CN110350177A - A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole - Google Patents

A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole Download PDF

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Publication number
CN110350177A
CN110350177A CN201910628221.6A CN201910628221A CN110350177A CN 110350177 A CN110350177 A CN 110350177A CN 201910628221 A CN201910628221 A CN 201910628221A CN 110350177 A CN110350177 A CN 110350177A
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lithium
hpbac
preparation
positive pole
composite positive
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张敏刚
郭锦
李占龙
闫晓燕
连晋毅
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Taiyuan University of Science and Technology
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Taiyuan 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M10/058—Construction or manufacture
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Abstract

The invention belongs to electrode material of lithium battery technical fields, more particularly to a kind of layered porous carbon of lithium-sulfur cell/sulphur composite positive pole preparation method, the following steps are included: S1, using bamboo as carbon source, bamboo is cut into small ring, it is boiled in NaOH solution, again plus hydrochloric acid is to neutrality, and washing is dried afterwards at least twice；S2, the small ring handled well is impregnated in concentrated phosphoric acid, and dry；S3, the small ring after above-mentioned drying is transferred in tube furnace, carbonizes the layered porous active carbon HPBAC that marshalling is made in an inert atmosphere；S4, HPBAC/S compound is prepared using melting diffusion method；S5, preparation HPBAC/S anode composite；S6, assembled battery.Specific surface area and the bigger carbon/sulphur composite positive pole of pore volume is made in the present invention, can not only improve the load capacity of sulphur, moreover it is possible to improve the electrochemical stability of sulfur electrode.The present invention is used for the preparation of lithium sulfur battery anode material.

Description

A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole
Technical field
The invention belongs to electrode material of lithium battery technical fields, and in particular to a kind of layered porous carbon/sulphur of lithium-sulfur cell is multiple Close the preparation method of positive electrode.
Background technique
Complicated, total electrode reaction is reacted in lithium-sulfur cell charge and discharge process are as follows:.? In discharge process, more lithium sulfide intermediate products that lithium and reaction of Salmon-Saxl generate are soluble in electrolyte, are partially soluble in electrolyte More lithium sulfides are further restored by lithium since concentration gradient effect diffuses to lithium anode surface and generate the more lithium sulfides of lower valency, Lead to the corrosion on cathode of lithium surface and the loss of active material in this way；During the charging process, more lithium sulfides of lower valency and lithium are anti- Readily soluble more lithium sulfides should be generated, inside battery self discharge is caused.This shuttle effect causes the stable circulation of battery Property is poor, and coulombic efficiency is lower, restricts the process of lithium-sulfur cell industrialization.In addition, final discharging product Li2S density is smaller, Positive electrode volume expansion destroys the structure of positive electrode, causes the decaying of cycle performance of battery.Meanwhile elemental sulfur is electronics With ion insulator (5 × 10-30 S·cm-1), reduce the utilization rate of sulphur.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of layered porous carbon of lithium-sulfur cell/sulphur composite positive poles Preparation method solves the problems, such as that lithium sulfur battery anode material poorly conductive, the electrochemical stability of electrode are poor.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows:
A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole, it is characterised in that: the following steps are included:
S1, using bamboo as carbon source, bamboo is cut into small ring, is boiled in NaOH solution, then plus hydrochloric acid to neutrality, washing at least two Drying after secondary；
S2, the above-mentioned small ring handled well is impregnated in concentrated phosphoric acid again, and dry；
S3, treated small ring is transferred in tube furnace, carbonizes the stratiform that marshalling is made in an inert atmosphere Porous activated carbon HPBAC；
S4, HPBAC/S compound is prepared using melting diffusion method；
S5, preparation HPBAC/S anode composite；
S6, assembled battery.
The processing method of bamboo in the S1 are as follows: the bamboo of natural air drying is cut into the small ring of 3 × 4 × 10 mm, is used Small ring is boiled 3 times by deionized water, naturally dry.
NaOH solution and the concentration of hydrochloric acid are 1 mol/L in the S1, and the time boiled in NaOH solution is 1 h.
Concentrated phosphoric acid mixture in the S2 by small ring and concentration more than or equal to 85% is placed in a beaker the temperature at 80 DEG C Degree impregnates down 12 h, and dries 12 h in air dry oven at a temperature of 120 DEG C.
Inert atmosphere in the S3 is 500 DEG C of nitrogen of flowing, and nitrogen flow rate is 40 mL min-1, the rate of heat addition 3 ℃∙min-1。
Carbonization time in the S3 in tube furnace is 4 h.
Melting diffusion method in the S4 is that the sublimed sulfur for crossing 400 meshes and HPBAC are pressed matter using planetary ball mill Amount with 180 r/min revolving speed mechanical ball mill, 6 h, then the porcelain boat for being placed with compound is placed in tube furnace than being that 8:2 is mixed, It is 40 mLmin in flow velocity-1N2It is compound that HPBAC/S is made in the lower 155 DEG C of heat preservations of atmosphere protection 12 h, 200 DEG C of 2 h of heat preservation Object, it is stand-by after 60 DEG C of 24 h of vacuum drying.
The method that HPBAC/S anode composite is prepared in the S5 is to be prepared by the way that slurry to be homogeneously applied on aluminium foil Sulfur electrode, electrode slurry contain the PVDF of the HPBAC/S compound of 70wt%, the AB of 20 wt% and 10 wt%, and NMP, which is used as, to be divided Then electrode slice is dried in vacuo 12 h by powder at 60 DEG C, metal lithium sheet is made to electrode, and Celgard 2500 is diaphragm, electricity Mixture of the solution matter by LiTFSI and DOL and DME(volume ratio for 1:1) forms.
Assembled battery carries out in the glove box full of argon gas in the S6.
Compared with prior art, the present invention having the beneficial effect that
Specific surface area and the bigger carbon/sulphur composite positive pole of pore volume is made in the present invention, can not only improve the load capacity of sulphur, and And charge and discharge process electrochemical reaction can be limited in hole by the active carbon of porous structure, and then limited polysulfide and be spread in In electrolyte, the loss of active material is reduced, improves the electrochemical stability of sulfur electrode.
Detailed description of the invention
Fig. 1 is HPBAC(a) and HPBAC/S(b) composite material SEM figure；
Fig. 2 is the TEM(a of HPBAC) and HRTEM(b) figure；
Fig. 3 is the XRD spectra of elemental sulfur, HPBAC and HPBAC/S composite material；
Fig. 4 is the TGA curve of S and HPBAC/S composite material；
Fig. 5 is HPBAC/S combination electrode in 100 mA g-1Charging and discharging curve；
Fig. 6 is HPBAC/S combination electrode in 100 mA g-1Cycle performance curve.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole, comprising the following steps:
S1, the small ring that the bamboo of natural air drying is cut into 3 × 4 × 10 mm are boiled small ring 3 times with deionized water, natural It dries.Small ring is boiled into 1 h with the NaOH solution of 1 mol/L, then plus concentration be 1 mol/L hydrochloric acid to neutrality, washing is at least It dries afterwards twice.
S2, the concentrated phosphoric acid mixture by the above-mentioned small ring handled well and concentration more than or equal to 85% are placed in a beaker 80 DEG C of 12 h of immersion, and in 120 DEG C of dry 12 h in air dry oven.
S3, the small ring after drying is transferred in tube furnace, is 40 mL min in nitrogen flow rate-1, the rate of heat addition 3 ℃∙min-1Nitrogen atmosphere in 500 DEG C of 4 h of heat preservation, carbonize be made marshalling layered porous active carbon HPBAC.
S4, using planetary ball mill by cross 400 meshes sublimed sulfur and HPBAC be in mass ratio 8:2 mix, with 180 6 h of r/min revolving speed mechanical ball mill, then the porcelain boat for being placed with compound is placed in tube furnace, it is 40 mLmin in flow velocity-1's N2HPBAC/S compound is made, after 60 DEG C of 24 h of vacuum drying in the lower 155 DEG C of heat preservations of atmosphere protection 12 h, 200 DEG C of 2 h of heat preservation For use.
S5, sulfur electrode is prepared by the way that slurry to be homogeneously applied on aluminium foil, electrode slurry contains 70wt%'s The PVDF of HPBAC/S compound, the AB of 20 wt% and 10 wt%, NMP are as dispersing agent, then by electrode slice at 60 DEG C 12 h are dried in vacuo, metal lithium sheet is made to electrode, and Celgard 2500 is diaphragm, and electrolyte is by LiTFSI's and DOL and DME Mixture composition.
S6, the assembled battery in the glove box full of argon gas.
Below will using FE-SEM, FE-TEM, TGA and XRD respectively to HPBAC, elemental sulfur and HPBAC/S composite material into Row characterization；Constant current charge-discharge test is carried out using battery of the Land CT2001A type battery test system to assembling.
Embodiment 1
As shown in Figure 1 and Figure 2, comparison diagram 1(a) and (b), HPBAC and sulphur with loose stratiform porous structure uniformly compound rear change It obtains finer and close.The TEM figure of HPBAC has further confirmed the presence (Fig. 2 (a)) of layered porous structure HPBAC.HPBAC's The graphitized area that electron-transport is convenient in part can be observed in HRTEM figure (Fig. 2 (b)), shows host material of the HPBAC as sulphur With excellent electron conduction.In Fig. 1 (b) the HRTEM figure of HPBAC/S compound can be observed with sulphur it is compound after still retaining holes Structure is not only convenient for the infiltration of electrolyte and the transmission of electronics, ion, and lives during capable of buffering lithiumation there are space The volume expansion of property substance, slows down the destruction of anode structure.
Embodiment 2
As shown in Figure 3, Figure 4, Fig. 3 is the XRD spectrum of elemental sulfur, HPBAC and HPBAC/S composite material.The wide diffraction at 25 ° Peak is shown to be unformed HPBAC.Compared with elemental sulfur, HPBAC/S composite material has the feature of apparent orthorhombic system sulphur Diffraction maximum (JCPDS 83-2283), and the remitted its fury of its characteristic diffraction peak, this shows that more elemental sulfur has incorporated HPBAC In hole.The content of sulphur in compound is calculated by TGA.Fig. 4 shows the TGA curve of elemental sulfur and HPBAC/S composite material.? In entire heating process, it can be seen from the figure that elemental sulfur DEG C gradually volatilizees from 160 DEG C to 400, compared with elemental sulfur, wave Hair rate is slower, this may be to cause waving for sulphur since HPBAC micropore abundant and surface functional group are closer to the constraint of sulphur Hair slows down.According to TGA result it is found that the sulfur content in HPBAC/S composite material is 74.9 wt%.
Embodiment 3
As shown in figure 5, HPBAC/S electrode is 100 mA g in current density-1Charging and discharging curve.In initial several circulations In, there is two apparent discharge platforms and a charging platform in the charging and discharging curve of HPBAC/S electrode, this in CV curve Two reduction peaks are consistent with an oxidation peak.In addition, since sulphur active material constantly activates in cyclic process, charging platform Current potential is almost unchanged, and discharge platform current potential is gradually increased to tend towards stability, it means that and HPBAC not only reduces polarization potential, And it ensure that the excellent cyclic reversibility of electrode.Before HPBAC/S the specific discharge capacity of 4 circulations be respectively 1217,1239, 1229 and 1207 mAh g-1, specific discharge capacity is in the trend of first increases and then decreases, shows higher specific discharge capacity, this is Entered inside the HPBAC of the layered porous structure of bigger serface due to more sulphur, increases reaction of Salmon-Saxl active site, improve sulphur Utilization rate.In addition, HPBAC/S polarization of electrode current potential is lower, show it with faster kinetics process.
Embodiment 4
As shown in fig. 6, HPBAC/S electrode is 100 mA g in current density-1Cycle performance curve.HPBAC/S electrode is put Increase trend is presented in the first two circulation in electric specific capacity, this may be since micropore, meso-hole structure HPBAC are close to elemental sulfur Constraint, sulphur does not activate completely during first charge-discharge.The HPBAC of layered porous structure can improve the electronics of electrode Conductibility is conducive to the fast transferring of lithium ion and electronics in charge and discharge process.In subsequent circulation, HPBAC/S electrode All show higher specific discharge capacity, this is because the melting of more sulphur diffuse into the hole of bigger serface HPBAC and Gap, to increase elemental sulfur and the contact area of HPBAC, elemental sulfur is fully used.In addition, the table of HPBAC conductive agent Face functional group can effectively limit the more lithium sulfides of hydrophily and diffuse out from electrode, and HPBAC/S electrode is shown preferably Cyclical stability.Activity in discharge process can be alleviated by not being filled up completely the HPBAC with micropore and meso-hole structure by elemental sulfur The volume expansion of substance improves the cyclical stability of electrode.After 200 circulations, the specific discharge capacity of HPBAC/S electrode is 722 mAh∙g-1, and its coulombic efficiency is up to 95%.
Only presently preferred embodiments of the present invention is explained in detail above, but the present invention is not limited to above-described embodiment, Within the knowledge of a person skilled in the art, it can also make without departing from the purpose of the present invention each Kind variation, various change should all be included in the protection scope of the present invention.

Claims (9)

1. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole, it is characterised in that: including following step It is rapid:
S1, using bamboo as carbon source, bamboo is cut into small ring, is boiled in NaOH solution, then plus hydrochloric acid to neutrality, washing at least two Drying after secondary；
S2, the above-mentioned small ring handled well is impregnated in concentrated phosphoric acid again, and dry；
S3, treated small ring is transferred in tube furnace, carbonizes the stratiform that marshalling is made in an inert atmosphere Porous activated carbon HPBAC；
S4, HPBAC/S compound is prepared using melting diffusion method；
S5, preparation HPBAC/S anode composite；
S6, assembled battery.
2. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the processing method of bamboo in the S1 are as follows: the bamboo of natural air drying is cut into the small ring of 3 × 4 × 10 mm, is used Small ring is boiled 3 times by deionized water, naturally dry.
3. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: NaOH solution and the concentration of hydrochloric acid are 1 mol/L in the S1, and the time boiled in NaOH solution is 1 h.
4. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the concentrated phosphoric acid mixture in the S2 by small ring and concentration more than or equal to 85% is placed in a beaker the temperature at 80 DEG C 12 h of lower immersion, and 12 h are dried in air dry oven at a temperature of 120 DEG C.
5. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the inert atmosphere in the S3 is 500 DEG C of nitrogen of flowing, and nitrogen flow rate is 40 mL min-1, the rate of heat addition 3 ℃∙min-1。
6. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the carbonization time in the S3 in tube furnace is 4 h.
7. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the melting diffusion method in the S4 is by the sublimed sulfur and HPBAC of crossing 400 meshes using planetary ball mill by quality Than with 180 r/min revolving speed mechanical ball mill, 6 h, then the porcelain boat for being placed with compound being placed in tube furnace for 8:2 mixing, Flow velocity is 40 mLmin-1N2It is compound that HPBAC/S is made in the lower 155 DEG C of heat preservations of atmosphere protection 12 h, 200 DEG C of 2 h of heat preservation Object, it is stand-by after 60 DEG C of 24 h of vacuum drying.
8. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: the method that HPBAC/S anode composite is prepared in the S5 is to be prepared by the way that slurry to be homogeneously applied on aluminium foil Sulfur electrode, electrode slurry contain the PVDF of the HPBAC/S compound of 70 wt%, the AB of 20 wt% and 10 wt%, NMP conduct Then electrode slice is dried in vacuo 12 h by dispersing agent at 60 DEG C, metal lithium sheet is made to electrode, and Celgard 2500 is diaphragm, Mixture of the electrolyte by LiTFSI and DOL and DME(volume ratio for 1:1) forms.
9. a kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole according to claim 1, special Sign is: assembled battery carries out in the glove box full of argon gas in the S6.
CN201910628221.6A 2019-07-12 2019-07-12 A kind of preparation method of the layered porous carbon of lithium-sulfur cell/sulphur composite positive pole Pending CN110350177A (en)

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