WO2006122736A2 - Systeme composite comprenant des nanotubes, son procede de production, et son utilisation dans des elements de chauffage - Google Patents

Systeme composite comprenant des nanotubes, son procede de production, et son utilisation dans des elements de chauffage Download PDF

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Publication number
WO2006122736A2
WO2006122736A2 PCT/EP2006/004557 EP2006004557W WO2006122736A2 WO 2006122736 A2 WO2006122736 A2 WO 2006122736A2 EP 2006004557 W EP2006004557 W EP 2006004557W WO 2006122736 A2 WO2006122736 A2 WO 2006122736A2
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Prior art keywords
nanotubes
fibers
composite
comprehensive
nanotube
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PCT/EP2006/004557
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German (de)
English (en)
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WO2006122736A3 (fr
Inventor
Walter Von Wirth
Klaus Hying
Ivica Kolaric
Dominik Nemec
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Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Priority claimed from DE200510023764 external-priority patent/DE102005023764A1/de
Priority claimed from DE202005013822U external-priority patent/DE202005013822U1/de
Priority claimed from DE202005014678U external-priority patent/DE202005014678U1/de
Application filed by Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Publication of WO2006122736A2 publication Critical patent/WO2006122736A2/fr
Publication of WO2006122736A3 publication Critical patent/WO2006122736A3/fr
Anticipated expiration legal-status Critical
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24D—DOMESTIC- OR SPACE-HEATING SYSTEMS, e.g. CENTRAL HEATING SYSTEMS; DOMESTIC HOT-WATER SUPPLY SYSTEMS; ELEMENTS OR COMPONENTS THEREFOR
    • F24D13/00—Electric heating systems
    • F24D13/02—Electric heating systems solely using resistance heating, e.g. underfloor heating
    • F24D13/022—Electric heating systems solely using resistance heating, e.g. underfloor heating resistances incorporated in construction elements
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/50—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by form
    • D21H21/52—Additives of definite length or shape
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/84—Heating arrangements specially adapted for transparent or reflecting areas, e.g. for demisting or de-icing windows, mirrors or vehicle windshields
    • H05B3/845—Heating arrangements specially adapted for transparent or reflecting areas, e.g. for demisting or de-icing windows, mirrors or vehicle windshields specially adapted for reflecting surfaces, e.g. bathroom - or rearview mirrors
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2214/00—Aspects relating to resistive heating, induction heating and heating using microwaves, covered by groups H05B3/00, H05B6/00
    • H05B2214/04—Heating means manufactured by using nanotechnology
    • 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
    • Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]

Definitions

  • the present invention relates to systems comprising nanotubes, in particular planar systems, as well as methods of their production and the use of systems comprising nanotubes in heating elements.
  • Nanotubes have a variety of interesting properties such as high thermal conductivity and excellent mechanical and electrical properties, which is why they are being investigated for a variety of applications.
  • a direct conversion from electrical to mechanical energy is possible (actor), so that a wealth of applications up to an artificial muscle are conceivable.
  • An artificial muscle are conceivable.
  • capacitors can be produced in combination with suitable dielectric materials. It is also possible to use it as a biological nutrient medium.
  • planar structures that consist entirely or to a large extent of nanotubes, in particular carbon nanotubes, is laborious, fraught with great difficulty and limited to small flat bodies.
  • the carbon nanotube raw material is first dispersed using ultrasound and using a surfactant.
  • the hydrophobic nature of the carbon nanotubes and the strong van der Waals interactions between the individual tubes cause poor dispersibility.
  • the carbon nanotube concentration is therefore limited to about 0.1% in an aqueous surfactant solution.
  • the suspension is centrifuged and then decanted off. Subsequently, the suspension is filtered off through a microliter, forming the flat Bucky paper. To accelerate the filtration process, the filtrate is either sucked through the filter with negative pressure or forced through the filter by means of overpressure.
  • the Bucky paper must be rinsed several times with distilled water. Finally, it is carefully separated from the filter and dried.
  • surfactants require the rinsing of the surfactant with distilled water in a further step.
  • carbon nanotubes can also be applied specifically to surfaces by deposition from the gas phase by the CVD method (chemical vapor deposition).
  • CVD method chemical vapor deposition
  • the use of this technology for targeted coating in a continuous process is currently unknown.
  • the production of a self-supporting planar structure, for example by separation of the carbon Nanotubes layer of a surface is currently not known.
  • the object of the present invention is to provide a Nanotubes comprehensive, in particular flat system, which is relatively easy and can be produced in larger quantities.
  • the nanotube-containing system of the present invention is a composite system comprising nanotubes and fibers wherein the nanotubes are substantially adsorbed to the fibers.
  • This composite system is in particular a planar system.
  • planar structures can be produced from these fibers with adsorbed nanotubes in a relatively simple manner, since the nanotubes adsorbed on the fibers can be combined with the known production processes for producing planar structures, for example on the usual devices and processes known from the paper industry planar composite of macroscopic fibers and nanotubes are further processed.
  • the nanotubes can be adsorbed on the fibers by dispersing the nanotubes together with the fibers, preferably by means of ultrasound, in a dispersion medium.
  • a significant advantage of the present invention is that the use of foreign fibers and taking advantage of the transfer process, in which the nanotubes draw on the foreign fiber, an industrieschreiber process for mass production of composites of Bucky papers with foreign fibers is possible, the largely classical Processes in the paper industry.
  • the adsorption of the nanotubes on the fibers can be determined in various ways, for example by means of SEM images or by resistance measurements.
  • the prerequisite of "essentially adsorption" is also present if the majority of the fibers on the SEM image show the adsorbates, even if nanotubes as agglomerates and / or fibers with few or no adsorbed nanotubes are present in addition to these adsorbates.
  • Another indication for the adsorption of the nanotubes on the fibers is the fact that from a concentration - the limit concentration - of nanotubes, which is sufficient for example to form a monolayer on the fiber surface, a clear effect on the electrical resistance of the composite of fibers and nanotubes is available.
  • the limiting concentration depends on the geometry of the nanotube and the surface of the fibers used. If the mass fraction of nanotubes is sufficient to fully occupy the fiber surface, the conductivity increases abruptly, that is, the resistance drops.
  • the unambiguous influence on the resistance lies with a calculated degree of coverage of the nanotubes on the surface of 50%.
  • the surfaces of various cellulose fibers at which the degree of coverage is calculated are shown in Table 5.
  • a clear indication of the stability of the fiber composition could be drawn from a first machine trial on a pilot paper machine.
  • a material according to the invention was produced with a grammage of 100 g / m 2 .
  • the corresponding resistance of the material was 220 ohms / cm (equivalent to 1700 ohms / sq).
  • the committee was, as usual in the paper industry, taken up with water and processed into a pulp. During the subsequent use of this material, the same ohmic resistance was achieved with the same basis weight.
  • the fiber occupancy can be achieved as follows: Either a pulp is mixed with the nanotubes, in particular the solid carbon nanotubes substance, and ultrasonicated (variant A) or the pulp is adjusted to a desired degree of grinding and then a pre-dispersed mother solution of nanotubes in water was added (variant B).
  • Variant A is particularly suitable for relatively high carbon nanotube concentrations.
  • the minimum concentration of carbon nanotubes for this process variant should preferably be 10%, based on the solids content in the pulp, since a uniform coverage of the fibers is more difficult to achieve below this concentration. It should be noted that the ultrasonic treatment causes an additional grinding effect, so that the mass is therefore to be checked exactly to the degree of grinding.
  • variant B Another advantage of variant B is that it is also customary in the paper industry to dose additives of polymer dispersions or pigment slurries inline, which is why the concept of the mother solution ideally fits the procedures customary in the paper industry.
  • the concentration range of at least 0.3% nanotubes, in which the mother liquor should preferably be prepared, also results from the fact that an approach below the concentration of the machine chest would not make sense because of an undesirable dilution of the pulp.
  • variant A direct use of solid carbon nanotubes in the pulp
  • a use of solid components in the machine chest is not common.
  • a pulp in the Mischbütte be set at 0.3 to 0.5% and are brought into the paper machine after appropriate treatment.
  • such a process is very costly for the grinding of the pulp and technically difficult to control, which is why for the Variant A is a range of 1 to 3% solids, that is, carbon nanotubes and fibers is recommended.
  • the laminar layers comprising nanotubes according to variant B with a mother solution in a conventional concentration range of 1 to 3 wt.% Nanotubes or according to variant A in a conventional paper industry Dispersion worked preferably with 1 to 3 wt.% Solid, that is, it is a more concentrated suspension of nanotubes used from which the ultrasonically dispersed nanotubes then adsorb to the surface of the fibers.
  • concentrations are common for the preparation of pulp in the paper industry and facilitate economical production.
  • the adsorption is based on the following transfer mechanism:
  • ultrasound By using ultrasound, at least some of the nanotubes are dispersed.
  • the dispersed nanotubes have an affinity for the surface of the fibers and are adsorbed thereto, further nanotubes are dispersed and subsequently adsorbed and so on until the nanotubes are substantially adsorbed to the surface.
  • anionic surfactants such as sodium dodecyl sulfate should be avoided, since these compete with the negative potential of the paper fibers and hinder or reverse the retention on the fibers.
  • the process cited here does not contain any surface-active substances.
  • the adsorption of the nanotubes on the fiber surface is promoted by the fact that the anionic surfactants, such as sodium dodecyl sulfate, which are customarily used as dispersants for the preparation of the nanotube dispersion, are not used to prepare the dispersion.
  • anionic surfactants such as sodium dodecyl sulfate
  • nanotubes without anionic surfactants are not stabilized in the dispersion as negatively charged particles which are repelled by the likewise partially negatively charged fiber surface.
  • the surface potential of the cellulose measured with a PCD 03 from Mütek, should preferably be between -500 mV and -1400 mV.
  • anionic surfactants such as sodium dodecylsulfate not only effective adsorption of the nanotubes is achieved on the fibers, but it also eliminates the multiple rinsing, which is required in the known production of Bucky paper to the surfactants added as a dispersant to remove.
  • a transfer of the paper fibers or the nanotube suspension in the positive area can be achieved by means of cationic surfactants.
  • the adsorption can be facilitated and a time savings in the preparation of the dispersion can be achieved by means of ultrasound.
  • reloading is ultimately not required for the process.
  • auxiliaries can be used in the preparation of the mother liquor or the direct adsorption, as they are usually used for the preparation of dispersions.
  • Substances which increase the negative surface potential of the carbon nanotubes are of course not advantageous since the cellulose inherently has a negative surface potential. However, if one has produced a positive potential by pretreatment of the cellulose, this can be advantageous.
  • a neutral polymer such as polyvinyl alcohol can also be used.
  • the solids concentration in the pulp for the process for producing the pulp should be about 0.01% to 10% by weight, preferably between 0.1 to 5% by weight, and more preferably between 0.2 to 2% by weight.
  • the solids concentration in the pulp for the process of production within the paper machine should be between about 0.1 to 1 wt.%.
  • the ratio of fiber to nanotube can be varied within wide limits, depending on which properties the laminar composite material should have.
  • the occupancy of the fibers with carbon nanotubes is the limiting factor. It may be assumed that there should be a minimal amount of monomolecular layer on the fibers to achieve significant conductivity.
  • VcN ⁇ , mono volume of a single-layer CNT layer on the fiber b) V ⁇ ⁇
  • T, mono X PcNT nicNT.mono
  • the surface area of the fibers was calculated according to Table 5, assuming that the fiber forms a nearly cylindrical body. If a degree of coverage of 0.4 is fallen below, a sudden increase in the electrical resistance was found in all cases. An erratic increase means an increase of at least two orders of magnitude.
  • resistivities for a 120 gm thick material range from 1 to 5 kOhm / cm (corresponding to 7.7 to 38.5 kOhms / sq), while when the underfill level falls below 0.4, it is a typical range of resistance for paper from 10 6 to 10 9 ohms / cm (corresponding to 7.7 x 10 6 to 7.7 x 10 9 ohms / sq).
  • the degree of coverage was calculated in practice between 0.4 and 1.2 and ranges in the majority of cases between 0.5 and 0.9.
  • Table 6 shows the experimental results on three different CNT types, all of which have a different average diameter.
  • a range of 0.8 to 95% by weight of nanotubes can be realized. Particularly advantageous in terms of material costs and achieved effect are 2 to 30%, and an optimum can be seen in the range of 10 to 20%.
  • the fibers used may be cellulose, modified cellulose, polyamide, polyacrylonitrile, polyolefin, teflon, silicate fibers, or other natural or synthetic fibers.
  • Liehe fibers are used, depending on the mechanical or electrical properties of the composite material should have.
  • cellulose fibers are particularly preferred.
  • long-chain cellulose fibers for example from softwoods, which are characterized by greater mechanical stability and strength
  • short-chained fibers such as poplar fibers can be used.
  • the cellulose fibers to be used are pretreated, in particular ground and spliced, as is customary in papermaking.
  • a multiplicity of dispersants can be used, for example water, preferably deionized, but also aqueous cationic surfactant solutions or polyvinyl alcohol solution.
  • aprotic, polar or nonpolar solvents for example dimethyl sulfoxide, vinylpyrrolidone or kerosene.
  • Water is the preferred solvent for the process according to the invention.
  • Surfactants are not necessary and are in the case of anionic surfactants - as already explained - even with a negative effect on the process.
  • the nanotubes from the suspension adsorb not only on the conventional cellulose fibers with a slightly negative surface charge, but also on fibers with a slightly positive surface charge.
  • a positive potential of the fibers or a positive potential of the nanotubes is advantageous and reduces the process times.
  • Another embodiment provides for orienting the nanotubes in the composite. This can be achieved according to the invention in that the fibers on which the nanotubes are adsorbed are oriented.
  • the paper industry wants turbulent flow conditions when the substance casseroles onto the sieve. This avoids flocculation on the one hand and supports a disorientation of the fibers, which are usually oriented in the direction of flow of the substance (longitudinal / transverse ratio).
  • 3rd stage diffuser block 3rd stage diffuser block.
  • Parallel diffusers lead to micro-turbulences in the area of the transition zones. Abandoning this constructive element also helps to keep the flow laminar.
  • the element is the first part of the wire section and puts the screen in vibrations of adjustable frequency and amplitude.
  • Three-layer headbox This element is often used on high-speed paper machines. The principle is based on the fact that the material from three slot nozzles instead of one exits. To generate turbulence, all three streams have different concentrations. If the concentration is set to the same value, then a strong longitudinal orientation can be achieved with such a machine.
  • fibers comprising nanotubes by means of high-voltage fields or by movement of the liquid phase through electro-magnetic fields. magnetic or magnetic fields or by calendering under the influence of strong magnetic or electromagnetic fields.
  • a non-statistic alignment of the nanotubes to one another is ultimately achieved by aligning the fibers with the nanotubes also oriented in a preferred direction on the surface thereof.
  • a subsequent removal of the cellulose components by thermal or chemical decomposition is possible, so that in a further process step, a bucky paper is available which consists exclusively of Carbo ⁇ nanotubes. Due to the biocompatibility of pure carbon nanotube structures, applications in tissue engineering are possible.
  • the composite according to the invention can then be subjected to a subsequent refinement.
  • a polymer coating of an aqueous phase is possible, wherein the deposition preferably takes place on the surface of the adsorbates, ie on the nanotubes, on account of their hydrophobic nature, so that a system of one conductive and two dielectric layers (capacitor) can be built up ,
  • mechanical and electrical properties can be set within wide limits and produced in close manufacturing tolerances. Reduced manufacturing costs allow a wide dissemination of the advantageous properties of nanotube systems, in particular carbon nanotube systems.
  • the composite according to the invention can be used in a variety of ways, for example as an actuator, sensor, substrate (medicine), tissue engineering, electrical conductors, as a heat conductor (cooling elements), as a resistance heater, as a filter, as a cell substrate, as a reinforcing material, as a flame retardant, etc.
  • a particularly preferred variant of the invention consists in the use of the composite system according to the invention in heating systems, which following are described in more detail:
  • Heating element in particular as Spieqelskyunq
  • the heating element comprises a planar composite system comprising nanotubes, which is electrically conductive and generates heat when current flows, as well as the electrical contacts required for the current flow.
  • a planar composite system comprising nanotubes, which is electrically conductive and generates heat when current flows, as well as the electrical contacts required for the current flow.
  • Nanotubes comprehensive composite system is a flat, especially paper-thin, composite system with a thickness between 20 microns and 10 mm and in particular a thickness between 100 microns and 500 microns.
  • the heating element is a surface heating element, which causes heating over its entire current-carrying surface.
  • the electrodes With a suitable arrangement of the electrodes, current flows through the entire composite system.
  • the heating element is also easy to manufacture, since only an adaptation to the required size and contacting are required.
  • the complex, the application of the electrical lines on the heating element concerned manufacturing steps of the conventional heating elements (etching) thus eliminated.
  • heating element is far less susceptible to interference than the previously known heating elements, as a power line in the entire composite material and thus heating takes place even if the material is damaged at one or the other point.
  • the material has a different resistance in current flow. These parameters can thus be used to set the resistance and thus the heat generated when current flows through.
  • the Nanotube composite system When used as a mirror heater, the Nanotube composite system, which is often paper-like, is adhered to one side to the back of the mirror, preferably with power supply connectors attached to the other side of the composite system.
  • power supply connectors attached to the other side of the composite system.
  • the heating element according to the invention can be operated with DC and AC voltage, in particular with the 12V DC voltage provided in automobiles, so that it can be used for the field of application in automobiles as exterior mirror heating and seat heating. Also, an operation with AC voltage, in particular 220 V, is possible, for example, for use as a mirror heater in the bathroom.
  • the electrical contacts are all mounted on one side of the composite material, since the electrical resistance and thus the heat generated in the one-sided contacting is greatest.
  • the resistivity of the composite comprising nanotubes at room temperature should be approximately between 600 and 7500 ⁇ mm 2 / m, and more preferably between 75 ⁇ mm 2 / m and 3,750 ⁇ mm 2 / m.
  • the area A in the YZ direction in FIG. 5 [mm 2 ] and the length L [mm] in the X direction enter into the same in accordance with the distance between the electrodes.
  • carbon nanotubes adsorbed on cellulose fibers with a layer thickness of about 200 ⁇ m were used as the composite material, which have distinguished themselves by the required stability, easy processability and good thermal performance.
  • a change in the desired heat generation of the heating element can also be achieved simply by selecting a thicker or thinner sheet-like composite material, since the heating power achieved is also dependent on the layer thickness of the sheet-like composite material.
  • the resistance and thus the recoverable heat can also be adjusted via the composition of the composite material or for a given composite material on the arrangement of the electrodes and their shape. The more contacts are provided on the composite material and the shorter their distance from each other, the lower the resistance.
  • the heating element according to the invention over the conventional is its lower susceptibility to corrosion.
  • the heat-generating composite material can be well attached, and it can be easily adapted to a variety of shapes, for example, by simply cutting with a pair of scissors. If desired, it can also be rolled or folded.
  • the resistivity of the laminated composite should be between 600 and 7,500 ⁇ mm 2 / m, preferably between 75 and 3,750 ⁇ mm 2 / mm.
  • the resistance of the heating element according to the invention is in the temperature range between - 20 0 C and + 20 0 C substantially constant and slightly higher than in the conventional mirror heating.
  • Heating element for example for use as a heat exchanger
  • a further variant of the present invention provides for the use of the composite material according to the invention in a heating element, wherein the composite material is formed as a planar layer and on each side of the sheet-like layer electrically conductive elements are provided which have a contact surface and abut the sheet-like layer, wherein the at least one composite system is received under at least light pressure between the elements.
  • a heating element is formed which is compact in its construction and can deliver the heat generated in the composite system to a solid, liquid or gaseous medium via the electrically conductive elements.
  • a voltage heat is generated in the composite system, with increasing heat, the resistance in the composite system is increased, which in turn a higher heat output can be achieved.
  • a relatively high temperature can be achieved in a very short time.
  • this embodiment also has the advantage that the heat is not emitted at points, but distributed over the entire surface of the composite system evenly distributed to the contact surfaces.
  • the composite system generates heat even when individual spots or areas should be damaged.
  • This heating element is also adaptable to various shapes and geometries, so that in addition to a compact design, the use in different applications is possible.
  • one or both contact surfaces can be pressurized. This reduces the contact resistance and increases the heat yield.
  • the contact surfaces of the electrically conductive elements are flat and plane parallel. This is preferably used with plate-shaped elements. This allows easy manufacture and assembly with the composite system. Alternatively, it can be provided that a corrugated or flat V-shaped shape of the O ber Assembly is provided to increase the contact surfaces. The opposing contact surfaces are formed congruent to each other, so that a uniform surface pressure of the sheet-like composite system between the two electrically conductive elements is given.
  • the electrical elements are formed of thermally conductive material. This allows a quick removal of the heat to the outside, ie away from the contact surfaces, carried out, whereby a transition of the heat energy is made possible in a solid, liquid or gaseous medium.
  • thermally conductive material For example, copper, silver, aluminum or the like can be used.
  • the electrically conductive elements are plate-shaped, half-shell-shaped, wave-shaped or formed by arbitrary free-forms, and have connection sections or heat-conducting elements opposite the contact surface.
  • slats may be provided as heat-conducting elements, which project into a flow channel, so that the flow of liquid and gaseous medium is heated.
  • the terminal portions may be formed as solid body portions which are to be heated or receive solid media for heating or have contact surfaces for heating solid media, liquid or gas-filled units.
  • the electrically conductive elements take on the connection sections on chambers, which are flowed through by a liquid or gas.
  • a heating of the liquid or of the gas can be achieved, the use of which is manifold.
  • such an arrangement may be provided in a boiler or hot water tank to heat the water or other liquid.
  • surface sections or volume of space can be heated.
  • the heating element is preferably adjustable with respect to its maximum heating temperature by the preselected voltage.
  • the composite system can be heated to a maximum temperature depending on its thickness, its design and its surface pressure acting thereon. By applying a specific voltage, the maximum heating temperature can be determined and limited.
  • a composite system in the form of a liquid or a gel is sprayed or applied to the contact surfaces of the electrically conductive elements.
  • the contact surfaces and the electrically conductive elements are optimally prepared and then positioned and fixed to each other.
  • the at least one composite system has a layer thickness in a range of 50 to 1000 microns.
  • a layer thickness in particular in a range between 150 and 200 microns, a particularly rapid heating was made possible.
  • a temperature of about 110 0 C was beginning with a starting temperature of about 28 0 C within about 170 sec. Attained.
  • nanotube / fiber composite systems according to the invention can be produced in various ways.
  • nanotubes according to variant A are dispersed directly with dry fibers in water (see the following experiment)
  • the nanotubes according to variant B can be dispersed as a stock solution (cf., subsequent experiments 2 and 6) and added to a prepared pulp (cf subsequent experiments 3, 4, 5 and 7).
  • the suspensions can be used both on a professional sheet former, for example, the company Haage, as well as a standard laboratory filter slide.
  • the resistances quoted in ohms / cm were measured with the measuring cell of an Hewlett Packard LCR meter.
  • the measuring cell consists of a circular contact in the center and an annular second contact, which is located at an exactly equal distance of 1 cm from the center.
  • the digital LCR meter used uses a measuring voltage of 3 V for resistance determination.
  • the surface charges of the dispersions were measured using a PCD 03 from Mira Mütek.
  • MWCNT multi-walled carbon nanotubes
  • 4.0 g of eucalyptus cellulose from Ceasa are mixed in 250 g of water for 15 minutes with an ultrasound machine from Banelin with a power of 100% corresponding to 200 W dispersed.
  • 100 g are diluted to a solids content of 0.5% and produced in a sheet former from Haage with a basis weight of 120 g / m 2 .
  • the resulting material has a resistance of 3.5 ohms / cm (corresponding to 27 ohms / sq). The covering is complete.
  • Example 2 demonstrates the preparation of a mother suspension without the use of dispensing aids.
  • a mother liquor is used to prepare a material with a total content of 10% CNT: 15 g suspension from example 2 (ml) are diluted with 85 g deionized water with stirring. This suspension is added slowly with stirring to 135 g of suspension of a 1% suspension of Norland pulp. The resulting mixture is aspirated on a 50 micron mesh metal screen.
  • the material has an ohmic resistance of 8.5 ohms / cm (corresponding to 65.5 ohms / sq).
  • the composite contains nanotubes at a concentration of 10%, the coverage is complete.
  • This example shows the use of wool as a pulp: 0.3 g of a 19 micron roving wool is mixed with 50 ml of deionized water. 1 g of the mother liquor according to Example 2 are added. The wool threads are removed after a contact time of 30 minutes from the solution and felted by heating in boiling water. The wool composite has a resistance of 8 k ⁇ hm / cm (corresponding to 61.6 k ⁇ hm / sq).
  • a material is prepared which demonstrates the conductivity limit: 1.5 g suspension from Example 2 (Ml) are diluted with stirring with 80 g deionized water. This suspension is slowly stirred into 148.5 g of a suspension
  • the resulting mixture is aspirated on a 50 micron mesh metal screen.
  • the material has an ohmic resistance of 2.7 kOhm / cm (corresponding to 20.8 kOhm / sq).
  • the composite contains nanotubes at a concentration of 1%. The calculated coverage is 0.83.
  • a strong cationic conductive resin is used to facilitate the deposition of CNTs on the fibers.
  • This example demonstrates that the conductivity achieved is higher by using the cationic excipients than in Reference Example 3: 15 g suspension of Example 6 (M2) are diluted with stirring 85 g deionized water.
  • This suspension is added slowly with stirring to 135 g of suspension of a 1% suspension of Norland pulp.
  • the resulting mixture is aspirated on a 50 micron mesh metal screen.
  • the material has an ohmic resistance of 3.4 ohms / cm (corresponding to
  • the composite contains nanotubes at a concentration of 10%, the coverage is complete.
  • PVA polyvinyl alcohol
  • M3 2 g of multi-walled carbon nanotubes (MWCNT) from the company Ahwahnee are slurried with 196.5 g of water. Thereafter, 1.5 g Mowiol 24/88 solution (10% in water, manufacturer Clariant) was added. The material is added with an ultrasonic device from Bandelin with 10% power accordingly. The material is dispersed with an ultrasonic device from Bandelin with 10% power corresponding to 20 W. Duration: 1 hour. The resulting stock quench contains nanotubes at a concentration of 1%.
  • MWCNT multi-walled carbon nanotubes
  • Example 8 15 g suspension of Example 8 (M3) are diluted with stirring with 85 g of deionized water. This suspension is added slowly with stirring to 135 g suspension with 1% suspension of Norland pulp. The resulting mixture is carried on a metal screen
  • the material has an ohmic resistance of 8.9 cm (corresponding to 68.5 ohms / sq).
  • the composite contains nanotubes at a concentration of 10%.
  • MWCNT multi-walled carbon nanotubes
  • SWCNT single-walled carbon nanotubes
  • the copper silk process uses the property of copper tetraar ⁇ ine complexes to dissolve cellulose.
  • the polymers comprising the nanotubes can then be further processed, for example, into planar structures.
  • the product has a resistance of 1,300 ohms / cm (equivalent to 10010 ohms / sq).
  • FIGS. 1 and 2 show an SEM image of a sample with a carbon nanotube content of 10% by weight on cellulose
  • FIGS. 3 and 4 the SEM images of a sample with a carbon nanotube content of 1% on cellulose.
  • Figures 1 and 2 and 3 and 4 differ in each case in the magnification.
  • Fig. 1 the composite of carbon nanotubes and cellulose fibers can be seen, the cellulose is clearly visible in the surface topography.
  • the cavities in the cellulosic structure are largely filled by carbon nanotubes.
  • Fig. 2 it can be clearly seen how the surface of the cellulose fibers is covered with the carbon nanotubes. Also individual particles can be seen. In Fig. 3, the cellulose fibers and the unfilled voids between the fibers are shown.
  • Fig. 4 can be seen on the surface very well individual nanotubes, not completely cover the surface of the cellulose fiber.
  • FIG. 5 shows a schematic representation of a mirror heater with the heating element according to the invention (exploded view)
  • FIG. 6 shows the side of the inventive (a) and a conventional (b) heating element adhered to the mirror
  • FIG. 7 various possible contacts (a, b) of the mirror heater
  • FIG. 10 shows temperature measurements on a device according to the invention
  • FIG. 11 is a perspective view of another variant of the heating element for liquid and gaseous media
  • FIG. 12 shows a diagram of a heating element in which the temperature is plotted as a function of the voltage
  • 13 shows a warm-up curve of a heat exchanger with the composite material according to the invention
  • Figure 14 is a perspective view of a heating element as a water heater.
  • the planar, nanotube composite system 12 in this embodiment is a composite of carbon nanotubes adsorbed on the surface of cellulosic fibers.
  • the composite material 12 is paper-like. With the side facing in the + z direction (in the xy plane), the composite material is adhered to the back of a mirror 16.
  • the contacts 13, 14 positive and negative electrodes are attached to apply the voltage required for the current flow.
  • the contacts can be done, for example, that they are glued directly to the surface of the composite material, the adhesive must of course be electrically conductive. Also, the contact strips can be glued to a foil and aligned with the contacting side on the surface of the composite system and all laminated together.
  • FIG. 7a shows the simplest and most cost-effective arrangement of the electrodes.
  • 7b shows "toothed" electrodes, because of the larger electrode area and the small distance between the electrodes, the resistance decreases.
  • the nanotube composite material consisting of carbon nanotubes substantially adsorbed on cellulosic fibers was investigated and the following measurements were obtained: approx. 6,000 ⁇ mm 2 / m - without power connection at ambient temperature + 20 0 C, approx. 4,200 ⁇ mm 2 / m - with a connection of 13.8 V and an ambient temperature of -10 0 C
  • the investigated composite material of adsorbed carbon nanotubes was 200 ⁇ m thick (its surface was approximately 14,000 mm 2 ).
  • FIGS. 8 and 9 show that with the heating elements according to the invention a faster heating takes place than with the conventional heating elements.
  • the temperature of 0 0 C melting temperature of the ice
  • the further temperature rise after The melting of the ice is also faster with the heating element according to the invention than in the conventional mirror heaters, which also brings a faster evaporation of thawed ice and condensation with it.
  • FIG. 10 shows the temperature increase (and thus the heating) as a function of the applied voltage in the low-voltage region on a heating element with the composite material according to the invention.
  • the results show that temperatures of 100 ° C. can be achieved with the heating element according to the invention.
  • the highest temperature increase (of about 100 ° C.) is observed at the lowest voltage of 3V and the lowest temperature increase is observed at a voltage of 6V.
  • FIG. 11 shows in perspective a further variant of the heating element 111 according to the invention, which can serve for heating liquid or gaseous media.
  • a composite system 114 is provided which comprises nanotubes.
  • Each of these electrically conductive elements 112 has contact surfaces 116 facing and resting against the composite system 114 and holding it between the elements 112.
  • An unspecified fastening system for example, by a detachable screw, clamping or clamping connection, an adjustable pressure on the elements 112 and their contact surfaces 116 can act on the sheet-like composite system 114.
  • an adhesive connection may be provided.
  • a positive electrode 118 is connected to the one element 112 and, opposite to the element 112, a negative electrode 119 is provided.
  • sealing or shielding elements can be provided between the two electrically conductive elements 112 in order to protect the laminar composite system 114 from external influences.
  • the composite system 114 may be formed equal to or smaller than the contact surfaces 116. Several composite systems 114 may also be provided to form a large-scale composite system 114.
  • the heating of the composite system 114 as a function of the voltage is shown in FIG.
  • the heating element according to Figure 11 can be heated to a temperature of for example 125 0 C. This temperature was tapped on the composite system 114.
  • a voltage of, for example 9 volts a temperature of 150 0 C can be achieved.
  • a warm-up curve of the heating element 111 shown in FIG. 11 is recorded by way of example.
  • a temperature of about 120 ° C. is reached in less than about 180 seconds.
  • a composite system 114 was used between two electrically conductive elements 112 made of aluminum, with the composite system 114 having a layer thickness in the range of 100 to 200 ⁇ m.
  • a further increase in the temperature is not given at a constant voltage, so that over the preselected voltage with respect to a particular composite system 114, a temperature setting is possible.
  • the heating element 111 of the invention is shown in an application as a water heater.
  • chambers 122 are provided at connection sections, each having a connection 123 for a supply line 124 and a discharge line 125.
  • a cool medium is supplied to the lower chamber 122 via the supply line 124.
  • the heat transferred from the composite system 114 to the electrically conductive elements 112 is transferred to the chamber 122.
  • the liquid is removed from the lower chamber 122 and fed to the upper chamber 122. From there, the heated liquid is supplied to the intended use.
  • the electrically conductive elements 112 and chambers 122 can in principle also be a unit.
  • the length I of the resistivity in the Z direction is measured and thus corresponds to the thickness of the sheet-like layer and the area A corresponds to the area of the composite system which bears against the contact surface 116 of the electrically conductive element 112.
  • a powerful heating element 111 is provided, which is also designed to be robust in function and allows a variety of applications due to the optional geometric design.
  • the laminar composite system 114 may be adapted to different geometries so as to enable different geometries of the electrically conductive elements 112 adapted to installation situations.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Inorganic Fibers (AREA)
  • Paper (AREA)

Abstract

L'invention se rapporte à un système comprenant des nanotubes. Ce système se présente sous la forme d'un système composite, en particulier d'un système composite plat qui comprend des nanotubes et des fibres, les nanotubes étant fixés sur les fibres par adsorption. La présente invention concerne également un procédé de production de ce système qui comporte des nanotubes, les nanotubes ainsi que les fibres étant dispersés dans un agent de dispersion. L'invention se rapporte en outre à l'utilisation de ces matériaux composites dans des éléments de chauffage.
PCT/EP2006/004557 2005-05-19 2006-05-15 Systeme composite comprenant des nanotubes, son procede de production, et son utilisation dans des elements de chauffage Ceased WO2006122736A2 (fr)

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Application Number Priority Date Filing Date Title
DE102005023764.9 2005-05-19
DE200510023764 DE102005023764A1 (de) 2005-05-19 2005-05-19 Nanotubes umfassende Verbundsysteme und Verfahren ihrer Herstellung
DE202005013822U DE202005013822U1 (de) 2005-05-19 2005-08-31 Heizelement
DE202005013822.3 2005-08-31
DE202005013821 2005-08-31
DE202005013821.5 2005-08-31
DE202005014678U DE202005014678U1 (de) 2005-05-19 2005-09-16 Heizelement mit zumindest einem Nanotubes umfasenden Verbundsystem
DE202005014678.1 2005-09-16

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WO2008090031A1 (fr) 2007-01-26 2008-07-31 Tesa Se Élément chauffant et vitre pouvant être chauffée par un élément chauffant
DE102007020058A1 (de) * 2007-04-27 2008-10-30 Siemens Ag Vorrichtung zum Einsatz in der Medizin oder Medizintechnik und Verwendung der Vorrichtung
EP1988747A3 (fr) * 2007-05-03 2009-06-17 Apro Systems Co., Ltd Procédé pour la fabrication d'un dispositif de chauffage de film à l'aide de verre cristallisé résistant à la chaleur
EP2043406A3 (fr) * 2007-09-28 2009-10-28 Tsinghua University Source de chaleur plane
WO2010028740A1 (fr) * 2008-09-15 2010-03-18 Beiersdorf Ag Pansement chauffant
DE102009053040A1 (de) 2008-11-24 2010-05-27 Luk Lamellen Und Kupplungsbau Beteiligungs Kg Fluidsystem
EP2224784A1 (fr) * 2009-02-26 2010-09-01 tesa SE Elément de surface chauffé
WO2011003634A1 (fr) * 2009-07-08 2011-01-13 Siemens Aktiengesellschaft Nanocomposite doté de nanotubes de nitrure de bore
WO2012041715A1 (fr) * 2010-09-29 2012-04-05 Siemens Aktiengesellschaft Nanocomposite électro-isolant présentant des nanoparticules semi-conductrices ou non conductrices, utilisation de ce nanocomposite et procédé pour le produire
DE102011008461A1 (de) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Trennstelle einer Leitungsdurchführung für eine HGÜ-Komponente
DE102011008456A1 (de) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Leitungsführung für HGÜ-Transformatorspulen oder HGÜ-Drosselspulen
DE102011008459A1 (de) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Leitungsdurchführung für die Kesselwand einer HGÜ-Komponente
DE102011008462A1 (de) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Schirmring für eine HGÜ-Transformatorspule oder eine HGÜ-Drosselspule
WO2012093053A1 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Dispositif d'isolation pour un composant de transmission de courant continu haute tension comportant des barrières aux solides de type paroi
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US5800706A (en) * 1996-03-06 1998-09-01 Hyperion Catalysis International, Inc. Nanofiber packed beds having enhanced fluid flow characteristics

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WO2008090031A1 (fr) 2007-01-26 2008-07-31 Tesa Se Élément chauffant et vitre pouvant être chauffée par un élément chauffant
DE102007020058A1 (de) * 2007-04-27 2008-10-30 Siemens Ag Vorrichtung zum Einsatz in der Medizin oder Medizintechnik und Verwendung der Vorrichtung
DE102007020058B4 (de) * 2007-04-27 2016-03-03 Siemens Aktiengesellschaft Vorrichtung zum Einsatz in der Medizin oder Medizintechnik und Verwendung der Vorrichtung
EP1988747A3 (fr) * 2007-05-03 2009-06-17 Apro Systems Co., Ltd Procédé pour la fabrication d'un dispositif de chauffage de film à l'aide de verre cristallisé résistant à la chaleur
EP2043406A3 (fr) * 2007-09-28 2009-10-28 Tsinghua University Source de chaleur plane
CN102159164A (zh) * 2008-09-15 2011-08-17 拜尔斯道夫股份有限公司 热敷布
WO2010028740A1 (fr) * 2008-09-15 2010-03-18 Beiersdorf Ag Pansement chauffant
DE102009053040A1 (de) 2008-11-24 2010-05-27 Luk Lamellen Und Kupplungsbau Beteiligungs Kg Fluidsystem
JP2010199071A (ja) * 2009-02-26 2010-09-09 Tesa Se 加熱平面要素
CN101848565A (zh) * 2009-02-26 2010-09-29 德莎欧洲公司 热平面元件
KR101650440B1 (ko) 2009-02-26 2016-08-23 테사 소시에타스 유로파에아 가열된 평면 소자
US8283612B2 (en) 2009-02-26 2012-10-09 Tesa Se Heated planar element
KR20100097629A (ko) * 2009-02-26 2010-09-03 테사 소시에타스 유로파에아 가열된 평면 소자
EP2224784A1 (fr) * 2009-02-26 2010-09-01 tesa SE Elément de surface chauffé
WO2011003634A1 (fr) * 2009-07-08 2011-01-13 Siemens Aktiengesellschaft Nanocomposite doté de nanotubes de nitrure de bore
WO2012041715A1 (fr) * 2010-09-29 2012-04-05 Siemens Aktiengesellschaft Nanocomposite électro-isolant présentant des nanoparticules semi-conductrices ou non conductrices, utilisation de ce nanocomposite et procédé pour le produire
US9171656B2 (en) 2010-09-29 2015-10-27 Siemens Aktiengesellschaft Electrically insulating nanocomposite having semiconducting or nonconductive nanoparticles, use of this nanocomposite and process for producing it
WO2012093054A1 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Point de coupure d'un passage de conduite pour un composant de transmission de courant continu haute tension
WO2012093055A1 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Guide de conduites pour des transformateurs de transmission de courant continu haute tension et des bobines de réactance de transmission de courant continu haute tension
WO2012093023A2 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Passage de conduite pour la paroi de cuve d'un composant de transmission de courant continu haute tension
WO2012093052A1 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Anneau de protection pour une bobine de transformateur de transmission de courant continu haute tension ou une bobine de réactance de transmission de courant continu haute tension
DE102011008454A1 (de) 2011-01-07 2012-07-26 Siemens Aktiengesellschaft Isolationsanordnung für eine HGÜ-Komponente mit wandartigen Feststoffbarrieren
WO2012093053A1 (fr) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Dispositif d'isolation pour un composant de transmission de courant continu haute tension comportant des barrières aux solides de type paroi
DE102011008462A1 (de) 2011-01-07 2012-07-12 Siemens Aktiengesellschaft Schirmring für eine HGÜ-Transformatorspule oder eine HGÜ-Drosselspule
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