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(12) United States Patent (10) Patent No.: US 7,273,567 B1 Wellinghoff Et Al

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(12) United States Patent (10) Patent No.: US 7,273,567 B1 Wellinghoff Et Al US007273567B1 (12) United States Patent (10) Patent No.: US 7,273,567 B1 Wellinghoff et al. (45) Date of Patent: *Sep. 25, 2007 (54) ENERGY-ACTIVATED COMPOSITIONS FOR (56) References Cited CONTROLLED SUSTAINED RELEASE OF A U.S. PATENT DOCUMENTS GAS 3,904,221 A 9, 1975 Shik1 et al. (75) Inventors: Stephen T. Wellinghoff, San Antonio, 4,561,994. A * 12/1985 Rubin et al. ........... 252,187.23 5,008,096 A 4, 1991 Ringo ........................ 423,477 TX (US); Joel J. Kampa, Boerne, TX 5,108,649 A 4, 1992 Matsumoto et al. ... 252188.28 (US); Michael D. Lelah, Chicago, IL 5,244,811 A 9, 1993 Matthews ................... 436,146 (US); Sumner A. Barenberg, Chicago, 5,306,440 A 4/1994 Ripley et al. ..... 252/186.33 IL (US); Peter N. Gray, Chicago, IL 5.330,661 A 7, 1994 Okuda et al. ............... 210,748 (US); Hong Dixon, Helotes, TX (US) 5,340,605 A 8/1994 Silver et al. ............. 427,126.3 5,360,609 A 11/1994 Wellinghoff ...... ... 514,772.3 (73) Assignee: MicroActive Corp., Reno, NV (US) 5,411,643 A 5/1995 Cawlfield et al. ........... 204,115 5,501,801 A 3/1996 Zhang et al. ..... ... 210,748 (*) Notice: Subject to any disclaimer, the term of this 5,616,532 A 4/1997 Heller et al. ...... ... 502,242 patent is extended or adjusted under 35 5,631,300 A 5/1997 Wellinghoff ............. 514,7723 U.S.C. 154(b) by 0 days. 5,639,295 A 6/1997 Wellinghoff et al. ..... 106.15.05 5,650,446 A 7/1997 Wellinghoff et al. ..... 514,7723 This patent is Subject to a terminal dis 5,658,841 A 8/1997 Tanaka et al. .............. 502,305 claimer. (Continued) (21) Appl. No.: 09/448,927 OTHER PUBLICATIONS Frank, et al. “Semiconductor Electrodes. 12. Photoassisted (22) Filed: Nov. 24, 1999 Oxidations and Photoelectrosynthesis at Polycrystalline TiO, Elec trodes,” Journal of the Am. Chemical Society, vol. 99, No. 14, pp. (51) Int. Cl. 4667-4675, 1977. COB II/06 (2006.01) COB II/It (2006.01) (Continued) COIB 7/50 (2006.01) A6IL 2/20 (2006.01) Primary Examiner Joseph D. Anthony A6IL 2/23 (2006.01) (74) Attorney, Agent, or Firm—Senniger Powers (52) U.S. Cl. ........................... 252/187.23; 252/187.21; (57) ABSTRACT 252/187.22; 252/1871; 252/188.1; 252/188.21; 252/187.25; 252/187.24; 252/186.43; 424/405: A composition for energy-controlled generation and release 424/406; 424/417; 424/604; 424/613; 424/614; of at least one gas, which includes an energy-activated 424/635; 422/5: 422/22; 422/24; 422/29: catalyst capable of being activated by electromagnetic 422/120: 422/121; 422/37 energy, and a Solid or a liquid containing anions capable of (58) Field of Classification Search ........... 252/186.43, 252/187.23, 187.24, 187.25, 187.21, 187.22, being oxidized by the activated catalyst or reacted with 252/187.1, 186.44, 188.1, 188.21; 149/5, species generated during activation of the catalyst to gen 149/46, 61, 74,76, 77: 424/405, 408, 417, erate at least one gas. The composition, when exposed to 424/604,613, 614, 635, 637, 646, 661, 565, electromagnetic energy, is capable of generating and releas 424/692, 700, 715, 717: 423/419.1, 421, ing the gas after activation of the catalyst and oxidation or 423/438, 473, 477, 478, 582, 610; 134/1; reaction of the anions. 422/5, 22, 24, 29, 37, 120, 121 See application file for complete search history. 20 Claims, 13 Drawing Sheets 14 LIGHT OFF 12 10 8 era 6 E S 4 S 2 O O 5 10 15 20 25 -2 TIME (DAYS) US 7,273,567 B1 Page 2 U.S. PATENT DOCUMENTS 5,914, 120 A 6/1999 Wellinghoff et al. ........ 424/406 5,922,776 A 7/1999 Wellinghoff et al. ..... 514/772.3 5,668,185 A 9, 1997 Wellinghoff............ 514,772.3 5,965,264 A 10/1999 Barenberg et al. 428/402 2. A 1. WE al .55 iii. 5,980,826. A 1 1/1999 Barenberg et al. ... 422/37 5,707,739 A 1/1998 Wellinghoff et al. ........ 428,403 6,306,352 B1 * 10/2001 Yoshida et al. ............. 422/120 5,736,165 A 4, 1998 Ripley et al. ........ ... 424,661 5,753,106 A 5, 1998 Schenck ..... 210,96.1 OTHER PUBLICATIONS 5,772,897 A 6, 1998 Hancock ..... ... 210,756 5,783,105 A 7/1998 Zhang et al. .. ... 252/18731 Inoue, et al. “Competitive Photosensitized Oxidation at TiO, 5,849,200 A 12/1998 Heller et al. ................ 210,748 Photoanode, Chemistry Letters, , pp. 1073-1076, 1977. 5,854,169 A 12/1998 Heller et al. ...... ... 502/242 International Search Report in PCT/US00/10804 dated Aug. 24. 5,868,924 A 2, 1999 Nachtman et al. ............ 210/85 2000 (4 pages). 5,872,072 A 2, 1999 Mouri et al. ................ 502,208 Patent Abstracts of Japan, vol. 012, No. 252 (C-512), Jul. 15, 1988 5,874,701 A 2f1999 Watanabe et all 204,157.15 & JP 63 040705 A (EBARA RES COLTD), Feb. 22, 1988. 5,880,067 A 3, 1999 Linkous ......... ... 504,151 Partial European Search Report for European Patent Application 5,883,330 A 3, 1999 Yoshida ......... ... 149.83 No. EP 00926243.7, dated Mar. 26, 2003, 5 pages. 5,888,528 A 3/1999 Wellinghoffetal 424/405 5,898,126 A 4, 1999 Yoshida ....................... 149/46 * cited by examiner U.S. Patent Sep. 25, 2007 Sheet 1 of 13 US 7,273,567 B1 FIG. 1A FIG. 1B 18 20 16 12 FIG. 1C U.S. Patent Sep. 25, 2007 Sheet 2 of 13 US 7,273,567 B1 FIG. 2 0-22.2 HOURS IN THE DARK 22.22 HOURS-END UNDER FLUORESCENT LIGHT 10 20 30 40 50 TIME (HRS.) 0.15 0-9344 SECONDS IN THE DARK 9344-20745 SECONDSHOURS FLUORESCENT LIGHT O 5000 10000 15000 20000 25000 TIME (SECONDS) O-6.95 HOURS UNDER FLUORESCENT LIGHT 6.95-23.85 HOURS IN THE DARK 0.15, 23.85-31.83 HOURS UNDER FLUORESCENT LIGHT 31.83-47.93 HOURS IN THE DARK 16 0.1 47.93HOURS-END UNDER FLUORESCENT LIGHT N- 0.05 (N O O O -0.05 O 10 20 30 40 50 60 TIME (HRS.) U.S. Patent Sep. 25, 2007 Sheet 3 of 13 US 7,273,567 B1 FIG. 5 O-14.7 HOURS IN THE DARK 14.7-89.1 HOURS UNDER FLUORESCENT LIGHT (82.2-86.7 HOURS DATA LOST DUE TO POWER FAILURE) 89.1-94.8 HOURS IN THE DARK 94.8-95 HOURS UNDER FLUORESCENT LIGHT 8 6 S 4 S 2 O O -2 O 20 40 60 80 100 TIME (HRS.) FIG. 6 O-17.2 HOURS UNDER FLUORESCENT LIGHT 17.2-17.7 HOURS IN THE DARK 17.7-22.1 HOURS UNDER FLUORESCENT LIGHT 20 22.1-24 HOURS IN THE DARK O 5 10 15 20 25 TIME (HRS.) U.S. Patent Sep. 25, 2007 Sheet 4 of 13 US 7,273,567 B1 3 O O f O N N t r (udd) COO U.S. Patent Sep. 25, 2007 Sheet S of 13 US 7,273,567 B1 (ELVOITIS9%GºO)OGO‘66–?}}}}}}9/6S)ELWOITIS96Z)GE0"66––– 980'66---- (’SHH)EWIL ~ GZ0ZGI0?G (udd) COO U.S. Patent Sep. 25, 2007 Sheet 6 of 13 US 7,273,567 B1 | SWIWIWIWIWW||||||| |…] (SAVCI)BWIL O'I 6"5DI COO WON U.S. Patent Sep. 25, 2007 Sheet 7 of 13 US 7,273,567 B1 r S (N L t V 3 s O d O (udd) COO U.S. Patent Sep. 25, 2007 Sheet 8 of 13 US 7,273,567 B1 0 SNOdS CON OZIWWON II'5OI U.S. Patent Sep. 25, 2007 Sheet 9 of 13 US 7,273,567 B1 FIG. 12 SAMPLE ILLUMINATED OS 10 \ St 5 SAMPLE BLACKOUT N O O O O 1.0 1.5 2.0 2.5 3.0 3.5 -5 TIME (DAYS) FIG. 13 - 14 DETECTOR OFF-SCALE ié SAMPLE ILLUMINATED St 8 N 6 O 4 O 2 O O 10 20 30 40 50 60 TIME (MIN.) U.S. Patent Sep. 25, 2007 Sheet 10 of 13 US 7,273,567 B1 FIG. 14 14 12 S 10 S. 8 S 4 2 9 5.0 10.0 15.O 20.0 25.0 30.0 TIME (HRS.) FIG. 15 SAMPLE REMOVED 2.0 3.0 4.0 TIME (HRS.) U.S. Patent Sep. 25, 2007 Sheet 11 of 13 US 7,273,567 B1 FIG. 16 1.4OE-03 1.2OE-03 1.OOE-03 8.00E-04 6.OOE-04 CO2 4. OOE-04 2.OOE-04 C2 O.OOE-00 O.O 5.0 10.0 15.0 TIME (HRS.) FIG. 17 1.2OE-03 1.OOE-03 8.00E-04 6.OOE-04 CO2 4.OOE-04 2.OOE-04 CI2 0.00E--00 O.O 1.0 2.0 3.0 4.0 5.0 TIME (HRS.) U.S. Patent US 7,273,567 B1 08GI (’SHH)EWIL U.S. Patent Sep. 25, 2007 Sheet 13 of 13 US 7,273,567 B1 f N –- O N f t gar CC S S L 2. - O H C O H - f V N O OO Vo V on O N y H. H. s (udd) COO US 7,273,567 B1 1.
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