CN108288712A - A kind of lithium ion battery negative material Fe2O3Preparation method - Google Patents
A kind of lithium ion battery negative material Fe2O3Preparation method Download PDFInfo
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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
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a kind of lithium ion battery negative material Fe2O3Preparation method, belong to lithium ion battery material technical field.The preparation method comprises the following steps：(1) surfactant is dissolved into the mixed liquor of oil phase and cosurfactant composition and obtains solution A, soluble iron salting liquid is instilled into solution A, make water-oil factor control 15 25, then sonic oscillation to solution is in clear, and microemulsion B is made；(2) microemulsion B is transferred in reaction kettle, 12 16h is reacted under the conditions of 60 80 DEG C, obtain reaction liquid C；(3) solid phase, washing, dry, the obtained Fe with nano-scale is collected by centrifugation in reaction liquid C2O3Powder.The present invention is readily able to the soluble ferric iron salt of hydrolysis, is limited in the microemulsion of the controllable Water-In-Oil of size, to make molysite hydrolysis can only occur in the water core of microemulsion, washes and dries finally by centrifugation, obtain the Fe of nano-scale2O3Powder.
Description
Technical field
The present invention relates to lithium ion battery material technical fields, and in particular to a kind of lithium ion battery negative material Fe2O3's
Preparation method.
Background technology
In recent years, non-renewable due to the deterioration of environment and traditional energy, green and recyclable lithium ion battery obtain
To rapid development.Lithium ion battery is because its operating voltage is high, energy density is big, have extended cycle life, operating temperature range is wide and peace
Start to play its value in electric vehicle field completely without the advantages that memory effect.However, negative material-graphite of Current commercial
Since gram volume is low, the capacity boost of lithium ion battery is largely limited.So improve negative material gram volume and
Finding the alternative materials of graphite is particularly important.
Fe2O3There is high specific capacity, high safety, cheap, ABUNDANT NATUREAL RESOURSES and nontoxic, quilt as negative material
It is considered most to promise to be the alternative materials of commercial graphite cathode.As 106328930 A of CN disclose a kind of lithium ion battery
Negative material α-Fe2O3Preparation method, including：(1) by FeCl3Solution and ethylene glycol are stirred at room temperature, and uniformly mix, obtain
To solution A；(2) NaOH solution and deionized water are added in solution A, stirring obtains solution B；(3) ten are added in solution B
Dialkyl benzene sulfonic acids sodium, obtains solution C；(4) solution C is transferred in autoclave, it is anti-under conditions of 200-250 DEG C, 5-6Mpa
20-30h is answered, by products therefrom Fe (OH)3It centrifuges, vacuum drying, heat treatment obtains negative material α-Fe2O3, test
Reach 956.6mAhg to its first charge-discharge specific capacity-1。
However, Fe2O3Since pole piece dusting caused by its big volume change prevents its practical to answer in charge and discharge process
With.People are by changing Fe2O3Pattern and Fe2O3Composite material reduce the influence that volume change is brought.With nanometer skill
The continuous development of art, the negative material of nanostructure is due to having faster lithium ion to deviate from/be embedded in dynamic performance and obtain
Extensive concern.There is the nano-particle negative material of reduced size efficient electron-transport path and shorter ion to spread road
Diameter, and the strain in charge and discharge process in structure can be buffered so that negative material structure is more stable.Therefore, how to obtain
Obtain the Fe with nano-scale2O3It is those skilled in the art's problem to be solved.
Invention content
The purpose of the present invention is to provide a kind of preparation processes simple, easy to implement to prepare lithium ion battery negative material
Fe2O3Method, Fe is prepared2O3With nanostructure, effectively overcome the problems, such as that its volume becomes larger, improves and be used as lithium ion
The chemical property of cell negative electrode material.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of lithium ion battery negative material Fe2O3Preparation method, include the following steps：
(1) surfactant is dissolved into the mixed liquor of oil phase and cosurfactant composition and obtains solution A, toward solution
Soluble iron salting liquid is instilled in A, makes water-oil factor control in 15-25, then sonic oscillation to solution is in clear, is made micro-
Lotion B；
(2) microemulsion B is transferred in reaction kettle, 12-16h is reacted under the conditions of 60-80 DEG C, obtain reaction liquid C；
(3) solid phase, washing, dry, the obtained Fe with nano-scale is collected by centrifugation in reaction liquid C2O3Powder.
The water-oil factor is the molar ratio of water and surfactant, and water-oil factor determines the grain size of water droplet in microemulsion,
Preferably, water-oil factor ω=20.Soluble ferric iron salt easily occurs hydrolysis and generates Fe2O3, received since hydrolysis is limited in
In meter-sized microemulsion water core, and then limit Fe2O3Size.Therefore, it can be obtained using the preparation method of the present invention
Obtain the Fe with nanostructure2O3。
The surfactant is cetyl trimethylammonium bromide (CTAB), two (2- ethylhexyls) sulfosuccinates
At least one of sodium (NaAOT), lauryl sodium sulfate (SDS), neopelex (SDBS).
The oil phase is at least one of isooctane, hexamethylene, normal heptane, normal octane.
The cosurfactant is at least one of n-butanol, isoamyl alcohol, isopropanol, glycerine.
The soluble ferric iron salt is iron chloride, ferric sulfate or ferric nitrate.
Preferably, in the soluble iron salting liquid iron ion a concentration of 0.02-1.0mol/L.
Preferably, in step (1), the volume ratio of oil phase and cosurfactant is 5-10 in the mixed liquor:1, institute
State a concentration of 0.05-0.15mol/L of surfactant in solution A.
Preferably, in step (1), the frequency of the ultrasound is 20-40kHz.
Preferably, in step (3), the temperature of the drying is 50-60 DEG C, time 5-6h.
The Fe being prepared by the method for the present invention2O3Structure is spherical, average diameter 50-100nm, as lithium ion
Negative material, nanostructure can buffer the strain in structure in charge and discharge process so that lithium ion battery negative electrode structure is more
For stabilization.
The present invention also provides a kind of negative electrode of lithium ion battery, including the lithium ion battery made from the preparation method is born
Pole material.
Preferably, the lithium ion battery negative material Fe2O3Additive amount account for cell negative electrode material gross mass
80-90%.
The advantageous effect that the present invention has：
(1) present invention is readily able to the soluble ferric iron salt of hydrolysis, is limited in the microemulsion of the controllable Water-In-Oil of size,
To make molysite hydrolysis can only occur in the water core of microemulsion, after washing and dry finally by centrifugation, nanometer is obtained
The Fe of size2O3Powder.The preparation method is simple for process, easy to implement, only needs one-step method that can be prepared, and is conducive to promote
Using.
(2) Fe made from preparation method of the present invention is utilized2O3, nano-grade size is conducive to electron-transport and lithium ion expands
It dissipates, while the strain in charge and discharge process in structure can be buffered, to substantially increase the chemical property of material.
Description of the drawings
Fig. 1 is negative material Fe prepared by embodiment 12O3X-ray diffraction (XRD) figure.
Fig. 2 is negative material Fe prepared by embodiment 12O3Low power (a) and high power (b) FESEM figure.
Fig. 3 is negative material Fe prepared by embodiment 12O3Charging and discharging curve figure (A) under different multiplying and high rate performance
Scheme (B).
Fig. 4 is negative material Fe prepared by embodiment 12O3Cycle performance figure under different multiplying, wherein (A) is 0.8C
Cycle performance under multiplying power, (B) are the cycle performance under 1.6C multiplying powers.
Fig. 5 is negative material Fe prepared by embodiment 12O33 times charging and discharging curve figure under 0.1C multiplying powers.
Specific implementation mode
The present invention is further explained in the light of specific embodiments.
Embodiment 1
1, high power capacity Fe2O3It is prepared by lithium ion battery negative material
At room temperature, the ferric nitrate solid for weighing 0.242g, is added in the deionized water of 20mL, fully vibrates so that
Ferric nitrate solid all dissolves, and the iron nitrate solution for being configured to 0.05M is spare.
0.5g CTAB, 10mL isooctane is sequentially added in the vial of 30mL, then 1mL n-butanols instill 0.5mL
Above-mentioned iron nitrate solution so that water-oil factor ω=20.Sonic oscillation a few minutes in ultrasonic cleaner, until mixed solution
Become clarification to get to the microemulsion containing iron nitrate solution.
Obtained microemulsion will be prepared to pour into the reaction kettle of polytetrafluoroethylene (PTFE) material, be put into 60 DEG C of baking ovens, shelve 12h
After take out, the liquid in reaction kettle is poured into centrifuge tube, by centrifugation washing 3 times after, obtain Fe2O3Powder.Then at 50 DEG C
Dry 6h, you can obtain high power capacity Fe2O3Negative material.
Fig. 1 is the XRD diagram of the present embodiment products therefrom, and as can be seen from the figure product is the Fe of α types2O3。
Fig. 2 is the Fe of nano-scale obtained by the present embodiment2O3Low power FESEM figure (Fig. 2 (a)) and high power FESEM figures (Fig. 2
(b)), as can be seen from the figure Fe2O3It is spherical, diameter is uniform, and size is between 50-100nm.
2, chemical property is analyzed
By the Fe of the nano-scale of the present embodiment2O3With acetylene black, Kynoar (PVDF) to match 8:1:1 (quality
Than) be sufficiently mixed and be tuned into paste even application on copper foil, applied thickness is 200 μm, and anode is made after 65 DEG C of drying, compacting
Piece.It (needs to illustrate herein：Fe2O3It is negative material, but is as anode in half-cell), using metal lithium sheet as cathode,
Cellgard2400 type polypropylene screens make diaphragm, 1M LiPF6Solution (ethylene carbonate+dimethyl carbonate (volume ratio=1：1))
For electrolyte, experimental cell is assembled into argon gas glove box.Then it is real constant current charge-discharge to be carried out to this battery at 25 DEG C
It tests.
The results are shown in Figure 3, the specific capacity at 0.1C, 0.2C, 0.4C, 0.8C, 1.6C, 3.2C, 6.4C, 12.8C, 16C
Respectively 1558.1,1015,837.5,780,720,707.5,625,485,445mAh g-1；It is recycled 10 times under 16C high magnifications
Afterwards, 0.1C cycles are come back to, capacity still can reach 1020mAh g-1, illustrate that material has excellent invertibity.
As shown in figure 4, from it as can be seen that recycling 150 weeks and 200 respectively in the cycle performance figure under 0.8C, 1.6C
Zhou Shi is respectively 75.46%, 59.95% relative to second of discharge capacitance, illustrates that material has preferable cycle
Performance.
As shown in figure 5, product is assembled into battery by the identical method of embodiment, electro-chemical test shows product in 0.1C
Lower cycle 3 times specific capacity be respectively 1447.5,983.75,996.25mAh g-1。
Embodiment 2
At room temperature, the ferric sulfate solid for weighing 0.16g, is added in the deionized water of 20mL, fully vibrates so that sulphur
Sour iron solid all dissolves, and the ferrum sulfuricum oxydatum solutum for being configured to 0.02M is spare.
0.824g NaAOT, 15mL hexamethylenes are sequentially added in the vial of 30mL, then 2mL isopropanols instill
Ferrum sulfuricum oxydatum solutum above-mentioned 0.5mL so that water-oil factor ω=15.Sonic oscillation a few minutes in ultrasonic cleaner, until mixed
It closes solution and becomes clarification to get to the microemulsion containing iron nitrate solution.
Obtained microemulsion will be prepared to pour into the reaction kettle of polytetrafluoroethylene (PTFE) material, be put into 70 DEG C of baking ovens, shelve 12h
After take out, the liquid in reaction kettle is poured into centrifuge tube, by centrifugation washing 3 times after, obtain Fe2O3Powder.Then at 50 DEG C
Dry 6h, you can obtain high power capacity Fe2O3Negative material.
Embodiment 3
At room temperature, the iron chloride solid for weighing 3.24g, is added in the deionized water of 20mL, fully vibrates so that chlorine
Change iron solid all to dissolve, the ferrum sulfuricum oxydatum solutum for being configured to 1.0M is spare.
0.32g SDS, 12mL normal octanes are sequentially added in the vial of 30mL, then 3mL isopropanols instill 0.5mL
Above-mentioned ferrum sulfuricum oxydatum solutum so that water-oil factor ω=25.Sonic oscillation a few minutes in ultrasonic cleaner, until mixed solution
Become clarification to get to the microemulsion containing iron nitrate solution.
Obtained microemulsion will be prepared to pour into the reaction kettle of polytetrafluoroethylene (PTFE) material, be put into 80 DEG C of baking ovens, shelve 12h
After take out, the liquid in reaction kettle is poured into centrifuge tube, by centrifugation washing 3 times after, obtain Fe2O3Powder.Then at 60 DEG C
Dry 5h, you can obtain high power capacity Fe2O3Negative material.
In summary, preparation method of the invention can prepare the Fe with nano-scale2O3, negative as lithium ion battery
Pole material has been greatly improved the chemical property of battery.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of lithium ion battery negative material Fe2O3Preparation method, which is characterized in that include the following steps：
(1) surfactant is dissolved into the mixed liquor of oil phase and cosurfactant composition and obtains solution A, into solution A
Soluble iron salting liquid is instilled, makes water-oil factor control in 15-25, then sonic oscillation to solution is in clear, and micro emulsion is made
Liquid B；
(2) microemulsion B is transferred in reaction kettle, 12-16h is reacted under the conditions of 60-80 DEG C, obtain reaction liquid C；
(3) solid phase, washing, dry, the obtained Fe with nano-scale is collected by centrifugation in reaction liquid C2O3Powder.
2. preparation method as described in claim 1, which is characterized in that the surfactant is cetyl trimethyl bromination
At least one of ammonium, two (2- ethylhexyls) sulfosuccinate sodium, lauryl sodium sulfate, neopelex.
3. preparation method as described in claim 1, which is characterized in that the oil phase is isooctane, hexamethylene, normal heptane, just
At least one of octane.
4. preparation method as described in claim 1, which is characterized in that the cosurfactant is n-butanol, isoamyl alcohol, different
At least one of propyl alcohol, glycerine.
5. preparation method as described in claim 1, which is characterized in that the soluble ferric iron salt is iron chloride, ferric sulfate or nitre
Sour iron.
6. preparation method as described in claim 1, which is characterized in that iron ion is a concentration of in the soluble iron salting liquid
0.02-1.0mol/L。
7. preparation method as described in claim 1, which is characterized in that oil phase and help surface in step (1), in the mixed liquor
The volume ratio of activating agent is 5-10:1, a concentration of 0.05-0.15mol/L of surfactant in the solution A.
8. preparation method as described in claim 1, which is characterized in that in step (1), the frequency of the ultrasound is 20-
40kHz。
9. preparation method as described in claim 1, which is characterized in that in step (3), the temperature of the drying is 50-60 DEG C,
Time is 5-6h.
10. a kind of negative electrode of lithium ion battery, including the lithium-ion electric made from claim 1-9 any one of them preparation methods
Pond negative material Fe2O3。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110165166A (en) * | 2019-05-13 | 2019-08-23 | 北京石油化工学院 | A kind of method of microemulsion assisted in situ coated lithium ion battery positive electrode |
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