CN106992295B - A kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet - Google Patents
A kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet Download PDFInfo
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- CN106992295B CN106992295B CN201710120611.3A CN201710120611A CN106992295B CN 106992295 B CN106992295 B CN 106992295B CN 201710120611 A CN201710120611 A CN 201710120611A CN 106992295 B CN106992295 B CN 106992295B
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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
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/052—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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- 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
The present invention relates to a kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet, include the following steps: that 1) P123 is dissolved in ethylene glycol, stirs, continue for ferric nitrate to be dissolved in ethylene glycol, obtain clear solution;The molar concentration of ferric nitrate is 0.5~2mol/L in the clear solution;2) KOH aqueous solution is added to the clear solution in step 1), obtains precursor solution russet;3) it is 180~200 DEG C in reaction temperature by the precursor solution in step 2), carries out 24~30h of hydro-thermal reaction, obtain monodisperse alpha-ferric oxide nanometer sheet.The preparation method technical process is simple, and easily controllable, non-environmental-pollution is at low cost, is easy to large-scale production;Gained monodisperse alpha-ferric oxide nanometer sheet has outstanding cycle performance as lithium ion battery negative material simultaneously.
Description
Technical field
The present invention relates to inorganic material to synthesize field, and in particular to a kind of preparation side of monodisperse alpha-ferric oxide nanometer sheet
Method.
Background technique
The situation of environmental pollution and energy crisis is increasingly serious, forces the mankind that must change tradition based on fossil fuel
Energy consumption structure, while actively finding substitution of the renewable energy as fossil energy.But compared to traditional fossil energy, newly
The renewable energy of type, such as solar energy, wind energy, tide energy, geothermal energy etc. are seriously limited by the uncontrollability of environment and inconsistent
Property.Therefore, realize effective energy storage and easily transport transmit battery, as it is a kind of can by electric energy Efficient Conversion be it is portable
Electrochemical system with chemical energy progresses into the research vision of global scientist.
Lithium ion battery is with its high working voltage platform and energy density, and memory-less effect is inexpensive, and low pollution is micro-
The features such as weak self discharge, good safety, it is widely used in portable electronic device, such as mobile phone, laptop, and next
For in the development of electric car and large-scale static energy storage system, huge application potential is shown.
At present on the positive and negative pole material for focusing on battery of Study on Li-ion batteries, researcher wants to look for
With high specific capacity, cycle performance excellent electrode material prepares lithium ion battery simultaneously to a kind of.α-Fe2O3Because its is special
Redox machinery the theoretical capacity of 1007mAh/g is held up to as lithium ion battery negative material, but as electrode
Its cycle performance of material is poor, in order to improve α-Fe2O3Cycle performance as lithium ion battery negative material.Researcher is uncommon
Hope the α-Fe that can prepare nano-scale2O3Particle improves lithium ion diffusion coefficient and electron conductivity, final to obtain electricity
The good lithium ion battery negative material of chemical property.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of preparation of monodisperse alpha-ferric oxide nanometer sheet
Method, the monodisperse alpha-ferric oxide being prepared have nano-scale, improve its cycle performance.
The technical solution of present invention solution above-mentioned technical problem:
A kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet, includes the following steps:
1) P123 is dissolved in ethylene glycol, stirs, continues for ferric nitrate to be dissolved in ethylene glycol, obtain clear solution;
The molar concentration of ferric nitrate is 0.5~2mol/L in the clear solution;
2) KOH aqueous solution is added to the clear solution in step 1), obtains precursor solution russet;
3) it is 180~200 DEG C in reaction temperature by the precursor solution in step 2), carries out 24~30h of hydro-thermal reaction, obtain
To monodisperse alpha-ferric oxide nanometer sheet.
In above-mentioned technical proposal, P123 is a kind of triblock copolymer, and full name is poly- for polyethylene oxide-polypropylene oxide-
Ethylene oxide triblock copolymer, molecular formula are as follows: PEO-PPO-PEO.P123 has the function of alpha-ferric oxide pattern,
P123 can be coated on ferric oxide nano piece surface in hydrothermal reaction process, reduce the reunion of ferric oxide nano piece, and in heat
One layer of unbodied C can be left after processing in alpha-ferric oxide nanometer sheet, so that alpha-ferric oxide nanometer sheet is as lithium-ion electric
Pond negative electrode material has outstanding cycle performance;Secondly, size uniformity can be obtained by the additional amount of control ferric nitrate, and
The smaller alpha-ferric oxide of particle size.
Preferably, the hydro-thermal reaction carries out in ptfe autoclave, hydro-thermal reaction product is filtered, clearly
It washes, is dried to obtain monodisperse alpha-ferric oxide nanometer sheet.
Preferably, P123 is dissolved in ethylene glycol in the step 1), 20-30h is stirred at room temperature.When passing through long
Between stirring P123 can be evenly dispersed in ethylene glycol, be more conducive to the preparation of monodisperse alpha-ferric oxide nanometer sheet.
Preferably, the mass concentration of P123 is 30~80g/L in clear solution in the step 1).
Preferably, the volume fraction of ethylene glycol is 60~80% in precursor solution in the step 2).Pass through control
The volume ratio of ethylene glycol and water in precursor solution can play the effect of ethylene glycol regulation alpha-ferric oxide pattern, avoid simultaneously
Excessive ethylene glycol makes Fe3+Being reduced prevents from obtaining Fe3O4, guarantee to obtain single-phase alpha-ferric oxide with this.
Preferably, in the step 2) ferric nitrate and KOH molar ratio are as follows: 0.25~1.25:1.
Preferably, the molar concentration of KOH aqueous solution is 4~6mol/L in the step 2).
Preferably, in the step 3) hydro-thermal reaction reaction temperature be 190~200 DEG C, the reaction time be 26~
30h.Under the reaction temperature and reaction time, it is more favorable for the Morphological control of monodisperse alpha-ferric oxide nanometer sheet, so that product
Pattern it is more regular, size is more uniform.
Preferably, the preparation method of the monodisperse alpha-ferric oxide nanometer sheet, includes the following steps:
1) P123 is dissolved in ethylene glycol, 23-24h is stirred at room temperature, continue for ferric nitrate to be dissolved in ethylene glycol,
Obtain clear solution;The molar concentration of ferric nitrate is 0.5~0.6mol/L in the clear solution;P123 in the clear solution
Mass concentration be 30~35g/L;
2) KOH aqueous solution is added to the clear solution in step 1), obtains precursor solution russet;The forerunner
The volume fraction of ethylene glycol is 70~80% in liquid solution;The molar ratio of the ferric nitrate and KOH are as follows: 0.3~0.4:1;
3) it is 190~200 DEG C in reaction temperature by the precursor solution in step 2), carries out 28~30h of hydro-thermal reaction, obtain
To monodisperse alpha-ferric oxide nanometer sheet.
Compared with the existing technology, the beneficial effects of the present invention are embodied in:
(1) present invention process process is simple, easily controllable, and non-environmental-pollution is at low cost, is easy to large-scale production;
(2) size diameter of monodisperse alpha-ferric oxide nanometer sheet produced by the present invention is about 100nm, and thickness is about 50nm,
Product quality is stablized, purity is high, powder granule good dispersion.
(3) monodisperse alpha-ferric oxide nanometer sheet surface prepared by the present invention has coated P123, after heat treatment can be in α-
Ferric oxide nano on piece leaves one layer of unbodied C, so that alpha-ferric oxide nanometer sheet has as lithium ion battery negative material
Outstanding cycle performance.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram for the monodisperse alpha-ferric oxide nanometer sheet that embodiment 1 synthesizes;
Fig. 2 is the scanning electron microscope diagram for the monodisperse alpha-ferric oxide nanometer sheet that embodiment 1 synthesizes;
Fig. 3 is the preceding charging and discharging curve three times for the monodisperse alpha-ferric oxide nanometer sheet that embodiment 1 synthesizes;
Fig. 4 is the scanning electron microscope diagram for the alpha-ferric oxide nanometer sheet that comparative example 1 synthesizes;
Fig. 5 is the preceding charging and discharging curve three times for the alpha-ferric oxide nanometer sheet that comparative example 1 synthesizes;
Fig. 6 is the scanning electron microscope diagram for the alpha-ferric oxide particle that comparative example 2 synthesizes;
Fig. 7 is the Fe that comparative example 3 synthesizes3O4Scanning electron microscope diagram.
Specific embodiment
The invention will be further described with Figure of description with reference to embodiments.
Embodiment 1
1) it takes 1g P123 to be dissolved in 30ml ethylene glycol, at room temperature by stirring for 24 hours, forms clear solution;It takes
0.015mol Fe(NO3)39H2O is dissolved in above-mentioned P123 ethylene glycol solution;
2) it takes 0.04mol KOH to be dissolved in the deionized water of 10ml simultaneously, is sufficiently stirred, form clear solution;
3) aqueous solution of above-mentioned KOH is slowly dropped in the ethylene glycol solution of P123 to form presoma russet molten
Precursor solution is transferred in 50ml ptfe autoclave and carries out 200 DEG C by liquid, and 30h hydro-thermal reaction produces hydro-thermal reaction
Object filtering, cleaning are dried to obtain monodisperse alpha-ferric oxide nanometer sheet.
XRD characterization is carried out to the resulting monodisperse alpha-ferric oxide nanometer sheet of embodiment 1, as shown in Figure 1, X-ray diffraction is surveyed
Bright product of taking temperature is pure phase, and miscellaneous phase Fe is not present3O4, it was demonstrated that the product crystallinity being prepared is good, is not introduced into reaction process
Impurity.
SEM characterization is carried out to the resulting monodisperse alpha-ferric oxide nanometer sheet of embodiment 1, as shown in Fig. 2, product is monodisperse
Alpha-ferric oxide nanometer sheet, diameter is about 100nm, and thickness is about 50nm, and product favorable dispersibility, does not occur reuniting existing
As.
Embodiment 2
1) it takes 1g P123 to be dissolved in 20ml ethylene glycol, passes through the stirring of 20h at room temperature, form clear solution;It takes
0.02mol Fe(NO3)39H2O is dissolved in P123 ethylene glycol solution;
2) it takes 0.035mol KOH to be dissolved in the deionized water of 10ml simultaneously, is sufficiently stirred, form clear solution;
3) aqueous solution of above-mentioned KOH is slowly dropped to formation bronzing precursor solution in the ethylene glycol solution of P123,
Precursor solution is transferred in 50ml ptfe autoclave and carries out 200 DEG C, for 24 hours hydro-thermal reaction, by hydro-thermal reaction product
Filtering, cleaning, is dried to obtain monodisperse alpha-ferric oxide nanometer sheet.
Embodiment 3
1) it takes 2g P123 to be dissolved in 25ml ethylene glycol, passes through the stirring of 30h at room temperature, form clear solution;It takes
0.02mol Fe(NO3)39H2O is dissolved in P123 ethylene glycol solution;
2) it takes 0.06molKOH to be dissolved in the deionized water of 10ml simultaneously, is sufficiently stirred, form clear solution;
3) aqueous solution of above-mentioned KOH is slowly dropped to formation bronzing precursor solution in the ethylene glycol solution of P123,
Precursor solution is transferred in 50ml ptfe autoclave and carries out 200 DEG C, for 24 hours hydro-thermal reaction, by hydro-thermal reaction product
Filtering, cleaning, is dried to obtain monodisperse alpha-ferric oxide nanometer sheet.
Comparative example 1:
1) 0.015mol Fe(NO3)39H2O is taken to be dissolved in 30ml ethylene glycol solution;
2) it takes 0.04mol KOH to be dissolved in the deionized water of 10ml simultaneously, is sufficiently stirred, form clear solution;
3) by the aqueous solution of above-mentioned KOH be slowly dropped in the ethylene glycol solution of ferric nitrate formed bronzing presoma it is molten
Precursor solution is transferred in 50ml ptfe autoclave and carries out 200 DEG C by liquid, and hydro-thermal reaction, hydro-thermal reaction is produced for 24 hours
Object filtering, cleaning are dried to obtain alpha-ferric oxide nanometer sheet.
The resulting alpha-ferric oxide nanometer sheet of comparative example 1 carries out SEM characterization, as shown in Figure 4.
It can be clearly seen that by Fig. 2 and Fig. 4, although alpha-ferric oxide nanometer can be obtained in the case where being not introduced into P123
Piece, but the reunion of alpha-ferric oxide nanometer sheet is very serious, these alpha-ferric oxides reunited together can be in the process of charge and discharge
In lose capacity (as shown in Figure 5) rapidly, the capacity of 500mAh/g is only maintained after 3 circulations, and after P123 is added, water
P123 can inhibit the reunion of alpha-ferric oxide nanometer sheet, obtain favorable dispersibility as surfactant in thermal process reactor
Alpha-ferric oxide nanometer sheet (as shown in Figure 2), and battery is assembled into excellent cycle performance, under same cycle-index
Capacity with 900mAh/g, and without apparent capacity attenuation in cyclic process.
Comparative example 2:
1) 0.01mol Fe(NO3)39H2O is taken to be dissolved in 30ml ethylene glycol solution;
2) it takes 0.04mol KOH to be dissolved in the deionized water of 10ml simultaneously, is sufficiently stirred, form clear solution;
3) by the aqueous solution of above-mentioned KOH be slowly dropped in the ethylene glycol solution of ferric nitrate formed bronzing presoma it is molten
Precursor solution is transferred in 50ml ptfe autoclave and carries out 200 DEG C by liquid, and hydro-thermal reaction, hydro-thermal reaction is produced for 24 hours
Object filtering, cleaning are dried to obtain alpha-ferric oxide particle.
The resulting alpha-ferric oxide particle of comparative example 2 carries out SEM characterization, as shown in Figure 6, it can be seen that obtained pattern is micro-
Grain, alpha-ferric oxide particle size cannot obtain the alpha-ferric oxide of nano-scale in 1 microns.It improves and adds in water-heat process
Fe (the NO entered3)3Amount, can promote the nucleus number formed in alpha-ferric oxide crystallization process, inhibit alpha-ferric oxide crystal grain into
One step-length is big, the final alpha-oxidation iron plate for obtaining nano-scale, and due to the Fe (NO of addition in comparative example 23)3Amount it is very few, obtain
Less than alpha-ferric oxide nanometer sheet.
Comparative example 3:
It takes 0.015mol Fe(NO3)39H2O to be dissolved in 40ml ethylene glycol solution, while 0.04molKOH being taken to be dissolved in
It states in the ethylene glycol solution of ferric nitrate, is sufficiently stirred, form black precursor solution, precursor solution is transferred to 50ml poly- four
200 DEG C are carried out in vinyl fluoride reaction kettle, hydro-thermal reaction, hydro-thermal reaction product is filtered for 24 hours, and cleaning is dried to obtain Fe3O4。
The resulting Fe of comparative example 33O4SEM characterization is carried out, as shown in fig. 7, in pure ethylene glycol solution known to comparative example 3
Middle carry out hydro-thermal reaction, excessive ethylene glycol can make part Fe in hydrothermal system3+It is reduced, the product finally obtained is size
It is distributed very non-uniform Fe3O4, cannot function as lithium ion battery negative material use.
Performance test: battery material chemical property is evaluated using button cell.
When preparing electrode plates, select PVDF and second block black respectively as binder and conductive agent, according to active material: viscous
Tie agent: the mass ratio of conductive agent 75:15:10 weighs three kinds of substances in agate mortar, and appropriate NMP wet-milling is added in dry grinding later
Homogeneous slurry is formed, is coated uniformly on copper foil later, is finally transferred in 70 DEG C of vacuum ovens dry.
After the completion of coating and drying process, the sequin that pole piece is punched to, i.e. test electrode used therein pole piece.
After pole piece is weighed, it is transferred to drying in vacuum oven, is transferred in the glove box full of argon gas later, with lithium piece
Electrode as a comparison, for type polypropylene perforated membrane as battery diaphragm, the LiPF6/DMC/EMC (1:1:1) that concentration is 1mol/L is mixed
Solution is closed as electrolyte, is sequentially placed, assembles battery, after plate pressing machine seals and stands, battery can be carried out accordingly
Electro-chemical test.
Example 1 and 1 products therefrom of comparative example carry out electro-chemical test as active material respectively, as a result as Fig. 3 with
Shown in Fig. 5, although alpha-ferric oxide nanometer sheet can be obtained in the case where being not introduced into P123, the reunion of alpha-ferric oxide nanometer sheet
Very serious, these alpha-ferric oxides reunited together can lose rapidly capacity (as shown in Figure 5) during charge and discharge,
The capacity of 500mAh/g is only maintained after 3 circulations;And after P123 is added, P123 is as surface-active in hydrothermal reaction process
Agent can inhibit the reunion of alpha-ferric oxide nanometer sheet, obtain the alpha-ferric oxide nanometer sheet of favorable dispersibility, and be assembled into battery
With excellent cycle performance (as shown in Figure 3), with the capacity of 900mAh/g under same cycle-index, and recycling
In the process without apparent capacity attenuation.
Claims (6)
1. a kind of preparation method of monodisperse alpha-ferric oxide nanometer sheet, which comprises the steps of:
1) P123 is dissolved in ethylene glycol, stirs, continues for ferric nitrate to be dissolved in ethylene glycol, obtain clear solution;It is described
The molar concentration of ferric nitrate is 0.5~2mol/L in clear solution;In the clear solution mass concentration of P123 be 30~
80g/L;
2) KOH aqueous solution is added to the clear solution in step 1), obtains precursor solution russet;The presoma is molten
The volume fraction of ethylene glycol is 60~80% in liquid;
3) it is 180~200 DEG C in reaction temperature by the precursor solution in step 2), carries out 24~30h of hydro-thermal reaction, obtain list
Disperse alpha-ferric oxide nanometer sheet.
2. the preparation method of monodisperse alpha-ferric oxide nanometer sheet according to claim 1, which is characterized in that the step 1)
It is middle that P123 is dissolved in ethylene glycol, 20-30h is stirred at room temperature.
3. the preparation method of monodisperse alpha-ferric oxide nanometer sheet according to claim 1, which is characterized in that the step 2)
The molar ratio of middle ferric nitrate and KOH are as follows: 0.25~1.25:1.
4. the preparation method of monodisperse alpha-ferric oxide nanometer sheet according to claim 3, which is characterized in that the step 2)
The molar concentration of middle KOH aqueous solution is 4~6mol/L.
5. the preparation method of monodisperse alpha-ferric oxide nanometer sheet according to claim 1, which is characterized in that the step 3)
The reaction temperature of middle hydro-thermal reaction is 190~200 DEG C, and the reaction time is 26~30h.
6. the preparation method of monodisperse alpha-ferric oxide nanometer sheet according to claim 1, which is characterized in that including walking as follows
It is rapid:
1) P123 is dissolved in ethylene glycol, 23-24h is stirred at room temperature, continued for ferric nitrate to be dissolved in ethylene glycol, obtain
Clear solution;The molar concentration of ferric nitrate is 0.5~0.6mol/L in the clear solution;The matter of P123 in the clear solution
Amount concentration is 30~35g/L;
2) KOH aqueous solution is added to the clear solution in step 1), obtains precursor solution russet;The presoma is molten
The volume fraction of ethylene glycol is 70~80% in liquid;The molar ratio of the ferric nitrate and KOH are as follows: 0.3~0.4:1;
3) it is 190~200 DEG C in reaction temperature by the precursor solution in step 2), carries out 28~30h of hydro-thermal reaction, obtain list
Disperse alpha-ferric oxide nanometer sheet.
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CN102936033A (en) * | 2012-12-04 | 2013-02-20 | 九江学院 | Method for preparing monodisperse zinc oxide ultrathin nanosheets |
CN106082353A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of ferric oxide nano sheet |
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CN106082353A (en) * | 2016-06-12 | 2016-11-09 | 常州大学 | A kind of preparation method of ferric oxide nano sheet |
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