CN108054367A - A kind of preparation method of carbon coating MgFe2O4 negative materials for sodium-ion battery - Google Patents
A kind of preparation method of carbon coating MgFe2O4 negative materials for sodium-ion battery Download PDFInfo
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- CN108054367A CN108054367A CN201711319652.1A CN201711319652A CN108054367A CN 108054367 A CN108054367 A CN 108054367A CN 201711319652 A CN201711319652 A CN 201711319652A CN 108054367 A CN108054367 A CN 108054367A
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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
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
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- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Abstract
The invention discloses a kind of carbon coating MgFe for sodium-ion battery2O4A certain proportion of magnesium nitrate, ferric nitrate, carbon source and comburant are dissolved in deionized water, obtain mixed solution by the preparation method of negative material；Solution is placed in experiment with being heated to 200~300 DEG C and 10~20min of constant temperature in micro-wave oven, products therefrom calcines the carbon coating MgFe that can obtain for sodium-ion battery under an argon atmosphere2O4Material.Present invention process is simply easily operated, and resulting materials have certain pore space structure and crystallinity is high, are capable of the stability of reinforcing material；Carbon coating can accelerate sodium ion electron-transport speed, increase the electro-chemical activity of material.Present invention process is at low cost, and step is simple, avoids the shortcomings of multi-step preparation complex process, cycle are long and equipment requirement is high, is suitble to industrial applications.
Description
Technical field
The invention belongs to materials synthesis and energy technology fields, and in particular to a kind of carbon coating for sodium-ion battery
The preparation method of MgFe2O4 negative materials.
Background technology
Lithium ion battery is current most widely used high-energy battery system, but with productions such as 3C Product, new-energy automobiles
Industry, which relies on lithium ion battery, aggravates, and limited lithium resource will face shortage problem.Sodium is provided as common elements, reserves than lithium
The high several orders of magnitude in source, account for the 2.64% of the earth's crust, and are evenly distributed, and are easy to refine.Therefore, more inexpensive sodium ion electricity
Pond is the secondary cell that there is development potentiality in a kind of pole.
For sodium-ion battery still in conceptual phase, researcher has carried out positive electrode extensive research, but to sodium from
The research of sub- cell negative electrode material is still at an early stage.Current existing negative material mainly have carbon-based material such as petroleum coke,
Titanium base material such as TiO2With sodium alloy material etc., but the theoretical capacity of these materials is relatively low（Less than 300mAh/g）, it is difficult to meet
The requirement of high-energy density sodium-ion battery.The research of nearest 2 years shows that ferrite anode material of lithium-ion battery has
Very high actual reversible capacity（Higher than 400mAh/g）.Wherein MgFe2O4With certain representativeness, MgFe2O4Generally use is consolidated
The problem of mutually or prepared by the methods of hydro-thermal method, these methods are there are complex process, operation difficulty is big and product crystallinity is low.In addition
MgFe2O4Electrons/ions conductivity it is low, cause high rate performance bad, it is extensive on sodium-ion battery cathode to limit it
It uses.
The content of the invention
For above-mentioned technical deficiency, it is an object of the invention to provide a kind of carbon coatings for sodium-ion battery
The preparation method of MgFe2O4 negative materials.This method simple process and low cost is honest and clean, and the physicochemical property of product is uniform, crystallinity
It is high；Preparing MgFe2O4While by carbon coating on its surface, can both accelerate the transmission speed of electrons/ions, improve multiplying power
Performance, and the storage stable sodium of material with the electro-chemical activity of reinforcing material, can be improved.
In order to achieve the above objectives, the technical solution adopted by the present invention comprises the following steps.
（1）Magnesium nitrate, ferric nitrate, carbon source and comburant are dissolved in deionized water in proportion, mixed solution is put into
Experiment obtains black loose powder with 200~300 DEG C, and 10~20min of constant temperature is heated in micro-wave oven.
（2）By step（1）Middle product under an argon atmosphere, 150~900 DEG C of high-temperature calcinations, you can obtain for sodium ion
The carbon coating MgFe of battery2O4Negative material.
Further, step（1）The molar ratio of middle magnesium nitrate and ferric nitrate is 1：2, the molar ratio of carbon source and nitrate is
1:（5~15）, the molar ratio of nitrate and comburant is 1：（1~5）.
Further, the comburant is at least one of glycine, citric acid, urea.
Further, the carbon source is one or two kinds of mixtures of dopamine, trishydroxymethylaminomethane.Using institute
Stating carbon source is advantageous in that simultaneously containing amino and hydroxyl, the complexing excellent effect with nitrate, and soluble easily in water, reaction generation
Carbon can preferably be dispersed in particle surface.
Further, step（2）Middle calcination condition is：3~10 DEG C/min of heating rate, calcination time are 0. 5~5h.
Further, the carbon coating MgFe2O4Carbon content is 1~10wt.% in negative material.
Further, the carbon coating MgFe2O4Carbon coating layer thickness is 100~2000 nm in negative material.Control carbon
Coating thickness is conducive to improve MgFe2O4The ion and electron transfer rate of negative material and the reversible of this material will not be reduced
Capacity.
The technical solution adopted in the present invention has following advantages compared with prior art.
1st, the present invention uses combustion method to prepare electrode material, is preparing MgFe2O4While by carbon coating in material table
Face, preparation method is simple, of low cost, reaction speed is fast.
2nd, electrode material surface carbon coated is conducive to accelerate the transmission speed of electrons/ions, has both improved material high rate performance,
Electro-chemical activity can be enhanced again, improve the storage stable sodium of material.
3rd, carbon coating MgFe prepared by the present invention2O4Electrode material has stronger cycle performance, MgFe2O4In 200mA/g
High current density under cycle 50 weeks reversible capacities up to more than 420mAh/g.
Description of the drawings
Fig. 1 is carbon coating MgFe in embodiment 12O4The XRD diagram of negative material.
Fig. 2 is carbon coating MgFe in embodiment 12O4The SEM figures of negative material.
Fig. 3 is carbon coating MgFe in embodiment 12O4The BET figures of negative material.
Fig. 4 is carbon coating MgFe in embodiment 12O4Cycle performance figure of the negative material under 200mA/g current densities.
Fig. 5 is carbon coating MgFe in embodiment 22O4Cycle performance figure of the negative material under 200mA/g current densities.
Fig. 6 is MgFe in comparative example2O4Cycle performance figure of the negative material under 200mA/g current densities.
Specific embodiment
Below by embodiment, the present invention is further illustrated, but not limited to this.
Embodiment 1
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）The magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the dopamine of 0.92g and the glycine of 2.25g are weighed, uniformly
It is dissolved in deionized water.Solution is put into experiment micro-wave oven and is warming up to 200 DEG C and constant temperature 20min.Mixed solution fires
It burns, obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 3 DEG C/min of heating rate, 150 DEG C of calcining heat, and calcination time is
2h, calcination atmosphere are argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 7%, carbon coating layer
Thickness is 1500 nm.
Carbon coating MgFe manufactured in the present embodiment2O4The XRD diagram of material is as shown in Figure 1, from fig. 1, it can be seen that carbon coating
MgFe2O4Material is spinel structure and free from admixture, and characteristic peak is sharp and background is gentle, illustrates that the crystallinity of material is higher.This
Carbon coating MgFe prepared by embodiment2O4The SEM figures of material are as shown in Fig. 2, as can be seen from Figure 2, which has dendroid hole knot
Structure.Carbon coating MgFe manufactured in the present embodiment2O4The specific surface area BET tests of material are as shown in figure 3, can by BET method calculating
Know, the specific surface area of this material is 4.0124 m2/ g further illustrates that pore space structure improves specific surface area.
Electrochemical property test：By obtained electrode material carbon coating MgFe2O4Material and acetylene black and carboxymethyl cellulose
Plain sodium（CMC）In mass ratio 8: 1: 1 are uniformly mixed, and add in appropriate amount of deionized water and are adjusted to slurry, slurry film is made on copper foil
Obtain electrode.The 110 DEG C of dryings in vacuum drying oven of this test electrode for 24 hours, then encapsulate battery in high-purity argon atmosphere glove box, are electrolysed
Liquid is NaPF6It is dissolved in EC：DEC（Volume ratio 1：1）Mixed liquor, using glass fiber filter paper as membrane, metallic sodium is born for battery
Pole is assembled into CR2016 type button cells.Put charge condition：3V is recharged to after discharging into 0.02V with identical current density,
The current density selected is 200mA/g.Above-mentioned battery is tested, test result such as Fig. 4, as can be seen from Figure 4, by embodiment 1
Electrode material charge and discharge under 200mA/g current densities prepared by method, reversible capacity is maintained at 435.0mAh/ after cycling 50 weeks
G illustrates carbon coating MgFe2O4Material has preferable capacity retention ratio and cyclical stability.
Embodiment 2
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）Weigh the magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the trishydroxymethylaminomethane of 0.21g and 28.82g
Citric acid, uniform dissolution is in deionized water.Solution is put into experiment micro-wave oven and is warming up to 240 DEG C and 15 min of constant temperature.It is mixed
It closes solution to burn, obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 5 DEG C/min of heating rate, 500 DEG C of calcining heat, and calcination time is
3h, calcination atmosphere are argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 1%, carbon coating layer
Thickness is 100 nm.
Electrochemical property test：The electro-chemical test of the present embodiment is same as Example 1, test result as shown in figure 5, from
Knowable to Fig. 4, carbon coating MgFe2O4After material cycles 50 weeks under 200mA/g current densities, reversible capacity is maintained at 423.2mAh/
G illustrates carbon coating MgFe2O4Material has preferable capacity retention ratio and cyclical stability.
Embodiment 3
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）Weigh the magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the dopamine of 0.56g and trishydroxymethylaminomethane
The citric acid of mixture and 5.74g, uniform dissolution is in deionized water.Solution is put into experiment micro-wave oven and is warming up to 300 DEG C
And constant temperature 10min.Mixed solution burns, and obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 10 DEG C/min of heating rate, 900 DEG C of calcining heat, calcination time
For 4.8h, calcination atmosphere is argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 3%, carbon bag
Coating thickness is 500 nm.
Electrochemical property test：The electro-chemical test of the present embodiment is same as Example 1, the present embodiment carbon coating MgFe2O4
Material cycled under 200mA/g current densities 50 weeks reversible capacity and embodiment 1 it is close, illustrate there is carbon coating MgFe2O4Material
With preferable capacity retention ratio and cyclical stability.
Embodiment 4
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）Weigh the magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the dopamine of 0.71g and trishydroxymethylaminomethane
Mixture and the citric acid of 10.03g and urea acid blend, uniform dissolution is in deionized water.Solution is put into experiment microwave
200 DEG C and constant temperature 20min are warming up in stove.Mixed solution burns, and obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 8 DEG C/min of heating rate, 800 DEG C of calcining heat, and calcination time is
4 h, calcination atmosphere are argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 5%, carbon coating
Layer thickness is 1000 nm.
Electrochemical property test：The electro-chemical test of the present embodiment is same as Example 1, the present embodiment carbon coating MgFe2O4
Material cycled under 200mA/g current densities 50 weeks reversible capacity and embodiment 1 it is close, illustrate carbon coating MgFe2O4Material has
There are preferable capacity retention ratio and cyclical stability.
Embodiment 5
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）Weigh the magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the dopamine of 1.22g and trishydroxymethylaminomethane
The citric acid of mixture and 12.3g, glycine and urea admixture, uniform dissolution is in deionized water.Solution is put into experiment
300 DEG C and constant temperature 12min are warming up in micro-wave oven.Mixed solution burns, and obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 8 DEG C/min of heating rate, 900 DEG C of calcining heat, and calcination time is
0.5h, calcination atmosphere are argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 10%, carbon bag
Coating thickness is 2000 nm.
Electrochemical property test：The electro-chemical test of the present embodiment is same as Example 1, the present embodiment carbon coating MgFe2O4
Material cycled under 200mA/g current densities 50 weeks reversible capacity and embodiment 1 it is close, illustrate there is carbon coating MgFe2O4Material
With preferable capacity retention ratio and cyclical stability.
Comparative example 1
Hydro-thermal method prepares sodium-ion battery MgFe2O4Material is as follows.
（1）Weigh the magnesium sulfate of 2.41g, the ferric sulfate of 7.99g is dissolved in 80ml deionized waters, add 90 ml second
Alcohol is mixed to get homogeneous solution.
（2）At ambient temperature, in step（1）Mixed solution in ammonium hydroxide be added dropwise and test pH value at any time, until
PH value rises to 10 and sustained response stirring 3h.Solution is poured into heating reaction 12h, heating temperature in the reaction kettle of Teflon liner
160℃。
（3）By step（2）Product is cleaned with deionized water, filtered 6 times, is put into air dry oven and is dried for 24 hours.
（4）By step（3）Products therefrom is calcined, and 500 DEG C of calcining heat, time 1h treats that furnace cooling but obtains sodium ion
Battery MgFe2O4Material.
Electrochemical property test：The electrochemical property test of this comparative example is same as Example 1, test result such as Fig. 6 institutes
Show, MgFe2O4Material cycles the reversible capacity 253.1mAh/g of 50 weeks under 200mA/g current densities.
Comparative example 2
A kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, is as follows.
（1）The magnesium nitrate of 2.56g, the ferric nitrate of 8.08g, the dopamine of 2.15g and the glycine of 2.25g are weighed, uniformly
It is dissolved in deionized water.Solution is put into experiment micro-wave oven and is warming up to 200 DEG C and constant temperature 20min.Mixed solution fires
It burns, obtains black loose powder.
（2）By step（1）Products therefrom is calcined, 3 DEG C/min of heating rate, 150 DEG C of calcining heat, and calcination time is
2h, calcination atmosphere are argon gas.It treats that stove is cooled to room temperature, obtains carbon coating MgFe2O4Material, wherein carbon content are 17%, carbon coating
Layer thickness is 2800 nm.
Electrochemical property test：The electro-chemical test of this comparative example is same as Example 1, this comparative example carbon bag
Cover MgFe2O4Material cycles the reversible capacity of 50 weeks as 380.2 mAh/g under 200mA/g current densities, smaller than embodiment 1
54.8·mAh/g。
Claims (7)
1. a kind of carbon coating MgFe for sodium-ion battery2O4The preparation method of negative material, which is characterized in that including following
Step：
（1）Magnesium nitrate, ferric nitrate, carbon source and comburant are dissolved in deionized water in proportion, mixed solution is put into experiment
With 200~300 DEG C, and 10~20min of constant temperature is heated in micro-wave oven, black loose powder is obtained；
（2）By step（1）Middle product under an argon atmosphere, 150~900 DEG C of high-temperature calcinations, you can obtain for sodium-ion battery
Carbon coating MgFe2O4Negative material.
2. preparation method as described in claim 1, it is characterised in that：Step（1）The molar ratio of middle magnesium nitrate and ferric nitrate is
1：2, the molar ratio of carbon source and nitrate is 1:（5~15）, the molar ratio of nitrate and comburant is 1：（1~5）.
3. preparation method as described in claim 1, which is characterized in that the comburant is glycine, in citric acid, urea
At least one.
4. preparation method as described in claim 1, it is characterised in that：The carbon source is dopamine, trishydroxymethylaminomethane
One or two kinds of mixtures.
5. preparation method as described in claim 1, it is characterised in that：Step（2）Middle calcination condition is：Heating rate 3~10
DEG C/min, calcination time is 0. 5~5h.
6. preparation method as described in claim 1, it is characterised in that：The carbon coating MgFe2O4Carbon content is in negative material
1~10wt.%.
7. preparation method as described in claim 1, it is characterised in that：The carbon coating MgFe2O4Carbon coating layer in negative material
Thickness is 100~2000 nm.
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Cited By (1)
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| CN114843469A (en) * | 2022-05-07 | 2022-08-02 | 广西师范大学 | MgFe 2 O 4 Modified P2/O3 type nickel-based layered sodium-ion battery positive electrode material and preparation method thereof |
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