CN106981634A - A kind of polypyrrole/Ti3C2Tx/ sulphur composite - Google Patents
A kind of polypyrrole/Ti3C2Tx/ sulphur composite Download PDFInfo
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- CN106981634A CN106981634A CN201710230128.0A CN201710230128A CN106981634A CN 106981634 A CN106981634 A CN 106981634A CN 201710230128 A CN201710230128 A CN 201710230128A CN 106981634 A CN106981634 A CN 106981634A
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- sulphur
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- polypyrrole
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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
- H01M4/366—Composites as layered products
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
Abstract
The present invention provides a kind of polypyrrole/Ti3C2Tx/ sulphur composite, the composite is by sulphur, sheet Ti3C2TxWith polypyrrole composition, internal layer is sulphur and Ti3C2TxComposite, outer layer is cladding sulphur and Ti3C2TxThe polypyrrole of composite, its polypyrrole：Ti3C2Tx：The mass ratio of sulphur is 0.05 0.2:0.05‑0.2:1.Clad polypyrrole can carry out physical protection to sulfenyl material in composite, and the polysulfide that limitation charge and discharge process is produced is inside polypyrrole, so as to reduce shuttle effect；The composite limits the movement of polysulfide, the effective life-span for improving lithium-sulfur cell simultaneously in terms of physics confinement and chemisorbed two.
Description
Technical field
The present invention relates to nano material synthesis, more particularly to a kind of preparation method of lithium sulfur battery anode material.
Background technology
Lithium-sulfur cell is that, using lithium metal as negative pole, elemental sulfur is the battery system of positive pole.Lithium-sulfur cell have two put
Level platform（About 2.4 V and 2.1 V）, but its electrochemical reaction mechanism is more complicated.Lithium-sulfur cell has specific energy high
（2600 Wh/kg）, specific capacity it is high（1675 mAh/g）, low cost and other advantages, it is considered to be very promising a new generation's electricity
Pond.But at present the problems such as there is low active material utilization, low cycle life and poor security, this seriously governs lithium
The development of sulphur battery.Causing the main cause of above mentioned problem has the following aspects：（1）Elemental sulfur is electronics and ion insulation
Body, room-temperature conductivity is low（5×10-30S·cm-1）, because the sulphur without ionic state is present, thus it is tired as positive electrode activation
It is difficult；（2）The high poly- many lithium sulfide Li of state produced in electrode process2Sn（8 ＞ n >=4）It is soluble in electrolyte, positive and negative
Concentration difference is formed between pole, negative pole is moved in the presence of concentration gradient, the high poly- many lithium sulfides of state are reduced into low by lithium metal
The poly- many lithium sulfides of state.The progress of reaction more than, the oligomeric many lithium sulfides of state are assembled in negative pole, finally formed between electrodes
Concentration difference, moves to positive pole and is oxidized to the high many lithium sulfides of poly- state again.This phenomenon is referred to as shuttle effect, reduces sulphur activity
The utilization rate of material.While insoluble Li2S and Li2S2Cathode of lithium surface is deposited on, lithium-sulfur cell is further degrading
Performance；（3）React final product Li2S is equally electronic body, can be deposited on sulfur electrode, and lithium ion vulcanizes in solid-state
Migration velocity is slow in lithium, makes electrochemical reaction kinetic rate slack-off；（4）Sulphur and final product Li2S density is different, works as sulphur
Rear volumetric expansion about 79% is lithiated, Li is easily caused2S efflorescence, causes the safety problem of lithium-sulfur cell.Above-mentioned not enough restriction
The development of lithium-sulfur cell, this is also the Important Problems that current lithium-sulfur cell research needs to solve.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of polypyrrole/Ti3C2Tx/ sulphur composite, the composite
Material is by sulphur, sheet Ti3C2TxConstitute, polypyrrole with good conductivity provides conductive network, gather simultaneously with the polypyrrole of external sheath
The cladding limitation sulfenyl material of pyrroles is moved freely, sheet Ti3C2TxTitanium can adsorb the dissolving of discharging product polysulfide, carry
The chemical property of high material.
The present invention provides a kind of polypyrrole/Ti3C2Tx/ sulphur composite, the composite is by sulphur, sheet Ti3C2TxWith it is poly-
Pyrroles constitutes, and internal layer is sulphur and Ti3C2TxComposite, outer layer is cladding sulphur and Ti3C2TxThe polypyrrole of composite, its poly- pyrrole
Cough up：Ti3C2Tx：The mass ratio of sulphur is 0.05-0.2:0.05-0.2:1.
The present invention provides a kind of polypyrrole/Ti3C2TxThe preparation method of/sulphur composite is as follows：
（1）By Ti3AlC2Ceramic powders, which are put into hydrofluoric acid, to be corroded, and solution adds deionized water and carries out centrifugal treating after corrosion,
Then sediment is dried, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By Ti3C2TxPowder and elemental sulfur in proportion 1:1 uniform mixing, is positioned in sealed reactor, in nitrogen
Heating response is to 155 °C in atmosphere, and constant temperature 5-12h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite wood
Material；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds pyrroles's stirring, then adds initiator mistake
Ammonium sulfate, stirring, standing, filtering, vacuum drying, obtains polypyrrole/Ti3C2Tx/ sulphur composite.
Step（1）The concentration of middle hydrofluoric acid is 20%-50%, and the time of corrosion is 4-24 hours;
Step（2）Middle Ti3C2TxThe mass ratio of powder and elemental sulfur is 0.05-0.2:1, heating response temperature is 155-165 DEG C,
Time is 5-12 hours;
Step（3）The ratio of middle pyrroles and elemental sulfur is 0.05-0.2:1；The ratio of initiator and pyrroles are 1：0.01-0.1, draws
Send out one kind that agent is selected in azodiisobutyronitrile, dibenzoyl peroxide, ammonium persulfate；
The present invention has the advantages that：Polypyrrole/Ti3C2TxTi in/sulphur composite3C2TxOn T for-F groups or
- OH groups, are highly polar group, and strong chemisorbed can be formed to the polysulfide formed in charge and discharge process, can be effective
Prevention polysulfide through barrier film reach negative pole；Clad polypyrrole can carry out physics to sulfenyl material in composite simultaneously
Protection, the polysulfide that limitation charge and discharge process is produced is inside polypyrrole, so as to reduce shuttle effect；The composite is from thing
Manage the movement that two aspects of confinement and chemisorbed limit polysulfide simultaneously, the effective life-span for improving lithium-sulfur cell.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is the charge-discharge performance figure of composite of the present invention.
Embodiment
Below in conjunction with the accompanying drawings, the preferably embodiment to the present invention is described in further detail：
Embodiment 1
（1）By Ti3AlC2Ceramic powders, which are put into the hydrofluoric acid that mass concentration is 20%, corrodes solution addition after 24h, corrosion
Deionized water carries out centrifugal treating, then dries sediment, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By 0.5g Ti3C2TxPowder is uniformly mixed with 10g elemental sulfurs, is positioned in sealed reactor, in the atmosphere of nitrogen
Middle heating response is to 155 °C, and constant temperature 12h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds 0.5g pyrroles's stirring, then adds 0.05g
Initiator azodiisobutyronitrile, stirring, standing, filtering, vacuum drying, obtains polypyrrole/Ti3C2Tx/ sulphur composite.
Embodiment 2
（1）By Ti3AlC2Ceramic powders are put into mass concentration and gone to corrode solution addition after 4h, corrosion in 50% hydrofluoric acid
Ionized water carries out centrifugal treating, then dries sediment, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By 2g Ti3C2TxPowder is uniformly mixed with 10g elemental sulfurs, is positioned in sealed reactor, in the atmosphere of nitrogen
Heating response is to 165 °C, and constant temperature 5h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds 2g pyrroles's stirring, then adds 0.02g and draws
Agent dibenzoyl peroxide is sent out, stirring, standing, filtering, vacuum drying obtain polypyrrole/Ti3C2Tx/ sulphur composite.
Embodiment 3
（1）By Ti3AlC2Ceramic powders, which are put into the hydrofluoric acid that mass concentration is 30%, corrodes solution addition after 20h, corrosion
Deionized water carries out centrifugal treating, then dries sediment, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By 1g Ti3C2TxPowder is uniformly mixed with 10g elemental sulfurs, is positioned in sealed reactor, in the atmosphere of nitrogen
Heating response is to 160 °C, and constant temperature 10h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds 1g pyrroles's stirring, then adds 0.05g and draws
Agent ammonium persulfate is sent out, stirring, standing, filtering, vacuum drying obtain polypyrrole/Ti3C2Tx/ sulphur composite.
Embodiment 4
（1）By Ti3AlC2Ceramic powders, which are put into the hydrofluoric acid that mass concentration is 40%, corrodes solution addition after 15h, corrosion
Deionized water carries out centrifugal treating, then dries sediment, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By 1.5g Ti3C2TxPowder is uniformly mixed with 10g elemental sulfurs, is positioned in sealed reactor, in the atmosphere of nitrogen
Middle heating response is to 162 °C, and constant temperature 8h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds 1.5g pyrroles's stirring, then adds 0.08g
Initiator azodiisobutyronitrile, stirring, standing, filtering, vacuum drying, obtains polypyrrole/Ti3C2Tx/ sulphur composite.
Embodiment 5
（1）By Ti3AlC2Ceramic powders, which are put into the hydrofluoric acid that mass concentration is 35%, corrodes solution addition after 13h, corrosion
Deionized water carries out centrifugal treating, then dries sediment, obtains the lamellar Ti of stacking3C2TxPowder；
（2）By 0.8g Ti3C2TxPowder is uniformly mixed with 10g elemental sulfurs, is positioned in sealed reactor, in the atmosphere of nitrogen
Middle heating response is to 157 °C, and constant temperature 9h is cooled to room temperature after the completion of reaction, obtains Ti3C2Tx/ sulphur composite；
（3）By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds 0.8g pyrroles's stirring, then adds 0.03g
Initiator dibenzoyl peroxide, stirring, standing, filtering, vacuum drying, obtains polypyrrole/Ti3C2Tx/ sulphur composite.
The preparation and performance test of electrode；By composite, acetylene black and PVDF in mass ratio 80：10：10 in NMP
Mixing, it is electrode film to be coated on aluminium foil, and metal lithium sheet is that, to electrode, CELGARD 2400 is barrier film, 1mol/L LiTFSI/
DOL-DME (volume ratios 1:1) it is electrolyte, 1mol/L LiNO3 is additive, button electricity is assembled into full of Ar glove boxes
Pond, constant current charge-discharge test is carried out using Land battery test systems.Charging/discharging voltage scope is 1-3V, and current density is
0.2C, performance is as shown in table 1.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| First discharge specific capacity（mAh/g） | 1052 | 1050 | 1048 | 1048 | 1053 |
Fig. 2 is the charge-discharge performance figure that the composite of the embodiment of the present invention 1 is prepared into lithium-sulfur cell.As can be seen from the figure charge and discharge
Electrical efficiency can reach more than 98%, and first charge-discharge capacity is 1052 mAh/g, and efficiency for charge-discharge is 98.1%, 500 charge and discharges
After electricity circulation, capacity still possesses 71.3%, illustrates the structure of the composite and can effectively suppress shuttle effect, improves sulphur battery
Life-span.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (5)
1. a kind of polypyrrole/Ti3C2Tx/ sulphur composite, it is characterised in that the composite is by sulphur, sheet Ti3C2TxWith poly- pyrrole
Composition is coughed up, internal layer is sulphur and Ti3C2TxComposite, outer layer is cladding sulphur and Ti3C2TxThe polypyrrole of composite, its poly- pyrrole
Cough up：Ti3C2Tx：The mass ratio of sulphur is 0.05-0.2:0.05-0.2:1.
2. one kind prepares the method as described in claim 1, it is characterised in that including following steps：
Step（1）：By Ti3AlC2Ceramic powders, which are put into hydrofluoric acid, to be corroded, and solution adds deionized water and centrifuged after corrosion
Processing, then sediment is dried, obtain the lamellar Ti of stacking3C2TxPowder；
Step（2）：By Ti3C2TxPowder is uniformly mixed in proportion with elemental sulfur, is positioned in sealed reactor, in nitrogen
Room temperature is cooled to after the completion of heating response in atmosphere, constant temperature, reaction, Ti is obtained3C2Tx/ sulphur composite；
Step（3）：By obtained Ti3C2Tx/ sulphur composite is added to the water stirring, adds pyrroles's stirring, then adds and triggers
Agent ammonium persulfate, stirring, standing, filtering, vacuum drying, obtains polypyrrole/Ti3C2Tx/ sulphur composite.
3. method as claimed in claim 2, it is characterised in that the step（1）The concentration of middle hydrofluoric acid is 20%-50%, rotten
The time of erosion is 4-24 hours.
4. method as claimed in claim 2, it is characterised in that the step（2）Middle Ti3C2TxThe quality of powder and elemental sulfur
Than for 0.05-0.2:1, heating response temperature is 155-165 DEG C, and the time is 5-12 hours.
5. method as claimed in claim 2, it is characterised in that the step（3）The ratio of middle pyrroles and elemental sulfur is 0.05-
0.2:1；The ratio of initiator and pyrroles are 1：0.01-0.1, initiator selects azodiisobutyronitrile, dibenzoyl peroxide, mistake
One kind in ammonium sulfate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710230128.0A CN106981634A (en) | 2017-04-10 | 2017-04-10 | A kind of polypyrrole/Ti3C2Tx/ sulphur composite |
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| CN201710230128.0A CN106981634A (en) | 2017-04-10 | 2017-04-10 | A kind of polypyrrole/Ti3C2Tx/ sulphur composite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878838A (en) * | 2018-06-29 | 2018-11-23 | 北京理工大学 | In the method for hollow sulphur ball surface cladding polypyrrole |
| CN109473646A (en) * | 2018-10-30 | 2019-03-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method and application of sulphur-polypyrrole-two-dimensional layer carbonization titanium composite material |
| CN110620235A (en) * | 2019-09-16 | 2019-12-27 | 安徽师范大学 | Polypyrrole-coated hollow porous cobalt manganate-loaded sulfur composite material, preparation method thereof, lithium-sulfur battery positive electrode and lithium-sulfur battery |
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| CN105098162A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Preparation method for titanium carbide nanosheet/graphene composite material capable of being used as anode of lithium ion battery |
| CN105633376A (en) * | 2016-02-18 | 2016-06-01 | 钟玲珑 | Preparation method of graphene/polypyrrole/sulfur composite anode material |
| CN105869910A (en) * | 2016-05-31 | 2016-08-17 | 陕西科技大学 | Composite material MoO3/Polyaniline/Ti3C2Tx and preparation method thereof |
| CN106450205A (en) * | 2016-11-02 | 2017-02-22 | 南京工业大学 | Two-dimensional transition metal carbide (nitride) and nano sulfur particulate composite as well as preparation and application thereof |
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2017
- 2017-04-10 CN CN201710230128.0A patent/CN106981634A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105098162A (en) * | 2015-09-14 | 2015-11-25 | 哈尔滨工业大学 | Preparation method for titanium carbide nanosheet/graphene composite material capable of being used as anode of lithium ion battery |
| CN105633376A (en) * | 2016-02-18 | 2016-06-01 | 钟玲珑 | Preparation method of graphene/polypyrrole/sulfur composite anode material |
| CN105869910A (en) * | 2016-05-31 | 2016-08-17 | 陕西科技大学 | Composite material MoO3/Polyaniline/Ti3C2Tx and preparation method thereof |
| CN106450205A (en) * | 2016-11-02 | 2017-02-22 | 南京工业大学 | Two-dimensional transition metal carbide (nitride) and nano sulfur particulate composite as well as preparation and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878838A (en) * | 2018-06-29 | 2018-11-23 | 北京理工大学 | In the method for hollow sulphur ball surface cladding polypyrrole |
| CN109473646A (en) * | 2018-10-30 | 2019-03-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method and application of sulphur-polypyrrole-two-dimensional layer carbonization titanium composite material |
| CN109473646B (en) * | 2018-10-30 | 2022-02-22 | 肇庆市华师大光电产业研究院 | Preparation method and application of sulfur-polypyrrole-two-dimensional layered titanium carbide composite material |
| CN110620235A (en) * | 2019-09-16 | 2019-12-27 | 安徽师范大学 | Polypyrrole-coated hollow porous cobalt manganate-loaded sulfur composite material, preparation method thereof, lithium-sulfur battery positive electrode and lithium-sulfur battery |
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