CN109449425A - A kind of preparation method of lithium-sulfur cell composite material and the application of the composite material - Google Patents
A kind of preparation method of lithium-sulfur cell composite material and the application of the composite material Download PDFInfo
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- CN109449425A CN109449425A CN201811379788.6A CN201811379788A CN109449425A CN 109449425 A CN109449425 A CN 109449425A CN 201811379788 A CN201811379788 A CN 201811379788A CN 109449425 A CN109449425 A CN 109449425A
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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
- H01M10/058—Construction or manufacture
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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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- 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
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- 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 belongs to the technical field of lithium-sulfur cell, the method for being related to preparing functional interlayer by active material, specifically a kind of lithium-sulfur cell use composite material preparation method and the composite material as lithium-sulfur cell functional interlayer application.It is a kind of technique using diamond heating to prepare iron phosphide/carbon cloth composite material (FeP/CC composite material).The FeP/CC composite material prepared not only accelerates the transmission rate of electronics and ion as lithium-sulfur cell with functional interlayer, promote redox reaction of the lithium-sulfur cell in charge and discharge process, polysulfide is adsorbed well simultaneously, it is suppressed that the shuttle effect of polysulfide.
Description
Technical field
The invention belongs to the technical field of lithium-sulfur cell, the method for being related to preparing functional interlayer by active material, specifically
It is preparation method and the composite material answering as lithium-sulfur cell functional interlayer that a kind of lithium-sulfur cell uses composite material that ground, which is said,
With.
Background technique
Lithium ion secondary battery because having many advantages, such as high working voltage, high-energy density, long-life and memory-less effect, at
For the preferred power supply of each electronic product.As electronic equipment further minimizes and electric car, large-scale energy-accumulating power station
Rapid development, more stringent requirements are proposed to its power supply by people.Existing lithium ion battery by theoretical specific capacity because being limited
It is difficult to meet people's demand, and there is very high theoretical energy density (2600Wh/kg) with the lithium-sulfur cell that sulphur makees anode, it is theoretical
Specific capacity reaches 1675mAh/g, and sulphur is cheap, resourceful, hypotoxicity, therefore becomes two of the high-energy density by favor
Primary cell system.
But lithium-sulfur cell still remains some critical problems, firstly, generated polysulfide ion in charge and discharge process
Li2Sx(x=3~8) can be dissolved in electrolyte and migrate, so that the effect that " shuttles " occur.The generation of " shuttle " effect, directly
The corrosion for connecing the loss and cathode of lithium that result in active material, makes circulating battery bad stability.In addition, elemental sulfur and its putting
The biggish volume change of anode, will lead to the specific discharge capacity of lithium-sulfur cell in the insulating properties of electric final product, charge and discharge process
Decline restricts the raising of lithium-sulfur cell performance.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of preparation method of lithium-sulfur cell composite material and this is multiple
Application of the condensation material as lithium-sulfur cell functional interlayer is a kind of technique using diamond heating to prepare iron phosphide/carbon
Cloth composite material (FeP/CC composite material).The FeP/CC composite material prepared as lithium-sulfur cell functional interlayer not only
The transmission rate for accelerating electronics and ion promotes redox reaction of the lithium-sulfur cell in charge and discharge process, while very
Good has adsorbed polysulfide, it is suppressed that the shuttle effect of polysulfide.
Technical scheme is as follows:
A kind of preparation method of lithium-sulfur cell composite material, the specific steps are as follows:
Step 1: ferroferric oxide/carbon cloth composite material (Fe3O4/ C/C composite) preparation:
It is respectively the Fe (NO of 20-50% by mass percent3)3·9H2The polyvinylpyrrolidone of O and 2.5-10%
(PVP) it is dissolved in DMF, then by preparing mixed solution in the case where temperature is 70-80 DEG C of being vigorously stirred, then at 20 DEG C
Under, with Dipcoat method on carbon cloth substrate deposition solution, and extra solution is removed, finally by modified carbon cloth in 600-
Sky heats solution 2-4 hours under conditions of 800 DEG C, obtains Fe3O4/ C/C composite.
Step 2: the preparation of iron phosphide/carbon cloth composite material (FeP/CC composite material):
Fe prepared by the first step3O4/ CC and NaHPO2It is respectively placed in two porcelain boats, the molar ratio of Fe and P are 1: 5-
20, then porcelain boat is placed in tube furnace, NaHPO is housed2Porcelain boat be positioned adjacent to be passed through one end of gas；Then,
Under an argon atmosphere by Fe3O4Then/CC naturally cools at room temperature in 300-400 DEG C of heating 2-4h, obtains iron phosphide/carbon cloth
Composite material.
Fe(NO3)3·9H2The mass ratio of O and polyvinylpyrrolidone is 1:1-1:2.
A kind of preparation method of above-mentioned lithium-sulfur cell FeP/CC composite material, related raw material pass through commercially available obtain
?.
Lithium-sulfur cell composite material of the invention is in lithium-sulfur cell as the application of functional interlayer.
Further preferably, the FeP/CC composite material of acquisition is finally cut into the disk of diameter 19mm by slitter
As lithium-sulfur cell functional interlayer.
Beneficial effects of the present invention are as follows:
(1) in design process of the invention, by the method for simple diamond heating, by iron phosphide nanometer particle film
It is grown on carbon cloth, realizes quick and continuous long range electron-transport, enhance dynamics of oxidation-reduction, it is suppressed that
The shuttle of polysulfide significantly improves the chemical property of lithium-sulfur cell.
(2) in design process of the invention, innovative proposing directly utilizes the carbon with excellent toughness and intensity
Carrier of the cloth as iron phosphide nanometer particle film, the stability of this functional interlayer design enhancing functional interlayer structure,
And mechanical compaction is not needed, it is easy to operate.
(3) FeP/CC composite material prepared by the method for the present invention is applied in lithium-sulfur cell functional interlayer, at 0.1C
The first charge-discharge specific capacity of battery reaches 1080mAh/g, with high discharge capacity and brilliant cyclical stability, electrochemistry
Performance is substantially better than the performance of lithium-sulfur cell without dissection.
In short, the present invention is modified lithium-sulfur cell, phosphatization iron dust as the functional interlayer of lithium-sulfur cell using FeP/CC
In transition metal phosphide, it is a kind of compound with satisfactory electrical conductivity, the transmission rate of electronics and ion can be accelerated, it is real
Now quick and continuous long range electron-transport, and there is efficient catalytic action, dynamics of oxidation-reduction is enhanced,
Redox reaction of the lithium-sulfur cell in charge and discharge process is promoted, polysulfide conversion reaction is conducive to, reduces vulcanization
The nucleation energy barrier surface of lithium, while iron phosphide has very strong chemical bonding effect to polysulfide, can be very good to adsorb more vulcanizations
Object inhibits the shuttle effect of polysulfide.Iron phosphide nanometer particle film is grown in carbon by simple diamond heating method
On cloth, carbon cloth has excellent flexibility and intensity as a kind of inexpensive and high electric conductivity textile, can be well
Play the role of supporting and fixing iron phosphide nanometer particle film, enhances the stability of functional interlayer structure, improve activity
The reuse ratio of material makes lithium-sulfur cell capacity boost, and enhances the stability of circulation.
Detailed description of the invention
Fig. 1 is iron phosphide/charge discharge of the carbon cloth composite material as lithium-sulfur cell interlayer obtained by embodiment 1
Curve.
Fig. 2 is high rate performance figure of the iron phosphide/carbon cloth composite material as lithium-sulfur cell interlayer obtained by embodiment 1.
Fig. 3 is Al obtained by comparative example2O3The charge discharge curve of/C/C composite as lithium-sulfur cell interlayer.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
Embodiment 1:
Step 1: Fe3O4The preparation of/C/C composite:
It is respectively 20% Fe (NO by mass percent3)3·9H2The PVP of O and 2.5% is dissolved in the mass ratio of 1:1
In the DMF of 20mL, then by being that (whole apparent velocity prepare at 0.2m/s or more) to be mixed for 70 DEG C be vigorously stirred in temperature
Close solution, then at 20 DEG C, with Dipcoat method on carbon cloth substrate deposition solution, and remove extra solution.Finally will
Modified carbon cloth sky under conditions of 600 DEG C heats solution 2 hours.
Step 2: the preparation of FeP/CC composite material:
Fe prepared by the first step3O4/ CC and NaHPO2It is respectively placed in two porcelain boats, the molar ratio of Fe and P are 1:
20, then porcelain boat is placed in tube furnace, NaHPO is housed2Porcelain boat be positioned adjacent to be passed through one end of gas.Then,
Under static argon atmosphere then sample is naturally cooled at room temperature in 300 DEG C of heating 2h.
Iron phosphide/the carbon cloth that finally will acquire cuts into the disk of diameter 19mm by slitter, uses as lithium-sulfur cell
Functional interlayer.
Fig. 1 is electrochemistry charge and discharge of the iron phosphide/carbon cloth composite material as lithium-sulfur cell interlayer obtained by the present embodiment
Electric curve.By the Fig. 1 as it can be seen that under 0.1C current density, the discharge capacity for the first time of the material is up to 1080mAh/g.
Fig. 2 is high rate performance figure of the iron phosphide/carbon cloth composite material as lithium-sulfur cell interlayer obtained by the present embodiment.
By the Fig. 2 as it can be seen that in different current density 0.1C, 0.5C, 1C, the specific capacity under 2C is respectively 1080mAh/g, 790mAh/g,
585mAh/g, 410mAh/g.
Embodiment 2:
Step 1: Fe3O4The preparation of/C/C composite:
It is respectively 25% Fe (NO by mass percent3)3·9H2The PVP of O and 5% is dissolved in the mass ratio of 1:2
In the DMF of 20mL, then by preparing mixed solution in the case where temperature is 80 DEG C of being vigorously stirred, then at 20 DEG C, with dipping
Rubbing method deposition solution on carbon cloth substrate, and remove extra solution.It is finally that modified carbon cloth is empty under conditions of 800 DEG C
Heat solution 4 hours.
Step 2: the preparation of FeP/CC composite material:
Fe prepared by the first step3O4/ CC and NaHPO2It is respectively placed in two porcelain boats, the molar ratio of Fe and P are 1:
20, then porcelain boat is placed in tube furnace, NaHPO is housed2Porcelain boat be positioned adjacent to be passed through one end of gas.Then,
Under static argon atmosphere then sample is naturally cooled at room temperature in 400 DEG C of heating 3h.The iron phosphide that finally will acquire/
Carbon cloth cuts into the disk of diameter 19mm by slitter.
Comparative example:
Step 1: Al2O3The preparation of/C/C composite:
Dry CC (diameter: 1/4 inch) is placed in atomic layer deposition system (BeNY-TFS 500), Al is used for2O3It is heavy
Product.Entire technique is carried out by carrier gas of 150 DEG C of High Purity Nitrogen, in order to keep the high conductivity of ACC as much as possible, is only carried out five times
ALD cycle, each circulation include the alternating flowing of trimethyl aluminium (TMA, 4s, Al precursor) and water (4s, oxidant), they pass through
Purity nitrogen air-flow (respectively 4s and 10s, carrier and clean gas) separation.Al can be obtained after the completion of deposition2O3/ CC composite wood
Material.
Fig. 3 is Al obtained by comparative example2O3The charge discharge curve of/C/C composite as lithium-sulfur cell interlayer.
It may be seen that the discharge capacity for the first time of the material reaches 890mAh/g, far below FeP/CC material under 0.1C current density
Discharge capacity for the first time.
Claims (4)
1. a kind of preparation method of lithium-sulfur cell composite material, the specific steps are as follows:
Step 1: ferroferric oxide/carbon cloth composite material (Fe3O4/ C/C composite) preparation:
It is respectively the Fe (NO of 20-50% by mass percent3)3·9H2The polyvinylpyrrolidone (PVP) of O and 2.5-10% dissolves
In DMF, then by preparing mixed solution in the case where temperature is 70-80 DEG C of being vigorously stirred, then at 20 DEG C, applied with dipping
Cloth method deposition solution on carbon cloth substrate, and extra solution is removed, finally by modified carbon cloth under conditions of 600-800 DEG C
Sky heats solution 2-4 hours, obtains Fe3O4/ C/C composite；
Step 2: the preparation of iron phosphide/carbon cloth composite material (FeP/CC composite material):
Fe prepared by the first step3O4/ CC and NaHPO2It being respectively placed in two porcelain boats, the molar ratio of Fe and P are 1: 5-20,
Then porcelain boat is placed in tube furnace, NaHPO is housed2Porcelain boat be positioned adjacent to be passed through one end of gas；Then, in argon
By Fe under gas atmosphere3O4Then/CC naturally cools at room temperature in 300-400 DEG C of heating 2-4h, it is compound to obtain iron phosphide/carbon cloth
Material.
2. the preparation method of lithium-sulfur cell composite material according to claim 1, which is characterized in that Fe (NO3)3·
9H2The mass ratio of O and polyvinylpyrrolidone is 1:1-1:2.
3. according to claim 1 or 2 obtained lithium-sulfur cells use composite material as the application of functional interlayer.
4. according to claim 1 or 2 obtained lithium-sulfur cells cut into the disk of diameter 19mm with composite material by slitter
As lithium-sulfur cell functional interlayer.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109920955A (en) * | 2019-04-05 | 2019-06-21 | 浙江理工大学 | A kind of cementite compound Nano carbon fiber film and preparation method thereof applied to lithium-sulfur cell interlayer |
| 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 |
| CN111477873A (en) * | 2020-04-14 | 2020-07-31 | 山东大学 | Lithium-sulfur battery conductive agent based on nano transition metal phosphide/carbon composite material and preparation method and application thereof |
| CN111483984A (en) * | 2020-04-21 | 2020-08-04 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| CN113130905A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof |
| CN113421990A (en) * | 2021-05-28 | 2021-09-21 | 西安理工大学 | Iron-based biomass carbon intermediate layer of lithium-sulfur battery, preparation method and lithium-sulfur battery |
| CN113937418A (en) * | 2021-10-11 | 2022-01-14 | 中科南京绿色制造产业创新研究院 | Lithium-sulfur battery diaphragm, preparation method thereof and lithium-sulfur battery |
| CN114447331A (en) * | 2021-12-16 | 2022-05-06 | 山东大学苏州研究院 | Biomass carbon source-based lithium-sulfur battery positive electrode composite material and preparation method and application thereof |
| CN115360478A (en) * | 2022-07-13 | 2022-11-18 | 南昌大学 | In-situ grown carbon nanotube type iron phosphate modified lithium-sulfur battery diaphragm and preparation method thereof, and lithium-sulfur battery |
| CN115377605A (en) * | 2022-08-22 | 2022-11-22 | 成都大学 | Hollow metal oxide-metal phosphide heterojunction material and preparation method and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109920955A (en) * | 2019-04-05 | 2019-06-21 | 浙江理工大学 | A kind of cementite compound Nano carbon fiber film and preparation method thereof applied to lithium-sulfur cell interlayer |
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| CN111477873A (en) * | 2020-04-14 | 2020-07-31 | 山东大学 | Lithium-sulfur battery conductive agent based on nano transition metal phosphide/carbon composite material and preparation method and application thereof |
| CN111483984A (en) * | 2020-04-21 | 2020-08-04 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery positive electrode material |
| CN113130905A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Ultra-small cobalt sulfide nanosheet/carbon cloth composite material and preparation method thereof |
| CN113421990A (en) * | 2021-05-28 | 2021-09-21 | 西安理工大学 | Iron-based biomass carbon intermediate layer of lithium-sulfur battery, preparation method and lithium-sulfur battery |
| CN113937418A (en) * | 2021-10-11 | 2022-01-14 | 中科南京绿色制造产业创新研究院 | Lithium-sulfur battery diaphragm, preparation method thereof and lithium-sulfur battery |
| CN113937418B (en) * | 2021-10-11 | 2023-11-17 | 中科南京绿色制造产业创新研究院 | Lithium-sulfur battery diaphragm, preparation method thereof and lithium-sulfur battery |
| CN114447331A (en) * | 2021-12-16 | 2022-05-06 | 山东大学苏州研究院 | Biomass carbon source-based lithium-sulfur battery positive electrode composite material and preparation method and application thereof |
| CN115360478A (en) * | 2022-07-13 | 2022-11-18 | 南昌大学 | In-situ grown carbon nanotube type iron phosphate modified lithium-sulfur battery diaphragm and preparation method thereof, and lithium-sulfur battery |
| CN115360478B (en) * | 2022-07-13 | 2024-03-29 | 南昌大学 | In-situ growth carbon nanotube type ferric phosphate modified lithium sulfur battery diaphragm, preparation method thereof and lithium sulfur battery |
| CN115377605A (en) * | 2022-08-22 | 2022-11-22 | 成都大学 | Hollow metal oxide-metal phosphide heterojunction material and preparation method and application thereof |
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