CN104409701B - Cathode material for sodium-ion battery and preparation method of cathode material - Google Patents
Cathode material for sodium-ion battery and preparation method of cathode material Download PDFInfo
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- CN104409701B CN104409701B CN201410669406.9A CN201410669406A CN104409701B CN 104409701 B CN104409701 B CN 104409701B CN 201410669406 A CN201410669406 A CN 201410669406A CN 104409701 B CN104409701 B CN 104409701B
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a cathode material for a sodium-ion battery and a preparation method of the cathode material. The cathode material consists of a base and a laminated structure, wherein the base is coated with the laminated structure, and carbon material-vanadium oxide-carbon material is taken as a repeating unit. The preparation method comprises the following steps: firstly preparing a vanadium oxide colloidal solution and a carbon material aqueous solution, then coating the base with the carbon material aqueous solution in a spin manner and baking, then coating the base with the vanadium oxide colloidal solution in a spin manner and baking, then coating a layer of carbon material again, and repeating the above steps according to requirements, and finally drying to obtain the cathode material. The prepared electrode material is more beneficial to the intercalation capacity of sodium ions and excellent de-intercalation reversibility; the crystal structure of the vanadium oxide is larger in frame, so that intercalation of sodium ions is facilitated, the material structures are prevented from collapsing during the de-intercalation process of the sodium ions, the carbon material can promote the stretchability of the material, the damage to the material in the intercalation process of the sodium ions is reduced, and the practical capacity of the battery is improved greatly and the cycle life of the battery is greatly prolonged.
Description
Technical field
The present invention relates to sodium ion battery electrode material field, and in particular to a kind of sodium-ion battery positive material and its system
Preparation Method.
Background technology
The existing energy is constantly consumed and promotes various countries constantly to seek alternative novel energy-storing material, and energy storage miscellaneous is produced
Product are also gradually commercially fast-selling, the secondary cell that electrochmical power source circle is also being explored always new high-energy-density, had extended cycle life.
Lithium ion battery and ultracapacitor are applied to military affairs, traffic, communication, doctor as new energy storage device with its unique advantage
Each fields such as treatment.But, a large amount of exploitations of lithium ore deposit cause lithium price to rise, and it is withered to further result in the predictable lithium ore deposit energy
Exhaust.Then, in recent years people are sought for replaceable novel battery, and sodium-ion battery is regarded hence into research worker
It is wild.Sodium reserves very abundant on earth, cheap, there is quite similar chemical property in of the same clan as lithium.Sodium from
Sub- battery is a kind of very promising lithium ion battery substituent, and it is to find suitable to develop one of key of sodium-ion battery
Positive electrode, make battery that there is sufficiently high sodium embedded quantity and good sodium deintercalation reversibility, with ensure battery high voltage,
Large Copacity and long circulation life.But reality exist a subject matter be, due to the diameter of sodium ion it is bigger than lithium ion
It is many, carry out easilying lead to the structural collapse of electrode material when ion is interspersed in cell reaction, therefore solve the circulation of battery
Stability is one of significant challenge that sodium-ion battery is faced at present.
The content of the invention
In view of this, an object of the present invention is to provide a kind of sodium-ion battery positive material, the structure of the material
Framework is easy to the interspersed of sodium ion, effectively reduces when sodium ion interts to structural damage；Present invention also offers the positive pole material
The preparation method of material.
Technical scheme is specific as follows：
A kind of sodium-ion battery positive material, the positive electrode is made up of substrate and laminated construction；The laminated construction with
Material with carbon element-barium oxide-material with carbon element is coated in substrate for repetitives.
Preferably, the substrate is aluminium flake.
Preferably, the barium oxide is vanadic anhydride.
Preferably, the material with carbon element is graphene oxide.
Preferably, the number of repetition of the repetitives is 1～6 time.
It is furthermore preferred that the number of repetition of the repetitives is 3 times.
Present invention also offers the preparation method of above-mentioned sodium-ion battery positive material, comprises the steps：
1) barium oxide colloid solution and material with carbon element aqueous solution are prepared；
2) by step 1) prepare material with carbon element aqueous solution and barium oxide colloid solution press material with carbon element aqueous solution-barium oxide
The order of colloid solution-material with carbon element aqueous solution is coated in substrate successively, and is often coated and once dried once；
3) finally the electrode material that finishes of coating is drying to obtain.
Preferably, step 2) after repeat step 2) at least one times.
Preferably, the step 1) described in barium oxide colloid solution for 0.1mol/L to saturated concentration colloid it is molten
Liquid, the concentration of the material with carbon element aqueous solution is 4～9mg/mL.
Preferably, the step 2) described in dry and dried to be heated to 40～70 DEG C.
Preferably, the step 3) described in be dried to be dried 12h in 120 DEG C under vacuum condition.
The beneficial effects of the present invention is：The electrode material prepared using the laminated construction of material with carbon element-barium oxide-material with carbon element
Material is more conducive to the embedded quantity and good deintercalation reversibility of sodium ion, also, the lattice structure framework of barium oxide is larger, is beneficial to
Sodium ion it is interspersed, it is ensured that sodium ion will not subside in deintercalation process in which materials structure, and material with carbon element can then lift material
Draftability, reduces the destruction to material in sodium ion inserting process, therefore, the electrode material of laminated construction of the present invention is significantly
Improve the actual capacity and cycle life of battery.Further, since barium oxide as potential window during electrode material than it
His metal-oxide is high so that the electrode material can to greatest extent play when in use the effect of each material, be conducive to
Lift the voltage of battery.
Description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below：
The preparation process schematic diagram of Fig. 1 sodium-ion battery positive materials；
Sodium-ion battery positive material SEM plane and sectional view that each embodiments of Fig. 2 are prepared；
First three charge and discharge of the button sodium-ion battery of sodium-ion battery positive material assembling prepared by Fig. 3 embodiments 1
Electric cyclic curve figure；
The button sodium-ion battery of sodium-ion battery positive material assembling prepared by each embodiments of Fig. 4 is in different electric discharges times
Capacity under rate-cycle-index curve chart；
The button sodium-ion battery of sodium-ion battery positive material assembling prepared by each embodiments of Fig. 5 is in same electric discharge times
Capacity under rate-cycle-index curve chart.
Specific embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.It is unreceipted concrete in embodiment
The experimental technique of condition, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
A kind of sodium-ion battery positive material, its preparation method is as follows：
1) the vanadic anhydride colloid solution of saturated concentration is prepared with vanadium pentoxide powder and hydrogen peroxide, is used in combination
Graphite powder is prepared into Hummers methods the graphene oxide water solution that concentration is 4mg/mL；
2) graphene oxide water solution is evenly applied on substrate aluminium flake, is then dried on 60 DEG C of warm table；
3) again vanadic anhydride colloid solution is coated uniformly on into step 2) what is prepared is loaded with the aluminium flake of graphene oxide
On, then dry on 60 DEG C of warm table；
4) and then by graphene oxide water solution be coated uniformly on step 3) prepare be loaded with graphene oxide and five oxygen
Change on the aluminium flake of two vanadium, and dry on 60 DEG C of warm table；
5) repeat step 2) to step 4) twice；
6) coated electrode material is dried into 12h with 120 DEG C of Temperature Vacuum, last vacuum state cooling is obtained final product.
Embodiment 2
A kind of sodium-ion battery positive material, its preparation method is as follows：
1) the vanadic anhydride colloid solution of saturated concentration is prepared with vanadium pentoxide powder and hydrogen peroxide, is used in combination
Graphite powder is prepared into Hummers methods the graphene oxide water solution that concentration is 9mg/mL；
2) graphene oxide water solution is spun on substrate aluminium flake, is then dried on 60 DEG C of warm table；
3) again vanadic anhydride colloid solution is spin-coated on into step 2) it is obtained be loaded with the aluminium flake of graphene oxide,
Dry on 60 DEG C of warm table；
4) and then by graphene oxide water solution be spun on step 3) prepare be loaded with graphene oxide and five oxidation two
On the aluminium flake of vanadium, and dry on 60 DEG C of warm table；
5) repeat step 2) to step 4) twice；
6) the good electrode material of spin coating is dried into 12h with 120 DEG C of Temperature Vacuum, last vacuum state cooling is obtained final product.
Embodiment 3
A kind of sodium-ion battery positive material, its preparation method is as follows：
1) the vanadic anhydride colloid solution that concentration is 0.1mol/L is prepared with vanadium pentoxide powder and hydrogen peroxide, is used in combination
Graphite powder is prepared into Hummers methods the graphene oxide water solution that concentration is 6mg/mL；
2) graphene oxide water solution is spun on substrate aluminium flake, is then dried on 40 DEG C of warm table；
3) again vanadic anhydride colloid solution is spin-coated on into step 2) it is obtained be loaded with the aluminium flake of graphene oxide,
Dry on 40 DEG C of warm table；
4) and then by graphene oxide water solution be spun on step 3) prepare be loaded with graphene oxide and five oxidation two
On the aluminium flake of vanadium, and dry on 40 DEG C of warm table；
5) the good electrode material of spin coating is dried into 12h with 120 DEG C of Temperature Vacuum, last vacuum state cooling is obtained final product.
Embodiment 4
A kind of sodium-ion battery positive material, its preparation method is as follows：
1) the vanadic anhydride colloid solution that concentration is 0.2mol/L is prepared with vanadium pentoxide powder and hydrogen peroxide, is used in combination
Graphite powder is prepared into Hummers methods the graphene oxide water solution that concentration is 4mg/mL；
2) graphene oxide water solution is spun on substrate aluminium flake, is then dried on 70 DEG C of warm table；
3) again vanadic anhydride colloid solution is spin-coated on into step 2) it is obtained be loaded with the aluminium flake of graphene oxide,
Dry on 70 DEG C of warm table；
4) and then by graphene oxide water solution be spun on step 3) prepare be loaded with graphene oxide and five oxidation two
On the aluminium flake of vanadium, and dry on 70 DEG C of warm table；
5) repeat step 2) to step 4) 5 times；
6) the good electrode material of spin coating is dried into 12h with 120 DEG C of Temperature Vacuum, last vacuum state cooling is obtained final product.
Interpretation of result
Fig. 1 for sodium-ion battery positive material preparation process schematic diagram, by the method for spin coating make vanadic anhydride and
Graphene oxide forms uniform laminated construction in substrate surface, so as to improve electrode material property, lifts the actual appearance of battery
Amount and cycle life.
Fig. 2 is the graphene oxide-vanadic anhydride-graphene oxide electrode material SEM plane and section for preparing
Figure, wherein, figure a is identical with structure shown in figure c, is the SEM figures of graphene oxide in laminated construction, except for the difference that, schemes putting for a
Big multiple is 10,000 times, and the amplification for scheming c is 1.5 ten thousand times, can be clearly observed by figure a and c and be coated over oxidation
Vanadic anhydride under Graphene；Figure b is amplification under conditions of 50,000 times, vanadic anhydride surface in laminated construction
SEM schemes；Figure d, e, f are the sectional view of laminated construction material difference angle under the conditions of 1.5 ten thousand times of amplification；By scheming a-f
As can be seen that graphene oxide-vanadic anhydride-graphene oxide the sodium-ion battery positive material of laminated construction is successfully made
It is standby, and form is more homogeneous.
First three charge and discharge cycles curve of the button sodium-ion battery that Fig. 3 is assembled by embodiment 1, it can be seen that
The close 225mAh/g of the first circle discharge capacity of embodiment 1, and first three circle illustrates filling for embodiment 1 almost without big capacity attenuation
Put sufficiently stable and capacity is higher.
The button sodium-ion battery that Fig. 4 is assembled by the four embodiments capacity-circulation under different discharge-rates time
Number curve.It can be seen that, in laminated construction, electrode material after big multiplying power charge and discharge when remaining able to return to little multiplying power
More than the 90% of capacity, illustrates that material can undergo big multiplying power discharging and stability is fine.Wherein, the capacity of embodiment 1 is each
All it is highest under individual charge and discharge multiplying power, particularly in large current density.After small current charge and discharge is returned to, its capacity is also showed
Increased phenomenon is gone out.
Fig. 5 is capacity-cycle-index of the button sodium-ion battery of four embodiment assemblings under same discharge-rate
Curve, it is seen then that embodiment 1 is that capacity is comprehensively best with stability.Embodiment 2 is made because the concentration of graphene oxide is too high
Into in material graphene oxide content height cause the electric conductivity of material to decline to ultimately result in capacity not high, but cyclical stability according to
It is so good.The capacity of embodiment 3 was once exceeding embodiment 1 but stability is not as good as embodiment 1.Embodiment 4 is more due to the number of plies, sodium
Ion completely penetrates through electrode material during charge and discharge needs the regular hour, therefore capacity is relatively low in front 150 circle, it was demonstrated that electricity
The pole number of plies can result in the need for multiple charge and discharge when excessive can just make electrode material reach optimum performance.
May certify that by above-mentioned experiment, the laminated construction that the sodium-ion battery positive material prepared by the present invention possesses
Due to more stable with lattice structure, in the embedded quantity and good deintercalation reversibility of sodium ion, incite somebody to action so as to advantageously
The material improves the actual capacity of battery as sodium-ion battery positive material, extends the service life cycle of battery.And
And the method for the invention preparation process is simple, have using the battery of sodium-ion battery positive material of the present invention assembling and hold
Amount is big, and power is big, good stability, repeatable high advantageous property, with potential using value and commercial value.
Finally illustrate, preferred embodiment above is only unrestricted to illustrate technical scheme, although logical
Cross above preferred embodiment to be described in detail the present invention, it is to be understood by those skilled in the art that can be
In form and in details various changes are made to it, without departing from claims of the present invention limited range.
Claims (9)
1. a kind of sodium-ion battery positive material, it is characterised in that the positive electrode is made up of substrate and laminated construction；It is described folded
Rotating fields are coated in substrate with material with carbon element-barium oxide-material with carbon element as repetitives, the sodium-ion battery positive material
Preparation method, comprises the steps：
1）Barium oxide colloid solution and material with carbon element aqueous solution are prepared, the barium oxide colloid solution is 0.1mol/L to saturation
The colloid solution of concentration, the concentration of the material with carbon element aqueous solution is 4 ~ 9mg/mL；
2）By step 1）The material with carbon element aqueous solution and barium oxide colloid solution of preparation presses material with carbon element aqueous solution-barium oxide colloid
The order of solution-material with carbon element aqueous solution is coated in substrate successively, and is often coated and once dried once；
3）Finally the electrode material that coating is finished is drying to obtain.
2. sodium-ion battery positive material according to claim 1, it is characterised in that the substrate is aluminium flake.
3. sodium-ion battery positive material according to claim 1, it is characterised in that the barium oxide is five oxidations two
Vanadium.
4. sodium-ion battery positive material according to claim 1, it is characterised in that the material with carbon element is graphite oxide
Alkene.
5. sodium-ion battery positive material according to claim 1, it is characterised in that the number of repetition of the repetitives
For 1 ~ 6 time.
6. the preparation method of sodium-ion battery positive material described in any one of claim 1 ~ 5, it is characterised in that including following step
Suddenly：
1）Barium oxide colloid solution and material with carbon element aqueous solution are prepared, the barium oxide colloid solution is 0.1mol/L to saturation
The colloid solution of concentration, the concentration of the material with carbon element aqueous solution is 4 ~ 9mg/mL；
2）By step 1）The material with carbon element aqueous solution and barium oxide colloid solution of preparation presses material with carbon element aqueous solution-barium oxide colloid
The order of solution-material with carbon element aqueous solution is coated in substrate successively, and is often coated and once dried once；
3）Finally the electrode material that coating is finished is drying to obtain.
7. the preparation method of sodium-ion battery positive material according to claim 6, it is characterised in that step 2）Repeat afterwards
Step 2）At least one times.
8. preparation method according to claim 6, it is characterised in that the step 2）Described in dry to be heated to 40 ~ 70
DEG C dry.
9. the preparation method according to any one of claim 6 ~ 8, it is characterised in that the step 3）Described in be dried be vacuum
Under the conditions of be dried 12h in 120 DEG C.
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| CN201410669406.9A CN104409701B (en) | 2014-11-19 | 2014-11-19 | Cathode material for sodium-ion battery and preparation method of cathode material |
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| CN201410669406.9A CN104409701B (en) | 2014-11-19 | 2014-11-19 | Cathode material for sodium-ion battery and preparation method of cathode material |
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| CN104409701B true CN104409701B (en) | 2017-04-19 |
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| CN107768668B (en) * | 2016-08-15 | 2020-08-18 | 福建新峰二维材料科技有限公司 | Preparation method of sodium ion battery positive electrode material |
| CN106946238B (en) * | 2017-05-19 | 2018-12-28 | 西南大学 | A kind of vanadium phosphate manganese sodium electrode material and its preparation method and application |
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| CN101373826B (en) * | 2007-08-24 | 2010-10-06 | 比亚迪股份有限公司 | Silicium cathode and lithium ion secondary battery containing the same, and method for preparing the same |
| KR101430615B1 (en) * | 2007-09-19 | 2014-08-14 | 삼성에스디아이 주식회사 | Cathode and lithium battery using the same |
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