CN105633344A - Molybdenum disulfide nanosheet/nanocellulose/carbon nanotube/graphene composite lithium battery thin film negative electrode material and preparation method therefor - Google Patents
Molybdenum disulfide nanosheet/nanocellulose/carbon nanotube/graphene composite lithium battery thin film negative electrode material and preparation method therefor Download PDFInfo
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Abstract
The invention relates to a molybdenum disulfide nanosheet/nanocellulose/carbon nanotube/graphene composite lithium battery thin film negative electrode material and a preparation method therefor. The negative electrode material takes nanocellulose as the flexible substrate; the molybdenum disulfide nanosheet, the graphene nanosheet and the carbon nanotube are uniformly mixed and embedded in a network of the nanocellulose to form a flexible self-supporting thin film electrode material with a compact network structure, wherein the composition and the percentage of the thin film negative electrode material are as follows: 60-80wt% of molybdenum disulfide nanosheet, 10-30wt% of nanocellulose, 5-20wt% of carbon nanotube and 5-20% of graphene. By adoption of the method, the renewable energy resource-cellulose can be utilized reasonably and effectively, so that a metal aluminum foil or a copper foil is not required to be used as a current collector; a fluorine-containing polymer is not required to be used as a binder; therefore, influences and hazards to the ecological environment can be greatly avoided; the electrode obtained by the method can be directly filter-pressed, assembled and molded without a tabletting process, so that the preparation method is high in efficiency; and in addition, the thin film negative electrode material is high in mechanical flexibility and continuous bending stability.
Description
Technical field
The present invention relates to a kind of flexible lithium ion battery film cathode material and its preparation method, particularly a kind of it is specifically related to utilize natural phant matter nano-cellulose as the flexible lithium battery film negative material of the molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound of flexible parent metal and its preparation method.
Background technology
Along with the rise of wearable electronic product, flexible electronic just develops to portable, bent, high-level efficiency, low cost and reusable edible direction, one of exploitation frivolous flexible lithium ion battery forward position becoming the research of energy storage field with bending stability. But it is not bent that the coating of current lithium ion battery and assembling technique determine tradition lithium ion battery, and bending can cause electrode materials to come off from collector and affect battery performance, even can be pierced through by barrier film, cause battery short circuit. Therefore, how to obtain frivolous flexibility and high performance lithium ion battery becomes the research focus in flexible electronics system field of future generation.
Realize flexible lithium ion battery, the electrode materials obtaining flexible bendable is crucial, mainly through preparing, flexible current-collecting body replaces tradition Copper Foil and aluminium foil in current existing work, and active material and collector are carried out integrated design, Mierocrystalline cellulose is that (every annual production is more than 7.5 �� 10 for the renewable organic polymer that on the earth, reserves are the highest10T), and cost is low, environmentally friendly, lightweight, the excellent properties such as collapsible, after nano-cellulose composite membrane-forming, prepare film cathode be expected to replace tradition Copper Foil and aluminium foil, simultaneously as collector and electrode materials, there is the advantages such as lightweight, flexibility and easy recycling disposal.
Molybdenumdisulphide, as cathode of lithium battery active material, has the features such as energy storage height, but is multilayer chip due to it, not easily the feature such as stripping and limit its application in lithium ion battery. The nano-cellulose aqueous solution that surface has active end group has excellent suspension stability, is conducive to the liquid phase mechanically peel of the two-dimensional layer material such as molybdenumdisulphide and Graphene.
The key issue of flexible electronic is still can the stability of retainer member when there is alternating bending and distortion, therefore higher requirement (Science is proposed for the characteristic of flexible parent metal and the interface performance between flexible parent metal and deposition material, 2009,323,1566). The flexible electrode reported is coat activated compound paste on carbon cloth and carbon nano-tube film, in this kind of electrode, there is between active substance and flexible current-collecting body poor bonding force, coming off of active substance can be caused through long-time bending, cause cycle performance to decline. Currently, flexible lithium ion battery field faces three aspect challenges: (1) has the flexible electrode material preparation of excellent bending stability; (2) raising of flexible electrode energy density and power density; (3) stability under the assembling of flexible lithium ion battery and bending state. The chemical property of the flexible lithium ion battery reported, particularly in high power performance (rapid charge), not yet reach the level of tradition lithium ion battery, therefore raising in high power performance is the difficult point of current flexible lithium ion battery research field, lower lithium ionic mobility and electroconductibility are the major reasons of restriction high power performance, another aspect major part flexible electrode research work is assembled into button-shaped half-cell and carries out chemical property, the chemical property of flexible electrode under bending state can not be studied, deviate practical application far away. Therefore, the novel flexible electrode structure with bending stability is urgently explored and develops, and the stability under the raising of flexible electrode energy density and power density and the assembling of flexible lithium ion battery and bending state becomes the key preparing flexible battery. Therefore, the present invention is by liquid phase mechanically peel, preparing individual layer or lack layer molybdenum disulfide nano sheet and single-layer graphene nanometer sheet, simultaneously using carbon nanotube as electro-conductive material, after compound, an one-step extrusion molding has prepared the fexible film negative material with excellent bending stability. In preparation process of the present invention, avoiding needing metal collector and organic adhesive when adopting tradition lithium cell to make, film cathode is simultaneously as electrode materials and collector, thus is conducive to preparing flexibility, lightweight, green recyclable lithium ion battery of future generation.
Summary of the invention
An object of the present invention is to provide the flexible lithium battery film negative material of a kind of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound.
The two of the object of the present invention are that the nano-cellulose water-sol providing utilization surface to have active end group is as liquid phase medium, the molybdenum disulfide nano sheet of minority layer is prepared by ultrasonication and ultrasonic stripping, with single-layer graphene jointly as active material, carbon nanotube is as electro-conductive material, nano-cellulose, as fiber mechanics skeleton and binding agent, prepares the method for flexible lithium ion thin film negative material.
For achieving the above object, the present invention adopts following technical scheme:
The flexible lithium battery film negative material of a kind of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound, it is characterized in that this negative material take nano-cellulose as flexible parent metal, being embedded in the network of described nano-cellulose, after molybdenum disulfide nano sheet, Graphene and carbon nanotube being mixed, the flexible self-supporting film electrode materials with fine and close network structure formed, the composition of this thin-film electrode material and mass percent be:
Molybdenum disulfide nano sheet 60��80wt%
Nano-cellulose 10��30wt%
Carbon nanotube 5��20wt%
Graphene 5��20wt%.
Above-mentioned Graphene is single-layer graphene nanometer sheet.
Above-mentioned molybdenumdisulphide obtains 1��5 layer of nanometer sheet through ultrasonic stripping.
Above-mentioned nano-cellulose is the nano-cellulose of surface with carboxyl, amino, acyl group or aldehyde groups modification.
The diameter of above-mentioned carbon nanotube is 30��50nm, and length is 5��12 ��m.
A kind of method of flexible lithium battery film negative material preparing above-mentioned molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound, it is characterised in that the concrete steps of the method are:
A. by after molybdenumdisulphide powder ball milling 20��30min, join mass percent concentration be 40 ~ 50wt% second alcohol and water mixed solvent in evenly disperse, then it is the nano-cellulose aqueous dispersions Homogeneous phase mixing of 1.0��3.0wt% with mass percent concentration, it is 600 ~ 900W at power, horn diameter is 0.6mm, under 10 ~ 20 DEG C of conditions after elementary ultrasonication process 8��20h, obtain few layer of molybdenum disulfide nano sheet/nano-cellulose mixed dispersion liquid;
B. in step a gained dispersion liquid, add Graphene, after ultrasonic stripping 2��3h, then add carbon nanotube, after continuing ultrasonic stripping 0.5��1h, evenly after dispersion, form the mixed dispersion liquid of molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube;
C. step b gained mixed dispersion liquid deionized water is diluted, obtain molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube aqueous dispersions that mass percent concentration is 20-30%, press filtration is extruded, make molybdenum disulfide nano sheet/graphene nanometer sheet/carbon nanotube be embedded in nano-cellulose network, form the wet film of fine and close network structure;
D. step C gained wet film is dried, obtain the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound.
The present invention prepares flexible cathode of lithium battery by press filtration extrusion molding, has following evident characteristic and advantage relative to conventional batteries negative pole:
(1) energy utilizing the inventive method rationally can efficiently utilize Mierocrystalline cellulose renewable, need not use metal aluminum foil, Copper Foil as collector, and fluoropolymer need not be used as tackiness agent, therefore greatly avoids the impact on ecotope and harm;
(2) utilize electrode that the inventive method obtains need not compressing tablet, direct press filtration assembled formation, efficiency height, and there is good mechanical flexibility and bend stability continuously.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail:
Embodiment one: concrete steps are as follows:
(1) elementary ultrasonication: get 0.2g ball milling 30min process after molybdenumdisulphide powder, join 20ml mass percent be 50wt%:50wt% second alcohol and water mixed solvent in evenly disperse. Then get the nano-cellulose of surface with carboxyl that 4.85g mass percent is 1.03wt%, it is diluted to, with deionized water, the even aqueous dispersion that mass percent is 0.25wt%, ultrasonic 15min. Joining in nano-cellulose dispersion liquid by molybdenumdisulphide dispersion liquid again, be 660w at power, horn is under 0.6mm ultrasound condition, under 15 DEG C of water cycle condensations after ultrasonication process 16h, obtains few layer of molybdenum disulfide nano sheet/nano-cellulose dispersion liquid. (2) secondary ultrasonic stripping: add 0.1g Graphene in molybdenumdisulphide ultrasonication processed/nano-cellulose dispersion liquid, then be 660w at power, horn is under 0.6mm ultrasound condition, and under 15 DEG C of water cycle condensations, ultrasonication processes ultrasonic 3h. Then by 10g mass percent concentration be 0.5wt% even carbon nanotube disperse wherein, continue supersound process 1h, finally forming uniform molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube dispersion liquid, its hundred points of mass ratioes are 60wt%:20wt%:10wt%:10wt%. (3) press filtration film forming and drying and processing: molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube mixed dispersion liquid deionized water is diluted, obtain the aqueous dispersions that mass percent is 20wt%, under the pressure effect of 1MPa, extrude dehydration, wet film is clipped in the middle of two sheet glass after completing by press filtration, 85 DEG C of vacuum-drying 15min, obtains flexible lithium battery film negative pole, thickness is 20 ��m, and square resistance is 100 Europe.
Embodiment two: concrete steps are as follows:
(1) elementary ultrasonication: by 0.3g ball milling 30min process after molybdenumdisulphide powder, join 20ml mass percent be 60wt%:40wt% second alcohol and water mixed solvent in evenly disperse. Getting the nano-cellulose of surface with acyl group that 3.9g mass percent is 1.54wt%, being diluted to mass percent with deionized water is 0.25wt%, ultrasonic 15min. Joining in nano-cellulose dispersion liquid by molybdenumdisulphide dispersion liquid again, be 660w at power, horn is under 0.6mm ultrasound condition, under 15 DEG C of water cycle condensations after ultrasonication process 20h, obtains few layer of molybdenum disulfide nano sheet/nano-cellulose dispersion liquid. (2) secondary ultrasonic stripping: add 0.12g Graphene in molybdenumdisulphide ultrasonication processed/nano-cellulose dispersion liquid, then be 660w at power, horn is under 0.6mm ultrasound condition, and under 15 DEG C of water cycle condensations, ultrasonication processes ultrasonic 3h. Then by 24g mass percent concentration be 0.5wt% even carbon nanotube disperse wherein, continue supersound process 1h, finally forming uniform molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube dispersion liquid, its mass percent is 50wt%:10wt%:20wt%:20wt%. (3) press filtration film forming and drying and processing: molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube mixed dispersion liquid deionized water is diluted, obtain the aqueous dispersions that mass percent is 20%, under the pressure effect of 1MPa, extrude dehydration, wet film is clipped in the middle of two sheet glass after completing by press filtration, 85 DEG C of vacuum-drying 15min, obtains flexible cathode of lithium battery film, thickness is 30 ��m, and square resistance is 60 Europe.
Although the solution of the present invention is open as above, but the technician for affiliated this area, it is possible to be easy to these embodiments are made various amendment. Therefore, the invention is not restricted to embodiment here, those skilled in the art are according to the announcement of the present invention, and improvement and the amendment the present invention made all should within protection scope of the present invention.
Claims (6)
1. the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound, it is characterized in that this negative material take nano-cellulose as flexible parent metal, being embedded in the network of described nano-cellulose, after molybdenum disulfide nano sheet, Graphene and carbon nanotube being mixed, the flexible self-supporting film electrode materials with fine and close network structure formed, the composition of this thin-film electrode material and mass percent be:
Molybdenum disulfide nano sheet 60��80wt%
Nano-cellulose 10��30wt%
Carbon nanotube 5��20wt%
Graphene 5��20wt%.
2. the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound according to claim 1, it is characterised in that described Graphene is single-layer graphene nanometer sheet.
3. the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound according to claim 1, it is characterised in that described molybdenumdisulphide obtains 1��5 layer of nanometer sheet through ultrasonic stripping.
4. the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound according to claim 1, it is characterised in that described nano-cellulose is the nano-cellulose of surface with carboxyl, amino, acyl group or aldehyde groups modification.
5. the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound according to claim 1, it is characterised in that the diameter of described carbon nanotube is 30��50nm, and length is 5��12 ��m.
6. prepare the method for the flexible lithium battery film negative material of the molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound according to Claims 1-4 for one kind, it is characterised in that the concrete steps of the method are:
A. by after molybdenumdisulphide powder ball milling 20��30min, join mass percent concentration be 40 ~ 50wt% second alcohol and water mixed solvent in evenly disperse, then it is the nano-cellulose aqueous dispersions Homogeneous phase mixing of 1.0��3.0wt% with mass percent concentration, it is 600 ~ 900W at power, horn diameter is 0.6mm, under 10 ~ 20 DEG C of conditions after elementary ultrasonication process 8��20h, obtain few layer of molybdenum disulfide nano sheet/nano-cellulose mixed dispersion liquid;
B. in step a gained dispersion liquid, add Graphene, after ultrasonic stripping 2��3h, then add carbon nanotube, after continuing ultrasonic stripping 0.5��1h, evenly after dispersion, form the mixed dispersion liquid of molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube;
C. step b gained mixed dispersion liquid deionized water is diluted, obtain molybdenum disulfide nano sheet/nano-cellulose/graphene/carbon nano-tube aqueous dispersions that mass percent concentration is 20-30%, press filtration is extruded, make molybdenum disulfide nano sheet/graphene nanometer sheet/carbon nanotube be embedded in nano-cellulose network, form the wet film of fine and close network structure;
D. step C gained wet film is dried, obtain the flexible lithium battery film negative material of molybdenum disulfide nano sheet/nano-cellulose/carbon nano tube/graphene compound.
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