CN106099076A - A kind of flower-shaped nitrogen-doped carbon cladding bismuth structural composite material and its preparation method and application - Google Patents
A kind of flower-shaped nitrogen-doped carbon cladding bismuth structural composite material and its preparation method and application Download PDFInfo
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- CN106099076A CN106099076A CN201610701833.XA CN201610701833A CN106099076A CN 106099076 A CN106099076 A CN 106099076A CN 201610701833 A CN201610701833 A CN 201610701833A CN 106099076 A CN106099076 A CN 106099076A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 flower-shaped nitrogen-doped carbon cladding bismuth structural composite material and its preparation method and application, which solving existing lithium ion battery negative material capacity and the highest technical problem of cyclical stability, it has following structure: the amorphous carbon of N doping is uniformly coated on flower-shaped bismuth nano grain surface；Described composite diameter 200nm～600nm, thickness 100～300nm, carbon-coating cladding thickness is 10～20nm.The present invention discloses its preparation method simultaneously.The present invention can be used for the preparation field of lithium ion battery negative material.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparation field, is specifically related to a kind of flower-shaped nitrogen-doped carbon cladding bismuth structure
Composite and its preparation method and application.
Background technology
Lithium ion battery is paid close attention to widely because having many advantages, and its application also expands constantly
Greatly, from mobile phone, digital camera, notebook computer electric automobile till now and military use product.
At present, commercial lithium ion battery negative material is mainly graphited material with carbon element.There is theoretical capacity in material with carbon element
Many deficiencies such as low, first charge-discharge efficiency is low, organic solvent embedding altogether, and start to restrict sending out of whole lithium ion battery
Exhibition.But being as the development of society, the requirement of capacity of lithium ion battery and charge-discharge velocity is constantly being carried by each field
Height because it directly affect the miniaturization of electronic product and the high-rate charge-discharge capability of some large-scale instrument stand-by power supplies and
The problems such as flying power, thus the development of high performance lithium ion battery for portable electric appts, electric automobile and other one
A little storage devices are particularly important.Research worker while as possible improving material with carbon element performance, also begin to develop new, can serve as
Lithium ion battery negative, material that performance is more superior.
In the last few years, lithium ion battery negative material had been carried out widely studied by researcher.At present, bismuth metal material
Research start to cause the attention of researcher.The mass theory capacity of bismuth is 386mA h/g, slightly above material with carbon element, but
It is that it has higher volume capacity 3765mAh/cm-3.Research method currently for bismuth material mainly has morphology control and carbon
Cladding, such as document (Su D, Dou S, Wang G.Bismuth:A new anode for the Na-ion battery.Nano
Energy, 2015,12:88-95.) nano composite material of bismuth and Graphene is prepared for sodium-ion battery negative pole,
Under the electric current density of 40mA/g, can keep higher reversible specific capacity, for 561mAh/g, but capacity and cyclical stability are also
Can there is further raising.
Summary of the invention
The present invention is contemplated to solve existing lithium ion battery negative material capacity and the highest technology of cyclical stability is asked
Topic, it is provided that a kind of flower-shaped nitrogen-doped carbon cladding bismuth structural composite material with outstanding multiplying power and cycle performance and preparation method thereof
And application.
To this end, the present invention provides a kind of flower-shaped nitrogen-doped carbon to be coated with bismuth structural composite material, it has following structure: compound
Material has following structure: the amorphous carbon of N doping is uniformly coated on flower-shaped bismuth nano grain surface；Described composite
Diameter 200nm～600nm, thickness 100～300nm, carbon-coating cladding thickness is 10～20nm.
Present invention simultaneously provides the preparation method of a kind of flower-shaped nitrogen-doped carbon cladding bismuth structural composite material, it includes as follows
Step: (1) claims the Na of 0.3～0.7 mass parts2CO3After being dissolved in the water of 50～90 mass parts, add 1.2～2 mass parts
Bismuth citrate stir, at 150～180 DEG C, carry out hydro-thermal reaction 20～30h, clean after being cooled to room temperature and dry
Presoma to bismuth；(2) will after in step (1), the aqueous solution of gained presoma mixes with buffer solution with salt acid for adjusting pH extremely
8.0～9.0, add 50～200 mass parts dopamine hydrochloride reactions, the response time is 8～56h, obtains poly-dopamine cladding
Presoma composite, filtration washing collecting reaction product；(3) the poly-dopamine obtained in step (2) is coated with presoma multiple
Condensation material in nitrogen atmosphere at 600～800 DEG C carburizing reagent 2～4h, i.e. can get flower-shaped nitrogen-doped carbon cladding bismuth structure
Composite.
Preferably, adding the buffer substance in described buffer solution is disodium hydrogen phosphate or trishydroxymethylaminomethane.
Present invention simultaneously provides flower-shaped nitrogen-doped carbon cladding bismuth structural composite material and prepare lithium ion battery negative material
In application.
The present invention, with the flower-shaped presoma of the bismuth of water heat transfer as template, with dopamine as carbon source, is existed by dopamine
Auto polymerization in buffer solution is uniformly coated on the surface of flower-shaped presoma, then high temperature cabonization, and the presoma of internal bismuth turns
Turn to bad student CO while bismuth oxide2Gas, causes generation hole between Bismuth oxide particles, and meanwhile bismuth oxide and carbon are at height
There is carbothermic reduction reaction under temperature, ultimately form flower-shaped nitrogen-doped carbon cladding bismuth structural composite material.In prepared composite,
Carbon-coating is coated with the electronic conductivity energy beneficially improving bismuth, can be effectively improved the high rate performance of this material；Bismuth active material it
Between hole, can volumetric expansion that effectively padded coaming produces during repeated charge, it is ensured that the Gao Xun of composite
Ring stability, and the transmission range of lithium ion can be shortened.
Flower-shaped nitrogen-doped carbon cladding bismuth structural composite material prepared by the present invention is used as lithium ion battery negative material can
To show outstanding chemical property.Carbon-coating is conducive to improving the electronic conductivity energy of bismuth, can be effectively improved this material
High rate performance；Space between bismuth active material in carbonization process, can effectively produce by padded coaming during repeated charge
Raw volumetric expansion, it is ensured that the high cyclical stability of composite, and the transmission range of lithium ion can be shortened.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of embodiment 1 product；
Fig. 2 is the XRD curve of embodiment 1 product；
Fig. 3 be have prepared by embodiment 1 flower-shaped nitrogen-doped carbon cladding bismuth structural composite material be lithium cell cathode material
High rate performance figure.
Detailed description of the invention
Elaborating embodiments of the invention below, the present embodiment is carried out under premised on technical solution of the present invention
Implement, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following enforcement
Example.
Embodiment 1
Claim 0.3g Na2CO3Add 1.2g bismuth citrate after being dissolved in 50mL water to stir, at 150 DEG C, carry out water
Thermal response 30h, cleans after being cooled to room temperature and dries the presoma obtaining bismuth.Again by the aqueous solution of presoma and trihydroxy methyl ammonia
With salt acid for adjusting pH to 8.0～9.0 after methylmethane mixing, adding the reaction of 50mg dopamine hydrochloride, the response time is 56h,
It is coated with presoma composite, filtration washing collecting reaction product to poly-dopamine.The poly-dopamine cladding presoma that will obtain
Composite in nitrogen atmosphere at 800 DEG C carburizing reagent 2h, i.e. can get flower-shaped nitrogen-doped carbon cladding bismuth structure composite material
Material.
The stereoscan photograph of product as it is shown in figure 1, the XRD curve of product as shown in Figure 2.Fig. 3 is that the multiplying power of material is filled
Discharge test figure.As can be seen from Figure 3 along with the increase of electric current density, its capacity suppression ratio is relatively slow, illustrates this
Material has preferable rate charge-discharge performance.And the circulation volume several times under each multiplying power keeps stable, when electric current is close
When degree returns low range, capacity can well recover, it was demonstrated that this material has good cyclical stability.
Embodiment 2
Claim 0.5g Na2CO3Add 1.6g bismuth citrate after being dissolved in 70mL water to stir, at 180 DEG C, carry out water
Thermal response 20h, cleans after being cooled to room temperature and dries the presoma obtaining bismuth.Again by the aqueous solution of presoma and trihydroxy methyl ammonia
With salt acid for adjusting pH to 8.0～9.0 after methylmethane mixing, adding the reaction of 125mg dopamine hydrochloride, the response time is 40h,
It is coated with presoma composite, filtration washing collecting reaction product to poly-dopamine.The poly-dopamine cladding presoma that will obtain
Composite in nitrogen atmosphere at 700 DEG C carburizing reagent 3h, i.e. can get flower-shaped nitrogen-doped carbon cladding bismuth structure composite material
Material.
Electro-chemical test part with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 3
Claim 0.7g Na2CO3Add 2g bismuth citrate after being dissolved in 90mL water to stir, at 170 DEG C, carry out hydro-thermal
Reaction 25h, cleans after being cooled to room temperature and dries the presoma obtaining bismuth.Again by the aqueous solution of presoma and trihydroxy methyl amino
With salt acid for adjusting pH to 8.0～9.0 after methane blended, adding the reaction of 200mg dopamine hydrochloride, the response time is 8h, obtains
Poly-dopamine cladding presoma composite, filtration washing collecting reaction product.The poly-dopamine obtained is coated with presoma multiple
Condensation material in nitrogen atmosphere at 600 DEG C carburizing reagent 4h, i.e. can get flower-shaped nitrogen-doped carbon cladding bismuth structural composite material.
Electro-chemical test part with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Claims (4)
1. a flower-shaped nitrogen-doped carbon cladding bismuth structural composite material, is characterized in that described composite has a following structure: nitrogen
The amorphous carbon of doping is uniformly coated on flower-shaped bismuth nano grain surface；Described composite diameter 200nm～600nm is thick
Degree 100～300nm, carbon-coating cladding thickness is 10～20nm.
2. a preparation method for flower-shaped nitrogen-doped carbon cladding bismuth structural composite material, is characterized in that comprising the steps:
(1) claim the Na of 0.3～0.7 mass parts2CO3After being dissolved in the water of 50～90 mass parts, add 1.2～2 mass parts
Bismuth citrate stirs, and carries out hydro-thermal reaction 20～30h at 150～180 DEG C, cleans and dries obtain after being cooled to room temperature
The presoma of bismuth；
(2) will after in step (1), the aqueous solution of gained presoma mixes with buffer solution with salt acid for adjusting pH to 8.0～9.0,
Adding 50～200 mass parts dopamine hydrochloride reactions, the response time is 8～56h, obtains poly-dopamine cladding presoma and is combined
Material, filtration washing collecting reaction product；
(3) by step (2) obtains poly-dopamine cladding presoma composite in nitrogen atmosphere at 600～800 DEG C
Carburizing reagent 2～4h, i.e. can get flower-shaped nitrogen-doped carbon cladding bismuth structural composite material.
The preparation method of flower-shaped nitrogen-doped carbon the most according to claim 2 cladding bismuth structural composite material, it is characterised in that
Adding the buffer substance in described buffer solution is disodium hydrogen phosphate or trishydroxymethylaminomethane.
Flower-shaped nitrogen-doped carbon the most as claimed in claim 1 cladding bismuth structural composite material is preparing lithium ion battery negative material
In material application.
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| CN107146915A (en) * | 2017-04-10 | 2017-09-08 | 中山大学 | A kind of preparation method of porous bismuth carbon composite |
| CN108281628A (en) * | 2018-01-05 | 2018-07-13 | 武汉理工大学 | Zinc cobalt sulfide/nitrogen-doped carbon composite material and preparation method and application |
| CN108689715A (en) * | 2018-04-18 | 2018-10-23 | 山东国瓷功能材料股份有限公司 | A kind of aluminium nitride powder and preparation method thereof |
| CN108832110A (en) * | 2018-06-26 | 2018-11-16 | 华南师范大学 | A kind of compound ZIF-8 negative electrode material of height ratio capacity bismuth nanoparticle and its preparation method and application |
| CN108899557A (en) * | 2018-06-07 | 2018-11-27 | 上海交通大学 | It is a kind of with through mesoporous N doping flower pattern carbon nanomaterial and preparation method |
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| CN112844351A (en) * | 2021-01-08 | 2021-05-28 | 杭州神起科技有限公司 | Flower-shaped Fe-doped TiO2Preparation method and application of porous carbon-loaded composite material |
| CN113363434A (en) * | 2021-05-12 | 2021-09-07 | 中国科学院过程工程研究所 | Multi-core multi-shell hollow material for encapsulating nano particles and preparation method and application thereof |
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| CN107146915A (en) * | 2017-04-10 | 2017-09-08 | 中山大学 | A kind of preparation method of porous bismuth carbon composite |
| CN108281628A (en) * | 2018-01-05 | 2018-07-13 | 武汉理工大学 | Zinc cobalt sulfide/nitrogen-doped carbon composite material and preparation method and application |
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| CN108689715A (en) * | 2018-04-18 | 2018-10-23 | 山东国瓷功能材料股份有限公司 | A kind of aluminium nitride powder and preparation method thereof |
| CN108899557A (en) * | 2018-06-07 | 2018-11-27 | 上海交通大学 | It is a kind of with through mesoporous N doping flower pattern carbon nanomaterial and preparation method |
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