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United States Patent (10) Patent No.: US 6, 720,240 B2 Gole Et Al

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United States Patent (10) Patent No.: US 6, 720,240 B2 Gole Et Al I lllll llllllll Ill lllll lllll lllll lllll lllll 111111111111111111111111111111111 US006720240B2 (12) United States Patent (10) Patent No.: US 6, 720,240 B2 Gole et al. (45) Date of Patent: Apr. 13, 2004 (54) SILICON BASED NANOSPHERES AND pp. 4572-4575.* NANO WIRES P.B. MirKarimi et al. , Investigating the growth of localized defects in thin films using gold nanospheres, Applied Phys­ (75) Inventors: James L. Gole, Atlanta, GA (US); ics Letters, vol. 77 No. 14, Oct. 2001 pp. 2343-2245.* John D. Stout, Atlanta, GA (US); P.B. Mirkarimi et al., Quantum Electronics Letters, IEEE Mark G. White, Woodstock, GA (US) Journal Of Quantum Electronics, vol. 37 , No. 12, Dec. 2001.* (73) Assignee: Georgia Tech Research Corporation, Gale, Stout, Rauch, Wang; Direct synthesis of silicon Atlanta, GA (US) nanowires, silica nanospheres, and wire-like nanosphere agglomerates; Applied Physics Letters, vol. 76, No. 17, Apr. ( *) Notice: Subject to any disclaimer, the term of this 24, 2000, pp. 2346-2348. patent is extended or adjusted under 35 Hu, Odom, Lieber; Chemistry and Physics in One Dimen­ U.S.C. 154(b) by 53 days. sion: Synthesis and Properties of N anowires and N anotubes, Acc. Chem. Res. 1999, vol. 32, No. 5, 1999, pp. 435-445. (21) Appl. No.: 09/820,413 Gale, White; Nanocatalysis: Selective Conversion of Etha­ nol to Acetaldehyde Using Monoatomically Dispersed Cop­ (22) Filed: Mar. 29, 2001 per on Silica Nanospheres; Journal of Catalysis, pp. 2-15. (65) Prior Publication Data Crooks, Zhao, Sun, Chechik, Yeung; Dendrimer-Encapsu­ lated Metal Nanoparticles: Synthesis, Characterization, and US 2002/0001977 Al Jan. 3, 2002 Applications to Catalysis; Accounts of Chemical Research, vol. 34, No. 3, Mar. 2001; pp. 181-189. Related U.S. Application Data Kenvin and White; Supported Catalysts Prepared from (60) Provisional application No. 60/192,846, filed on Mar. 29, 2000, and provisional application No. 60/192,844, filed on Mononuclear Copper Complexes: Catalytic Properties; Mar. 29, 2000. Journal of Catalysis; 1992; pp. 81-91. (51) Int. Cl.7 ...................... HOlL 21/20; HOlL 21/4763 Primary Examiner-Wael Fahmy (52) U.S. Cl. ....................... 438/487; 438/618; 438/623; Assistant Examiner---Shrinivas H Rao 438/931; 438/940; 438/962 ABSTRACT (58) Field of Search ................................. 438/618, 962, (57) 438/487, 940, 931, 623 A nanowire, nanosphere, metallized nanosphere, and meth­ ods for their fabrication are outlined. The method of fabri­ (56) References Cited cating nanowires includes fabricating the nanowire under U.S. PATENT DOCUMENTS thermal and non-catalytic conditions. The nanowires can at least be fabricated from metals, metal oxides, metalloids, 5,783,498 A * 7/1998 Dotta ......................... 438/778 and metalloid oxides. In addition, the method of fabricating 5,801,092 A * 9/1998 Ayers ......................... 438/623 nanospheres includes fabricating nanospheres that are sub­ 5,937,313 A * 8/1999 Kang ......................... 438/478 stantially monodisperse. Further, the nanospheres are fabri­ 5,976,957 A * 11/1999 Westwater et al. .......... 438/478 cated under thermal and non-catalytic conditions. Like the (List continued on next page.) nanowires, the nanospheres can at least be fabricated from metals, metal oxides, metalloids, and metalloid oxides. In OTHER PUBLICATIONS addition, the nanospheres can be metallized to form metal­ R.C.Salvarezza et al., Edward-Wilkinson Behavior of crys­ lized nanospheres that are capable as acting as a catalyst. tal Surfaces Grown by Sedimentation of Si02 Nanoshperes, 1996, Physical review letters, vol. 77, No. 22, Nov. 25, 1996 9 Claims, 1 Drawing Sheet 20 ~ 22 PROVIDING A COMPOSITION 24 VAPORIZING THE COMPOSITION FORMING A NANOSTRUCTURE VIA A CONDENSATION REACTION UNDER NON­ CATAL YTIC CONDITIONS US 6, 720,240 B2 Page 2 U.S. PATENT DOCUMENTS 6,359,288 Bl * 3/2002 Ying et al. .................... 257/14 6,365,493 Bl * 4/2002 Vekris et al. ............... 438/558 6,130,143 A * 10/2000 Westwater et al. .......... 438/478 6,461,528 Bl * 10/2002 Scherer et al. ................ 216/56 6,143,211 A * 11/2000 Mathiowitz et al. ........... 264/4 2001/0042932 Al * 11/2001 Mathiowitz et al. ......... 264/4.1 6,235,224 Bl * 5/2001 Mathiowitz et al. ........... 264/4 2002/0175408 Al * 11/2002 Majumdar et al. .......... 257 /734 6,268,041 Bl * 7/2001 Goldstein ................... 428/208 6,297,063 Bl * 10/2001 Brown et al. .................. 438/2 6,313,015 Bl * 11/2001 Lee et al. ................... 438/478 * cited by examiner U.S. Patent Apr. 13, 2004 US 6, 720,240 B2 10 ~ 14 t ZZ 77 Z 77 Z Z Z Z Z C, Z Z Z 77 ZZI FIG. 1 20 ~ ( 22 PROVIDING A COMPOSITION ,, (24 VAPORIZING THE COMPOSITION ,, (2 6 FORMING A NANOSTRUCTURE VIA A CONDENSATION REACTION UNDER NON- CATALYTIC CONDITIONS FIG. 2 US 6, 720,240 B2 1 2 SILICON BASED NANOSPHERES AND activity of the supported metals or metal ions is changed by NANO WIRES interaction with the support metal ions or oxygen atoms. Thus, some supports are not benign towards the catalytic CROSS-REFERENCE TO RELATED agents. Moreover, the catalytic properties of these agents are APPLICATION 5 often compromised as a result of the efforts to synthesize supported catalysts having high dispersions of the active This application claims priority to copending U.S. Pro­ ingredient. These uniquely assembled catalysts might then visional application entitled, "Silicon Based Nanowires and be used to more efficiently control combustion processes, Nanospheres", filed with the United States Patent and Trade­ and reactions such as hydrocarbon reforming. mark Office on Mar. 29, 2000, and assigned Ser. No. 10 60/192,846, and U.S. provisional application entitled "New Thus a heretofore unaddressed need exists in the industry to addr~ss the aforementioned deficiencies and inadequa- Cu/Si02 Based Catalyst for Selective Ethanol-Acetaldehyde Conversion", filed with the United States Patent and Trade­ c1es. mark Office on Mar. 29, 2000, and assigned Ser. No. SUMMARY OF THE INVENTION 60/192,844, which are both entirely incorporated herein by 15 reference. An embodiment of the present invention provides for a nanowire and method of fabrication thereof. The method TECHNICAL FIELD includes fabricating the nanowires under thermal and non­ The present invention is generally related to nanostruc­ catalytic conditions. The nanowires can be fabricated from at least metals, metal oxides, metalloids, and metalloid tures and, more particularly, is related to nanowires and 20 nanospheres and methods for their preparation and use. oxides. A preferred embodiment of the present invention includes, but is not limited to, the fabrication of a silicon BACKGROUND OF THE INVENTION dioxide sheathed crystalline silicon nanowire, where the axis of the crystalline silicon nanowire core is substantially Semiconductor nanostructures, nanoagglomerates, and 25 parallel to a <111> plane and is substantially free of defects. nanowires have attracted considerable attention because of Another embodiment of the present invention provides for their potential applications in mesoscopic research, the a nanosphere and method of fabrication thereof. The method development of nanodevices, and the potential application includes fabricating the substantially monodisperse nano­ of large surface area structures. For several decades, the spheres under thermal and non-catalytic conditions. The vapor-liquid-solid (VLS) process, where gold particl~s act 30 nanospheres can at least be fabricated from metals, metal as a mediating solvent on a silicon substrate formmg a oxides, metalloids, and metalloid oxides. A preferred molten alloy, has been applied to the generation of silicon embodiment of the present invention includes, but is not whiskers. The diameter of the whisker is established by the limited to, fabricating amorphous silicon dioxide nano­ diameter of the liquid alloy droplet at its tip. The VLS spheres. reaction generally leads to the growth of silicon whiskers 35 Still another embodiment of the present invention pro­ epitaxially in the <111> direction on single crystal silicon vides for a metallized nanosphere and method of fabrication <111> substrates. In addition, laser ablation techniques have thereof. The method includes fabricating the subtantially been performed on metal-containing (iron or gold) silicon monodisperse nanospheres under thermal and non-catalytic targets, producing bulk quantities of silicon nanowires. conditions. The nanospheres can be fabricated from at least Further, thermal techniques have been used to produce a 40 metals, metal oxides, metalloids, and metalloid oxides. The jumble of silicon dioxide (Si0 ) coated crystalline nanow­ 2 nanospheres can be metallized to form metallized nano­ ires that have their axes parallel to the <112> direction. spheres that are capable of having catalytic properties. In Further these nanowires are deficient because of twinning, addition, the formation of the nanospheres and metallization high order grain boundaries, and stacking faults. of the nanospheres can be performed substantially in one Recently, national lab researchers, in an effort to begin an 45 step. A preferred embodiment of the present invention ongoing dialogue to forecast the direction of environmental includes fabricating amorphous silicon dioxide nanospheres science and technology, ranked the top ten environmental and depositing three weight percent (%) copper onto the technology breakthroughs for 2008. Not surprisingly, nanosphere. molecular design is expected to play an important
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