WO2011047743A1 - COMPOSITE MATERIALS CONSISTING OF METALS IN WHICH CARBON NANOTUBES (CNTs) ARE DISPERSED - Google Patents
COMPOSITE MATERIALS CONSISTING OF METALS IN WHICH CARBON NANOTUBES (CNTs) ARE DISPERSED Download PDFInfo
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- WO2011047743A1 WO2011047743A1 PCT/EP2010/004781 EP2010004781W WO2011047743A1 WO 2011047743 A1 WO2011047743 A1 WO 2011047743A1 EP 2010004781 W EP2010004781 W EP 2010004781W WO 2011047743 A1 WO2011047743 A1 WO 2011047743A1
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- 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
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
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- 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
Definitions
- the present invention relates to the production of composites of metals or metal alloys having carbon nanotubes (CNTs) dispersed therein.
- CNTs carbon nanotubes
- Composites of metals and CNTs are known and have a high mechanical strength, good thermal conductivity and a low specific gravity. These properties make composites of metals and CNTs interesting materials for high thermal stress machine parts, e.g. for pistons in internal combustion engines.
- DE 10 2007 051 570 discloses the production of CNT metal composites by heating a laminate of CNT material and metal foils so that the metal penetrates and "infiltrates" the CNT layer, a similar process described in WO 2009/056544 by the infiltration of paper-like, non-woven layers of CNT material with metals at elevated temperature.In order to improve the infiltration, first a treatment of the CNTs with the wetting-promoting metal alloys is carried out.
- this object is achieved by a method for producing composite materials from carbon nanotubes (CNTs) and metals
- the mixtures used according to the invention contain one or more first metals and / or metal alloys.
- the mixture contains metals / metal alloys, which are the dispersion of the CNTs in a molten metal improve.
- Suitable as the first metal or metal alloy are one or more substances selected from the group nickel, aluminum, titanium.
- the mixtures may contain 0, 1 - 10 weight percent, preferably 2 - 6 weight percent (based on the total amount of the mixture) of CNTs.
- the mixture of the CNTs and the first metals or metal alloys is produced by a common grinding process.
- Ball mills are particularly suitable for this purpose.
- the meal in a ball mill for a maximum of 0.5 hours at a maximum speed of 200 rpm (revolutions per minute).
- the milling process is carried out so that the mixture after the grinding process has a mean particle size d 50 more than 75 microns, preferably greater than 100 microns. If the grinding or mixing process is carried out to a powder particle size of d 5 o ⁇ 75 microns, this can lead to the destruction of the CNTs.
- the resulting mixture is sintered, pressed or extruded at elevated temperature. It has proven to be advantageous to press the mixture in tablet form before this processing step, since in particular sintered tablets are easier to handle in the following.
- the processed, in particular sintered CNT / metal mixtures are dispersed in the next process step in the melt of at least one second metal and / or a second metal alloy.
- first and second metals and / or metal alloys may be the same or different.
- second metal or metal alloy it is also possible to use one or more substances selected from the group of aluminum alloys and cast alloys. To improve the dispersion, it is recommended to mix the melt with an agitator (impeller).
- the resulting composites may be made by any known powder and melt metallurgy processes such as extrusion, thixoforming, casting, die casting or gravity casting and by molding techniques, e.g. by forming, forging, continuous casting or extrusion.
- the composite materials produced according to the invention have an increased basic strength while retaining the original elongation behavior and the modulus of elasticity and are particularly suitable for the production of thermally stressed components, such as e.g. Piston suitable in internal combustion engines.
- the following powder mixtures (particle size ⁇ 45 ⁇ m) were initially used as matrix material for the sintered tablets:
- the meal was redetermined and set at 0.5 h (at a rotational speed of 200 rpm). Using these parameters, tablets of pure aluminum with 4 wt% and Ti 6 Al 4 V with 4 wt% CNTs were subsequently produced. In the melt test, the tablets of pure aluminum showed a very limited melting. It formed in the crucible a swamp that was soft, but still largely had the shape of the tablets. The aluminum probably melted, but the CNT network of the tablet could not be dissolved (see Figures 2 and 3).
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
Description
Verbundwerkstoffe aus Metallen mit darin dispensierten Carbon-Nanotubes (CNTs) Composites of metals with carbon nanotubes (CNTs) dispensed therein
Beschreibung description
Die vorliegende Erfindung betrifft die Herstellung von Verbundwerkstoffen aus Metallen oder Metalllegierungen mit darin dispergierten Carbon-Nanotubes (CNTs). Verbundwerkstoffe aus Metallen und CNTs sind bekannt und weisen eine hohe mechanische Belastbarkeit, gute Wärmeleitfähigkeiten und ein niedriges spezifisches Gewicht auf. Diese Eigenschaften machen Verbundwerkstoffe aus Metallen und CNTs zu interessanten Werkstoffen für thermisch hoch belastete Maschinenteile, z.B. für Kolben in Verbrennungsmotoren. The present invention relates to the production of composites of metals or metal alloys having carbon nanotubes (CNTs) dispersed therein. Composites of metals and CNTs are known and have a high mechanical strength, good thermal conductivity and a low specific gravity. These properties make composites of metals and CNTs interesting materials for high thermal stress machine parts, e.g. for pistons in internal combustion engines.
Bei der Herstellung solcher Verbundmaterialien müssen die CNTs in einer Metallmatrix dispergiert werden, was aufgrund der geringen Mischbarkeit bzw. Benetzbarkeit der CNTs mit Metallen in der Schmelze schwierig ist. Es wurden daher Verfahren zur Herstellung von Verbundwerkstoffe aus Metallen mit CNTs entwickelt, die weitgehend die Verwendung von Metallschmelzen vermeiden. So offenbart zum Beispiel die DE 10 2007 051 570 die Herstellung von CNT-Metallverbundwerkstoffen, indem ein Schichtkörper aus CNT-Material und Metallfolien erhitzt wird, sodass das Metall in die CNT-Schicht eindringt und diese„infiltriert". Ein ähnliches Verfahren die beschreibt WO 2009/056544 durch die Infiltration von papierartigen, non-woven- Schichten von CNT-Material mit Metallen bei erhöhter Temperatur. Zur Verbesserung der Infiltration wird zunächst eine Behandlung der CNTs mit der Benetzung fördernden Metalllegierungen durchgeführt. In the production of such composite materials, the CNTs must be dispersed in a metal matrix, which is difficult due to the low miscibility or wettability of the CNTs with metals in the melt. Therefore, methods have been developed for producing composites of metals with CNTs that largely avoid the use of molten metals. For example, DE 10 2007 051 570 discloses the production of CNT metal composites by heating a laminate of CNT material and metal foils so that the metal penetrates and "infiltrates" the CNT layer, a similar process described in WO 2009/056544 by the infiltration of paper-like, non-woven layers of CNT material with metals at elevated temperature.In order to improve the infiltration, first a treatment of the CNTs with the wetting-promoting metal alloys is carried out.
Die Infiltration einer CNT-Matrix durch Metalle erfolgt unterhalb der Schmelzetemperatur der Metalle und ist dementsprechend ein langwieriger und aufwendiger Prozess und für die Herstellung von größeren Mengen an Verbundwerkstoff zu kostenintensiv. The infiltration of a CNT matrix by metals is below the melt temperature of the metals and is accordingly a lengthy and consuming process and for the production of larger amounts of composite too expensive.
Es ist ebenfalls bekannt, CNTs in eine Metallschmelze einzubringen, was aber aufgrund der schlechten Benetzbarkeit von CNTs mit Metallschmelzen nicht zu befriedigenden Ergebnissen führt. Auch die Aktivierung/Beschichtung von CNTs durch z.B. Zinn, Nickel oder Titan durch chemische Abscheidung schafft hier keine Abhilfe, sondern führt häufig zum Verbrennen der CNTs in der Metallschmelze. Der Erfindung liegt daher die Aufgabe zu Grunde, ein Verfahren zur kostengünstigen Herstellung von Verbundwerkstoffen aus CNTs und Metallen zur Verfügung zu stellen. It is also known to incorporate CNTs into a molten metal, but this does not give satisfactory results due to the poor wettability of CNTs with molten metals. Also, the activation / coating of CNTs by e.g. Tin, nickel or titanium by chemical deposition does not provide a remedy, but often leads to the burning of CNTs in the molten metal. The invention is therefore based on the object to provide a method for cost-effective production of composites of CNTs and metals available.
Erfindungsgemäß ist diese Aufgabe gelöst durch ein Verfahren zur Herstellung von Verbundmaterialien aus Carbon-Nanotubes (CNTs) und Metallen durch According to the invention, this object is achieved by a method for producing composite materials from carbon nanotubes (CNTs) and metals
a) Mischen von single-walled und/oder multiwalled CNTs oder aktivierten/funktionalisierten/beschichteten single-walled und/oder multiwalled CNTs mit mindestens einem ersten Metall und/oder einer ersten Metalllegierung a) mixing single-walled and / or multiwalled CNTs or activated / functionalized / coated single-walled and / or multiwalled CNTs with at least a first metal and / or a first metal alloy
b) Pressen, Sintern und/oder Strangpressen des Gemisches und c) Einbringen des gemäß b) bearbeiteten Gemischs in eine Schmelze aus mindestens einem zweiten Metall und/oder einer zweiten Metalllegierung oder b) pressing, sintering and / or extruding the mixture and c) introducing the mixture processed according to b) into a melt of at least one second metal and / or a second metal alloy or
d) Weiterverarbeitung des Gemischs aus b) durch ein Formgebungsverfahren wie zum Beispiel durch Umformen, Schmieden, d) further processing of the mixture from b) by a shaping process, such as by forming, forging,
Stranggießen oder Strangpressen. Continuous casting or extrusion.
Die erfindungsgemäß verwendeten Mischungen enthalten ein oder mehrere erste Metalle und/oder Metalllegierungen. Bevorzugt enthält die Mischung Metalle/Metalllegierungen, die die Dispergierung der CNTs in einer Metallschmelze verbessern. Geeignet als erstes Metall oder Metalllegierung sind ein oder mehrere Stoffe, ausgewählt aus der Gruppe Nickel, Aluminium, Titan. The mixtures used according to the invention contain one or more first metals and / or metal alloys. Preferably, the mixture contains metals / metal alloys, which are the dispersion of the CNTs in a molten metal improve. Suitable as the first metal or metal alloy are one or more substances selected from the group nickel, aluminum, titanium.
Die Mischungen können 0, 1 - 10 Gewichtsprozent, bevorzugt 2 - 6 Gewichtsprozent (bezogen auf die Gesamtmenge der Mischung) CNTs enthalten. The mixtures may contain 0, 1 - 10 weight percent, preferably 2 - 6 weight percent (based on the total amount of the mixture) of CNTs.
Bevorzugt wird die Mischung der CNTs und der ersten Metalle oder Metalllegierungen durch einen gemeinsamen Mahlvorgang hergestellt. Hierzu eignen sich insbesondere Kugelmühlen. Um eine Zerstörung der CNT im Mahlprozess zu vermeiden, empfiehlt sich die Mahlzeit in einer Kugelmühle auf maximal 0,5 Stunden bei einer Umdrehungsgeschwindigkeit von maximal 200 rpm (Umdrehungen pro Minute) einzustellen. Bevorzugt wird der Mahlprozess so durchgeführt, dass die Mischung nach dem Mahlvorgang eine mittlere Partikelgröße d50 mehr als 75 Mikrometer, bevorzugt größer 100 Mikrometer beträgt. Wird der Mahl- bzw. Mischvorgang bis zu einer Pulverpartikelgröße von d5o < 75 Mikrometer durchgeführt, kann dies zur Zerstörung der CNTs führen. Preferably, the mixture of the CNTs and the first metals or metal alloys is produced by a common grinding process. Ball mills are particularly suitable for this purpose. To avoid destroying the CNT in the grinding process, it is recommended to set the meal in a ball mill for a maximum of 0.5 hours at a maximum speed of 200 rpm (revolutions per minute). Preferably, the milling process is carried out so that the mixture after the grinding process has a mean particle size d 50 more than 75 microns, preferably greater than 100 microns. If the grinding or mixing process is carried out to a powder particle size of d 5 o <75 microns, this can lead to the destruction of the CNTs.
Im folgenden Verfahrensschritt wird die erhaltene Mischung bei erhöhter Temperatur gesintert, gepresst oder stranggepresst. Es hat sich als vorteilhaft erwiesen, die Mischung vor diesem Verarbeitungsschritt in Tablettenform zu pressen, da insbesondere gesinterte Tabletten im Folgenden leichter zu handhaben sind. In the following process step, the resulting mixture is sintered, pressed or extruded at elevated temperature. It has proven to be advantageous to press the mixture in tablet form before this processing step, since in particular sintered tablets are easier to handle in the following.
Die darauf aufbereiteten, insbesondere gesinterten CNT/Metallgemische werden im nächsten Verfahrensschritt in der Schmelze mindestens eines zweiten Metalls und/oder einer zweiten Metalllegierung dispergiert. The processed, in particular sintered CNT / metal mixtures are dispersed in the next process step in the melt of at least one second metal and / or a second metal alloy.
Die jeweils ersten und zweiten Metalle und/oder Metalllegierungen können gleich oder unterschiedlich sein. Als zweites Metall oder Metalllegierung können auch eine oder mehrere Stoffe, ausgewählt aus der Gruppe Aluminiumknetlegierungen und - gusslegierungen, verwendet werden. Zur Verbesserung der Dispergierung empfiehlt es sich, die Schmelze mit einem Rührwerk (Impeller) zu durchmischen. The respective first and second metals and / or metal alloys may be the same or different. As the second metal or metal alloy, it is also possible to use one or more substances selected from the group of aluminum alloys and cast alloys. To improve the dispersion, it is recommended to mix the melt with an agitator (impeller).
Nach Abkühlung der zunächst schmelzförmigen Dispersion der CNTs in den Metallen können die so erhaltenen Verbundwerkstoffe durch alle bekannten pulver- und schmelzmetallurgischen Verfahren wie Extrusionsverfahren, Thixoforming, Gießverfahren, Druckguss oder Schwerkraftguss und durch Formgebungsverfahren, z.B. durch Umformen, Schmieden, Stranggießen oder Strangpressen, weiterverarbeitet werden. Die erfindungsgemäß hergestellten Verbundwerkstoffe weisen eine erhöhte Grundfestigkeit unter Beibehaltung des ursprünglichen Dehnungsverhalten und des Elastizitätsmoduls auf und sind besonders zur Herstellung von thermisch belasteten Bauteilen wie z.B. Kolben in Verbrennungsmotoren geeignet. Als Matrixmaterial für die Sintertabletten wurden zunächst folgende Pulvermischungen (Partikelgröße < 45 μιτι) verwendet: After cooling the initially melted dispersion of the CNTs in the metals, the resulting composites may be made by any known powder and melt metallurgy processes such as extrusion, thixoforming, casting, die casting or gravity casting and by molding techniques, e.g. by forming, forging, continuous casting or extrusion. The composite materials produced according to the invention have an increased basic strength while retaining the original elongation behavior and the modulus of elasticity and are particularly suitable for the production of thermally stressed components, such as e.g. Piston suitable in internal combustion engines. The following powder mixtures (particle size <45 μm) were initially used as matrix material for the sintered tablets:
AI +10 wt% Ti6AI4V Al +10 wt% Ti 6 Al 4 V
AI + 10 wt% Ni Al + 10 wt% Ni
Diese Pulver wurden mit 4 wt% CNT in einer Kugelmühle bei einer Mahlzeit von 2 h vermischt, anschließend in einer Heißpresse zu Tabletten gesintert und jeweils in etwa 9 kg Aluminiumschmelze (AISigMgMn) gegeben. Nach der Zugabe lösten sich die Tabletten mit 10 wt% Ti6AI4V deutlich besser auf (siehe Fig.1 ) wie die Tabletten mit 10 wt% Nickel. These powders were mixed with 4 wt% CNT in a ball mill at a meal of 2 hours, then sintered into tablets in a hot press and each added to about 9 kg of aluminum melt (AISigMgMn). After the addition, the tablets dissolved significantly better with 10 wt% Ti 6 Al 4 V (see FIG. 1), as did the tablets containing 10 wt% nickel.
Parallel zu den Schmelzversuchen wurden Pulveranalysen durchgeführt, welche Aufschluss über die CNT-Verteilung in der Tablette geben sollten. Hierbei konnten keine CNTs in dem Pulver nachgewiesen werden. Diese werden wahrscheinlich im Mahlprozess zerstört. Nachdem bei einer Pulverpartikelgröße von < 75 μιη bei den gleiche Mahlparametern CNTs nachgewiesen wurde, erscheint die Partikelgröße als ein sehr ernstzunehmender Parameter, der bei künftigen Versuchen mehr Beachtung finden muss. In parallel with the melting tests, powder analyzes were carried out, which should give information about the CNT distribution in the tablet. No CNTs could be detected in the powder. These will probably be in the Grinding process destroyed. After CNTs have been detected at a powder particle size of <75 μm under the same grinding parameters, the particle size appears to be a very serious parameter which must receive more attention in future experiments.
Um folglich eine Zerstörung der CNTs im Mahlprozess zu vermeiden, wurde die Mahlzeit neu ermittelt und auf 0,5 h (bei einer Umdrehungsgeschwindigkeit von 200 rpm) festgelegt. Mit diesen Parametern wurden anschließend Tabletten aus reinem Aluminium mit 4 wt% und Ti6AI4V mit 4 wt% CNTs hergestellt. Im Schmelzversuch zeigte sich bei den Tabletten aus reinem Aluminium ein sehr eingeschränktes Aufschmelzen. Es bildete sich im Schmelztiegel ein Sumpf, der weich war, jedoch noch weitestgehend die Form der Tabletten besaß. Wahrscheinlich schmolz das Aluminium auf, das CNT- Netzwerk der Tablette konnte jedoch nicht aufgelöst werden, (siehe Fig. 2 und 3). Consequently, to avoid destroying the CNTs in the grinding process, the meal was redetermined and set at 0.5 h (at a rotational speed of 200 rpm). Using these parameters, tablets of pure aluminum with 4 wt% and Ti 6 Al 4 V with 4 wt% CNTs were subsequently produced. In the melt test, the tablets of pure aluminum showed a very limited melting. It formed in the crucible a swamp that was soft, but still largely had the shape of the tablets. The aluminum probably melted, but the CNT network of the tablet could not be dissolved (see Figures 2 and 3).
Die Tabletten aus Ti6AI4V schmolzen in der Schmelze nicht auf, und bildeten eine harte Schlacke. Nach dem Abgießen lagen diese unverändert vor. In einer Analyse der Schmelztabletten konnten keine CNTs nachgewiesen werden. Da vor dem Sinterprozess CNTs anwesend waren, werden somit beim Sintern von Titan die CNTs zerstört bzw. es bildet sich Titancarbid, was das schlechte Aufschmelzen erklärt (siehe Fig.4). The tablets of Ti 6 Al 4 V did not melt in the melt, forming a hard slag. After pouring, these were unchanged. In an analysis of the orodispersible tablets no CNTs could be detected. Since CNTs were present before the sintering process, the CNTs are thus destroyed or titanium carbide is formed during the sintering of titanium, which explains the poor melting (see FIG. 4).
Claims
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP10743030A EP2491154A1 (en) | 2009-10-19 | 2010-08-04 | COMPOSITE MATERIALS CONSISTING OF METALS IN WHICH CARBON NANOTUBES (CNTs) ARE DISPERSED |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102009049963.6 | 2009-10-19 | ||
| DE102009049963 | 2009-10-19 |
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| WO2011047743A1 true WO2011047743A1 (en) | 2011-04-28 |
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| WO (1) | WO2011047743A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372209A (en) * | 2014-10-28 | 2015-02-25 | 苏州莱特复合材料有限公司 | Aluminum-base powder-metallurgy composite material and preparation method thereof |
| CN104789805A (en) * | 2014-11-27 | 2015-07-22 | 北京工业大学 | Preparation method of carbon nanotube enhanced metal-matrix composite material |
| CN105734322A (en) * | 2016-03-02 | 2016-07-06 | 昆明理工大学 | Preparation method of carbon nanotube strengthened aluminum-based composite material |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107988507B (en) * | 2017-12-10 | 2020-05-08 | 北京工业大学 | Preparation method of metal-based composite material with high carbon nanotube content |
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| EP1696046A1 (en) * | 2003-12-18 | 2006-08-30 | Shimane Prefectual Government | Metal base carbon fiber composite material and process for producing the same |
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-
2010
- 2010-08-04 EP EP10743030A patent/EP2491154A1/en not_active Withdrawn
- 2010-08-04 WO PCT/EP2010/004781 patent/WO2011047743A1/en not_active Ceased
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| EP1696046A1 (en) * | 2003-12-18 | 2006-08-30 | Shimane Prefectual Government | Metal base carbon fiber composite material and process for producing the same |
| WO2008052642A1 (en) * | 2006-10-31 | 2008-05-08 | Alcan Technology & Management Ltd. | Materials containing carbon nanotubes, process for producing them and use of the materials |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104372209A (en) * | 2014-10-28 | 2015-02-25 | 苏州莱特复合材料有限公司 | Aluminum-base powder-metallurgy composite material and preparation method thereof |
| CN104789805A (en) * | 2014-11-27 | 2015-07-22 | 北京工业大学 | Preparation method of carbon nanotube enhanced metal-matrix composite material |
| CN105734322A (en) * | 2016-03-02 | 2016-07-06 | 昆明理工大学 | Preparation method of carbon nanotube strengthened aluminum-based composite material |
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| EP2491154A1 (en) | 2012-08-29 |
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