CN105140494B - A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C - Google Patents
A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C Download PDFInfo
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- CN105140494B CN105140494B CN201510378518.3A CN201510378518A CN105140494B CN 105140494 B CN105140494 B CN 105140494B CN 201510378518 A CN201510378518 A CN 201510378518A CN 105140494 B CN105140494 B CN 105140494B
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Abstract
The present invention relates to a kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C.This method is template and carbon source using cheap, native cellulose cotton, is first made active nano cellulose, then with FeCl3·6H2The O aqueous solution is mixed, and then adding ammoniacal liquor makes it produce precipitation, then by hydro-thermal process formation presoma Fe3O4With the mixture of cellulose；It is heat-treated in a nitrogen atmosphere, Fe is obtained3O4/ Fe/C nano composite materials.Composite prepared by the present invention is as lithium cell cathode material, available for preparing power lithium-ion battery.
Description
Technical field
The present invention relates to a kind of iron oxide/iron/carbon (Fe with good chemical property3O4/ Fe/C) nano combined battery
The biomimetic synthesis method of electrode material, belongs to lithium ion battery material technical field.
Background technology
Transition metal oxide, particularly nanocrystalline transition metal oxide, because with raw material sources are abundant, cost compared with
It is excellent that low, metal oxide particle size (from nanometer to micron) is easy to adjustment, theoretical energy density height etc. with shape and positioning
Gesture, and as important lithium ion battery negative material.
In transition metal oxide, iron oxide due to the advantage such as theoretical specific capacity height, nature rich reserves, nontoxic,
Cause domestic and international people greatly to pay close attention to, it is considered to be the lithium ion battery negative material of great application potential.But oxidation
Iron Volume Changes in charge and discharge process are larger, and along with larger Volume Changes, easily cause the efflorescence of electrode material, cause
The rapid decay of capacity, decays rapid especially under high current density, far from meet current commercial li-ion battery for
The big multiplying power of electrode material, long-life demand.
Relevant synthetic iron oxide material also has some document reports at present, for example, Chinese patent literature CN103022422A
A kind of method that active carbon nanotube/ferric oxide lithium ion battery electrode material is prepared with solid phase method is disclosed, this method is utilized
Original carbon nanotubes surface texture is modified in phase oxidative agent, while significantly improving specific surface area of carbon nanotube, by iron nanometer
Grain is direct oxidation into iron oxide.But CNT used by this method has high cost, preparation method complexity and material source can not
The shortcomings of regeneration.
Chinese patent literature CN104157832A discloses a kind of ferroferric oxide/carbon composite lithium ion battery material
Preparation method.Bombax cotton after purified treatment is immersed certain density Fe (NO by this method first3)3In solution, kapok is treated
Fiber, which becomes to take out after uniform yellow, to be drained.The presoma for obtaining iron hydroxide/carbon is spread using ammonia, is produced after heat treatment
To Fe3O4/ C composite.But ammonia diffusion process requires higher to experiment condition, and iron hydroxide is crystallized in prepared presoma
Degree is poor, and final calcining produces Fe3O4Grain structure ruptures, and easily reunites.
The existing modification for transition metal oxide has that agents useful for same is poisonous, dangerous, synthesis technique is complicated, cost
The problems such as expensive, building-up process hardly possible is controlled.According to the market demand of lithium ion battery and energy-conserving and environment-protective requirement, it is badly in need of research and opens
The negative material for sending out new, further improves its chemical property, and reduction synthesis cost reduces environmental pollution and reproducible utilization,
So as to the need for meeting new energy field to lithium ion battery material.
The content of the invention
The deficiency of cycle performance and the high rate performance difference existed for existing iron oxide material, the present invention provides a kind of
Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C.The present invention is by biotechnology and chemical synthesis process
It is combined, obtained material can be used as lithium ion battery negative material.
Term explanation
Bio-mimetic syntheses：The process that reaction and natural goods structure in mimic biology body are synthesized.
Technical scheme is as follows：
A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, including step are as follows：
(1) preparation of nano-cellulose biological template
In the sulfuric acid solution that amount of substance concentration (10~15) mol/L is soaked in after native cellulose is shredded, in 30 DEG C~
60 DEG C are incubated 30~60 minutes, and separation of solid and liquid, solid is washed to neutrality, and active nano cellulose, active nano are made after drying
Cellulose is used as biological template；
(2)) the preparation of composite material precursor
It is (0.06~0.069) mol/L's that active nano cellulose made from step (1) is dipped in into amount of substance concentration
FeCl3·6H2In the O aqueous solution, active nano cellulose and FeCl3·6H2The mass volume ratio of the O aqueous solution is：1：(60~
80), unit g/ml；1-3h is stirred at room temperature, pH=8 is then adjusted, and forms Fe (OH)3With the mixed sediment of cellulose, adjust
The mixed liquor after pH is saved in 160 DEG C~200 DEG C hydro-thermal process 2h~6h, separation of solid and liquid, washing obtains presoma Fe after drying3O4
With the mixture of cellulose；
(3) heat treatment of composite material precursor
By presoma Fe made from step (2)3O4Mixture with cellulose is warming up to 600 DEG C under inert gas shielding
~800 DEG C carry out heat treatment 3~5 hours, after natural cooling, and Fe is made3O4/ Fe/C nano composite materials.
It is cotton, fiber crops or silk flosssilk wadding, highly preferred, described day according to currently preferred, described native cellulose
Right cellulose is cotton, and native cellulose is cut into 3~6mm of length chip.
According to currently preferred, in step (1), the mass volume ratio of native cellulose and sulfuric acid solution is：1：(10~
15), unit g/ml, the amount of substance concentration of sulfuric acid solution is preferably 15mol/L.
According to currently preferred, in step (1), reaction temperature is 40 DEG C~50 DEG C, and the reaction time is 30~50 minutes,
It is preferred that, reaction temperature is 45 DEG C, and the reaction time is 40 minutes.
According to currently preferred, in step (1), drying temperature is 50 DEG C~60 DEG C.
According to currently preferred, in step (2), active nano cellulose and FeCl3·6H2The quality volume of the O aqueous solution
Than for：1：80, unit g/ml, FeCl3·6H2The amount of substance concentration of the O aqueous solution is 0.069mol/L.
According to currently preferred, in step (2), hydro-thermal process temperature is 170 DEG C~190 DEG C, the hydro-thermal time is 3~
5h, it is preferred that hydro-thermal process temperature is 180 DEG C, the hydro-thermal time is 4h.
According to currently preferred, in step (2), drying temperature is 70 DEG C~80 DEG C.
According to currently preferred, in step (2), ammonia spirit regulating system pH=8 is added, the quality of ammonia spirit is dense
Spend for 25~35wt%.
According to currently preferred, in step (3), heat treatment temperature is 650 DEG C~800 DEG C, and heat treatment time 4~5 is small
When, it is preferred that heat treatment temperature is 700 DEG C, and heat treatment time is 4h.
According to currently preferred, in step (3), inert gas is nitrogen.
, according to the invention it is preferred to, synthetic method of the invention is by biotechnology and chemical synthesis phase in step (3)
With reference to by positively charged Fe3+Mixed with negatively charged cellulose solution, the active force attracted each other between positive and negative charge
Under, make iron ion be easier to adsorb on the green alga sphaerocyst for depositing to cellulose.After heat treatment, on cellulose template surface
20~100nm of upper formation Fe3O4Nano particle, so as to realize the bio-mimetic syntheses of nano-sized iron oxide.During bio-mimetic syntheses,
Cellulose has not only acted as the effect of stay in place form, and to prepare Fe3O4/ Fe/C nano composite materials provide conductive carbon
Source and nanoparticle binder, so as to improve Fe3O4Bulk density, electric conductivity and the specific capacity of/Fe/C nano composite materials.
It is currently preferred, above-mentioned Fe3O4The application of/Fe/C nano composite materials, the Fe3O4The nano combined materials of/Fe/C
Expect the negative material as lithium ion battery.
Specific application process is as follows：
(1) by Fe3O4/ Fe/C nano composite materials are fully ground with conductive agent and binding agent mix after, add N- methyl pyrroles
Pyrrolidone solvent, obtains precoating refined slurries after stirring；
(2) above-mentioned precoating is refined into slurries to be coated on Copper Foil, then will produces lithium-ion electric after electrode slice drying process
Pond negative electricity pole piece, gained lithium ion battery negative electrode slice is used for button-type battery or soft-package battery lithium ion battery.
Fe prepared by the inventive method3O4/ Fe/C nano composite materials, are that 0~3.0V and 1A/g is big in charging/discharging voltage
First charge-discharge specific capacity under current density respectively reaches 596.8mAh/g and 903.8mAh/g；Electric discharge ratio after circulating 60 times
Capacity still can reach 524.6mAh/g.
The present invention compared with the prior art, it is advantageous that being stay in place form and conductive carbon source using native cellulose cotton
And nanoparticle binder, using simple preparation technology, bio-mimetic syntheses have good circulation performance and high rate performance
Fe3O4/ Fe/C nano composite anode materials, the reagent that uses is nontoxic, synthesis technique is simple, cost is relatively low, can be used as negative material
For preparing power lithium-ion battery.
Brief description of the drawings
Fig. 1 is presoma Fe made from the embodiment of the present invention 13O4Mixture, Fe with cellulose3O4/ Fe/C is nano combined
The XRD of material, wherein left ordinate is intensity, abscissa is angle of diffraction (2 θ).
Fig. 2 is Fe made from the embodiment of the present invention 13O4The SEM figures of/Fe/C nano composite materials；
Fig. 3 is Fe made from the embodiment of the present invention 13O4The electrochemistry cycle performance curve of/Fe/C nano composite materials
Figure.
Embodiment
With reference to embodiment, the present invention will be further described, but not limited to this.
Embodiment 1
A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, preparation process is as follows：
(1) 3g cottons are cut into the chip that length is 5mm and are soaked in the sulfuric acid solution that 45mL amount of substance concentration is 15mol/L
In, 40 minutes are incubated through 45 DEG C, separation of solid and liquid, solid is washed to neutrality and dried under the conditions of 60 DEG C, obtain active nano fine
Dimension element, active nano cellulose is used as biological template.
(2) active nano cellulose lg made from step (1)) is dipped in the FeCl that 80ml concentration is 0.069mol/L3·
6H2In the O aqueous solution, 2h is stirred at room temperature, is then added mass concentration 25wt% ammonia spirits regulation pH=8, is formed Fe (OH)3
With the mixed sediment of cellulose, the mixed liquor after pH will be adjusted in 180 DEG C of hydro-thermal process 4h, separation of solid and liquid, 4 washings, in
Presoma Fe is obtained after 80 DEG C of dryings3O4With the mixture of cellulose；
The presoma Fe that this step is obtained3O4XRD with the mixture of cellulose is as shown in Figure 1.
(3) again by obtained presoma Fe3O4With the mixture of cellulose in a nitrogen atmosphere, 700 DEG C are warming up to and carries out heat
Processing 4 hours, after natural cooling, is made Fe3O4/ Fe/C nano composite materials.
The Fe that the present embodiment is obtained3O4The XRD of/Fe/C nano composite materials is as shown in figure 1, SEM figures are as shown in Figure 2.
Electrochemical property test
Fe prepared by the embodiment3O4/ Fe/C nano composite materials are used as lithium ion battery negative material, using coating
Method prepares electrode.By Fe3O4/ Fe/C nano composite materials, acetylene black and Kynoar (PVDF) press 80：10：10 mass ratio
Mixing is fully ground, obtains precoating refined slurries after addition 1-METHYLPYRROLIDONE stirring solvent is uniform；Above-mentioned precoating is refined
Slurries are respectively coated on Copper Foil, are cut into directly using sheet-punching machine after drying 6h or 20 DEG C of vacuum drying 12h, natural cooling through 60 DEG C
Footpath 15cm disk, that is, be made lithium ion battery negative electrode slice.
According to anode cover-electrode slice-electrolyte-barrier film-electrolyte-lithium piece-pad-spring leaf-negative electrode casing order according to
Secondary assembling, recycles sealing machine by cell sealing, you can CR2032 type button half-cells are made.
It is last that constant current charge-discharge test is carried out to battery in A713-2008S-3TGF-A types high-precision discharge and recharge instrument.Fill
Discharging condition：First discharge specific capacity in 0~3.0V voltage ranges and under 1A/g current densities is 903.8mAh/g, is passed through
Specific discharge capacity after 60 circulations still can reach 524.6mAh/g, and test result is as shown in Figure 3.
Embodiment 2
A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, preparation process is as follows：
(1) 3g cottons are cut into the chip that length is 5mm and are soaked in the sulfuric acid solution that 45mL amount of substance concentration is 15mol/L
In, 60 minutes are incubated through 30 DEG C, separation of solid and liquid, solid is washed to neutrality and dried under the conditions of 60 DEG C, obtain active nano fine
Dimension element, active nano cellulose is used as biological template.
(2) active nano cellulose lg made from step (1)) is dipped in the FeCl that 80ml concentration is 0.069mol/L3·
6H2In the O aqueous solution, 2h is stirred at room temperature, is then added mass concentration 25wt% ammonia spirits regulation pH=8, is formed Fe (OH)3
With the mixed sediment of cellulose, the mixed liquor after pH will be adjusted in 160 DEG C of hydro-thermal process 6h, separation of solid and liquid, 4 washings, in
Presoma Fe is obtained after 80 DEG C of dryings3O4With the mixture of cellulose；
(3) again by obtained presoma Fe3O4With the mixture of cellulose in a nitrogen atmosphere, 600 DEG C are warming up to and carries out heat
Processing 5 hours, after natural cooling, is made Fe3O4/ Fe/C nano composite materials.
The composite is constituted into half-cell of the lithium piece to electrode, is that 0~3.0V and 1A/g electric currents are close in charging/discharging voltage
First discharge specific capacity under degree is 453.6mAh/g, and the discharge capacity after 50 charge and discharge cycles is 102.3mAh/g.
Embodiment 3
A kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, preparation process is as follows：
(1) 3g cottons are cut into the chip that length is 5mm and are soaked in the sulfuric acid solution that 45mL amount of substance concentration is 15mol/L
In, 30 minutes are incubated through 60 DEG C, separation of solid and liquid, solid is washed to neutrality and dried under the conditions of 60 DEG C, obtain active nano fine
Dimension element, active nano cellulose is used as biological template.
(2) active nano cellulose lg made from step (1)) is dipped in the FeCl that 80ml concentration is 0.069mol/L3·
6H2In the O aqueous solution, 2h is stirred at room temperature, is then added mass concentration 25wt% ammonia spirits regulation pH=8, is formed Fe (OH)3
With the mixed sediment of cellulose, the mixed liquor after pH will be adjusted in 200 DEG C of hydro-thermal process 2h, separation of solid and liquid, 5 washings, in
Presoma Fe is obtained after 80 DEG C of dryings3O4With the mixture of cellulose；
(3) again by obtained presoma Fe3O4With the mixture of cellulose in a nitrogen atmosphere, 800 DEG C are warming up to and carries out heat
Processing 3 hours, after natural cooling, is made Fe3O4/ Fe/C nano composite materials.
The composite is constituted into half-cell of the lithium piece to electrode, is that 0~3.0V and 1A/g electric currents are close in charging/discharging voltage
First discharge specific capacity under degree is 750mAh/g, and the discharge capacity after 10 charge and discharge cycles is 206mAh/g.
Claims (10)
1. a kind of Fe3O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, including step are as follows：
（1）The preparation of nano-cellulose biological template
Amount of substance concentration is soaked in after native cellulose is shredded（10~15）In mol/L sulfuric acid solution, in 30 DEG C~60 DEG C
Insulation 30~60 minutes, separation of solid and liquid, solid is washed to neutrality, and active nano cellulose, active nano fiber are made after drying
Element is used as biological template；
（2）The preparation of composite material precursor
By step（1）Obtained active nano cellulose is dipped in amount of substance concentration（0.06~0.069）Mol/L FeCl3•
6H2In the O aqueous solution, active nano cellulose and FeCl3•6H2The mass volume ratio of the O aqueous solution is：1：（60~80）, unit g/
ml；1-3h is stirred at room temperature, pH=8 is then adjusted, and forms Fe（OH）3With the mixed sediment of cellulose, the mixing after pH is adjusted
Liquid obtains presoma Fe in 160 DEG C~200 DEG C hydro-thermal process 2h~6h, separation of solid and liquid, washing after drying3O4With mixing for cellulose
Compound；
（3）The heat treatment of composite material precursor
By step（2）Obtained presoma Fe3O4Mixture with cellulose under inert gas shielding, be warming up to 600 DEG C~
800 DEG C carry out heat treatment 3~5 hours, after natural cooling, and Fe is made3O4/ Fe/C nano composite materials.
2. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In described native cellulose is cotton or fiber crops；Native cellulose is cut into 3~6mm of length chip.
3. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（1）In, the mass volume ratio of native cellulose and sulfuric acid solution is：1：（10~15）, unit g/ml, sulfuric acid solution
Amount of substance concentration be 15mol/L.
4. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（1）In, reaction temperature is 40 DEG C~50 DEG C, and the reaction time is 30~50 minutes.
5. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（1）In, drying temperature is 50 DEG C~60 DEG C.
6. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（2）In, active nano cellulose and FeCl3•6H2The mass volume ratio of the O aqueous solution is：1：80, unit g/ml,
FeCl3•6H2The amount of substance concentration of the O aqueous solution is 0.069mol/L.
7. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（2）In, hydro-thermal process temperature is 170 DEG C~190 DEG C, and the hydro-thermal time is 3~5h；Drying temperature is 70 DEG C~80 DEG C.
8. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（2）In, ammonia spirit regulating system pH=8 is added, the mass concentration of ammonia spirit is 25~35wt%.
9. Fe according to claim 13O4The biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C, its feature exists
In step（3）In, heat treatment temperature is 650 DEG C~800 DEG C, heat treatment time 4~5 hours；The inert gas used is nitrogen
Gas.
10. the Fe described in claim 13O4Fe made from the biomimetic synthesis method of the nano combined battery electrode materials of/Fe/C3O4/
The application of Fe/C nano composite materials, the Fe3O4/ Fe/C nano composite materials as lithium ion battery negative material,
Specific application process is as follows：
（1）By Fe3O4/ Fe/C nano composite materials are fully ground with conductive agent and binding agent mix after, add N- crassitudes
Ketone solvent, obtains precoating refined slurries after stirring；
（2）Above-mentioned precoating is refined into slurries to be respectively coated on Copper Foil, then lithium-ion electric will be produced after electrode slice drying process
Pond negative electricity pole piece, gained lithium ion battery negative electrode slice is used for button-type battery or soft-package battery lithium ion battery.
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| CN105645477B (en) * | 2016-03-21 | 2017-04-26 | 黄山学院 | Preparation method of ferroferric oxide |
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