CN106532049A - Preparation method of carbon electrode material of porous structure sodium-ion battery - Google Patents

Preparation method of carbon electrode material of porous structure sodium-ion battery Download PDF

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CN106532049A
CN106532049A CN201611228907.9A CN201611228907A CN106532049A CN 106532049 A CN106532049 A CN 106532049A CN 201611228907 A CN201611228907 A CN 201611228907A CN 106532049 A CN106532049 A CN 106532049A
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ion battery
preparation
electrode material
carbon electrode
structure sodium
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CN106532049B (en
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曹丽云
胡海玲
黄剑锋
许占位
李嘉胤
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Shaanxi University of Science and Technology
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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
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a preparation method of a carbon electrode material of a porous structure sodium-ion battery. The preparation method comprises the steps of firstly, washing leaves of cirsium segestum with deionized water, and carrying out freeze-drying and grinding to obtain ground dried leaves of cirsium segestum; secondly, placing an activator and the ground dried leaves of cirsium segestum into distilled water according to a mass ratio of (0.5 to 5):1, stirring to form mixed suspension, then performing a hydrothermal reaction, and after the reaction is ended, concentrating the obtained mixture to obtain a slurry product, wherein 1 to 5g of dried leaves of cirsium segestum is added into each 50ml of distilled water; then carrying out calcination on the slurry product in protective gas to obtain a calcined product; and finally, removing the activator in the calcined product, then washing the product with deionized water, and until filtrate is neutral, carrying out drying to obtain the carbon electrode material of the porous structure sodium-ion battery. The carbon material prepared by the preparation method disclosed by the invention has a large specific surface area and a unique three-dimensional pore structure, shows excellent electrochemical performance, and is simple in preparation process, low in cost and easy to implement industrialization.

Description

A kind of preparation method of loose structure sodium-ion battery carbon electrode material
Technical field
The present invention relates to a kind of preparation method of sodium ion secondary battery negative material, and in particular to a kind of loose structure sodium The preparation method of ion battery carbon electrode material.
Background technology
Since 21 century, with day by day exhausted, the Yi Jiqi of the Fossil fuel non-renewable resources such as coal, oil, natural gas The problem of environmental pollution that burning brings, the energy and environmental problem have become the significant bottleneck for affecting world today's sustainable development A property difficult problem.In order to solve this world-famous puzzle, seek to substitute the renewable green energy resource of conventional fossil fuel and seek people and ring The harmonious development in border seems particularly urgent.Lithium rechargeable battery has that voltage is high, specific energy is big, has extended cycle life, electric discharge property Can stable, good, pollution-free safety and the advantages of operating temperature range width, be with a wide range of applications, become in recent years Study hotspot.And lithium ore deposit reserves are limited on earth, and skewness is concentrated mainly on America, and China's lithium ore deposit is less, if Lithium power technology is widely used in clean energy resource energy storage device and electric motor car industry, lithium ore deposit price will certainly be improved, be unfavorable for length Sustainable development long.And sodium ore reserves enriches in world wide, with low cost, also there is substantial amounts of sodium ore deposit in China, therefore develops room Warm sodium-ion battery is come the trend that replaces lithium ion battery to be following secondary energy storage battery.
Material with carbon element has good electric conductivity and a structural stability, and outstanding person has been shown on lithium cell negative pole material The advantage for going out, such as：Graphite has been business-like lithium cell negative pole material, and wherein graphite is with low cost, battery specific capacity is higher simultaneously And good cycling stability；Graphene is because with very big specific surface area, reaching 1100mAh as lithium cell negative pole material specific capacity g-1.But the radius ratio lithium ion of sodium ion is big 1.4 times, and the interlamellar spacing of graphite and Graphene is not enough to receiving sodium ion and inserts Enter, cause them but can not be as sodium cell negative pole material.Therefore, it is necessary to explore prepare other new sodium ion carbon material used as anode.
Porous carbon has preferable heat stability and chemical stability, higher specific surface area and electronic conductance, in the energy Storage and electrochemical field are widely used.Porous carbon can be prepared for template using mesoporous silicon, but this side Method technique is excessively complicated, the electrode material difficult quality guarantee of preparation.Rising in recent years is directly prepared using biomaterial The sodium electrode that porous carbon, Jianhua Hou etc. are prepared for using microalgae at 900 DEG C is up to 450mAhg-1Porous carbon materials, B.E.Conway et al. is prepared for sodium electrode less than 450mAhg Jing after potassium hydroxide treatment using Pericarppium arachidis hypogaeae at 800 DEG C-1Porous Material with carbon element, the capacity prepared using these porous carbon materials be not high, it is difficult to which what the modern electrode material of satisfaction and electric power developed will Ask.At present, HERBA CIRSII is widely distributed, and in addition to small part is used as feedstuff, medical material, the overwhelming majority is removed as weeds, is both made The wasting of resources is formed again into environmental pollution, therefore research HERBA CIRSII prepares porous carbon electrode material as raw material and has environmental conservation With economic benefit bilayer meaning.
The content of the invention
It is an object of the invention to provide a kind of preparation method of loose structure sodium-ion battery carbon electrode material, to overcome The defect that above-mentioned prior art is present, material with carbon element prepared by the present invention have a larger specific surface area, unique three-D pore structure, Excellent chemical property is shown, is a kind of more satisfactory sodium ion negative material, and preparation process is simple, low cost It is honest and clean, it is easy to industrialization.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
A kind of preparation method of loose structure sodium-ion battery carbon electrode material, comprises the following steps：
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator with crush Herba Cirsii cured leaf according to mass ratio be (0.5～5)：1 is put in distilled water, wherein, often 1-5g Herba Cirsii cured leafs are added in 50mL distilled water, stirring forms the slurry that is suspended, then carries out hydro-thermal reaction, after question response terminates, will Obtaining mixture carries out being concentrated to give muddy product；
3) muddy product is calcined under a shielding gas, is obtained calcined product；
4) calcined product is removed into activator, then adopt deionized water wash until filtrate for neutrality after drying, obtain Loose structure sodium-ion battery carbon electrode material.
Further, step 2) in activator be KOH, NaOH, ZnCl2、K2CO3Or Na2CO3In one kind.
Further, step 2) in hydro-thermal reaction temperature be 120-220 DEG C, the time is 2-24h.
Further, step 2) in concentration be magnetic agitation 4-6h at 60-80 DEG C.
Further, step 3) in protective gas be nitrogen or argon, and the flow velocity of protective gas is 20sccm- 100sccm。
Further, step 3) in calcining be specially：It is warming up to 500-1100 DEG C and protects with 1-10 DEG C/min of heating rate Warm 1-6h.
Further, step 4) in remove activator be that calcined product is soaked into 6-12h in 80 DEG C of hydrochloric acid solutions.
Further, the concentration of the hydrochloric acid solution is 1-3mol/L.
Compared with prior art, the present invention has following beneficial technique effect：
The raw material HERBA CIRSII of the present invention is common abandoned biomass, and wide material sources are cheap, environmental protection.This Bright preparation process is simple, it is easy to operate, it is adaptable to large-scale production.The aperture of bigger serface prepared by the present invention concentrates on The material with carbon element structure of the loose structure of 40-60nm can be effectively improved the performance of sodium-ion battery.Big specific surface area is increased Contact of the electrode material with electrolyte, it is meant that have higher electro-chemical activity.The structure of multi-pore channel is conducive to electronics to enter, contracting Short intercalation distance, the method that the present invention prepares the carbon electrode material of porous using common HERBA CIRSII shell, and the carbon electricity Pole material can be applied to the energy storage devices such as sodium-ion battery.
Further, by controlling reaction condition, the material with carbon element that the present invention is prepared through activation carbonization, with certain stone Mo Hua, shows good storage sodium performance.As sode cell negative pole, discharge capacity is to 600mAh/g 200 to the material with carbon element first After circle circulation, capacity is maintained at 232mAh/g；
Description of the drawings
Fig. 1 is schemed for the SEM that material with carbon element is prepared in the embodiment of the present invention 1；
The nitrogen adsorption of porous carbon materials of the Fig. 2 to prepare in the embodiment of the present invention 1 is desorbed and aperture demeanour scattergram；
Fig. 3 is to prepare the cycle performance figure of material with carbon element in the embodiment of the present invention 1.
Specific embodiment
Below the present invention is described in further detail：
A kind of preparation method of loose structure sodium-ion battery carbon electrode material, comprises the following steps：
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator KOH, NaOH, ZnCl2、K2CO3Or Na2CO3Herba Cirsii cured leaf with crushing is (0.5 according to mass ratio ～5)：1 is put in distilled water, wherein, add 1-5g Herba Cirsii cured leafs, magnetic agitation 2h to form the slurry that is suspended in every 50mL distilled water, Then hydro-thermal reaction 2-24h at a temperature of 120-220 DEG C, after question response terminates, will obtain mixture magnetic force at 60-80 DEG C and stir Mix 4-6h and obtain muddy product；
3) muddy product is warming up to into 500- with 1-10 DEG C/min of heating rate under protective gas nitrogen or argon 1100 DEG C and 1-6h is incubated, obtains calcined product, the wherein flow velocity of protective gas is 20sccm-100sccm；
4) by calcined product 80 DEG C concentration for 1-3mol/L hydrochloric acid solution in soak 6-12h remove activator, so Adopt deionized water wash afterwards until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material Material.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator K2CO3Herba Cirsii cured leaf with crushing is 1 according to mass ratio：1 is put in distilled water, wherein, per 50mL 1g Herba Cirsii cured leafs, magnetic agitation 2h is added to form the slurry that is suspended, be then transferred in water heating kettle (packing ratio is 50%) in distilled water Hydro-thermal reaction 12h at a temperature of 180 DEG C, after question response terminates, will obtain mixture magnetic agitation 5h at 80 DEG C and obtain mud Shape product；
3) muddy product is transferred in atmosphere furnace, with heating rate under argon gas atmosphere protection of the air-flow for 50sccm 10 DEG C/min is warming up to 700 DEG C and is incubated 2h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 2mol/L hydrochloric acid solution in soak 6h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.
Fig. 1 is the multiporous biological charcoal material with carbon element SEM figures prepared in the present embodiment 1, and as can be seen from the figure material with carbon element occurs Uniform pore structure, and 35-60nm is concentrated in aperture；Fig. 2 is the N2 adsorption-desorption and pore-size distribution of multiporous biological charcoal material with carbon element Figure, the figure explanation porous carbon materials have the more uniform pore structure of larger specific surface area and size, and the structure can increase Material and the contact area of electrolyte, shorten ion transmission path, with the performance of reinforcing material；Fig. 3 is multiporous biological material with carbon element Negative pole is prepared in 100mA g-1Sodium-ion battery cycle performance figure under the conditions of constant current charge-discharge, it can be seen that battery capacity first Up to 623mAh g-1Circulation remains to reach 240mAhg for more than 100 times-1Specific capacity.
Embodiment 2
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator NaOH with crush Herba Cirsii cured leaf according to mass ratio be 5：1 is put in distilled water, wherein, per 50mL 5g Herba Cirsii cured leafs, magnetic agitation 2h is added to form the slurry that is suspended, be then transferred in water heating kettle (packing ratio is 50%) in distilled water Hydro-thermal reaction 2h at a temperature of 120 DEG C, after question response terminates, will obtain mixture magnetic agitation 4h at 60 DEG C and obtain muddy Product；
3) muddy product is transferred in atmosphere furnace, with heating rate under nitrogen atmosphere protection of the air-flow for 20sccm 5 DEG C/min is warming up to 1100 DEG C and is incubated 4h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 1mol/L hydrochloric acid solution in soak 12h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.
Embodiment 3
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator Na2CO3Herba Cirsii cured leaf with crushing is 0.5 according to mass ratio：1 is put in distilled water, wherein, often Add 3g Herba Cirsii cured leafs, magnetic agitation 2h to form the slurry that is suspended in 50mL distilled water, be then transferred in water heating kettle that (packing ratio is 50%) hydro-thermal reaction 10h at a temperature of 220 DEG C, after question response terminates, will obtain mixture magnetic agitation 6h at 70 DEG C and obtain Muddy product；
3) muddy product is transferred in atmosphere furnace, with the speed that heats up under argon gas atmosphere protection of the air-flow for 400sccm 2 DEG C/min of rate is warming up to 500 DEG C and is incubated 1h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 2mol/L hydrochloric acid solution in soak 8h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.
Embodiment 4
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator K2CO3Herba Cirsii cured leaf with crushing is 2 according to mass ratio：1 is put in distilled water, wherein, per 50mL 2g Herba Cirsii cured leafs, magnetic agitation 2h is added to form the slurry that is suspended, be then transferred in water heating kettle (packing ratio is 50%) in distilled water Hydro-thermal reaction 16h at a temperature of 180 DEG C, after question response terminates, will obtain mixture magnetic agitation 5h at 65 DEG C and obtain mud Shape product；
3) muddy product is transferred in atmosphere furnace, with heating rate under nitrogen atmosphere protection of the air-flow for 60sccm 1 DEG C/min is warming up to 600 DEG C and is incubated 6h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 2mol/L hydrochloric acid solution in soak 4h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.
Embodiment 5
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator KOH with crush Herba Cirsii cured leaf according to mass ratio be 3：1 is put in distilled water, wherein, per 50mL 1g Herba Cirsii cured leafs, magnetic agitation 2h is added to form the slurry that is suspended, be then transferred in water heating kettle (packing ratio is 50%) in distilled water Hydro-thermal reaction 20h at a temperature of 200 DEG C, after question response terminates, will obtain mixture magnetic agitation 6h at 75 DEG C and obtain mud Shape product；
3) muddy product is transferred in atmosphere furnace, with heating rate under argon gas atmosphere protection of the air-flow for 80sccm 6 DEG C/min is warming up to 1000 DEG C and is incubated 5h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 3mol/L hydrochloric acid solution in soak 6h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.
Embodiment 6
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator ZnCl2Herba Cirsii cured leaf with crushing is 4 according to mass ratio：1 is put in distilled water, wherein, often Add 1g Herba Cirsii cured leafs, magnetic agitation 2h to form the slurry that is suspended in 50mL distilled water, be then transferred in water heating kettle that (packing ratio is 50%) hydro-thermal reaction 24h at a temperature of 150 DEG C, after question response terminates, will obtain mixture magnetic agitation 6h at 60 DEG C and obtain Muddy product；
3) muddy product is transferred in atmosphere furnace, with the speed that heats up under argon gas atmosphere protection of the air-flow for 100sccm 8 DEG C/min of rate is warming up to 800 DEG C and is incubated 2h, obtains calcined product；
4) by calcined product 80 DEG C concentration for 3mol/L hydrochloric acid solution in soak 10h, to remove activator, then Adopt deionized water wash until filtrate for neutral after in 80 DEG C of dryings, obtain loose structure sodium-ion battery carbon electrode material.

Claims (8)

1. a kind of preparation method of loose structure sodium-ion battery carbon electrode material, it is characterised in that comprise the following steps：
1) Herba Cirsii blade of grass is washed with deionized, lyophilization and crushing obtain crush Herba Cirsii cured leaf；
2) by activator with crush Herba Cirsii cured leaf according to mass ratio be (0.5～5)：1 is put in distilled water, wherein, per 50mL 1-5g Herba Cirsii cured leafs, stirring is added to form the slurry that is suspended, then carry out hydro-thermal reaction, after question response terminates, will obtain in distilled water Mixture carries out being concentrated to give muddy product；
3) muddy product is calcined under a shielding gas, is obtained calcined product；
4) calcined product is removed into activator, then adopt deionized water wash until filtrate for neutrality after drying, obtain porous Structure sodium-ion battery carbon electrode material.
2. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 2) in activator be KOH, NaOH, ZnCl2、K2CO3Or Na2CO3In one kind.
3. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 2) in hydro-thermal reaction temperature be 120-220 DEG C, the time is 2-24h.
4. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 2) in concentration be magnetic agitation 4-6h at 60-80 DEG C.
5. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 3) in protective gas be nitrogen or argon, and the flow velocity of protective gas is 20sccm-100sccm.
6. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 3) in calcining be specially：It is warming up to 500-1100 DEG C and is incubated 1-6h with 1-10 DEG C/min of heating rate.
7. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 1, its feature exist In step 4) in remove activator be that calcined product is soaked into 6-12h in 80 DEG C of hydrochloric acid solutions.
8. the preparation method of a kind of loose structure sodium-ion battery carbon electrode material according to claim 7, its feature exist In the concentration of the hydrochloric acid solution is 1-3mol/L.
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CN107331833A (en) * 2017-05-27 2017-11-07 深圳大学 A kind of preparation method of anode material of lithium-ion battery
CN107611435A (en) * 2017-09-13 2018-01-19 陕西科技大学 A kind of method that three-dimensional porous sodium-ion battery carbon material used as anode is prepared based on peanut coat
CN107732209A (en) * 2017-10-18 2018-02-23 中南大学 It is a kind of to mix the method that bacteria residue waste material prepares lithium ion carbon negative pole material
CN108011107A (en) * 2017-11-24 2018-05-08 电子科技大学 A kind of preparation method of compound bio charcoal
CN109037677A (en) * 2017-06-12 2018-12-18 四川大学 A kind of porous carbon negative pole material of lithium ion battery and preparation method thereof
CN111009648A (en) * 2019-12-10 2020-04-14 华南农业大学 Silicon-carbon composite material and preparation method thereof

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CN105731452A (en) * 2016-01-22 2016-07-06 青岛大学 Active carbon electrode material as well as preparation method and application thereof
CN105914372A (en) * 2016-06-24 2016-08-31 陕西科技大学 Three-dimensional porous biomass carbon nanomaterial prepared from pomace, and preparation method and application therefor
CN106207179A (en) * 2016-07-07 2016-12-07 陕西科技大学 The method that a kind of KOH activation pomelo peel prepares sodium-ion battery negative material

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CN105692617A (en) * 2016-01-15 2016-06-22 陕西科技大学 Method for preparing porous lithium ion battery carbon electrode material based on rape seed husks
CN105731452A (en) * 2016-01-22 2016-07-06 青岛大学 Active carbon electrode material as well as preparation method and application thereof
CN105914372A (en) * 2016-06-24 2016-08-31 陕西科技大学 Three-dimensional porous biomass carbon nanomaterial prepared from pomace, and preparation method and application therefor
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Publication number Priority date Publication date Assignee Title
CN107331833A (en) * 2017-05-27 2017-11-07 深圳大学 A kind of preparation method of anode material of lithium-ion battery
CN109037677A (en) * 2017-06-12 2018-12-18 四川大学 A kind of porous carbon negative pole material of lithium ion battery and preparation method thereof
CN107611435A (en) * 2017-09-13 2018-01-19 陕西科技大学 A kind of method that three-dimensional porous sodium-ion battery carbon material used as anode is prepared based on peanut coat
CN107732209A (en) * 2017-10-18 2018-02-23 中南大学 It is a kind of to mix the method that bacteria residue waste material prepares lithium ion carbon negative pole material
CN107732209B (en) * 2017-10-18 2020-08-25 中南大学 Method for preparing lithium ion carbon negative electrode material from mixed bacteria residue waste
CN108011107A (en) * 2017-11-24 2018-05-08 电子科技大学 A kind of preparation method of compound bio charcoal
CN111009648A (en) * 2019-12-10 2020-04-14 华南农业大学 Silicon-carbon composite material and preparation method thereof

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