EP1673825A1 - Procede et plasmatron pour la production d'un materiau modifie et materiau modifie correspondant - Google Patents

Procede et plasmatron pour la production d'un materiau modifie et materiau modifie correspondant

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Publication number
EP1673825A1
EP1673825A1 EP04789988A EP04789988A EP1673825A1 EP 1673825 A1 EP1673825 A1 EP 1673825A1 EP 04789988 A EP04789988 A EP 04789988A EP 04789988 A EP04789988 A EP 04789988A EP 1673825 A1 EP1673825 A1 EP 1673825A1
Authority
EP
European Patent Office
Prior art keywords
plasma
gas
plasmatron
carbon
carbon material
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Withdrawn
Application number
EP04789988A
Other languages
German (de)
English (en)
Inventor
Jörg FRIEDRICH
Gerhard KÜHN
Reinhard Mach
Heinz-Eberhard Maneck
Walter Schütz
Ludwig JÖRISSEN
Ulrich Storr
Margret Wohlfahrt-Mehrens
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.)
Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Bundesanstalt fuer Materialforschung und Pruefung BAM
Future Carbon GmbH
Original Assignee
Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Bundesanstalt fuer Materialforschung und Pruefung BAM
Future Carbon 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
Priority claimed from DE102004002236A external-priority patent/DE102004002236A1/de
Application filed by Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg, Bundesanstalt fuer Materialforschung und Pruefung BAM, Future Carbon GmbH filed Critical Zentrum fuer Sonnenenergie und Wasserstoff Forschung Baden Wuerttemberg
Publication of EP1673825A1 publication Critical patent/EP1673825A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/0054—Plasma-treatment, e.g. with gas-discharge plasma
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00853—Uses not provided for elsewhere in C04B2111/00 in electrochemical cells or batteries, e.g. fuel cells

Definitions

  • the present invention initially relates to a method for producing a modified material.
  • the invention further relates to a plasmatron for the production of a modified material and a corresponding material.
  • This can be, for example, modified carbon materials or other oxidizable materials.
  • the invention will be described variously on the basis of modified carbon material for better clarification, the invention of course not being limited to the examples described.
  • Lithium-ion batteries were introduced commercially in the early 1990s. Compared to known alkaline-manganese batteries or nickel-cadmium batteries, these have a higher charge density and better energy release behavior. Depending on the temperature, discharge current and discharge voltage, the behavior is quite different. However, lithium-ion batteries are usually much lighter, which results in a higher energy density.
  • the anode is made of carbon, a "light" material.
  • LiCoO 2 is predominantly used as the cathode material.
  • the anode consists, for example, of graphite, in which lithium ions migrating from the cathode can be reversibly incorporated during the charging process of the battery.
  • Li-ion accumulators that do not consist of graphite but of other carbon materials such as hard carbon, a mixture of different carbon materials, or the like.
  • the purest electrolyte used is usually high-purity organic solvents such as ethylene carbonate or propylene carbonate, to which lithium-containing conductive salts, such as LiCIO, have been added.
  • LiPF ⁇ is mostly used; a standard electrolyte, for example, consists of a mixture of ethylene and dimethyl carbonate (1: 1) with LiPF 6 (1 molar).
  • Lithium-ion batteries are used primarily in portable devices, for example video cameras, radio telephones, portable computers, digital cameras and the like, where, in addition to minimized space requirements, high energy density is also required.
  • lithium-ion batteries are also being developed for use in automobiles in order to meet the greatly increased power requirements of modern vehicles. Some manufacturers are also developing new batteries, for example for the future 40 V vehicle electrical system.
  • the layer should be as thin as possible because it is an irreversible reaction, which means that the lithium is supplied by the cathode and is no longer accessible for further cycles.
  • Pure graphite has a perfect layer structure and can store lithium ions between the graphene layers. Each lithium ion is surrounded by six carbon atoms. An intermediate layer is always completely filled with Li ions, but the next step is not to fill up the directly adjacent layer, but rather a more distant one. Only at the end are the neighboring layers filled up. If lithium ions are embedded between all graphene layers, the compound LiC ⁇ is formed; in the case of incomplete storage, other stoichiometric ratios can of course also arise, for example LiCs, LiC-12 and the like.
  • the compound LiC 6 corresponds to a capacity of 372 mAh / g, this is the maximum possible for graphitic carbons. Non-graphitic carbons can sometimes achieve higher storage values through other storage mechanisms.
  • MCMB me carbon microbeads
  • MCMB me carbon microbeads
  • a suitable binder for example PVDF
  • conductive carbon black to the electrode mass.
  • Other manufacturers use hard carbons or mixtures of different carbon materials.
  • MCMB consist of carbon particles, which in turn are baked together to form larger spherical particles (1-80 ⁇ m).
  • Such cells provided with MCMB anodes achieve a specific capacity in the range of approximately 350 mAh / g.
  • a disadvantage of MCMB is the high price, which is why we are looking for materials that are as similar as possible but cheaper.
  • MCMB is manufactured using a very complex multi-stage process, which means the high costs. Another disadvantage is that the MCMB material cannot be produced in Europe due to environmental regulations.
  • the general goal of further improvements to lithium-ion batteries is to achieve an increase in energy density, reduce irreversible Li losses, achieve high cycle stability and enable safe cell operation.
  • the consumption of Li for the formation of the SEI film must be reduced to a minimum.
  • the SEI is essential for the function, but should be thin and adherent (see above).
  • the formation of the SEI depends on many factors, such as impurities, type of electrolyte, additives to the electrolyte (for example vinyl carbonates), surface properties of the carbon material (surface groups, roughness, accessibility of the “edge sites”, amorphous carbon), BET surface area and the like.
  • a known approach to improving anode material for Li-ion batteries consists in modifying the graphite surface by generating functional groups by means of gas or liquid phase oxidation, which is followed by a high-temperature treatment. Oxidation increases the proportion of surface groups containing oxygen and thereby increases the formation of SEI.
  • closed structures form on the graphite edges of the particles (the closed structures form during the high-temperature treatment (HTT), approx. 2500 ° C.), which are similar to the “platelef structure of GNF (graphite nanofiber) or the tip of nanotubes and are referred to as "nanoterminated surface structure" (NTSS) (Moriguchi et al., J. Appl. Phys. 88 (2000), page 6369 ff, Physica B 323 (2002), page 127 ff).
  • Another approach to the surface modification of carbon materials consists of a high-temperature treatment in an argon atmosphere, which is intended to achieve a type of cleaning of the surface, and the subsequent reaction of the graphite surface with reactive molecules such as NH 3 , O 2 , CO2, SO2, H 2 S, C2H2 and so on.
  • the reactive gases can also contribute to the modification of the surface morphology (Buqa. Et al., J. Power Sources 97-98 (2001), page 122 ff).
  • the object of the present invention is therefore to provide a modified material, in particular a carbon material, with improved properties and at low cost.
  • Claim 1 a plasmatron according to independent claim 13, a carbon material according to independent claims 20 and 21, and by using a carbon material according to independent claims 25 and 28. Further advantageous refinements, aspects and details of the present invention result from the dependent Claims, the description and the accompanying drawings. Features and details that are described in connection with the method according to the invention also apply in connection with the plasmatron according to the invention, the carbon material according to the invention and the use according to the invention, and vice versa.
  • the invention is based on the principle of carrying out a surface modification of a material by treatment with a thermal plasma at a specific oxygen partial pressure.
  • these can be modified carbon materials and other oxidizable materials.
  • metals or other materials can be coated with a thin oxide layer in order to modify their magnetic, optical or adhesive properties.
  • the invention according to the first aspect is directed to a method for producing a modified material, which comprises the following steps:
  • the treated material is then removed.
  • the method according to the invention is a method that is not only accessible for batch operation, but also for continuous operation, provided that the starting material is fed in continuously and the modified material is removed continuously. All steps of the method according to the invention thus take place simultaneously. However, the different steps are interdependent, since a plasma can only be generated with an existing high-frequency field and introduced plasma gas, and the modification of the material can only be carried out with an existing plasma.
  • the invention is not limited to certain types of plasmas.
  • the plasma can be generated from all possible gases, and reducing gases are also possible. But oxygen partial pressure is absolutely necessary for spheroidization and for the production of oxygen-containing functional groups, so that the plasma is preferably oxygen-containing.
  • oxygen-containing functional groups such as -CH- or -C-NH x -terminated surfaces.
  • the method according to the invention is suitable for modifying a wide variety of materials.
  • Carbon materials can preferably be modified with the method.
  • all materials that react with oxygen (oxidize) and whose oxidation products are volatile in plasma are generally suitable.
  • oxygen oxygen
  • this is CO 2 .
  • the method according to the invention is suitable for producing modified carbon material which has graphitic and / or non-graphitic carbon fractions and optionally also hydrocarbon fractions.
  • the subject of the method is in particular the modification of carbon material with the objectives: - spheroidization of irregularly shaped particles.
  • Materials that can melt in the plasma jet form spherical, spherical particles (metals, oxides and so on) due to the surface tension.
  • - Materials that do not melt, such as carbon, but form volatile oxidation products (CO, CO 2 ) should also be spheroidizable.
  • the edges of the particles are preferably oxidized, resulting in spheroidized (rounded) particles. This is done in thermal plasma using a plasma with a certain oxygen partial pressure. The partial pressure of oxygen, in the case of carbon, is essential.
  • O-containing functional groups (-OH, - COOH, -CHO) are generated on the surface, which when using these modified C materials as anode material in Li-ion batteries that influence the formation of the SEI layer.
  • the pore structure of the C material is changed, whereby meso and micro pores are also created.
  • the carbon material to be modified can generally be carbon powders of various grain sizes.
  • the process is not limited to nanomaterials and not only to graphite. Rather, all carbon materials (hard, soft carbons, graphitic and non-graphitic carbons, as well as carbon nano fibers and nanotubes) can be modified according to this process, specifically in the sense of creating the surface groups and changing the pore structure. But spheroidization in the sense of burning off the edges can only be used for oxidizable and volatile reaction products, as well as various other substances such as metals, silicon, and so on.
  • the carbon material used can come from various sources, such as natural coal, natural graphite, graphite, hard carbons, soft carbons, graphitizable and non-graphitizable carbons, anthracites or the like.
  • a thermal treatment of the starting materials is carried out by the method according to the invention.
  • Spherical particles are obtained by oxidation, preferably at the edges of the material - for example the graphite particles.
  • non-graphitic carbon materials can also preferably be oxidized in comparison to graphitic carbon materials.
  • graphite especially natural graphite, always contains a certain amount of non-graphitic carbon materials.
  • certain non-graphitic carbons are also graphitized during the thermal treatment in plasma, so that the graphite content also increases in this way. As a result, a product with improved purity can be obtained.
  • Starting material for example carbon material
  • a conveying gas Argon is preferably used as the conveying gas, but any other gases, including reactive gases, can also be used.
  • the grain of the material is actually arbitrary, so that the process also works with smaller particles in the submicron to nano range.
  • the grain size is preferably between 5 and 80 ⁇ m, but can also be smaller and larger if this is necessary or advantageous for a specific application.
  • Spherodized particles in the nanometer range are of interest, for example, for optoelectronic applications.
  • the process can be carried out at any pressure.
  • the method can be characterized in that it can be carried out completely at normal pressure or almost at normal pressure. This has the advantage that it is possible to work with an open system that allows continuous operation and that the products can be removed without interrupting the process. Furthermore, the various gases can be introduced without any problems.
  • the possibility of carrying out the process at normal pressure is important; the partial pressure of oxygen can be reduced by adding inert gas or increased by adding oxygen.
  • the introduction of the material can take place at various points in the plasmatron, depending on the reaction conditions. This means that the introduction is not restricted to specific positions.
  • the starting material such as the carbon material
  • the starting material is introduced into the chamber directly at the beginning of the high-frequency field or the plasma. This can be achieved, for example, by leading a feed pipe to just before or even in the region of the plasma and by dispensing the material particles, for example the carbon particles, or other suitable carbon material at an open end of the feed pipe.
  • the material is preferably passed through the plasma by means of an introduction pressure of the conveying gas and, after a defined passage time in the plasma, leaves the plasma on the side essentially opposite an introduction side of the plasma.
  • An inlet side is to be understood here as an end face of the plasma (that is to say an area beyond which the plasma remains below a certain concentration) at which the starting material, for example carbon material, is supplied to the plasma, that is to say introduced.
  • the starting material generally traverses on one by various sizes such as properties of the starting material (including density, diameter, morphology), Introduction conditions and / or plasma parameters defined the plasma path and emerges from the plasma on an essentially opposite side.
  • the conditions already mentioned in the previous sentence set the dwell time and thus the duration of the modification treatment of the material.
  • the material can also be fed to the plasma below an inductor of the plasmatron. This can be done, for example, radially or tangentially from the outside perpendicular to the plasma axis.
  • the starting material generally traverses on one of various sizes such as properties of the starting material (including density, diameter,
  • introduction conditions and / or plasma parameters defined the plasma path and emerges from the plasma on a side lying essentially perpendicular to the axis of the feed direction.
  • the dwell time is also determined here by all other process parameters.
  • material can also be introduced several times or at several locations, for example to create different layers (for composite materials) or to complete a reaction.
  • the method according to the invention can further be characterized in that it has the further step, separating the modified material, for example carbon material, in the chamber by means of a mechanical filter, or a cyclone, or another known separation method, or also by continuously operating filter systems (separator).
  • a textile or metal filter with a pore size (mesh size) suitable for the synthesis product is preferably used as the mechanical filter. It can be removed from the synthesis apparatus to remove the product.
  • the plasma gas has a defined oxygen partial pressure, in particular from 10 to 10,000 Pa. In particular, a partial pressure of approximately 2,000 Pa is preferred.
  • the oxygen content in the plasma gas is preferably 0.01 to 10% by volume in order to be able to produce the desired modifications of the material; and in particularly preferred embodiments is around 2% by volume.
  • the plasma gas can consist of different types of gas and gas compositions.
  • the plasma gas preferably contains as inert a gas as possible, for example a noble gas such as helium or neon.
  • Argon is particularly preferred as the usable noble gas because it is required for the initialization of the plasma and is also inexpensive.
  • the reaction can also be influenced by means of a reaction gas and / or a quench gas which is introduced into the chamber.
  • the reaction gas can be, for example, oxygen.
  • the quench gas is used to rapidly cool the gases leaving the plasmatron. This quickly lowers the temperature of the particles and you can freeze certain states of the particles that would change if they cooled slowly (freezing high-temperature phases, quenching speed up to 10 8 K / s).
  • the high-frequency field applied to the chamber for generating the plasma in a certain predetermined range preferably has a frequency in a range from 1 to 30 MHz, for example from 4 MHz.
  • the invention is further directed to a system for producing such a modified material, for example a carbon material.
  • a modified material for example a carbon material.
  • the invention is therefore directed to a plasmatron for producing a modified material (for example modified carbon materials and other oxidizable materials), which comprises:
  • a chamber a high-frequency inductor arranged on at least one area of the chamber, a gas feed line for introducing a plasma gas into the area of a high-frequency field generated by the high-frequency inductor, and a material feed line for blowing carbon material with a conveying gas into the plasma generated by the high-frequency inductor with the plasma gas.
  • the chamber can be a chamber which is customary for piasmatrons, for example made of a glass, ceramic or quartz material.
  • the high-frequency inductor can also be a customary inductor, for example a three-turn inductor if the chamber is suitably dimensioned.
  • the feed lines consist of materials customary for piasmatrons in the arrangement specific to the invention for carrying out, for example, the method according to the invention described above.
  • the material feed for the starting material for example the carbon material
  • the material feed line is preferably connected to a powder conveyor for producing a graphite material / gas mixture which is operated with a conveying gas.
  • a powder conveyor is a device which mixes the powder homogeneously with a carrier gas stream and allows this mixture to be transported continuously with a constant volume flow.
  • the high-frequency inductor is preferably connected to an energy generator for generating high-frequency current, which can couple energy into the chamber for generating a plasma.
  • the high-frequency generator can, for example, have a frequency in the range described in the method according to the invention, in particular at 4 MHz.
  • the plasmatron according to the invention also contains a gas feed line for introducing a reaction gas and / or a quench gas, which is arranged behind the inductor from the introduction side of the plasma.
  • a gas feed line for introducing a reaction gas and / or a quench gas, which is arranged behind the inductor from the introduction side of the plasma.
  • the plasmatron according to the invention preferably also has a mechanical filter for separating the modified material.
  • the invention is also directed to a carbon material.
  • This carbon material is a carbon material provided with modified edges by the action of plasma and oxygen, or a carbon material that can be produced by the method according to the invention or with the plasmatron according to the invention.
  • the carbon material preferably has modified edges which have a rounded shape in comparison to unmodified edges, for example a graphite starting material which is to be subjected to the method according to the invention.
  • a graphite starting material which is to be subjected to the method according to the invention.
  • the oxidation of the surface always starts first at the so-called “edge sites” (ends of the graphene layers). Oxygen-containing groups, for example -COOH, form there, which then release CO 2 under the reaction conditions. The material is burned off at these points. If there is a protruding edge at such a point, the oxidation will take place from both sides and the material will be rounded off at this point.
  • the BET surface area is reduced and the “edge sites” are cleaned of impurities (for example oxygen-containing groups or amorphous carbon), which makes lithium intercalation easier.
  • the carbon material according to the invention preferably has a reduced irreversible absorption capacity for alkali and / or alkaline earth metal ions, for example for the lithium ions used in batteries, in comparison to untreated starting carbon material. This means that the formation of SEI films during the first start-up of an anode of a battery provided with a corresponding carbon material according to the invention is reduced compared to previous anodes constructed with MCMB.
  • the carbon material according to the invention preferably has a BET surface area ⁇ 5 m 2 / g.
  • BET is the abbreviation for "Brunauer-Emmett-Teller", after the inventors of this surface determination method. This property is particularly required for electrode material for Li-ion batteries.
  • the carbon material can be, for example, a carbon material which has graphitic and / or non-graphitic carbon fractions and possibly also hydrocarbon fractions.
  • a carbon material which has graphitic and / or non-graphitic carbon fractions and possibly also hydrocarbon fractions.
  • it can be a graphite powder.
  • the invention is also directed to the use of a carbon material according to the invention as an electrode material in a lithium-ion accumulator, the electrode material preferably being an anode material.
  • the use preferably has the process step that the carbon material is formed into an anode.
  • the invention is also directed to the use of a carbon material according to the invention as an additive for batches.
  • the use can be made in that a starting material is mixed with the carbon material in order to form a composite material.
  • Metal / carbon mixtures, carbon / polymer mixtures and other mixtures can be considered as target composite materials.
  • the method and plasmatron according to the invention leads to the production of a carbon material with improved properties for the intercalation of metals, in particular lithium. In particular, this results in an improvement in the surface properties and thus an indirect improvement in the lithium intercalation.
  • the BET surface area becomes smaller and the coal surface area of
  • modified carbon materials graphitic and non-graphitic which can be used for the production of battery or accumulator electrodes. It provides carbon materials with modified surfaces in terms of surface groups, nanoporosity and BET surface area.
  • the invention is described below with reference to a specific embodiment, reference being made to the attached drawing in FIG. 1, in which a plasmatron according to the invention is shown.
  • the plasmatron 1 according to the invention in the preferred embodiment presented here comprises a multi-section but one-pot chamber 2, for example a quartz tube, a high-frequency inductor 3 and a feed mechanism 4 for feeding carbon material.
  • the chamber 2 has three different sections of different diameters, a first section 5, around which a three-turn inductor 6 is wound in the specific case, a modulation area 7 and a collecting area 8 with a filter 9 attached to its end.
  • the required plasma gases are blown into the chamber and then reach the region of the high-frequency field formed by the inductor 6.
  • the carbon material M is blown into the chamber 2 via a material feed line 12 which leads directly to the windings of the inductor (when viewed from the side).
  • a powder conveyor 13 is used for this purpose and is supplied with a conveying gas, for example argon, via a feed line 14.
  • the energy supply to the inductor coils 6 takes place via a high-frequency generator 15, which is designed so that the high-frequency field generated by it with the aid of the inductor coils is able to convert the plasma gases into a plasma.
  • graphite powder for example, but not exclusively, with a grain size of 50-80 ⁇ m, can now be subjected to treatment at normal pressure in a one-step and one-pot process.
  • the plasmatron 1 used consists, for example, of an air-cooled quartz tube with an inner diameter of 50 mm, into which the energy is coupled via the three-wind inductor 6, for example from a 50 kW generator 15.
  • the graphite or another carbon powder is supplied via the material feed line 12 (probe) with an outer diameter of 6 mm and an opening diameter 2.2 mm are blown into the "head" of the plasma.
  • the probe tip is preferably positioned at the level of the uppermost inductor turn.
  • the total amount of gas is preferably 45 standard liters / min with an Ar content of 98 percent by volume and an O 2 content of 2% by volume
  • the generator output can typically be 2.5, 5 or even up to 40 kW
  • the carbon powder for example graphite powder, can be supplied to the plasma at 35 g / h in the dimensions and values given above
  • the treated powder is separated from the gas stream with a mechanical filter 9 at the end of the chamber 2 opposite the feed line.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Secondary Cells (AREA)

Abstract

L'invention concerne un procédé pour la production d'un matériau modifié, par exemple d'un matériau de carbone, ledit procédé comprenant les étapes suivantes : production d'un champ haute fréquence dans une chambre (2) d'un plasmatron (1) ; introduction d'un gaz plasma dans la chambre (2) ; production d'un plasma à partir du gaz plasma par l'intermédiaire du champ haute fréquence ; et introduction du matériau de départ dans le plasma. L'invention concerne également un plasmatron (1) servant à produire un matériau modifié (M), présentant : une chambre (2), au moins un inducteur haute fréquence (3) placé dans au moins une zone de la chambre (2), une conduite d'amenée de gaz (10, 11) servant à introduire un gaz plasma dans la zone d'un champ haute fréquence produit par l'inducteur haute fréquence (3), et une conduite d'amenée de matériau (4) servant à introduire le matériau de départ, au moyen d'un gaz de transport, dans le plasma produit par l'inducteur haute fréquence (3) à partir du gaz plasma. L'invention concerne également un matériau de carbone modifié, produit selon ledit procédé.
EP04789988A 2003-10-16 2004-10-14 Procede et plasmatron pour la production d'un materiau modifie et materiau modifie correspondant Withdrawn EP1673825A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10348193 2003-10-16
DE102004002236A DE102004002236A1 (de) 2003-10-16 2004-01-15 Verfahren und Plasmatron zur Herstellung eines modifizierten Materials sowie entsprechend modifiziertes Material
PCT/DE2004/002286 WO2005041328A1 (fr) 2003-10-16 2004-10-14 Procede et plasmatron pour la production d'un materiau modifie et materiau modifie correspondant

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WO2012020113A1 (fr) 2010-08-13 2012-02-16 Sgl Carbon Se Stabilisation de charges nanoparticulaires dans des formulations de résine

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CA2570442A1 (fr) 2005-05-06
WO2005041328A1 (fr) 2005-05-06
JP2007513747A (ja) 2007-05-31
US20070275304A1 (en) 2007-11-29

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