CN101924246A - Preparation method of composite solid electrolyte based on polyphosphazene carbide micro-nanometer material - Google Patents

Preparation method of composite solid electrolyte based on polyphosphazene carbide micro-nanometer material Download PDF

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Publication number
CN101924246A
CN101924246A CN2010102754522A CN201010275452A CN101924246A CN 101924246 A CN101924246 A CN 101924246A CN 2010102754522 A CN2010102754522 A CN 2010102754522A CN 201010275452 A CN201010275452 A CN 201010275452A CN 101924246 A CN101924246 A CN 101924246A
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polyphosphazene
nanometer material
carbide micro
solid electrolyte
composite solid
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黄小彬
张家维
唐小真
陈奎永
顾晓俊
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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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 relates to a preparation method of composite solid electrolyte based on a polyphosphazene carbide micro-nanometer material, which belongs to the technical field of lithium batteries, the polyphosphazene carbide micro-nanometer material is dispersed in acetonitrile, then polyoxyethylene and lithium hypochlorite are sequentially added and evenly stirred by magnetic force, and then the mixed solution is poured into a polytetrafluoroethylene mould board, thus obtaining the composite solid polymer electrolyte. Compared with the existing electrolyte, the product has higher conductivity and larger lithium ion transference number, good mechanical properties and good electrochemical stability.

Description

Method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material
Technical field
What the present invention relates to is dielectric of a kind of technical field of lithium batteries and preparation method thereof, specifically is a kind of method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material.
Background technology
The all solid state lithium ion polymer battery is owing to having high-energy-density, excellent cycle performance, can being processed into arbitrary shape and plurality of advantages such as safe and reliable is expected to become one of following most promising advanced power supply.The PEO base polymer electrolyte is subjected to extensive concern for a long time because of the electrolyte that it may substitute the liquid electrolyte in traditional lithium ion battery and becomes in all solid state lithium ion polymer battery.Active development has higher conductivity at room temperature and lithium ion transference number TLi +, the polymer dielectric of the electrochemical stability window of good electrode interface stability performance, excellent mechanics and processing characteristics and broad is the important foundation of development all solid state lithium ion polymer battery.Studies show that in a large number above-mentioned performance all can suitably be improved after mixing inorganic filler in the PEO base polymer electrolyte obtains composite polymer electrolyte.But traditional inorganic ceramic filler and the layered fillers effect aspect ionic conductivity that improves polymer dielectric and lithium ion transference number reported of document at present is less, and therefore the exploitation new packing that can more effectively improve the ionic conductivity of PEO base polymer electrolyte and lithium ion transference number is of great importance to the practical application of all solid state lithium ion polymer battery.
Since the eighties in 20th century, along with some have the new carbon of nano-scale, as C 20, C 60Deng the discovery of fullerene family, carbon nano-tube, carbon nano-fiber etc., material with carbon element has caused common people's extensive concern day by day owing to the diversity of its form.In recent years, size spherical material with carbon element different with structure from the nanoscale to the micron order successfully prepares by diverse ways, greatly enriched the research field of material with carbon element.Carbosphere, carbon nano-tube, carbon fiber etc. have high-specific surface area, large pore volume, chemical stability and favorable mechanical performance usually, thereby are with a wide range of applications.The aperture of most porous carbons all below 2nm, belongs to micropore (rnicroporous) material, and their microporous properties can obtain applications well at aspects such as absorption, separation, ultracapacitor and micromolecule catalytic reactions.This class material is mainly obtained through charing and then activation by presoma at present.
The poly phosphazene micro Nano material is based on the micro Nano material of the organic inorganic hybridization of the class novelty that ring cross-linking type poly phosphazene obtains, the poly phosphazene micro Nano material has different patterns, its component units is mainly organic principle, with various macromolecular materials good compatibility and affinity are arranged all, a lot of superiority is arranged with respect to inorganic nano material.And the poly phosphazene micro Nano material also possesses the advantage of the easy chemical modification of poly phosphazene material, can obtain the surface of various chemical property by simple nucleophilic substitution.Adopt the poly phosphazene micro Nano material to do filler and design composite polymer electrolyte, be expected to obtain combining the NEW TYPE OF COMPOSITE polymer dielectric of poly phosphazene electrolyte advantage, obtain the better chemical property of composite polymer electrolyte, the development and application of greatly expanding composite polymer electrolyte than traditional inorganic nano-particle doping.
Find through literature search prior art, Zhang Jiawei, Huang Xiaobin, Tang Xiaozhen etc. are at Chinese patent " based on the method for preparing composite solid electrolyte of polyphosphazenes micron-sphere " (application number: 201010136533.4), mention with PEO 8-LiClO 4Make parent, polyphosphazenes micron-sphere is a filler, makes PEO 8-LiClO 4The serial composite polymer electrolyte of-PZSMS (x%) is measured this electrolytical conductivity, lithium ion transference number and electrochemical stability window.The result shows that micro-nano filler of poly phosphazene and PEO matrix have good compatibility, and the introducing of polyphosphazenes micron-sphere has significantly improved the conductivity of composite solid electrolyte, reaches 1.2 * 10 in the time of 25 ℃ -5S cm -1, lithium ion transference number also is improved, and reaches 0.29, and electrochemical stability window is 5.0V.But the surface area of the poly phosphazene micro Nano material that in-situ polymerization generates is less and the space is less, limited the further raising of the electrolytical electrical property of solid composite polymeric thing, therefore, utilize high porosity but still hybridized atom that contain on the poly phosphazene promotes the particle of the electrolytical electrical property of solid composite polymeric thing just to become a valuable research direction as filler.The poly phosphazene micro-and nano-particles not only can be prepared variforms such as multiform polyphosphazene nanotube, nanofiber and poly (organophosphazenes) microsphere under gentle and easy condition, conveniently carry out surface chemical modification, and results of elemental analyses shows that these micro Nano materials have the carbon content up to about 45%, can under inert atmosphere conditions, carry out high temperature cabonization to these polymeric materials, drive away non-carbon component, obtain char-forming material fast, obtain carbon nano-tube, carbon nano-fiber and the carbosphere of porous.This provides a brand-new approach for the electrolytical exploitation of nano composite polymer.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material is provided, pass through polyphosphazene, polyphosphazene nanotube and polyphosphazenes micron-sphere are presoma, prepared carbon nano-fiber by high temperature cabonization, carbon nano-tube and carbosphere and be that filler has prepared composite polymer electrolyte with the material after the carbonization have obtained the solid composite polymeric thing electrolyte that conductivity and lithium ion transference number all improve.Composite solid electrolyte conductivity height of the present invention, satisfactory mechanical property has good electrochemical stability.
The present invention is achieved by the following technical solutions, to add polyethylene glycol oxide and lithium hypochlorite and magnetic agitation behind the acetonitrile successively even by polyphosphazene carbide micro-nanometer material is scattered in the present invention, mixed solution is cast to obtains the complex solid polymer dielectric in the polytetrafluoroethylene template again.
Described polyethylene glycol oxide and polyphosphazene carbide micro-nanometer material mass percent are 0.1%～1%;
The oxygen atom in the described polyethylene glycol oxide and the molar percentage of the lithium atom in the lithium hypochlorite are: 8%～20%;
Described dispersion is meant: ultrasonic dispersion 10～60 minutes;
Described magnetic agitation is 5～25 hours.
Described being cast in the polytetrafluoroethylene template is meant: mixed solution is cast on the polytetrafluoroethylene template with the volatilization acetonitrile under 50 ℃ vacuum environment dry 24～48 hours then.
The molecular weight Mw of described polyethylene glycol oxide is 100,000～1000,000;
The molecular weight Mw of described lithium hypochlorite is 106.5;
The filler molecular weight Mw of described polyphosphazene carbide micro-nanometer material is 500～1380, is specially polyphosphazenes micron-sphere, nanotube or nanofiber through the inert atmosphere high temperature cabonization.
The present invention has emphasized the improved action of different polyphosphazene carbide micro-nanometer materials to complex solid polymer dielectric (CPE).The form of polyphosphazene carbide micro-nanometer material and content are to conductivity, lithium ion transference number and the electrochemical stability window important influence of composite polymer electrolyte.
Complex solid polymer dielectric prepared in accordance with the present invention, especially use the complex solid polymer dielectric of polyphosphazene carbide micro-nanometer material as filler, room-temperature conductivity height not only, and satisfactory mechanical property, do not contain any liquid component, smooth surface is smooth, and internal composition is even, and high lithium ion transference number and electrochemical stability window are arranged.
Description of drawings
Fig. 1 is the scanning electron microscopy SEM photo of polyphosphazene carbide micron ball.
Fig. 2 is the scanning electron microscopy SEM photo of polyphosphazene carbide nanotube.
Fig. 3 is the scanning electron microscopy SEM photo of polyphosphazene carbide nanofiber.
Fig. 4 is the scanning electron microscopy SEM photo of the complex solid polymer dielectric that polyphosphazene carbide micron ball mixes among the embodiment 1.
Fig. 5 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide micron balls in the system.X=0.5 represents that the polyphosphazene carbide micron ball that adds is 0.5%, and X=1 represents that the polyphosphazene carbide micron ball that adds is 1%.
Fig. 6 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide nanotubes in the system.X=0.5 represents that the polyphosphazene carbide nanotube that adds is 0.5%, and X=1 represents that the polyphosphazene carbide nanotube that adds is 1%.
Fig. 7 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide nanofibers in the system.X=0.5 represents that the polyphosphazene carbide nanofiber that adds is 0.5%, and X=1 represents that the polyphosphazene carbide nanofiber that adds is 1%.
Embodiment
Below embodiments of the invention are elaborated, present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed execution mode and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1 takes by weighing 0.005g polyphosphazene carbide micron ball (polyphosphazene carbide micron ball quality be PEO quality 0.5%) and joins in the 30ml acetonitrile ultrasonic dispersion 15 minutes;
Step 2 takes by weighing the PEO (Mw～300,000) of 1.0g and the LiClO of 0.242g respectively 4(PEO and LiClO 4The O/Li mol ratio be 10: 1) join in the acetonitrile dispersion liquid of polyphosphazene carbide micron ball magnetic stirrer dissolving 8 hours;
Step 3 is cast to the mixed solution that obtains on the polytetrafluoroethylene template, solvent flashing 6 hours;
Step 4 is transferred to the polymer dielectric film that obtains in the step 3 in the vacuum drying chamber, and 50 ℃ were continued down dry 24 hours, and can obtain the complex solid polymer dielectric.
The implementation result of present embodiment: Fig. 1 is the scanning electron microscopy SEM photo of the polyphosphazene carbide micron ball of preparation.As can be seen from the figure, poly (organophosphazenes) micron bulb diameter distribution homogeneous, decentralization is fine; Fig. 4 is the scanning electron microscopy SEM photo of the complex solid polymer dielectric of the polyphosphazene carbide micron ball doping of preparation.As can be seen from the figure, the surface smoothing homogeneous of film proves that polyphosphazene carbide micron ball and PEO polymer dielectric matrix have good compatibility.Fig. 5 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide micron balls in the system.The room-temperature conductivity that sign by composite polymer electrolyte calculates is 2.7 * 10 -5S cm -1, improving two orders of magnitude than the room-temperature conductivity of pure PEO, lithium ion transference number is 0.44, electrochemical stability window is 5.0V.Above characterization result shows that this composite polymer electrolyte has high room-temperature conductivity and high electrochemical stability window, and high lithium ion transference number, can be used as the lithium ion battery solid electrolyte material and uses.
Embodiment 2
Step 1 takes by weighing 0.0025g polyphosphazene carbide nanotube (polyphosphazene carbide nanotube quality be PEO quality 0.25%) and joins in the 40ml acetonitrile ultrasonic dispersion 20 minutes;
Step 2 takes by weighing the PEO (Mw～400,000) of 1.0g and the LiClO of 0.3025g respectively 4(PEO and LiClO 4The O/Li mol ratio be 8: 1) join in the acetonitrile dispersion liquid of polyphosphazene carbide nanotube magnetic stirrer dissolving 9 hours;
Step 3 is cast to the mixed solution that obtains on the polytetrafluoroethylene template, solvent flashing 7 hours,
Step 4 is transferred to the polymer dielectric film that obtains in the step 3 in the vacuum drying chamber, and 50 ℃ were continued down dry 28 hours, and can obtain the complex solid polymer dielectric.
The implementation result of present embodiment: the sign of complex solid polymer dielectric such as embodiment 1.Fig. 2 is the scanning electron microscopy SEM photo of the polyphosphazene carbide nanotube of preparation.As can be seen from the figure, the diameter distribution homogeneous of polyphosphazene carbide nanotube, the polyphosphazene nanotube length after the carbonization is several microns, and the two ends external diameter is about 150 nanometers, and decentralization is fine; Fig. 6 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide nanotubes in the system.This composite polymer electrolyte room-temperature conductivity is 2.67 * 10 -5S cm -1, lithium ion transference number is 0.5, electrochemical stability window is 5.0V.This composite polymer electrolyte has high room-temperature conductivity and high electrochemical stability window equally, and high lithium ion transference number, can be used as the lithium ion battery solid electrolyte material and uses.
Embodiment 3
Step 1 takes by weighing 0.0075g polyphosphazene carbide nanofiber (polyphosphazene carbide nanofiber quality be PEO quality 0.75%) and joins in the 45ml acetonitrile ultrasonic dispersion 30 minutes;
Step 2 takes by weighing the PEO (Mw～500,000) of 1.0g and the LiClO of 0.2017g respectively 4(PEO and LiClO 4The O/Li mol ratio be 12: 1) join in the acetonitrile dispersion liquid of polyphosphazene carbide nanofiber magnetic stirrer dissolving 10 hours;
Step 3 is cast to the mixed solution that obtains on the polytetrafluoroethylene template, solvent flashing 8 hours,
Step 4 is transferred to the polymer dielectric film that obtains in the step 3 in the vacuum drying chamber, and 50 ℃ were continued down dry 32 hours, and can obtain the complex solid polymer dielectric.
The implementation result of present embodiment: the sign of complex solid polymer dielectric such as embodiment 1.Fig. 3 is the scanning electron microscopy SEM photo of the polyphosphazene carbide nanofiber of preparation.As can be seen from the figure, polyphosphazene diameter distribution homogeneous, the polyphosphazene length after the carbonization is several microns, and the two ends external diameter is about the 200-500 nanometer, and decentralization is fine; Fig. 7 is at PEO 10-LiClO 4Conductivity-the temperature curve that adds different amount polyphosphazene carbide nanofibers in the system.This composite polymer electrolyte room-temperature conductivity is 3.25 * 10 -5S cm -1, lithium ion transference number is 0.51, electrochemical stability window is 5.0V.This composite polymer electrolyte has high room-temperature conductivity and high electrochemical stability window equally, and high lithium ion transference number, can be used as the lithium ion battery solid electrolyte material and uses.

Claims (10)

1. method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material, it is characterized in that, to add polyethylene glycol oxide and lithium hypochlorite and magnetic agitation behind the acetonitrile successively even by polyphosphazene carbide micro-nanometer material is scattered in, and mixed solution is cast to obtains the complex solid polymer dielectric in the polytetrafluoroethylene template again.
2. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, described polyethylene glycol oxide and polyphosphazene carbide micro-nanometer material mass percent are 0.1%～1%.
3. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, the oxygen atom in the described polyethylene glycol oxide and the molar percentage of the lithium atom in the lithium hypochlorite are: 8%～20%.
4. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, described dispersion is meant: ultrasonic dispersion 10～60 minutes.
5. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, described magnetic agitation is 5～25 hours.
6. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1, it is characterized in that, described being cast in the polytetrafluoroethylene template is meant: mixed solution is cast on the polytetrafluoroethylene template with the volatilization acetonitrile under 50 ℃ vacuum environment dry 24～48 hours then.
7. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, the molecular weight Mw of described polyethylene glycol oxide is 100,000～1000,000.
8. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1 is characterized in that, the molecular weight Mw of described lithium hypochlorite is 106.5.
9. the method for preparing composite solid electrolyte based on polyphosphazene carbide micro-nanometer material according to claim 1, it is characterized in that, the filler molecular weight Mw of described polyphosphazene carbide micro-nanometer material is 500～1380, is specially polyphosphazenes micron-sphere, nanotube or nanofiber through the inert atmosphere high temperature cabonization.
10. a composite solid electrolyte is characterized in that, described preparation method obtains by above-mentioned arbitrary claim.
CN2010102754522A 2010-09-07 2010-09-07 Preparation method of composite solid electrolyte based on polyphosphazene carbide micro-nanometer material Pending CN101924246A (en)

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN105280952A (en) * 2015-09-17 2016-01-27 上海交通大学 Composite all-solid-state polymer electrolyte material and preparation method thereof
CN107615553A (en) * 2015-06-08 2018-01-19 富士胶片株式会社 Solid electrolyte composition, solid state secondary battery electrode slice, solid state secondary battery and the manufacture method of solid state secondary battery electrode slice and solid state secondary battery
CN108927185A (en) * 2018-08-02 2018-12-04 临沂大学 A kind of oxygen reduction catalyst and preparation method thereof of the carbon nanotube loaded phosphatization Fe nanometer particles of Heteroatom doping
CN113078352A (en) * 2021-03-26 2021-07-06 无锡纤发新材料科技有限公司 Solvent and porous carbon reinforced composite polymer electrolyte and method thereof
CN113823766A (en) * 2021-11-22 2021-12-21 河南电池研究院有限公司 Cathode for solid lithium ion battery and preparation method thereof

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CN1915807A (en) * 2006-09-07 2007-02-21 上海交通大学 Method for preparing Nano carbon fiber
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Publication number Priority date Publication date Assignee Title
CN107615553A (en) * 2015-06-08 2018-01-19 富士胶片株式会社 Solid electrolyte composition, solid state secondary battery electrode slice, solid state secondary battery and the manufacture method of solid state secondary battery electrode slice and solid state secondary battery
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CN108927185A (en) * 2018-08-02 2018-12-04 临沂大学 A kind of oxygen reduction catalyst and preparation method thereof of the carbon nanotube loaded phosphatization Fe nanometer particles of Heteroatom doping
CN113078352A (en) * 2021-03-26 2021-07-06 无锡纤发新材料科技有限公司 Solvent and porous carbon reinforced composite polymer electrolyte and method thereof
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CN113823766A (en) * 2021-11-22 2021-12-21 河南电池研究院有限公司 Cathode for solid lithium ion battery and preparation method thereof

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Application publication date: 20101222