CN108682791A - A kind of method that vapor phase method prepares the inorganic perovskite negative material of layer structure - Google Patents

A kind of method that vapor phase method prepares the inorganic perovskite negative material of layer structure Download PDF

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CN108682791A
CN108682791A CN201810246688.XA CN201810246688A CN108682791A CN 108682791 A CN108682791 A CN 108682791A CN 201810246688 A CN201810246688 A CN 201810246688A CN 108682791 A CN108682791 A CN 108682791A
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negative material
vapor phase
bromide
layer structure
inorganic perovskite
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CN108682791B (en
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周皖岳
童国庆
王双双
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0421—Methods of deposition of the material involving vapour deposition
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • 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
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
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  • Battery Electrode And Active Subsutance (AREA)
  • Physical Vapour Deposition (AREA)
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Abstract

The invention discloses a kind of methods that vapor phase method prepares the inorganic perovskite negative material of layer structure, it is related to lithium ion battery negative material preparing technical field, it is under vacuum, lead bromide, cesium bromide are sequentially or simultaneously deposited to by vapor phase method in copper foil substrate, again in air heating anneal to get.The present invention is according to the principle of physical vapour deposition (PVD) and chemical vapor deposition, using inorganic lead bromide and cesium bromide as raw material, it is deposited into copper foil substrate surface by heating evaporation, and by regulating and controlling evaporation rate, deposition thickness and thickness proportion, and handled through subsequent anneal, the purely inorganic perovskite material of dense uniform is prepared, lithium ion battery negative material is used it for, good thermodynamic stability and excellent physical and chemical performance are shown, it is simple for process.

Description

A kind of method that vapor phase method prepares the inorganic perovskite negative material of layer structure
Technical field
The present invention relates to lithium ion battery negative material preparing technical fields more particularly to a kind of vapor phase method to prepare stratiform knot The method of the inorganic perovskite negative material of structure.
Background technology
It is also increasingly severe to the dependence of fossil energy with the continuous development and progress of human society.With coal, oil Problem of environmental pollution is increasingly serious caused by exhaustion and utilization in the process Deng the fossil energy for representative.Therefore, it sends out It is extremely urgent to open up novel renewable and clean energy resource, and was obtained in recent years as the novel renewable energy of representative using solar energy, wind energy Sufficient development and utilization are arrived.But how efficiently to realize energy conversion and storage, it is always focus of people's attention. Lithium ion battery many advantages, such as because of its higher operating voltage, higher energy storage density, longer cycle life, is answered extensively It is energy-saving and environment-friendly new especially under the dual-pressure of the energy and environment in electronic product, power battery, energy-storage system Energy automobile is stepping into market, and fast-developing.But cost how is reduced, improve energy density and cycle performance one It is directly the emphasis studied both at home and abroad.
Common cathode material of lithium ion battery mainly based on graphite cathode, because of it with good cycle performance and Material easily obtains, and storage capacity is big, has been widely used in electronic consumer products and power battery field.But low theoretical specific volume Amount, high-rate discharge ability difference and removal lithium embedded current potential and the close easy precipitation lithium of lithium current potential form Li dendrite, to cause short circuit The shortcomings of will restrict its low cost, high-energy density application.Currently, commercialized negative material includes mainly graphite Particle, carbon coating graphite particle cathode and the compound material etc. of silicon-carbon.Since the negative materials such as graphite are needed in hot conditions The techniques such as lower carry out graphitization processing, and follow-up cladding so that production process is complex and costly for preparation.
Invention content
Technical problems based on background technology, the present invention propose a kind of vapor phase method preparation layer structure inorganic calcium titanium The method of mine negative material, simple for process, the material of preparation has good thermodynamic stability and excellent physical chemistry Performance.
The method that a kind of vapor phase method proposed by the present invention prepares the inorganic perovskite negative material of layer structure, is in vacuum item Under part, lead bromide, cesium bromide are sequentially or simultaneously deposited to by vapor phase method in copper foil substrate, then heating anneal in air, To obtain the final product.
Preferably, include the following steps：
S1, two heating that lead bromide, cesium bromide powder are respectively placed in vapo(u)rization system burn on boat, and copper foil are pasted On the pallet of surface；
S2, vapo(u)rization system is vacuumized, sequentially or simultaneously heating fills the burning boat of lead bromide, cesium bromide, into promoting the circulation of qi It mutually deposits, film thickness is monitored using film thickness gauge in deposition process；
S3, after reaction closes vapo(u)rization system, copper foil taking-up is placed on warm table, in air in 130-140 DEG C Anneal 20-40min to get even compact perovskite negative material.
Preferably, in the S1, it is 10 to be evacuated to vacuum degree-3Pa。
Preferably, in the S2, deposition rate isDeposition total time is 3-5h, and lead bromide and cesium bromide are heavy Product thickness proportion is 1.8-2.2：1.
Preferably, in the S2, the thickness of the lead bromide and cesium bromide that are sequentially depositing is respectively 10 μm and 5 μm.
Preferably, in the S3, annealing temperature is 130 DEG C, annealing time 30min.
Preferably, in the S3, gained perovskite negative material is CsPb2Br5Or CsPb2Br5-CsPbBr3Mixing Phase.
Advantageous effect：The present invention is according to the principle of physical vapour deposition (PVD) and chemical vapor deposition, with inorganic lead bromide and bromine Change caesium is raw material, is deposited into copper foil substrate surface by heating evaporation, and by regulating and controlling evaporation rate, deposition thickness and thickness Degree ratio, and handled through subsequent anneal, the purely inorganic perovskite material of dense uniform is prepared, it is negative to use it for lithium ion battery Pole material shows good thermodynamic stability and excellent physical and chemical performance, solves graphite negative electrode of lithium ion battery Material needs to add organic solvent and binder in preparation process, and needs to be graphitized under the high temperature conditions, carbon packet It the processing such as covers, simplifies technique, reduce production cost, while raw material lead bromide and cesium bromide raw material easily obtain, price It is cheap, it is suitble to large-scale production.
Description of the drawings
Fig. 1 is the SEM figures of inorganic perovskite material prepared by the embodiment of the present invention 1；
Fig. 2 is the XRD diagram of inorganic perovskite material prepared by the embodiment of the present invention 2；
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
The method that a kind of vapor phase method proposed by the present invention prepares the inorganic perovskite negative material of layer structure, including following step Suddenly：
S1, a certain amount of lead bromide, cesium bromide powder being weighed, two heating for being respectively placed in vapo(u)rization system are burnt on boat, and Copper foil is pasted onto on the pallet of surface；
S2, system vacuum to be evaporated are evacuated to 10-3When Pa, start to be vapor-deposited.It is first turned on film thickness gauge, and heats and fills The burning boat (heating source) of lead bromide starts Thickness Monitoring, after reacting 2.5h, closes lead bromide heating source, opens cesium bromide heating Source, while film thickness gauge parameter is converted, start to monitor cesium bromide film thickness, after 2.5h heating evaporations, closes cesium bromide heating source.Its The thickness of middle cesium bromide is about 5 μm, and the thickness of lead bromide is about 10 μm；
S3, it waits for after reaction, closing vapo(u)rization system, takes out sample, and be put on warm table, add for 130 DEG C in air Thermal annealing 30min, you can obtain the perovskite negative material of even compact.
SEM characterizations are carried out to the pattern of perovskite negative material obtained, from figure 1 it appears that using the present embodiment In the obtained perovskite negative material structure even compact of method.
Embodiment 2
The method that a kind of vapor phase method proposed by the present invention prepares the inorganic perovskite negative material of layer structure, including following step Suddenly：
S1, a certain amount of lead bromide, cesium bromide powder being weighed, two heating for being respectively placed in vapo(u)rization system are burnt on boat, and Copper foil is pasted onto on the pallet of surface；
S2, system vacuum to be evaporated are evacuated to 10-3When Pa, start to be vapor-deposited, is first turned on film thickness gauge, and heat simultaneously The burning boat (heating source) for filling cesium bromide and lead bromide starts to monitor cesium bromide and lead bromide film thickness, after reacting 5h, closes bromination Caesium and lead bromide heating source；The thickness of the cesium bromide wherein evaporated is about 5 μm, and the thickness of lead bromide is about 10 μm；
S3, it waits for after reaction, closing vapo(u)rization system, takes out sample, and be put on warm table, add for 130 DEG C in air Thermal annealing 30min, you can obtain the perovskite negative material of even compact.
XRD characterization is carried out to perovskite negative material obtained, according to the method in the present embodiment by lead bromide, cesium bromide It deposits in FTO glass matrixs, then carries out XRD characterization, result is Fig. 2-a curves, then by CsPbBr3Standard items deposit to On FTO glass, to CsPbBr3Standard items and FTO glass matrixs carry out XRD characterization, as a result respectively 2-b, 2-c curve, from Fig. 2 In as can be seen that the ingredient that perovskite negative material is made in the present embodiment is CsPb2Br5-CsPbBr3Mixed phase, object phase Standard is mutually consistent with the reference substance of PDF cards.
Embodiment 3
The method that a kind of vapor phase method proposed by the present invention prepares the inorganic perovskite negative material of layer structure, including following step Suddenly：
S1, a certain amount of lead bromide, cesium bromide powder being weighed, two heating for being respectively placed in vapo(u)rization system are burnt on boat, and Copper foil is pasted onto on the pallet of surface；
S2, system vacuum to be evaporated are evacuated to 10-3When Pa, start to be vapor-deposited, is first turned on film thickness gauge, and heat simultaneously The burning boat (heating source) for filling cesium bromide and lead bromide starts to monitor cesium bromide and lead bromide film thickness, after reacting 3h, closes bromination Caesium and lead bromide heating source；The Film Thickness Ratio of the lead bromide and cesium bromide that wherein evaporate is 1.8：1, the thickness of cesium bromide is 5 μm；
S3, it waits for after reaction, closing vapo(u)rization system, takes out sample, and be put on warm table, add for 135 DEG C in air Thermal annealing 20min, you can obtain the perovskite negative material of even compact.
Embodiment 4
The method that a kind of vapor phase method proposed by the present invention prepares the inorganic perovskite negative material of layer structure, including following step Suddenly：
S1, a certain amount of lead bromide, cesium bromide powder being weighed, two heating for being respectively placed in vapo(u)rization system are burnt on boat, and Copper foil is pasted onto on the pallet of surface；
S2, system vacuum to be evaporated are evacuated to 10-3When Pa, start to be vapor-deposited, is first turned on film thickness gauge, and heat and fill The burning boat (heating source) of lead bromide starts Thickness Monitoring, after reacting 3h, closes lead bromide heating source, opens cesium bromide heating source, Film thickness gauge parameter is converted simultaneously, starts to monitor cesium bromide film thickness, after 2h heating evaporations, closes cesium bromide heating source；Wherein steam The Film Thickness Ratio of the lead bromide and cesium bromide that send out is 2.2：1, the thickness of cesium bromide is 5 μm；
S3, it waits for after reaction, closing vapo(u)rization system, takes out sample, and be put on warm table, add for 140 DEG C in air Thermal annealing 40min, you can obtain the perovskite negative material of even compact.
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 (7)

1. a kind of method that vapor phase method prepares the inorganic perovskite negative material of layer structure, which is characterized in that be in vacuum condition Under, lead bromide, cesium bromide are sequentially or simultaneously deposited to by vapor phase method in copper foil substrate, then heating anneal in air, i.e., .
2. the method that vapor phase method according to claim 1 prepares the inorganic perovskite negative material of layer structure, feature exist In including the following steps：
S1, two heating that lead bromide, cesium bromide powder are respectively placed in vapo(u)rization system burn on boat, and copper foil are pasted onto just On the pallet of top；
S2, vapo(u)rization system is vacuumized, sequentially or simultaneously heating fills the burning boat of lead bromide, cesium bromide, and it is heavy to carry out gas phase It is long-pending, film thickness is monitored using film thickness gauge in deposition process；
S3, after reaction closes vapo(u)rization system, and copper foil taking-up is placed on warm table, in air in 130-140 DEG C of annealing 20-40min to get even compact perovskite negative material.
3. the method that vapor phase method according to claim 1 or 2 prepares the inorganic perovskite negative material of layer structure, feature It is, in the S1, it is 10 to be evacuated to vacuum degree-3Pa。
4. the method that vapor phase method according to claim 1 or 2 prepares the inorganic perovskite negative material of layer structure, feature It is, in the S2, deposition rate isDeposition total time is 3-5h, and lead bromide and cesium bromide deposition thickness ratio are 1.8-2.2：1.
5. the method that vapor phase method according to claim 4 prepares the inorganic perovskite negative material of layer structure, feature exist In in the S2, the thickness of the lead bromide and cesium bromide that are sequentially depositing is respectively 10 μm and 5 μm.
6. the method that vapor phase method according to claim 1 or 2 prepares the inorganic perovskite negative material of layer structure, feature It is, in the S3, annealing temperature is 130 DEG C, annealing time 30min.
7. the method that vapor phase method according to claim 1 or 2 prepares the inorganic perovskite negative material of layer structure, feature It is, in the S3, gained perovskite negative material is CsPb2Br5Or CsPb2Br5-CsPbBr3Mixed phase.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109065834A (en) * 2018-07-12 2018-12-21 合肥国轩高科动力能源有限公司 A kind of lithium ion derivative preparation method for mutually making negative electrode material of inorganic perovskite
CN109713100A (en) * 2018-12-21 2019-05-03 华中科技大学 A method of preparing full-inorganic perovskite light emitting diode active layer
CN111326657A (en) * 2020-03-09 2020-06-23 成都信息工程大学 CsPbBr3/CsPb2Br5Composite film and preparation method 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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CN106876533A (en) * 2017-01-22 2017-06-20 郑州大学 One kind is based on MgO CsPbBr3Luminescent device of structure and preparation method thereof
CN107381624A (en) * 2017-06-21 2017-11-24 浙江大学 A kind of preparation method of the ultra-thin inorganic lead halogen perovskite nanocluster based on chemical vapor deposition

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CN106876533A (en) * 2017-01-22 2017-06-20 郑州大学 One kind is based on MgO CsPbBr3Luminescent device of structure and preparation method thereof
CN107381624A (en) * 2017-06-21 2017-11-24 浙江大学 A kind of preparation method of the ultra-thin inorganic lead halogen perovskite nanocluster based on chemical vapor deposition

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109065834A (en) * 2018-07-12 2018-12-21 合肥国轩高科动力能源有限公司 A kind of lithium ion derivative preparation method for mutually making negative electrode material of inorganic perovskite
CN109065834B (en) * 2018-07-12 2021-07-09 合肥国轩高科动力能源有限公司 Preparation method of inorganic perovskite derivative phase used as negative electrode material for lithium ions
CN109713100A (en) * 2018-12-21 2019-05-03 华中科技大学 A method of preparing full-inorganic perovskite light emitting diode active layer
CN109713100B (en) * 2018-12-21 2020-10-16 华中科技大学 Method for preparing active layer of all-inorganic perovskite light-emitting diode
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
CN111326657A (en) * 2020-03-09 2020-06-23 成都信息工程大学 CsPbBr3/CsPb2Br5Composite film and preparation method thereof
CN111326657B (en) * 2020-03-09 2021-03-16 成都信息工程大学 CsPbBr3/CsPb2Br5Composite film 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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