CN106374092A - Preparation method of foamed nitrogen-doped carbon composite material and application thereof in sodium ion battery - Google Patents
Preparation method of foamed nitrogen-doped carbon composite material and application thereof in sodium ion battery Download PDFInfo
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- CN106374092A CN106374092A CN201610965399.6A CN201610965399A CN106374092A CN 106374092 A CN106374092 A CN 106374092A CN 201610965399 A CN201610965399 A CN 201610965399A CN 106374092 A CN106374092 A CN 106374092A
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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
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/58—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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- 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 invention discloses a preparation method of a foamed nitrogen-doped carbon composite material and an application thereof in a sodium ion battery. The preparation method comprises the following steps: ball milling and mixing gelatin and zinc chloride to obtain a precursor; performing heat treatment on the precursor, and washing the precursor to obtain the foamed nitrogen-doped carbon composite material. The method has the advantages of being easy to obtain raw materials, simple in process and good in repeatability; and the prepared foamed nitrogen-doped carbon composite material has the advantages of uniform distribution of nitrogen atoms, rich pores, large specific surface area, rich reaction active sites, moderate interlayer distance, good electrical conductivity and the like, and the foamed nitrogen-doped carbon composite material represents good battery performance when being applied to the sodium ion battery.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen-doped carbon composite, particularly to a kind of, there is pumiceous texture
The preparation method and applications of doping carbon composite, belong to sodium-ion battery field.
Background technology
Sodium-ion battery relies on sodium rich reserves, can use for reference the advantages such as existing battery achievement, become secondary cell of new generation
The study hotspot of system.But the problems such as sodium-ion battery cathode voltage is high big with sodium ion radius, opens to efficient sodium-ion battery
Send out and propose a lot of difficult problems.Electrode material decides the important parameter such as capacity, running voltage and cycle life of battery.Although
Response mechanism in sodium-ion battery is similar to lithium ion battery, however, sodium ion is bigger than lithium ion, leads to sodium ion in phase
With the often all relative difficulty of the embedded and diffusion in structural material, it is simultaneously embedded in abjection and more significant structural volume can be brought to change
Become, when causing common batteries material as sodium ion battery electrode material, material efflorescence easily occurs and the phenomenon such as caves in, electrode material
The specific capacity of material, dynamic performance and cycle performance etc. are all correspondingly deteriorated, and seriously constrain the exploitation of sodium-ion battery and answer
With.The material of storage sodium excellent performance therefore must be developed for sodium ion feature.
In existing anode material of lithium-ion battery, material with carbon element is that to study be also the more negative material of research earliest.Hard carbon
Material relies on its specific capacity high, good rate capability, the advantages of having extended cycle life, becomes the more material with carbon element species of research.For
Hard carbon storage sodium capacity is mainly derived from avtive spot, low graphitization crystallite area and micropore area etc., and routine prepares the side of hard carbon material
How method, add activation two-step thermal processing method using direct carbonization, preparation process is complicated, and energy utilization rate is low.Meanwhile common
Hard carbon material porosity is low, and specific surface area is little, and sterically hindered big, storage sodium performance is unsatisfactory.Improve hard carbon material porosity many
Using soft or hard template, and using the extremely strong Fluohydric acid. of corrosivity or hot concentrated caustic solution, subsequent treatment stream more than follow-up removing template
Journey is long, increases immense pressure to environment simultaneously.Therefore it is badly in need of developing a kind of preparation process few, the simple porous hard of preparation method
The preparation method of material with carbon element.
Content of the invention
The problem existing for existing anode material of lithium-ion battery, it is an object of the present invention to provide a kind of duct
The system with porous foam shape nitrogen-doped carbon composite that abundant, porosity is high, specific surface area is big, reactivity site is enriched
Preparation Method, the method raw material is easy to get, with low cost, environmental protection, degree of controllability is high, reproducible, be easily achieved industrialized production.
Another object of the present invention is to be to be applied to prepare sodium ion by porous foam shape nitrogen-doped carbon composite
Battery, the sodium-ion battery high rate performance of preparation is excellent, good cycle.
In order to realize above-mentioned technical purpose, the invention provides a kind of preparation side of cystose nitrogen-doped carbon composite
Method, the method is by gelatin and zinc chloride ball milling mixing, obtains presoma；Described presoma is carried out at heat at 200～1000 DEG C
After reason, washing, obtain final product.
Technical scheme, it is critical only that the method combining molten-salt growth method pore-creating using ball milling mixing prepares cystose nitrogen
Doping carbon composite.Can be by gelatin and zinc chloride with nano molecular rank mix homogeneously, for follow-up equal by ball milling mixing
Even pore-creating provides favourable precondition.On this basis, using zinc chloride fusing point in more than 200 degrees Celsius, boiling point 800
The feature of degrees centigrade, strictly controls heat treatment temperature, makes zinc chloride be in molten state, molten state zinc chloride has very high
Reactivity, chloride ion and zinc ion have catalysis pore-creating effect, molten state zinc chloride pair simultaneously to the carbonisation of material with carbon element
Material with carbon element has souring, promotes the formation of porous foam structure nitrogen-doped carbon composite.With zinc chloride as pore creating material, mould
Plate agent and catalyst carry out, to precursor, the multi-step heat treatment that carbonization pore-creating can avoid Conventional porous hard carbon material by molten-salt growth method
Step and costly template handling process.
Preferably scheme, described zinc chloride is 0.1～500:1 with the mass ratio of described gelatin；It is more preferably (1～100):
1；Most preferably (1～50 :): 1.Technical scheme is passed through to adjust the ratio of zinc chloride and gelatin, you can regulation and control porous
The pore volume of cystose nitrogen-doped carbon composite and specific surface area, control ability is strong.
Preferably scheme, the condition of described ball milling mixing: revolution is 10～1000r/min, the time is 0.1～40h；More excellent
The ball milling mixing condition of choosing: rotating speed is 100～600r/min, the time is 1～10h；Most preferably ball milling mixing condition: rotating speed is
200～400r/min, the time is 2～8h.By sufficient ball milling, so that zinc chloride and gelatin material is sufficiently mixed, be conducive to carrying
The high porous foam shape nitrogen-doped carbon material road degree of cross linking.
Preferably scheme, the time of described heat treatment is 0.1～10h；It is more preferably 1～8h, more preferably 3～5h.
More preferably scheme, the pore volume of described cystose nitrogen-doped carbon composite is 0.1～4cm3/ g, more preferably for
0.5～1.5cm3/g；Specific surface area is 200～3500m2/ g, more preferably for 300～3000m2/g.Technical scheme
In, the porous foam shape nitrogen-doped carbon composite duct obtaining is enriched, porosity is high, the duct degree of cross linking is high, specific surface area is big
And reactivity site is abundant, and specific surface area and pore volume etc. easily regulate and control.
Preferably scheme, in described cystose nitrogen-doped carbon composite, nitrogen atom doping amount is 0.1wt%～5wt%.
Preferably scheme, heat treatment temperature is 300～800 DEG C；More preferably 600～700 DEG C.
In technical scheme, presoma, after heat treatment, directly adopts washing, you can to leach zinc chloride
Reclaim, be recycled zinc chloride through pervaporation recrystallization, gained reclaims zinc chloride and can be recycled, stock utilization is high, process
Technique and its simple, environmental effect is good.
Present invention also offers a kind of preparation method of cystose nitrogen-doped carbon composite, by described cystose N doping
Carbon negative pole material is applied to prepare sodium-ion battery as negative material.
The porous foam shape nitrogen-doped carbon composite that technical scheme obtains is good with electrolyte wettability, duct
Abundant, reactivity site is enriched, and storage sodium behavior dynamicss condition is good, has good sodium ion and embeds and abjection ability, hands over
The duct of Lian Dugao is conducive to electrolyte to transmit kinetics with sodium ion, and loose structure has solely for alleviating volumetric expansion contraction
Special advantage, can significantly improve the forthright again of battery and cycle performance for sodium-ion battery.
The biomass gelatin being widely present using nature in technical scheme is as nitrogen source and carbon source, and adopts
Zinc chloride can be with recycling, raw material availability is high, and emission index is low, and environmental effect is good.
With respect to prior art, the Advantageous Effects that technical scheme is brought:
1st, technical scheme adopts biomass gelatin as nitrogen source and carbon source, using zinc chloride as template,
Pore creating material and catalyst, are thermally treated resulting in cystose nitrogen-doped carbon composite by a step molten-salt growth method, are removed using simple washing
Remove zinc chloride in material with carbon element, heat treatment step is short and simply easily realizes；Gained zinc chloride recovered liquid can obtain zinc chloride further,
Realization recycles, and raw material availability is high.In sum, the raw material that technical solution of the present invention adopts is cheap and easy to get, process is simple,
Green production capable of circulation, favorable reproducibility, environmental friendliness, environmental protection, suitable industrialized production.
2nd, the gelatin that technical scheme adopts, using self-contained nitrogen and carbon as nitrogen source and carbon source, realizes nitrogen former
Sub- Uniform Doped, obtains porous foam shape nitrogen-doped carbon composite using molten-salt growth method, and it has duct and enriches, and porosity is high,
Specific surface area is big, the advantages of reactivity site is enriched.
3rd, technical scheme overcomes reactivity site shortage and the duct obturation of hard carbon material generally existing
Problem, the N doping porous carbon foam material of molten-salt growth method preparation, duct is enriched, and porosity is high, and specific surface area is big, reactivity
Site is enriched, and provides abundant storage sodium site and space, can promote the transmission of electrolyte and sodium ion, alleviates sodium ion embedded de-
Powder phenomenon-tion is shunk in the volumetric expansion bringing during going out.
4th, the porous foam shape nitrogen-doped carbon composite of the present invention is used for sodium-ion battery, can obtain specific capacity high, again
Rate performance is good, have extended cycle life, the sodium-ion battery of long circulating stable performance.
Brief description
[Fig. 1] is the scanning electron microscope (SEM) photograph (sem) of the porous foam shape nitrogen-doped carbon composite that embodiment 1 is obtained.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but these embodiments must not be construed to this
The restriction of invention protection domain.
Embodiment 1
2g gelatin and 10g zinc chloride are placed in ball grinder, control ball milling revolution 200r/min, Ball-milling Time 2h, gained
Gelatin zinc chloride mixture, is placed in quartz tube furnace, 600 DEG C of heat treatment temperature, heat treatment time 2h, and gained material with carbon element passes through
Massive laundering, obtains porous foam shape nitrogen-doped carbon composite, and pore volume is 0.5cm3/ g, specific surface area is 350m2/ g, nitrogen is former
Sub- content is 2.4wt%, and filtrate, through pervaporation, is recycled zinc chloride.
It is working electrode using porous foam shape nitrogen-doped carbon composite manufactured in the present embodiment, sodium is to electrode, group
Dress up button cell, under the electric current density of 50ma/g, test loop performance；In the different electricity such as 1000ma/g, 2000ma/g
The high rate performance of battery is tested under current density.Test result shows, the sode cell negative pole of this example preparation has good electrochemistry
Performance: under the current density of 50ma/g, after circulation 100 circle, remain to keep the specific capacity of 301ma/g；In 1000ma/g and
Under the power-discharging density of 2000ma/g, remain to keep the specific capacity of 152mah/g and 110mah/g respectively.
Embodiment 2
2g gelatin and 20g zinc chloride are placed in ball grinder, control ball milling revolution 300r/min, Ball-milling Time 2h, gained
Gelatin zinc chloride mixture, is placed in quartz tube furnace, 700 DEG C of heat treatment temperature, heat treatment time 3h, and gained material with carbon element passes through
Massive laundering, obtains porous foam shape nitrogen-doped carbon composite, and pore volume is 1.2cm3/ g, specific surface area is 2400m2/ g, nitrogen is former
Sub- content is 3.2wt%, and filtrate, through pervaporation, is recycled zinc chloride.
It is working electrode using porous foam shape nitrogen-doped carbon composite manufactured in the present embodiment, sodium is to electrode, group
Dress up button cell, under the electric current density of 50ma/g, test loop performance；In the different electricity such as 1000ma/g, 2000ma/g
The high rate performance of battery is tested under current density.Test result shows, the sode cell negative pole of this example preparation has good electrochemistry
Performance: under the current density of 50ma/g, after circulation 100 circle, remain to keep the specific capacity of 311ma/g；In 1000ma/g and
Under the power-discharging density of 2000ma/g, remain to keep the specific capacity of 168mah/g and 121mah/g respectively.
Embodiment 3
2g gelatin and 100g zinc chloride are placed in ball grinder, control ball milling revolution 400r/min, Ball-milling Time 8h, gained
Gelatin zinc chloride mixture, is placed in quartz tube furnace, 700 DEG C of heat treatment temperature, heat treatment time 5h, and gained material with carbon element passes through
Massive laundering, obtains porous foam shape nitrogen-doped carbon composite, and pore volume is 0.6cm3/ g, specific surface area is 2980m2/ g, nitrogen is former
Sub- content is 4.7wt%, and filtrate, through pervaporation, is recycled zinc chloride.
It is working electrode using porous foam shape nitrogen-doped carbon composite manufactured in the present embodiment, sodium is to electrode, group
Dress up button cell, under the electric current density of 50ma/g, test loop performance；In the different electricity such as 1000ma/g, 2000ma/g
The high rate performance of battery is tested under current density.Test result shows, the sode cell negative pole of this example preparation has good electrochemistry
Performance: under the current density of 50ma/g, after circulation 100 circle, remain to keep the specific capacity of 334ma/g；In 1000ma/g and
Under the power-discharging density of 2000ma/g, remain to keep the specific capacity of 167mah/g and 133mah/g respectively.
Comparative example 1
2g gelatin is placed in quartz tube furnace, 700 DEG C of heat treatment temperature, heat treatment time 5h, gained material with carbon element passes through
Massive laundering, obtains nitrogen-doped carbon material, and pore volume is 0.1cm3/ g, specific surface area is 120m2/ g, nitrogen atom content is
2.3wt%.
Nitrogen-doped porous carbon material using comparative example 1 preparation is working electrode, and sodium is to electrode, is assembled into button
Battery, under the electric current density of 50ma/g, test loop performance；Under the different electric current density such as 1000ma/g, 2000ma/g
The high rate performance of test battery.Test result shows, the sode cell negative pole of preparation has poor chemical property: in 50ma/g
Current density under, circulation 100 circle after, be only capable of keep 181ma/g specific capacity；Power-discharging density in 1000ma/g and 2000ma/g
Under, it is only capable of keeping the specific capacity of 122mah/g and 90mah/g respectively.
Claims (7)
1. a kind of preparation method of cystose nitrogen-doped carbon composite it is characterised in that: by gelatin and zinc chloride ball milling mixing,
Obtain presoma；After described presoma carries out heat treatment at 200～1000 DEG C, washing, obtain final product.
2. cystose nitrogen-doped carbon composite according to claim 1 preparation method it is characterised in that: described chlorination
Zinc is (0.1～500) with the mass ratio of described gelatin: 1.
3. cystose nitrogen-doped carbon composite according to claim 1 preparation method it is characterised in that: described ball milling
The condition of mixing: revolution is 10～1000r/min, the time is 0.1～40h.
4. cystose nitrogen-doped carbon composite according to claim 1 preparation method it is characterised in that: described heat at
The time of reason is 0.1～10h.
5. the preparation method of the cystose nitrogen-doped carbon composite according to any one of Claims 1 to 4, its feature exists
In: the pore volume of described cystose nitrogen-doped carbon composite is 0.1～4cm3/ g, specific surface area is 200～3500m2/g.
6. cystose nitrogen-doped carbon composite according to claim 5 preparation method it is characterised in that: described foam
In shape nitrogen-doped carbon composite, nitrogen atom doping amount is 0.1wt%～5wt%.
7. the application of the cystose nitrogen-doped carbon composite of preparation method preparation described in any one of claim 1～6, it is special
Levy and be: be applied to prepare sodium-ion battery as negative material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106935861A (en) * | 2017-03-23 | 2017-07-07 | 中南大学 | A kind of sodium-ion battery carbon negative pole material and preparation method thereof |
| CN107331867A (en) * | 2017-07-05 | 2017-11-07 | 中国矿业大学 | Nitrogen-doped porous carbon material preparation method as sodium-ion battery negative pole |
| CN115332538A (en) * | 2022-10-12 | 2022-11-11 | 宁德新能源科技有限公司 | Hard carbon material, preparation method thereof, electrochemical device and electronic device |
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| CN105932234A (en) * | 2016-05-05 | 2016-09-07 | 华东师范大学 | Doped porous carbon spheres used for negative electrode material of sodium ion battery and preparation method for doped porous carbon spheres |
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| CN106935861A (en) * | 2017-03-23 | 2017-07-07 | 中南大学 | A kind of sodium-ion battery carbon negative pole material and preparation method thereof |
| CN106935861B (en) * | 2017-03-23 | 2019-09-27 | 中南大学 | A kind of sodium-ion battery carbon negative pole material and preparation method thereof |
| CN107331867A (en) * | 2017-07-05 | 2017-11-07 | 中国矿业大学 | Nitrogen-doped porous carbon material preparation method as sodium-ion battery negative pole |
| CN115332538A (en) * | 2022-10-12 | 2022-11-11 | 宁德新能源科技有限公司 | Hard carbon material, preparation method thereof, electrochemical device and electronic device |
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