CN109888206A - A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application - Google Patents
A kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application Download PDFInfo
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- CN109888206A CN109888206A CN201910065592.8A CN201910065592A CN109888206A CN 109888206 A CN109888206 A CN 109888206A CN 201910065592 A CN201910065592 A CN 201910065592A CN 109888206 A CN109888206 A CN 109888206A
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- 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 lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application belong to inorganic material preparation and nanometer energy field.The invention mainly comprises two partial contents: (1) bismuth salt being dissolved in the mixed solvent first, organic acid complexing agent is then added, pass through the complex of solvent structure bismuth；(2) under the action of protecting gas, the complex of bismuth prepared by heat treatment step (1) obtains Bi/Bi2O3/ C composite.Under the current density of 100mA/g, Bi/Bi2O3The first discharge specific capacity of/C composite is up to 352mAh/g.Bi/Bi of the invention2O3Preparation method is simple for/C composite, the nano-sized carbon and Bi and Bi that ligand pyrolysis is generated2O3It is bound tightly together, is conducive to the electric conductivity and stability for increasing active site, improving material, Bi/Bi2O3/ C composite is as lithium ion battery negative material, and between 20~100 circulations, specific capacity maintains essentially in 220mAh/g or so.Bi/Bi2O3/ C composite has broad application prospects in lithium ion battery negative material.
Description
Technical field
The invention belongs to inorganic material preparation and nanometer energy fields, and in particular to a kind of lithium ion battery negative material
Bi/Bi2O3/ C and its preparation and application.
Background technique
Bismuth oxide (Bi2O3) it is a kind of important functional material, it is extensive since it is with special physical property
Applied to photoelectric conversion material, high temperature superconducting materia and electron ceramic material etc..In addition, Bi2O3It can also be used in chemical reagent, prevent
Fiery material, high refractive index glass, nuclear engineering glass manufacture and nuclear reactor fuel etc..Since bismuth oxide has excellent electricity
Chemical stability, preferable redox reversible, therefore, bismuth oxide are considered as a kind of potential electrode material.In order to obtain
There must be the battery of high-energy density and long circulating stability, there is an urgent need to develop the negative electrode materials with excellent properties.Metal
Invertibity height and electrochemical window mouth width of the bismuth due to redox reaction, and the extensive concern by scientific worker.However, at present
The specific capacity and stability of the bismuth cathode of report are not of great satisfaction.Therefore, it is necessary to develop Bi base complex or miscellaneous
Compound improves the performance of Bi cathode.
The 1000-1006 pages of volume 80 of " ChemPlusChem " 2015 discloses " a Bi2O3@reduced graphene
oxide nanocomposite:an anode material for sodium-ion storage".Author is first in paper
Under stiring, by Bi (NO3)3·5H2O, CTAB is added in graphene oxide dispersion, and NaBH is then added dropwise4, filtered,
It is dried to obtain Bi2O3@RGO compound, is then used as the negative electrode material of battery.Under 350mA/g current density, through 200 times
Circulation volume retention rate only has 70.2%.Although the Bi of this method preparation2O3@RGO compound features go out higher specific capacity, but
Cyclical stability is poor, is unfavorable for practical application.
Up to the present, it there are no reported in literature Bi/Bi2O3/ C composite is as lithium ion battery negative material.
Summary of the invention
The object of the present invention is to provide a kind of lithium ion battery negative material Bi/Bi2O3/ C and its preparation and application.Pass through
One step is pyrolyzed bismuth-organic acid complex, obtains Bi/Bi2O3/ C composite is conducive to the electric conductivity and work that improve composite material
Property bit number of points, to further increase its performance.This method simple process, easy to operate, mild condition are suitable for industrialization
Production.
Specific technical solution is as follows:
The present invention provides a kind of lithium ion battery negative material Bi/Bi2O3The preparation method of/C, this method include following step
It is rapid:
(1) in a solvent by bismuth salt dissolution, organic acid complexing agent is then added, forms reaction mixture；
(2) mixed liquor obtained by step (1) is carried out solvent thermal reaction to be cooled to room temperature after reaction, reaction is mixed
Object is post-processed to obtain the complex of bismuth；
(3) step (2) resulting complex is finely ground；
(4) under protection gas effect, heat treatment step (3) resulting powder, obtains Bi/Bi in tube furnace2O3/ C is compound
Material.
Wherein, bismuth salt described in step (1) is one or two kinds of in bismuth chloride or bismuth nitrate.
Wherein, solvent described in step (1) be one of n,N-Dimethylformamide, methanol, formamide or ethyl alcohol or
It is two or more.
Wherein, solvent described in step (1) is mixed solvent, and affiliated mixed solvent is n,N-Dimethylformamide and first
One of alcohol, formamide and methanol, formamide and ethyl alcohol, n,N-Dimethylformamide and ethyl alcohol, corresponding volume ratio is
1:5~5:1.
Wherein, organic acid ligand agent described in step (1) is 1,3,5- benzenetricarboxylic acids, terephthalic acid (TPA) or 4,4 '-biphenyl
One or more of dioctyl phthalate.
Wherein, bismuth salt and the molar ratio of organic acid ligand described in step (1) are 1:1~1:4；Bismuth salt is in a solvent
Concentration is 5-50g/L.
Wherein, the temperature of step (2) described solvent thermal reaction is 100~160 DEG C, and the reaction time is 6~12h.
Wherein, in step (2), mixed liquor obtained by step (1) is transferred to polytetrafluoroethyllining lining, and be packed into outside reaction kettle
Shell, the post-processing be by reaction after product be centrifuged, later using n,N-Dimethylformamide, formamide,
One of methanol or ethyl alcohol a variety of are washed.Optionally, successively with n,N-Dimethylformamide or formamide, methanol or
Precipitating after ethanol washing separation.
Wherein, after step (2) post-processing is mixture centrifugation, will wash, 60~90 DEG C of vacuum drying are deposited in.
Wherein, heat treatment described in step (4) is in 400~600 DEG C of processing 60-120min；The protective gas is lazy
The one or more of property gases argon or nitrogen.
On the other hand, this application provides a kind of Bi/Bi according to made from above-mentioned preparation method2O3/ C composite.
On the other hand, a kind of Bi/Bi according to please itself be provide2O3/ C composite is in negative electrode of lithium ion battery
Application in material.
Beneficial effects of the present invention are as follows:
1) present invention process is simple, easy to operate, mild condition, favorable repeatability.
2) nano-sized carbon and Bi and Bi generated pyrolysis2O3It is bound tightly together, is conducive to increase active site, mention
The electric conductivity and stability of high material.
3)Bi/Bi2O3/ C composite, which is used as lithium ion battery negative material, has good cyclical stability.
Detailed description of the invention
Fig. 1 is Bi/Bi prepared by embodiment 12O3The XRD diagram of/C composite.
Fig. 2 is Bi/Bi prepared by embodiment 12O3The CV of/C cathode schemes.
Fig. 3 is Bi/Bi prepared by embodiment 12O3The cycle performance figure of/C cathode.
Fig. 4 is Bi/Bi prepared by embodiment 22O3The cycle performance figure of/C cathode.
Specific embodiment
The method of the present invention is explained further with reference to embodiments, is illustrated.
Embodiment 1
Bi/Bi2O3The preparation method of/C composite the following steps are included:
(1) it measures 10.0mL DMF and 20.0mL methanol to be uniformly mixed, and by five water bismuth nitrate of 0.97g and 0.84g 1,3,
5- benzenetricarboxylic acid is dissolved in the mixed solvent.
(2) by reaction mixture obtained by step (1) be transferred to polytetrafluoroethyllining lining, be sealed in stainless steel cauldron carry out it is molten
Agent thermal response, reaction temperature are 120 DEG C, reaction time 12h, after reaction, cooled to room temperature, centrifuge separation, and
Precipitating is successively washed with DMF and methanol, 60 DEG C of vacuum drying is deposited in, obtains powdered complex.
(3) the powdered complex of 1.0g is finely ground, be packed into porcelain boat, be put into tube furnace, under protection of argon gas, with 2 DEG C/
The heating rate of min is warming up to 600 DEG C, and keeps the temperature 2h, and Bi/Bi can be obtained after reaction2O3/ C composite, Bi/
Bi2O3The XRD diagram of/C composite is as shown in Figure 1.
Embodiment 2
(1) it measures 20.0mL DMF and 10.0mL methanol to be uniformly mixed, and by five water bismuth nitrate of 0.97g and 0.66g to benzene
Dioctyl phthalate is dissolved in the mixed solvent.
(2) by reaction mixture obtained by step (1) be transferred to polytetrafluoroethyllining lining, be sealed in stainless steel cauldron carry out it is molten
Agent thermal response, reaction temperature are 160 DEG C, reaction time 12h, after reaction, cooled to room temperature, centrifuge separation, and
Precipitating is successively washed with DMF and ethyl alcohol, 60 DEG C of vacuum drying is deposited in, obtains powdered complex.
(3) the powdered complex of 1.0g is finely ground, be packed into porcelain boat, be put into tube furnace, under protection of argon gas, with 5 DEG C/
The heating rate of min is warming up to 500 DEG C, and keeps the temperature 1h, and Bi/Bi can be obtained after reaction2O3/ C composite.
Embodiment 3
(1) it measures 15.0mL formamide and 15.0mL methanol to be uniformly mixed, and by 0.63g bismuth chloride and 0.97g 4,4 '-
Biphenyl dicarboxylic acid is dissolved in the mixed solvent.
(2) by reaction mixture obtained by step (1) be transferred to polytetrafluoroethyllining lining, be sealed in stainless steel cauldron carry out it is molten
Agent thermal response, reaction temperature are 100 DEG C, reaction time 12h, after reaction, cooled to room temperature, centrifuge separation, and
Precipitating is successively washed with DMF and ethyl alcohol, 60 DEG C of vacuum drying is deposited in, obtains powdered complex.
(3) the powdered complex of 1.0g is finely ground, be packed into porcelain boat, be put into tube furnace, under protection of argon gas, with 2 DEG C/
The heating rate of min is warming up to 400 DEG C, and keeps the temperature 2h, and Bi/Bi can be obtained after reaction2O3/ C composite.
The Bi/Bi prepared with embodiment 12O3/ C composite is the cathode of lithium ion battery, assembles button cell, follows
Shown in ring volt-ampere curve Fig. 2.As seen from Figure 2, there is the last one reduction peak near 0.26V, reduction potential is lower；In 1.29V
Nearby there is a Strong oxdiative peak.Lower reduction peak facilitates its use as the negative electrode material of lithium ion battery.Fig. 3 is in 100mA/g
Current density under, Bi/Bi2O3The cycle performance figure of/C cathode.From the figure 3, it may be seen that specific capacity is about through between 105 circulations
220.7mAh/g.Between 20~100 circulations, specific capacity maintains essentially in 220mAh/g or so, illustrates Bi/Bi2O3/ C is compound
Material has excellent cyclical stability.
With prior art ratio, this application provides a kind of completely new lithium ion battery negative material, present invention process letters
It is single, easy to operate, mild condition, favorable repeatability.The nano-sized carbon and Bi and Bi that pyrolysis is generated2O3It is bound tightly together,
Be conducive to the electric conductivity and stability for increasing active site, improving material.And Bi/Bi2O3/ C composite is used as lithium-ion electric
Pond negative electrode material has good cyclical stability.
The Bi/Bi prepared with embodiment 22O3/ C composite is the cathode of lithium ion battery, assembles button cell,
Cycle performance under 200mA/g current density is as shown in Figure 4.As seen from Figure 4, through between 280 circulations, specific capacity is about
191.8mAh/g.Between 20~280 circulations, specific capacity maintains essentially in this numerical value or so, further illustrates Bi/
Bi2O3/ C composite has excellent cyclical stability.
Certainly, the invention may also have other embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding variations, increase and decrease or replacement in accordance with the present invention, but these change accordingly
Change also should fall within the scope of protection of the appended claims of the present invention.
Claims (12)
1. a kind of lithium ion battery negative material Bi/Bi2O3The preparation method of/C, comprising the following steps:
(1) in a solvent by bismuth salt dissolution, organic acid complexing agent is then added, forms reaction mixture；
(2) mixed liquor obtained by step (1) solvent thermal reaction is carried out to be cooled to room temperature after reaction, by reaction mixture into
Row post-processing obtains the complex of bismuth；
(3) step (2) resulting complex is finely ground；
(4) under protection gas effect, heat treatment step (3) resulting powder, obtains Bi/Bi in tube furnace2O3/ C composite wood
Material.
2. Bi/Bi according to claim 12O3The preparation method of/C composite, wherein bismuth salt described in step (1) is chlorine
Change one or two kinds of in bismuth or bismuth nitrate.
3. Bi/Bi according to claim 1 or claim 22O3The preparation method of/C composite, wherein solvent described in step (1)
For one or more of N,N-dimethylformamide, methanol, formamide or ethyl alcohol.
4. Bi/Bi according to claim 32O3The preparation method of/C composite, wherein solvent described in step (1) is mixed
Bonding solvent, affiliated mixed solvent are n,N-Dimethylformamide and methanol, formamide and methanol, formamide and ethyl alcohol, N, N- bis-
One of methylformamide and ethyl alcohol, corresponding volume ratio are 1:5~5:1.
5. Bi/Bi according to claim 1 or claim 22O3The preparation method of/C composite, wherein organic described in step (1)
Sour ligand agent is one or more of 1,3,5- benzenetricarboxylic acid, terephthalic acid (TPA) or 4,4 '-biphenyl dicarboxylic acids.
6. Bi/Bi according to claim 1 or claim 22O3The preparation method of/C composite, wherein bismuth salt described in step (1)
Molar ratio with organic acid ligand is 1:1~1:4；The concentration of bismuth salt in a solvent is 5-50g/L.
7. Bi/Bi according to claim 12O3The preparation method of/C composite, wherein step (2) described solvent thermal reaction
Temperature be 100~160 DEG C, the reaction time be 6~12h.
8. according to claim 1 or 7 Bi/Bi2O3The preparation method of/C composite, wherein in step (2), by step
(1) gained mixed liquor is transferred to polytetrafluoroethyllining lining, and is packed into reaction kettle shell, and the post-processing is the product after reacting
It is centrifuged, using one of n,N-Dimethylformamide, formamide, methanol or ethyl alcohol or a variety of is washed later
It washs.
9. according to claim 1 or 7 Bi/Bi2O3The preparation method of/C composite, wherein step (2) described post-processing
After being centrifuged, washing by mixture, gained is deposited in 60~90 DEG C of vacuum drying.
10. Bi/Bi according to claim 12O3The preparation method of/C composite, wherein heat treatment described in step (4)
It is in 400~600 DEG C of processing 60-120min；The protective gas is the one or more of inert gas argon gas or nitrogen.
11. Bi/Bi made from preparation method described in a kind of any one of claims 1 to 102O3/ C composite.
12. application of the composite material described in claim 11 in lithium ion battery negative material.
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| CN114735690A (en) * | 2022-04-19 | 2022-07-12 | 湖南铂威新能源科技有限公司 | Preparation method of artificial graphite composite negative electrode material for lithium ion battery |
| CN115799518A (en) * | 2023-02-02 | 2023-03-14 | 暨南大学 | Bismuth/bismuth oxide nanodot/carbon sheet composite material, preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113594481A (en) * | 2021-07-22 | 2021-11-02 | 中国科学院上海硅酸盐研究所 | Carbon dioxide reduction electrocatalyst and preparation method and application thereof |
| CN113839038A (en) * | 2021-08-12 | 2021-12-24 | 山东大学 | MOF-derived Bi @ C nano composite electrode material and preparation method thereof |
| CN113877528A (en) * | 2021-10-28 | 2022-01-04 | 云南中烟工业有限责任公司 | Porous composite material, preparation method and application thereof |
| CN114551828A (en) * | 2022-01-28 | 2022-05-27 | 同济大学 | Bi-MOF derived bismuth oxide-based negative electrode material and preparation and application thereof |
| CN114735690A (en) * | 2022-04-19 | 2022-07-12 | 湖南铂威新能源科技有限公司 | Preparation method of artificial graphite composite negative electrode material for lithium ion battery |
| CN114735690B (en) * | 2022-04-19 | 2022-10-28 | 湖南铂威新能源科技有限公司 | Preparation method of artificial graphite composite negative electrode material for lithium ion battery |
| CN115799518A (en) * | 2023-02-02 | 2023-03-14 | 暨南大学 | Bismuth/bismuth oxide nanodot/carbon sheet composite material, preparation method and application thereof |
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