CN110028051A - A method of sodium-ion battery is prepared with porous carbon negative pole material based on sucrose - Google Patents
A method of sodium-ion battery is prepared with porous carbon negative pole material based on sucrose Download PDFInfo
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- CN110028051A CN110028051A CN201910333125.9A CN201910333125A CN110028051A CN 110028051 A CN110028051 A CN 110028051A CN 201910333125 A CN201910333125 A CN 201910333125A CN 110028051 A CN110028051 A CN 110028051A
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- sodium
- sucrose
- negative pole
- ion battery
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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
A method of the porous carbon negative pole material of sodium-ion battery is prepared based on sucrose, will be dissolved in after sucrose and potassium hydroxide mixed grinding in ethylene glycol-water mixed solvent and obtain solution A；Solution A freeze-drying is placed in tube-type atmosphere furnace and carries out a step pyrolysis and the carbonized product that is carbonized to obtain；Carbonized product is subjected to filtering and washing to neutrality, the porous carbon negative pole material of sodium-ion battery is obtained after drying and grinding.Present invention process process is simple, and reaction temperature is low, the time is short, is not necessarily to subsequent processing, environmentally friendly；And prepared product morphology is evenly distributed, have porous structure, be conducive to the complete infiltration of electrolyte and electrode material come into full contact with electrolyte, the chemical property of material can be significantly improved, and have the advantages that it is at low cost, can be mass-produced.
Description
Technical field
The invention belongs to Carbon negative electrode material of sodium ion battery preparation technical fields, and in particular to a kind of base is prepared based on sucrose
The method of the porous carbon negative pole material of sodium-ion battery.
Technical background
Sodium-ion battery (SIBs) is considered as the large-scale fixed most promising secondary cell of energy storage, because sodium source takes it
Not to the utmost, nexhaustible, it is at low cost, it is environmental-friendly.However develop SIBs and be still within the starting stage, most of research all collects
In in the selection of current electrode material.In recent years, such as layered oxide and phosphatic positive material has had been extensively studied
Material, and sizable specific capacity, high rate performance and stable circulation are shown by optimization form and structure, some of which
Property.Especially Na3V2(PO4)3, show excellent comprehensive performance, it is considered to be potential business positive electrode.In contrast,
The research of negative electrode material is slow and insufficient, this has become the bottleneck of SIBs progress.It is well known that for the required negative of SIBs
Pole material should have the feature that high sodium ion memory capacity, good structural stability during sodium insertion and extraction are good
Electronic conductivity, resource abundance etc..So far, many materials, such as alloy, phosphorus, organic compound, titanium-based oxide and without fixed
Shape carbon [S.Komaba, W.Murata, T.Ishikawa, N.Yabuuchi, T.Ozeki, T.Nakayama, et al.,
Electrochemical Na insertion and solid electrolyte interphase for hard-carbon
electrodes and application to Na-ion batteries,Adv.Funct.Mater.21(20)(2011)
3859-3867.], studied as cathode, SIBs is studied.Alloy shows biggish reversible capacity, and
The expansion of the large volume of Sn (~520%) and Sb (~390%) limits their cyclical stability during Sodiation.Phosphorus and
Organic compound can also provide high reversible capacity, but due to its low electron conduction, their high rate performance cannot make us full
Meaning.Ti base oxide typically exhibits limited sodium storage capacity.In contrast, amorphous carbon is most promising.Stevens
With Dahn [D.Stevens, J.Dahn, High capacity anode materials for rechargeable
Sodium-ion batteries, J.Electrochem.Soc.147 (4) (2000) 1271-1273.] prove the reversible of hard carbon
Capacity can reach 300mAh g-1.The high electron conduction of carbon and good structural stability make it easier to be developed as have
The negative electrode material of high magnification capacity and cyclical stability.In addition, carbon resource is abundant, and it is at low cost, it is increased as SIB anode material
The attraction of material.However, the solid-state diffusion coefficient of sodium is very low in carbon, this leads to undesirable high rate performance.Adelhelm
[S.Wenzel,T.Hara,J.Janek,P.Adelhelm,Room-temperature sodium-ion batteries:
improving the rate capability of carbon anode materials by templating
Strategies, Energy Environ.Sci.4 (9) (2011) 3342-3345.] it has been proved that reducing the transport of sodium ion
Length is to mention powerful effective ways.Hereafter, hollow Nano carbon balls and carbon nano-fiber are considered as the anode material of SIB.
Due to its special structure, their two kinds of rate capabilities all improve a lot.However, the long circulating stability of these materials
(> 500) not yet realize report.It is well known that porous structure is also the effective ways for shortening sodium ion conveying length.In addition, more
Pore structure has proved to be the effective ways of volume change in the insertion of buffering lithium ion battery intermediate ion and extraction process
[F.Wang,R.Song,H.Song,X.Chen,J.Zhou,Z.Ma,et al.,Simple synthesis of novel
hierarchical porous carbon microspheres and their application to rechargeable
lithium-ion batteries,Carbon 81(2015)314–321.].So research porous structure is to SIBs carbon anode
The influence of material is meaningful.
Summary of the invention
The purpose of the present invention is to provide it is a kind of be easily achieved, low cost and high conduction performance based on sucrose prepare sodium from
The method of the porous carbon negative pole material of sub- battery, prepared porous carbon negative pole material can be effectively improved diffusion and the electricity of ion
Son transmission, improve the performance of battery, and have the advantages that it is at low cost, be easy to the factorial production.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) it takes 1g sucrose and 0.3~1g potassium hydroxide to be dissolved in ethylene glycol-aqueous solvent of 20~60ml and obtains solution A；
2) solution A is freeze-dried, obtains white precursor B；
3) by presoma be B be transferred in crucible, after put it into tube-type atmosphere furnace, with 2 under argon atmosphere
The rate of~10 DEG C/min heats up from room temperature to 600~900 DEG C of 1~3h of heat preservation, then with the rate of temperature fall of 10 DEG C/min
Room temperature, which is naturally cooled to, after being cooled to 300 DEG C obtains carbonized product；
4) by carbonized product respectively with dehydrated alcohol and deionized water filtering and washing up to being washed till neutrality, grinding is after drying
Obtain the porous carbon negative pole material of sodium-ion battery.
30~60min of sucrose and potassium hydroxide mixed grinding of the step 1).
Ethylene glycol-aqueous solvent of the step 1) is water: ethylene glycol is mixed by the volume ratio of 1~9:1.
Step 2) the freeze-drying temperature is -80~-20 DEG C DEG C, and sublimation drying is 12~36h.
The crucible of the step 3) is aluminum oxide crucible.
The argon gas flow velocity of the step 3) is 0.1~1.0sccm/min.
The step 4) is first used carbonized product washes of absolute alcohol 3 times, is then cleaned again with deionized water to neutrality.
The drying temperature of the step 4) is 80~120 DEG C, and the time is 8~12h.
The aperture of the porous carbon negative pole material of sodium-ion battery obtained by the step 4) is 400~800nm.
The beneficial effects of the present invention are embodied in:
1) present invention uses simple step solid-phase process preparation, and without adding other templates, pyrolysis and carbonization are anti-
It should disposably be completed in tube-type atmosphere furnace, be not necessarily to other post-processings, reduce production cost；
2) porous carbon negative pole material aperture made from the method is in 400-800nm range.It is formed between carbon material three-dimensional mutual
Join network structure, makes it have biggish specific surface area, can be come into full contact with electrode material, more attachment is provided for sodium ion
Site, to improve the efficiency of electrode reaction；
3) raw material of the present invention is chemical composition stability, cheap sucrose and potassium hydroxide, and we
The process flow of method is simple, is easy to the factorial production.
Detailed description of the invention
Fig. 1 is the scanning figure (SEM) of the porous carbon negative pole material of sodium-ion battery prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning figure (TEM) of the porous carbon negative pole material of sodium-ion battery prepared by the embodiment of the present invention 1；
Fig. 3 is the figure (XRD) of the porous carbon negative pole material of sodium-ion battery prepared by the embodiment of the present invention 1；
Specific embodiment
The present invention is further elaborated with reference to the accompanying drawings and embodiments, but the present invention is not limited to following implementation
Example.
Embodiment 1:
1) 1g sucrose and 0.3g potassium hydroxide mixed grinding 30min are taken, water: ethylene glycol is mixed into system by the volume ratio of 1:1
At ethylene glycol-aqueous solvent, then the mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 20ml and obtains solution A；
2) solution A is obtained into white precursor B in -80 DEG C of freeze-drying 12h；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
To be heated up from room temperature to 600 DEG C of heat preservation 3h, then under the argon atmosphere of 0.1sccm/min with the rate of 2 DEG C/min
It is cooled to the rate of temperature fall of 10 DEG C/min and naturally cools to room temperature after 300 DEG C and obtain carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 80 DEG C of dry 12h, which grind,.
Fig. 1 is the SEM photograph of porous carbon negative pole material manufactured in the present embodiment, in conjunction with Fig. 1 photo it is found that prepared carbon
Material has porous structure, while having laminated structure, is conducive to coming into full contact with and electrolyte for electrolyte and electrode material
Infiltration completely, improves the diffusion of ion and the transmission of electronics, can significantly improve the chemical property of material
Transmission electron microscope (TEM) figure of prepared porous carbon negative pole material as seen from Figure 2, it was demonstrated that made
Standby carbon material has apparent porous structure, consistent with the result observed in SEM, and porous and laminated structure is conducive to electronics
Transmission, reduce the diffusion path of Na+.
Show the sample of preparation in X-ray diffraction (XRD) figure of prepared porous carbon negative pole material as seen from Figure 3
Product show two wide characteristic peaks at 23.0 ° and 44.0 ° respectively, correspond respectively to (002) and (100) diffraction crystal face, are
The property of typical amorphous carbon.
Embodiment 2:
1) 1g sucrose and 0.5g potassium hydroxide mixed grinding 30min are taken, water: ethylene glycol is mixed into system by the volume ratio of 3:1
At ethylene glycol-aqueous solvent, then the mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 30ml and obtains solution A；
2) solution A is freeze-dried for 24 hours at -50 DEG C, obtains white precursor B；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
To be heated up from room temperature to 700 DEG C of heat preservation 2h, then under the argon atmosphere of 0.5sccm/min with the rate of 2 DEG C/min
It is cooled to the rate of temperature fall of 10 DEG C/min and naturally cools to room temperature after 300 DEG C and obtain carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 100 DEG C of dry 10h, which grind,.
Embodiment 3:
1) 1g sucrose and 0.7g potassium hydroxide mixed grinding 40min are taken, water: ethylene glycol is mixed into system by the volume ratio of 7:1
At ethylene glycol-aqueous solvent, then the mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 40ml and obtains solution A；
2) solution A is obtained into white precursor B in -30 DEG C of freeze-drying 30h；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
To be heated up from room temperature to 800 DEG C of heat preservation 1h, then under the argon atmosphere of 0.8sccm/min with the rate of 10 DEG C/min
It is cooled to the rate of temperature fall of 10 DEG C/min and naturally cools to room temperature after 300 DEG C and obtain carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 90 DEG C of dry 11h, which grind,.
Embodiment 4:
1) 1g sucrose and 0.9g potassium hydroxide mixed grinding 50min are taken, water: ethylene glycol is mixed into system by the volume ratio of 9:1
At ethylene glycol-aqueous solvent, then the mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 50ml and obtains solution A；
2) solution A is obtained into white precursor B in -40 DEG C of freeze-drying 27h；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
To be heated up from room temperature to 900 DEG C of heat preservation 1h, then under the argon atmosphere of 0.3sccm/min with the rate of 3 DEG C/min
It is cooled to the rate of temperature fall of 10 DEG C/min and naturally cools to room temperature after 300 DEG C and obtain carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 120 DEG C of dry 8h, which grind,.
Embodiment 5:
1) 1g sucrose and 1g potassium hydroxide mixed grinding 30min are taken, water: ethylene glycol is mixed by the volume ratio of 5:1
Then mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 60ml and obtains solution A by ethylene glycol-aqueous solvent；
2) solution A is obtained into white precursor B in -60 DEG C of freeze-drying 18h；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
Be to be heated up with the rate of 7 DEG C/min from room temperature to 900 DEG C of heat preservation 3h under the argon atmosphere of 1sccm/min, then with
The rate of temperature fall of 10 DEG C/min naturally cools to room temperature after being cooled to 300 DEG C and obtains carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 110 DEG C of dry 9h, which grind,.
Embodiment 6:
1) 1g sucrose and 0.3g potassium hydroxide mixed grinding 60min are taken, water: ethylene glycol is mixed into system by the volume ratio of 4:1
At ethylene glycol-aqueous solvent, then the mixture after grinding is dissolved in ethylene glycol-aqueous solvent of 50ml and obtains solution A；
2) solution A is obtained into white precursor B in -20 DEG C of freeze-drying 36h；
3) by presoma be B be transferred in aluminum oxide crucible, after put it into tube-type atmosphere furnace, in argon gas flow velocity
To be heated up from room temperature to 800 DEG C of heat preservation 1.5h, so under the argon atmosphere of 0.6sccm/min with the rate of 5 DEG C/min
It is cooled to afterwards with the rate of temperature fall of 10 DEG C/min and naturally cools to room temperature after 300 DEG C and obtain carbonized product；
4) carbonized product is first filtered into cleaning 3 times with dehydrated alcohol, is then filtered and is cleaned to neutrality with deionized water again, in
The porous carbon negative pole material of sodium-ion battery that it is 400~800nm up to aperture that 100 DEG C of dry 10h, which grind,.
Claims (9)
1. a kind of prepare the sodium-ion battery method of porous carbon negative pole material based on sucrose, which is characterized in that including following step
It is rapid:
1) it takes 1g sucrose and 0.3~1g potassium hydroxide to be dissolved in ethylene glycol-aqueous solvent of 20~60ml and obtains solution A；
2) solution A is freeze-dried, obtains white precursor B；
3) by presoma be B be transferred in crucible, after put it into tube-type atmosphere furnace, with 2~10 under argon atmosphere
DEG C/rate of min heats up from room temperature to 600~900 DEG C of 1~3h of heat preservation, then cooled down with the rate of temperature fall of 10 DEG C/min
Room temperature, which is naturally cooled to, after to 300 DEG C obtains carbonized product；
4) carbonized product is ground after dry respectively with dehydrated alcohol and deionized water filtering and washing up to being washed till neutrality up to sodium
The porous carbon negative pole material of ion battery.
2. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, 30~60min of sucrose and potassium hydroxide mixed grinding of the step 1).
3. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, ethylene glycol-aqueous solvent of the step 1) is water: ethylene glycol is mixed by the volume ratio of 1~9:1.
4. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, step 2) the freeze-drying temperature is -80~-20 DEG C, and sublimation drying is 12~36h.
5. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, the crucible of the step 3) is aluminum oxide crucible.
6. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, the argon gas flow velocity of the step 3) is 0.1~1.0sccm/min.
7. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, the step 4) is first used carbonized product washes of absolute alcohol 3 times, is then cleaned again with deionized water to neutrality.
8. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, the drying temperature of the step 4) is 80~120 DEG C, and the time is 8~12h.
9. according to claim 1 prepare the sodium-ion battery method of porous carbon negative pole material, feature based on sucrose
It is, the aperture of the porous carbon negative pole material of sodium-ion battery obtained by the step 4) is 400~800nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110255528A (en) * | 2019-07-25 | 2019-09-20 | 燕山大学 | The method and its application of porous carbon materials are prepared using dyestuff waste liquid |
| CN114634171A (en) * | 2022-02-28 | 2022-06-17 | 东南大学 | Preparation method and application of biomass-based cage-shaped porous carbon based on ice template regulation and control |
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| CN114634171A (en) * | 2022-02-28 | 2022-06-17 | 东南大学 | Preparation method and application of biomass-based cage-shaped porous carbon based on ice template regulation and control |
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Application publication date: 20190719 |