CN105789579B - A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C - Google Patents
A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C Download PDFInfo
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- 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
- H01M4/364—Composites as mixtures
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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
- H01M10/052—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
- 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
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- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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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
- H01M4/58—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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- 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 lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C；This method uses biochemical process, is stay in place form, carbon source and reducing agent using the serious black liquid of discarded, environmental pollution, by adsorbing Fe3+And hydro-thermal reaction, form presoma Fe3O4With the mixture of plant fiber, three phase heat treatments of lower progress are protected through nitrogen atmosphere, obtain lithium ion battery negative material Fe3O4/Fe2O3/Fe/C.The material is as lithium ion battery negative material, and excellent electrochemical performance, synthesis technology is simple, cost is relatively low, reduces environmental pollution, available for preparing small portable or large-sized power lithium ion battery.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium ion battery negative material, are specifically a kind of bionical using black liquid
Lithium ion battery negative material Fe of the synthesis with excellent chemical property3O4/Fe2O3The method of/Fe/C, belongs to lithium-ion electric
Pond negative material technical field.
Background technology
Transition-metal oxide MO (Co3O4、Fe2O3、Fe3O4With NiO etc.), based on MO+2Li++2e-=Li2O+M is converted
Mechanism, they have higher theoretical reversible capacity, and cost of material is low, and chemical stability is good, nontoxic and abundance,
So as to substitute graphite as lithium ion battery negative material.In cyclic process, MO is reduced to metal M during embedding lithium, raw simultaneously
Into Li2O takes off return reset condition reversible during lithium.These transition-metal oxides are showed as lithium ion battery negative material
Go out higher reversible specific capacity and energy density, this is because oxidation state is fully used in transfer process, and not
Only an electronics participates in reaction.
In above-mentioned oxide, Fe3O4Because of its natural rich reserves, environment friendly, low cost, high theoretical capacity
(924mAh g-1) and the characteristics such as nontoxicity and as the lithium ion battery negative material of most development potentiality.However, in charge and discharge
In electric cyclic process, Fe3O4Base negative material is subject to the reunion of serious volume change and active material particle, so as to draw
Structure collapses are played, it is caused to decay rapidly, capacitance loss is serious, far can not meet lithium ion of the commercialization to long circulation life
The requirement of battery.
Recent years, with continuous breakthrough of the researcher in terms of nanosecond science and technology, iron oxide is as lithium ion battery
Negative material, chemical property are greatly improved, such as：Synthesize special appearance (spherical or hollow sphere, flower-shaped and core
Shell structure etc.) iron oxide, can not only shorten the transmission range of lithium ion and electronics, but also some special patterns can delay
The volume change of iron oxide is rushed, makes its structure remained stable, largely improves the cycle performance and multiplying power of iron oxide
Performance.But at the same time can increase solid electrode resistance and contact resistance (referring to：Li Zhao,Miaomiao Gao,
Wenbo Yue, Yang Jiang,Yuan Wang,Yu Ren,and Fengqin Hu,ACS
Appl.Mater.Interfaces,2015,7, 9709-9715).The defects of in order to solve pure phase iron oxide, by iron oxide with
Carbon material is compound, and carbon material not only has excellent electrical conductivity, can improve the efficiency of transmission of lithium ion, and can reduce and receive
Contacting directly for the surface energy of nano composite material, prevention active electrode material and electrolyte, inhibits ferric oxide particles and reunites, and
Can buffer its in cyclic process volume change (referring to：L.J.Fu,H.Liu,C.Li,Y.P.Wu,E.Rahm,
R.Holze,H.Q.Wu,Solid State Sci.2006, 8,113)。
In addition, the synthesis on ferric oxide composite material has patent to disclose report, e.g., Chinese patent literature at home
CN103022422A discloses a kind of method that activated carbon nano-tube/lithium iron oxide ion electrode materials are prepared with solid phase method, should
Method modifies original carbon nanotubes surface texture using phase oxidative agent, will while significantly improving specific surface area of carbon nanotube
Iron nano-particle is direct oxidation into iron oxide, and this process simplify synthesis technologies, and still, it is artificial to operate carbon nanotubes used
Synthesis, building-up process is more difficult to control, is unfavorable for commercially producing.
Pulp and paper industry is one of important industry of Chinese national economy, however it is to the pollution problem caused by environment
Also become increasingly conspicuous.Paper waste containing a large amount of fibers, pigment and inorganic salts makes water body blackening (being known as black liquid), and has spy
Different peculiar smell, biochemical oxygen consumption magnitude is very high, can largely consume the dissolved oxygen in water, influence water quality；It is a large amount of existing in black liquor
Alkaline matter makes water PH value drastically raise, and destroys water body balance.If substance in black liquid can be carried out comprehensive sharp again
With lithium ion battery electrode material of the synthesis with superperformance can not only reduce its pollution to environment, but also can be real
Now certain economic benefit.
The content of the invention
Profit is seriously polluted and its recycled caused by environment for deficiency and black liquid existing for existing iron oxide material
With the present invention is a kind of to utilize black liquid bio-mimetic syntheses lithium ion battery negative material Fe3O4/Fe2O3The method of/Fe/C is made
Material can be used as lithium ion battery negative material.
Raw material explanation：
The raw material black liquid that the present invention uses is the waste liquid discharged in alkali paper-making production process.Containing micro in waste liquid
Soluble ion and the organic matters such as a large amount of celluloses, lignin, hemicellulose, wherein the content of lignin is in waste liquid
The content of 20wt% or so, cellulose and hemicellulose is 25wt% or so.
Term explanation
Bio-mimetic syntheses：The process that the in vivo reaction of mimic biology and natural goods structure are synthesized.
Technical solution of the present invention is as follows：
A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is as follows including step：
(1) plant fiber is to Fe3+Absorption
Black liquid is taken, Fe is added dropwise under stirring3+Solution to system pH is 6~8, and 1~2h of stirring and adsorbing makes papermaking
Plant fiber fully adsorbs Fe in black liquor3+Fe in solution3+, obtain mixed sediment；
(2) preparation of composite material precursor
Hydro-thermal process 8h~the 12h at 160 DEG C~190 DEG C of temperature of mixed sediment made from step (1), separation of solid and liquid,
Washing obtains composite material precursor after dry；
(3) heat treatment of composite material precursor
By composite material precursor made from step (2) under inert gas shielding, through three phase heat treatment 7h~13h,
Lithium ion battery negative material Fe is obtained after natural cooling3O4/Fe2O3/Fe/C。
Preferred according to the present invention, the black liquid in step (1) is the waste liquid discharged in alkali paper-making production process.
It is preferred according to the present invention, Fe3+The concentration of solution is 0.5~3mol/L, it is preferred that Fe3+The concentration of solution is
1mol/L。
Preferred according to the present invention, described Fe3+Solution is iron chloride or iron nitrate solution.
Preferred according to the present invention, in step (2), hydro-thermal process temperature is 170 DEG C~180 DEG C, the reaction time for 8h~
10h；Preferably, 180 DEG C of hydro-thermal process temperature, reaction time 10h.
It is preferred according to the present invention, in step (2), wash and washed for washing and alcohol.
Preferred according to the present invention, in step (2), the drying temperature is 50~70 DEG C, drying time 1h.
Preferred according to the present invention, in step (3), three phase heat treatments are specially：Respectively through 300~400 DEG C, 500~
After 600 DEG C of 2~4h of heat treatment, then it is warming up to 700~900 DEG C and carries out 3~5h of heat treatment.
It is further preferred that three phase heat treatments are specially：300 DEG C of heat treatment 2h, are progressively warming up to 550 DEG C of heat treatments
4h is finally warming up to 800 DEG C of heat treatment 4h.
Preferred according to the present invention, in step (3), inert gas is nitrogen.
The synthetic method of the present invention is to be combined biotechnology with chemical synthesis, by positively charged Fe3+It is negative with band
The plant fiber solution of charge mixes, and under the active force to attract each other between positive and negative charge, makes Fe3+Easily absorption deposits to
On the plant fibers such as lignin, cellulose and hemicellulose.After heat treatment, ferriferous oxide nanometer is formed in plant fibre surface
Particle.In the synthesis process, the organic matter in black liquid has not only acted as the effect of stay in place form and reducing agent, and is system
Standby Fe3O4/Fe2O3/ Fe/C nanocomposites provide conductive carbon source, improve Fe3O4/Fe2O3/ Fe/C nanocomposites
Chemical property；Meanwhile some in black liquid are difficult to the organic matter degraded realize recycle, it significantly reduces pair
The harm of environment.
The Fe that step (3) of the present invention obtains3O4/Fe2O3/ Fe/C composite materials are carried out as lithium ion battery negative material
Using specific application process is as follows：
1) by Fe3O4/Fe2O3/ Fe/C composite materials are fully ground with conductive agent and binding agent mix after, add in N- methyl
Pyrrolidinone solvent obtains precoating refined slurries after stirring evenly；
2) precoating of step (1) is refined slurries to be coated on copper foil, then by after electrode slice drying process up to lithium from
Sub- battery cathode electrode slice, gained negative electrode of lithium ion battery electrode slice are used for button-type battery or soft-package battery lithium ion battery.
Fe prepared by the present invention3O4/Fe2O3/ Fe/C nanocomposites are 0~3V in charging/discharging voltage, in 50mA/
Initial charge, specific discharge capacity under the current density of g respectively reach 1137mAh/g and 2343.6mAh/g；It is cycling 80 times
Afterwards, specific discharge capacity stabilization is in 557.7mAh/g.
Beneficial effects of the present invention are as follows：
Compared with prior art, the present invention it is advantageous that it is stay in place form using the organic matter in black liquid, conduction
Carbon source and reducing agent, using immature earthen sites, the bio-mimetic syntheses lithium ion battery negative material of excellent electrochemical performance
Fe3O4/Fe2O3/ Fe/C composite materials, synthesis technology is simple, cost is relatively low, reduces environmental pollution, available for preparing miniature portable
Formula or large-sized power lithium ion battery.
Description of the drawings
Fig. 1 is the lithium ion battery negative material Fe that embodiment 1 synthesizes3O4/Fe2O3The XRD diagram of/Fe/C, wherein ordinate
For diffracted intensity, abscissa is angle of diffraction (2 θ).
Fig. 2 is the lithium ion battery negative material Fe that embodiment 1 synthesizes3O4/Fe2O3The chemical property curve of/Fe/C
Figure.
Specific embodiment
Below by specific embodiment and with reference to attached drawing, the present invention will be further described, but not limited to this.
Raw materials used in embodiment is convenient source.
Embodiment 1
A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C, step are as follows：
(1) 50mL alkali paper-making black liquors are taken, the Fe that concentration is 1mol/L is added dropwise under the conditions of being stirred at room temperature3+Solution is to pH
It is worth for 7, is then sufficiently stirred 1.5h, forms Fe (OH)3With the mixed sediment of plant fiber；
(2) mixed sediment is transferred to 180 DEG C of reaction 10h in reaction kettle, is washed after separation of solid and liquid through 3 times, 1 alcohol
It washes, composite material precursor Fe is obtained after 60 DEG C of dry 1h3O4With the mixture of plant fiber；
(3) again by composite material precursor under the conditions of nitrogen atmosphere, through 300 DEG C of heat treatment 2h, 550 DEG C are progressively warming up to
4h is heat-treated, 800 DEG C of heat treatment 4h is finally warming up to, lithium ion battery negative material Fe is made after natural cooling3O4/Fe2O3/
Fe/C, XRD diagram are as shown in Figure 1.
Electrochemical property test
By lithium ion battery negative material Fe made from the embodiment3O4/Fe2O3/ Fe/C is used as negative electrode of lithium ion battery material
Material, electrode is prepared using rubbing method.By F lithium ion battery negative materials Fe3O4/Fe2O3/ Fe/C, acetylene black and Kynoar
(PVDF) 80 are pressed：10：10 mass ratio is fully ground mixing, is obtained after addition N-Methyl pyrrolidone stirring solvent is uniform pre-
Apply refined slurries；Above-mentioned precoating is refined slurries to be respectively coated on copper foil, after 60 DEG C of dry 6h, is done through 110 DEG C of vacuum
Dry 10h is cut into the disk of diameter 15mm after natural cooling using sheet-punching machine, that is, negative electrode of lithium ion battery electrode slice is made.
According to the suitable of anode cover-electrode slice-lithium electrolyte-membrane-lithium electrolyte-lithium piece-gasket-spring leaf-negative electrode casing
Sequence is assembled successively, recycles sealing machine by cell sealing, you can CR2032 type button half-cells are made.Finally in A713-
2008S-3TGF-A types high-precision charge and discharge instrument carries out constant current charge-discharge test to battery.
First discharge specific capacity in 0~3V voltage ranges and under 50mA/g current densities is 2343.7mAh/g；Xun Huan
After 80 times, specific discharge capacity stabilization is in 557.7mAh/g (being more than the theoretical specific capacity 375mAh/g of graphite electrode), electrification
It is as shown in Figure 2 to learn cycle performance.
Embodiment 2
A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C, step are as follows：
(1) 50mL alkali paper-making black liquors are taken, the Fe that concentration is 1mol/L is added dropwise under the conditions of being stirred at room temperature3+Solution is to pH
It is worth for 8, is then sufficiently stirred 1h, forms Fe (OH)3With the mixed sediment of plant fiber；
(2) mixed sediment is transferred to 160 DEG C of reaction 12h in reaction kettle, is washed after separation of solid and liquid through 3 times, 1 alcohol
It washes, composite material precursor Fe is obtained after 60 DEG C of dry 1h3O4With the mixture of plant fiber；
(3) again by composite material precursor under the conditions of nitrogen atmosphere, through 300 DEG C of heat treatment 3h, 550 DEG C are progressively warming up to
2h is heat-treated, 800 DEG C of heat treatment 5h is finally warming up to, lithium ion battery negative material Fe is made after natural cooling3O4/Fe2O3/
Fe/C。
By lithium ion battery negative material Fe made from the embodiment3O4/Fe2O3/ Fe/C is used as negative electrode of lithium ion battery material
Material, the experimental method as described in embodiment 1 are made negative electrode of lithium ion battery electrode slice, are then assembled into button half-cell, carry out
Constant current charge-discharge is tested；In 0~3V voltage ranges and under 50mA/g current densities, first discharge specific capacity is
2153.8mAh/g；After Xun Huan 80 times, specific discharge capacity 377.4mAh/g.
Embodiment 3,
A kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C, step are as follows：
(1) 50mL alkali paper-making black liquors are taken, the Fe that concentration is 1mol/L is added dropwise under the conditions of being stirred at room temperature3+Solution is to pH
It is worth for 6, is then sufficiently stirred 2h, forms Fe (OH)3With the mixed sediment of plant fiber；
(2) mixed sediment is transferred to 190 DEG C of reaction 8h in reaction kettle, is washed after separation of solid and liquid through 3 washings, 1 alcohol,
Composite material precursor Fe is obtained after 60 DEG C of dry 1h3O4With the mixture of plant fiber；
(3) again by composite material precursor under the conditions of nitrogen atmosphere, through 300 DEG C of heat treatment 4h, 550 DEG C are progressively warming up to
3h is heat-treated, 900 DEG C of heat treatment 3h is finally warming up to, lithium ion battery negative material Fe is made after natural cooling3O4/Fe2O3/
Fe/C。
By lithium ion battery negative material Fe made from the embodiment3O4/Fe2O3/ Fe/C is used as negative electrode of lithium ion battery material
Material, the experimental method as described in embodiment 1 are made negative electrode of lithium ion battery electrode slice, are then assembled into button half-cell, carry out
Constant current charge-discharge is tested；In 0~3V voltage ranges and under 50mA/g current densities, first discharge specific capacity is
1157.6mAh/g；After Xun Huan 80 times, specific discharge capacity stabilization is in 265.3mAh/g.
Claims (8)
1. a kind of lithium ion battery negative material Fe3O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is as follows including step：
（1）Plant fiber is to Fe3+Absorption
Black liquid is taken, Fe is added dropwise under stirring3+Solution to system pH is 6~8, and 1~2h of stirring and adsorbing makes black liquid
Middle plant fiber fully adsorbs Fe3+Fe in solution3+, obtain mixed sediment；
（2）The preparation of composite material precursor
Step（1）Mixed sediment obtained hydro-thermal process 8h~12h at 160 DEG C~190 DEG C of temperature, separation of solid and liquid, washing,
Composite material precursor is obtained after drying；
（3）The heat treatment of composite material precursor
By step（2）Composite material precursor obtained is under inert gas shielding, through three phase heat treatment 7h~13h, three ranks
Section is heat-treated：After 300~400 DEG C are heat-treated 2~4h again after 500~600 DEG C are heat-treated 2~4h, then be warming up to
700~900 DEG C carry out 3~5h of heat treatment；Lithium ion battery negative material Fe is obtained after natural cooling3O4/Fe2O3/Fe/C。
2. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, step（1）In black liquid be the waste liquid discharged in alkali paper-making production process.
3. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, Fe3+The concentration of solution is 0.5~3mol/L.
4. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, step（2）In, hydro-thermal process temperature is 170 DEG C~180 DEG C, and the reaction time is 8h~10h.
5. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, step（2）In, it washs and is washed for washing and alcohol.
6. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, step（2）In, the drying temperature is 50~70 DEG C, drying time 1h.
7. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is that three phase heat treatments are specially：300 DEG C of heat treatment 2h are progressively warming up to 550 DEG C of heat treatment 4h, are finally warming up to 800
DEG C heat treatment 4h.
8. lithium ion battery negative material Fe according to claim 13O4/Fe2O3The biomimetic synthesis method of/Fe/C, it is special
Sign is, step（3）In, inert gas is nitrogen.
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| CN106315686B (en) * | 2016-08-03 | 2018-01-16 | 江苏大学 | A kind of ball cactus shape magnetic Fe3O4/Fe2O3Nano heterogeneous body material and preparation method thereof |
| CN107452960A (en) * | 2017-07-06 | 2017-12-08 | 陕西科技大学 | A kind of preparation method of black liquid conversion porous carbon anode material of lithium-ion battery |
| CN107507978B (en) * | 2017-07-28 | 2019-10-08 | 齐鲁工业大学 | A kind of sodium-ion battery FeS2/Fe3O4/ C negative electrode material and preparation method thereof |
| CN108598409B (en) * | 2018-04-19 | 2020-07-10 | 齐鲁工业大学 | Lithium ion battery cathode material FeS/Fe/C and preparation method thereof |
| JP7059951B2 (en) * | 2019-02-05 | 2022-04-26 | トヨタ自動車株式会社 | Negative electrode layer and all-solid-state battery |
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