Fluorescent single walled nanotube/silica composite materials
View Patent ↗Fluorescent composites of surfactant-wrapped single-walled carbon nanotubes (SWNTs) were prepared by exposing suspensions of surfactant-wrapped carbon nanotubes to tetramethylorthosilicate (TMOS) vapor. Sodium deoxycholate (DOC) and sodium dodecylsulphate (SDS) were the surfactants. No loss in emission intensity was observed when the suspension of DOC-wrapped SWNTs were exposed to the TMOS vapors, but about a 50% decrease in the emission signal was observed from the SDS-wrapped SWNTs nanotubes. The decrease in emission was minimal by buffering the SDS/SWNT suspension prior to forming the composite. Fluorescent xerogels were prepared by adding glycerol to the SWNT suspensions prior to TMOS vapor exposure, followed by drying the gels. Fluorescent aerogels were prepared by replacing water in the gels with methanol and then exposing them to supercritical fluid drying conditions. The aerogels can be used for gas sensing.
1. A process for preparing a fluorescent composite of single-walled carbon nanotubes wrapped in surfactant in a silica gel matrix, comprising:
preparing an aqueous suspension of single-walled carbon nanotubes in an aqueous solvent with surfactant, and
exposing the aqueous suspension to vapor of tetramethylorthosilicate, whereby a rigid fluorescent composite of single-walled carbon nanotubes in a silica gel matrix is formed.
2. The process of claim 1 , wherein the surfactant comprises deoxycholate or dodecylsulphate.
3. The process of claim 1 , wherein the aqueous suspension comprises a polyalcohol.
4. The process of claim 3 , wherein the polyalcohol comprises glycerol.
5. The process of claim 1 , wherein the aqueous suspension comprises a buffer.
6. The process of claim 5 , wherein the buffer comprises phosphate and the pH of the aqueous suspension is approximately 7.00.
7. The process of claim 1 , wherein the carbon nanotubes are prepared by decomposition of carbon monoxide.
8. A process for preparing a fluorescent composite of single-walled carbon nanotubes in a silica gel matrix, comprising:
preparing a buffered aqueous suspension of single-walled carbon nanotubes with a dodecylsulphate surfactant and a buffer, and
exposing the aqueous suspension to vapor of tetramethylorthosilicate, whereby a rigid composite of single-walled carbon nanotubes wrapped in dodecylsulphate in a silica gel matrix is formed.
9. The process of claim 8 , wherein the buffered suspension comprises phosphate.
10. A process for preparing a fluorescent xerogel of single-walled carbon nanotubes and silica, comprising:
preparing a suspension of single-walled carbon nanotubes in an aqueous solvent with glycerol and a surfactant,
exposing the aqueous suspension to vapor of tetramethylorthosilicate whereby the tetramethylorthosilicate hydrolyzes to form a fluorescent composite, and
drying the fluorescent composite to form a xerogel of carbon nanotubes and silica.
11. The process of claim 10 , wherein the surfactant is selected from sodium deoxycholate and sodium dodecylsulphate.
12. A process for preparing a fluorescent aerogel of carbon nanotubes and silica, comprising:
preparing an aqueous suspension of single-walled carbon nanotubes and a surfactant;
exposing the aqueous suspension to tetramethylorthosilicate and a base to form a first gel,
exposing the first gel to methanol which replaces water in the first gel to form a second gel, and
drying the gel with supercritical fluid to form an aerogel of single-walled carbon nanotubes and silica.
13. The process of claim 12 , wherein the surfactant is selected from sodium dodecylsulphate or sodium deoxycholate.
14. The process of claim 13 , wherein the aqueous suspension of single-walled carbon nanotubes further comprises glycerol.
15. The process of claim 12 , wherein the supercritical fluid comprises methanol, ethanol, or carbon dioxide.
16. A process for preparing a fluorescent aerogel of carbon nanotubes and silica, comprising:
preparing an aqueous suspension of single-walled carbon nanotubes and a surfactant;
exposing the aqueous suspension to tetramethylorthosilicate vapor to form a first gel,
exposing the first gel to methanol which replaces water in the first gel to form a second gel, and
drying the second gel with supercritical fluid to form an aerogel of single-walled carbon nanotubes and silica.
17. The process of claim 16 , wherein the surfactant is selected from sodium dodecylsulphate or sodium deoxycholate.
18. The process of claim 16 , wherein the aqueous suspension of single-walled carbon nanotubes further comprises glycerol.
19. A process for sensing a gas, comprising
preparing an aqueous suspension of single-walled carbon nanotubes and a surfactant;
exposing the aqueous suspension to tetramethylorthosilicate vapor to form a first gel,
exposing the first gel to methanol which replaces water in the first gel to form a second gel, and
drying the second gel with a supercritical fluid to form an aerogel of single-walled carbon nanotubes and silica,
measuring the fluorescence from the single-walled carbon nanotubes in the aerogel in a first dielectric medium comprising a vacuum,
changing the first dielectric medium to a second dielectric medium comprising a gas, and thereafter
measuring the fluorescence from the single walled carbon nanotubes in a second dielectric medium, and then
comparing the fluorescence from the aerogel in a vacuum with the fluorescence from the aerogel in a gas.
20. The process of claim 19 , wherein the first dielectric medium comprises a vacuum.
21. The process of claim 19 , wherein the second dielectric medium comprises air.
22. The process of claim 19 , wherein the second dielectric medium comprises carbon dioxide.
23. A process for sensing a gas, comprising
preparing an aqueous suspension of single-walled carbon nanotubes and a surfactant,
exposing the aqueous suspension to tetramethylorthosilicate and a base to form a first gel,
exposing the first gel to methanol which replaces water in the first gel to form a second gel, and
drying the second gel with a supercritical fluid to form an aerogel of single-walled carbon nanotubes and silica,
measuring the fluorescence from the single-walled carbon nanotubes in the aerogel in a first dielectric medium comprising a vacuum,
changing the first dielectric medium to a second dielectric medium comprising a gas, and thereafter
measuring the fluorescence from the single walled carbon nanotubes in a second dielectric medium, and then
comparing the fluorescence from the aerogel in a vacuum with the fluorescence from the aerogel in a gas.
24. The process of claim 23 , wherein the first dielectric medium comprises a vacuum.
25. The process of claim 23 , wherein the second dielectric medium comprises air.
26. The process of claim 23 , wherein the second dielectric medium comprises carbon dioxide.