CN106532048B - A kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material - Google Patents
A kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material Download PDFInfo
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- CN106532048B CN106532048B CN201611227947.1A CN201611227947A CN106532048B CN 106532048 B CN106532048 B CN 106532048B CN 201611227947 A CN201611227947 A CN 201611227947A CN 106532048 B CN106532048 B CN 106532048B
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material, field first wins field thistle and takes its stem and be washed with distilled water clean, the acquisition field thistle scapus after vacuum drying；Secondly the field thistle scapus of acquisition is put into diluted acid, adds H2O2Solution carries out hydro-thermal reaction after stirring, is down to room temperature naturally after reaction, then washed respectively with water and ethyl alcohol, then carries out vacuum drying treatment, obtains hydrothermal pretreatment carbon material；Hydrothermal pretreatment carbon material is finally subjected to calcination processing under an inert atmosphere, is cooled to room temperature after calcining, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.Carbon material prepared by the present invention has larger specific surface area, and unique three-dimensional spiral shape structure shows excellent chemical property, is a kind of more satisfactory sodium ion negative material, and preparation process is simple, is easy to industrialization.
Description
Technical field
The present invention relates to room temperature anode material of lithium-ion battery technical fields, and in particular to a kind of three-dimensional spiral shape sodium ion
The preparation method of battery carbon electrode material.
Background technology
Lithium ion battery with its high-energy density, compare dry cell high voltage and become most widely used daily energy storage
Element, and the lithium ion battery also good characteristic with memory-less effect.However since reserves are limited on earth for lithium mine, and
And be unevenly distributed, application cost is high, limits it and is widely applied.And sodium ore reserves is abundant in world wide, it is of low cost, I
Also there is an a large amount of sodium mine in state, therefore develops room temperature sodium-ion battery to replace lithium ion battery be becoming for the following secondary energy storage battery
Gesture.
For comparing dilute scattered precious metal element lithium, sodium is the metallic element that source is very extensive, reserves are very considerable, as
The most promising substitute of lithium ion battery --- sodium-ion battery holds the balance in future source of energy storage.But sodium ion
Radius is much bigger than lithium ion, and diffusion is poor, and embedded potential barrier is high, and alloy is inclined to small, common graphite cathode sodium-ion battery
Theoretical capacity strongly limits sodium-ion battery and moves towards practical less than 30mAh/g.
The study found that the carbon material of some class graphite have larger interlamellar spacing, disordered structure allow sodium ion into
Enter body, while to provide more active sites, improving its energy-storage property.But the carbon material of the graphite-like structure is mostly from plant
Object extract or chemical industry synthesis object, Costco Wholesale is higher, does not meet the view of science of sustainable development.
Invention content
The purpose of the present invention is to provide a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material, with gram
The problems of the above-mentioned prior art is taken, carbon material prepared by the present invention has larger specific surface area, unique three-dimensional spiral
Shape structure shows excellent chemical property, is a kind of more satisfactory sodium ion negative material, and preparation process is simple,
It is easy to industrialization.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material, includes the following steps：
1) field wins field thistle and takes its stem and be washed with distilled water clean, the acquisition field thistle scapus after vacuum drying；
2) the field thistle scapus of acquisition is put into the diluted acid of a concentration of 1-3mol/L, wherein it is put into 1 in per 40mL diluted acids~
Then 5g field thistle scapus adds the H that mass fraction is 10%-30%2O2Solution, wherein 8- is added in per 40mL diluted acids
10mLH2O2Solution carries out hydro-thermal reaction after stirring, is down to room temperature naturally after reaction, then washed respectively with water and ethyl alcohol,
Then vacuum drying treatment is carried out, hydrothermal pretreatment carbon material is obtained；
3) hydrothermal pretreatment carbon material is subjected to calcination processing under an inert atmosphere, is cooled to room temperature after calcining, i.e.,
Obtain three-dimensional spiral shape sodium-ion battery carbon electrode material.
Further, diluted acid is any one in hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid in step 2).
Further, stirring is specially in step 2)：Magnetic agitation 10-120min.
Further, hydro-thermal reaction is specially in step 2)：2-24h is reacted in the environment of temperature is 120-230 DEG C.
Further, it is washed respectively 3 times using water and ethyl alcohol in step 2).
Further, vacuum drying treatment is to be dried in vacuo 8-24h under the conditions of temperature is 60-100 DEG C in step 2).
Further, inert atmosphere is Ar or N in step 3)2Atmosphere.
Further, calcination processing is heated up with the heating rate of 2-10 DEG C/min in step 3), is warming up to 500-
2-12h is calcined after 1000 DEG C.
Compared with prior art, the present invention has technique effect beneficial below：
The preparation method of the present invention has easy to operation, repeatable strong, at low cost, realization environment warp of turning waste into wealth
The characteristics of benefit of helping.The three-dimensional structure charcoal prepared using this method, can as the negative material of room temperature sodium-ion battery
Overcome the problems, such as that low-dimensional carbon material battery capacity is low, Volumetric expansion is serious, has that cyclical stability is strong, battery capacity is high
Feature.This method has the characteristics that easy to operate, repeatable high, of low cost.
Further, by controlling reaction condition, the present invention is pre-processed using hydro-thermal reaction, subsequent high annealing carbonization
Mode obtains three-dimensional structure charcoal carbon material.Multiple components etc. can carry out carbon key in the hydrothermal pretreatment stage, field thistle stem
Coupling crosslinking carries out the carbonization crosslinking of the light degree such as dehydrogenation.So as to avoid the drastically cross-linking process of direct carbonization calcining.Simultaneously
Effectively remove acid-soluble minerals in field thistle stem.The original three-dimensional structure of biology is not only remained after hydrothermal treatment,
And the carbon ball that par-tial polysaccharide is formed through carbonization deposits on three-dimensional structure, and about 100nm is formed after subsequent high-temperature calcination
Carbon particle.Particle size becomes smaller, and can increase specific surface area, to increase the contact with electrolyte, further increases battery
Capacity and cyclical stability.
Description of the drawings
Fig. 1 is the XRD diagram of the three-dimensional spiral shape carbon material prepared in the embodiment of the present invention 7；
Fig. 2 is the SEM figures of the three-dimensional spiral shape carbon material prepared in the embodiment of the present invention 7；
Fig. 3 is the cycle performance figure of the three-dimensional spiral shape carbon material prepared in the embodiment of the present invention 7.
Specific implementation mode
The present invention is described in further detail below：
A kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material, includes the following steps：
1) field wins field thistle and takes its stem and be washed with distilled water clean, the acquisition field thistle scapus after vacuum drying；
2) the field thistle scapus of acquisition is put into the diluted acid of a concentration of 1-3mol/L, the diluted acid is hydrochloric acid, phosphoric acid, nitre
Acid, any one in sulfuric acid, wherein be put into 1~5g field thistle scapus in per 100mL diluted acids, then adding mass fraction is
The H of 10%-30%2O2Solution, wherein 8-10mLH is added in per 40mL diluted acids2O2Solution, then after magnetic agitation 10-120min
Hydro-thermal reaction is carried out, specifically 2-24h is reacted in the environment of temperature is 120-230 DEG C, is down to room temperature naturally after reaction, so
It is washed respectively 3 times with water and ethyl alcohol afterwards, 8-24h is then dried in vacuo under the conditions of temperature is 60-100 DEG C, obtained hydro-thermal and locate in advance
Manage carbon material；
3) by hydrothermal pretreatment carbon material in Ar or N2Calcination processing is carried out under atmosphere, specifically with the heating of 2-10 DEG C/min
Rate heats up, and 2-12h is calcined after being warming up to 500-1000 DEG C, is cooled to room temperature after calcining, that is, obtains three-dimensional spiral
Shape sodium-ion battery carbon electrode material.
The present invention is described in further detail with reference to embodiment：
Embodiment 1
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 2g scapus to be put into the hydrochloric acid of 40mL1mol/L, adds the H that 10mL mass fractions are 10%2O2Solution, magnetic force
It is transferred in 100mL hydrothermal reaction kettles after stirring 10min, 2h is reacted in the environment of temperature is 120 DEG C, reaction terminates to wait for nature
It is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, 8h is then dried in vacuo at 60 DEG C, obtains hydrothermal pretreatment carbon material.
3) 500 DEG C under an ar atmosphere by hydrothermal pretreatment carbon material, are risen to the heating rate of 2 DEG C/min, 2h is calcined, forges
It is sintered beam cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 2
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 5g scapus to be put into 40mL 3mol/L hydrochloric acid, adds the H that 8mL mass fractions are 30%2O2Solution, magnetic force
It is transferred in 100mL hydrothermal reaction kettles, is reacted in the environment of temperature is 230 DEG C for 24 hours after stirring 60min, reaction terminates to wait for certainly
It so is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, 20h is then dried in vacuo at 100 DEG C, obtains hydrothermal pretreatment carbon materials
Material.
3) by hydrothermal pretreatment carbon material in N2Under atmosphere, 1000 DEG C are risen to the heating rate of 10 DEG C/min, calcining
12h, calcining terminate cooled to room temperature, that is, obtain three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 3
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 3g scapus to be put into 40mL 2mol/L phosphoric acid, adds the H that 10mL mass fractions are 30%2O2Solution, magnetic
It is transferred in 100mL hydrothermal reaction kettles after power stirring 50min, 12h is reacted in the environment of temperature is 150 DEG C, reaction terminates to wait for
Naturally it is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, 12h is then dried in vacuo at 70 DEG C, obtains hydrothermal pretreatment carbon materials
Material.
3) 600 DEG C under an ar atmosphere by hydrothermal pretreatment carbon material, are risen to the heating rate of 5 DEG C/min, 6h is calcined, forges
It is sintered beam cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 4
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 4g scapus to be put into the phosphoric acid of 40mL3mol/L, adds the H that 8mL mass fractions are 20%2O2Solution, magnetic
It is transferred in 100mL hydrothermal reaction kettles, is reacted in the environment of temperature is 200 DEG C for 24 hours after power stirring 120min, reaction terminates to wait for
Naturally it is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, is then dried in vacuo at 80 DEG C for 24 hours, obtains hydrothermal pretreatment carbon materials
Material.
3) by hydrothermal pretreatment carbon material in N2Under atmosphere, 900 DEG C are risen to the heating rate of 8 DEG C/min, 8h is calcined, forges
It is sintered beam cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 5
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 2g scapus to be put into the sulfuric acid of 40mL1mol/L, adds the H that 10mL mass fractions are 25%2O2Solution, magnetic
It is transferred in 100mL hydrothermal reaction kettles after power stirring 100min, 8h is reacted in the environment of temperature is 180 DEG C, reaction terminates to wait for
Naturally it is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, 8h is then dried in vacuo at 100 DEG C, obtains hydrothermal pretreatment carbon materials
Material.
3) by hydrothermal pretreatment carbon material in N2Under atmosphere, 800 DEG C are risen to the heating rate of 5 DEG C/min, calcines 10h,
Calcining terminates cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 6
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 1g scapus to be put into the nitric acid of 40mL 3mol/L, adds the H that 10mL mass fractions are 15%2O2Solution,
It is transferred to after magnetic agitation 80min in 150ml hydrothermal reaction kettles, reacts 18h in the environment of temperature is 120 DEG C, reaction terminates
It waits for that nature is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, 12h is then dried in vacuo at 100 DEG C, obtain hydrothermal pretreatment
Carbon material.
3) by hydrothermal pretreatment carbon material in N2Under atmosphere, 1000 DEG C are risen to the heating rate of 2 DEG C/min, calcines 6h,
Calcining terminates cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Embodiment 7
1) field wins fresh field thistle and takes its stem and be washed with distilled water totally, and it is dry that field thistle is obtained after vacuum drying
Stem；
2) it takes 2g scapus to be put into the nitric acid of 40mL 2mol/L, adds the H that 10mL mass fractions are 20%2O2Solution,
It is transferred in 100mL hydrothermal reaction kettles, is reacted for 24 hours in the environment of temperature is 180 DEG C, reaction terminates after magnetic agitation 120min
It waits for that nature is down to room temperature, is then respectively washed 3 times with water and ethyl alcohol, be then dried in vacuo at 100 DEG C for 24 hours, obtain hydrothermal pretreatment
Carbon material.
3) 600 DEG C under an ar atmosphere by hydrothermal pretreatment carbon material, are risen to the heating rate of 10 DEG C/min, calcines 2h,
Calcining terminates cooled to room temperature, that is, obtains three-dimensional spiral shape sodium-ion battery carbon electrode material.
Referring to the XRD diagram of the three-dimensional spiral shape carbon material of Fig. 1, wherein abscissa is angle；Ordinate is relative intensity,
The carbon material that carbonization can have been seen in figure, in the diffraction maximum that 2 θ are 25 ° of very weak graphite.Referring to Fig. 2, as seen from the figure, carbon materials
Material retains original three-dimensional structure of field thistle grass blade, and has the carbon ball of 100nm to deposit on helical mount.The structure has larger ratio
Surface area further increases battery capacity and cyclical stability to increase the contact with electrolyte.Nanometer as seen from Figure 3
Carbon material initial charge specific capacity is 480mAh/g, and specific capacity is close to 190mAh/g after 3 charge and discharge cycles, warp
Specific capacity remains to be maintained at 180mAh/g after crossing 140 cycles, and coulombic efficiency is kept almost at 100%；Illustrate by appropriate
Control reaction condition can obtain the three-dimensional structure charcoal carbon material with preferable chemical property.
The present invention passes through simple hydrothermal carbonization and high temperature cabonization technique, system using cheap HERBA CIRSII as presoma
Sodium-ion battery carbon material used as anode is obtained, is a kind of low cost, environmentally protective, chemical property is good to prepare three based on HERBA CIRSII
Tie up helical form sodium-ion battery carbon electrode material preparation method, this method using the abundant HERBA CIRSII of renewable source as raw material,
By simple hydro-thermal, the methods of heat treatment prepares three-dimensional spiral shape carbon material, and in confirming this three in world wide for the first time
Tieing up structure-biological charcoal carbon material has very high sodium electricity specific capacity, for the first time up to 248mAh/g, can be as sodium cell negative pole material
It uses.
Claims (7)
1. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material, which is characterized in that include the following steps：
1) field wins field thistle and takes its stem and be washed with distilled water clean, the acquisition field thistle scapus after vacuum drying；
2) the field thistle scapus of acquisition is put into the diluted acid of a concentration of 1-3mol/L, wherein it is small to be put into 1~5g in per 40mL diluted acids
Then Ji scapus adds the H that mass fraction is 10%-30%2O2Solution, wherein 8-10mLH is added in per 40mL diluted acids2O2
Solution, after stirring temperature be 120-230 DEG C in the environment of hydro-thermal reaction 2-24h, be down to room temperature naturally after reaction, then
It is washed respectively with water and ethyl alcohol, then carries out vacuum drying treatment, obtain hydrothermal pretreatment carbon material；
3) hydrothermal pretreatment carbon material is subjected to calcination processing under an inert atmosphere, is cooled to room temperature, that is, obtains after calcining
Three-dimensional spiral shape sodium-ion battery carbon electrode material.
2. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, diluted acid is any one in hydrochloric acid, phosphoric acid, nitric acid, sulfuric acid in step 2).
3. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, the middle stirring of step 2) is specially：Magnetic agitation 10-120min.
4. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, is washed respectively 3 times using water and ethyl alcohol in step 2).
5. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, vacuum drying treatment is to be dried in vacuo 8-24h under the conditions of temperature is 60-100 DEG C in step 2).
6. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, inert atmosphere is Ar or N in step 3)2Atmosphere.
7. a kind of preparation method of three-dimensional spiral shape sodium-ion battery carbon electrode material according to claim 1, feature
It is, calcination processing is heated up with the heating rate of 2-10 DEG C/min in step 3), is calcined after being warming up to 500-1000 DEG C
2-12h。
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| CN106033813A (en) * | 2016-06-08 | 2016-10-19 | 陕西科技大学 | Method for preparing sodium-ion battery negative electrode material with sodium alga acid as carbon source |
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| CN106033813A (en) * | 2016-06-08 | 2016-10-19 | 陕西科技大学 | Method for preparing sodium-ion battery negative electrode material with sodium alga acid as carbon source |
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