CN106654268A - Method for preparing porous carbon material for lithium/sodium-ion battery - Google Patents
Method for preparing porous carbon material for lithium/sodium-ion battery Download PDFInfo
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- CN106654268A CN106654268A CN201611125708.5A CN201611125708A CN106654268A CN 106654268 A CN106654268 A CN 106654268A CN 201611125708 A CN201611125708 A CN 201611125708A CN 106654268 A CN106654268 A CN 106654268A
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- ion battery
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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
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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
- 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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- 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
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to the field of electrochemistry, and discloses a method for preparing a porous carbon material as an anode material of a lithium/sodium-ion battery. The preparation method comprises the following steps: calcinating a series of sodium salts such as sodium alginate, sodium ascorbate and sodium gluconate in a tube furnace protected by an inert atmosphere, and performing purification to obtain a series of porous carbon materials by using a hydrochloric acid solution. The porous carbon material is large in specific surface area, uniform in aperture distribution, large in carbon layer spacing and extensive in use, and particularly has high cycle stability and relatively high specific capacity when being used as the anode material of the lithium/sodium-ion battery.
Description
Technical field
The invention belongs to electrochemistry and material chemistry technical field, more particularly to a kind of preparation of porous carbon materials, specifically
For a kind of preparation method of the negative material of lithium/sodium-ion battery.
Background technology
The use of traditional fossil fuel causes the environmental problems such as greenhouse effects, acid rain, air pollution increasingly to sharpen.With can
The development of the renewable sources of energy, too can energy, hydroelectric generation, tidal power generation and underground heat etc. provide endlessly energy.In order to tackle
The development of different energy storage demand and power supply chemistry, lithium ion battery with its low cost, have extended cycle life, self discharge is little and ring
The features such as border is friendly, occupies rapidly the market of the portable electronic devices such as mobile phone, notebook computer.But with electric automobile
With the earth's crust amount of storage of the further increase of the scale energy storage device market demand, and metal lithium resource only have 20 ppm and
Distribution on global is uneven, and lithium ion battery cost will certainly be caused to raise.
Metal sodium element, is second most light and minimum alkali metal, with the physico-chemical property similar with lithium.Together
When, metal sodium element earth's crust content is evenly distributed more than 1%, wide material sources, can effective reduces cost.With to sodium
The further optimizing research of electrode material, electrolyte, the barrier film of ion battery etc., especially in following extensive energy storage facility
On, it is potential to substitute lithium ion battery and be widely used.
Alloy material metallic tin, antimony, metal oxide and carbon-based material etc. may serve to as lithium ion and sodium from
The negative material of sub- battery.Adopting cheap graphite-like material with carbon element, reason the negative material of commercial Li-ion batteries at present more
It is 372 mAh/g by capacity.But for sodium-ion battery, due to Na+Radius（1.02 Å）Compare Li+（ 0.76 Å）Want big by one
A bit, away from only 0.37 nm, sodium ion is difficult to be embedded into graphite layers graphite layers, only forms NaC64High-order compound, quality
Specific capacity only has 35 mAh/g.Because the interlamellar spacing of the non-graphite material with carbon element such as soft carbon, hard carbon is larger, the degree of disorder is higher, very
Be conducive to the deintercalation of sodium ion, be the extensive class material of research.The carbon-based hollow nanospheres that for example prepared by hydro-thermal method, high warm
Solution carbon, template material with carbon element that template is prepared etc., all in cycle performance, the aspect such as specific capacity serves certain improvement
Effect.But it is complicated that these preparation methods are related to the experimental procedures such as template, hydro-thermal, relatively costly, is unfavorable for large-scale production.
And other alloy type negative materials are very big in sodium ion deintercalation process Volumetric expansion, it is unfavorable for cyclical stability.Therefore,
A kind of material with carbon element being readily synthesized of searching is needed badly as lithium ion and the negative material of sodium-ion battery.
The content of the invention
For overcome lithium/anode material of lithium-ion battery cycle performance and high rate performance difference and cyclical stability difference ask
Topic, the invention provides high porous carbon materials of a kind of good cycling stability, theoretical specific capacity and preparation method thereof, the preparation side
Method is simple and easy to do, low cost, pollution-free.
The technical scheme is that：A kind of preparation method of the porous carbon materials for lithium/sodium-ion battery, including such as
Lower step：
Step one：Raw material is put into porcelain boat, porcelain boat is put into tube furnace, protective atmosphere is passed through in tube furnace, heat up speed
Rate is 1-10 DEG C/min, and calcining heat is 400-1300 DEG C, and calcination time is 2-10h, obtains intermediate product；The raw material includes
Sodium alginate or sodium isoascorbate or sodium gluconate or sodium glutamate；
Step 2：The intermediate product that step one is obtained is immersed in post-treatment solution, deionized water and ethanol are molten after stirring
Liquid is washed respectively, the product after washing is put in vacuum drying chamber is dried afterwards, obtains porous carbon materials；After described
Processing solution is using hydrochloric acid or nitric acid or sulfuric acid or acetic acid or oxalic acid.
Protective atmosphere in the step one includes one or any two in nitrogen, argon gas, helium, argon hydrogen, neon
Kind either any three kinds either any four or any five kinds of mixed gas.
Post-treatment solution mass fraction in the step 2 is between 1-100%.
Mixing time in the step 2 is 1-48h, and baking temperature is 40-90 DEG C, drying time 12-48 h.
Compared with existing invention, the present invention can produce following beneficial effect：
The present invention adopts wide material sources, using the raw material such as sodium alginate that can be easily obtained, sodium isoascorbate, sodium gluconate
Deng, low cost and nontoxic pollution-free.Preparation technology is very simple, is conducive to large-scale production.The porous carbon for finally obtaining
Material has nano-grade size, and specific surface area is big（Specific surface area can be controlled in 33-1300 m according to the difference of calcining heat2/g
In the range of）, cavernous structure is evenly distributed, and micro- sodium size can shorten the transmission path of lithium ion/sodium ion, and specific surface area is big
Contact of the electrolyte with electrode material, loose structure is conducive to be conducive to increasing storage lithium/storage sodium avtive spot.According to present invention system
Standby porous carbon materials, are assembled into lithium ion and sodium-ion battery, and cyclical stability is good, has extended cycle life, and circulates specific capacity
Height, high rate performance is good.Therefore porous carbon materials in the present invention and preparation method thereof, are the further of lithium/sodium-ion battery
Using there is provided possible.
Description of the drawings
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing the present invention is made into
The detailed description of one step.
Accompanying drawing 1 is the transmission electron microscope photo of the porous carbon materials prepared in the embodiment of the present invention 1.
Accompanying drawing 2 is the porous carbon materials prepared in the embodiment of the present invention 2 following of being assembled into after lithium ion battery that test obtains
Ring performance map.
Accompanying drawing 3 is the transmission electron microscope photo of the porous carbon materials prepared in the embodiment of the present invention 3.
Specific embodiment
A kind of preparation method of the porous carbon materials for lithium/sodium-ion battery, comprises the steps：
Step one：Raw material is put into porcelain boat, porcelain boat is put into tube furnace, protective atmosphere is passed through in tube furnace, heat up speed
Rate is 1-10 DEG C/min（May be selected 1 DEG C/min, 4 DEG C/min, 6 DEG C/min, 8 DEG C/min, 10 DEG C/min）, calcining heat is
400-1300℃（400℃、600℃、800℃、1000℃、1200℃、1300℃）, calcination time is 2-10h（Optional 2h,
4h、6h、8h、10h）, obtain intermediate product；The raw material includes sodium alginate or sodium isoascorbate or sodium gluconate or paddy
Propylhomoserin sodium；
Step 2：The intermediate product that step one is obtained is immersed in post-treatment solution, deionized water and ethanol are molten after stirring
Liquid is washed respectively, the product after washing is put in vacuum drying chamber is dried afterwards, obtains porous carbon materials；After described
Processing solution is using hydrochloric acid or nitric acid or sulfuric acid or acetic acid or oxalic acid.
Protective atmosphere in the step one includes one or any two in nitrogen, argon gas, helium, argon hydrogen, neon
Kind either any three kinds either any four or any five kinds of mixed gas.
Post-treatment solution mass fraction in the step 2 is in 1-100%（May be selected 1%, 20%, 40%, 60%, 80%,
100%）Between.
Mixing time in the step 2 is 1-48h（Optional 1h, 10h, 20h, 30h, 48h）, baking temperature is 40-
90℃（May be selected 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C）, drying time 12-48 h（Optional 12h, 20 h, 26
h、32 h、40 h、48 h）.
Below with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail：It should be appreciated that preferred embodiment
Only for the explanation present invention, rather than in order to limit the scope of the invention.
Embodiment 1
Raw material sodium alginate is put into porcelain boat, in tube furnace argon atmosphere is passed through, with the heating rate of 5 DEG C/min,
800 degree are risen to from room temperature, after constant temperature is kept for 2 hours, room temperature is naturally cooled to, intermediate product is prepared.
Intermediate product is put into 250 ml dilute hydrochloric acid solutions, hydrochloric acid solution mass fraction is 17%, stirs 12 h, then
Product is carried out into suction filtration, is washed respectively 3 times with distilled water and ethanol, vacuum drying chamber is vacuumized, 60 degree are dried 12h, obtain
Final product.
The product specific surface area that specific-surface area detection instrument test is obtained is adopted for 510 m2/ g, pore-size distribution is 2-20 nm.
The transmission electron microscope photo of the porous carbon materials is accompanying drawing 1.
Using the porous carbon materials in the present embodiment as negative material, lithium ion battery is assembled.Electrolyte is dense using 1 mole
The LiPF of degree6It is dissolved in volume ratio 1：1：The dimethyl carbonate of 1 mixing（DMC）, ethylene carbonate（EC）And methyl ethyl carbonate
（DMC）In the mixed solvent of composition.Barrier film selects Celgard 2300, lithium paper tinsel to be assembled into as to electrode and reference electrode
CR2032 button cells are tested.First by products therefrom porous carbon materials and conductive agent acetylene black, binding agent PVDF and molten
Agent NMP is according to 8：1：1 mass ratio mixing, grinds uniformly slurry.Then with scraper by slurry even application in Copper Foil
On, applied thickness is controlled at 200 μm, is placed in vacuum drying chamber 60 degree and is dried 12h, with roll squeezer to roller after, be cut into directly
The mm disks of footpath 12.Button cell is assembled into the glove box full of argon atmosphere, performance and forthright again is circulated
A series of electrochemical property tests such as energy, charge and discharge platform.
When carrying out sodium-ion battery assembling, NaClO of the electrolyte from 1 molar concentration4It is dissolved in volume ratio 1：1 carbonic acid
In the mixed solvent of methyl esters and diethyl carbonate, or the NaClO of 1 molar concentration4In being dissolved in propene carbonate, while addition
Appropriate fluorinated ethylene carbonate is used as electrolysis additive.Barrier film selects Whatman GF/F, and sodium piece is used as to electrode and ginseng
Compare electrode.Remaining operation is consistent with above-mentioned assembling lithium ion battery.
Embodiment 2
Raw material sodium ascorbate is put into magnetic boat, argon gas is passed through in tube furnace as protective atmosphere, with the intensification speed of 5 DEG C/min
Rate, from room temperature 500 degree are risen to, and after constant temperature is kept for 2 hours, naturally cool to room temperature, prepare intermediate product.
Intermediate product is put into 250 ml dilute hydrochloric acid solutions, hydrochloric acid solution mass fraction is 17%, stirs 12 h, then
Product is carried out into suction filtration, is washed respectively 3 times with distilled water and ethanol, vacuum drying chamber is vacuumized, 60 degree are dried 12h, obtain
Final product.
The porous carbon materials specific surface area for preparing is 515 m2/ g, pore-size distribution is 2-20 nm.
For the porous carbon materials obtained in this, the assembling of lithium ion and sodium-ion battery, the same embodiment of step are carried out
1.Sodium-ion battery cycle performance figure of the porous carbon materials prepared in the present embodiment under the current density of 100 mA/g is attached
Fig. 2.
Embodiment 3
Raw materials of glucose acid sodium is placed into magnetic boat, in the tube furnace of argon atmosphere is passed through, 10 DEG C of heating rate/
Min, from room temperature 600 degree are risen to, and constant temperature is kept for 2 hours, then naturally cools to room temperature, prepares intermediate product.
Intermediate product is put into 100 ml dilute hydrochloric acid solutions, hydrochloric acid solution mass fraction is 17%, 12h is stirred, to product
Suction filtration process is carried out, is washed 3 times with distilled water and ethanol respectively, in vacuum drying chamber, 60 degree are dried 12h, are finally produced
Thing.
The porous carbon materials specific surface area for preparing is 605 m2/g.The porous carbon materials of preparation is saturating in the present embodiment
Electromicroscopic photograph is penetrated for accompanying drawing 3.
For the porous carbon materials obtained in this, the assembling of lithium ion and sodium-ion battery, the same embodiment of step are carried out
1。
Embodiment 4
Raw material sodium glutamate is put into magnetic boat, in the tube furnace of argon atmosphere, heating rate is 5 DEG C/min, from
Room temperature rises to 600 degree, and constant temperature is kept for 2 hours, then naturally cools to room temperature, prepares intermediate product.
Intermediate product is put into 100ml dilute hydrochloric acid solutions, hydrochloric acid solution mass fraction is 17%, 12h is stirred, to product
Suction filtration process is carried out, is washed 3 times with distilled water and ethanol respectively, in vacuum drying chamber, 60 degree are dried 12h, are finally produced
Thing.
The porous carbon materials specific surface area for preparing is 505 m2/g。
For the porous carbon materials obtained in this, the assembling of lithium ion and sodium-ion battery, the same embodiment of step are carried out
1。
The preferred embodiments of the present invention are the foregoing is only, the present invention is not limited to, it is clear that those skilled in the art
Member the present invention can be carried out it is various change and modification without departing from the spirit and scope of the present invention.So, if the present invention
These modifications and modification belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to comprising these
Including change and modification.
Claims (4)
1. a kind of preparation method of the porous carbon materials for lithium/sodium-ion battery, it is characterised in that comprise the steps：
Step one：Raw material is put into porcelain boat, porcelain boat is put into tube furnace, protective atmosphere is passed through in tube furnace, heat up speed
Rate is 1-10 DEG C/min, and calcining heat is 400-1300 DEG C, and calcination time is 2-10h, obtains intermediate product；The raw material includes
Sodium alginate or sodium isoascorbate or sodium gluconate or sodium glutamate；
Step 2：The intermediate product that step one is obtained is immersed in post-treatment solution, deionized water and ethanol are molten after stirring
Liquid is washed respectively, the product after washing is put in vacuum drying chamber is dried afterwards, obtains porous carbon materials；After described
Processing solution is using hydrochloric acid or nitric acid or sulfuric acid or acetic acid or oxalic acid.
2. a kind of preparation method of porous carbon materials for lithium/sodium-ion battery according to claim 1, its feature exists
In, the protective atmosphere in the step one include one or any two kinds in nitrogen, argon gas, helium, argon hydrogen, neon or
Any three kinds either any four or any five kinds of mixed gas.
3. the preparation method of a kind of porous carbon materials for lithium/sodium-ion battery according to claim 1 and 2, it is special
Levy and be, the post-treatment solution mass fraction in the step 2 is between 1-100%.
4. the preparation method of a kind of porous carbon materials for lithium/sodium-ion battery according to claim 1 and 2, it is special
Levy and be, the mixing time in the step 2 is 1-48 h, baking temperature is 40-90 DEG C, drying time 12-48 h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107565133A (en) * | 2017-08-24 | 2018-01-09 | 武汉工程大学 | A kind of modified sodium alginate with high storage sodium performance derives the preparation method of carbon negative pole material |
| CN107604375A (en) * | 2017-07-12 | 2018-01-19 | 青岛科技大学 | Difunctional VPO catalysts of the porous carbon complex of nitrogen cobalt codope and its preparation method and application |
| CN109148884A (en) * | 2018-06-08 | 2019-01-04 | 中国科学院物理研究所 | A kind of carbon based negative electrodes material and its preparation method and application with high slope capacity |
| CN114388763A (en) * | 2022-01-18 | 2022-04-22 | 太原理工大学 | NiS/graphene @ carbon composite material and preparation method and application thereof |
| CN115261890A (en) * | 2022-09-26 | 2022-11-01 | 苏州仕净科技股份有限公司 | Method for preparing porous carbon material by electrochemically reducing carbon dioxide |
| WO2024000885A1 (en) * | 2022-06-28 | 2024-01-04 | 广东邦普循环科技有限公司 | Preparation method for sodium ion battery porous hard carbon material, and product and use thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107604375A (en) * | 2017-07-12 | 2018-01-19 | 青岛科技大学 | Difunctional VPO catalysts of the porous carbon complex of nitrogen cobalt codope and its preparation method and application |
| CN107565133A (en) * | 2017-08-24 | 2018-01-09 | 武汉工程大学 | A kind of modified sodium alginate with high storage sodium performance derives the preparation method of carbon negative pole material |
| CN109148884A (en) * | 2018-06-08 | 2019-01-04 | 中国科学院物理研究所 | A kind of carbon based negative electrodes material and its preparation method and application with high slope capacity |
| CN114388763A (en) * | 2022-01-18 | 2022-04-22 | 太原理工大学 | NiS/graphene @ carbon composite material and preparation method and application thereof |
| CN114388763B (en) * | 2022-01-18 | 2024-02-20 | 太原理工大学 | NiS/graphene@carbon composite material and preparation method and application thereof |
| WO2024000885A1 (en) * | 2022-06-28 | 2024-01-04 | 广东邦普循环科技有限公司 | Preparation method for sodium ion battery porous hard carbon material, and product and use thereof |
| CN115261890A (en) * | 2022-09-26 | 2022-11-01 | 苏州仕净科技股份有限公司 | Method for preparing porous carbon material by electrochemically reducing carbon dioxide |
| CN115261890B (en) * | 2022-09-26 | 2023-01-17 | 苏州仕净科技股份有限公司 | Method for preparing porous carbon material by electrochemically reducing carbon dioxide |
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