Reactor and method for synthesizing metal oxide impregnated carbon nanotubes
US-9670103-B1 · Jun 6, 2017 · US
US9834444B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9834444-B2 |
| Application number | US-201715496732-A |
| Country | US |
| Kind code | B2 |
| Filing date | Apr 25, 2017 |
| Priority date | Mar 22, 2016 |
| Publication date | Dec 5, 2017 |
| Grant date | Dec 5, 2017 |
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A vertical chemical vapor deposition (CVD) reactor and a method for synthesizing metal oxide impregnated carbon nanotubes. The CVD reactor includes a preheating zone portion and a reaction zone portion, and preferably an additional cooling zone portion and a product collector. The method includes (a) subjecting a liquid reactant solution comprising an organic solvent, a metallocene, and a metal alkoxide to atomization in the presence of a gas flow comprising a carrier gas and a support gas to form an atomized mixture, and (b) heating the atomized mixture to a temperature of 200° C.-1400° C., wherein the heating forms a metal oxide and at least one carbon source compound, wherein the metallocene catalyzes the formation of carbon nanotubes from the at least one carbon source compound and the metal oxide is incorporated into or on a surface of the carbon nanotubes to form the metal oxide impregnated carbon nanotubes.
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The invention claimed is: 1. A method of synthesizing carbon nanotubes impregnated with aluminum oxide, the method comprising: (a) ultrasonically atomizing a liquid reactant solution in the presence of at least one gas flow comprising at least one carrier gas and at least one support gas, wherein the liquid reactant solution comprises at least one organic solvent, at least one metallocene, and aluminum isopropoxide, to form an atomized mixture comprising droplets of the liquid reactant solution and the at least one gas flow, and (b) heating the atomized mixture to a temperature of 200° C.-1400° C. in a chemical vapor deposition reactor, wherein the heating forms aluminum oxide and at least one carbon source compound, wherein the at least one metallocene catalyzes the formation of carbon nanotubes from the at least one carbon source compound and the aluminum oxide is incorporated into or on a surface of the carbon nanotubes to form the carbon nanotubes impregnated with the aluminum oxide, wherein 1-99 wt % of the aluminum oxide incorporated into or on the surface of the carbon nanotubes is in corundum phase. 2. The method of claim 1 , further comprising collecting the carbon nanotubes impregnated with the aluminum oxide. 3. The method of claim 1 , wherein the at least one carrier gas is at least one selected from the group consisting of He, N 2 , and Ar. 4. The method of claim 1 , wherein the at least one support gas is selected from the group consisting of CO 2 , H 2 O, H 2 and NH 3 . 5. The method of claim 1 , wherein the at least one organic solvent is selected from the group consisting of 2-methoxy ethanol, 2-ethoxy ethanol, 2-methoxy propanol, 2-ethoxy propanol, 2-propoxy propanol, 2-butoxy propanol, 2-butoxy butanol, cyclohexane, heptane, octane, benzene, toluene, ethyl benzene, xylene, cumene, and styrene. 6. The method of claim 1 , wherein the at least one metallocene is selected from the group consisting of a metallocene of Ni, a metallocene of Co, a metallocene of Fe, a metallocene of Cr, a metallocene of Mo, a metallocene of Rh, a metallocene of Ti, a metallocene of W, a metallocene of V, and a metallocene of Zr. 7. The method of claim 1 , wherein the carbon nanotubes are multi-walled carbon nanotubes, and wherein the multi-walled carbon nanotubes impregnated with the aluminum oxide have a BET surface area of 450-2000 m 2 /g.
by producing an aerosol and subsequent evaporation of the droplets or particles · CPC title
Filled nanotubes · CPC title
having atoms interior to the carbon cage · CPC title
Manufacture or treatment of nanostructures · CPC title
Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title
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