CN110739428A - Preparation method of functional diaphragm of lithium-sulfur battery - Google Patents

Preparation method of functional diaphragm of lithium-sulfur battery Download PDF

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CN110739428A
CN110739428A CN201911035170.2A CN201911035170A CN110739428A CN 110739428 A CN110739428 A CN 110739428A CN 201911035170 A CN201911035170 A CN 201911035170A CN 110739428 A CN110739428 A CN 110739428A
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rgo
nicl
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cloth
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CN110739428B (en
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张永光
邱伟龙
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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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
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/403—Manufacturing processes of separators, membranes or diaphragms
    • 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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
    • 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 relates to a preparation method of functional diaphragms of lithium-sulfur batteries, which take carbon cloth as a substrate and are loaded with Ni3S2the/RGO material not only accelerates the transmission efficiency of electrons and ions in the charging and discharging process of the battery, but also promotes the redox reaction of the lithium-sulfur battery in the charging and discharging process, and can well prevent the shuttle effect of polysulfide through chemical adsorption and physical adsorption, thereby improving the cycle and rate capability of the battery.

Description

Preparation method of functional diaphragm of lithium-sulfur battery
Technical Field
The technical scheme of the invention relates to a preparation method of lithium-sulfur battery functional diaphragms taking carbon cloth as a substrate material, belonging to the field of material chemistry.
Background
With the rapid development of electric vehicles and other portable devices, kinds of high-energy-density secondary batteries with high energy density, ultra-long endurance time and good cycle performance are urgently needed by consumers to further meet the requirements of efficient and convenient production and life.
In the using process of the lithium-sulfur battery, sulfur is subjected to oxidation-reduction reaction between 0 valence and-2 valence, and the sulfur anode has theoretical specific capacity up to 1672mAh/g and is far higher than the specific capacity of the anode material of the traditional lithium ion battery (such as a lithium iron phosphate anode material with the specific capacity of about 170 mAh/g).
Firstly, the positive electrode material of the lithium-sulfur battery is elemental sulfur, the conductivity of the elemental sulfur is extremely low, and the reaction between solids is difficult to carry out at normal temperature, so that the elemental sulfur and the conductive material are required to be compounded, and simultaneously, an electrolyte system capable of dissolving polysulfide is used for regulating and controlling the conversion between solid phases of an active substance, so that the battery can be effectively charged and discharged, however, the soluble polysulfide intermediate product brings about new problems, such as polysulfide penetrating through a diaphragm, oxidation-reduction reaction occurring at a positive electrode and a negative electrode, polysulfide "shuttle effect" and the like.
The functional diaphragm is typically designed with a carbon-coated diaphragm, namely, a carbon material capable of reacting and depositing polysulfide is coated on a porous film to reduce sulfur loss in a circulation process, and in addition, metal oxide and metal sulfide which have strong adsorption on polysulfide can be compounded with carbon to be used as the functional battery diaphragm.
Based on the prior art, it would be desirable to combine a conductive carbon-based material with a material having significant electrochemical catalytic activity for polysulfides. The catalytic active material supported on the conductive carbon-based material promotes the electrochemical reaction of polysulfide, and the nucleation and deposition of solid-phase products are more stable and uniform due to the synergistic effect of the carbon-based material and the catalytic active substance. The conversion, reaction and deposition of the battery active substance are greatly optimized, the coulombic efficiency, specific capacity and cycling stability are greatly improved, and the battery also has better cycling capability under high-rate charge and discharge.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides carbon cloth as a substrate loaded with Ni3S2A preparation method of a functional diaphragm of a/RGO lithium-sulfur battery is used for solving the problems of the existing lithium-sulfur battery, especially the high-load and large-rate circulation. The Ni3S2/RGO @ C cloth material is used as a functional diaphragm of the lithium-sulfur battery, so that the transmission efficiency of electrons and ions in the charging and discharging processes of the battery is accelerated, the redox reaction of the lithium-sulfur battery in the charging and discharging processes is promoted, and the shuttle effect of polysulfide can be well prevented through chemical adsorption and physical adsorption.
The preparation method of lithium-sulfur battery functional diaphragms specifically comprises the following steps:
step, preparation of NiCl2-CH3CSNH2-RGO dispersion:
and (3) dispersing Reduced Graphene Oxide (RGO) into deionized water, and performing ultrasonic treatment for 30min to obtain an RGO dispersion liquid. Weighing appropriate amount of NiCl2·6H2O is added to the RGO dispersion and stirring is continued until NiCl2·6H2O was completely dissolved, and amount of thioacetamide (CH) was added3CSNH2) Quickly adding into the mixed solution, stirring until the mixture is completely dissolved to obtain NiCl2-CH3CSNH2-RGO dispersion.
step, in the step, NiCl is prepared2-CH3CSNH2The mass volume ratio of the reduced graphene oxide to the deionized water adopted by the RGO dispersion liquid is 5-7.5 g/L, and the NiCl2·6H2The mass volume ratio of O to deionized water is 15g/L, and the mass volume ratio of thioacetamide to deionized water is 7.5 g/L.
The second step is that: preparation of Ni3S2the/RGO @ C cloth composite functional membrane is as follows:
carbon cloths are taken and ultrasonically cleaned in proper amount of ethanol for 30min and then dried in a blast drier, NiCl prepared in the step is dried2-CH3CSNH2The RGO dispersion was transferred to a dry reactor, and the cleaned carbon cloth was added and sealed. Putting the reaction kettle into an electric heating drying box for heating reaction, and naturally cooling after the reaction is finished to obtain Ni3S2the/RGO @ C cloth is compounded with a functional diaphragm.
, in the second step, the carbon cloth is WOS1009 type, and the area is 2.5cm multiplied by 2.5 cm;
further , the drying temperature of the forced air dryer was 60 ℃.
step, heating the reaction kettle to 150-190 deg.C for 18 h.
The preparation method of the Ni3S2/RGO @ C cloth composite material functional diaphragm of the lithium-sulfur battery is commercially available.
The invention has the following beneficial effects:
(1) in the design process of the invention, the structural problem of the sulfur-based negative electrode material in the negative electrode material of the lithium-sulfur battery is fully considered, and the invention innovatively provides that the carbon cloth is used as the substrate of the diaphragm, and a functional material capable of inhibiting the shuttle effect of polysulfide grows on the carbon cloth and is used for replacing the traditional industrial diaphragm, thereby greatly improving the electrochemical performance of the lithium-sulfur battery.
(2) The carbon cloth substrate is used as a material, a binder is avoided, and the high specific surface area of the three-dimensional structure of the carbon cloth greatly improves the loading capacity of the functional material, so that the inhibition on the shuttle effect of polysulfide is enhanced.
Drawings
FIG. 1 shows Ni prepared in example 13S2And the diagram of the previous 100 times of the button cell with the/RGO @ C cloth composite material as the diaphragm.
FIG. 2 shows Ni prepared in example 13S2Multiplying power performance diagram of button cell with/RGO @ C cloth composite material as diaphragm.
Example 1:
step, preparation of NiCl2-CH3CSNH2-RGO dispersion:
0.24g of Reduced Graphene Oxide (RGO) was weighed and added to 40ml of deionized water, and the mixture was subjected to ultrasonic treatment for 30min to obtain an RGO dispersion. 0.6g of NiCl is weighed out2·6H2O, added to the RGO dispersion and stirred continuously until NiCl2·6H2The O is completely dissolved. 0.3g of thioacetamide (CH)3CSNH2) Quickly adding the mixture into the mixed solution, and stirring the mixture until the mixture is completely dissolved to obtain NiCl2-CH3CSNH2-RGO dispersion.
The second step is that: preparation of Ni3S2the/RGO @ C cloth composite co-functional membrane:
pieces of WOS1009 carbon cloth are cut into 2.5cm multiplied by 2.5cm, ultrasonically cleaned in proper amount of ethanol for 30min and dried in a blast drier at 60 ℃, NiCl2-CH3CSNH2-RGO dispersion liquid prepared in the step is transferred into a 100ml drying reaction kettle, the cleaned carbon cloth is added and sealed, the reaction kettle is placed into an electrothermal drying box, the reaction temperature is set to be 170 ℃, the reaction time is 18h, and the reaction kettle is naturally cooled after the reaction is finished, so that the Ni3S2/RGO @ C cloth composite functional diaphragm is obtained.
As can be seen from figure 1, under the current density of 0.1C, the button cell assembled by the functional diaphragm prepared by the method has the first discharge specific capacity of 1400mAh/g, and can still maintain higher specific capacity after 100 cycles.
As can be seen from FIG. 2, the button cell assembled by the functional diaphragm prepared by the method of the invention has good rate capability, and can still maintain the specific capacity of nearly 1100mAh/g after the battery returns to 0.1C.
Example 2:
step, preparation of NiCl2-CH3CSNH2-RGO dispersion:
0.3g of Reduced Graphene Oxide (RGO) was weighed, added to 40ml of deionized water, and subjected to ultrasonic treatment for 30min to obtain an RGO dispersion. 0.6g of NiCl is weighed out2·6H2O, added to the RGO dispersion and stirred continuously until NiCl2·6H2The O is completely dissolved. 0.3g of thioacetamide (CH)3CSNH2) Quickly adding the mixture into the mixed solution, and stirring the mixture until the mixture is completely dissolved to obtain NiCl2-CH3CSNH2-RGO dispersion.
The second step is that: preparation of Ni3S2the/RGO @ C cloth composite functional membrane is as follows:
pieces of WOS1009 carbon cloth are cut into 2.5cm multiplied by 2.5cm, ultrasonically cleaned in proper amount of ethanol for 30min and dried in a blast drier at 60 ℃, NiCl2-CH3CSNH2-RGO dispersion liquid prepared in the step is transferred into a 100ml drying reaction kettle, the cleaned carbon cloth is added and sealed, the reaction kettle is placed into an electrothermal drying box, the reaction temperature is set to be 150 ℃, the reaction time is 18h, and the reaction kettle is naturally cooled after the reaction is finished, so that the Ni3S2/RGO @ C cloth composite functional diaphragm is obtained.
Example 3:
step of preparing NiCl2-CH3CSNH2-RGO dispersion:
0.24g of Reduced Graphene Oxide (RGO) was weighed and added to 40ml of deionized water, and the mixture was subjected to ultrasonic treatment for 30min to obtain an RGO dispersion. 0.6g of NiCl is weighed out2·6H2O, added to the RGO dispersion and stirred continuously until NiCl2·6H2The O is completely dissolved. 0.3g of thioacetamide (CH)3CSNH2) Quickly adding the mixture into the mixed solution, and stirring the mixture until the mixture is completely dissolved to obtain NiCl2-CH3CSNH2-RGO dispersion.
The second step is that: preparation of Ni3S2the/RGO @ C cloth composite functional membrane is as follows:
pieces of WOS1009 carbon cloth are cut into 2.5cm multiplied by 2.5cm, ultrasonically cleaned in proper amount of ethanol for 30min and dried in a blast drier at 60 ℃, NiCl2-CH3CSNH2-RGO dispersion liquid prepared in the step is transferred into a 100ml drying reaction kettle, the cleaned carbon cloth is added and sealed, the reaction kettle is placed into an electrothermal drying box, the reaction temperature is set to be 190 ℃, the reaction time is 18h, and the reaction kettle is naturally cooled after the reaction is finished, so that the Ni3S2/RGO @ C cloth composite functional diaphragm is obtained.

Claims (5)

1, preparation method of functional diaphragm of lithium-sulfur battery, wherein the functional diaphragm is Ni3S2The preparation process of the/RGO @ C cloth composite functional diaphragm comprises the following steps:
step, preparation of NiCl2-CH3CSNH2-RGO dispersion:
dispersing Reduced Graphene Oxide (RGO) into deionized water, and performing ultrasonic treatment for 30min to obtain an RGO dispersion liquid; weighing appropriate amount of NiCl2·6H2O is added to the RGO dispersion and stirring is continued until NiCl2·6H2O was completely dissolved, and amount of thioacetamide (CH) was added3CSNH2) Quickly adding into the mixed solution, stirring until the mixture is completely dissolved to obtain NiCl2-CH3CSNH2-an RGO dispersion;
the second step is that: preparation of Ni3S2the/RGO @ C cloth composite functional membrane is as follows:
ultrasonically cleaning carbon cloth in appropriate amount of ethanol for 30min, drying in a forced air drier, and mixing NiCl prepared by steps2-CH3CSNH2Transferring the-RGO dispersion liquid into a dry reaction kettle, adding cleaned carbon cloth, sealing, putting the reaction kettle into an electric heating drying box for heating reaction, and naturally cooling after the reaction is finished to obtain Ni3S2the/RGO @ C cloth is compounded with a functional diaphragm.
2. The method of claim 1, wherein in the step, NiCl is prepared2-CH3CSNH2The mass volume ratio of the reduced graphene oxide to deionized water adopted by the RGO dispersion liquid is 5-7.5 g/L, and the NiCl2·6H2The mass volume ratio of O to deionized water is 15g/L, and the mass volume ratio of thioacetamide to deionized water is 7.5 g/L.
3. The method of claim 1, wherein in the second step, the carbon cloth is of a WOS1009 type and has an area of 2.5cm x 2.5 cm.
4. The production method according to claim 1, wherein in the second step, the drying temperature of the forced air dryer is 60 ℃.
5. The preparation method according to claim 1, wherein in the second step, the reaction temperature is 150-190 ℃ and the time is 18 h.
CN201911035170.2A 2019-10-29 2019-10-29 Preparation method of functional diaphragm of lithium-sulfur battery Active CN110739428B (en)

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