Browsing by Author "Margrave, Mary Lou"
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Item Fabrication of carbon nanotube reinforced epoxy polymer composites using functionalized carbon nanotubes(2009-10-13) Khabashesku, Valery N.; Zhu, Jiang; Peng, Haiqing; Barrera, Enrique V.; Margrave, John L.; Margrave, Mary Lou; Rice University; United States Patent and Trademark OfficeThe present invention is directed to methods of integrating carbon nanotubes into epoxy polymer composites via chemical functionalization of carbon nanotubes, and to the carbon nanotube-epoxy polymer composites produced by such methods. Integration is enhanced through improved dispersion and/or covalent bonding with the epoxy matrix during the curing process. In general, such methods involve the attachment of chemical moieties (i.e., functional groups) to the sidewall and/or end-cap of carbon nanotubes such that the chemical moieties react with either the epoxy precursor(s) or the curing agent(s) (or both) during the curing process. Additionally, in some embodiments, these or additional chemical moieties can function to facilitate dispersion of the carbon nanotubes by decreasing the van der Waals attractive forces between the nanotubes.Item Fiber-reinforced polymer composites containing functionalized carbon nanotubes(2012-05-29) Zhu, Jiang; Khabashesku, Valery N.; Peng, Haiqing; Barrera, Enrique V.; Margrave, John L.; Margrave, Mary Lou; Rice University; United States Patent and Trademark OfficeThe present invention is directed to methods of integrating carbon nanotubes into epoxy polymer composites via chemical functionalization of carbon nanotubes, and to the carbon nanotube-epoxy polymer composites produced by such methods. Integration is enhanced through improved dispersion and/or covalent bonding with the epoxy matrix during the curing process. In general, such methods involve the attachment of chemical moieties (i.e., functional groups) to the sidewall and/or end-cap of carbon nanotubes such that the chemical moieties react with either the epoxy precursor(s) or the curing agent(s) (or both) during the curing process. Additionally, in some embodiments, these or additional chemical moieties can function to facilitate dispersion of the carbon nanotubes by decreasing the van der Waals attractive forces between the nanotubes.Item Functionalization of nanodiamond powder through fluorination and subsequent derivatization reactions(2010-10-26) Khabashesku, Valery N.; Liu, Yu; Margrave, John L.; Margrave, Mary Lou; Rice University; United States Patent and Trademark OfficeThe present invention is directed to functionalized nanoscale diamond powders, methods for making such powders, applications for using such powders, and articles of manufacture comprising such powders. Methods for making such functionalized nanodiamond powders generally comprise a fluorination of nanodiamond powder. In some embodiments, such methods comprise reacting fluorinated nanodiamond powder with a subsequent derivatization agent, such as a strong nucleophile.Item Method for functionalizating carbon naontubes utilizing peroxides(2011-07-12) Khabashesku, Valery N.; Peng, Haiqing; Margrave, John L.; Margrave, Mary Lou; Billups, Edward W.; Ying, Yunming; Rice University; United States Patent and Trademark OfficeA method for functionalizing the wall of single-wall or multi-wall carbon nanotubes involves the use of acyl peroxides to generate carbon-centered free radicals. The method allows for the chemical attachment of a variety of functional groups to the wall or end cap of carbon nanotubes through covalent carbon bonds without destroying the wall or endcap structure of the nanotube. Carbon-centered radicals generated from acyl peroxides can have terminal functional groups that provide sites for further reaction with other compounds. Organic groups with terminal carboxylic acid functionality can be converted to an acyl chloride and further reacted with an amine to form an amide or with a diamine to form an amide with terminal amine. The reactive functional groups attached to the nanotubes provide improved solvent dispersibility and provide reaction sites for monomers for incorporation in polymer structures. The nanotubes can also be functionalized by generating free radicals from organic sulfoxides.Item Method for functionalizing carbon nanotubes utilizing peroxides(2006-10-24) Khabashesku, Valery N.; Peng, Haiqing; Margrave, Mary Lou; Billups, Edward W.; Ying, Yunming; Rice University; United States Patent and Trademark OfficeA method for functionalizing the wall of single-wall or multi-wall carbon nanotubes involves the use of acyl peroxides to generate carbon-centered free radicals. The method allows for the chemical attachment of a variety of functional groups to the wall or end cap of carbon nanotubes through covalent carbon bonds without destroying the wall or endcap structure of the nanotube. Carbon-centered radicals generated from acyl peroxides can have terminal functional groups that provide sites for further reaction with other compounds. Organic groups with terminal carboxylic acid functionality can be converted to an acyl chloride and further reacted with an amine to form an amide or with a diamine to form an amide with terminal amine. The reactive functional groups attached to the nanotubes provide improved solvent dispersibility and provide reaction sites for monomers for incorporation in polymer structures. The nanotubes can also be functionalized by generating free radicals from organic sulfoxides.Item Method for functionalizing carbon nanotubes utilizing peroxides(2010-06-22) Khabashesku, Valery N.; Peng, Haiqing; Margrave, John L.; Margrave, Mary Lou; Billups, Edward W.; Ying, Yunming; Rice University; United States Patent and Trademark OfficeA method for functionalizing the wall of single-wall or multi-wall carbon nanotubes involves the use of acyl peroxides to generate carbon-centered free radicals. The method allows for the chemical attachment of a variety of functional groups to the wall or end cap of carbon nanotubes through covalent carbon bonds without destroying the wall or endcap structure of the nanotube. Carbon-centered radicals generated from acyl peroxides can have terminal functional groups that provide sites for further reaction with other compounds. Organic groups with terminal carboxylic acid functionality can be converted to an acyl chloride and further reacted with an amine to form an amide or with a diamine to form an amide with terminal amine. The reactive functional groups attached to the nanotubes provide improved solvent dispersibility and provide reaction sites for monomers for incorporation in polymer structures. The nanotubes can also be functionalized by generating free radicals from organic sulfoxides.Item Nanotube-amino acids and methods for preparing same(2012-01-10) Khabashesku, Valery N.; Peng, Haiqing; Margrave, John L.; Margrave, Mary Lou; Rice University; United States Patent and Trademark OfficeThe present invention is directed toward compositions comprising carbon nanotubes (CNTs) that are sidewall-functionalized with amino acid groups, and to amino acid compositions comprising carbon nanotubes. The present invention is also directed to simple and relatively inexpensive methods for the preparation of such compositions. Such compositions are expected to greatly extend the bio-medical applications of CNTs.Item Sidewall functionalization of nanotubes with hydroxyl terminated moieties(2009-12-15) Khabashesku, Valery N.; Zhang, Lei; Margrave, John L.; Margrave, Mary Lou; Rice University; United States Patent and Trademark OfficeThe present invention is directed to methods of forming sidewall-functionalized carbon nanotubes, wherein such functionalized carbon nanotubes have hydroxyl-terminated moieties covalently attached to their sidewalls. Generally, such methods involve chemistry on carbon nanotubes that have first been fluorinated. In some embodiments, fluorinated carbon nanotubes (“fluoronanotubes”) are reacted with mono-metal salts of a dialcohol, MO—R—OH, where M is a metal and R is hydrocarbon or other organic chain and/or ring structural unit. In such embodiments, —O—R—OH displaces —F on the nanotube, the fluorine leaving as MF. Generally, such mono-metal salts are formed in situ by the addition of MOH to one or more dialcohols in which the fluoronanotubes have been dispersed. In some embodiments, fluoronanotubes are reacted with amino alcohols, such as being of the type H2N—R—OH, wherein —N(H)—R—OH displaces —F on the nanotube, the fluorine leaving as HF.Item Sidewall functionalization of single-wall carbon nanotubes through C-N bond forming substitutions of fluoronanotubes(2008-11-18) Khabashesku, Valery N.; Margrave, Mary Lou; Stevens, Joel L.; Derrien, Gaelle Armelle; Rice University; United States Patent and Trademark OfficeThe present invention is directed toward a method of sidewall-functionalizing single-walled carbon nanotubes (SWNTs) through C—N bond forming substitution reactions with fluorinated SWNTs (fluoronanotubes), and to the sidewall-functionalized SWNTs comprising C—N bonds between carbons of the SWNT sidewall and nitrogens of the functionalizing groups made by these methods. Furthermore, when diamine species are utilized as reactants, novel materials like crosslinked SWNTs and “nanotube-nylons” can be generated. In some embodiments, SWNTs with functional groups covalently attached to their side walls through C—N bonds are prepared by either the direct interaction of fluoronanotubes with terminal alkylidene diamines or diethanolamine, or by a two-step procedure involving consecutive treatments with Li3N in diglyme and RCl (R=H, n-butyl, benzyl) reagents. Evidence for sidewall attachment of amine-derived groups has been provided by Raman, FTIR, and UV-vis-NIR spectra, SEM/EDAX and TEM data, and thermal degradation studies. The demonstrated new C—N functionalization methods offer a wide range of further SWNT derivatizations, including their covalent binding to aminoacids, DNA, and polymer matrixes.