CN110350198A - A kind of preparation method of sodium phosphate surface modification sodium-ion battery positive material - Google Patents
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- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
The present invention relates to sodium-ion battery field of material technology more particularly to a kind of preparation methods of sodium phosphate surface modification sodium-ion battery positive material.The present invention provides a kind of preparation methods of sodium phosphate surface modification sodium-ion battery positive material, including step 1: reducing agent is added in sodium source, vanadium source and phosphorus source and dispersant ball milling obtains mix powder；Step 2: the mix powder being pre-sintered to obtain vanadium phosphate sodium presoma；Step 3: dispersing progress ultrasound in deionized water solution for the vanadium phosphate sodium presoma and obtain suspension, phosphorus source solution is added to the suspension；Step 4: product, sodium source and dispersing agent progress ball milling mixing are sintered to obtain sodium phosphate surface modification sodium-ion battery positive material.The present invention provides a kind of preparation methods of sodium phosphate surface modification sodium-ion battery positive material, can effectively solve the less technical problem of the surface modification method type of existing sodium-ion battery positive material.
Description
Technical field
The present invention relates to sodium-ion battery field of material technology more particularly to a kind of sodium phosphate surface modification sodium-ion batteries
The preparation method of positive electrode.
Background technique
In recent years, since sodium element has many advantages, such as resourceful, widely distributed, at low cost, increasingly mature sodium ion
Battery is increasingly becoming the research hotspot of energy storage field.Sodium-ion battery positive material is the important component of sodium-ion battery,
Wherein polyanionic compound vanadium phosphate sodium Na3V2(PO4)3As sodium-ion battery positive material, there is ideal specific volume
Amount, voltage platform and cyclical stability, to have received widespread attention.Na3V2(PO4)3Belong to sodium superionic conductors material,
Its structural framework forms stable storage sodium vacancy, and open three-dimensional ionic transport passages are conducive to improve the expansion of sodium ion
It dissipates.
Na3V2(PO4)3In spite of the above plurality of advantages, but its electronic conductivity is lower, has seriously affected electrochemistry
Energy.In order to solve Na3V2(PO4)3The problem of intrinsic poorly conductive, effective method are that synthesis has nanostructure
Na3V2(PO4)3, much research is improved by nano materials such as synthesis nano particle, 1-dimention nano fiber, three-dimensional porous structures
Material electronics electric conductivity not only can be improved in material property, this material with special nanostructure, also shortens ion biography
Defeated path is conducive to the insertion and abjection of sodium ion.In addition to this, there is good electron conduction at one layer of its surface modification
Material, such as carbon coating can improve Na3V2(PO4)3Electric conductivity, while can be reduced material again and being contacted with the direct of electrolyte,
Inhibit the volume change in electrode material charge and discharge process, improves material high rate performance and cyclical stability.Sodium phosphate is a kind of
Good sodium ion conductor material is conducive to the deintercalation of sodium ion, but utilizes sodium phosphate to sodium-ion battery positive material phosphorus
There is not been reported for the surface modified research of sour vanadium sodium.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of sodium phosphate surface modification sodium-ion battery positive material,
It can effectively solve the less technical problem of the surface modification method type of existing sodium-ion battery positive material.
The present invention provides a kind of preparation methods of sodium phosphate surface modification sodium-ion battery positive material, including following step
It is rapid:
Step 1: reducing agent and dispersant 5~15h of ball milling being added in sodium source, vanadium source and phosphorus source, is ground after dry
Obtain mix powder；
Step 2: the mix powder being pre-sintered under atmosphere of inert gases, vanadium phosphate sodium is obtained after being cooled to room temperature
Presoma；
Step 3: dispersing progress ultrasound in deionized water solution for the vanadium phosphate sodium presoma and obtain suspension, by phosphorus
Source solution is added in the suspension, after being evaporated deionized water at 80-100 DEG C, and dry 8~20 at 100-120 DEG C
Hour obtains product；
Step 4: the product, the sodium source and dispersing agent being subjected to ball milling mixing, carried out under the atmosphere of inert gas
It is sintered and cooled to room temperature up to sodium phosphate surface modification sodium-ion battery positive material.
Preferably, the sodium source is one or more of sodium acetate, sodium carbonate, sodium nitrate, sodium hydroxide.
Preferably, the vanadium source in step 1 be vanadic anhydride, ammonium metavanadate, vanadic sulfate, vanadyl acetylacetonate and
One or more of vanadyl oxalate.
Preferably, phosphorus source described in step 1 and step 3 be ammonium dihydrogen phosphate, it is diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, secondary
One or more of phosphoric acid, and the concentration range of phosphorus source solution described in step 3 is 0.0002-0.1mol/L.
Preferably, the reducing agent in step 1 is one of oxalic acid, citric acid, tartaric acid, ascorbic acid or several
Kind；
The molar ratio of the vanadium phosphate sodium and the reducing agent is 1:(1-5).
Preferably, the dispersing agent is one of water, ethyl alcohol, acetone；
The molar ratio of the vanadium phosphate sodium and the dispersing agent is 1:(0.1-5).
Preferably, the temperature of the pre-sintering is 300~600 DEG C；
The time of the pre-sintering is 3-8h.
Preferably, the temperature of the sintering is 400~900 DEG C；
The time of the sintering is 5~15h.
Preferably, the molar ratio of sodium source described in step 4 and phosphorus source is (3~3.15): 1.
Preferably, inert gas described in step 2 and step 4 is in nitrogen, argon gas, nitrogen and hydrogen mixture or argon hydrogen gaseous mixture
One kind.
Compared with prior art, the invention has the advantages that and technical effect:
The present invention is reacted by simple solid-phase ball milling, surface modification and high temperature solid-phase sintering, prepares sodium phosphate surface
The sodium-ion battery positive material of modification, sodium phosphate have good sodium ion conductive capability, are more conducive to after surface modification
The deintercalation of sodium ion.Compared with traditional carbon coating layer, sodium phosphate finishing coat can not only reduce the electrification of material interface
Impedance is learned, sacrifice agent is also used as, with HF and H micro in electrolyte2O reacts, and reduces HF and H in electrolyte2O
Content, therefore reduce electrode material and electrolyte and side reaction occur, keep stable structure, thus improve its cycle performance and
High rate performance.In addition, the raw material of preparation method of the present invention are easy to get, easy to operate, at low cost, favorable reproducibility, be able to satisfy sodium from
The various needs of sub- battery practical application, can be realized industrialization large-scale production.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 is the X-ray diffraction of sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1
Figure；
Fig. 2 is the SEM figure of sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1；
Fig. 3 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention and comparative example at 1C times
First charge-discharge under rate recycles correlation curve；
Fig. 4 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention and comparative example at 1C times
Multiple charge and discharge cycles curve under rate；
Fig. 5 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1 and comparative example not
Charging and discharging curve under same multiplying；
Fig. 6 is the SEM figure of sodium phosphate surface modification sodium-ion battery positive material made from comparative example 1.
Specific embodiment
The embodiment of the invention provides a kind of preparation methods of sodium phosphate surface modification sodium-ion battery positive material, can have
The less technical problem of the surface modification method type of the existing sodium-ion battery positive material of effect solution.
The technical scheme in the embodiments of the invention will be clearly and completely described below.
Embodiment 1
(1) according to synthesis 0.1mol Na3V2(PO4)3Elemental mole ratios, weigh the inclined vanadium of 15.90g sodium carbonate, 23.40g
19.21g citric acid is added in sour ammonium, 34.51g ammonium dihydrogen phosphate, is scattered in 50mL dehydrated alcohol, and ball milling 10h is obtained after dry
Mix powder.
(2) mix powder is put into tube furnace, under nitrogen and hydrogen mixture atmosphere, 350 DEG C of pre-sintering 4h are cooled to room
Grinding obtains vanadium phosphate sodium presoma after temperature.
(3) it disperses vanadium phosphate sodium presoma in 100mL deionized water solution, ultrasound 1 hour obtains suspension, claims
It takes the ammonium dihydrogen phosphate of 0.1g that the phosphorus source solution for being made into 0.05mol/L is added in deionized water, configured phosphorus source solution is dripped
It is added in suspension, it is 8 hours dry at 100 DEG C after being evaporated deionized water at 80 DEG C.
(4) product and 0.14g sodium carbonate obtained step (3) carries out ball milling mixing, then adds the mixing of 50mL ethyl alcohol
Ball milling 8 hours, mixture is put into tube furnace after dry, under nitrogen and hydrogen mixture atmosphere, 12h is sintered at 700 DEG C, is cooled to
Room temperature is up to sodium phosphate surface modification sodium-ion battery positive material Na3V2(PO4)3/Na3PO4。
Fig. 1 is the X-ray diffraction of sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1
Figure, as shown in Figure 1, the present embodiment products therefrom maintain vanadium phosphate sodium structure, and crystallinity is high, no miscellaneous phase.
Fig. 2 is the SEM figure of sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1, by Fig. 2
It is found that particle size distribution is uniform, rough surface illustrates successfully in surface modification sodium phosphate.
Fig. 3 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1 under 1C multiplying power
First charge-discharge cyclic curve, as shown in figure 3, carrying out charge and discharge in 2.0-4.0V voltage range at 25 DEG C with 1C multiplying power
When circulation, discharge capacity is 106.4mAh/g to the sodium-ion battery positive material vanadium phosphate sodium of sodium phosphate surface modification for the first time.
Fig. 4 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1 under 1C multiplying power
Multiple charge and discharge cycles curve, as shown in figure 4, discharge capacity is 101.2mAh/g after 500 circle of circulation, capacity retention ratio is
95.1%, it is shown that excellent cyclical stability.
Fig. 5 is sodium phosphate surface modification sodium-ion battery positive material made from the embodiment of the present invention 1 under different multiplying
Charging and discharging curve, as shown in figure 5, the charge and discharge under 0.5C, 1C, 2C, 5C, 10C, 15C multiplying power, sodium phosphate surface modification sodium from
The specific discharge capacity of sub- battery positive pole material phosphoric acid vanadium sodium is respectively 122.6,106.3,94.6,80.7,62.8,45.0mAh/g,
Present good high rate performance.
Embodiment 2
(1) according to synthesis 0.05mol Na3V2(PO4)3Elemental mole ratios, weigh 20.41g sodium acetate trihydrate, 9.1g five
9.00g oxalic acid is added in V 2 O, 19.81g diammonium hydrogen phosphate, is scattered in 25mL acetone, and ball milling 5h is mixed after dry
Object powder.
(2) mix powder is put into tube furnace, under nitrogen atmosphere, 400 DEG C of pre-sintering 5h are ground after being cooled to room temperature
Mill obtains vanadium phosphate sodium presoma.
(3) it disperses vanadium phosphate sodium presoma in 80mL deionized water solution, ultrasound 0.5 hour obtains suspension, claims
It takes the diammonium hydrogen phosphate of 0.2g that the phosphorus source solution for being made into 0.01mol/L is added in deionized water, configured phosphorus source solution is dripped
It is added in suspension, it is 8 hours dry at 110 DEG C after being evaporated deionized water at 90 DEG C；
(4) by step (3) obtain product and 0.62g sodium acetate trihydrate carry out ball milling mixing, then add 100mL go from
Mixture is put into tube furnace after dry, under inertia or reproducibility atmosphere, is sintered at 750 DEG C by sub- water mixing and ball milling 6 hours
15h is cooled to room temperature up to sodium phosphate surface modification sodium-ion battery positive material vanadium phosphate sodium.
At 25 DEG C, when charge and discharge cycles are carried out in 2.0-4.0V voltage range with 1C multiplying power, sodium phosphate surface modification
Discharge capacity is 105.9mAh/g to sodium-ion battery positive material vanadium phosphate sodium for the first time, and discharge capacity is after 500 circle of circulation
103.5mAh/g, capacity retention ratio 97.7%, it is shown that excellent cyclical stability.In 0.5C, 1C, 2C, 5C, 10C, 15C
Charge and discharge under multiplying power, the specific discharge capacity of sodium phosphate surface modification sodium-ion battery positive material vanadium phosphate sodium is respectively 120.5,
105.3,97.6,89.7,75.8,60.5mAh/g, present good high rate performance.
Embodiment 3
(1) according to synthesis 0.2mol Na3V2(PO4)3Elemental mole ratios, weigh 24.00g sodium hydroxide, 106.06g second
35.22g ascorbic acid is added in acyl acetone vanadyl, 89.45g ammonium phosphate, is scattered in 100mL deionized water, ball milling 15h, after dry
Obtain mix powder.
(2) mix powder is put into tube furnace, under argon atmosphere, 500 DEG C of pre-sintering 8h are ground after being cooled to room temperature
Mill obtains vanadium phosphate sodium presoma.
(3) it disperses vanadium phosphate sodium presoma in 150mL deionized water, ultrasound 2 hours obtains suspension, weighs 1g
Ammonium phosphate be added in deionized water and be made into the phosphorus source solution of 0.1mol/L, configured phosphorus source solution is added drop-wise to suspension
In, it is 8 hours dry at 120 DEG C after being evaporated deionized water at 100 DEG C；
(4) product and 0.80g sodium hydroxide obtained step (3) carries out ball milling mixing, then adds the anhydrous second of 150mL
Alcohol mixing and ball milling 20 hours, mixture is put into tube furnace after dry, under argon atmosphere, 10h is sintered at 800 DEG C, it is cooling
To room temperature up to sodium phosphate surface modification sodium-ion battery positive material.
At 25 DEG C, when charge and discharge cycles are carried out in 2.0-4.0V voltage range with 1C multiplying power, sodium phosphate surface modification
Discharge capacity is 110.5mAh/g to sodium-ion battery positive material for the first time, and discharge capacity is 106.7mAh/g after 500 circle of circulation, is held
Measuring conservation rate is 96.5%, it is shown that excellent cyclical stability.The charge and discharge under 0.5C, 1C, 2C, 5C, 10C, 15C multiplying power,
The specific discharge capacity of sodium phosphate surface modification sodium-ion battery positive material is respectively 125.7,110.8,100.5,91.2,
75.6,66.1mAh/g has good high rate performance.
Comparative example 1
(1) according to synthesis 0.1mol Na3V2(PO4)3Elemental mole ratios, weigh the inclined vanadium of 15.90g sodium carbonate, 23.40g
19.21g citric acid is added in sour ammonium, 34.51g ammonium dihydrogen phosphate, is scattered in 50mL ethyl alcohol, and ball milling 10h is mixed after dry
Object powder.
(2) mix powder is put into tube furnace, under nitrogen and hydrogen mixture atmosphere, 350 DEG C of pre-sintering 4h, at 700 DEG C
It is sintered 12h, is cooled to room temperature up to sodium-ion battery positive material Na3V2(PO4)3。
Fig. 6 is the SEM figure of sodium phosphate surface modification sodium-ion battery positive material made from comparative example 1, can from Fig. 6
Particle size distribution is uniform out.
At 25 DEG C, when charge and discharge cycles are carried out in 2.0-4.0V voltage range with 1C multiplying power, sodium-ion battery anode
Discharge capacity is 95.5mAh/g (as shown in Figure 3) to material phosphoric acid vanadium sodium for the first time, and discharge capacity is only after 500 circle of circulation
76.7mAh/g, capacity retention ratio are 80.3% (as shown in Figure 4).The charge and discharge under 0.5C, 1C, 2C, 5C, 10C, 15C multiplying power,
The specific discharge capacity of sodium-ion battery positive material vanadium phosphate sodium is respectively 109.7,92.5,80.2,62.7,38.7,7.7mAh/
G (as shown in Figure 5).
Obviously, as described above, described embodiments are only a part of the embodiments of the present invention, rather than whole implementation
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of sodium phosphate surface modification sodium-ion battery positive material, which comprises the following steps:
Step 1: reducing agent and dispersant 5~15h of ball milling being added in sodium source, vanadium source and phosphorus source, grinds and obtains after dry
Mix powder；
Step 2: the mix powder being pre-sintered under atmosphere of inert gases, vanadium phosphate sodium forerunner is obtained after being cooled to room temperature
Body；
Step 3: progress ultrasound in deionized water solution, which is dispersed, by the vanadium phosphate sodium presoma obtains suspension, phosphorus source is molten
Liquid is added in the suspension, after being evaporated deionized water at 80-100 DEG C, and it is 8~20 hours dry at 100-120 DEG C
Obtain product；
Step 4: the product, the sodium source and dispersing agent are subjected to ball milling mixing, are sintered under the atmosphere of inert gas,
It is cooled to room temperature up to sodium phosphate surface modification sodium-ion battery positive material.
2. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the sodium source is one or more of sodium acetate, sodium carbonate, sodium nitrate, sodium hydroxide.
3. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the vanadium source in step 1 is in vanadic anhydride, ammonium metavanadate, vanadic sulfate, vanadyl acetylacetonate and vanadyl oxalate
It is one or more of.
4. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In, phosphorus source described in step 1 and step 3 be one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, hypophosphorous acid or
It is several, and the concentration of phosphorus source solution described in step 3 is 0.0002-0.1mol/L.
5. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In reducing agent described in step 1 is one or more of oxalic acid, citric acid, tartaric acid, ascorbic acid；
The molar ratio of the vanadium phosphate sodium and the reducing agent is 1:(1-5).
6. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the dispersing agent is one of water, ethyl alcohol, acetone；
The molar ratio of the vanadium phosphate sodium and the dispersing agent is 1:(0.1-5).
7. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the temperature of the pre-sintering is 300~600 DEG C；
The time of the pre-sintering is 3-8h.
8. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the temperature of the sintering is 400~900 DEG C；
The time of the sintering is 5-15h.
9. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In the molar ratio of sodium source described in step 4 and phosphorus source is (3~3.15): 1.
10. the preparation method of sodium phosphate surface modification sodium-ion battery positive material according to claim 1, feature exist
In inert gas described in step 2 and step 4 clock is one of nitrogen, argon gas, nitrogen and hydrogen mixture or argon hydrogen gaseous mixture.
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| CN111082058A (en) * | 2019-12-20 | 2020-04-28 | 华南理工大学 | Nasicon structure sodium titanium phosphate surface modified P2 type manganese-based sodium ion battery positive electrode material and preparation method thereof |
| CN111082058B (en) * | 2019-12-20 | 2023-03-21 | 华南理工大学 | Nasicon structure sodium titanium phosphate surface modified P2 type manganese-based sodium ion battery positive electrode material and preparation method thereof |
| CN111009661A (en) * | 2019-12-24 | 2020-04-14 | 攀枝花学院 | Flexible self-supporting Na3(VO)2(PO4)2F material and preparation method and application thereof |
| CN111009661B (en) * | 2019-12-24 | 2022-02-08 | 攀枝花学院 | Flexible self-supporting Na3(VO)2(PO4)2F material and preparation method and application thereof |
| CN111439737A (en) * | 2020-03-10 | 2020-07-24 | 西安交通大学 | Vanadium-based sodium oxyfluorophosphate type sodium battery positive electrode material and modified preparation method thereof |
| CN111439737B (en) * | 2020-03-10 | 2021-11-30 | 西安交通大学 | Vanadium-based sodium oxyfluorophosphate type sodium battery positive electrode material and preparation method thereof |
| CN114335529A (en) * | 2021-11-05 | 2022-04-12 | 四川龙蟒磷化工有限公司 | Preparation method of vanadium sodium phosphate type sodium battery positive electrode material |
| CN114335529B (en) * | 2021-11-05 | 2024-01-26 | 四川龙蟒磷化工有限公司 | Preparation method of vanadium sodium phosphate type sodium battery positive electrode material |
| CN116262635A (en) * | 2021-12-15 | 2023-06-16 | 浙江钠创新能源有限公司 | Modified sodium nickel manganese oxide electrode material, sodium ion battery, preparation method and application |
| CN116081594A (en) * | 2023-02-23 | 2023-05-09 | 武汉工程大学 | Preparation method of sodium ion battery anode material |
| WO2024197434A1 (en) * | 2023-03-24 | 2024-10-03 | 广东邦普循环科技有限公司 | Modified sodium ion positive electrode material, preparation method therefor, and use thereof |
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