mL deionized waters, and stirring 20min fully dissolves to it, afterwards
It is in orange-yellow to color that stirring 30min after the interphase liquid after cooling, completion of dropping is slowly added dropwise into beaker.It will burn afterwards
Liquid is dried to volume concentration for original half in 60 DEG C of convection oven in cup, by liquid obtained by carbon paper immersion after concentration
In 2 hours, and in 60 DEG C of convection oven in 30h dry.By the 350 DEG C of pre-burning 4h in a nitrogen atmosphere of the carbon paper after drying,
And calcined at 750 DEG C self-supporting NaVPO is obtained after 9h, natural cooling4F/C electrodes.Electricity is assembled in the way of embodiment 1
Pond.Fig. 3 shows, the NaVPO prepared by embodiment 14Charge and discharge capacity is respectively 122.1 Hes to F/C self-supportings electrode first
110.3 mAh/g, charge and discharge capacity is respectively 102.9 and 101.5 mAh/g after 100 circulations, it is shown that preferably electrochemical
Learn performance.
Claims (4)
1. a kind of self-supporting lithium ion battery NaVPO4F/C combination electrodes, its pattern is compound pattern, is by grain fraction
NaVPO4F/C homoepitaxials are on carbon base body, it is characterised in that the preparation technology of the self-supporting electrode is as follows：
（1）Sodium source, vanadium source, hexamethylenetetramine are weighed in container, deionized water is added, is sufficiently stirred for 20min complete to its
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, appropriate deionized water is added, 20min is sufficiently stirred for and is completely dissolved to it, incited somebody to action
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 extremely after dripping
Liquid by liquid in beaker, is dried to different volumes concentration in orange-yellow in 60 DEG C of convection oven；
（3）Carbon base body is immersed in step（2）1-4 hours in middle gained liquid, and dried in 60 DEG C of convection oven in 36h
It is dry, by the 350 DEG C of 2 ~ 6h of pre-burning in a nitrogen atmosphere of the carbon base body after immersion, 6 ~ 12h, natural cooling are calcined at 650 ~ 850 DEG C
After obtain self-supporting NaVPO4F/C electrodes.
2. lithium ion battery NaVPO according to claim 14The preparation method of F/C combination electrodes, it is characterised in that sodium,
The mol ratio of vanadium, phosphorus and hexamethylenetetramine is 1：1：1：1 ~ 5, described carbon source accounts for the 0 ~ 10% of gross mass.
3. lithium ion battery NaVPO according to claim 14The preparation method of F/C combination electrodes, it is characterised in that described
Sodium source be sodium fluoride, vanadium source is the sour ammonium of vanadic anhydride or inclined alum, and phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or phosphoric acid
Ammonium, carbon source is citric acid, glucose, sucrose or ascorbic acid.
4. lithium ion battery NaVPO according to claim 14The preparation method of F/C combination electrodes, it is characterised in that described
Carbon base body be grapheme foam, carbon cloth or carbon paper.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037621A (en) * | 2018-07-12 | 2018-12-18 | 西安交通大学 | A kind of preparation method of the sodium-ion battery cathode material of high power high stable |
| CN109742327A (en) * | 2018-12-29 | 2019-05-10 | 西安鸿钧睿泽新材料科技有限公司 | Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material |
| CN110690462A (en) * | 2019-10-13 | 2020-01-14 | 浙江大学 | Preparation and application methods of self-supporting positive electrode with lithium ion conduction capability |
| CN111293281A (en) * | 2018-12-09 | 2020-06-16 | 中国科学院大连化学物理研究所 | Sodium vanadium phosphate self-supporting electrode and preparation and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109037621A (en) * | 2018-07-12 | 2018-12-18 | 西安交通大学 | A kind of preparation method of the sodium-ion battery cathode material of high power high stable |
| CN111293281A (en) * | 2018-12-09 | 2020-06-16 | 中国科学院大连化学物理研究所 | Sodium vanadium phosphate self-supporting electrode and preparation and application thereof |
| CN111293281B (en) * | 2018-12-09 | 2021-06-04 | 中国科学院大连化学物理研究所 | Sodium vanadium phosphate self-supporting electrode and preparation and application thereof |
| CN109742327A (en) * | 2018-12-29 | 2019-05-10 | 西安鸿钧睿泽新材料科技有限公司 | Preparation method of self-supporting flexible lithium ion battery carbon cloth loaded LiFePO4 positive electrode material |
| CN110690462A (en) * | 2019-10-13 | 2020-01-14 | 浙江大学 | Preparation and application methods of self-supporting positive electrode with lithium ion conduction capability |
| CN110690462B (en) * | 2019-10-13 | 2020-10-23 | 浙江大学 | Preparation and application methods of self-supporting positive electrode with lithium ion conduction capability |
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