CN108511706A - A kind of preparation method of lithium battery Two-dimensional Inorganic perovskite negative material - Google Patents
A kind of preparation method of lithium battery Two-dimensional Inorganic perovskite negative material Download PDFInfo
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- CN108511706A CN108511706A CN201810204709.1A CN201810204709A CN108511706A CN 108511706 A CN108511706 A CN 108511706A CN 201810204709 A CN201810204709 A CN 201810204709A CN 108511706 A CN108511706 A CN 108511706A
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- lithium battery
- inorganic perovskite
- dimensional inorganic
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- perovskite negative
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/582—Halogenides
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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 invention discloses a kind of lithium battery preparation methods of Two-dimensional Inorganic perovskite negative material, include the following steps：N, N dimethylformamides is added in lead bromide, cesium bromide, heating stirring is passed through protective gas in whipping process, obtains mixed material；Mixed material is dried in vacuo to obtain forerunner's material；Toluene is added in forerunner's material, is centrifuged, centrifugation obtained solid object is dried in vacuo to obtain lithium battery Two-dimensional Inorganic perovskite negative material.The preparation method of lithium battery proposed by the present invention Two-dimensional Inorganic perovskite negative material, using simple one-step synthesis technique, by simply dissolving, extraction process, it can obtain the perovskite material of high-purity high crystalline, solve conventional lithium cell cathode material need to be graphitized under the high temperature conditions, the preparation processes such as carbon coating it is complicated, the higher problem of cost.
Description
Technical field
It is negative with Two-dimensional Inorganic perovskite that the present invention relates to lithium cell cathode material technical fields more particularly to a kind of lithium battery
The preparation method of pole material.
Background technology
Cathode material of lithium ion battery mainly uses graphite-like carbon negative pole material, and raw material sources are extensive, price is relatively low,
Electrochemistry cycle performance is excellent, has become the commercialized main material of field of lithium especially power battery industry.But
It is that graphite-like carbon negative pole material theoretical specific capacity (372mAh/g) is relatively low, it is poor and in charge and discharge process with the compatibility of solvent
In be easy to happen the precipitation of Li dendrite, battery short circuit is caused, to influence the safety of battery.And the silicium cathode material proposed in recent years
Material, although its have very high theoretical specific capacity, lower removal lithium embedded current potential, the advantages such as low with electrolyte reactivity,
There are this serious volume expansion in charge and discharge process, 300-400% is reached as high as, cathode particle is be easy to cause and falls off, to
Substantially reduce the cyclical stability of battery.
Currently, common negative electrode of lithium ion battery is mainly graphite cathode, carbon coating graphite cathode and silicon-carbon cathode material
Material etc., because of techniques such as its preparation process needs to be graphitized under the high temperature conditions, carbon coatings so that preparation process is complicated, at
This is higher.
Invention content
Technical problems based on background technology, the present invention propose a kind of lithium battery Two-dimensional Inorganic perovskite cathode
The preparation method of material solves current lithium ion battery negative material and needs to be graphitized under the high temperature conditions and carbon coating etc.
Preparation process complexity, the higher problem of cost.
A kind of preparation method of lithium battery Two-dimensional Inorganic perovskite negative material proposed by the present invention, including following step
Suddenly：
S1, n,N-Dimethylformamide is added in lead bromide, cesium bromide, heating stirring is passed through protection gas in whipping process
Body obtains mixed material；
S2, mixed material is dried in vacuo to obtain forerunner's material；
S3, toluene is added in forerunner's material, centrifuged, centrifugation obtained solid object is dried in vacuo to obtain lithium battery two dimension
Inorganic perovskite negative material.
Preferably, in S1, lead bromide, cesium bromide molar ratio be 2：1.
Preferably, in S1, the temperature of heating stirring is 68-72 DEG C, and the time of heating stirring is 2-3h.
Preferably, in S1, protective gas is one or more of nitrogen, neon, argon gas composition.
Preferably, in S2, vacuum drying temperature is 78-82 DEG C, vacuum drying time 11-13h.
Preferably, in S2, forerunner's material is white.
Preferably, in S3, vacuum drying temperature is 68-72 DEG C, vacuum drying time 1.5-2.5h.
Preferably, in S3, it is 3 times to centrifuge number.
Preferably, in S3, lithium battery is CsPb with Two-dimensional Inorganic perovskite negative material2Br5Or CsPb2Br5-CsPbBr3
Mixed phase.
The present invention uses the method that solwution method prepares lithium ion battery perovskite negative material, using lead bromide and bromination
Caesium is reacted in organic solvent, by regulating and controlling ratio and the reaction time of reactant, is prepared with two-dimensional layered structure
Inorganic perovskite material, and the new function material of physical and chemical performance with good stability and excellent.
The present invention utilizes the principle of chemical solution synthesis, using simple one-step synthesis technique, with lead bromide and cesium bromide
For precursor material, by extracting, being centrifugally separating to obtain Two-dimensional Inorganic perovskite material, it is proposed that a kind of novel lithium cell negative pole material
Material.
The present invention solve conventional lithium cell cathode material need to be graphitized under the high temperature conditions, the preparations such as carbon coating
Complex process, the higher problem of cost.
Description of the drawings
Fig. 1 is the crystal structure figure of present invention gained lithium battery Two-dimensional Inorganic perovskite negative material.
Fig. 2 is the SEM surface topographies of present invention gained lithium battery Two-dimensional Inorganic perovskite negative material.
Fig. 3 is the XRD diagram of present invention gained lithium battery Two-dimensional Inorganic perovskite negative material.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1, it is 2 in molar ratio by lead bromide, cesium bromide：1 is added n,N-Dimethylformamide, is heated to 68 DEG C, stirring
3h is passed through nitrogen in whipping process, obtains mixed material；
S2, mixed material is carried out to vacuum drying 11h, vacuum drying temperature is 82 DEG C, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 1.5h, vacuum drying
Temperature is 72 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Embodiment 2
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1, it is 2 in molar ratio by lead bromide, cesium bromide：1 is added n,N-Dimethylformamide, is heated to 72 DEG C, stirring
2h is passed through argon gas in whipping process, obtains mixed material；
S2, mixed material is carried out to vacuum drying 13h, vacuum drying temperature is 78 DEG C, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 2.5h, vacuum drying
Temperature is 68 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Embodiment 3
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1, it is 2 in molar ratio by lead bromide, cesium bromide：1 is placed in three neck beakers, and 1mL N, N- dimethyl formyls are added
Amine is heated to 70 DEG C, stirs 2.5h, the mixed gas of nitrogen and neon is passed through to avoid the shadow of humidity in air in whipping process
It rings, obtains mixed material；
S2, mixed material is poured into clean beaker, is placed in vacuum drying chamber, vacuum drying temperature is 80 DEG C, very
Empty drying time is 12h, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 2h, vacuum drying temperature
Degree is 70 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Embodiment 4
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1,2mol lead bromides are placed in three neck beakers, are subsequently added into 1mL n,N-Dimethylformamide, are heated to 70
DEG C, stirring makes it fully dissolve, and adding 1mol cesium bromides, the reaction was continued, and entire reaction process continues 2.5h, obtains mixture
Material is continually fed into the mixed gas of nitrogen and argon gas, avoids the influence of humidity in air in stirring and reaction process；
S2, mixed material is poured into clean beaker, is placed in vacuum drying chamber, vacuum drying temperature is 80 DEG C, very
Empty drying time is 12h, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 2h, vacuum drying temperature
Degree is 70 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Embodiment 5
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1,1mol cesium bromides are placed in three neck beakers, are subsequently added into 1mL n,N-Dimethylformamide, are heated to 70
DEG C, stirring makes it fully dissolve, and adding 2mol lead bromides, the reaction was continued, and entire reaction process continues 2.5h, obtains mixture
Material is continually fed into the mixed gas of neon and argon gas, avoids the influence of humidity in air in stirring and reaction process；
S2, mixed material is poured into clean beaker, is placed in vacuum drying chamber, vacuum drying temperature is 80 DEG C, very
Empty drying time is 12h, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 2h, vacuum drying temperature
Degree is 70 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Embodiment 6
A kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, includes the following steps：
S1, it is 2 in molar ratio by lead bromide, cesium bromide：1 mixing, is placed in mortar and grinds 0.5h, is subsequently placed in three necks burning
In cup, 1mL n,N-Dimethylformamide is added, is heated to 70 DEG C, stirs 2.5h, neon is passed through to avoid sky in whipping process
The influence of humidity, obtains mixed material in gas；
S2, mixed material is poured into clean beaker, is placed in vacuum drying chamber, vacuum drying temperature is 80 DEG C, very
Empty drying time is 12h, obtains white forerunner's material；
S3, toluene is added in forerunner's material, centrifuged 3 times, centrifugation obtained solid object is dried in vacuo 2h, vacuum drying temperature
Degree is 70 DEG C, obtains lithium battery Two-dimensional Inorganic perovskite negative material.
Referring to Fig.1, Fig. 1 is the crystal structure figure of lithium battery Two-dimensional Inorganic perovskite negative material obtained by the present embodiment.
It is the SEM surface topographies of lithium battery Two-dimensional Inorganic perovskite negative material obtained by the present embodiment with reference to Fig. 2, Fig. 2.
It is the XRD diagram of lithium battery Two-dimensional Inorganic perovskite negative material obtained by the present embodiment with reference to Fig. 3, Fig. 3.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of lithium battery preparation method of Two-dimensional Inorganic perovskite negative material, which is characterized in that include the following steps：
S1, n,N-Dimethylformamide is added in lead bromide, cesium bromide, heating stirring is passed through protective gas in whipping process, obtains
To mixed material；
S2, mixed material is dried in vacuo to obtain forerunner's material；
S3, toluene is added in forerunner's material, centrifuged, centrifugation obtained solid object is dried in vacuo to obtain lithium battery Two-dimensional Inorganic
Perovskite negative material.
2. the preparation method of lithium battery Two-dimensional Inorganic perovskite negative material according to claim 1, which is characterized in that S1
In, lead bromide, cesium bromide molar ratio be 2：1.
3. the lithium battery according to claim 1 or claim 2 preparation method of Two-dimensional Inorganic perovskite negative material, feature exist
In in S1, the temperature of heating stirring is 68-72 DEG C, and the time of heating stirring is 2-3h.
4. special according to the preparation method of any one of claim 1-3 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S1, protective gas is one or more of nitrogen, neon, argon gas composition.
5. special according to the preparation method of any one of claim 1-4 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S2, vacuum drying temperature is 78-82 DEG C, vacuum drying time 11-13h.
6. special according to the preparation method of any one of claim 1-5 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S2, forerunner's material is white.
7. special according to the preparation method of any one of claim 1-6 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S3, vacuum drying temperature is 68-72 DEG C, vacuum drying time 1.5-2.5h.
8. special according to the preparation method of any one of claim 1-7 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S3, it is 3 times to centrifuge number.
9. special according to the preparation method of any one of claim 1-8 lithium battery Two-dimensional Inorganic perovskite negative materials
Sign is, in S3, lithium battery is CsPb with Two-dimensional Inorganic perovskite negative material2Br5Or CsPb2Br5-CsPbBr3Mixed phase.
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| CN109361014A (en) * | 2018-09-12 | 2019-02-19 | 北京理工大学 | A kind of lithium secondary battery solid state electrolysis composite material, preparation method and lithium secondary battery |
| CN109786718A (en) * | 2019-01-30 | 2019-05-21 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of inorganic perovskite cladding MXene two-dimensional layer negative electrode material |
| CN110950375A (en) * | 2019-12-02 | 2020-04-03 | 山东省分析测试中心 | CsPb2Br5Middle doped CsPbBr3Composite perovskite material and preparation method and application thereof |
| CN111384361A (en) * | 2018-12-29 | 2020-07-07 | 北京大学 | Two-dimensional organic perovskite lithium ion battery electrode and preparation method thereof |
| CN112234190A (en) * | 2020-10-14 | 2021-01-15 | 中国计量大学 | Lead-based negative electrode material |
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| CN111384361A (en) * | 2018-12-29 | 2020-07-07 | 北京大学 | Two-dimensional organic perovskite lithium ion battery electrode and preparation method thereof |
| CN111384361B (en) * | 2018-12-29 | 2021-08-20 | 北京大学 | Two-dimensional organic perovskite lithium ion battery electrode and preparation method thereof |
| CN109786718A (en) * | 2019-01-30 | 2019-05-21 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of inorganic perovskite cladding MXene two-dimensional layer negative electrode material |
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| CN110950375A (en) * | 2019-12-02 | 2020-04-03 | 山东省分析测试中心 | CsPb2Br5Middle doped CsPbBr3Composite perovskite material and preparation method and application thereof |
| CN110950375B (en) * | 2019-12-02 | 2022-03-15 | 山东省分析测试中心 | CsPb2Br5Middle doped CsPbBr3Composite perovskite material and preparation method and application thereof |
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Application publication date: 20180907 |