CN105336924A - Preparation method of carbon coated vanadium sodium phosphate positive electrode material - Google Patents
Preparation method of carbon coated vanadium sodium phosphate positive electrode material Download PDFInfo
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- CN105336924A CN105336924A CN201510616627.4A CN201510616627A CN105336924A CN 105336924 A CN105336924 A CN 105336924A CN 201510616627 A CN201510616627 A CN 201510616627A CN 105336924 A CN105336924 A CN 105336924A
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- positive electrode
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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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- 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
-
- 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
- H01M4/62—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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- 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
Abstract
A preparation method of a carbon coated vanadium sodium phosphate positive electrode material comprises the steps: with glucose as a reducing agent and a carbon source and water as a dispersant, carrying out ball milling of NH4VO3, NaH2PO4.2H2O and glucose in water, carrying out spray drying, calcining, and thus obtaining the carbon coated vanadium sodium phosphate positive electrode material. The method has the advantages of low synthesis temperature, simple steps, easily obtained raw materials, and advantageous industrialization; the obtained carbon coated vanadium sodium phosphate positive electrode material has a structure with uniform primary particles, has the particle size of 100-200 nm, and has the characteristics of short sodium ion diffusion distance, fast transmission speed, high specific surface area, high electrical conductivity and fast ion transmission and the like. The obtained carbon coated vanadium sodium phosphate positive electrode material is assembled into a battery; in a voltage scope of 2.0-3.75 V and under 1 C multiplying power, the highest first charge and discharge capacity per gram can reach 93.5 mAh*g<-1>, the capacity retention rate can be up to 97.7% after cycling for 50 circles with the 1C multiplying power, and excellent electrochemical performance is showed.
Description
Technical field
The present invention relates to a kind of preparation method of sodium-ion battery positive material, be specifically related to the preparation method of the coated vanadium phosphate sodium positive electrode of a kind of carbon.
Background technology
From the nineties in 20th century, lithium ion battery, because having the advantages such as high-energy-density, quality be light, is widely used in the electronic installations such as mobile device.But there is the defects such as price is high, reserves are limited in lithium ion battery, and has many similarities with the sodium ion of main group and the character of lithium ion, and sodium ion completely likely becomes a kind of widely used secondary cell.And sodium-ion battery comparatively lithium ion battery, its cost of material is lower than lithium ion battery, and cell potential is higher than corresponding lithium ion battery current potential, and security performance is good.
NASICON refers to that a class has the solid electrolyte of fabulous ionic conductance performance under moderate temperature conditions.Just because of the ionic conduction characteristic that it is good, the material with NASICON structure is used as anode material for lithium-ion batteries, has attracted the attention of numerous researchers, and wherein, what people paid close attention to the most will count Li
3v
2(PO
4)
3material, and vanadium phosphate sodium (Na
3v
2(PO
4)
3) be also a kind of material with NASICON structure, in such an embodiment, Na
+ion can move fast in lattice.Existing preparation Na
3v
2(PO
4)
3method have hydro-thermal assisting sol-gel method, solid-phase ball milling method, coprecipitation.
CN104733731A discloses a kind of method preparing uniform carbon coated vanadium phosphate sodium material; Adopt glucose as carbon source, by hydro-thermal assisting sol-gel method, make crystal grain in growth, obtain particle diameter about 50 ~ 100nm, carbon-coating is evenly coated, and carbon layers having thicknesses is the Na of 8 ~ 10nm
3v
2(PO
4)
3material.Concrete steps are as follows: (1) is by V
2o
5, NH
4h
2pO
4and Na
2cO
3or NH
4vO
3, H
3pO
4and Na
2cO
3soluble in water, stir; (2) in above-mentioned solution, add glucose to mix, Na
3v
2(PO
4)
3be 2:3 ~ 4:3 with the mol ratio of glucose; (3) transfer in hydrothermal reaction kettle by above-mentioned solution, carry out reaction of guanosine, temperature is 70 ~ 95 DEG C; (4) drive still after cooling under room temperature, make it be uniformly dispersed by ultrasonic for the suspension-turbid liquid obtained, then stir transpiring moisture at water-bath lower magnetic force and obtain colloidal sol, colloidal sol in an oven drying obtains gel; (5) above-mentioned gel is fully ground and pre-burning in argon gas; Pre-sintered sample fully grinds again, in argon gas atmosphere, with 650 ~ 800 DEG C of temperature lower calcination 6 ~ 8h, obtains the Na that uniform carbon is coated
3v
2(PO
4)
3material.The defect that the method exists is that process is loaded down with trivial details, and flow process is longer.
CN104733731A discloses a kind of method preparing uniform carbon coated vanadium phosphate sodium material, and concrete steps are as follows: (1) is by V
2o
5, NH
4h
2pO
4and Na
2cO
3or NH
4vO
3, H
3pO
4and Na
2cO
3be dissolved in distilled water, the mol ratio making Na:V:P is 3:2:3, stirs; (2) in above-mentioned solution, add glucose to mix, Na
3v
2(PO
4)
3be 2:3 ~ 4:3 with the mol ratio of glucose; (3) transfer in hydrothermal reaction kettle by above-mentioned solution, carry out reaction of guanosine, reaction of guanosine condition is under hydrothermal condition, 180 DEG C of thermotonus 12 ~ 40h; (4) drive still after cooling under room temperature, make it be uniformly dispersed by ultrasonic for the suspension-turbid liquid obtained, then stir transpiring moisture at 70 ~ 95 DEG C of water-bath lower magnetic forces and obtain colloidal sol, colloidal sol dry 6 ~ 12h in 60 ~ 80 DEG C of baking ovens obtains gel; (5) above-mentioned gel fully ground and calcine 6 ~ 8h in 650 ~ 800 DEG C of argon gas, obtaining the Na that uniform carbon is coated
3v
2(PO
4)
3material.The defect that the method exists is, process is complicated, and reaction condition is difficult to control, and is unfavorable for suitability for industrialized production.
CN103474662A discloses a kind of anode material for lithium-ion batteries Na
3v
2(PO
4)
3high temperature process heat method, it is characterized in that, include following concrete steps: (1) stoichiometrically takes sodium oxalate, vanadic oxide, ammonium dihydrogen phosphate, acetylene black, namely the mol ratio of primary raw material is: sodium oxalate: vanadic oxide: ammonium dihydrogen phosphate: acetylene black=1.5:1:3:1.1, fully grinds 1 ~ 4 hour in mortar; (2), by the mix powder after above-mentioned abundant grinding, in a nitrogen atmosphere, at 600 ~ 900 DEG C, calcining 15 ~ 20h, naturally cools to room temperature, obtains target product.Synthesized Na
3v
2(PO
4)
3specific discharge capacity is first 105mAh/g, and through 50 circulations, its specific discharge capacity maintains 60 ~ 65mAh/g.The defect that the method exists is, although synthetic method is simple, and the Na of synthesis
3v
2(PO
4)
3material property is not good.
Summary of the invention
Technical problem to be solved by this invention is, overcome the above-mentioned defect that prior art exists, there is provided a kind of operating procedure simple, easy control of reaction conditions, can suitability for industrialized production, gained positive electrode has homogeneous primary particle, and discharge and recharge gram volume is higher, the preparation method of the vanadium phosphate sodium positive electrode that the carbon of good cycle is coated.
The technical solution adopted for the present invention to solve the technical problems is as follows: the preparation method of the vanadium phosphate sodium positive electrode that a kind of carbon is coated, using glucose as reducing agent and carbon source, water is dispersant, by NH
4vO
3, NaH
2pO
42H
2o and glucose carry out ball milling in water, through spraying dry, after calcining, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
Further, specifically comprise the following steps:
(1) by NH
4vO
3, NaH
2pO
42H
2o and glucose are placed in ball grinder according to the ratio of mass ratio 2:4:1 ~ 2, then add water, mix, ball milling, obtain yellow suspension;
(2) step (1) gained yellow suspension is carried out spraying dry, obtain Powdered presoma;
(3) the Powdered presoma of step (2) gained is calcined under an inert atmosphere, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
In step (1), NH
4vO
3, NaH
2pO
42H
2o and glucose ratio are that 2:4:1 ~ 2 can reduce V(V effectively) be V(III), glucose consumption too much can cause carbon residual volume too much thus affect material property, and glucose consumption crosses that I haven't seen you for ages causes vanadium ion reduction not thorough.
Further, in step (3), the condition of described calcining is: under an inert atmosphere, prior to 300 ~ 400 DEG C of calcining 3 ~ 5h, then in 600 ~ 750 DEG C of calcining 6 ~ 10h.First at lower temperature, then the degree of crystallinity of crystal can be improved in higher temperature calcining; If the too high meeting of calcining heat causes the adverse consequences of material burning, if the too low meeting of calcining heat causes sintering insufficient adverse consequences.Due to glucose pyrogenetic decomposition under an inert atmosphere, make part carbon be coated on bulk material surface, being coated with of carbon is beneficial to the conductivity increasing material.
Further, in step (3), the condition of described calcining is: under an inert atmosphere, prior to 320 ~ 380 DEG C of calcining 3.5 ~ 4.5h, then in 650 ~ 720 DEG C of calcining 7 ~ 9h.
Further, in step (1), by NH
4vO
3, NaH
2pO
42H
2o and glucose are placed in ball grinder according to the ratio of mass ratio 2:4:1.2 ~ 1.8.
Further, in step (1), the consumption of described water is NH
4vO
3, NaH
2pO
42H
2o and glucose gross mass 4 ~ 6 times.
Further, in step (1), described in be mixed into ultrasonic mixing, ultrasonic frequency is 50 ~ 400kHz, and the ultrasonic time is 0.5 ~ 4h.Ultrasonic mixing can play the effect of effectively dispersion.
Further, in step (1), the speed of described ball milling is 200 ~ 300r/min, and the time of ball milling is 4 ~ 10h.Ball milling can make sufficient mechanical activation and dispersion between raw material, ball milling condition be according to material between milling intensity determine.
Further, in step (2), the intake air temperature of described spraying dry spray dryer used is 150 ~ 200 DEG C, and air outlet temperature is 100 ~ 150 DEG C, and charging rate is 5 ~ 20mL/min.Spraying dry can not only realize drying, also has the effect of granulation.
Step (3) described inert atmosphere refers to that calcination process carries out under the protection such as high pure nitrogen, high-purity argon gas, high-purity gas purity >=99.99%.
The inventive method has the following advantages: the inventive method synthesis temperature is low, and step is simple, and raw material is easy to get, and is convenient to industrialization.The coated vanadium phosphate sodium positive electrode of prepared carbon has the architectural characteristic of homogeneous primary particle, primary particle particle diameter is 100 ~ 200nm, has the characteristics such as sodium ion diffusion length is short, transmission rate fast, high-specific surface area, high conductivity, ion transfer are fast.Vanadium phosphate sodium positive electrode coated for gained carbon is assembled into battery, and in 2.0 ~ 3.75V voltage range, under 1C multiplying power, first charge-discharge gram volume reaches as high as 93.5mAhg
-1; In charge and discharge process, have good cycle performance due to stable structure, after 1C circulation 50 circle, capability retention can reach 97.7%, and electrode and electrolyte side reaction reduce.The coated vanadium phosphate sodium positive electrode of carbon shows excellent chemical property, and can be used as the positive electrode of secondary sodium-ion battery, fail safe is high, and low price is widely used, and can be applicable to energy storage device, back-up source, redundant electrical power etc.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the coated vanadium phosphate sodium positive electrode of the embodiment of the present invention 1 gained carbon;
Fig. 2 is the SEM figure of the coated vanadium phosphate sodium positive electrode of the embodiment of the present invention 1 gained carbon;
Fig. 3 is the TEM figure of the coated vanadium phosphate sodium positive electrode of the embodiment of the present invention 1 gained carbon;
Fig. 4 is the 1C first charge-discharge curve chart of the coated vanadium phosphate sodium positive electrode of the embodiment of the present invention 1 gained carbon;
Fig. 5 is specific discharge capacity and the capability retention figure of 1C circulation 50 circle of the coated vanadium phosphate sodium positive electrode of the embodiment of the present invention 1 gained carbon.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
The embodiment of the present invention uses high-purity argon gas purity >=99.99%; The chemical reagent used, if no special instructions, is all obtained by routine business approach.
embodiment 1
(1) by 5gNH
4vO
3, 10gNaH
2pO
42H
2o and 3.75g glucose is placed in ball grinder, then adds 100mL water and make dispersant, under 250kHz, and ultrasonic mixing 2h, then with the rotating speed ball milling 7h of 250r/min, obtain yellow suspension; (2) by step (1) gained yellow suspension in spray dryer, be 180 DEG C with intake air temperature, air outlet temperature is 130 DEG C, and charging rate is that 10mL/min carries out spraying dry, obtains Powdered presoma; (3) by the Powdered presoma of step (2) gained under high-purity argon gas, prior to 350 DEG C calcining 4h, then in 700 DEG C calcining 8h, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
As shown in Figure 1, the coated vanadium phosphate sodium positive electrode degree of crystallinity of gained carbon is high, and crystal formation is complete, and what detect is vanadium phosphate sodium pure phase.
As shown in Figure 2, the coated vanadium phosphate sodium positive electrode primary particle of gained carbon is homogeneous, and particle diameter is 100 ~ 200nm.
As shown in Figure 3, there is obvious carbon coating layer on the vanadium phosphate sodium positive electrode surface that gained carbon is coated.
Battery is assembled: take 0.24g the present embodiment gained Na respectively
3v
2(PO
4)
3material is as positive electrode, add 0.03g acetylene black (SP) and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, 2mLNMP dispersion mixing is added after abundant grinding, slurry on 16 μm of thick aluminium foils of sizing mixing evenly makes anode pole piece, in anaerobism glove box with sodium metal sheet for negative pole, with WhatmanGF/D glass fibre for barrier film, 1mol/LNaClO
4/ EC:PC(volume ratio 1:1) be electrolyte, be assembled into the button cell of CR2025.
As shown in Figure 4, by battery in 2.0 ~ 3.75V voltage range, under 1C multiplying power, surveying its first charge-discharge gram volume is 93.5mAhg
-1.
As shown in Figure 5, by battery in 2.0 ~ 3.75V voltage range, under 1C multiplying power, after circulation 50 circle, capability retention is 97.7%.
embodiment 2
(1) by 5gNH
4vO
3, 10gNaH
2pO
42H
2o and 2.5g glucose is placed in ball grinder, then adds 100mL water and make dispersant, under 50kHz, and ultrasonic mixing 4h, then with the rotating speed ball milling 4h of 200r/min, obtain yellow suspension; (2) by step (1) gained yellow suspension in spray dryer, be 150 DEG C with intake air temperature, air outlet temperature is 120 DEG C, and charging rate is that 5mL/min carries out spraying dry, obtains Powdered presoma; (3) by the Powdered presoma of step (2) gained under high-purity argon gas, prior to 300 DEG C calcining 3h, then in 600 DEG C calcining 6h, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
Battery is assembled: take 0.24g the present embodiment gained Na respectively
3v
2(PO
4)
3material is as positive electrode, add 0.03g acetylene black (SP) and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, 2mLNMP dispersion mixing is added after abundant grinding, slurry on 16 μm of thick aluminium foils of sizing mixing evenly makes anode pole piece, in anaerobism glove box with sodium metal sheet for negative pole, with WhatmanGF/D glass fibre for barrier film, 1mol/LNaClO
4/ EC:PC(volume ratio 1:1) be electrolyte, be assembled into the button cell of CR2025.By battery in 2.0 ~ 3.75V voltage range, under 1C multiplying power, surveying its first charge-discharge gram volume is 83.7mAhg
-1.
embodiment 3
(1) by 5gNH
4vO
3, 10gNaH
2pO
42H
2o and 5g glucose is placed in ball grinder, then adds 100mL water and make dispersant, under 400kHz, and ultrasonic mixing 0.5h, then with the rotating speed ball milling 10h of 300r/min, obtain yellow suspension; (2) by step (1) gained yellow suspension in spray dryer, be 200 DEG C with intake air temperature, air outlet temperature is 150 DEG C, and charging rate is that 20mL/min carries out spraying dry, obtains Powdered presoma; (3) by the Powdered presoma of step (2) gained under high-purity argon gas, prior to 400 DEG C calcining 5h, then in 750 DEG C calcining 10h, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
Battery is assembled: take 0.24g the present embodiment gained Na respectively
3v
2(PO
4)
3material is as positive electrode, add 0.03g acetylene black (SP) and make conductive agent and 0.03gPVDF(HSV-900) make binding agent, 2mLNMP dispersion mixing is added after abundant grinding, slurry on 16 μm of thick aluminium foils of sizing mixing evenly makes anode pole piece, in anaerobism glove box with sodium metal sheet for negative pole, with WhatmanGF/D glass fibre for barrier film, 1mol/LNaClO
4/ EC:PC(volume ratio 1:1) be electrolyte, be assembled into the button cell of CR2025.By battery in 2.0 ~ 3.75V voltage range, under 1C multiplying power, surveying its first charge-discharge gram volume is 89.1mAhg
-1.
Claims (9)
1. a preparation method for the vanadium phosphate sodium positive electrode that carbon is coated, it is characterized in that: using glucose as reducing agent and carbon source, water is dispersant, by NH
4vO
3, NaH
2pO
42H
2o and glucose carry out ball milling in water, through spraying dry, after calcining, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
2. the preparation method of the vanadium phosphate sodium positive electrode that carbon is coated according to claim 1, is characterized in that, specifically comprise the following steps:
(1) by NH
4vO
3, NaH
2pO
42H
2o and glucose are placed in ball grinder according to the ratio of mass ratio 2:4:1 ~ 2, then add water, mix, ball milling, obtain yellow suspension;
(2) step (1) gained yellow suspension is carried out spraying dry, obtain Powdered presoma;
(3) the Powdered presoma of step (2) gained is calcined under an inert atmosphere, obtain the vanadium phosphate sodium positive electrode that carbon is coated.
3. the preparation method of the vanadium phosphate sodium positive electrode that carbon is coated according to claim 2, it is characterized in that: in step (3), the condition of described calcining is: under an inert atmosphere, prior to 300 ~ 400 DEG C of calcining 3 ~ 5h, then in 600 ~ 750 DEG C of calcining 6 ~ 10h.
4. the preparation method of the vanadium phosphate sodium positive electrode that carbon is coated according to Claims 2 or 3, it is characterized in that: in step (3), the condition of described calcining is: under an inert atmosphere, prior to 320 ~ 380 DEG C of calcining 3.5 ~ 4.5h, then in 650 ~ 720 DEG C of calcining 7 ~ 9h.
5., according to the preparation method of the coated vanadium phosphate sodium positive electrode of the described carbon of one of claim 2 ~ 4, it is characterized in that: in step (1), by NH
4vO
3, NaH
2pO
42H
2o and glucose are placed in ball grinder according to the ratio of mass ratio 2:4:1.2 ~ 1.8.
6., according to the preparation method of the coated vanadium phosphate sodium positive electrode of the described carbon of one of claim 2 ~ 5, it is characterized in that: in step (1), the consumption of described water is NH
4vO
3, NaH
2pO
42H
2o and glucose gross mass 4 ~ 6 times.
7., according to the preparation method of the coated vanadium phosphate sodium positive electrode of the described carbon of one of claim 2 ~ 6, it is characterized in that: in step (1), described in be mixed into ultrasonic mixing, ultrasonic frequency is 50 ~ 400kHz, and the ultrasonic time is 0.5 ~ 4h.
8., according to the preparation method of the coated vanadium phosphate sodium positive electrode of the described carbon of one of claim 2 ~ 7, it is characterized in that: in step (1), the speed of described ball milling is 200 ~ 300r/min, and the time of ball milling is 4 ~ 10h.
9. according to the preparation method of the coated vanadium phosphate sodium positive electrode of the described carbon of one of claim 2 ~ 8, it is characterized in that: in step (2), the intake air temperature of described spraying dry spray dryer used is 150 ~ 200 DEG C, air outlet temperature is 100 ~ 150 DEG C, and charging rate is 5 ~ 20mL/min.
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