CN103700815A - Flexible transparent lithium ion battery electrode material and preparation method thereof - Google Patents

Flexible transparent lithium ion battery electrode material and preparation method thereof Download PDF

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CN103700815A
CN103700815A CN201310663888.2A CN201310663888A CN103700815A CN 103700815 A CN103700815 A CN 103700815A CN 201310663888 A CN201310663888 A CN 201310663888A CN 103700815 A CN103700815 A CN 103700815A
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silicon nanowires
lithium ion
ion battery
graphene
battery electrode
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王成新
庞春雷
崔浩
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • 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
    • 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
    • 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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  • Electrochemistry (AREA)
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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a flexible transparent lithium ion battery electrode material and a preparation method thereof. The lithium ion battery electrode material comprises a flexible transparent silicon nanometer-wire network membrane and graphene, wherein a silicon nanometer wire is wrapped with the graphene, and a hollow space is formed between the silicon nanometer wire and the graphene. By utilizing the composite material of the silicon and graphene, the flexible transparent lithium ion battery electrode is high in capacity and good in circulating property and has no conductive agent and binder, the energy-mass ratio is increased, and the property of the material can be improved through the hollow structure.

Description

A kind of flexible and transparent lithium ion battery electrode material and preparation method thereof
Technical field
The present invention relates to the technical fields such as electrochemistry, semiconductor, relate in particular to a kind of flexible and transparent lithium ion battery electrode material and preparation method thereof.
Background technology
In recent years, the fast development of environmental protection battery, lithium ion battery (Lithium Ion Battery is called for short LIB) is the third generation small battery after nickel-cadmium cell, Ni-MH battery.As a kind of novel chemical power source, it is outstanding that it has advantages of that operating voltage is high, specific energy is large, discharge potential curve is steady, self discharge is little, have extended cycle life, cryogenic property is good, memoryless, pollution-free etc., can meet people to the needed battery miniaturization and of portable electronics and environmentally friendly double requirements, being widely used in mobile communication, notebook computer, taking the photograph compact electronic devices such as putting all-in-one, is also the ideal source that following electric vehicle is used.
What commercial Li-ion battery electrode material adopted at present is graphite-like material with carbon element, but its theoretical specific capacity only has 372mAh/g, thereby limited the further raising of lithium ion battery specific energy, can not meet the demand of growing high-energy Portable power source, and material with carbon element exists charge/discharge capacity low, high-rate charge-discharge capability is poor, the problem such as less stable in electrolyte, thereby Nano Electrode Material of Lithium Ion Batteries becomes international research focus.The research direction of negative material has started to tilt to silicon materials aspect at present, and composite material containing silicon especially receives publicity.
Transparence and softnessization are important directions of current scientific and technological electronic product development, receive especially in recent years more concern, such as transparent solar cell, and transparent conductive film, all-transparent mobile phone, transparent lithium ion battery etc.Wherein the demand of transparent battery is also very strong, but enlivens material and cannot manufacture transparence with good pliability due to crucial in battery, makes this imagination always in the conceptual phase.Several transparent battery only existing of scientific research personnel's development at present, energy density and storage electric power still can not provide the normal use of mobile phone electronic product.
Therefore, those skilled in the art is devoted to develop a kind of transparent flexible lithium ion battery electrode material and preparation method.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is to provide a kind of transparent flexible lithium ion battery electrode material and preparation method thereof, utilize the composite material of silicon and Graphene, there is higher capacity and good cycle performance, without conductive agent and binding agent, increased energy quality ratio, being designed with of hollow structure is beneficial to the performance that improves material.
For achieving the above object, the invention provides a kind of flexible and transparent lithium ion battery electrode material, comprise silicon nanowires nethike embrane and Graphene, described Graphene wraps up described silicon nanowires, between described silicon nanowires and described Graphene, has a layer hollow space.
In better embodiment of the present invention, the diameter of described silicon nanowires is 10nm, and etween the lines has uniform hole.
The present invention also provides a kind of transparent flexible lithium ion battery electrode material preparation method, comprising:
A) adopt the method for SiO thermal evaporation, SiO powder thermal evaporation growth Si nano wire, form and erect film, cooling is taken out;
B) adopt the method for microwave plasma chemical vapour deposition, growing graphene on silicon nanowires nethike embrane;
C) by the method for hydrofluoric acid corrosion, erode the oxide layer of surface of silicon nanowires, produce silicon nanowires and graphene layer hollow space, for silicon nanowires, in charge and discharge process, expand and shrink.
In another better embodiment of the present invention, described steps A) in, the method step of SiO thermal evaporation is:
A1) SiO powder is placed in the graphite crucible of a vertical high-frequency induction furnace system, heats described graphite crucible, make material be heated to rapidly 1600 ℃, SiO powder generation disproportionated reaction produces Si and SiO2 steam in described vertical high-frequency induction furnace system;
A2) in described vertical high-frequency induction furnace system, pass into N2 as carrier gas, described Si steam is taken to the graphite guide nozzle portion of described vertical high-frequency induction furnace system, in described graphite guide nozzle portion grow silicon nanowires, simultaneously, described silicon nanowires is woven into mutually around a circle in described graphite guide aperture and erects film under the effect of described N2, and after one hour, cooling is taken out.
In another better embodiment of the present invention, described step B) in, the method step of microwave plasma chemical vapour deposition is:
B1) from described silicon nanowires nethike embrane, by electrode size, cut a slice, put into described vertical high-frequency induction furnace system furnace chamber base top;
B2) to the forvacuum of described vertical high-frequency induction furnace system to 2Pa, then pass into H2 to 650Pa, increasing microwave input power is that 600W heats to 300 ℃ to described nethike embrane;
B3) in described vertical high-frequency induction furnace system, pass into CH4 gas and carry out Graphene growth, keep 30s, close power, after cooling, take out.
In another better embodiment of the present invention, described step C) described in, in hydrofluoric acid caustic solution, hydrofluoric acid corrosion working concentration is 4%, and etching time is 10min, cleans later with deionized water and absolute ethyl alcohol.
Transparent flexible lithium ion battery electrode material provided by the invention is the composite material of silicon and Graphene, has higher capacity and good cycle performance; Without conductive agent and binding agent, increased energy quality ratio; Being designed with of hollow structure is beneficial to the performance that improves material.
Below with reference to accompanying drawing, the technique effect of design of the present invention, concrete structure and generation is described further, to understand fully object of the present invention, feature and effect.
Accompanying drawing explanation
Fig. 1 is the silicon nanowires nethike embrane transmission electron microscope photo of a preferred embodiment of the present invention;
Fig. 2 is the transparent silicon nano wire nethike embrane optical photograph of a preferred embodiment of the present invention;
Fig. 3 is optical photograph after the growing graphene of a preferred embodiment of the present invention;
Fig. 4 is that the motor negative material of a preferred embodiment of the present invention is made of vertical Efco-Northrup furnace system configuration schematic diagram;
Fig. 5 is the cycle performance of lithium ion battery resolution chart being obtained by a preferred embodiment of the present invention;
Fig. 6 is the lithium ion battery high rate performance resolution chart being obtained by a preferred embodiment of the present invention.
Embodiment
The invention provides a kind of transparent flexible lithium ion battery electrode material, comprise silicon nanowires nethike embrane and Graphene, described Graphene wraps up described silicon nanowires, between described silicon nanowires and described Graphene, has a layer hollow space.As shown in Figure 1, figure 2 and figure 3.
The composite material of silicon and Graphene, has higher capacity and good cycle performance; Without conductive agent and binding agent, increased energy quality ratio; Being designed with of hollow structure is beneficial to the performance that improves material.
The embodiment of the present invention provides the manufacture method of above-mentioned transparent flexible lithium ion battery electrode material, utilize a kind of vertical high-frequency induction furnace system as shown in Figure 4, this high-frequency induction furnace system comprises graphite crucible 1, heat insulation graphite felt 2, quartz cover clock 3, heating inner core 4, copper coil 5 and furnace chamber base 6, quartz cover clock 3 covers on furnace chamber base 6 tops, form enclosure space, it is inner that graphite crucible 1, heat insulation graphite felt 2 and heating inner core 4 are positioned at this enclosure space, and copper coil 5 is positioned at quartz cover clock 3 both sides external.
The manufacture method detailed process of transparent flexible lithium ion battery electrode material is as follows:
The method of preparing the soft silicon nanowires nethike embrane of printing opacity: adopt the method for simple SiO thermal evaporation.SiO powder is placed in the graphite crucible 1 of vertical high-frequency induction furnace system, utilize high-frequency induction copper coil 5 heating crucibles, make material be heated to rapidly 1600 ℃, SiO powder generation disproportionated reaction, produces Si and SiO2 steam, pass into N2 as carrier gas, Si steam is taken to the graphite guide nozzle portion of vertical high-frequency induction furnace system, the Si nano wire of here growing, simultaneously, silicon nanowires is woven into mutually around a circle in aperture and erects film under the effect of N2, and after one hour, cooling is taken out.
This silicon nanowires diameter is very even, and in 10nm left and right, etween the lines has uniform hole, therefore has good light transmission.
Test method at surface of silicon nanowires growing graphene: the method that adopts microwave plasma chemical vapour deposition.From silicon nanowires nethike embrane, by electrode size, cut a slice, put into furnace chamber base 6 tops of vertical high-frequency induction furnace system, first the forvacuum of vertical high-frequency induction furnace system is to 2Pa, pass into again H2 to 650Pa, increasing microwave input power is that 600W heats to 300 ℃ to nethike embrane, then passes into CH4 gas and carries out Graphene growth, keeps 30s, close power, after cooling, take out.
Hydrofluoric acid corrosion working concentration is 4%, and etching time is 10min, cleans later with deionized water and absolute ethyl alcohol.
Material prepared by said method can directly be tested as lithium ion battery electrode material, and as shown in Figure 5, charging and discharging lithium battery cycle performance test curve as shown in Figure 6 for charging and discharging lithium battery cycle performance test curve.Test shows that this electrode has outstanding lithium ion performance, and capacity can reach 2500mAh/g first, discharges and recharges, more than after 100 circulations, capacity still can reach 1000mAh/g under the current density of 1A/g.In addition, the silicon nanowires nethike embrane that the present invention is prepared, can be widely used in multiple sciemtifec and technical sphere, such as the microchip of flexible and transparent, and printing opacity piezoelectric, solar cell, touch-screen etc.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area just can design according to the present invention be made many modifications and variations without creative work.Therefore, all technical staff in the art, all should be in the determined protection range by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.

Claims (6)

1. a flexible and transparent lithium ion battery electrode material, is characterized in that, comprises silicon nanowires nethike embrane and Graphene, and described Graphene wraps up described silicon nanowires, between described silicon nanowires and described Graphene, has a layer hollow space.
2. flexible and transparent lithium ion battery electrode material as claimed in claim 1, is characterized in that, the diameter of described silicon nanowires is 10nm, has uniform hole between described silicon nanowires and line.
3. a flexible and transparent lithium ion battery electrode material preparation method, is characterized in that, comprises the steps:
A) adopt the method for SiO thermal evaporation, SiO powder thermal evaporation growth Si nano wire, form and erect film, cooling is taken out;
B) adopt the method for microwave plasma chemical vapour deposition, growing graphene on silicon nanowires nethike embrane;
C) by the method for hydrofluoric acid corrosion, erode the oxide layer of surface of silicon nanowires, produce silicon nanowires and graphene layer hollow space, for silicon nanowires, in charge and discharge process, expand and shrink.
4. flexible and transparent lithium ion battery electrode material preparation method as claimed in claim 3, is characterized in that described steps A) described in the method step of SiO thermal evaporation be:
A1) SiO powder is placed in a graphite crucible with vertical high-frequency induction furnace system, heats described graphite crucible, make material be heated to rapidly 1600 ℃, SiO powder generation disproportionated reaction produces Si and SiO2 steam in described vertical high-frequency induction furnace system;
A2) in described vertical high-frequency induction furnace system, pass into N2 as carrier gas, described Si steam is taken to the graphite guide nozzle portion of described vertical high-frequency induction furnace system, in described graphite guide nozzle portion grow silicon nanowires, simultaneously, described silicon nanowires is woven into mutually around a circle in described graphite guide aperture and erects film under the effect of described N2, and after one hour, cooling is taken out.
5. flexible and transparent lithium ion battery electrode material preparation method as claimed in claim 3, is characterized in that described step B) described in the method step of microwave plasma chemical vapour deposition be:
B1) from described silicon nanowires nethike embrane, by electrode size, cut a slice, put into described vertical high-frequency induction furnace system furnace chamber base top;
B2) to the forvacuum of described vertical high-frequency induction furnace system to 2Pa, then pass into H2 to 650Pa, increasing microwave input power is that 600W heats to 300 ℃ to described nethike embrane;
B3) in described vertical high-frequency induction furnace system, pass into CH4 gas and carry out Graphene growth, keep 30s, close power, after cooling, take out.
6. flexible and transparent lithium ion battery electrode material preparation method as claimed in claim 3, it is characterized in that described step step C) described in hydrofluoric acid caustic solution, hydrofluoric acid corrosion working concentration is 4%, etching time is 10min, cleans later with deionized water and absolute ethyl alcohol.
CN201310663888.2A 2013-12-11 2013-12-11 Flexible transparent lithium ion battery electrode material and preparation method thereof Pending CN103700815A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103972484A (en) * 2014-05-20 2014-08-06 李学耕 Preparation method of nanometer silicon/grapheme lithium ion battery negative electrode material
CN105226249A (en) * 2015-09-11 2016-01-06 王晓亮 A kind of 3 SiC 2/graphite alkene core-shell material and Synthesis and applications thereof with gap
CN105355893A (en) * 2015-12-16 2016-02-24 西北工业大学 Preparation method of flexible lithium ion battery negative material
CN105449173A (en) * 2014-08-29 2016-03-30 国家纳米科学中心 Cavity-structuralized silicon-carbon core-shell nanowire array, and preparation method and use thereof
CN108306009A (en) * 2018-03-12 2018-07-20 中国科学院宁波材料技术与工程研究所 A kind of silicon-carbon oxide composite negative pole material, preparation method and lithium ion battery
JP2020502723A (en) * 2016-10-06 2020-01-23 ナノテク インストゥルメンツ, インコーポレイテッドNanotek Instruments, Inc. Lithium-ion battery anode containing silicon nanowires grown in situ within the pores of graphene foam and method of making
CN112582590A (en) * 2020-12-01 2021-03-30 上海集成电路研发中心有限公司 Nanowire electrode structure and preparation method thereof
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US11633785B2 (en) 2019-04-30 2023-04-25 6K Inc. Mechanically alloyed powder feedstock
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11839919B2 (en) 2015-12-16 2023-12-12 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
US11855278B2 (en) 2020-06-25 2023-12-26 6K, Inc. Microcomposite alloy structure
US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
US11963287B2 (en) 2020-09-24 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103972484A (en) * 2014-05-20 2014-08-06 李学耕 Preparation method of nanometer silicon/grapheme lithium ion battery negative electrode material
CN105449173A (en) * 2014-08-29 2016-03-30 国家纳米科学中心 Cavity-structuralized silicon-carbon core-shell nanowire array, and preparation method and use thereof
CN105449173B (en) * 2014-08-29 2019-04-12 国家纳米科学中心 A kind of cavity structure silico-carbo core-shell nano linear array, preparation method and its usage
CN105226249A (en) * 2015-09-11 2016-01-06 王晓亮 A kind of 3 SiC 2/graphite alkene core-shell material and Synthesis and applications thereof with gap
CN105355893A (en) * 2015-12-16 2016-02-24 西北工业大学 Preparation method of flexible lithium ion battery negative material
US11839919B2 (en) 2015-12-16 2023-12-12 6K Inc. Spheroidal dehydrogenated metals and metal alloy particles
JP7113818B2 (en) 2016-10-06 2022-08-05 ナノテク インストゥルメンツ，インコーポレイテッド Lithium ion battery anode containing in situ grown silicon nanowires within pores of graphene foam and method of manufacture
JP2020502723A (en) * 2016-10-06 2020-01-23 ナノテク インストゥルメンツ, インコーポレイテッドNanotek Instruments, Inc. Lithium-ion battery anode containing silicon nanowires grown in situ within the pores of graphene foam and method of making
CN108306009A (en) * 2018-03-12 2018-07-20 中国科学院宁波材料技术与工程研究所 A kind of silicon-carbon oxide composite negative pole material, preparation method and lithium ion battery
US11633785B2 (en) 2019-04-30 2023-04-25 6K Inc. Mechanically alloyed powder feedstock
US11717886B2 (en) 2019-11-18 2023-08-08 6K Inc. Unique feedstocks for spherical powders and methods of manufacturing
US11590568B2 (en) 2019-12-19 2023-02-28 6K Inc. Process for producing spheroidized powder from feedstock materials
US11855278B2 (en) 2020-06-25 2023-12-26 6K, Inc. Microcomposite alloy structure
US11963287B2 (en) 2020-09-24 2024-04-16 6K Inc. Systems, devices, and methods for starting plasma
US11919071B2 (en) 2020-10-30 2024-03-05 6K Inc. Systems and methods for synthesis of spheroidized metal powders
CN112582590A (en) * 2020-12-01 2021-03-30 上海集成电路研发中心有限公司 Nanowire electrode structure and preparation method thereof

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Application publication date: 20140402