CN104741014A - Device and method for preparing sulfur-carbon composite cathode material for lithium sulfur battery - Google Patents
Device and method for preparing sulfur-carbon composite cathode material for lithium sulfur battery Download PDFInfo
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- CN104741014A CN104741014A CN201310726817.2A CN201310726817A CN104741014A CN 104741014 A CN104741014 A CN 104741014A CN 201310726817 A CN201310726817 A CN 201310726817A CN 104741014 A CN104741014 A CN 104741014A
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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 device and method for preparing a sulfur-carbon composite cathode material for lithium sulfur batteries. The device includes a mixing tank, and a mixing paddle and a dispersion impeller, which are installed in the mixing tank; and the mixing paddle and the dispersion impeller are respectively controlled through a drive motor group. The outer wall of the mixing paddle is provided with a heat conducting oil jacket layer; the heat conducting oil jacket layer is filled with a heating medium, and provided with a heating rod and a temperature probe, which are connected with a temperature control member and a heating power; a cooling pipe is also arranged in the heat conducting oil jacket layer; and the mixing tank is in a sealing design, and is provided with a vacuum interface and a high pressure gas interface. The method is as below: placing porous carbon and sublimed sulfur in a stirring tank, keeping the pressure in the stirring tank at 100-105 Pa, stirring and dispersing at 110 to 350 DEG C for 0.5-10 h with stirring speed of 10rpm-100 rpm and dispersing line speed of 10-30 m / s; cooling to obtain a sulfur carbon composite material; subjecting the composite to ball milling for 0.5-24 h; and screening to obtain the sulfur-carbon composite cathode material for lithium sulfur batteries. The process provided by the invention is simple, easy to control and realize large scale production.
Description
Technical field
The present invention relates to a kind of Apparatus and method for preparing lithium-sulfur cell sulphur carbon composite anode material, belong to anode material for lithium-ion batteries technical field.
Background technology
Lithium rechargeable battery has vital effect in the grand strategy fields such as electric automobile, electric tool, intelligent grid, distributed energy resource system, national defence.The energy density improving battery is the theme of lithium rechargeable battery research and development always.But through the development of two more than ten years, lithium ion battery reaches its theoretical energy density limit substantially, and its development space is very limited.Meanwhile, for solving the energy and pollution problem, global ev industry upsurge is risen once again, and electric automobile has become the emerging pollution-free industry that the Chinese government actively promotes.But current lithium ion battery is difficult to the continual mileage (being greater than 300KM) that pure electric automobile provides satisfied.Therefore, new lithium secondary battery system is built to obtain the inevitable direction that higher energy density has become secondary cell industry development.
Lithium-sulfur rechargeable battery has the theoretical capacity up to 2600Wh/Kg, much larger than the commercialization secondary cell that present stage uses, and because its abundant raw materials is cheap, environmental friendliness, therefore receives research field and industrial circle is more and more approved and pays close attention to.But lithium-sulfur cell cycle performance is poor is the main cause suppressing its development.
At present, a kind of mainstream development direction of lithium-sulfur cell is by the sulphur of positive electrode and the hot compound of conductive carbon material, with the capacitance loss suppressing the dissolving of sulphur and polysulfide to cause, thus improves its cycle performance.The technique of current sulphur material with carbon element compound mostly is mixing, roasting, and this method technique is loaded down with trivial details, harsh, and not easily homogeneous heating.
Because lithium-sulfur cell is still in development at present, the equipment that market is not designed for sulphur carbon hot composition process, being usually subject to equipment limitation, hindering the research and development of lithium-sulfur cell to a great extent when preparing sulphur carbon composite.
Summary of the invention
The object of the present invention is to provide a kind of equipment preparing lithium-sulfur cell sulphur carbon composite anode material; this device height is integrated with terms and conditions required in sulphur carbon combination process; greatly can simplify the production procedure of positive material for lithium-sulfur battery, be easy to large-scale production.
Another object of the present invention is to provide a kind of method using described equipment to prepare lithium-sulfur cell sulphur carbon composite anode material, the method is simple, and cheaper starting materials is easy to get, and is easy to large-scale production application.
For achieving the above object, the present invention is by the following technical solutions:
Prepare an equipment for lithium-sulfur cell sulphur carbon composite anode material, comprise agitator tank and the paddle that is arranged in this agitator tank and dispersion impeller, paddle and dispersion impeller control respectively by drive motors group; The outer wall of this agitator tank is provided with conduction oil chuck layer, is full of heat medium, and is provided with the heating rod, the temp probe that are connected with temperature control device and heating power supply in this conduction oil chuck layer; Also cooling pipe is provided with in this conduction oil chuck layer; This agitator tank is Seal Design, and is provided with vacuum interface and pressurized gas interface, and vacuum interface connects vacuum table, valve and vavuum pump successively by vacuum pipe; Pressurized gas interface connects malleation table, valve and gas source successively by high-pressure gas pipelines.
Wherein, described agitator tank has the upper cover be tightly connected with it, and the turning cylinder of described paddle and dispersion impeller passes this upper cover in the mode of movable sealing respectively, connects drive motors group.
Preferably, in described upper cover, be provided with sealing ring, be tightly connected by snap close between this upper cover and agitator tank.
Preferably, described cooling pipe is arranged in conduction oil chuck layer in a spiral form.Spiral stream guidance bar is provided with in described conduction oil chuck layer.
Preferably, the mixing speed control range of described paddle is 0 ~ 100rpm; Vacuum cavitations scope in described agitator tank is 100pa ~ 0.1Mpa; Over-pressure control scope is 0.1Mpa ~ 0.5Mpa; Temperature controlling range is-10 DEG C ~ 400 DEG C.
Use described equipment to prepare a method for lithium-sulfur cell sulphur carbon composite anode material, comprise the following steps:
(1) porous carbon and sublimed sulfur are placed in agitator tank, keep the air pressure range in agitator tank to be 100pa ~ 10
5pa, carry out stirring and dispersion treatment 0.5 ~ 10h at 110 DEG C ~ 350 DEG C, mixing speed is 10rpm ~ 100rpm, and discrete lines speed is 10 ~ 30m/s; Sulphur carbon composite is obtained after cooling;
(2) this sulphur carbon composite is carried out ball milling 0.5 ~ 24h, obtain lithium-sulfur cell sulphur carbon composite anode material through screening.
Wherein, the particle diameter D50 of described step (1) porous carbon is less than 5 μm, and be preferably 50 ~ 500nm, the particle diameter D50 of sublimed sulfur is less than 50 μm, is preferably less than 10 μm.
In described step (1), the mass percent of porous carbon, sublimed sulfur is respectively 10% ~ 50%, 50% ~ 90%; Preferably, the mass percent of porous carbon, sublimed sulfur is respectively 10% ~ 30%, 70% ~ 90%.
Reaction temperature in described step (1) is preferably 130 DEG C ~ 150 DEG C; Air pressure range is preferably 100pa ~ 1000pa; Mixing speed is preferably 30rpm ~ 60pm; Discrete lines speed is preferably 20 ~ 30m/s.
The invention has the advantages that:
Device height of the present invention is integrated with terms and conditions required in sulphur carbon combination process; greatly simplify the production procedure of positive material for lithium-sulfur battery; make the preparation technology of lithium-sulfur cell sulphur carbon composite anode material simple and easy to control, be easy to large-scale production.
Method raw material of the present invention is easy to get, and technique is simple, and in the composite obtained, sulphur can be evenly distributed in the hole of porous carbon, thus the capacitance loss suppressing the dissolving of sulphur and polysulfide to cause, improve the electrochemical cycle stability performance of lithium-sulfur cell.
Accompanying drawing explanation
Fig. 1 is the structural representation of present device.
Fig. 2 is the sectional view of the agitator tank of present device.
Fig. 3 is the SEM figure of gained sulphur carbon composite anode material in the embodiment of the present invention 1.
Fig. 4 be in the embodiment of the present invention 1 gained composite first, the charge discharge curve of the 2nd time, the 3rd time and the 4th.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described, but the present invention is not limited to these embodiments.
As shown in Figure 1, 2, the equipment preparing lithium-sulfur cell sulphur carbon composite anode material of the present invention comprises agitator tank 1 and the paddle 2 that is arranged in this agitator tank 1 and dispersion impeller 3, agitator tank 1 has the upper cover be tightly connected with it, the turning cylinder of paddle 2 and dispersion impeller 3 passes this upper cover in the mode of movable sealing respectively, connect drive motors group 4, drive motors group 4 comprises motor 5 and reductor 6.Be provided with sealing ring in described upper cover, agitator tank 1 is provided with snap close 21, by lifting machine 20 agitator tank 1 is promoted to upper cover and utilizes sealing ring and snap close to be tightly connected in working order.The outer wall of agitator tank 1 is provided with conduction oil chuck layer 7, is full of heat medium 8 in this conduction oil chuck layer 7, and is provided with the heating rod 9, the temp probe that are connected with temperature control device (can be such as PID temperature control device) and heating power supply; Spiral circulation type cooling pipe 10 is also provided with in this conduction oil chuck layer; The outside of this conduction oil chuck layer 7 is provided with heat-insulation layer 11.This agitator tank is Seal Design, and is provided with vacuum interface 12 and pressurized gas interface 13, and vacuum interface 12 connects vacuum table, valve and vavuum pump successively by vacuum pipe; Pressurized gas interface 13 connects malleation table, valve and gas source successively by high-pressure gas pipelines.
Thermostable heat-conductive oil can be selected as the heat medium in conduction oil chuck layer.Also be provided with spiral stream guidance bar 14 in conduction oil chuck layer, its effect guides conduction oil to flow to, and makes heating effect more even.
Cold water or other cryogenic media can be selected, to reduce the temperature in agitator tank fast as the cooling medium in cooling pipe.
The equipment with above structure can realize the pressure control function in agitating function, divergent function, agitator tank, the temp. control function in agitator tank simultaneously.Can by automatic controlling system paddle and the drive motors group of dispersion impeller and the heating power supply of conduction oil chuck layer.
When actual production lithium-sulfur cell is with sulphur carbon composite anode material, the original state of equipment as shown in Figure 1, first according to process requirements, a certain proportion of sublimed sulfur and conductive carbon are placed in agitator tank 1, then by lifting machine, agitator tank is promoted to upper cover place, and the sealing utilizing sealing ring and snap close to realize between agitator tank 1 and upper cover.By vacuum pipe, vacuum interface 12 is connected with vacuum table, valve and vavuum pump successively; By high-pressure gas pipelines by pressurized gas interface 13 successively with malleation table, the gentle body tied to source of valve.Close conduction oil chuck layer sewage draining exit 15, conduction oil is added entrance 16 along conduction oil and adds in conduction oil chuck layer 7.Need to adjust the air pressure in agitator tank 1 according to technique.Open motor 5 and reductor 6, make paddle 2 and dispersion impeller 3 by certain speed work.Open heating power supply, heating conduction oil, utilize the temp probe in insertion conduction oil chuck layer 7 and coupled PID temperature control device to control the temperature of conduction oil, and then control the temperature of material in agitator tank.When technique needs cooling, water inlet 17 and the delivery port 18 of spiral circulation type cooling pipe 11 can be opened, make cold water flow through spiral circulation type cooling pipe 11, to reach the object of cooling rapidly.
Embodiment 1
Take 1600g porous carbon (D50 is 50nm), 2400g sublimed sulfur (D50 is 10 μm) raw material in agitator tank, at 150 DEG C, carry out under 100Pa air pressure conditions stirring and dispersion treatment, speed of agitator is 30rpm, dispersion impeller linear velocity is 20m/s, process 3h after be cooled to room temperature obtain hot compound after sulphur carbon composite.Obtain finely dispersed sulphur carbon composite anode material by after the sulphur carbon composite ball milling 2h obtained and screening, be illustrated in figure 3 the SEM figure of gained sulphur carbon composite anode material, material particle size is evenly distributed on 30 ~ 50nm.
The chemical property of gained sulphur carbon composite anode material is evaluated by soft-package battery, its concrete manufacturing process is as follows: take above-mentioned gained sulphur carbon composite anode material, positive conductive agent 1 (conductive carbon black BP2000) and positive conductive agent 2 (conductive carbon black S-p), three's proportioning is 69: 17.2: 6.9, under rotating speed is 300rpm, ball milling 1h, obtains mix products.Take this mix products, binding agent PVDF, NMP, three's mass ratio is 93.1: 6.9: 260, and mix and blend 1h obtains slurry, by coating, roll-in, die-cut cut-parts, then by lamination, assembling, welding, heat-sealing, after fluid injection and forming and capacity dividing, obtains soft-package battery.This soft-package battery carries out the test of 0.1C charge and discharge cycles under Land TCH test channel, obtains chemical property.As shown in Figure 4, the specific discharge capacity that in resulting materials, sulphur shows is 1010.4mAh/g, and coulombic efficiency proportion by subtraction is 99.4% first, shows good chemical property.
Embodiment 2
Take 1200g porous carbon (D50 is 200nm), 2800g sublimed sulfur (D50 is 30 μm) raw material in agitator tank, at 160 DEG C, carry out under 500Pa air pressure conditions stirring and dispersion treatment, speed of agitator is 50rpm, when dispersion impeller linear velocity is 20m/s, process 4h after be cooled to room temperature obtain hot compound after sulphur carbon composite.Sulphur carbon composite anode material is obtained by after the sulphur carbon composite ball milling 3h obtained and screening.
The preparation method of lithium-sulfur cell and method of testing are with embodiment 1.The specific discharge capacity that in resulting materials, sulphur shows is 926mAh/g, and coulombic efficiency proportion by subtraction is 99.1% first, shows good chemical property.
Embodiment 3
Take 800g porous carbon (D50 is 500nm), 3200g sublimed sulfur raw material (D50 is 50 μm) in agitator tank, at 180 DEG C, carry out under 1000Pa air pressure conditions stirring and dispersion treatment, speed of agitator is 50rpm, when dispersion impeller linear velocity is 30m/s, process 5h after be cooled to room temperature obtain hot compound after sulphur carbon composite.Sulphur carbon composite anode material is obtained by after the sulphur carbon composite ball milling 5h obtained and screening.
The preparation method of lithium-sulfur cell and method of testing are with embodiment 1.The specific discharge capacity that in resulting materials, sulphur shows is 992.6mAh/g, and coulombic efficiency proportion by subtraction is 88.2% first, shows good chemical property.
Claims (11)
1. prepare an equipment for lithium-sulfur cell sulphur carbon composite anode material, it is characterized in that, comprise agitator tank and the paddle that is arranged in this agitator tank and dispersion impeller, paddle and dispersion impeller control respectively by drive motors group;
The outer wall of this agitator tank is provided with conduction oil chuck layer; Be full of heat medium in this conduction oil chuck layer, and be provided with the heating rod, the temp probe that are connected with temperature control device and heating power supply; Also cooling pipe is provided with in this conduction oil chuck layer;
This agitator tank is Seal Design, and is provided with vacuum interface and pressurized gas interface, and vacuum interface connects vacuum table, valve and vavuum pump successively by vacuum pipe; Pressurized gas interface connects malleation table, valve and gas source successively by high-pressure gas pipelines.
2. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 1, it is characterized in that, described agitator tank has the upper cover be tightly connected with it, and the turning cylinder of described paddle and dispersion impeller passes this upper cover in the mode of movable sealing respectively, connects drive motors group.
3. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 2, is characterized in that, is provided with sealing ring in described upper cover, is tightly connected between this upper cover and agitator tank by snap close.
4. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 1, is characterized in that, described cooling pipe is arranged in conduction oil chuck layer in a spiral form.
5. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 1, is characterized in that, is provided with spiral stream guidance bar in described conduction oil chuck layer.
6. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 1, is characterized in that, the mixing speed control range of described paddle is 0 ~ 100rpm.
7. the equipment preparing lithium-sulfur cell sulphur carbon composite anode material according to claim 1, is characterized in that, the vacuum cavitations scope in described agitator tank is 100pa ~ 0.1Mpa; Over-pressure control scope is 0.1Mpa ~ 0.5Mpa; Temperature controlling range is-10 DEG C ~ 400 DEG C.
8. use the equipment according to any one of claim 1 ~ 7 to prepare a method for lithium-sulfur cell sulphur carbon composite anode material, it is characterized in that, comprise the following steps:
(1) porous carbon and sublimed sulfur are placed in agitator tank, keep the air pressure range in agitator tank to be 100pa ~ 10
5pa, carry out stirring and dispersion treatment 0.5 ~ 10h at 110 DEG C ~ 350 DEG C, mixing speed is 10rpm ~ 100rpm, and discrete lines speed is 10 ~ 30m/s; Sulphur carbon composite is obtained after cooling;
(2) this sulphur carbon composite is carried out ball milling 0.5 ~ 24h, obtain lithium-sulfur cell sulphur carbon composite anode material through screening.
9. method according to claim 8, is characterized in that, the particle diameter D50 of described step (1) porous carbon is less than 5 μm, and the particle diameter D50 of sublimed sulfur is less than 50 μm.
10. method according to claim 8, is characterized in that, in described step (1), the mass percent of porous carbon and sublimed sulfur is respectively 10% ~ 50%, 50% ~ 90%.
Method according to any one of 11. according to Claim 8 ~ 10, is characterized in that, the reaction temperature in described step (1) is 130 DEG C ~ 150 DEG C; Air pressure range is 100pa ~ 1000pa; Mixing speed is 30rpm ~ 60pm; Discrete lines speed is 20 ~ 30m/s.
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| CN201310726817.2A CN104741014A (en) | 2013-12-25 | 2013-12-25 | Device and method for preparing sulfur-carbon composite cathode material for lithium sulfur battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195868A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of sulphur anode composite material preparation facilities and control method based on sodium thiosulfate and acid reaction |
| CN111653728A (en) * | 2019-03-04 | 2020-09-11 | 中南大学 | Lithium-sulfur battery porous positive electrode and preparation method and application thereof |
| CN112957957A (en) * | 2021-02-03 | 2021-06-15 | 浙江快驴科技有限公司 | Special mixing device for lithium battery material and use method thereof |
| CN115312716A (en) * | 2022-04-28 | 2022-11-08 | 湘潭大学 | Method for preparing sulfur-carbon composite material for all-solid-state lithium-sulfur battery by injecting sulfur through high-pressure gas phase method |
-
2013
- 2013-12-25 CN CN201310726817.2A patent/CN104741014A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107195868A (en) * | 2017-01-06 | 2017-09-22 | 中国计量大学 | A kind of sulphur anode composite material preparation facilities and control method based on sodium thiosulfate and acid reaction |
| CN107195868B (en) * | 2017-01-06 | 2019-08-13 | 中国计量大学 | A kind of sulphur anode composite material preparation facilities and control method based on sodium thiosulfate and acid reaction |
| CN111653728A (en) * | 2019-03-04 | 2020-09-11 | 中南大学 | Lithium-sulfur battery porous positive electrode and preparation method and application thereof |
| CN111653728B (en) * | 2019-03-04 | 2022-02-01 | 中南大学 | Lithium-sulfur battery porous positive electrode and preparation method and application thereof |
| CN112957957A (en) * | 2021-02-03 | 2021-06-15 | 浙江快驴科技有限公司 | Special mixing device for lithium battery material and use method thereof |
| CN115312716A (en) * | 2022-04-28 | 2022-11-08 | 湘潭大学 | Method for preparing sulfur-carbon composite material for all-solid-state lithium-sulfur battery by injecting sulfur through high-pressure gas phase method |
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