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WO2017207036A1 - Procédé de production d'un nanocomposite, nanocomposite et utilisation de celui-ci - Google Patents

Procédé de production d'un nanocomposite, nanocomposite et utilisation de celui-ci Download PDF

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Publication number
WO2017207036A1
WO2017207036A1 PCT/EP2016/062294 EP2016062294W WO2017207036A1 WO 2017207036 A1 WO2017207036 A1 WO 2017207036A1 EP 2016062294 W EP2016062294 W EP 2016062294W WO 2017207036 A1 WO2017207036 A1 WO 2017207036A1
Authority
WO
WIPO (PCT)
Prior art keywords
nanocomposite
carbon nanostructures
ethylene carbonate
producing
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2016/062294
Other languages
German (de)
English (en)
Inventor
Stefan Matthias Winfried Theuerkauf
Mihail Rudolfovich PREDTECHENSKIY
Aleksandr Evgenevich BEZRODNY
Dmitriy Vladimirovich YUDAEV
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TARANIS GmbH
Original Assignee
TARANIS GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by TARANIS GmbH filed Critical TARANIS GmbH
Priority to PCT/EP2016/062294 priority Critical patent/WO2017207036A1/fr
Publication of WO2017207036A1 publication Critical patent/WO2017207036A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • H01M4/62—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

Definitions

  • the present invention relates to a method for producing a nanocomposite, nanocomposite and its use
  • Nanoscale composites also referred to as nanocomposite (s) s, are materials of at least two components, of which at least one component has a nanoscale structure, ie. H. at least one dimension is in the range of 1 to 100 nm.
  • the second component may be a liquid
  • thermoplastic or crosslinked polymers into consideration, wherein the thermoplastic materials predominate in the application.
  • nanoparticles as a component for composites are typically highly agglomerated.
  • Nanoparticles in the matrix prevent a loss of the surface, so that unique and special properties of the composites can be achieved by the interaction of the different phases at their interface.
  • nanostructured composites is max. 5% by weight, the surface / volume correlation of the filler phase being very high.
  • the properties of the nanostructured composites are usually very closely related to the particle morphology of their fillers and to the interreaction of the interacting constituents.
  • the effect of nanostructuring usually occurs when using nanoparticles with extended molecules of complicated geometrical shapes, such as nanotubes, nanofibres, etc., because they have a very large surface area.
  • New scientific studies show that carbon nanotubes, thanks to their enormous mechanical strength and elasticity, are very future-oriented nanostructured
  • Nanoparticles present in the matrix are present in the matrix.
  • composites using carbon nanotubes should therefore not form bundles and / or agglomerates of carbon nanotubes or, if they arise or are present, be dissolved. Dispersing when using rotary mixers, piston homogenizers, ball and colloid mills can not guarantee the required degree of separation.
  • a process in which liquid ethylene carbonate is contacted with a given amount of carbon nanostructures is subjected, thus obtained a mixture of liquid ethylene carbonate and carbon nanostructures, an ultrasonic treatment until a uniform distribution of
  • Carbon nanostructures is achieved in the liquid ethylene carbonate, and the mixture is then converted into the solid phase.
  • Carbon nanostructures dispersed by means of ultrasonic treatment in a matrix which is solid under normal conditions. It has surprisingly been found that
  • Ultrasonic treatment can also be chopped, which is particularly noticeable when using "long"
  • Carbon nanostructures has a positive effect on the later properties.
  • Carbon nanostructures which are all liquid, have the disadvantage that they segregate over time, ie the compositions can only be used for a relatively short time without reprocessing.
  • Opposite polymers Ethylene carbonate has the advantage that this relatively easy from a manufactured on the basis of the nanocomposite
  • the carbon nanostructures are brought into contact with liquid ethylene carbonate.
  • the mixture is granulated after conversion into the solid phase.
  • the carbon nanostructures in the ethylene carbonate can be dispersed very well by means of ultrasonication, to such an extent that agglomerates of a plurality of carbon nanostructures are broken up.
  • ultrasonication it is provided in a preferred embodiment that before
  • At least one dispersant selected from a group comprising polyvinylpyrrolidone, polyvinyl acetate, polyvinyl alcohol, block copolymer
  • Vinylpyrrolidone and vinylcaprolactam or at least one
  • the dispersing agent or a corresponding mixture, can be used before or during the
  • Sonication be added. In order to achieve the best possible effect of the dispersant, it is preferred that this already before contacting the ethylene carbonate with the carbon nanostructures to add the ethylene carbonate. It is also possible successively to add different dispersants or mixtures thereof.
  • the dispersant (s) used may have a
  • Dispersant based on the amount
  • Carbon nanostructures have special physical properties
  • the object of the invention is further achieved by a
  • Nanocomposite for producing an electrode for a lithium-ion battery obtainable according to the previously described
  • the solid form of the nanocomposite prevents it from becoming segregated over time, so that the homogeneity of the distribution of the carbon nanostructures is lost.
  • the nanocomposite according to the invention comprises ethylene carbonate as matrix material and 0.01-1% by weight, preferably 0.01-0.1% by weight, of carbon nanostructures as filler, wherein the
  • Carbon nanostructures are selected from a group comprising single-walled, two-walled or multi-walled
  • the nanocomposite according to the invention can furthermore have from 0.3 to 20% by weight, preferably from 0.3 to 10% by weight, of at least one dispersant, based on the amount of carbon nanostructures.
  • the dispersing agent may be selected from a group comprising polyvinylpyrrolidone, polyvinyl acetate, polyvinyl alcohol,
  • Block copolymer of vinylpyrrolidone and vinylcaprolactam or mixtures thereof.
  • the invention further relates to the use of a
  • Nanocomposites comprising carbon nanostructures and
  • Ethylene carbonate for producing electrodes of lithium-ion batteries.
  • the electrodes For the preparation of the electrodes, the
  • nanocomposite for example, granulated nanocomposite, together with other constituents of the later electrode, can be extruded.
  • Dispersant prepared by adding the ethylene carbonate to about
  • Carbon nanostructures and dispersants are added.
  • the resulting mixture is about 30 minutes one
  • the ultrasound treatment can be both continuous and in cycles of about 0.5-5
  • Carbon nanostructures in the ethylene carbonate, agglomerates are broken up. After sonication, the carbon nanostructures are evenly distributed in the
  • filler carbon nanotubes are used as filler carbon nanotubes.
  • the proportion of actual carbon nanotubes on the filler is at least 75%.
  • the carbon nanotubes have a diameter of 1-2 nm and a length of 1-2 mm.
  • Dispersant is polyvinylpyrrolidone (Luvitec K30, BASF) is used.
  • concentration of carbon nanotubes is 0.01 to 0.1 wt.% Of the matrix, that is ethylene carbonate.
  • the mass of polyvinylpyrrolidone is between 0.3 to 10% by weight of the carbon nanotubes.
  • the filler and the dispersant are fed to the ethylene carbonate heated to 50 ° C. Subsequently, the mixture is subjected to an ultrasonic treatment, namely by means of an ultrasound system (company U-Sonic Type UZTA-0,4 / 22-OM, power 400 W, frequency 22kHz). The ultrasound treatment is carried out in 2.5-minute cycles over a period of 30 minutes. The obtained dispersion is cooled to room temperature and hardens.
  • the preparation of the nanocomposite is carried out according to the method described in Example 1.
  • the preparation of the nanocomposite is carried out according to the method described in Example 1.
  • Dispersant polyvinyl acetate 25, plastic polymer
  • the preparation of the nanocomposite is carried out according to the method described in Example 1.
  • the preparation of the nanocomposite is carried out according to the method described in Example 1.
  • Dispersion with constant stirring the following substances, preferably in succession, are fed: conductive carbon with 0.001 wt.% Of the dispersion, lithium ferrum phosphate with 0.8 wt.% Of the dispersion, polyvinylidene fluoride with 0.06 wt.% Of
  • the resulting paste is dried with an IR lamp.
  • the recovered cathode material for the production of lithium-ion batteries contains no harmful solvent (such as the otherwise usual in the manufacture of electrodes N-methylpyrrolidone) and is thus considered completely harmless from an ecological point of view.
  • the nanocomposite obtained in Example 2 is subjected to inert
  • Dispersion with constant stirring the following substances, preferably in succession, are fed: conductive carbon with 0.03 wt.% Of the dispersion, lithium ferrum phosphate with 1 wt.% Of the dispersion, polyvinylidene fluoride with 0.08 wt.% Of the dispersion.
  • the resulting paste is dried with an IR lamp.
  • the recovered cathode material for the production of lithium-ion batteries contains no harmful solvent (such as the otherwise usual in the manufacture of electrodes N-methylpyrrolidone) and is thus considered completely harmless from an ecological point of view.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

La présente invention concerne un procédé de production d'un nanocomposite, le nanocomposite lui-même et son utilisation. Dans les nanocomposite connus comportant des nanostructures de carbone comme matière de remplissage, le degré élevé d'agglomération de la matière de remplissage est un problème. Selon l'invention, cet problème est résolu en ce que du carbonate d'éthylène liquide est mis en contact avec une quantité prédéterminée de nanostructures de carbone, en ce qu'un mélange ainsi obtenu de carbonate d'éthylène liquide et de nanostructures de carbone est mis à un traitement par ultrasons jusqu'à obtenir une distribution uniforme des nanostructures de carbone dans le carbonate d'éthylène liquide, et en ce que le mélange est transformé en la phase solide. Le traitement par ultrasons du carbonate d'éthylène liquide permet de briser les agglomérats et de les empêcher de se reformer. La transformation en la phase solide permet de stocker le nanocomposite obtenu pendant une longue période sans que la matière de charge ne s'agglomère à nouveau.
PCT/EP2016/062294 2016-05-31 2016-05-31 Procédé de production d'un nanocomposite, nanocomposite et utilisation de celui-ci Ceased WO2017207036A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/EP2016/062294 WO2017207036A1 (fr) 2016-05-31 2016-05-31 Procédé de production d'un nanocomposite, nanocomposite et utilisation de celui-ci

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2016/062294 WO2017207036A1 (fr) 2016-05-31 2016-05-31 Procédé de production d'un nanocomposite, nanocomposite et utilisation de celui-ci

Publications (1)

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WO2017207036A1 true WO2017207036A1 (fr) 2017-12-07

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100272978A1 (en) * 2007-10-11 2010-10-28 Georgia Tech Research Corporation Carbon fibers and films and methods of making same
JP2011076948A (ja) * 2009-09-30 2011-04-14 Toray Ind Inc 導電性複合体およびリチウムイオン電池用負極。
US20140001416A1 (en) * 2010-12-21 2014-01-02 Bayer Intellectual Property Gmbh Method for producing powdery polymer/carbon nanotube mixtures

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100272978A1 (en) * 2007-10-11 2010-10-28 Georgia Tech Research Corporation Carbon fibers and films and methods of making same
JP2011076948A (ja) * 2009-09-30 2011-04-14 Toray Ind Inc 導電性複合体およびリチウムイオン電池用負極。
US20140001416A1 (en) * 2010-12-21 2014-01-02 Bayer Intellectual Property Gmbh Method for producing powdery polymer/carbon nanotube mixtures

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
VAISMAN ET AL: "Polymer-nanoinclusion interactions in carbon nanotube based polyacrylonitrile extruded and electrospun fibers", POLYMER, ELSEVIER SCIENCE PUBLISHERS B.V, GB, vol. 48, no. 23, 17 October 2007 (2007-10-17), pages 6843 - 6854, XP022313444, ISSN: 0032-3861, DOI: 10.1016/J.POLYMER.2007.09.032 *

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