US20060235136A1 - Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same - Google Patents
Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same Download PDFInfo
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- US20060235136A1 US20060235136A1 US11/417,286 US41728606A US2006235136A1 US 20060235136 A1 US20060235136 A1 US 20060235136A1 US 41728606 A US41728606 A US 41728606A US 2006235136 A1 US2006235136 A1 US 2006235136A1
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- nanocomposite structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Definitions
- This invention relates to material structures that are mechanically strong. More specifically, the invention relates to nanocomposite structures that are mechanically strong, thermally stable, and electrically conductive, as well as a method of fabricating same.
- the state-of-the-art in lightweight and mechanically strong structures is centered around graphite fiber composites. While graphite fibers have excellent mechanical properties, they do not have the desired thermal or electrical conductivities. Accordingly, when graphite fiber composites are to be used in high temperature environments, specialized high temperature or thermally conductive coatings are applied to the structure. When graphite fiber composite structures and/or their surrounding environment must be monitored, sensors and their associated wiring must be attached to or embedded in the structure. These extra coatings, sensors and/or wiring add weight and cost to the ultimate structure.
- Another object of the present invention is to provide a method of fabricating a high-strength structure that is stable in high temperature environments and has electrical conductivity characteristics.
- a nanocomposite structure and method of fabricating same are provided.
- the nanocomposite structure is a polymer in an extruded shape with a plurality of carbon nanotubes (CNTs) longitudinally disposed and dispersed in the extruded shape along a dimension thereof.
- the polymer is characteristically defined as having a viscosity of at least approximately 100,000 poise at a temperature of 200° C.
- the CNTs are mixed with the polymer at a temperature of at least 200° C. to form a viscous mixture.
- An inert gas is passed through the viscous mixture to purge oxygen therefrom during mixing.
- the viscous mixture is cooled to form a solid form of the viscous mixture that is then broken into pieces not to exceed approximately 0.125 inches in diameter.
- the pieces are converted into an extruded shape to thereby align the CNTs longitudinally along a dimension of the extruded shape.
- FIG. 1 is a schematic view of the method used to fabricate a nanocomposite structure in accordance with the present invention
- FIG. 2 is a perspective view of an extruded-fiber nanocomposite structure fabricated in accordance with the present invention.
- FIG. 3 is a perspective view of an extruded-ribbon nanocomposite structure fabricated in accordance with the present invention.
- FIG. 1 a schematic view of the nanocomposite structure fabrication process of the present invention is shown. It is to be understood at the outset that the fabrication process steps can be carried out using a variety of different equipment/apparatus without departing from the scope of the present invention.
- the raw materials consist of a polymer 10 and carbon nanotubes (CNTs) 12 .
- CNTs carbon nanotubes
- One of the goals of the present invention is to produce a mechanically strong nanocomposite structure that is stable at relatively high temperatures (e.g., on the order of 150° C. or greater).
- polymer 10 must be selected from a class of thermally-stable polymer materials.
- the characteristics of polymer 10 are defined as a polymer material having a viscosity of at least approximately 100,000 poise at a temperature of approximately 200° C.
- the second raw materials used in the nanocomposite structure and process of the present invention are CNTs 12 .
- CNTs are single or multi-wall graphene cylinders.
- Single-wall CNTs or SWCNTs typically have diameters on the order of nanometers with lengths of several microns.
- the SWCNTs used to fabricate the present invention's nanocomposite structure are defined by a length-to-diameter aspect ratio of 100 or more.
- Multi-wall CNTs can have two, a few or many walls, thereby increasing their overall diameters.
- CNT-type is not a limitation of the present invention although it was found that the weight/volume percent of CNTs required was lower for SWCNTs (approximately 1% or less) than for multi-wall CNTs (approximately 5% or less).
- melt mixing operation 100 that utilizes a conventional melt mixer apparatus (not shown) well known in the art.
- operation 100 melts polymer 10 while mixing CNTs 12 therein such that a viscous mixture is generated.
- a pressurized purge gas is pumped through the viscous mixture in order to displace oxygen from the mixture.
- the purge gas should be an inert gas such as nitrogen, argon or helium.
- melt mixing operation 100 produces a viscous mixture that is then cooled to a solid mixture by a cooling operation 102 .
- Such cooling can be achieved in an active or passive fashion without departing from the scope of the present invention.
- the resulting solid mixture is next provided to a sizing operation 104 .
- Sizing operation 104 reduces the above-described solid mixture to pieces small enough to undergo an extrusion operation.
- state-of-the-art extruders require the pieces to be no larger than approximately 0.125 inches in diameter. Accordingly, sizing operation 104 can be accomplished by any of a variety of pelletizing or pulverizing (e.g., ground, crushed or otherwise reduced in size) operations/apparatus.
- the reduced-size pieces of the solid mixture are stored in a tank or hopper 16 .
- Pressurized purge gas 18 e.g., nitrogen, argon, helium, etc.
- pressurized purge gas 18 is flowed through the reduced-size pieces in hopper 16 in order to displace oxygen from the spaces between the pieces. In this way, the pieces supplied to a temperature-controlled extrusion operation 106 have little or no oxygen accompanying them during extrusion.
- Temperature-controlled extrusion operation 106 is any process/apparatus capable of generating an extrudate while controlling the temperature of the materials being extruded.
- One such extruder is disclosed by D. C. Working et al. in “Microextruder for Polymer Characterization,” SAMPE Technical Conference, 1994, 26:700.
- Temperature used in extrusion operation 106 should be sufficient to melt the polymer portion of the pieces (i.e., the CNTs do not melt) of the solid mixture.
- Extrusion operation 106 generates shear forces such that the CNTs in the molten portion of the pieces tend to align themselves longitudinally in the direction that the material is being drawn by operation 106 .
- operation 106 produces a nanocomposite structure having an extruded shape 20 that has CNTs longitudinally aligned along the drawn dimension of shape 20 .
- Extrusion operation 106 can be used to generate a variety of geometrically-shaped extrudates depending on the extrusion die. Two such typical shapes of a nanocomposite structure are illustrated in FIGS. 2 and 3 . More specifically, the process of the present invention can be used to produce a fiber-shaped nanocomposite structure 20 A ( FIG. 2 ) or a ribbon-shaped nanocomposite structure 20 B ( FIG. 3 ). In either case, each nanocomposite structure has CNTs 12 longitudinally disposed and dispersed within the surrounding polymer 10 where CNTs 12 are longitudinally aligned along a dimension (e.g., the length) of the structure.
- a dimension e.g., the length
- nanocomposite fibers were made in accordance with the above-described process and tested.
- the examples were made using the polyimide ULTEM (available from General Electric) and SWCNTs.
- the example formulations along with their mechanical properties are summarized below where the ULTEM polyimide properties are also shown for comparison. Additional discussion is provided by E. J. Siochi et al. in “Melt Processing of SWCNT-polyimide nanocomposite fibers,” Composites. Part B: Engineering, 35(5): 439, 2004, incorporated herein by reference in its entirety.
- the tensile modulus and yield strength improved significantly with very small amounts of SWCNT inclusions.
- the resulting nanocomposite will have good thermal characteristics owing to the properties of the base polymers.
- the longitudinal alignment of the CNTs (which was confirmed spectroscopically using Raman spectroscopy and visually via High Resolution Scanning Electron Microscopy (HRSEM)) should provide a degree of electrical conductivity.
- HRSEM High Resolution Scanning Electron Microscopy
Abstract
Description
- This invention was made in part by employees of the United States Government and may be manufactured and used by or for the Government of the United States of America for governmental purposes without the payment of any royalties thereon or therefor.
- Pursuant to 35 U.S.C. §119, the benefit of priority from provisional application 60/673,394, with a filing date of Apr. 18, 2005, is claimed for this non-provisional application.
- 1. Field of the Invention
- This invention relates to material structures that are mechanically strong. More specifically, the invention relates to nanocomposite structures that are mechanically strong, thermally stable, and electrically conductive, as well as a method of fabricating same.
- 2. Description of the Related Art
- The state-of-the-art in lightweight and mechanically strong structures is centered around graphite fiber composites. While graphite fibers have excellent mechanical properties, they do not have the desired thermal or electrical conductivities. Accordingly, when graphite fiber composites are to be used in high temperature environments, specialized high temperature or thermally conductive coatings are applied to the structure. When graphite fiber composite structures and/or their surrounding environment must be monitored, sensors and their associated wiring must be attached to or embedded in the structure. These extra coatings, sensors and/or wiring add weight and cost to the ultimate structure.
- Accordingly, it is an object of the present invention to provide a high-strength structure that is stable in high temperature environments and that has electrical conductivity characteristics.
- Another object of the present invention is to provide a method of fabricating a high-strength structure that is stable in high temperature environments and has electrical conductivity characteristics.
- Other objects and advantages of the present invention will become more obvious hereinafter in the specification and drawings.
- In accordance with the present invention, a nanocomposite structure and method of fabricating same are provided. The nanocomposite structure is a polymer in an extruded shape with a plurality of carbon nanotubes (CNTs) longitudinally disposed and dispersed in the extruded shape along a dimension thereof. The polymer is characteristically defined as having a viscosity of at least approximately 100,000 poise at a temperature of 200° C.
- In the fabrication method, the CNTs are mixed with the polymer at a temperature of at least 200° C. to form a viscous mixture. An inert gas is passed through the viscous mixture to purge oxygen therefrom during mixing. The viscous mixture is cooled to form a solid form of the viscous mixture that is then broken into pieces not to exceed approximately 0.125 inches in diameter. The pieces are converted into an extruded shape to thereby align the CNTs longitudinally along a dimension of the extruded shape.
-
FIG. 1 is a schematic view of the method used to fabricate a nanocomposite structure in accordance with the present invention; -
FIG. 2 is a perspective view of an extruded-fiber nanocomposite structure fabricated in accordance with the present invention; and -
FIG. 3 is a perspective view of an extruded-ribbon nanocomposite structure fabricated in accordance with the present invention. - Referring now to the drawings, and more particularly to
FIG. 1 , a schematic view of the nanocomposite structure fabrication process of the present invention is shown. It is to be understood at the outset that the fabrication process steps can be carried out using a variety of different equipment/apparatus without departing from the scope of the present invention. - Before describing the nanocomposite structure fabrication process, the two raw materials operated on thereby will first be described. In general, the raw materials consist of a
polymer 10 and carbon nanotubes (CNTs) 12. One of the goals of the present invention is to produce a mechanically strong nanocomposite structure that is stable at relatively high temperatures (e.g., on the order of 150° C. or greater). To achieve this,polymer 10 must be selected from a class of thermally-stable polymer materials. For purpose of the present invention, the characteristics ofpolymer 10 are defined as a polymer material having a viscosity of at least approximately 100,000 poise at a temperature of approximately 200° C. While these types of polymers provide a high degree of thermal stability, they are also extremely difficult to process where processing requires the melting thereof. That is, while these polymers require high processing temperatures, material degradation generally occurs at temperatures that are not that much greater than the melt processing temperature. Accordingly, these materials generally present small windows of effective processing temperatures. However, as will be explained further below, the process of the present invention improves the processability of these polymers. - The second raw materials used in the nanocomposite structure and process of the present invention are
CNTs 12. As is well known in the art, CNTs are single or multi-wall graphene cylinders. Single-wall CNTs (or SWCNTs) typically have diameters on the order of nanometers with lengths of several microns. In general, the SWCNTs used to fabricate the present invention's nanocomposite structure are defined by a length-to-diameter aspect ratio of 100 or more. Multi-wall CNTs can have two, a few or many walls, thereby increasing their overall diameters. The choice of CNT-type is not a limitation of the present invention although it was found that the weight/volume percent of CNTs required was lower for SWCNTs (approximately 1% or less) than for multi-wall CNTs (approximately 5% or less). - Appropriate quantities of
polymer 10 andCNTs 12 are processed together in amelt mixing operation 100 that utilizes a conventional melt mixer apparatus (not shown) well known in the art. In essence,operation 100 meltspolymer 10 while mixingCNTs 12 therein such that a viscous mixture is generated. Duringmelt mixing operation 100, a pressurized purge gas is pumped through the viscous mixture in order to displace oxygen from the mixture. The purge gas should be an inert gas such as nitrogen, argon or helium. By displacing oxygen from the mixture, degradation ofpolymer 10 during the melting thereof is prevented or, at the very least delayed, thereby allowingmelt mixing operation 100 to continue for a longer period of time than would be possible without the oxygen purge. In this way, good CNT dispersion within the melted polymer is achieved. - As just mentioned,
melt mixing operation 100 produces a viscous mixture that is then cooled to a solid mixture by acooling operation 102. Such cooling can be achieved in an active or passive fashion without departing from the scope of the present invention. The resulting solid mixture is next provided to asizing operation 104. -
Sizing operation 104 reduces the above-described solid mixture to pieces small enough to undergo an extrusion operation. In general, state-of-the-art extruders require the pieces to be no larger than approximately 0.125 inches in diameter. Accordingly,sizing operation 104 can be accomplished by any of a variety of pelletizing or pulverizing (e.g., ground, crushed or otherwise reduced in size) operations/apparatus. - The reduced-size pieces of the solid mixture are stored in a tank or hopper 16. Pressurized purge gas 18 (e.g., nitrogen, argon, helium, etc.) is flowed through the reduced-size pieces in
hopper 16 in order to displace oxygen from the spaces between the pieces. In this way, the pieces supplied to a temperature-controlledextrusion operation 106 have little or no oxygen accompanying them during extrusion. - Temperature-controlled
extrusion operation 106 is any process/apparatus capable of generating an extrudate while controlling the temperature of the materials being extruded. One such extruder is disclosed by D. C. Working et al. in “Microextruder for Polymer Characterization,” SAMPE Technical Conference, 1994, 26:700. Temperature used inextrusion operation 106 should be sufficient to melt the polymer portion of the pieces (i.e., the CNTs do not melt) of the solid mixture.Extrusion operation 106 generates shear forces such that the CNTs in the molten portion of the pieces tend to align themselves longitudinally in the direction that the material is being drawn byoperation 106. As a result,operation 106 produces a nanocomposite structure having an extrudedshape 20 that has CNTs longitudinally aligned along the drawn dimension ofshape 20. -
Extrusion operation 106 can be used to generate a variety of geometrically-shaped extrudates depending on the extrusion die. Two such typical shapes of a nanocomposite structure are illustrated inFIGS. 2 and 3 . More specifically, the process of the present invention can be used to produce a fiber-shapednanocomposite structure 20A (FIG. 2 ) or a ribbon-shapednanocomposite structure 20B (FIG. 3 ). In either case, each nanocomposite structure hasCNTs 12 longitudinally disposed and dispersed within the surroundingpolymer 10 whereCNTs 12 are longitudinally aligned along a dimension (e.g., the length) of the structure. - By way of example, nanocomposite fibers were made in accordance with the above-described process and tested. The examples were made using the polyimide ULTEM (available from General Electric) and SWCNTs. The example formulations along with their mechanical properties are summarized below where the ULTEM polyimide properties are also shown for comparison. Additional discussion is provided by E. J. Siochi et al. in “Melt Processing of SWCNT-polyimide nanocomposite fibers,” Composites. Part B: Engineering, 35(5): 439, 2004, incorporated herein by reference in its entirety.
SWCNT Tensile Mod. Yield Stress (wt %) (GPa) (MPa) 0 2.2 74 0.1 2.6 86 0.3 2.8 94 1.0 3.2 100 - As is clearly evident, the tensile modulus and yield strength improved significantly with very small amounts of SWCNT inclusions. The resulting nanocomposite will have good thermal characteristics owing to the properties of the base polymers. The longitudinal alignment of the CNTs (which was confirmed spectroscopically using Raman spectroscopy and visually via High Resolution Scanning Electron Microscopy (HRSEM)) should provide a degree of electrical conductivity. Thus, the present invention can be used to provide a new class of mechanically strong, thermally stable and electrically conductive nanocomposites.
- Although the invention has been described relative to a specific embodiment thereof, there are numerous variations and modifications that will be readily apparent to those skilled in the art in light of the above teachings. It is therefore to be understood that, within the scope of the appended claims, the invention may be practiced other than as specifically described.
Claims (22)
Priority Applications (2)
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US11/417,286 US20060235136A1 (en) | 2005-04-18 | 2006-04-12 | Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same |
US13/053,633 US8608993B2 (en) | 2005-04-18 | 2011-03-22 | Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same |
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US67339405P | 2005-04-18 | 2005-04-18 | |
US11/417,286 US20060235136A1 (en) | 2005-04-18 | 2006-04-12 | Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same |
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US13/053,633 Expired - Fee Related US8608993B2 (en) | 2005-04-18 | 2011-03-22 | Mechanically strong, thermally stable, and electrically conductive nanocomposite structure and method of fabricating same |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20100269416A1 (en) * | 2009-04-27 | 2010-10-28 | Rohm and Haas Electroinic Materials CMP Holidays, Inc. | Method for manufacturing chemical mechanical polishing pad polishing layers having reduced gas inclusion defects |
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US8608993B2 (en) | 2013-12-17 |
US20110169187A1 (en) | 2011-07-14 |
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