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(12) United States Patent (10) Patent No.: US 7,879,310 B2 Spear Et Al US00787931 OB2 (12) United States Patent (10) Patent No.: US 7,879,310 B2 Spear et al. (45) Date of Patent: Feb. 1, 2011 (54) SILANES ASA SOURCE OF HYDROGEN 5,328,779 A 7, 1994 Tannenberger et al. ........ 429/32 5,508,128 A 4/1996 Akagi ......................... 429/30 (75) Inventors: Scott K. Spear, Bankston, AL (US); 5,650,132 A 7/1997 Murata et al. ............... 423,650 Daniel T. Daly, Tuscaloosa, AL (US); 5,741,408 A 4/1998 Helmer-Metzmann Richard P. Swatloski, Tuscaloosa, AL et al. ............................... 13.8 (US); Raymond E. Paggi, Winchester, 5,840,270 A 1 1/1998 Werth ......................... 423,658 VA (US); Michael D. Redemer, 5,858,541 A 1/1999 Hiraoka et al. .... ... 428,429 Danville, CA (US) 6,060,026 A 5/2000 Goldstein et al. ........... 422, 186 (73) Assignee: Board of Trustees of the University of Alabama, Tuscaloosa, AL (US) (Continued) (*) Notice: Subject to any disclaimer, the term of this patent is extended or adjusted under 35 FOREIGN PATENT DOCUMENTS U.S.C. 154(b) by 1156 days. SU 1286,506 4f1985 (21) Appl. No.: 11/497,638 (22) Filed: Aug. 2, 2006 (Continued) Prior Publication Data (65) OTHER PUBLICATIONS US 2010/O255392 A1 Oct. 7, 2010 Harreld, John H. et al., Surfactant and pH-mediated Control over the Related U.S. Application Data Molecular Structure of Poly(phenylsilsesquioxane) Resins, 2002, Chem. Mater, 14, pp. 1174-1182.* (60) Provisional application No. 60/705.331, filed on Aug. 3, 2005. (Continued) (51) Int. Cl. Primary Examiner David M. Brunsman COIB 3/02 (2006.01) Assistant Examiner Kevin MJohnson HOLM 8/06 (2006.01) (74) Attorney, Agent, or Firm McKeon Meunier Carlin & Curfman LLC (52) U.S. Cl. .................................... 423/648.1; 429/416 (58) Field of Classification Search ................. 423/627, (57) ABSTRACT 423/644, 648.1-658.3; 429/416 425 See application file for complete search history. (56) References Cited Disclosed are compositions, methods, and devices that gen erally relate to silanes and silicides and to uses thereof for U.S. PATENT DOCUMENTS hydrogen generation. Methods and devices for generating 3,328,481 A 6, 1967 Vincent ...................... 525/477 hydrogen for fuel cells and for other applications such as fuel 3,673,115 A 6, 1972 Linsen et al. ............... 5O2,259 or a Supplementary fuel for internal combustion engines and 4,637,867 A 1, 1987 Herbst ......... 204,157.52 reducing agents to improve catalyst efficiency are also dis 5,079,103 A 1/1992 Schramm ..................... 429.17 closed. 5,273,837 A 12/1993 Aitken et al. .................. 429/30 5,306,578 A 4, 1994 Ohashi et al. ................. 429/27 13 Claims, 10 Drawing Sheets Reaction Chamber (16) with non woven polyaniline (or similar function) fabric with integral skeletal silicate precipitate Silane (ary or aliphatic) b Hydrogen out (17) fuelin (11) 121O Check valves t 4-1 Hydrogen permeable membrane (18) Water in from fuel cell (13) US 7,879,310 B2 Page 2 U.S. PATENT DOCUMENTS Browning, Darren, “DERA Research on H2 storage and Generation Methods for Fuel Cells' Sep. 2006. 6,080,503 A 6/2000 Schmid et al. ................ 429/35 Hahn, John, “Hydrogen production from Biomass,” dissertation, 6,087.033 A 7/2000 Grune et al. ... ... 429.26 University of Missouri, p. 76-78, Dec. 2006. 6,106,963 A 8/2000 Nitta et al. ........ ... 429/10 Nath et al. “Hydrogen from Biomass' Current Science 85(3):267. 6,336,430 B2 1/2002 De Souza et al. ... 123.3 2003. 6,348,278 B1 2/2002 LaPierre et al. ... ... 429, 17 Neal et al. “Primary Reaction Channels and Kinetics of the Thermal 6,399,235 B1 6/2002 Yen et al. ....... ... 429/33 Decomposition of Phenylsilane” Journal of Physical Chemistry 6,544.400 B2 4/2003 Hockaday ... ... 205/.338 99.9397, 1995. 6,572,837 B1 6, 2003 Holland et al. 423,648.1 International Search Report for PCT/US08/052127, dated Oct. 16, 6,582,676 B2 6, 2003 Chaklader et al. 423,648.1 2008. 6,733,916 B2 5/2004 Mizuno ....................... 429/30 International Search Report for PCT/US08/072523, dated Apr. 2, 7,037,484 B1 5/2006 Brandenburg .. 423,648.1 2009. 2003/0215679 A1* 11/2003 Reinke et al. ................. 429/13 Bhandakar, “Modeling of Silicon Hydride Clustering In A Low Pressure Silane Plasma.” J Phys D. Appl Phys, 33:2731-2746, 2000. FOREIGN PATENT DOCUMENTS Chernov et al., “Production of Hydrogen From Siloxene 1.” Zhurnal WO WO2005/037421 4/2005 Prikladnoi Khimi, 63(8): 1802-6, 1990 (Translated). WO WO2006/O13753 2, 2006 Chung et al., “Nature of the Active Silane Alcoholysis Catalyst in the WO WO2006/099.716 9, 2006 Ru,CI,(CO),(PMes) (w, x, y, z=1 or 2) System; Ru(u- WO WO2007/054290 5/2007 CI)CI(CO),(PMe) as a New Catalyst for Silane Alcoholysis in a WO WO2008/094840 8, 2008 Polar Solvent.” CanJ Chem/Rev Can Chim, 79(5-6): 949-957, 2001. WO WO2009/023535 2, 2009 Fargas et al., "Calorimetry of Hydrogen Desorption From a Si-Nanoparticle.”. 2002. OTHER PUBLICATIONS Mitzel et al., “The Molecular Structures of Three Disilylbenzenes Determined in the Gas Phase, The Solid State, and Ab Initio Calcu Schubert, Ulrich and Catrin Lorenz, Conversion of Hydrosilanes to lations.” Z. Naturforsch. 57b:202-14, 2002. Silanols and Silyl Esters Catalyzed by Ph3PCuH]6, 1997. Inorganic Workshop Proceedings, “Hydrogen Storage and Generation.” Army Chemistry, 36, pp. 1258-1259.* Research Office and the Central Intelligence Agency, 1997. International Search Report, PCT/US2006/030083, filing date Aug. 2, 2006. * cited by examiner U.S. Patent Feb. 1, 2011 Sheet 1 of 10 N U.S. Patent Feb. 1, 2011 Sheet 2 of 10 US 7,879,310 B2 30e?ums?SÁ?e?eoJoQuelqueW 01, Se6uÐ6OupÁH Á?Indu6?H U.S. Patent Feb. 1, 2011 Sheet 3 of 10 US 7,879,310 B2 ??qe9uuuedue6oupÁH (89)?uelquuauu U.S. Patent Feb. 1, 2011 Sheet 4 of 10 US 7,879,310 B2 S00L U.S. Patent US 7,879,310 B2 (#79)?uelqueue?qeeuuledue6oupÁH U.S. Patent Feb. 1, 2011 Sheet 7 of 10 US 7,879,310 B2 FIG. 7 60 SS 50 aa 545 A PS --PdAc C B PS - NaOH 99 40 C PS - Pd Ac GD D PS + CuAc 35 E PS+ CuAc g) S 30 F PS + CuAc E G DSB + PdAc S 25 F DSB + CuAc C) H DSB 20 I DSB + Hot H20 1 É.1 A B C D E F G F H I U.S. Patent Feb. 1, 2011 Sheet 8 of 10 US 7,879,310 B2 FIG. 8 5 aa 4 SS A PS +PdAc C B PS + NaOH 2 C PS + Pd Ac S 3 D PS + CuAc S E PS + CuAc 2 F PS + CuAc G DSB + PdAc 2 F DSB + CuAc 30 H DSB DSB + Hot H20 > 1 O A B C D E F G F H I U.S. Patent Feb. 1, 2011 Sheet 9 of 10 US 7,879,310 B2 FIG. 9 O Pd black s al- Pd(x, PhSiH, Pd(0) -t- H-Pd-H PhSiHOH H2 H u PhSiHOH RSiH + Pd(0) --> RSiPd-H H >- Pd(0) -H. Pd H . H2 PhSiH, 2Cu(II) H -e- 2Cu() -- H2 -e- Cu(solid) -- Cu(II) U.S. Patent Feb. 1, 2011 Sheet 10 of 10 US 7,879,310 B2 (Z) (I) US 7,879,310 B2 1. 2 SILANES ASA SOURCE OF HYDROGEN electrolyte surface. When hydrogen or methanol fuel feed through the anode catalyst/electrolyte interface, an electro CROSS REFERENCE TO RELATED chemical reaction occurs, generating electrons and protons APPLICATIONS (hydrogen ions). The electrons, which cannot pass through the polymer electrolyte membrane, flow from the anode to the This application claims the benefit of priority to U.S. Pro cathode through an external circuit containing a motor or visional Application No. 60/705,331, filed Aug. 3, 2005, other electrical load, which consumes the power generated by which is incorporated by reference herein in its entirety. the cell. The protons generated at the anode catalyst migrate through the polymer electrolyte membrane to the cathode. At FIELD 10 the cathode catalyst interface, the protons combine with elec The subject matter disclosed herein generally relates to trons and oxygen to give water. silanes and silicides and uses thereof to generate hydrogen. One major challenge for fuel cell development and com Methods and devices for generating hydrogen for fuel cells mercialization has been the supply of fuel to the fuel cell. and for other applications such as fuel or a Supplementary fuel 15 While hydrogen gas is generally the most efficient fuel, the for internal combustion engines and reducing agents to use of hydrogen gas is complicated by storage concerns. For improve catalyst efficiency are also disclosed. example, in order to Supply significant amounts of hydrogen gas, especially for portable fuel cells, the hydrogen gas must BACKGROUND be stored under pressure in specialized tanks. Such pressur ized containers can add weight and complexity to a fuel cell A fuel cell is a device that converts energy of a chemical apparatus, in addition to the costs associated with purifying reaction into electrical energy (electrochemical device) with and compressing hydrogen gas. Another concern regarding out combustion. A fuel cell generally comprises an anode, cathode, electrolyte, backing layers, and current collectors. hydrogen gas is that it can easily ignite. Since the voltage of a typical fuel cell is usually small, they 25 A Direct Methanol Fuel Cell (DMFC) is a popular type of are often stacked in series.
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