CN107697912A - A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material - Google Patents
A kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material Download PDFInfo
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- CN107697912A CN107697912A CN201710916769.1A CN201710916769A CN107697912A CN 107697912 A CN107697912 A CN 107697912A CN 201710916769 A CN201710916769 A CN 201710916769A CN 107697912 A CN107697912 A CN 107697912A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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 belongs to sodium-ion battery preparing technical field, it is related to a kind of technology of preparing of the battery of carbon nano-sphere structure, more particularly to a kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material, pass through the extraction of natural melanin from inkfish capsule, it is activated using KOH, prepares biomass-based porous, agraphitic carbon nanosphere electrode material；Its preparation technology includes the steps such as extraction of natural melanin powder, carbonization and activation；It is used as the negative material of sodium-ion battery, improves the stability at negative pole structure and interface, improve the cyclical stability of negative pole, is advantageous to commercially produce and applies；Negative material storage sodium prepared by the present invention, in 1000mA g‑1First discharge specific capacity under current density is up to 265mAh g‑1。
Description
Technical field：
The invention belongs to sodium-ion battery preparing technical field, is related to a kind of preparation of the battery of carbon nano-sphere structure
Technology, and in particular to a kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material, by from inkfish capsule
Extraction of natural melanin, it is activated using KOH, prepare biomass-based porous, agraphitic carbon nanosphere electrode material.
Background technology：
In recent years, growing with energy conversion and energy storage demand, energy storage material and equipment development are rapid, especially
In small-sized movable electronics field.Sodium-ion battery is because raw material sources are extensive, preparation technology is simple, cost is low, security
It is high and the advantages that be easy to apply in groups on a large scale, it is considered to be the ideal substitute of lithium ion battery.Sodium-ion battery is born at present
Pole material is mainly various carbon-based materials, such as graphite, carbonaceous mesophase spherules, hard carbon.The chemical property of carbon-based material and its
Each self-structure is closely related.Such as graphite has been the negative material of commercialized lithium ion battery, but due to sodium ion half
With graphite layers away from mismatch, it is very weak that it stores up sodium ability in footpath.And the degree of graphitization of amorphous carbon is low, its structure is mainly by big
Measure the accumulation that interlocks of unordered carbon crystallite to form, graphite layers contain a large amount of nano apertures, provided for the storage of sodium ion away from big again
Preferable avtive spot, therefore amorphous carbon material has higher reversible storage sodium capacity.Porous carbon have specific surface area it is big,
The advantages that good conductivity, high chemical stability, excellent performance is shown on sodium cell negative pole material.In general, biomass
Or high polymer derivative carbon material has larger interlamellar spacing, interlaced layer structure can effectively store sodium ion, not have
Have because curling caused by volumetric expansion, sodium ion quickly, have good overriding by the migration of surface gap.Base
In this, seek to provide a kind of preparation method of biomass-based porous agraphitic carbon nanosphere electrode material, there is good society
Benefit and economic benefit.
The content of the invention：
In order to overcome the shortcomings of the prior art, seek a kind of biomass-based porous agraphitic carbon nanometer ball electrode of design
The preparation method of material, by the extraction of natural melanin from inkfish capsule, it is activated using KOH, prepared biomass-based
Porous, agraphitic carbon nanosphere, and then prepare the sodium-ion battery of high-performance high stability.
To achieve the above object, the preparation work of biomass-based porous agraphitic carbon nanosphere electrode material of the present invention
Skill, comprise the following steps：
(1) extract black liquor from fresh inkfish capsule, add after ultra-pure water carries out centrifuge washing 2-10 times, after centrifugation
Melanin liquid be transferred to bag filter and dialysed, periodic replacement ultra-pure water 2-3 days, the melanin after the purification that will dialyse is carried out
It is standby to obtain natural black pigment powder to powder for freeze-drying；
(2) the melanin powder that step (1) obtains is transferred in tube-type atmosphere furnace under argon atmosphere and carries out 600-900
Degree Celsius carbonization, be then cooled to room temperature；
(3) carbonized product for obtaining step (2) and KOH are according to mass ratio 1:Ground uniformly after 10 mixing, be placed into pipe
In formula stove, under argon atmosphere carry out 700-800 degrees Celsius activation, be then cooled to room temperature, wash, be drying to obtain it is biomass-based
Porous agraphitic carbon nanosphere electrode material；
Further, the carbonisation in step (2), programming rate are 1-10 degrees celsius/minutes, soaking time 1-10
Hour, cooling rate is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, the activation process in step (3), programming rate are 1-10 degrees celsius/minutes, soaking time 1-10
Hour, cooling rate is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, step (3) washing process is：By the product after activation, ground with mortar into powder, pour into 0.1-
In 10Mol hydrochloric acid solution, sealed membrane sealing, magnetic agitation is transferred in baking oven insulation 12 under 80 degrees Celsius after one hour small
When, carry out filtering and washing with ultra-pure water.
Further, step (3) drying process is that oven drying, the time is 10-24 hours under 60 degrees Celsius.
Biomass-based porous agraphitic carbon nanosphere electrode material primary raw material parts by weight of the present invention are：Natural black
Pigment 1-5 parts, KOH 1-30 parts.
Compared with prior art, its preparation method is simple, green and effective by the present invention；The present invention is from natural inkfish juice
Middle extraction melanin, is changed into the carbon ball of N doping after carbonization, it is activated with KOH, obtains unformed and porous Nano carbon balls；
It is used as the negative material of sodium-ion battery, improves the stability at negative pole structure and interface, the circulation for improving negative pole is steady
It is qualitative, be advantageous to commercially produce and apply；Negative material storage sodium prepared by the present invention, in 1000mA g-1Under current density
First discharge specific capacity is up to 265mAh g-1。
Brief description of the drawings：
Fig. 1 is the high-resolution-ration transmission electric-lens figure of biomass-based porous agraphitic carbon nanometer spherical structure prepared by the present invention.
Fig. 2 is the cyclic voltammogram of biomass-based porous agraphitic carbon nanosphere sodium-ion battery of the present invention.
Fig. 3 is the cyclical stability figure of biomass-based porous agraphitic carbon nanosphere sodium-ion battery of the present invention.
Embodiment：
It is described further by way of example and in conjunction with the accompanying drawings.
Embodiment 1：
The preparation technology for the biomass-based porous agraphitic carbon nanosphere electrode material that the present embodiment is related to, including it is following
Step：
(1) extract black liquor from fresh inkfish capsule, add after ultra-pure water carries out centrifuge washing 2-10 times, after centrifugation
Melanin liquid be transferred to bag filter and dialysed, periodic replacement ultra-pure water 2-3 days, the melanin after the purification that will dialyse is carried out
It is standby to obtain natural black pigment powder to powder for freeze-drying；
(2) the melanin powder that step (1) obtains is transferred in tube-type atmosphere furnace under argon atmosphere and carries out 600-900
Degree Celsius carbonization, be then cooled to room temperature；
(3) carbonized product for obtaining step (2) and KOH are according to mass ratio 1:Ground uniformly after 10 mixing, be placed into pipe
In formula stove, under argon atmosphere carry out 700-800 degrees Celsius activation, be then cooled to room temperature, wash, be drying to obtain it is biomass-based
Porous agraphitic carbon nanosphere electrode material；
Further, the carbonisation in step (2), programming rate are 1-10 degrees celsius/minutes, soaking time 1-10
Hour, cooling rate is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, the activation process in step (3), programming rate are 1-10 degrees celsius/minutes, soaking time 1-10
Hour, cooling rate is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, step (3) washing process is：By the product after activation, ground with mortar into powder, pour into 0.1-
In 10Mol hydrochloric acid solution, sealed membrane sealing, magnetic agitation is transferred in baking oven insulation 12 under 80 degrees Celsius after one hour small
When, carry out filtering and washing with ultra-pure water.
Further, step (3) drying process is that oven drying, the time is 10-24 hours under 60 degrees Celsius.
The biomass-based porous agraphitic carbon nanosphere electrode material primary raw material parts by weight that the present embodiment is related to are：Naturally
Melanin 1-5 parts, KOH 1-30 parts.
Embodiment 2：
The biomass-based porous agraphitic carbon nanosphere electrode material primary raw material parts by weight that the present embodiment is related to are：Naturally
5 parts of melanin, 20 parts of KOH.
The preparation technology for the biomass-based porous agraphitic carbon nanosphere sodium-ion battery that the present embodiment is related to, including it is following
Step：
Biomass-based porous agraphitic carbon nanosphere electrode material preparation technology, comprise the following steps：
(1) extract black liquor from fresh inkfish capsule, add after ultra-pure water carries out centrifuge washing 8 times, after centrifugation
Melanin liquid is transferred to bag filter and dialysed, periodic replacement ultra-pure water 2 days, and the melanin after purifying that will dialyse is freezed
Dry to powder, it is standby to obtain natural black pigment powder；
(2) the melanin powder that step (1) obtains is transferred in tube-type atmosphere furnace carried out under argon atmosphere it is 800 Celsius
Degree carbonization, is then cooled to room temperature；
(3) carbonized product for obtaining step (2) and KOH are according to mass ratio 1:Ground uniformly after 10 mixing, be placed into pipe
In formula stove, under argon atmosphere carry out 800 degrees Celsius activation, be then cooled to room temperature, wash, be drying to obtain it is biomass-based porous
Agraphitic carbon nanosphere electrode material；
Further, the carbonisation in step (2), programming rate are 10 degrees celsius/minutes, and soaking time is 10 small
When, cooling rate is 10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, the activation process in step (3), programming rate are 10 degrees celsius/minutes, and soaking time is 10 small
When, cooling rate is 10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
Further, step (3) washing process is：By the product after activation, ground with mortar into powder, pour into 10Mol
Hydrochloric acid solution in, sealed membrane sealing, magnetic agitation is transferred in baking oven under 80 degrees Celsius after one hour and be incubated 12 hours, with surpassing
Pure water carries out filtering and washing.
Further, step (3) drying process is oven drying under 60 degrees Celsius, and the time is 18 hours.
Further, the drying blanking process in step (4) is：Copper foil is placed under the infrared baking lamp that temperature is 60 DEG C
Bake to dry tack free, then copper foil of the lamp after roasting is placed in vacuum drying oven and toasts 10h at 100 DEG C, then by the copper after baking
Paper tinsel roll-in and the Nano carbon balls electrode slice for being cut to a diameter of 12mm.
By Nano carbon balls material prepared by step (3) and acetylene black and Kynoar in mass ratio 8:1:1 mixing, is added dropwise
1-METHYLPYRROLIDONE is fully ground as solvent in agate mortar so that mixture is dispersed；Then by its even spread
In being punched into Nano carbon balls electrode slice on copper foil, after vacuum drying；Using Nano carbon balls electrode slice as battery negative electrodes, metallic sodium
As to electrode, carry out being assembled into finished battery in the glove box full of argon gas.
As shown in figure 1, the distribution of Nano carbon balls scantling is homogeneous made of the present embodiment, diameter is about 100 nanometers, point
It is good to dissipate stability.
Manufactured battery is subjected to constant current charge-discharge test, electrolyte is 1.0Mol NaClO4It is dissolved in EC (ethylene carbonates
Ester) and DMC (dimethyl carbonate) in the mixed solvents EC:DMC=1:1Vol%, and add 5%FEC (fluorinated ethylene carbonate)；
The performance of negative material is tested using electrochemical workstation and blue electric battery test system；Using cyclic voltammetric and perseverance electricity
Stream discharge and recharge characterizes to the performance of material；The voltage range of cyclic voltammetric (CV) test is 0.01V-3V, and sweep speed is
0.1mV s-1, constant current weight discharge current density is 1000mA g-1, voltage range 0.01V-3V；Its result such as Fig. 2, Fig. 3
Shown, Fig. 2 is the cyclic voltammogram of biomass-based porous agraphitic carbon nanosphere sodium-ion battery of the present invention, and the figure is
Typical carbon material cyclic voltammetry curve, first three circle curve co-insides is fine, illustrates that the battery has good stability；Fig. 3 is this
The cyclical stability figure for the biomass-based porous agraphitic carbon nanosphere sodium-ion battery being related to is invented, in 1000mA g-1Electric current
First discharge specific capacity under density is up to 265mAh g-1, have by 300 circulations and still keep stable, capacity is reachable
160mAh g-1, illustrate that the battery has good specific capacity and cyclical stability.
Claims (6)
- A kind of 1. preparation method of biomass-based porous agraphitic carbon nanosphere electrode material, it is characterised in that its preparation technology bag Include following steps：(1) extract black liquor from fresh inkfish capsule, add after ultra-pure water carries out centrifuge washing 2-10 times, will be black after centrifugation Pigment liquid is transferred to bag filter and dialysed, periodic replacement ultra-pure water 2-3 days, and the melanin after purifying that will dialyse is freezed Dry to powder, it is standby to obtain natural black pigment powder；(2) by the melanin powder that step (1) obtains be transferred in tube-type atmosphere furnace under argon atmosphere carry out 600-900 it is Celsius Degree carbonization, is then cooled to room temperature；(3) carbonized product for obtaining step (2) and KOH are according to mass ratio 1:Ground uniformly after 10 mixing, be placed into tube furnace In, under argon atmosphere carry out 700-800 degrees Celsius activation, be then cooled to room temperature, wash, be drying to obtain it is biomass-based porous Agraphitic carbon nanosphere electrode material.
- 2. the preparation method of biomass-based porous agraphitic carbon nanosphere electrode material according to claim 1, its feature It is：Carbonisation in the step (2), programming rate are 1-10 degrees celsius/minutes, and soaking time is 1-10 hours, drop Warm speed is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
- 3. the preparation method of biomass-based porous agraphitic carbon nanosphere electrode material according to claim 1, its feature It is：Activation process in the step (3), programming rate are 1-10 degrees celsius/minutes, and soaking time is 1-10 hours, drop Warm speed is 1-10 degrees celsius/minutes, cools to 300 degrees Celsius, continues to naturally cool to room temperature.
- 4. the preparation method of biomass-based porous agraphitic carbon nanosphere electrode material according to claim 1, its feature It is：Step (3) washing process is：By the product after activation, the salt for into powder, pouring into 0.1-10Mol is ground with mortar In acid solution, sealed membrane sealing, magnetic agitation is transferred in baking oven under 80 degrees Celsius after one hour and is incubated 12 hours, uses ultra-pure water Carry out filtering and washing.
- 5. the preparation method of biomass-based porous agraphitic carbon nanosphere electrode material according to claim 1, its feature It is：Step (3) drying process is that oven drying, the time is 10-24 hours under 60 degrees Celsius.
- 6. the preparation method of biomass-based porous agraphitic carbon nanosphere electrode material according to claim 1, its feature It is：The biomass-based porous agraphitic carbon nanosphere electrode material primary raw material parts by weight are：Natural black pigment 1-5 parts, KOH 1-30 parts.
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Cited By (2)
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| CN112086642A (en) * | 2020-08-19 | 2020-12-15 | 广东工业大学 | Graphitized carbon-coated high-specific-surface-area porous carbon sphere and preparation method and application thereof |
| CN112820848A (en) * | 2021-02-08 | 2021-05-18 | 天津工业大学 | Preparation method of flexible self-supporting melanin electrode |
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Application publication date: 20180216 |