EP1687360A1 - Polymergebundene, funktionale werkstoffe - Google Patents
Polymergebundene, funktionale werkstoffeInfo
- Publication number
- EP1687360A1 EP1687360A1 EP04765825A EP04765825A EP1687360A1 EP 1687360 A1 EP1687360 A1 EP 1687360A1 EP 04765825 A EP04765825 A EP 04765825A EP 04765825 A EP04765825 A EP 04765825A EP 1687360 A1 EP1687360 A1 EP 1687360A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- mat
- shear
- polymer
- rolling
- materials
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
Definitions
- the invention relates to a process for the production of polymer composites, consisting of a polymer matrix, preferably composed of polytetrafluoroethylene (PTFE), in which a particulate material of certain functionality is incorporated.
- PTFE polytetrafluoroethylene
- Polymer composites derived therefrom and their specific applications are also the subject of the invention.
- U.S. Patents 3,556,161 and 3,890,417 describe the manufacture of pure, free-standing and porous Teflon films.
- a paste is preferably mixed from Teflon powder, solvent and metal powders or salts, which are insoluble in the solvent and can be easily removed, kneaded, and finally rolled out into a film.
- the film is then folded once, rotated by 90 ° with respect to the preferred (rolling) direction and rolled out again under the application of pressure.
- the distance between the rollers can be reduced after each process to adjust the final thickness.
- the folding / turning / rolling out process is repeated several times until a cross-linked structure is built up from polymer thread.
- a subsequent, combined folding / The rolling process as described above converts the dough into a stable, free-standing compound, and the porosity of the electrode is adjusted according to established processes by evaporating liquids that were added to the dough before the RoU process after the manufacturing process.
- the highly fibrillated mixtures after the shear-grinding process can also be rolled out directly and without the described Fal Roll process to free-standing electrodes.
- this direct rolling process can be used in a continuous process.
- a thermal sintering step is often used to support the mechanical properties of these directly applied foils, which are lower compared to excessive shear / fibrillation in repeated folding / rolling processes. Examples of these methods are described in U.S. Patents 4,354,958, 4,379,772 and 6,335,857.
- a disadvantage of the methods used hitherto is the elevated temperature which is necessary for processing or for achieving a good result. Furthermore, a composite with a very high density cannot be created because the solvent present in the processing process prevents further compression.
- the object of the invention is to produce free-standing polymer-bound mats in a cold-forming process, which optimized using low process pressures Have properties with regard to their functionality and mechanical properties. No elevated temperature is necessary for the process. Processing prior to rolling, such as grinding the mixture, is also not required.
- the properties of the film are achieved by deliberately using a bimodal particle size distribution between polymer particles and shear particles. This increases the shear forces on the polymer particles and improves the fibrillation properties. Using low process pressures during a folding / rolling process, a highly fibrillated network can be built up without the need for additional, stabilizing sintering steps.
- a high packing density of the active, functional material in the polymer composite can be achieved by continuously drying the composite during the shear / fibrillation processes.
- the mass to be processed is specifically moistened in the first folding / rolling steps and then, if there is sufficient stability during the scrubbing process, is specifically dried using moisture-absorbing methods.
- e.g. B. battery electrodes this leads to a high energy density; in the case of e.g. So ⁇ tionsfolien, which are made of activated carbon, to a high volumetri see Adso ⁇ tionskraft; in the case of e.g. Films for electrostatic shielding for a high electrical conductivity in the composite.
- the new process can also be used to produce a completely new form of graphite composite mat.
- the mechanical forces during fibrillation cause the graphite crystallite structure to be deformed.
- This structure has a positive effect on the charging / discharging properties when used as an intercalation electrode for rechargeable lithium-ion batteries.
- the present invention relates to the following aspects and embodiments:
- a first aspect relates to a process for the production of polymer composites, produced from one or more shear materials, materials and shearable polymer particles, the polymer particles having a share of 0.1-20% by weight in the total mass of the end product, and the size ratio of Shear to Polyme ⁇ umble from 5: 1 to 2000: 1, with the following steps: providing one or more shear materials, materials and Polyme ⁇ art specially; Dispersing the materials in a solvent to form a dough; intensive mixing of the dough obtained; Rolling out the dough into a mat; folding the mat thus obtained one or more times and rolling it out at an angle between 45 ° and 135 °, preferably 90 ° (vertical), to the respective previous rolling / preferred direction.
- the special stability of the film is achieved by using a bimodal particle size distribution between the polymer article and the article.
- the shear particles of the shear material are spun by the sheared polymer particles during the process. This creates a fibrillated network that holds the entire network together.
- the polymer particles must be shearable or inelastically deformable. Cross-linking of the individual strands is not necessary.
- the Polyme ⁇ elle therefore need not be cross-linked by condensation or other types of polymerization.
- the proportion of polymer in the total mass of the films is in the range from 0.1 to 20% by weight, preferably in the range from 1 to 15% by weight and more preferably in the range from 5 to 10% by weight.
- the size distribution of the Sche ⁇ umble and the Polyme ⁇ modifier is essential for the invention. There must be a bimodal particle distribution. This bimodal distribution increases the shear forces and improves the fibrillation properties. Using low process pressures, a highly fibrillated network can be built up during a folding / rolling process without the need for additional, stabilizing sintering steps.
- the size ratio of the shear material to the polymer article is between 5: 1 and 2000: 1, preferably between 10: 1 and 500: 1, more preferably between 15: 1 and 100: 1.
- the materials are dispersed in a solvent to form a dough. The solvent facilitates a homogeneous mixture of all substances involved and an adsorption of the polymer to the shear / material particles. The solvent must not change the substances involved.
- Suitable for this are, inter alia, water and -CC 8 alcohols, branched or straight-chain.
- the resulting dough should no longer contain any excess solvent and should be easy to process in a kneading machine or roller.
- excess solvent in the mixture can be filtered off through a paper filter, for example using a water jet pump.
- the moist dough can then be kneaded.
- This dough can then be rolled out to a mat.
- a flat, coherent dough sheet is created.
- the mat is, for example, folded in the middle, placed one on top of the other, rotated by an angle between 45 ° and 135 °, preferably 90 ° (vertical), to the preferred (rolling) direction and rolled out again.
- the preferred (roll) direction is understood to be the roll-out direction of the previous roll-out process.
- the folding / rolling process can be repeated several times.
- the layer height can be reduced continuously or in steps during the rolling process until the final desired film thickness is reached.
- the final compression of the mat can take place under further folding / rolling steps, for example on a mechanical 2-roll apparatus, the roll spacing of which can also be continuously reduced.
- the shear materials are powders with a particle / agglomerate size of> 1 ⁇ m, preferably between 1 ⁇ m and 1 mm, particularly preferably between 2 ⁇ m and 800 ⁇ m and very particularly preferably between 5 ⁇ m and 500 ⁇ m.
- the polymer particles have a size of ⁇ 1 ⁇ m, preferably between 50 nm and 1 ⁇ m, particularly preferably between 100 nm and 900 nm.
- the material (s) are identical to the shear material (s), the size ratio defined above being taken into account in each case. However, the shear material can also differ from the material.
- the polyme particles are made from polytetrafluoroethylene (PTFE).
- PTFE polytetrafluoroethylene
- other polymers which can be sheared well or deformed inelastically are also suitable for the production of the material mats according to this document.
- Polymers are suitable here which do not undergo any reactions such as cross-linking, be it through condensation or other types of polymerization or cross-linking agents.
- a great advantage of the method is that it can be carried out at moderate temperatures in the range from 15 ° C. to 40 ° C., preferably at ambient temperature. This eliminates the need for a heating step (eg sintering) which, on the one hand, entails an increased energy requirement and, on the other hand, reduces the group of usable polymer articles.
- the thickness of the mat can be reduced continuously or in steps after a plurality of folding / rolling steps at a constant thickness during the rolling out.
- the lower limit for this is around 50 nm, although smaller thicknesses can also be achieved with suitable process optimization.
- Another advantage of this method is the possibility of removing parts of the solvent during the rolling out and thus of being able to produce a film with a higher packing density or lower porosity.
- the mat is slightly moistened with the solvent to make it easier to process.
- the solvent cannot be compressed or can only be compressed to a very small extent. Therefore, the mat is compressed and packed more tightly if parts of the solvent can be removed during the rolling. This can be done by placing a solvent-absorbing substance during the rolling process.
- the solvent absorbent is a paper towel.
- a shear material and / or a material is LiMnO 2 spinel, graphite powder, activated carbon or quartz sand.
- both the shear material and the material are graphite. The shear forces that occur change the crystal structure during processing in such a way that the resulting mats can preferably be used as an intercalation electrode for rechargeable lithium-ion batteries.
- the invention provides a polymer composite that can be produced by the above method.
- the polymer composite can be used as an energy store, in particular as an anode (intercalation electrode) and as a cathode for rechargeable lithium-ion batteries, as an air filter or moisture absorber in the automotive sector, as a membrane, as a textile, as protective clothing, for example as an activated carbon coating for ABC protective clothing or for sweat absorption, e.g.
- a decisive prerequisite for the feasibility of the method according to the invention is the presence of the two main components, the polymer and functional material or shear article, in particle form, the bimodal particle size of the components having to be such that the extent of the shear particles is substantially greater than that of the shear particles ,
- the local forces exerted on the polymer particles by the rolling process are greater in the case of larger chip articles - with a clearly anisotropic preferred direction.
- the forces are distributed isotropically over the mixture / polymer with a low anisotropic shear effect. This leads to less fibrillation or anisotropic expansion of the polymer.
- Fig. 1 tensile strength of different activated carbon / PTFE mats according to embodiment 2 depending on the number of folds during the manufacturing process and the relative content of bimodal particle distribution.
- Fig. 2 Rem recording of the activated carbon 2 + 1 composite mat from embodiment 2.
- the fibers are made of strongly sheared PTFE particles.
- Coarse particles activated carbon 2.
- Fine agglomerates activated carbon 1.
- FIG. 4 Rem photograph of the graphite / PTFE composite mat from exemplary embodiment 3.
- Polymer - bound quartz mat 10g quartz sand (Mikrosil and Sigrano silver sand) from the company Euroquarz with different grain sizes is mixed with 20 wt.% PTFE in the form of aqueous PTFE dispersion (PTFE particle size approx. 200 nm) and approx. 100 ml distilled water with stirring in a beaker approx 10 minutes mixed. Excess solvent in the mixture is filtered off through a paper filter using a water jet pump. The moist, filtered dough is then kneaded manually for about 2 minutes and then rolled out manually with a glass roller on a glass plate to form a 2 mm thick mat.
- the mat is folded in half, placed on top of one another, turned by 90 and rolled out again.
- the folding / rolling process is carried out 5 times with a layer height of 2 mm.
- the layer height is then reduced by reducing the spacing plates between the glass plate and the glass roll, and the folding / rolling process is continued 5 times at a height of 1 mm.
- the final compression of the mat under further folding / rolling steps takes place on a mechanical 2-roll apparatus, the roll spacing of which is continuously reduced to a thickness of 200 ⁇ m.
- a paper towel is placed on one side of the surface of the mat and rolled so that the composite dries during the compression process and can be compressed to a higher degree.
- Table 1 Physical data of quartz sand / PTFE composite mats
- the stability of the films is given in Table 2 in the form of the tensile strength of the films after a total of 30 folding / rolling steps. The evaluation was carried out as in Example 1.
- Tab. 2 Physical data of activated carbon / PTFE composite mats.
- the activated carbon mat shows the clear influence of a pronounced bimodal particle structure (grain size active material »particle size PTFE) on the stability of the mat.
- N the stability of the electrodes with increasing folding / rolling steps N increases.
- the rise of the curves varies depending on the grain size; ie the grain size is responsible for the effective fibrillation and stability of the framework.
- This “effective fibrillation” of the network is assigned here to the slope of the logarithmically plotted curves in FIG. 1.
- an “(achievable) degree of fibrillation” ⁇ can be defined for a specific particle structure.
- the number of folds N and the degree of fibrillation ⁇ thus enter exponentially into the tensile stress Z or the stability of the composite according to the method used here (see FIG. 1). 1 shows in a first approximation:
- the pure activated carbon 1 composite with low, hardly self-supporting stability is only converted into a stable, elastic and rubber-like mat after admixing large activated carbon 2 particles.
- Figure 3 shows the strong fibrillation of the network, caused by the strong shear forces of the coarse activated carbon 2 particles.
- the activated carbon 1 structures correspond to the small agglomerates in FIG. 3 and are loosely integrated into the teflon threads.
- Polymer-bound graphite 5g graphite powder (spherical shape, see Fig. 3) with an average particle size of 25 microns with 5 wt.% PTFE in the form of aqueous PTFE dispersion (PTFE particle size approx. 200 nm) and approx. 100 ml of distilled water Stirring mixed in a beaker for about 10 minutes and processed to 200 ⁇ m thick mats according to the method given in Example 1.
- the SEM photographs of the original graphite in FIG. 3 in comparison to the polymer composite mat in FIG. 4 show a significantly changed morphology of the graphite after the mat production.
- the original particle shape is dissolved in the stable composite.
- the morphological changes of the graphite are listed in Table 3:
- the BET surface area of the graphite decreases, the crystallite expansion in the c-direction (Lc) (determined from the peak height and half-width of the 002 peak in the XRD spectra at a diffraction angle of 26.4 ° ) increases dramatically - there is a different graphite modification in the composite, caused by the continuous application of shear forces to the spherical graphite particles of the starting material during the manufacturing process used.
- the changed morphology and structure of the electrode or the integrated graphite has an advantageous effect on the intercalation property of the electrode when used as an anode in secondary lithium ion batteries:
- the comparison of the foil electrode (produced according to the above folding / rolling process) with the Electrode of the comparative example shows significantly higher reversible storage capacities and lower irreversible losses of the composite structure compared to the standard.
- Another advantage of the technology used here is a realizable high electrode density of 1.6 g / cm 3 and an electrical conductivity of the electrode of over 6 S / cm, which eliminates the otherwise usual use of conductive carbon black to increase the electrical conductivity of the electrodes ,
- Tab. 3 Physical data of graphite / PTFE composite mat according to example 3 (film) and electrode of the comparative example.
- Polymer-bound lithium manganese oxide 5g LiMn ⁇ 2 spinel powder with an average particle size of 10-15 ⁇ m are mixed with 5% by weight PTFE in the form of aqueous PTFE dispersion (PTFE particle size approx. 200 nm), 5% by weight> conductive carbon black and Approx. 100 ml of ethanol are mixed with stirring in a beaker for approx. 10 minutes and processed into 200 ⁇ m thick mats according to the method given in Example 1.
- the electrochemical characterization of the stable mats as cathode material in secondary lithium-ion batteries resulted in a reversible capacity of> 100mAh / g.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10354339 | 2003-11-20 | ||
PCT/EP2004/011116 WO2005049700A1 (de) | 2003-11-20 | 2004-10-05 | Polymergebundene, funktionale werkstoffe |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1687360A1 true EP1687360A1 (de) | 2006-08-09 |
Family
ID=34609173
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP04765825A Withdrawn EP1687360A1 (de) | 2003-11-20 | 2004-10-05 | Polymergebundene, funktionale werkstoffe |
Country Status (2)
Country | Link |
---|---|
EP (1) | EP1687360A1 (de) |
WO (1) | WO2005049700A1 (de) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101685710B (zh) * | 2008-09-26 | 2012-07-04 | 通用电气公司 | 制备组合物、包含组合物的薄片及包含薄片的电极的方法 |
EP2532421A1 (de) | 2011-06-10 | 2012-12-12 | Süd-Chemie AG | Verbundmaterial aus fluorhaltigem Polymer, hydrophoben Zeolith-Partikeln und metallischem Werkstoff |
DE102017213388A1 (de) | 2017-08-02 | 2019-02-07 | Lithium Energy and Power GmbH & Co. KG | Elektrodenherstellungsverfahren mittels Binderfibrillierung mit partikulärem Fibrillierungshilfsmittel |
DE102017213377A1 (de) | 2017-08-02 | 2019-02-07 | Robert Bosch Gmbh | Batteriezelle mit separatorseitig und/oder stirnseitig kontaktiertem Anodenschichtüberstand und/oder Kathodenschichtüberstand |
DE102017213403A1 (de) | 2017-08-02 | 2019-02-07 | Lithium Energy and Power GmbH & Co. KG | Elektrodenherstellungsverfahren mittels Binderfibrillierung |
DE102018209416A1 (de) | 2018-06-13 | 2019-12-19 | Robert Bosch Gmbh | Verfahren zur Herstellung eines Kompositmaterials |
DE102018209964A1 (de) | 2018-06-20 | 2019-12-24 | Robert Bosch Gmbh | Herstellung von Elektroden mit Elektrolytlösungsmittel und/oder ionischen Flüssigkeiten gefüllten Elektrodenmaterialien |
DE102018209937A1 (de) | 2018-06-20 | 2019-12-24 | Robert Bosch Gmbh | Verfahren zur Herstellung eines Polymerverbundwerkstoffs für eine elektrochemische Zelle mittels eines gequollenen Polymers |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4208194A (en) * | 1977-09-26 | 1980-06-17 | Minnesota Mining And Manufacturing Company | Monitoring device |
US5248428A (en) * | 1991-06-28 | 1993-09-28 | Minnesota Mining And Manufacturing Company | Article for separations and purifications and method of controlling porosity therein |
US6207251B1 (en) * | 1994-01-10 | 2001-03-27 | Minnesota Mining And Manufacturing Company | Reinforced particle-loaded fibrillated PTFE web |
-
2004
- 2004-10-05 WO PCT/EP2004/011116 patent/WO2005049700A1/de not_active Application Discontinuation
- 2004-10-05 EP EP04765825A patent/EP1687360A1/de not_active Withdrawn
Non-Patent Citations (1)
Title |
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See references of WO2005049700A1 * |
Also Published As
Publication number | Publication date |
---|---|
WO2005049700A1 (de) | 2005-06-02 |
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Inventor name: FRICKE, JOCHEN Inventor name: WIENER, MATTHIAS Inventor name: PROEBSTLE, HARTMUT Inventor name: SCHLIERMANN, THOMAS Inventor name: REICHENAUER, GUDRUN |
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