CN107958998A - A kind of manufacture method of flexible self-supporting lithium sulfur battery anode material - Google Patents
A kind of manufacture method of flexible self-supporting lithium sulfur battery anode material Download PDFInfo
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- CN107958998A CN107958998A CN201610898880.8A CN201610898880A CN107958998A CN 107958998 A CN107958998 A CN 107958998A CN 201610898880 A CN201610898880 A CN 201610898880A CN 107958998 A CN107958998 A CN 107958998A
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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
- 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
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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
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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
- 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
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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
- 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
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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
- 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
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Abstract
The invention discloses a kind of self-supporting lithium sulfur battery anode material.Conductive matrices of the MOF/CNT self-supportings composite membrane for active material sulphur are used, the pore structure enriched using MOF, by the effectively constraint of active material sulphur with MOF holes, alleviating its solution loss, suppresses battery shuttle effect.CNT provides good electric conductivity for electrode at the same time, ensures active material electrochemical kinetics property, while provide tough mechanical stability and self-supporting energy for electrode.By the synergistic effect of MOF materials and CNT, high power capacity, the battery performance of high circulation stability are obtained.The method of the present invention is simple, of low cost, beneficial to popularization, has a significant effect and good practicality, is expected to be used widely in high-energy flexible battery of new generation.
Description
Technical field
The present invention relates to lithium-sulfur rechargeable battery, more particularly to a kind of flexible self-supporting lithium sulfur battery anode material.
Technical background
As the energy and the continuous of environmental problem protrude, and the continuous development of electronic electric equipment, people are for energy storage
System proposes the requirement of higher.Conventional lithium ion battery has the advantages that to have extended cycle life, security is good and is widely used
In market-oriented electronic electric equipment, but limited be subject to its relatively low theoretical specific capacity, be gradually difficult to meet society
Develop the demand for battery high-energy-density.Lithium-sulfur cell is using elemental sulfur as cathode, and lithium metal is the battery system of anode, its
Theoretical specific capacity is up to 2600Wh kg-1, while positive active material sulphur derives from a wealth of sources, and it is cheap, it is environmental-friendly.Therefore,
Lithium-sulfur cell be considered as one of most promising high-energy battery system (Rosenman A, et al.,
Adv.EnergyMater.2015,5,1500212).However, active material poorly conductive in lithium-sulfur cell, charge and discharge process electricity
Pole volume change is big, intermediate product in the electrolytic solution there is dissolubility and adjoint " shuttle effect " etc., cause lithium sulphur electric
The cycle life in pond is poor, hinders its commercialized development (Manthiram A, Account of Chemical
Research.2013,46,1125-1134)。
In recent years, research staff is improved sulphur cathode by various methods, effectively increases the electrification of lithium-sulfur cell
Learn performance.Wherein, application of metal organic frame (MOF) material in lithium-sulfur cell has received widespread attention.MOF has abundant
Pore structure and higher aperture controllability, there is good physical absorption to imitate lithium-sulfur cell intermediate product polysulfide ion
Should, while the chemical complexing effect between the polysulfide ion of wherein lewis acidic metal ion and lewis base provides good change
Learn adsorption capacity (Zhou JW, et al., Energy Environ.Sci., 2014,7,2715-2724；Wang ZQ,et
Al., Cryst.Growth Des.2013,13,5116-5120) by cathode introduce MOF materials can effectively improve battery
Cycle performance.In addition, the introducing of nano-carbon material can improve the electric conductivity of material, while its abundant pore structure can accommodate work
Property material sulphur and buffer its volume change in charge and discharge process, the pore space structure for passing through its wiener scale suppresses polysulfide
Migration and shuttle, improve battery capacity and efficiency (Yang Y, et al., Chem.Soc.Rev., 2013,42,3018-
3032).Carbon nanotubes (carbon nanotube, CNT) has the one-dimensional tubular nanostructures curled into by graphene.Its
In with sp2 hybrid forms bonding carbon atom cause CNT that there is very high Young's modulus, there is higher fracture strength, it is splendid
Toughness and the adjustable surface of chemistry, be easily worked the flexible electrode material to form self-supporting.And prepared by self-supporting electrode
During need not add binding agent and conductive agent, but directly active material is supported on conductive matrices, manufacturing process side
Just it is simple, while reduce the dead volume of electrode material, the surface area of active material is added, enhances whole electrode material
Electric conductivity, avoids the generation of electrode material powder phenomeneon in charge and discharge process, thus improve active material utilization and
Electrode cycle stability.It can be appreciated that self-supporting composite electrode has very big answer in the every field of future life
With value.
The content of the invention
It is an object of the invention to, there are problem and application demand, be proposed a kind of easy and effective for current lithium-sulfur cell
Method, obtain the conductive network based on flexible back bone, provide active material good physics, chemistry is supported, and had
The positive electrode of self-supporting property, and develop its technology of preparing, so as to obtain high performance flexible lithium sulphur battery electrode material.
Technical scheme is as follows：
Metal nitrate is immersed in ethylaminoethanol and obtains metal hydroxides nano wire within 2 days in the solution.
Gained metal hydroxides nano wire and single-wall carbon nanotubes are uniformly mixed in the solution, existed in diameter 2cm
Filtered on porous matrix, be dried to obtain the MHNs/CNT composite membranes of self-supporting.
Gained MHNs/CNT is compounded in in the water of organic acid and the mixed solution of ethanol immersion reaction 1h at room temperature, is taken out
Filter, it is dry, obtain MHNs/CNT composite membranes.And the disk of diameter 14mm is cut into, weigh stand-by.
Sublimed sulfur is dissolved in CS under heating stirring2In obtain S/CS2Solution.By resulting solution by certain mass than instilling
In composite membrane, slowly it is evaporated, and the positive electrode MOF/CNTS that 8h obtains self-supporting is heat-treated at 140 DEG C.
In Ar atmosphere glove box, using gained pole piece as cathode, 2400 polypropylene porous films of Celgard are membrane, metal
Lithium paper tinsel is anode, is assembled into CR2025 button cells.Electrolyte is 1M LiTFSI/DME+DOL (v:V=1:1) mixing is molten
Liquid, wherein the lithium nitrate additive containing 1wt.%.
The preparation method and structure design of the present invention is suitable for a variety of MOF materials (HKUST-1, ZIF-5, ZIF-5) at the same time.
Another technical characteristic in the present invention is in the hole of the dispersed MOF materials of active material, the aperture of MOF materials
For 0.34~1.5nm.
It is 15~75 μm that technical characteristic, which also resides in gained pole piece thickness, in the present invention.
The present invention compared with prior art, has following a little with protruding effect：The present invention uses simple and practicable solwution method
It is prepared for self-supporting MOF/CNT composite membranes, and the lithium-sulphur cell positive electrode material of self-supporting is obtained as the conducting matrix grain of sulphur cathode
Material.The pore structure enriched by MOF, by the effectively constraint of active material sulphur with MOF holes, alleviating its solution loss, suppresses battery
Shuttle effect.CNT provides good electric conductivity for electrode at the same time, ensures active material electrochemical kinetics property, while is electricity
Pole provides tough mechanical stability and self-supporting energy.By the synergistic effect of MOF materials and CNT, high power capacity is obtained, it is high
The battery performance of cyclical stability.The method of the present invention is simple, of low cost, beneficial to popularization, has a significant effect and good
Practicality, is expected to be used widely in high-energy flexible battery of new generation.
Brief description of the drawings
Fig. 1 is the bending schematic diagram of gained self-supporting pole piece in embodiment 1.Gained HKUST-1/CNTS electrodes are shown in figure
With good mechanical flexibility.
Fig. 2 is the cross-sectional scans electron microscope of gained self-supporting HKUST-1/CNT composite membranes in embodiment 1.Institute is first said in figure
Obtaining composite membrane has uniform layer structure, and carbon managed network is interspersed in whole electrode, and MOF crystal sizes are more homogeneous, and
It is even to be distributed in electrode.
Fig. 3 is the cycle performance of electrode of the gained of embodiment 1~3 based on different MOF.
Embodiment
The present invention provides a kind of self-supporting MOF/CNTS positive electrodes for lithium-sulfur cell, it is characterised in that with reference to MOF
To the support of the physics of active material, chemisorption and CNT materials to electric conductivity and mechanical performance, obtain has surely material
Determine the lithium-sulfur cell of structure and excellent properties.
Several specific embodiments are enumerated below, and to further understand the present invention, but the present invention is not only limited to following implementation
Example.
Embodiment 1
Copper nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains Kocide SD nanowire dispersion after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 1mg
Dispersion mixing is uniform in water by certain mass ratio for Kocide SD nano wire and 2mg carbon nanotubes, in diameter 2cm in porous base
Filtered in matter, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting.By gained Kocide SD/CNT composite membranes immersion
In water/alcohol mixed solution of the trimesic acid of 20mM, solvent volume ratio is 1：1.At room temperature after immersion reaction 1h
To the HKUST-1/CNT composite membranes of self-supporting.Sublimed sulfur is dissolved in CS under stirring at room temperature2In obtain S/CS2Solution.By gained
Solution presses certain mass than adding in gained HKUST-1/CNT composite membranes, is slowly heat-treated at room temperature after drying at 140 DEG C
8h obtains the positive electrode HKUST-1/CNTS of self-supporting, as cell positive material.Sulphur carrying capacity is 1mg cm wherein on pole piece-2。
Embodiment 2
Zinc nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains zinc hydroxide nano-wire dispersion liquid after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 1mg
Dispersion mixing is uniform in water for zinc hydroxide nano-wire and 2mg carbon nanotubes, is filtered on the porous matrix of diameter 2cm, is dry
Obtain zinc hydroxide/carbon nano-tube compound film of self-supporting.Gained zinc hydroxide/CNT composite membranes are immersed in the 2- first of 25mM
In water/alcohol mixed solution of base imidazoles, solvent volume ratio is 4：1.At room temperature self-supporting is obtained after immersion reaction 24h
ZIF-8/CNT composite membranes.Sublimed sulfur is dissolved in CS under stirring at room temperature2In obtain S/CS2Solution.Resulting solution is pressed into certain matter
Measure than in addition gained ZIF-8/CNT composite membranes, at room temperature slowly after drying, 8h acquisition self-supportings are heat-treated at 140 DEG C
Positive electrode ZIF-8/CNTS, as cell positive material.Sulphur carrying capacity is 1mg cm wherein on pole piece-2。
Embodiment 3
Zinc nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains zinc hydroxide nano-wire dispersion liquid after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 1mg
Dispersion mixing is uniform in water for zinc hydroxide nano-wire and 2mg carbon nanotubes, is filtered on the porous matrix of diameter 2cm, is dry
Obtain zinc hydroxide/carbon nano-tube compound film of self-supporting.By gained zinc hydroxide/CNT composite membranes be immersed in 20mM to benzene
In water/alcohol mixed solution of dioctyl phthalate, solvent volume ratio is 4：1.At 120 DEG C self-supporting is obtained after immersion reaction 12h
ZIF-5/CNT composite membranes.Sublimed sulfur is dissolved in CS under stirring at room temperature2In obtain S/CS2Solution.Resulting solution is pressed into certain matter
Measure than in addition gained ZIF-5/CNT composite membranes, at room temperature slowly after drying, 8h acquisition self-supportings are heat-treated at 140 DEG C
Positive electrode ZIF-5/CNTS, as cell positive material.Sulphur carrying capacity is 1mg cm wherein on pole piece-2。
Embodiment 4
Copper nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains Kocide SD nanowire dispersion after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 2mg
Dispersion mixing is uniform in water by certain mass ratio for Kocide SD nano wire and 4mg carbon nanotubes, in diameter 2cm in porous base
Filtered in matter, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting.By gained Kocide SD/CNT composite membranes immersion
In water/alcohol mixed solution of the trimesic acid of 20mM, solvent volume ratio is 1：1.Obtained at room temperature after immersion reaction 1h
Obtain the HKUST-1/CNT composite membranes that thickness is 2 times of self-supporting in embodiment 1.
Embodiment 5
Copper nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains Kocide SD nanowire dispersion after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 3mg
Dispersion mixing is uniform in water by certain mass ratio for Kocide SD nano wire and 6mg carbon nanotubes, in diameter 2cm in porous base
Filtered in matter, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting.By gained Kocide SD/CNT composite membranes immersion
In water/alcohol mixed solution of the trimesic acid of 20mM, solvent volume ratio is 1：1.Obtained at room temperature after immersion reaction 1h
Obtain the HKUST-1/CNT composite membranes that thickness is 3 times of self-supporting in embodiment 1.
Embodiment 6
Copper nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains Kocide SD nanowire dispersion after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 4mg
Dispersion mixing is uniform in water by certain mass ratio for Kocide SD nano wire and 8mg carbon nanotubes, in diameter 2cm in porous base
Filtered in matter, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting.By gained Kocide SD/CNT composite membranes immersion
In water/alcohol mixed solution of the trimesic acid of 20mM, solvent volume ratio is 1：1.Obtained at room temperature after immersion reaction 1h
Obtain the HKUST-1/CNT composite membranes that thickness is 4 times of self-supporting in embodiment 1.
Embodiment 7
Copper nitrate and ethylaminoethanol are uniformly mixed in the solution, immersion obtains Kocide SD nanowire dispersion after 2 days.
Single-wall carbon nanotubes is obtained into the negatively charged carbon nanotubes in surface for 1 day in nitric acid with heated oxide at 80 DEG C.By gained 5mg
Dispersion mixing is uniform in water by certain mass ratio for Kocide SD nano wire and 10mg carbon nanotubes, in diameter 2cm porous
Filtered in matrix, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting.By gained Kocide SD/CNT composite membranes leaching
For bubble in water/alcohol mixed solution of the trimesic acid of 20mM, solvent volume ratio is 1：1.At room temperature after immersion reaction 1h
Obtain the HKUST-1/CNT composite membranes that thickness is 5 times of self-supporting in embodiment 1.
Claims (1)
1. a kind of method for manufacturing self-supporting lithium sulfur battery anode material, includes the following steps：
The first step：Copper nitrate and ethylaminoethanol are uniformly mixed and soak aging in the solution and obtains Kocide SD nano wire within 2 days
Dispersion liquid；
Second step：Single-wall carbon nanotubes is obtained into the negatively charged nano-sized carbon in surface for 1 day in nitric acid with heated oxide at 80 DEG C
Pipe；By gained 1mg Kocide SDs nano wire and 2mg carbon nanotubes, by certain mass ratio, dispersion mixing is uniform in water, in diameter
Suction filtration, the dry Kocide SD/carbon nano-tube compound film for obtaining self-supporting on porous matrix of 2cm；
3rd step：Gained Kocide SD/CNT composite membranes are immersed in water/alcohol mixed solution of the trimesic acid of 20mM,
Solvent volume ratio is 1：1；At room temperature the HKUST-1/CNT composite membranes of self-supporting are obtained after immersion reaction 1h；
4th step：Sublimed sulfur is dissolved in CS2 under stirring at room temperature and obtains S/CS2 solution.Resulting solution is pressed into certain mass ratio
Add in gained HKUST-1/CNT composite membranes, at room temperature slowly after drying, heat treatment 8h is obtaining self-supporting just at 140 DEG C
Pole material HKUST-1/CNTS, as cell positive material.Sulphur carrying capacity is 1mg cm wherein on pole piece-2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600656A (en) * | 2019-09-12 | 2019-12-20 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery diaphragm material |
| CN111653729A (en) * | 2020-05-20 | 2020-09-11 | 佛山科学技术学院 | Lithium-sulfur battery composite positive electrode and preparation method thereof |
-
2016
- 2016-10-15 CN CN201610898880.8A patent/CN107958998A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110600656A (en) * | 2019-09-12 | 2019-12-20 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery diaphragm material |
| CN110600656B (en) * | 2019-09-12 | 2022-03-25 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery diaphragm material |
| CN111653729A (en) * | 2020-05-20 | 2020-09-11 | 佛山科学技术学院 | Lithium-sulfur battery composite positive electrode and preparation method thereof |
| CN111653729B (en) * | 2020-05-20 | 2022-03-25 | 佛山科学技术学院 | Lithium-sulfur battery composite positive electrode and preparation method thereof |
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Application publication date: 20180424 |