WO2011141461A1 - Composition thermoconductrice comprenant des nanotubes de carbone thermoconducteurs et une phase métallique continue - Google Patents

Composition thermoconductrice comprenant des nanotubes de carbone thermoconducteurs et une phase métallique continue Download PDF

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Publication number
WO2011141461A1
WO2011141461A1 PCT/EP2011/057516 EP2011057516W WO2011141461A1 WO 2011141461 A1 WO2011141461 A1 WO 2011141461A1 EP 2011057516 W EP2011057516 W EP 2011057516W WO 2011141461 A1 WO2011141461 A1 WO 2011141461A1
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Prior art keywords
carbon nanotubes
polymer
thermally conductive
metal
weight
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PCT/EP2011/057516
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German (de)
English (en)
Inventor
Stephanie Reich
Thomas STRAßBURG
Vitaliy Datsyuk
Stephan Arndt
Izabela Firkowska
Katayoun Gharagozloo-Hubmann
Milana Lisunova
Svitlana Trotsenko
Anna-Maria Vogt
Maria Kasimir
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Freie Universität Berlin
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Publication of WO2011141461A1 publication Critical patent/WO2011141461A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/174—Derivatisation; Solubilisation; Dispersion in solvents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1005—Pretreatment of the non-metallic additives
    • C22C1/101—Pretreatment of the non-metallic additives by coating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/10—Alloys containing non-metals
    • C22C1/1094—Alloys containing non-metals comprising an after-treatment
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • C22C2026/006—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes with additional metal compounds being carbides

Definitions

  • the present invention relates to polymer-modified carbon nanotubes according to claim 1, a thermally conductive composition according to claim 7, their use according to claim 13 and a process for producing the polymer-modified carbon nanotubes according to claim 14 and a process for the preparation thereof the thermally conductive composition according to claim 17.
  • Aluminum is currently the most widely used material for dissipating and spreading heat due to its low cost, low density, availability and good processibility. Copper is also very well suited for heat dissipation, but is more difficult to process and has a 3.5 times higher density than aluminum. Although copper has a higher thermal conductivity at 380 W / m * K than aluminum, which has a thermal conductivity of 180 W / m * K, the density of copper is 8.9 gm / cm 3 above the density of aluminum ( 2.7 gm / cm 3 ). Also, the coefficient of thermal expansion of copper at 16.6 ppm / K is too large for use in a semiconductor. In addition, the ratio of thermal conductivity to density for copper is 44, whereas for aluminum this ratio is 64. For this reason, aluminum is preferably used for dissipating heat to copper, especially when the weight plays an important role.
  • the resulting waste heat is an ever greater problem.
  • the geometry of the heat dissipator made of aluminum or copper is a limiting factor.
  • the heat sink must have relatively large dimensions, while using copper as a heat sink outweighs the weight and geometry issues.
  • the geometry of a heat dissipater must fit into the room, which after optimized packing of the device is present. This results in the need to use a Cyprusabieiters that is arbitrarily malleable.
  • Carbon nanotubes are large macromolecules in the form of graphite films (a hexagonal lattice with sp 2 configuration), which are rolled up in the form of a cylinder ("single-walled carbon nanotubes", SWNT).
  • single-walled carbon nanotubes In addition to the single-walled carbon nanotubes, carbon nanotubes with two or more walls are also known (“double-walled carbon nanotubes", MWNT), the latter being described as one cylinder incorporated into another cylinder.
  • Carbon nanotubes are characterized by high strength, low weight, specific electronic structure, high stability and excellent thermal conductivity.
  • the thermal conductivity of carbon nanotubes at room temperature can be between 1800 to 6000 W / m * K (Hone et al., Synthetic metals, 1999, 103: 2498), with the coefficient of thermal expansion (CTE) at values of 0 ppm / k (Deng et al., Mat. Lett, 2008, 62: 2301-2302).
  • the fabrication of such devices requires the control of various process conditions, such as the deposition of adhesion and diffusion layers, the orientation and configuration of carbon nanotubes, or the temperature to be employed.
  • Another significant disadvantage is that the heat flow from the carbon nanotubes to the surface of the metallic conductor is limited by the presence of adhesion, diffusion and catalyst layers.
  • control of the orientation and spacing between the carbon nanotubes is significantly dependent on the preparation of the catalyst particles.
  • the catalyst particles are first patterned by means of photolithography, microcontact printing or deposition by means of a metal mask.
  • the deposition of carbon nanotubes over a relatively large substrate surface is necessary.
  • the present invention is therefore based on the problem to provide a thermally conductive composition and a process for their preparation, which does not have the disadvantages mentioned above.
  • the present invention relates to polymer modified carbon nanotubes, in particular single-walled carbon nanotubes (SWNT), two-walled carbon nanotubes (DWNT), multi-walled carbon nanotubes (MWNT) or mixtures thereof.
  • SWNT single-walled carbon nanotubes
  • DWNT two-walled carbon nanotubes
  • MWNT multi-walled carbon nanotubes
  • the carbon nanotubes preferably have a diameter between 0.2 and 100 nm, with the aspect ratio not exceeding 1, 000,000.
  • the thermal conductivity of the carbon nanotubes used is at least 10 W / mK.
  • the carbon nanotubes are preferably modified with a side chain homopolymer and / or copolymer selected from a group comprising poly (sodium 4-styrenesulfonate), poly (vinyl sulfate), poly (phenyl alcohol) and poly (methacrylic acid).
  • the side chains preferably have a negative charge, but may also be uncharged. Importantly, these side chains allow the attachment of cations, especially metal cations, to the polymer surface.
  • the polymers are preferably adsorbed non-covalently on the nanotubes and envelop them.
  • the preferred polymers have functionalities that allow further modification of the carbon nanotubes.
  • metal ions are bound to the polymer surface of the nanotubes.
  • the metal ions may be selected from a group containing aluminum, copper, silver, gold, nickel, iron ions and a mixture thereof.
  • the carbon nanotubes have metal oxides bonded to the polymer surface.
  • the present invention also relates to a thermally conductive composition
  • a thermally conductive composition comprising at least one continuous metal phase and thermally conductive carbon nanotubes (CNT).
  • the composition according to the invention is characterized in that the thermally conductive carbon nanotubes are dispersed homogeneously but undirectedly in the at least one metal phase.
  • the composition of the present invention thus has a metallic phase having a plurality of carbon nanotubes which has high thermal conductivity, a low coefficient of thermal expansion (CET) and a low density and thus is well suited for use as a heat sink in semiconductor devices.
  • the metal phase extends substantially the entire width or thickness of the composition, with the majority of the carbon nanotubes being uniformly covered by the continuous metal phase.
  • the summary preferably does not include any other materials other than
  • Carbon nanotubes and the metal or metal alloys Carbon nanotubes and the metal or metal alloys.
  • the thermally conductive composition according to the invention allows the targeted adjustment of the coefficient of thermal expansion by variations of the individual components of the composition. Thus, it is possible to tailor this coefficient specifically to the material of the semiconductors or insulating materials.
  • the composition preferably has an amount ratio of 0.2 to 80% by weight, preferably 1 to 70% by weight, particularly preferably 1 to 50% by weight of carbon nanotubes and 20 to 99.8% by weight, preferably 30 to 99% by weight, particularly preferably 50 to 99% by weight of the at least one metal.
  • the thermally conductive carbon nanotubes (CNT) used are preferably selected from the group consisting of single-walled carbon nanotubes (SWNT), two-walled carbon nanotubes (DWNT), multi-walled carbon nanotubes (MWNT) or mixtures thereof.
  • the composition comprises the polymer-modified carbon nanotubes described above, in particular the metal ion-modified carbon nanotubes.
  • the continuous metal phase is preferably a metal selected from a group containing aluminum, copper, silver, gold, nickel, iron or a mixture thereof.
  • the thermal conductivity of the composition of the present invention is preferably in a range of 10 to 700 W / mK, preferably 50 to 500 W / mK, particularly preferably 100 to 300 W / mK and the coefficient of thermal expansion (CTE) in a range of 5 to 15 ppm / K, preferably 7 to 12 ppm / K and is dependent on the content of carbon nanotubes.
  • composition of the invention is preferably used as a thermo-regulatable material, for the production of heat sinks or heat spreaders.
  • the composition can also be used for electronic packaging or electromagnetic shielding. Also, applications in the field of thermal management are possible.
  • the object of the present invention is likewise achieved by a method for producing the polymer-modified carbon nanotubes according to claim 14 and a method for producing the composition according to the invention as claimed in claim 17.
  • the process for producing the polymer-modified carbon nanotubes thus comprises the following steps: dispersion of carbon nanotubes in at least one Polymer solution and applying ultrasound for a period of 1 to 10 h and removing the excess polymer and optionally washing the residue. If necessary, this process step can be repeated up to three times. Subsequently, the modified carbon nanotubes are dried at temperatures of 60 ° C in air. The carbon nanotubes are now partially or completely surrounded by a polymer.
  • homopolymers and / or copolymers selected from a group containing poly (sodium 4-styrenesulfonate), poly (vinyl sulfate), poly (ethylene oxide), poly (ethylene glycol), poly (phenyl alcohol) and poly (methacrylate) are used.
  • the polymer-modified carbon nanotubes can then be dispersed in a suitable solvent, suitable solvents being selected from the group comprising water, N, N-dimethylformamide, dimethyl sulfoxide, alcohols, in particular methanol, ethanol, isopropanol, propanol, butanol, or ketones, in particular acetone.
  • suitable solvents being selected from the group comprising water, N, N-dimethylformamide, dimethyl sulfoxide, alcohols, in particular methanol, ethanol, isopropanol, propanol, butanol, or ketones, in particular acetone.
  • a homogeneous distribution of the polymer-modified carbon nanotubes in the solvent is achieved by applying ultrasound.
  • At least one metal salt is added to this homogeneous dispersion, a suitable metal salt being selected from a group comprising copper citrate, copper acetate, copper butyrate, copper cyclohexane butyrate, copper ethylacetoacetate, copper 2-ethylhexanoate, copper formate, copper gluconate, copper decanoate, copper oxalate, copper acetate, aluminum nitrate, aluminum acetate, Aluminum n-butoxide, aluminum sec-butoxide, aluminum tert-butoxide, aluminum dimethyl amide, aluminum ethoxide, aluminum pentanedionate, or mixtures thereof.
  • a suitable metal salt being selected from a group comprising copper citrate, copper acetate, copper butyrate, copper cyclohexane butyrate, copper ethylacetoacetate, copper 2-ethylhexanoate, copper formate, copper gluconate, copper decanoate, copper oxalate,
  • a homogeneous dispersion is also produced in this step.
  • These homogeneous dispersions are then stirred for a period of 5 to 20 hours, preferably 7 to 15 hours, more preferably 12 hours, to form chemical bonds between the negatively charged functionalities on the surface of the polymer-coated carbon nanotubes and the metal cations.
  • the solvent is preferably removed by heating the dispersion to temperatures between 50 and 70 ° C and a powder comprising polymer-modified carbon nanotubes with metal ions bound on the polymer surface is obtained.
  • this powder may be a calcination at temperatures between 200 and 350 ° C over a period of 30 min to 5 h, preferably 1 h to 4h, more preferably 1 h, wherein the metal ions undergo oxidation to the corresponding metal oxide to provide a powder of polymer-clad carbon nanotubes with a surface modified with a metal oxide.
  • the calcined powder containing metal oxide-modified carbon nanotubes may subsequently undergo reduction in a reducing atmosphere, especially hydrogen amosphere, at temperatures between 150 ° C and 500 ° C, preferably between 200 ° C and 350 ° C, more preferably at 250 ° C, for a period of 30 minutes to 5 hours, preferably 1 hour to 4 hours, particularly preferably 1 hour.
  • This reduction step results in the preparation of the inventive composition of polymer-modified carbon nanotubes and reduced metal, wherein the carbon nanotubes are homogeneously dispersed in the metal phase.
  • the powder can be compacted at pressures between 50 to 70 MPa and optionally sintered.
  • the inventive thermally conductive composition consisting of a continuous metal phase and thermally conductive carbon nanotubes is therefore produced in a preferred embodiment by means of the method steps described.
  • An important aspect of the production process is that the metal ions or metal oxides arranged on the carbon nanotubes cause the formation of the continuous metallic phase during the reduction step. This ensures a homogeneous and non-directional distribution of the carbon nanotubes in the metallic phase.
  • the carbon nanotubes are therefore arranged directly in the metal and not on its surface.
  • Such compositions have an ideal microstructure enabling their use as a thermally conductive material.
  • FIG. 1 shows a flow chart for illustrating the method steps for producing a composition according to the invention
  • Figure 2 is an electron micrograph of a bundle of carbon nanotubes
  • Figure 3 is an electron micrograph of polymer modified
  • FIG. 4 shows a scanning electron micrograph of polymer-modified carbon nanotubes provided with a metal oxide
  • Figure 5 is a diagram with a Raman spectrum of a novel
  • Multi-walled carbon nanotubes (0.5 g) (FIG. 2) are dispersed in an aqueous solution of 1% by weight of poly (sodium 4-styrenesulfonate) and exposed to ultrasound for 5 hours. Excess polymer is then removed by filtration and the residue washed with water. This step can be repeated up to three times.
  • the polymer modified carbon nanotubes are dried at 60 ° C in the presence of air.
  • FIG. 3 shows a picture of carbon nanotubes modified in this way.
  • the sonicated dispersion is stirred for 12 hours, allowing the formation of chemical bonds between the copper ions and those on the Surface of the carbon nanotubes arranged negatively charged side chains of the polymer comes.
  • the dispersion After stirring, the dispersion is heated to temperatures above 70 ° C to remove the ethanol and then calcined at 200 ° C and 350 ° C for one hour, respectively. In this case, a powder comprising copper oxide-modified carbon nanotubes is obtained (see FIG. 4).
  • the powder is reduced under hydrogen gas atmosphere in an oven at 250 ° C for one hour. This results in the reduction of the copper oxide to metallic copper, which forms a continuous metallic phase, in which the carbon nanotubes are dispersed.
  • the reduced powder was examined by X-ray diffraction analysis and the phase state of the reduced powder was determined (FIG. 7).
  • the reduced powder is compacted at a pressure of 50 MPa and sintered at 750 ° C for 10 minutes.
  • the thermal diffusion ⁇ of the inventive composition of embodiment 1 is determined by means of the xenon flash method (XFA 500, Linseis, Germany). The determined value of the thermal diffusion ⁇ is 0.35 cm 2 / s.
  • the specific heat c p is measured by differential scanning calorimetry (DSC, Linseis, Germany). The determined value of the specific heat c p is 5.5 J / gK
  • the coefficient of thermal expansion CTE is determined by means of a dilatometer (DI L L76, Linseis, Germany). The determined value of the thermal expansion ⁇ is 12 ppm / K (at 25 ° C).
  • the density of the copper nanocomposites with a proportion of 5% by weight of carbon nanotubes is 6.28 g / cm 3 .
  • the thermal conductivity k of the powdered composition is determined by means of the xenon flash method (XFA 500, Linseis, Germany) and hot-disk method (TPS 2500, Hot Disc AB, Sweden). The thermal conductivity k of the composition is also determined by the following equation:
  • Embodiment 2 Another embodiment of the composition of the present invention is prepared similarly to the process steps described in Example 1, using as the polymer poly (vinyl sulfate) instead of poly (sodium 4-styrene sulfonate).

Abstract

La présente invention concerne des nanotubes de carbone modifiés par des polymères, une composition thermoconductrice comprenant au moins une phase métallique continue et des nanotubes de carbone (CNT) thermoconducteurs, ainsi que des procédés de fabrication de ceux-ci.
PCT/EP2011/057516 2010-05-10 2011-05-10 Composition thermoconductrice comprenant des nanotubes de carbone thermoconducteurs et une phase métallique continue WO2011141461A1 (fr)

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DE102010028801A DE102010028801A1 (de) 2010-05-10 2010-05-10 Thermisch leitfähige Zusammensetzung umfassend thermisch leitfähige Kohlenstoffnanoröhren und eine kontinuierliche Metallphase

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2990390A1 (fr) 2014-08-27 2016-03-02 D. Swarovski KG Composition de verre luminescent

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