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Nanotube Polymer Composite Composition and Methods of Making

a composite composition and nanotube technology, applied in the field of nanotube polymer composite composition and, can solve the problems of increasing the cost of nanocomposite, difficulty in dispersing nanotubes, and hampered achievement of the full potential of single-wall carbon nanotube properties in polymers, and achieve the effect of less particles and less expensiv

Inactive Publication Date: 2010-10-21
ENTEGRIS INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0014]In some embodiments of the invention, molding the composition comprising the nanotubes dispersed in the polymer provides an article that is electrically dissipative. The conductivity, surface resistivity, or volume resistivity of the article can be modified by extensional flow. In other embodiments of the invention, molding the composition comprising the nanotubes dispersed in the polymer provides an article that is flame retardant and or can maintain its shape and prevent dripping of polymer. In still other embodiments of the invention, molding the composition comprising the nanotubes dispersed in the polymer provides an article that is electrically dissipative and flame retardant.
[0030]Advantageously SWNT are stronger than carbon particles, for applications where reduction or elimination of particle shedding is important, the use of SWNT would provide less particles. SWNTs are cleaner than carbon powders. Because lower nanotube loading can be utilized to achieve the flame retardant or electrically dissipative properties and a continuous process can used to prepare the polymer / SWNT dispersion in embodiments of the invention, composites and articles made from them in embodiments of the present invention can be less expensive per pound compared to multiwall nanotube polymer composites.

Problems solved by technology

However, achieving the full potential of the properties of single-wall carbon nanotubes in polymers has been hampered by the difficulty of dispersing the nanotubes.
These treatments add impurities and additional steps to the process which increase the costs of the nanocomposite.
The additional dispersal, casting, and solvent removal steps to enhance the affinity between the nanotubes and the polymer at the interface add time, generate waste, and increase the cost of such nanocomposite.
797-802 state that the literature discloses that solution casting methods have limited applicability for producing highly conductive films because SWNT composites tend to saturate at 1-2% nanotube content as the excess nanotubes aggregate.
This limits the compositions that can be formed by this method.
: 20050029498 discloses that highly pure SWNT cannot be separated from the ropes as easily as less pure SWNT and that the shear forces developed during the extrusion process are not as effective at breaking up the aggregates of SWNTs formed by highly pure SWNTs.
Pitch is an unacceptable material for many high purity applications and those requiring high wear resistance.
They also reported that SWNTs appeared to be more difficult to disperse than MWNTs and that complete dispersion of SWNTs was not achieved at the processing times studied.

Method used

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  • Nanotube Polymer Composite Composition and Methods of Making
  • Nanotube Polymer Composite Composition and Methods of Making
  • Nanotube Polymer Composite Composition and Methods of Making

Examples

Experimental program
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Effect test

example 2

[0136]Single walled nanotubes (SWNTs) from supplier CNI (Carbon Nanotechnologies Inc, Houston Tex.) were used without sonication.

[0137]The resistivity of an extruded sample prepared as in Example 1 was measured and was 105 to about 106 ohm / sq. The extruded sample output was fed back into the extruder for 5, 10, 15, 20 additional extrusion cycles as illustrated in FIG. 11A. A sample of extruded material was taken after 5th 10th, 15th and 20th cycles and the resistivity and G′ of the sample measured. There was essentially no increase in the measured storage modulus illustrating that the dispersion of the SWNTs in the polymer was stable and essentially invariant and that the properties did not change over time within the variation of the processing conditions. This result illustrates that the extrusion compounded composition is insensitive to shear history.

[0138]The properties of a molded article of this extrusion compounded nanotube and polymer composition could be modified by the she...

example 3

[0139]Single walled nanotubes (SWNTs) from supplier CNI (Carbon Nanotechnologies Inc, Houston Tex.) were used without sonication and combined with PEEK thermoplastic as in Example 1 by injection molding. The extractables of the composite were determined by ICP-MS on acid digested samples as shown in the Table 2 below.

[0140]The extractables can be determined via Microwave Digestion and filtration. For example, weigh 1.0 gram polymer and SWNT composite sample pellets and place pellets in 125-ml PFA sample digestion vessel. Add 10 ml 16.0 N HNO3, cap and seal vessel(s). Place vessel(s) in insulated sleeves and into sample vessel carousel. Place in microwave digestion oven which can be heated according to the Oven profile: (Stage 1) Heat at 50% power to 20 p.s.i. and hold 10 minutes. (Stage 2) Heat at 50% power to 50 p.s.i and hold 10 minutes. (Stage 3) Heat at 50% power to 90 p.s.i. and hold 10 minutes. (Stage 4) Heat at 50% power to 100 p.s.i. and hold 10 minutes. (Stage 5) Heat at 50...

example 4

[0141]Single walled nanotubes (SWNTs) from supplier CNI (Carbon Nanotechnologies Inc, Houston Tex.) were used without sonication and combined with PEEK thermoplastic as in Example 1.

[0142]Squeeze flow or Gap testing was performed on a melt of the sample using an Advance Rheometric Expansion System (ARES) Rheometer at 380° C. in a nitrogen atmosphere. FIG. 6 illustrates force gap test results on a melt of the samples heated to 380° C. FIG. 6 illustrates the squeeze flow rheometry for SWNT dispersion on the properties of the materials prepared. NT4 is prepared by the dry melt method, NT1 is side stuff method. FIG. 6 illustrates the behavior of NT1 and NT4 under constant normal force and an initial gap of about 4 mm. A sample of the material was placed between the plates and heated above the melting or glass transition temperature, for example to 380° C. The initial behavior (to about 75 sec) may be due to the sample filling the void between the plates, the void between the plates is e...

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Abstract

Embodiments of the invention include compositions comprising a polymer an amount of nanotubes extrusion compounded together. The amount of the nanotubes dispersed in the polymer forms a composition with a storage modulus G′ that does not increase further extrusion compounding of the composition. Extrusion compounded compositions of conductive nanotubes and polymer can be molded into electrically dissipative articles whose resistivity decreases with decreasing shear flow in the molding process.

Description

CROSS REFERENCE TO RELATED APPLICATIONS[0001]This application claims the benefit of to U.S. Provisional Patent Application No. 60 / 775,569, filed on Feb. 22, 2006 which is incorporated herein by reference in its entirety.BACKGROUND[0002]Nanocomposites are compositions in which a continuous phase has dispersed or distributed in it at least one additional constituent such as particles, rods, or tubes where the additional constituent has one or more dimensions, such as length, width or thickness, in the nanometer or molecular size range. In order to effectively improve the physical or mechanical properties of the composite it is important to disperse these additional constituents throughout the polymer in order to promote more interfaces and enhance the affinity between the additional constituents and polymer. If the added constituent is uniformly dispersed throughout the polymer, less material may be added to the nanocomposite composition without adversely affecting the physical proper...

Claims

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Application Information

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IPC IPC(8): C08K3/04
CPCB82Y30/00C08J5/005C08J2371/10C08J2379/08B29C47/0021Y10T428/1372B29C47/1018B29C45/0013H01L21/67336H01B13/0036B29C47/0071B29C48/08B29C48/14B29C48/287C08K3/041C08K7/00C08K2201/011
Inventor BHATT, SANJIV M.
Owner ENTEGRIS INC
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