CN110010869A - A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof - Google Patents

A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof Download PDF

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Publication number
CN110010869A
CN110010869A CN201910265871.9A CN201910265871A CN110010869A CN 110010869 A CN110010869 A CN 110010869A CN 201910265871 A CN201910265871 A CN 201910265871A CN 110010869 A CN110010869 A CN 110010869A
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electrically conductive
conductive polyaniline
polyaniline
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cathode
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张成如
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Shandong Xinghuo Science Technology Institute
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Shandong Xinghuo Science Technology Institute
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • 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
    • H01M4/36—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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • H01M4/602—Polymers
    • 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
    • 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 relates to a kind of three-dimensional grapheme conductive networks for cathode of lithium battery and preparation method thereof, the following steps are included: N-Methyl pyrrolidone is added in electrically conductive polyaniline, by phenolic resin, ethanol solution is added, form phenolic aldehyde/ethanol solution, then it mixes, nano silica fume and graphene oxide powder is added, Si/GO/ electrically conductive polyaniline/phenolic resin suspension is made, suspension is taken to be spray-dried, obtain Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film, by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in argon gas/nitrogen atmosphere, calcine 2h~3h, obtain Si/ graphene/pyrolysis polyaniline-amorphous carbon composite material.The utility model has the advantages that using nano silica fume, graphene oxide, electrically conductive polyaniline and phenolic resin as raw material, obtained spherical porous second particle is heat-treated, form spherical composite porous material, with 3 D stereo conductive network structure, with very high specific capacity, removal lithium embedded current potential is moderate, and safety is good.

Description

A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof
Technical field
The present invention relates to lithium battery materials to prepare preparation field, and in particular to a kind of three-dimensional grapheme conductive network is used for lithium Battery cathode and preparation method thereof.
Background technique
With the development of electric car and large-scale energy storage facility, the demand to lithium ion battery with high energy density is increasingly compeled It cuts.Currently, commercial Li-ion battery generally uses graphite Carbon materials as cathode, however the theoretical specific capacity of graphite is lower (372mAh/g) is easy " analysis lithium " in fast charging and discharging and has security risk, and this severely limits lithium ion battery energy The raising of density and power density, therefore, scientific workers are being to find high capacity, high security, the lithium of long-life always Ion battery material does unremitting effort.
In the lithium ion battery negative material system being currently known, silicon possesses higher specific capacity and preferable safety Can, extensive concern and the research of academia are obtained in last decade.To be overcome in practical application two of silicium cathode mainly ask Topic is that bulk effect and conductivity be not high.One of solution is the silicon materials for preparing nanoscale；Another is solved Mode is that the second phase is introduced into silicon materials, such as carbon material, active metal or inert metal.Wherein, carbon material has excellent The bulk effect of silicon can be effectively relieved in different mechanical performance, and carbon material is also the good conductor of ion and electronics, can be effective Increase the conductivity of electrode material, therefore silicon carbon material is a kind of system of silica-base material of most study.
Graphene is a kind of two-dimensional material of single layer chip architecture being made of carbon atom, and wherein carbon atom is with SP2 hydridization rail Road form forms the flat film that hexagon is in honeycomb lattice, is the most thin material being currently known.Graphene has excellent machine Tool performance, biggish specific surface area, extraordinary ion and electronic conductance rate and good chemical resistance, are answered extensively With in the preparation of electrode material and a kind of ideal silicium cathode host material.The silicon reported at present and graphene it is compound It is compound that material mainly uses the methods of mechanical mixture, freeze-drying to carry out silicon particle and graphene, not due to silicon particle It can be coated completely by graphene, due to bulk effect in charge and discharge process, silicon particle is easy from graphene intermediate peeling, compound The cyclical stability of electrode is poor.
Summary of the invention
In order to solve the deficiencies in the prior art, it is negative for lithium battery that the present invention provides a kind of three-dimensional grapheme conductive networks Pole and preparation method thereof.
The technical solution adopted by the present invention to solve the technical problems is: a kind of three-dimensional grapheme conductive network is electric for lithium Pond cathode and preparation method thereof, comprising the following steps:
(1) 5g~10g electrically conductive polyaniline is added in the N-Methyl pyrrolidone of 100ml~200ml, ultrasonic agitation 30~ 60min forms electrically conductive polyaniline/N-Methyl pyrrolidone solution, then weighs 10g~20g phenolic resin, be added 100ml~ In the ethanol solution of 200ml, 30~60min is stirred by ultrasonic, phenolic aldehyde/ethanol solution is formed, then by electrically conductive polyaniline/N- methyl Pyrrolidone solution and phenolic aldehyde/ethanol solution are mixed in volume 1:1 ratio, and 60 DEG C~80 DEG C 30~60min of ultrasonic agitation are formed Electrically conductive polyaniline/phenolic aldehyde composite solution；
(2) 1g~5g nano silica fume is weighed, is added in 200ml~400ml electrically conductive polyaniline/phenolic aldehyde composite solution, ultrasound 30~60min is stirred, the graphene oxide powder of 1g~5g, 60 DEG C~80 DEG C ultrasonic agitation 2h~5h is then added, ball milling mixes 1h~2h is closed, Si/GO/ electrically conductive polyaniline/phenolic resin suspension is formed；
(3) it takes Si/GO/ electrically conductive polyaniline/phenolic resin suspension of 200ml to be spray-dried, obtains Si/GO/ and lead Conducting polyaniline/novolak resin precursor body thin film；
(4) by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in air atmosphere with 5 DEG C/min~ The heating rate of 10 DEG C/min is warming up to 200 DEG C~300 DEG C, and 1~2h of constant temperature, carries out stabilization processes, then in protection gas In atmosphere, 2h~3h is calcined at 700 DEG C~900 DEG C, naturally cools to room temperature then to get Si/ graphene/pyrolysis polyaniline-is arrived The composite material of amorphous carbon.
Further, the spray drying, equipment setting parameter are that fltting speed is set as 0.5ml/h, spray head to receiver Distance is 10cm, and electrostatic spray is carried out under the high voltage electric field of 25kV.
Further, the protective atmosphere is argon gas/nitrogen atmosphere.
The invention has the following advantages: being original with nano silica fume, graphene oxide, electrically conductive polyaniline and phenolic resin Material, spherical porous compound second particle is prepared for using spray drying process, then by obtained spherical porous second particle into Row heat treatment forms spherical composite porous material, has 3 D stereo conductive network structure, has very high specific capacity, deintercalation Lithium current potential is moderate, and safety is good, resourceful, is the contenders of next-generation ion cathode material lithium.
Specific embodiment
It is described in detail to various aspects of the present invention below, unless specific instructions, various raw materials of the invention can pass through It is prepared or is commercially available according to the conventional method of this field.
Embodiment 1
A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof, comprising the following steps:
(1) 5g electrically conductive polyaniline is added in the N-Methyl pyrrolidone of 100ml, 30min is stirred by ultrasonic, formed conductive poly- Aniline/N-Methyl pyrrolidone solution, then weighs 10g phenolic resin, is added in the ethanol solution of 100ml, ultrasonic agitation 30min forms phenolic aldehyde/ethanol solution, then presses electrically conductive polyaniline/N-Methyl pyrrolidone solution and phenolic aldehyde/ethanol solution The mixing of volume 1:1 ratio, 60 DEG C of ultrasonic agitation 30min form electrically conductive polyaniline/phenolic aldehyde composite solution；
(5) 1g nano silica fume is weighed, is added in 200ml electrically conductive polyaniline/phenolic aldehyde composite solution, 30min is stirred by ultrasonic, so The graphene oxide powder of 1g is added afterwards, 60 DEG C of ultrasonic agitations 2h, ball milling mixing 1h form Si/GO/ electrically conductive polyaniline/phenolic aldehyde Resin suspension；
(6) it takes Si/GO/ electrically conductive polyaniline/phenolic resin suspension of 200ml to be spray-dried, obtains Si/GO/ and lead Conducting polyaniline/novolak resin precursor body thin film；
(7) by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in air atmosphere with 5 DEG C/min's Heating rate is warming up to 200 DEG C, and constant temperature 1h, carries out stabilization processes and calcines 2h at 700 DEG C, so then in protective atmosphere Naturally cool to room temperature afterwards to get Si/ graphene/pyrolysis polyaniline-amorphous carbon composite material is arrived.
Further, the spray drying, equipment setting parameter are that fltting speed is set as 0.5ml/h, spray head to receiver Distance is 10cm, and electrostatic spray is carried out under the high voltage electric field of 25kV.
Further, the protective atmosphere is argon gas/nitrogen atmosphere.
Embodiment two
A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof, comprising the following steps:
(1) 8g electrically conductive polyaniline is added in the N-Methyl pyrrolidone of 150ml, 45min is stirred by ultrasonic, formed conductive poly- Aniline/N-Methyl pyrrolidone solution, then weighs 15g phenolic resin, is added in the ethanol solution of 150ml, ultrasonic agitation 45min forms phenolic aldehyde/ethanol solution, then presses electrically conductive polyaniline/N-Methyl pyrrolidone solution and phenolic aldehyde/ethanol solution The mixing of volume 1:1 ratio, 70 DEG C of ultrasonic agitation 60min form electrically conductive polyaniline/phenolic aldehyde composite solution；
(8) 3g nano silica fume is weighed, is added in 400ml electrically conductive polyaniline/phenolic aldehyde composite solution, 60min is stirred by ultrasonic, so The graphene oxide powder of 5g is added afterwards, 80 DEG C of ultrasonic agitations 3h, ball milling mixing 1h form Si/GO/ electrically conductive polyaniline/phenolic aldehyde Resin suspension；
(9) it takes Si/GO/ electrically conductive polyaniline/phenolic resin suspension of 200ml to be spray-dried, obtains Si/GO/ and lead Conducting polyaniline/novolak resin precursor body thin film；
(10) by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in air atmosphere with 7 DEG C/min Heating rate be warming up to 250 DEG C, and constant temperature 2h, carry out stabilization processes and calcine 3h at 800 DEG C then in protective atmosphere, Then room temperature is naturally cooled to get Si/ graphene/pyrolysis polyaniline-amorphous carbon composite material is arrived.
Further, the spray drying, equipment setting parameter are that fltting speed is set as 0.5ml/h, spray head to receiver Distance is 10cm, and electrostatic spray is carried out under the high voltage electric field of 25kV.
Further, the protective atmosphere is argon gas/nitrogen atmosphere.
Embodiment 3
A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof, comprising the following steps:
(1) 10g electrically conductive polyaniline is added in the N-Methyl pyrrolidone of 100ml, 60min is stirred by ultrasonic, formed conductive Polyaniline/N-Methyl pyrrolidone solution, then weighs 20g phenolic resin, is added in the ethanol solution of 200ml, ultrasonic agitation 60min forms phenolic aldehyde/ethanol solution, then presses electrically conductive polyaniline/N-Methyl pyrrolidone solution and phenolic aldehyde/ethanol solution The mixing of volume 1:1 ratio, 80 DEG C of ultrasonic agitation 60min form electrically conductive polyaniline/phenolic aldehyde composite solution；
(11) 5g nano silica fume is weighed, is added in 200ml electrically conductive polyaniline/phenolic aldehyde composite solution, 60min is stirred by ultrasonic, Then the graphene oxide powder of 5g is added, 80 DEG C of ultrasonic agitations 5h, ball milling mixing 2h form Si/GO/ electrically conductive polyaniline/phenol Urea formaldehyde suspension；
(12) it takes Si/GO/ electrically conductive polyaniline/phenolic resin suspension of 200ml to be spray-dried, obtains Si/GO/ and lead Conducting polyaniline/novolak resin precursor body thin film；
(13) by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in air atmosphere with 10 DEG C/min Heating rate be warming up to 300 DEG C, and constant temperature 2h, carry out stabilization processes and calcine 3h at 900 DEG C then in protective atmosphere, Then room temperature is naturally cooled to get Si/ graphene/pyrolysis polyaniline-amorphous carbon composite material is arrived.
Further, the spray drying, equipment setting parameter are that fltting speed is set as 0.5ml/h, spray head to receiver Distance is 10cm, and electrostatic spray is carried out under the high voltage electric field of 25kV.
Further, the protective atmosphere is argon gas/nitrogen atmosphere.
The present invention is not limited to the embodiment, anyone should learn that the structure made under the inspiration of the present invention becomes Change, the technical schemes that are same or similar to the present invention are fallen within the scope of protection of the present invention.
Technology not described in detail in the present invention, shape, construction portion are well-known technique.

Claims (3)

1. a kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof, it is characterised in that: including following step It is rapid:
(1) 5g~10g electrically conductive polyaniline is added in the N-Methyl pyrrolidone of 100ml~200ml, ultrasonic agitation 30~ 60min forms electrically conductive polyaniline/N-Methyl pyrrolidone solution, then weighs 10g~20g phenolic resin, be added 100ml~ In the ethanol solution of 200ml, 30~60min is stirred by ultrasonic, phenolic aldehyde/ethanol solution is formed, then by electrically conductive polyaniline/N- methyl Pyrrolidone solution and phenolic aldehyde/ethanol solution are mixed in volume 1:1 ratio, and 60 DEG C~80 DEG C 30~60min of ultrasonic agitation are formed Electrically conductive polyaniline/phenolic aldehyde composite solution；
(2) 1g~5g nano silica fume is weighed, is added in 200ml~400ml electrically conductive polyaniline/phenolic aldehyde composite solution, ultrasonic agitation Then the graphene oxide powder of 1g~5g, 60 DEG C~80 DEG C ultrasonic agitations 2h~5h, ball milling mixing 1h are added in 30~60min ~2h forms Si/GO/ electrically conductive polyaniline/phenolic resin suspension；
(3) it takes Si/GO/ electrically conductive polyaniline/phenolic resin suspension of 200ml to be spray-dried, it is poly- to obtain Si/GO/ conduction Aniline/novolak resin precursor body thin film；
(4) by Si/GO/ electrically conductive polyaniline/novolak resin precursor body thin film of acquisition in air atmosphere with 5 DEG C/min~10 DEG C/heating rate of min is warming up to 200 DEG C~300 DEG C, and 1~2h of constant temperature, stabilization processes are carried out, then in protective atmosphere In, 2h~3h is calcined at 700 DEG C~900 DEG C, naturally cools to room temperature then to get Si/ graphene/pyrolysis polyaniline-nothing is arrived The composite material of setting carbon.
2. a kind of three-dimensional grapheme conductive network according to claim 1 is used for cathode of lithium battery and preparation method thereof, Be characterized in that: the spray drying, equipment setting parameter are that fltting speed is set as 0.5ml/h, and the distance of spray head to receiver is 10cm carries out electrostatic spray under the high voltage electric field of 25kV.
3. a kind of three-dimensional grapheme conductive network according to claim 1 is used for cathode of lithium battery and preparation method thereof, Be characterized in that: the protective atmosphere is argon gas/nitrogen atmosphere.
CN201910265871.9A 2019-04-03 2019-04-03 A kind of three-dimensional grapheme conductive network is for cathode of lithium battery and preparation method thereof Withdrawn CN110010869A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110429249A (en) * 2019-07-16 2019-11-08 河北工业大学 A kind of preparation method of rubber removing graphene combination electrode material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108232139A (en) * 2017-12-20 2018-06-29 中国科学院福建物质结构研究所 A kind of graphene composite material and preparation method thereof
CN109461890A (en) * 2017-09-06 2019-03-12 丰域科技（北京）有限公司 Silicon-carbon cathode material, preparation method and lithium ion battery

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109461890A (en) * 2017-09-06 2019-03-12 丰域科技（北京）有限公司 Silicon-carbon cathode material, preparation method and lithium ion battery
CN108232139A (en) * 2017-12-20 2018-06-29 中国科学院福建物质结构研究所 A kind of graphene composite material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110429249A (en) * 2019-07-16 2019-11-08 河北工业大学 A kind of preparation method of rubber removing graphene combination electrode material
CN110429249B (en) * 2019-07-16 2022-01-28 河北工业大学 Preparation method of rubber-stripped graphene composite electrode material

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Application publication date: 20190712