CN110380052B - High-conductivity sulfur-based composite material for lithium-sulfur battery positive electrode - Google Patents

High-conductivity sulfur-based composite material for lithium-sulfur battery positive electrode Download PDF

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CN110380052B
CN110380052B CN201910656421.2A CN201910656421A CN110380052B CN 110380052 B CN110380052 B CN 110380052B CN 201910656421 A CN201910656421 A CN 201910656421A CN 110380052 B CN110380052 B CN 110380052B
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sulfur
lithium oxide
lithium
composite material
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CN110380052A (en
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田韬
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Dongying Kunyu Power Supply Technology Co ltd
Shenzhen Kunyu Power Technology Co ltd
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Shenzhen Guangyu Power Technology Co ltd
Dongying Kunyu Power Supply Technology Co ltd
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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
    • 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
    • H01M10/04—Construction or manufacture in general
    • H01M10/0422—Cells or battery with cylindrical casing
    • H01M10/0427—Button cells
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/624—Electric conductive 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 relates to the technical field of lithium-sulfur secondary battery anode materials, and discloses a high-conductivity sulfur-based composite material for a lithium-sulfur battery anode, which comprises the following components in percentage by weight: mixing conductive filler oxygen nanometer copper powder (Cu) and lithium oxide (Li)2O) porous ceramic is subjected to ball milling treatment to obtain a uniformly dispersed nano copper powder-lithium oxide porous ceramic composite conductive carrier, and elemental sulfur anode sulfur powder (S) is subjected to melting infiltration8) And impregnating the nano copper powder and the lithium oxide into the pores of the porous ceramic composite conductive carrier to prepare the high-conductivity sulfur-based composite material. The invention solves the technical problem of low room temperature electrochemical reaction kinetics speed caused by the difficulty in electron and ion transmission at the anode because elemental sulfur and discharge products thereof are insulators of electrons and ions of the sulfur anode used by the anode material of the lithium-sulfur secondary battery at present.

Description

High-conductivity sulfur-based composite material for lithium-sulfur battery positive electrode
Technical Field
The invention relates to the technical field of lithium-sulfur secondary battery positive electrode materials, in particular to a high-conductivity sulfur-based composite material for a lithium-sulfur battery positive electrode.
Background
At present, the one-time charging driving mileage of an electric automobile is lower than 1/3 of a traditional oil vehicle, and in order to meet the development requirements of electric automobile technology and upcoming intelligent automobile technology, the performance of a power battery must be comprehensively improved. Therefore, the development of a novel cathode material having a higher specific capacity and more excellent electrochemical properties becomes a key to the development of the next-generation lithium secondary battery.
Lithium sulfur batteries are one of the hot spots in the research of high-capacity lithium ion batteries in recent years, and are compatible with conventional lithium ion battery oxide electrode materials (such as LiCoO)2，LiFePO4Etc.), the sulfur positive electrode has unique advantages in specific capacity, energy density, power density, etc. Theoretically, LiS is formed after complete reaction of lithium with sulfur2The lithium ion battery can realize 2 electronic reactions, the atomic weight of elemental sulfur is obviously lighter than that of an intercalation compound anode material of the current commercial lithium ion battery, the theoretical specific capacity of an electrode can reach 1675mAh/g, and the theoretical energy density of a lithium/sulfur secondary battery system constructed by sulfur and metal lithium reaches 2600 Wh/kg.
The electrochemical reaction of the sulfur anode involves a multi-step redox reaction accompanied by sulfidationComplex phase transfer process of substances, solid phase elemental sulfur S during discharge8(S) first dissolved to form elemental sulphur S in liquid phase8(l) Then, the sulfur bond is gradually broken to be reduced, and then according to the reaction equation: s8(l)+2e-→S8 2-、3S8 2-+2e-→4S6 2-、2S6 2-+2e-→3S4 2-、S4 2-+2e-→2S6 2-、S2 2-+2e-→S2-Stepwise formation of a series of soluble, medium-length chain polysulphide anions (S)n 2-) The equation: s8(l)+2e-→S8 2-、3S8 2-+2e-→4S6 2-、2S6 2-+2e-→3S4 2-Denotes a liquid phase simple substance S8Is gradually reduced to Sn 2-(4. ltoreq. n.ltoreq.8) which are readily soluble in the electrolyte as shown by the following equation: s4 2-+2e-→2S6 2-、S2 2-+2e-→S2-、S2 2-+2Li+→Li2S2↓、S2-+2Li+→Li2S ↓, the long chain polysulfide ion is further reduced with the deepening of the discharge depth, and S of low valence state is generated2 2-And S2-Combine with lithium ions to form an insoluble end product Li2S2And Li2S; during the charging process, reversible reverse reaction occurs, and the discharge product Li2S2And Li2S is gradually oxidized to grow chain polysulfide lithium and is finally oxidized to elemental sulfur; lithium sulfur batteries have two typical discharge plateaus, typically a high voltage plateau from 2.45V to 2.1V, corresponding to elemental sulfur S8Through a series of soluble polysulphide anions, S is finally generated4 2-The voltage of the low voltage platform is maintained between 2.1V and 1.7V, which indicates that S is generated4 2-Is finally reduced to Li2S2And Li2S。
The oxidation-reduction mechanism makes the sulfur positive electrode capable of breaking through the limit of the capacity of the traditional intercalation compound and showing the capacity far higher than that of the traditional positive electrode material, but the battery system has the following difficulties to be overcome urgently: due to the insulating nature of sulfur, elemental sulfur and its discharge products are both electronic and ionic insulators (sulfur has a conductivity of only 5 × 10 at room temperature-30S/cm), the transport of electrons and ions at the positive electrode is difficult, resulting in a slow rate of kinetics of the electrochemical reaction at room temperature.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a high-conductivity sulfur-based composite material for a lithium-sulfur battery anode, which solves the technical problem that the room-temperature electrochemical reaction kinetics speed is low because elemental sulfur and discharge products thereof are insulators of electrons and ions and the electrons and the ions are difficult to transmit at the anode of the sulfur anode used by the conventional lithium-sulfur secondary battery anode material.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a high-conductivity sulfur-based composite material for a lithium-sulfur battery positive electrode comprises the following raw materials in parts by weight: 40-60 parts of micron-sized lithium oxide ceramic particles, 30-50 parts of micron-sized diatomite, 6-15 parts of silica sol, 10-20 parts of polyethylene glycol sealant, 100 parts of n-hexane solvent, 8-15 parts of nano copper powder (Cu), and 200 parts of sulfur powder (S)8)；
Mixing conductive filler oxygen nanometer copper powder (Cu) and lithium oxide (Li)2O) porous ceramic is subjected to ball milling treatment to obtain a uniformly dispersed nano copper powder-lithium oxide porous ceramic composite conductive carrier, and elemental sulfur anode sulfur powder (S) is subjected to melting infiltration8) And impregnating the nano copper powder and the lithium oxide into the pores of the porous ceramic composite conductive carrier to prepare the high-conductivity sulfur-based composite material.
Preferably, the average particle size of the micron-sized lithium oxide ceramic particles is less than or equal to 75 um.
Preferably, the average particle size of the micron-sized diatomite is less than or equal to 48 um.
Preferably, the average particle size of the copper nanoparticles (Cu) is 500 nm.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
the invention uses conductive filler oxygen nanometer copper powder (Cu) and lithium oxide (Li)2O) porous ceramic is subjected to ball milling treatment to obtain a uniformly dispersed nano copper powder-lithium oxide porous ceramic composite conductive carrier, and elemental sulfur anode sulfur powder (S) is subjected to melting infiltration8) Impregnating the nano copper powder and the lithium oxide into pores of the porous ceramic composite conductive carrier to prepare a high-conductivity sulfur-based composite material;
the high-conductivity sulfur-based composite material is used as a positive electrode active material, Li metal is used as a counter electrode, a 2025 type button cell is assembled in a glove box filled with Ar gas, and electrochemical performance tests are carried out on the button cell, and the results are as follows: constant current charging and discharging at 0.1C multiplying power, the first discharging capacity is 754.3-755.6 mAh/g, and after 50 times of charging and discharging circulation, the discharging capacity is 687.4-687.8 mAh/g;
therefore, the technical problem of low room-temperature electrochemical reaction kinetics speed caused by the fact that elemental sulfur and discharge products thereof are insulators of electrons and ions and the electrons and the ions are difficult to transmit at the positive electrode of the sulfur positive electrode used by the conventional lithium-sulfur secondary battery positive electrode material is solved.
Detailed Description
Lithium oxide (Li)2O) ceramic, white powder, density 2.013g/cm3The content is more than or equal to 98.5 percent, Shanghai Longjin Metal materials Co., Ltd;
sulfur powder (S)8) 400 mesh, content more than or equal to 99.9%, industrial grade, melting point 114 ℃, density of 2.36g/cm3Zhengzhou Enteng chemical products, Inc.;
copper nanoparticles (Cu) with average particle size of 500nm and purity of 99.5%, Shanghai Chaowei nanotechnology Co.
The first embodiment is as follows:
(1) lithium oxide (Li)2O) preparation of porous ceramics
a. Weighing 40g of lithium oxide ceramic particles with the average particle size of less than or equal to 75um, 30g of diatomite with the average particle size of less than or equal to 48um and 6g of silica sol for later use; wherein the mass fraction of the silicon dioxide in the silica sol is 25 percent;
b. dissolving 10g of polyethylene glycol sealant in 100g of n-hexane solvent to obtain pretreatment liquid; vacuumizing the kieselguhr in the step (a) until the vacuum degree is 5Pa, adding the kieselguhr into the pretreatment liquid for pretreatment for 1h, and then filtering and drying to obtain pretreated kieselguhr;
c. ball-milling the lithium oxide ceramic particles obtained in the step (a) with 20g of absolute ethyl alcohol for 3 hours to obtain silicon carbide-doped lithium oxide ceramic slurry;
d. ball-milling the silica sol in the step (a), the diatomite in the step (b), the lithium oxide ceramic slurry in the step (c), 8g of nano copper powder (Cu) and absolute ethyl alcohol together at the speed of 180rpm for 3 hours, drying, carrying out static pressure forming treatment, and carrying out heat preservation sintering at the temperature of 850 ℃ for 2 hours to prepare the nano copper powder-lithium oxide porous ceramic composite conductive carrier;
(2) 200g of sulfur powder (S)8) Placing the mixture into an alumina crucible, placing the alumina crucible into an oven, and melting the mixture at the temperature of 135 ℃;
then, immersing the nano copper powder-lithium oxide porous ceramic composite conductive carrier in the step (1) in a sulfur melt, preserving heat for 1h at the temperature of 135 ℃, taking out the lithium oxide porous ceramic from the sulfur melt, removing the adhesive melt on the surface, and cooling to room temperature to prepare the high-conductivity sulfur-based composite material;
(3) performing performance test on the high-conductivity sulfur-based composite material prepared in the step (2), wherein the impregnation rate is 42.6 percent and the volume impregnation rate is 53.8 percent;
after that, the high conductive sulfur-based composite material was used as a positive electrode active material, Li metal was used as a counter electrode, and a 2025 type button cell was assembled in a glove box filled with Ar gas and subjected to electrochemical performance test, with the results that: the discharge capacity is 754.3mAh/g for the first time when the constant current charge-discharge is carried out under the multiplying power of 0.1C, and after 50 charge-discharge cycles, the discharge capacity is 687.4 mAh/g.
Example two:
(1) lithium oxide (Li)2O) preparation of porous ceramics
a. Weighing 60g of lithium oxide ceramic particles with the average particle size of less than or equal to 75um, 50g of diatomite with the average particle size of less than or equal to 48um and 15g of silica sol for later use; wherein the mass fraction of the silicon dioxide in the silica sol is 30 percent;
b. dissolving 20g of polyethylene glycol sealant in 100g of n-hexane solvent to obtain pretreatment liquid; vacuumizing the kieselguhr in the step (a) until the vacuum degree is 10Pa, adding the kieselguhr into the pretreatment liquid for pretreatment for 1h, and then filtering and drying to obtain pretreated kieselguhr;
c. ball-milling the lithium oxide ceramic particles obtained in the step (a) with 20g of absolute ethyl alcohol for 5 hours to obtain silicon carbide-doped lithium oxide ceramic slurry;
d. ball-milling the silica sol in the step (a), the diatomite in the step (b), the lithium oxide ceramic slurry in the step (c), 15g of nano copper powder (Cu) and absolute ethyl alcohol together at the speed of 300rpm for 3 hours, drying, carrying out static pressure forming treatment, and carrying out heat preservation sintering at the temperature of 900 ℃ for 5 hours to prepare the nano copper powder-lithium oxide porous ceramic composite conductive carrier;
(2) 200g of sulfur powder (S)8) Placing the mixture into an alumina crucible, placing the alumina crucible into an oven, and melting the mixture at the temperature of 150 ℃;
then, immersing the nano copper powder-lithium oxide porous ceramic composite conductive carrier in the step (1) in a sulfur melt, preserving heat for 1h at the temperature of 150 ℃, taking the lithium oxide porous ceramic out of the sulfur melt, removing the adhesive melt on the surface, and cooling to room temperature to prepare the high-conductivity sulfur-based composite material;
(3) performing performance test on the high-conductivity sulfur-based composite material prepared in the step (2), wherein the impregnation rate is 44.3%, and the volume impregnation rate is 54.4%;
after that, the high conductive sulfur-based composite material was used as a positive electrode active material, Li metal was used as a counter electrode, and a 2025 type button cell was assembled in a glove box filled with Ar gas and subjected to electrochemical performance test, with the results that: the discharge capacity is 754.9mAh/g for the first time when the constant current charge-discharge is carried out under the multiplying power of 0.1C, and after 50 charge-discharge cycles, the discharge capacity is 687.7 mAh/g.
Example three:
(1) lithium oxide (Li)2O) preparation of porous ceramics
a. Weighing 50g of lithium oxide ceramic particles with the average particle size of less than or equal to 75um, 40g of diatomite with the average particle size of less than or equal to 48um and 12g of silica sol for later use; wherein the mass fraction of the silicon dioxide in the silica sol is 30 percent;
b. dissolving 18g of polyethylene glycol sealant in 100g of n-hexane solvent to obtain pretreatment liquid; vacuumizing the kieselguhr in the step (a) until the vacuum degree is 9Pa, adding the kieselguhr into the pretreatment liquid for pretreatment for 1h, and then filtering and drying to obtain pretreated kieselguhr;
c. ball-milling the lithium oxide ceramic particles obtained in the step (a) with 20g of absolute ethyl alcohol for 4 hours to obtain silicon carbide-doped lithium oxide ceramic slurry;
d. ball-milling the silica sol in the step (a), the diatomite in the step (b), the lithium oxide ceramic slurry in the step (c), 12g of nano copper powder (Cu) and absolute ethyl alcohol for 3 hours at the speed of 240rpm, drying, carrying out static pressure forming treatment, and carrying out heat preservation sintering at the temperature of 850 ℃ for 3 hours to prepare the nano copper powder-lithium oxide porous ceramic composite conductive carrier;
(2) 200g of sulfur powder (S)8) Placing the mixture into an alumina crucible, placing the alumina crucible into an oven, and melting the mixture at the temperature of 140 ℃;
then, immersing the nano copper powder-lithium oxide porous ceramic composite conductive carrier in the step (1) in a sulfur melt, preserving heat for 1h at the temperature of 140 ℃, taking the lithium oxide porous ceramic out of the sulfur melt, removing the adhesive melt on the surface, and cooling to room temperature to prepare the high-conductivity sulfur-based composite material;
(3) performing performance test on the high-conductivity sulfur-based composite material prepared in the step (2), wherein the impregnation rate is 44.1%, and the volume impregnation rate is 54.2%;
after that, the high conductive sulfur-based composite material was used as a positive electrode active material, Li metal was used as a counter electrode, and a 2025 type button cell was assembled in a glove box filled with Ar gas and subjected to electrochemical performance test, with the results that: the discharge capacity is 755.6mAh/g for the first time when the constant current charge-discharge is carried out under the multiplying power of 0.1C, and after 50 charge-discharge cycles, the discharge capacity is 687.8 mAh/g.

Claims (1)

1. A preparation method of a high-conductivity sulfur-based composite material for a lithium-sulfur battery positive electrode is characterized in that (1) lithium oxide (Li)2O) preparation of porous ceramics
a. Weighing 60g of lithium oxide ceramic particles with the average particle size of less than or equal to 75um, 50g of diatomite with the average particle size of less than or equal to 48um and 15g of silica sol for later use; wherein the mass fraction of the silicon dioxide in the silica sol is 30 percent;
b. dissolving 20g of polyethylene glycol sealant in 100g of n-hexane solvent to obtain pretreatment liquid; firstly, vacuumizing the diatomite in the step (a) until the vacuum degree is 10Pa, adding the diatomite into the pretreatment liquid for pretreatment for 1h, and then filtering and drying to obtain pretreated diatomite;
c. ball-milling the lithium oxide ceramic particles obtained in the step (a) with 20g of absolute ethyl alcohol for 5 hours to obtain silicon carbide-doped lithium oxide ceramic slurry;
d. ball-milling the silica sol in the step (a), the diatomite in the step (b), the lithium oxide ceramic slurry in the step (c), 15g of nano copper powder (Cu) and absolute ethyl alcohol together at the speed of 300rpm for 3 hours, drying, carrying out static pressure forming treatment, and carrying out heat preservation sintering at the temperature of 900 ℃ for 5 hours to prepare the nano copper powder-lithium oxide porous ceramic composite conductive carrier;
(2) 200g of sulfur powder (S)8) Placing the mixture into an alumina crucible, placing the alumina crucible into an oven, and melting the mixture at the temperature of 150 ℃;
then, immersing the nano copper powder-lithium oxide porous ceramic composite conductive carrier in the step (1) in a sulfur melt, preserving heat for 1h at the temperature of 150 ℃, taking the lithium oxide porous ceramic out of the sulfur melt, removing the adhesive melt on the surface, and cooling to room temperature to prepare the high-conductivity sulfur-based composite material;
(3) performing performance test on the high-conductivity sulfur-based composite material prepared in the step (2), wherein the impregnation rate is 44.3%, and the volume impregnation rate is 54.4%;
after that, the high conductive sulfur-based composite material was used as a positive electrode active material, Li metal was used as a counter electrode, and a 2025 type button cell was assembled in a glove box filled with Ar gas and subjected to electrochemical performance test, with the results that: the discharge capacity is 754.9mAh/g for the first time when the constant current charge-discharge is carried out under the multiplying power of 0.1C, and after 50 charge-discharge cycles, the discharge capacity is 687.7 mAh/g.
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