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That the Ultimine THAT THEUS009765271B2ULTIMINE (12 ) United States Patent ( 10 ) Patent No. : US 9 ,765 , 271 B2 Myrick (45 ) Date of Patent: Sep . 19 , 2017 (54 ) NANOPARTICLES, COMPOSITIONS, ( 52 ) U . S . CI. MANUFACTURE AND APPLICATIONS CPC .. .. .. .. CI0L 1 /28 ( 2013 .01 ) ; COIB 33 / 027 (2013 2013 . 01 ) ; C06B 33/ 06 (2013 .01 ) ; C06B 45 /30 (71 ) Applicant: James J . Myrick , Glencoe, IL (US ) ( 2013 .01 ) ; Y10T 428 / 12181 ( 2015 .01 ) ( 58 ) Field of Classification Search ( 72 ) Inventor: James J .Myrick , Glencoe, IL (US ) CPC .. C23C 14 / 0057 ; C01B 33 /037 ( * ) Notice : Subject to any disclaimer , the term of this See application file for complete search history. patent is extended or adjusted under 35 (56 ) References Cited U . S . C . 154 ( b ) by 0 days. U . S . PATENT DOCUMENTS ( 21 ) Appl . No . : 14 / 190 , 082 3 ,008 , 887 A * 11/ 1961 Herglotz . .. C01B 33/ 037 422 / 186 .04 (22 ) Filed : Feb . 25 , 2014 6 ,455 , 455 B1 * 9 /2002 Deller .. .. B82Y 30 /00 423 / 327 . 2 (65 ) Prior Publication Data 2007/ 0158182 A1* 7 / 2007 Takahashi .. .. C23C 14 /0057 204 / 192 . 12 US 2014 /0227548 A1 Aug. 14 , 2014 2008 /0248307 A1 * 10 /2008 Jurbergs .. .. .. .. B82Y 30 /00 Related U . S . Application Data 428 / 405 (63 ) Continuation - in -part of application No . 13 /929 , 771 , * cited by examiner filed on Jun . 27 , 2013 . Primary Examiner — Aileen B Felton (60 ) Provisional application No. 61/ 745 ,810 , filed on Dec . (74 ) Attorney , Agent, or Firm — Husch Blackwell LLP 25 , 2012 , provisional application No . 61/ 664 , 987 , (57 ) ABSTRACT filed on Jun . 27 , 2012 . There are disclosed energetic nanoparticle compositions and materials containing silicon and other energetic elements , (51 ) Int. Ci. and methods ofmanufacturing the same, including reacting C23C 14 /00 ( 2006 .01 ) silicon nanoparticles and unsaturated alkene or alkyne to COIB 33 /037 ( 2006 . 01 ) CI0L 1 /28 ( 2006 .01 ) form covalently bonded surface coatings passivated against C06B 45 /30 ( 2006 . 01 ) surface oxidation , for combination with a fuel, explosive or COIB 33 /027 ( 2006 .01 ) oxidizer. C06B 33 / 06 ( 2006 . 01) 7 Claims, 29 Drawing Sheets Raw Si, power, cooling Cooler 208 to Vacuum pump condense and and purification Plasma recycle vapor system 210 to torch 202 Sinanopowder collection collect and return system 206 (eg , liquid (may include inert gas (Argon ) walled cyclone trap , distillation to continuous momentum classifier , purification to process use . electrostatic precipitator , remove non etc . May include reactor Silicon for Si particle surface impurities chemistry modification Nanosilicon output Argon /H2 return U . S . Patent Sep. 19 , 2017 Sheet 1 of 29 US 9 ,765 , 271 B2 FIGURE 1 132 133 133 140 24 106 124 130 108 104 W 140 Plasma Torch 100 Plasma Arc 112 De Laval expansion cooling nozzle 114 (supersonic ) FIGURE 2 Raw Si, power , cooling Cooler 208 to Vacuum pump condense and and purification Plasma recycle vapor system 210 to torch 202 Si nanopowder collection collect and return system 206 ?eg , liquid (may include inert gas (Argon ) distillation to continuous walled cyclone trap , purification to momentum classifier , process use . electrostatic precipitator, remove non etc . May include reactor Silicon for Si particle surface impurities chemistry modification Nanosilicon output Argon /H2 return U . S . Patent Sep . 19, 2017 Sheet 2 of 29 US 9 ,765 , 271 B2 FIGURE ZA 4Si + SiCl4 at 1 Bar kmol File : C : \ Program Files \Gibbs In .OGI 5 . 0 Si ( g ) ett SO ) * OK * * * 0 .5 SiC13 ( g ) Sizin * Temperature 0 . 0 wwww wwwwwwwviermi 500500 1000 15001 500 20002000 2500 30003000 35003500 4000 FIGURE 3B 2 Si + SiBr4 at 1 bar kmol File : C : \ Program Files \GibbsIn .OGI - - Br( g ) 7An - - - Sig ) - - - - - - - - - - - I - - - - - - - - - - - - - - - - - - - - - - - - - - - 09 - .2 - . SiBr in . - . - * *** * $ 18319 DR S3 e Temperature 0 500 10001000 1500 20002000 2500 3000 3500 4000 U . S . Patent Sep. 19 , 2017 Sheet 3 of 29 US 9 , 765, 271 B2 FIGURE 3C 2 Si + B + SiC14 at 1 Bar kmol File : C : \ Program Files \Gibbs 11 .OGI hebbende? SC14 ) BCI g ) - S? ( g ) - - - - .. ) 301369m ( 1 . 1 ) K ODDDDDDDDDDDDDDDDDDDD Temperature 0 500500 1000 1500 20002000) 25042500) 30003100 3500 40004000 FIGURE 3D 2 Si + 1 B + SiC14 + 0 . 25 Fe + 0 .25 Al at 1 Bar kmol File : C : \Program Files\ Gibbsin .OGI 2 . 0 - - - 1. 5 - - - - 1 .0 XC40 TL B - 0 . 5 003 SiC3( ) Zing *** * SIZ ( ) Temperature 0 . 0 500 4182 1000 1500 feb 2000 2500 Penn 3000 3500 4000 W * FeSi2 . 33 FOC12 ( e ) og U . S . Patent Sep . 19, 2017 Sheet 4 of 29 US 9 ,765 , 271 B2 FIGURE ZE 2 Si + BF3 at 1 Bar kmol File : C : \ Program Files \Gibbsin . OGI 1 . 5 - - - - - - - - - - - - - - - - - - - - - - 0 . 8 N1343: . 1 Sif2 ( g ) V 0 , 5 mes MB .0 . 4 - - - - > - - 0 . 1 * * SAD ) Temperature 0 . 0 w wwwwwwww wwwwwwwwwww w wwwSi3 * * ( g )* * * * * * 500500 1000 1500 20002000 2500 3000 FIGURE 3F 1 Si + 1 . 5 H2 at 1 Bar kmol File : C : \ Program Files \Gibbsin .OGI DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDD- bank Hig ) i s? X 8 SH2 ( g Temperature en * * * * * * * * 0 500 1000 1500 20002000 2500 30003000 35003500 40004000 C U . S . Patent Sep. 19 , 2017 Sheet 5 of 29 US 9 , 765, 271 B2 FIGURE 3G - 1 45i + 3H2 + 0 . 05 SiF4 + 0 . 05 SiC14 + 0 . 025A1 + 0 . 025B at 0 . 01 Bar kmol File : C : \ Program Files \Gibbs In .OGI H ( g ) Silo FITOTT * : . 4 . ' 31xg) CIX SICHA (g ) BHFU) HCIO ) SiCl( g ) VV v - v 0 sub sssssssssssssss 54swoiminut88 Temperaturepointu 50, 1000200 *2000 15000 2000 2500 3000 3500 4000 C FIGURE 3G - 2 4Si + 3H2 + 0 . 05SiF4 + 0 .05 Sic14 + 0 . 025Al + 0 . 025B at 0 .01 bar kmol File : C : \ Program Files \GibbsIn .OGI 0 . 031) HCKg) Sima) 0 . 025 Burg . SiC14 ( g ) 0 . 020 - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - 0 .015 AT + + 0 . 010 AIC12F ( g ) *** . ..my .. * * . AlClglig ) .. -- 0 .005 AICO ( g ) Sie 0 . 000 Temperature 500 X 700 SiCIF3 ( g ) 900 6 * 3 * 1 100 1300 , SiCl( g ) 1500 C $ 03389 SIC136 AUB ) U . S . Patent Sep . 19, 2017 Sheet 6 of 29 US 9 ,765 , 271 B2 FIGURE 3H 3Al + 2H2 in 1 Ar at 1 bar kmo ) File : C : \ Program Files \GibbsIn . OGI A } eboere . * bainab?sb xia Al2 ( g ) Me BOOOOOooosssssssssssssssssssssss Temperature 500500 1000 1500 2000 25002590 3000 3500 40004000 C FIGURE 31 B203 + 2 .50 + 0 . 25 CH4 + 2 . 25Ar at 1 bar kmo1 File: C : \ Program Files Gibbsin . OGI 3 , 0 CON 2 . 5 2 . 0 1 . 5 . *. * . * .* . ? ????? B203 0 5HBOX. H38 028 BO ) B203 ( g ) BCNetetter Temperature 500 1000 1500 2000 2500 3000 3500 4000 atent Sep . 19 , 2017 Sheet 7 of 29 US 9 , 765 , 271 B2 FIGURE 31 B203 + 3 Si - 2 . 5 C + {} , 25 C14 + 2 . 25 Arg) kmol File : C : \ Program Files \Gibbsin .OGI 3 . 0 Si( g ) CO ( g ) Jario ) Appar , Art , , , , , , , , , , , , , par , , , 4 , 4 , 4 , 4 , - , - , - , - , - , - , - , , - , , , - , , - , , - , - , , , , , , , - , , , , - , - , , , , - , - , - , , - , , - , - , - , , - , - , - , , , - , , - , , - , , , , - , - , , - , - , . " . 2 . 0 . , . itu . 1 . 5 S02 10 Hy) . Sog 0 . 5 ma - - - Red- 7 - 7 $ 30 $ 320 ) W B203 ( g ) 0 . 0 d Temperature raon B2Crona SEX ( 4000 C 500 1000 1500 2000 2542500 Sichu ) Sizc (X g ) 2 0Xg ? SBC ) FIGURE 22 2200 2202 2204 2206 2208 U . S . Patent Sep . 19, 2017 Sheet 8 of 29 US 9 ,765 , 271 B2 FIGURE 3K CH4 + Al + 0 . 75 B - +- 0 . 5 Si at 0 .01 bar bone kmol File : C : \ Program Files GihbsIn .OGI 2 . 5 T 2 . 0 Izlet 1 . 5 10 sic 0 . 5 * * - - -- A3403 ** * * BC2BC ( g ) HX 0 . 0 www w ww . Temperature 500 1000 1500 2000 2500 * * * * 3000 3500 4000 C FIGURE 3L 2H2 + 2 Ce + 2 Si + 2 AL at 0 . 01 bar kmo) File : C : \ Program Files \Gibbs In .OGI HO) Silg ) H269 022 AL 0412 Litter- - - . CeAl4 SIZ ( )SH . Temperature ??????????????? O 500500 1000 15001500 20002000 25002500 30003000 3500 40004000 C U . S . Patent _ Sep . 19 ,2017 _ Sheet 9 of 29 US 9 , 765 ,271 B2 FIGURE 4 - - - 5 442 - ... * * * * *- 420 *“ , - %?????????s89$8????????????????????????8 - +" • . “- -"--. * *( * " **.* + *+ + ¢“ +.-` +& * ??? * ** 8 • *.* “. a * ? • . ? *- ' % * ????? * ? * % ? * ? ? ? %=88 *&% % % % 412 %& 404 %888???????????????????????????????? *-&% _ ??? % ???? 440 ? ? ? 424 406 ? ??? ?????? _ ?????? ,"- ?????? ????%8 ,&• * % ?? 426 *???????? ???? %9$ ? * ??? . • • “ • . * • * * ** * ** * * * * ** * *. .' ? ? $ $% % 418 ? ????????? E %=>9$??8 ww w =kw - w - ??w 408 416 416 U . S . Patent Sep . 19, 2017 Sheet 10 of 29 US 9 , 765, 271 B2 FIGURE 5A 510 ** 512 506 505 9 ? 22222222222222 112222222222222LLLLLL2 LLLLLL zzzzzZZZZZZZZZZZZZZZZZZZZZzzzzzzzzzzzzZZZZZZZZZZZZZZZZZZZZZZZZzzzzzzzzzzZZZZZZZZZZZZ 502 520 N 504 U . S . Patent Sep. 19 , 2017 Sheet 11 of 29 US 9 , 765, 271 B2 FIGURE 5B 550 560 512 560 SET TIZIE ViYTT - - - 560 31 408 FIGURE 6 600 604 602 A 670 635 63829 Lt 634 606 630 635 U . S . Patent Sep. 19 , 2017 Sheet 12 of 29 US 9 , 765, 271 B2 FIGURE ZA FIGURE 8 704 704 719 7708 FIGURE 7B 760 770 62 770 772 764 752 790 768 FIGURE 9A 766 Covalently attach protective 904 and /or oxidative groups to surface by Grignard reaction or hydrosilylation Si nanoparticle 902 with Si nanoparticle 902 with - Clor -- H surface groups Grafted surface layer 904 906 FIGURE 9B ** Covalently graft energetic ** ** * ** *XXXXXX Oligomer or polymer to Silicon ** nanoparticle surface U . S . Patent Sep . 19, 2017 Sheet 13 of 29 US 9 , 765, 271 B2 FIGURE 9C Covalently graft energetic oligomer to Silicon nanoparticle surface FIGURE 9D FIGURE 9E lesU . S . novesPatent Sepacom . 19, 2017 wwwenSheet 14 of 29 . US 9 , 765, 271 B2 FIGURE 9F CooFIGURE 9G FIGURE 9H 00000 000 Og 2088 De t DCer Power Supply 1002 0 - 10 V FIGURE 10A 1000 Program Controller 1004 1022 Electrodeposition Cell 1006 Substrate 1010 Temperature sensor 1018 Counterelectrode 1014 WWW Reference electrode 1020 lectrolyte : 1: 07 1023 U . S . Patent Sep . 19, 2017 Sheet 15 of 29 US 9 ,765 ,271 B2 FIGURE 10 F { GURE 11 1100 Spols 1116 Cathode sLbstrate 1102 - Guides { { { 0 Trrrrr Cathode Contacts 108 Counteelectrcdes 304 Plaing Tank 1334 ag electrolyte { { 06 FIGURE 10 105 1052 1056 | 1061060 » 1070 154- ?? 1059 062?? U .
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