CN108539182B - Preparation method of composite sulfur positive electrode material and application of composite sulfur positive electrode material in all-solid-state lithium-sulfur battery - Google Patents
Preparation method of composite sulfur positive electrode material and application of composite sulfur positive electrode material in all-solid-state lithium-sulfur battery Download PDFInfo
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Abstract
A preparation method of a composite sulfur anode material and application of the composite sulfur anode material in an all-solid-state lithium sulfur battery belong to the technical field of battery material preparation. The method comprises the following steps: dispersing a sulfur material, a solid electrolyte and a conductive agent in a solvent, wherein the solid content is 30-70%, and after ball milling and mixing are carried out uniformly, drying to obtain a first mixture; dispersing a conductive agent in a solvent, wherein the solid content is 30-70%, then adding the conductive agent into the first mixture, adding the conductive agent into the first mixture according to 5-10% of the mass of the first mixture, performing ball milling and mixing uniformly, and drying to obtain a second mixture; and adding a solvating ionic liquid accounting for 2-5% of the mass of the second mixture into the second mixture, and grinding and uniformly mixing the mixture by using a mortar to obtain the composite sulfur anode material. The composite sulfur positive electrode is applied to an all-solid-state lithium sulfur battery. The invention also provides a method for filling the solid particle gaps with a small amount of solvated ionic liquid compatible with each component, and the solvated ionic liquid has an ionic conduction effect and can further strengthen the ionic conduction path of the sulfur material in the electrode.
Description
Technical Field
The invention belongs to the technical field of battery material preparation, and particularly relates to a preparation method of a composite sulfur positive electrode material and application of the composite sulfur positive electrode material in an all-solid-state lithium sulfur battery.
Background
The all-solid-state battery is a new type high-safety lithium ion battery using solid electrolyte to replace traditional liquid electrolyte, and its electrolyte is mainly divided into polymer solid electrolyte and inorganic solid electrolyte. Among them, inorganic solid electrolytes have been receiving wide attention and rapidly developed due to higher safety. Meanwhile, along with the expansion of the lithium ion battery from intelligent wearable equipment to electric vehicles and then to the field of large-scale energy storage, higher requirements are put forward on the energy density and the power density of the battery, and the all-solid-state lithium sulfur battery is considered to be one of the battery systems with the most application prospect in numerous lithium battery systems.
However, all solid-state lithium sulfur batteries still have problems. Compared with a liquid lithium-sulfur battery, the solid lithium-sulfur battery adopts the solid electrolyte, so that the shuttle effect existing in the liquid lithium-sulfur battery is well inhibited, but a good solution for the problem of poor electronic conductivity and ionic conductivity of a sulfur material is not provided, and meanwhile, a good relieving method for capacity loss caused by volume change of sulfur in the charging and discharging processes is not provided. In order to solve the above problems, research and development of a composite process of sulfur, a solid electrolyte and a conductive agent and an electrode preparation technology are required.
Disclosure of Invention
The invention aims to solve the problems of poor electronic conductivity and ionic conductivity and capacity loss of the conventional sulfur composite anode, and provides a preparation method of a composite sulfur anode material and application of the composite sulfur anode material in an all-solid-state lithium-sulfur battery.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a composite sulfur positive electrode material comprises the following specific steps:
the method comprises the following steps: mixing a sulfur material, a solid electrolyte and a conductive agent according to the weight ratio of 40-60: 20-40: dispersing 5-10 mass percent of the mixture in a solvent, wherein the solid content is 30-70%, ball-milling and mixing for 10-40 h at the rotating speed of 200-500 r/min, and drying for 24 h at the temperature of 60 ℃ after uniform mixing to obtain a first mixture;
step two: dispersing a conductive agent in a solvent, wherein the solid content is 30-70%, then adding the conductive agent into the first mixture, adding the conductive agent into the first mixture according to 5-10% of the mass of the first mixture, performing ball milling and mixing for 10-40 h, rotating at 30-50 r/min, and after uniformly mixing, drying at 60 ℃ for 24 h to obtain a second mixture;
step three: and adding a solvating ionic liquid accounting for 2-5% of the mass of the second mixture into the second mixture, and grinding and uniformly mixing the mixture by using a mortar to obtain the composite sulfur anode material.
The composite sulfur positive electrode is applied to an all-solid-state lithium sulfur battery.
Compared with the prior art, the invention has the beneficial effects that:
1. at present, a ball milling method is usually used for preparing a composite sulfur anode material, and because the ball milling rotating speed is high, the structure of an electrode material is easy to damage in the ball milling process to cause the performance reduction of the electrode; and secondly, supplementing the conductive agent again to a proper electrode proportion, performing ball milling at a low rotating speed, maintaining the self structure of the conductive agent material, and repairing the conductive agent structure damaged in the ball milling at the first step, so that a good ion and electron conduction path required by charging and discharging of the sulfur material in the electrode is constructed.
2. Because the solid electrode is difficult to realize 100% density, the invention simultaneously provides that a small amount of solvated ionic liquid compatible with each component is added and filled in the gaps of solid particles, and meanwhile, the solvated ionic liquid has an ionic conduction effect and can further strengthen the ionic conduction path of the sulfur material in the electrode.
3. The addition of the solvated ionic liquid with certain fluidity can also well solve the problem of capacity loss caused by separation of the sulfur material from the electrolyte and the conductive agent due to volume change before and after charging and discharging of the sulfur material.
Drawings
Fig. 1 is a capacity cycle curve diagram of a composite sulfur positive electrode prepared by the method in an all-solid-state lithium sulfur battery;
FIG. 2 is a charge-discharge curve diagram of the composite sulfur positive electrode prepared by the method in an all-solid-state lithium-sulfur battery;
FIG. 3 is a graph showing the capacity cycling curve of a sulfur electrode prepared by a conventional method in a liquid lithium-sulfur battery;
fig. 4 is a graph showing the charge and discharge curves of the sulfur electrode prepared by the conventional method in a liquid lithium-sulfur battery.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
The first embodiment is as follows: the embodiment describes a method for preparing a composite sulfur positive electrode material, which comprises the following specific steps:
the method comprises the following steps: mixing a sulfur material, a solid electrolyte and a conductive agent according to the weight ratio of 40-60: 20-40: dispersing 5-10 mass percent of the mixture in a solvent, wherein the solid content is 30-70%, ball-milling and mixing for 10-40 h at the rotating speed of 200-500 r/min, and drying for 24 h at the temperature of 60 ℃ after uniform mixing to obtain a first mixture;
step two: dispersing a conductive agent in a solvent, wherein the solid content is 30-70%, then adding the conductive agent into the first mixture, adding the conductive agent into the first mixture according to 5-10% of the mass of the first mixture, performing ball milling and mixing for 10-40 h, rotating at 30-50 r/min, and after uniformly mixing, drying at 60 ℃ for 24 h to obtain a second mixture;
step three: and adding a solvating ionic liquid accounting for 2-5% of the mass of the second mixture into the second mixture, and grinding and uniformly mixing the mixture by using a mortar to obtain the composite sulfur anode material.
The second embodiment is as follows: in the first step and the second step, the solvent is one or a mixture of carbon disulfide, acetonitrile, rosin water, xylene, tetrahydrofuran, low paraffin, alcohols, or ether solvents.
The third concrete implementation mode: in the preparation method of the composite sulfur positive electrode material according to the first embodiment, in the first step, the sulfur material is one or more of sulfur or metal sulfide; the metal sulfide is TiS2、CoS2、FeS2、NiS、Cu2S、SnS、SnS2、MoS2、SeS2Or ZnS.
Detailed description of the inventionIn the first step, the solid electrolyte material is a sulfide-based inorganic solid electrolyte, a polymer-based solid electrolyte or an oxide-based inorganic solid electrolyte, and the sulfide-based inorganic solid electrolyte is L i10GeP2S12、75Li2S-25P2S5、70Li2S-30P2S5、50Li2S-10P2S5-10L iCl or 50L i2S-10P2S5-10Li3N、Li6PS5Cl、Li10SnP2S12、Li9.54P3S12Si1.74P1.44S11.7Cl0.3、75 Li2S-24P2S5-P2O5The polymer-based solid electrolyte is PEO-based polymer electrolyte, LL ZO, L AGP, L ATP or LL ZTO.
The fifth concrete implementation mode: in the first step and the second step of the preparation method of the composite sulfur positive electrode material according to the first embodiment, the conductive agent is one of Vapor Grown Carbon Fiber (VGCF), carbon nanotube, activated carbon, or acetylene black.
Sixth embodiment mode the method for preparing a composite sulfur positive electrode material according to first embodiment mode is characterized in that in step three, the solvated ionic liquid is a mixture of triethylene glycol dimethyl ether (Triglyme, G3) and lithium bistrifluoromethylsulfonimide (L iTFSI) (L iG 567) (ether-based solvated ionic liquid), a mixture of tetraethylene glycol dimethyl ether (Tetraglyme, G4) and lithium bistrifluoromethylsulfonimide (L iTFSI) (L iG 4) (ether-based solvated ionic liquid) L I [ TFSA ] - [ e ] [ TFSA ] (lithium bis- (trifluoromethyl-sulfonyl) amide-N, N-dimethyl-sulfonyl) -amide), 1-methyl-3 methyl-azo-methyl-sulfonate [ si-3-methyl ] [ 1-methyl-sulfonyl ] (N, N-dimethyl-methyl-sulfonyl) amide), 1-methyl-3 methyl-imide-methyl-sulfonate [ 1-methyl ] [ 1-methyl ] amide, 1-methyl-sulfonate [ 1-methyl ] 3-methyl ] imide [ 1-methyl ] 3-methyl ] bromide ] 3-methyl-sulfonyl ] [ 1-methyl ] amide.
The seventh embodiment: an application of the composite sulfur positive electrode material prepared according to any one of the first to sixth embodiments is to apply the composite sulfur positive electrode to an all-solid-state lithium-sulfur battery.
Example 1:
a preparation method of a composite sulfur positive electrode material comprises the following specific steps:
the method comprises the following steps: mixing a sulfur material, a solid electrolyte and a conductive agent according to a ratio of 40: 40: 10, the solid content is 40%, ball milling and mixing are carried out for 10 h at the rotating speed of 250 r/min, and after uniform mixing, drying is carried out for 24 h at the temperature of 60 ℃ to obtain a first mixture;
step two: dispersing a conductive agent in a solvent, wherein the solid content is 30-70%, then adding the conductive agent into the first mixture, adding the conductive agent into the first mixture according to 5-10% of the mass of the first mixture, performing ball milling and mixing for 10 hours at a rotating speed of 30 r/min, and after uniformly mixing, drying for 24 hours at a temperature of 60 ℃ to obtain a second mixture;
step three: and adding the solvating ionic liquid accounting for 3% of the mass of the second mixture into the second mixture, and grinding and uniformly mixing the mixture by using a mortar to obtain the composite sulfur cathode material.
Example 2:
firstly, taking 5m of L rosin water, adding 0.4 g of sulfur and L i of sulfur10GeP2S120.4 g of solid electrolyte and 0.1 g of VGCF, ball-milling and mixing for 10 h at the rotating speed of 250 r/min, then drying for 24 h at the drying temperature of 60 ℃ to obtain a first mixture, adding 0.1 g of VGCF and 5m L rosin water into the first mixture again, ball-milling and mixing for 10 h at the rotating speed of 30 r/min, then drying for 24 h at the drying temperature of 60 ℃ to obtain a second mixture, finally adding 0.03 g of L iG3 into the second mixture, and uniformly mixing by using a mortar to obtain the composite sulfur anode material.
The discharge capacity and the cycle performance of the composite sulfur positive electrode prepared in the embodiment are measured and compared with the discharge capacity and the cycle performance of the composite sulfur positive electrode prepared by a common method to obtain figures 1-4, wherein #1 represents the composite sulfur positive electrode prepared in the embodiment and #2 represents the composite sulfur positive electrode prepared by the common method, and the discharge capacity and the cycle performance of the material are obviously improved.
Claims (7)
1. A preparation method of a composite sulfur positive electrode material is characterized by comprising the following steps: the method comprises the following specific steps:
the method comprises the following steps: mixing a sulfur material, a solid electrolyte and a conductive agent according to the weight ratio of 40-60: 20-40: dispersing 5-10 mass percent of the mixture in a solvent, wherein the solid content is 30-70%, ball-milling and mixing for 10-40 h at the rotating speed of 200-500 r/min, and drying for 24 h at the temperature of 60 ℃ after uniform mixing to obtain a first mixture;
step two: dispersing a conductive agent in a solvent, wherein the solid content is 30-70%, then adding the conductive agent into the first mixture, adding the conductive agent into the first mixture according to 5-10% of the mass of the first mixture, performing ball milling and mixing for 10-40 h, rotating at 30-50 r/min, and after uniformly mixing, drying at 60 ℃ for 24 h to obtain a second mixture;
step three: adding a solvating ionic liquid accounting for 2-5% of the mass of the second mixture into the second mixture, and grinding and uniformly mixing the mixture by using a mortar to obtain a composite sulfur positive electrode material; the solvating ionic liquid is a mixture of triethylene glycol dimethyl ether and lithium bis (trifluoromethyl) sulfonyl imide in an equal molar ratio or a mixture of tetraethylene glycol dimethyl ether and lithium bis (trifluoromethyl) sulfonyl imide in an equal molar ratio.
2. The method for preparing a composite sulfur positive electrode material according to claim 1, characterized in that: in the first step and the second step, the solvent is one or a mixture of carbon disulfide, acetonitrile, rosin water, xylene, low paraffin hydrocarbon, alcohol or ether solvent.
3. The method for preparing a composite sulfur positive electrode material according to claim 1, characterized in that: in the first step, the sulfur material is one or more of sulfur or metal sulfide.
4. According to claimThe preparation method of the composite sulfur cathode material is characterized in that in the step one, the solid electrolyte material is sulfide inorganic solid electrolyte, polymer-based solid electrolyte or oxide inorganic solid electrolyte, and the sulfide inorganic solid electrolyte is L i10GeP2S12、75Li2S-25P2S5、70Li2S-30P2S5、50Li2S-10P2S5-10LiCl、50Li2S-10P2S5-10Li3N、Li6PS5Cl、Li10SnP2S12Or 75L i2S-24P2S5-P2O5The polymer-based solid electrolyte is PEO-based polymer electrolyte, and the oxide-based inorganic solid electrolyte is LL ZO, L AGP, L ATP or LL ZTO.
5. The method for preparing a composite sulfur positive electrode material according to claim 1, characterized in that: in the first step and the second step, the conductive agent is one of vapor-grown carbon fiber, carbon nanotube, activated carbon or acetylene black.
6. The method for preparing a composite sulfur positive electrode material according to claim 2, characterized in that: the ether solvent is tetrahydrofuran.
7. The application of the composite sulfur cathode material prepared by the preparation method of the composite sulfur cathode material as claimed in any one of claims 1 to 6 is characterized in that: the composite sulfur positive electrode is applied to an all-solid-state lithium sulfur battery.
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