Closeout Action: v/w Date n=f-«submitted

CA8120 Georgia Institute of Technology Office of Contract Administration PROJECT CLOSEOUT - NOTICE ' Page: 1 24-FEB-1998 09:32 Closeout Notice Date 24-FEB-1998 Project Number E-18-T33 Doch Id 49504 Center Number 10/24-6-R0881-0A0 Project Director BERTA, YOLANDE Project Unit MSE Sponsor COLUMBIAN CHEMICALS COMPANY/SWARTZ, LO Division Id 14167 Contract Number AGR DTD 29 DEC 1997 Contract Entity GTRC Prime Contract Number Title CARBON NANOPARTICLE ANALYSIS Effective Completion Date 20-FEB-1998 (Performance) 20-FEB-1998 (Reports) Closeout Action: v/w Date n=f-«submitted Final Invoice or Copy of Final Invoice Final Report of Inventions and/or Subcontracts Government Property Inventory and Related Certificate Classified Material Certificate Release and Assignment Other Comments Distribution Required: Project Director/Principal Investigator Research Administrative Network Accounting Research Security Department Reports Coordinator Research Property Team Supply Services Department/Procurement Georgia Tech Research Corporation Project File

'GeorgiaDL^ {S(M^ / J t?tech[ji](o)d(o)@]^7 =3 School of Materials Science and Engineering February 13, 1998 Dr. Charles Herd Columbian Chemicals Company P.O. Box 96 Swartz, LA 71281 Dear Charles and Paul, Enclosed are 9 printouts from EDS analyses, and 37 negatives, with corresponding contact prints, for images obtained of your samples with the field emission and high voltage microscopes, January 20 - February 6. The bulk of the work was completed January 20-22, while you were both here. The follow-up imaging was done in the last week of January and the first week of February, after maintenance on our instruments. The 5 samples successfully imaged are 1) 234 G1, 2) globes, 3) CSDP, 4) 234 G3, and 5) LI-NT. The test material, graphitized carbon black, also produced 3 great images. The sample without usable negatives is "234 standard"; EDS analysis indicated trace amounts of oxygen and sulfur present in this sample (see analysis sheets 2 and 3, and compare to analysis sheet 1, pure carbon film). Following is a list of negative numbers with corresponding sample descriptions and experimental notes. HF2000 Field emission microscope Neq# mag description 8585 1M graphitized carbon black 8586 500K graphitized carbon black 8587 500K graphitized carbon black 8593* 500K 234 G1 * black mark due to light exposure before developing 8594* 500K 234 G1 8595* 500K 234 G1 8596* 500K 234 G1 8597* 500K 234 G1 image slightly distorted by astigmatism 8598* 500K 234 G1 8599* 500K 234 G1 image slightly distorted by astigmatism 8600* 500K 234 G1 image slightly distorted by astigmatism 8601* 500K 234 G1 EDS spectrum taken in region indicated on contact print; - spectrum (sheet 7a) and analysis (sheet 7b) show that O, Si and S were detected School of Materials Science and Engineering, Atlanta, Georgia 30332-0245 U.S.A., fax 404-894-9140 A Unit of the University System of Georgia An Equal Education and Employment Opportunity Institution

8602* 200K 234 G1 EDS spectrum taken in region indicated on contact print; spectrum (sheet 8a) and analysis (sheet 8b) show O, Si and S were detected; Si: O ratio is 1 : 2, suggesting that the compound Si0 2 is present; these findings were confirmed by analysis sheets 4 and 6b analysis sheet 5 only confirms Si; sheets 7b and 9b confirm all three elements, but not the Si: O ratio 8603 0.8m diff pattern of EDS area (too bright, but perhaps still useful) 8609 0.8m Au standard for camera length calculation for #8603 JEM 4000EX hiqh voltaqe microscope 2394 2 n*m globe at edge, 2.0 is the camera constant, LX, in units of nm*cm 2396 400K globe from which diff pattern taken 2397 60K globe overview 2398 2 n*m carbon film 2399 2 n*m 234 G1 particles 2402 150K CSDP 2405 400K CSDP 2406 2 n*m CSDP 2408 400K 234 G3 density of negative is light; may be difficult to print 2409 400K 234 G3 density of negative is light; may be difficult to print 2410 400K 234 G3 density of negative is light; may be difficult to print 2411 400K 234 G3 density of negative is light; may be difficult to print 2412 2 n*m 234 G3 2413 60K LI-NT particle overview, high mag images didn't turn out 2419 400K LI-NT; high mag of particle in #2422 2420 400K LI-NT; high mag of particle in #2422 2422 60K LI-NT particle overview 2433 400K 234 G3 2434 400K 234 G3 2435 200K 234 G3 2436 2 n*m particles from previous image, using smallest aperture 2437 400K 234 G3

If you have any questions about the data, analyses, or negatives, please contact at (404) 894-2545. It was a pleasure working with you both. Thank you for the graphitized carbon black sample; perhaps it will help in finding the reason for the sample contamination in our field emission instrument. Yolande Berta Research Scientist II Georgia Institute oftechnology (404) 894-2545 Enclosures

Refit _0 -K' _0 -K" _S -K' S -K" Refit _0 -K _S -K Wed Jan 21 16:28:05 1998 Chi-sqd = 4.91 Livetime = 68.0 Sec, Standardless Analysis Element Net Error Counts (1-Sigma) C -K 1463 +/- 44 0 -K 0 +/- 0 Cu-K 262 +/- 22 Cu-L 45 +/- 12 S -K 0 +/- 0 Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % x C x C C -K 1463 1.0000 100.00 100.00 0 -K 0 0.3412 0.00 0.00 S -K 0 0.0825 0.00 0.00 Total 100.00 100.00

** Warning ** Undefined detector subtype. Using default value subtype= 2 Refit _0 -K' _0 -K" Refit _0 -K Wed Jan 21 16:20:33 1998 Chi-sqd =4.70 Livetime =59.0 Sec Standardless Analysis Element Net Error Counts (1-Sigma) C -K 1950 +/- 52 O -K 0 +/- 0 Cu-K 209 +/- 25 Cu-L 90 +/- 14 S -K 42 +/- re- Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % X C X C C -K 1949 1.0000 --- 99.82 99.93 0 -K 0 0.3412 0.00 0.00 S -K 42 0.0825 0.18 0.07 Total 100.00 100.00

Refit 0 -K' 0 -K Wed Jan 21 16:24:36 1998 Chi-sqd =3.72 Livetime = 7 6.0 Sec. Standardless Analysis Element Net Error Counts (1-Sigma) C -K 1876 +/- 50 O -K 2 +/- 23 Cu-K 252 +/- 26 Cu-L 68 +/- 14 S -K 41 +/- 16 Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % x C x C C -K 1875 1.0000 --- 99.81 99.92 0 -K 1 0.3412 0.02 0.01 S -K 40 0.0825 0.18 0.07 Total 100.00 100.00

Refit Refit _0 -K" _S -K" _Si-K' _Si-K" Thu Jan 22 10:16:57 1998 Chi-sqd = 2.82 Livetime = 71.0 Sec, Standardless Analysis Element Net Error Counts (1-Sigma) C -K 983 +/- 39 O -K 62 +/- 11 Cu-K 488 +/- 33 Cu-L 9 +/- 11 S -K 56 +/- 8, Si-K 201 +/- 14 Adjustment Factors XM L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % x,c x,c C -K 982 1.0000 95.93 97.59 0 -K 61 0.3412 2.03 1.55 S -K 56 0.0825 0.45 0.17 Si-K 201 0.0805 1.58 0.69 Total 100.00 100.00

Refit _0 -K' _0 -K" _S -K' _S -K" _Si-K / Si-K" Refit _0 -K _S -K Wed Jan 21 17:25:30 1998 Chi-sqd =5.30 Livetime = 72.0 Sec, Standardless Analysis Element Net Error Counts (1-Sigma) C -K 2349 +/- 56 0 -K 0 +/- 0 Cu-K 414 +/- 30 Cu-L 41 +/- 14 S -K 0 +/- _ J ^. Si-K 10 +/- 9 Adjustment Factors Z-Balance: Shell: T 0.0000 1.0000 L 0.0000 1.0000 M 0.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std C -K 2348 x,c 1.0000 x,c 0 -K 0 0.3412 S -K 0 0.0825 Si-K Total 9 0.0805 Wt % 99.97 0.00 0.00 0.03 100.00 Atom % 99.99 0.00 0.00 0.01 100.00

75 70A 65 60-] 55 c o u n t s 50-45 40^ 35 30-25 20-1 15 1(M 5 OA Energy (kev) 2.5 Co limn Take-off angle Acquisition type Creation tine Livetime Deadt ime Channels Channel width Detector type Window type Window thickness Contamination material Contamination thickness File name : HITACHI,GEORGIA TECH 33 Accelerating voltage 200 eds Magnification 1 98/01/21 17:06 Charge 79 79 Beam current 1 32.328 Beam spot size 0 2048 Beam location 0,0 10 Working distance 13.4 Stage X 0 Stage Y 0 0.3 Stage Z 0 none Stage tilt 0 0 Stage rotation 0 Notes: < > 3 > ^ / < S - Wed Jan 21 17:08:29 1998 Livetime : 79.0 Sec. Technique: Peak Location Elements Present: C ( 6), Si(14), Cu(29) Possible Additional Elements: 0s(76) Energy Intensity Element 0.140 69 unidentified 0.278 1631 C Ka 1.750 111 Si Ka 8.036 399 Cu Kal 8.905 62 Cu Kbl or 0s Lai

** Warning ** Undefined detector subtype. Using default value subtype= 2. Refit _0 -K' _0 -K" _S -K' _S -K" Refit _Si-K' _Si-K" Wed Jan 21 17:10:47 1998 Chi-sqd = 4.47 Livetime = 79.0 Sec. Standardless Analysis Element Net Error Counts (1-Sigma) C -K 2327 +/- 56 O -K 24 +/- 14 Cu-K 518 +/- 33 Cu-L 72 +/- 16 S -K 31 +/- 11 Si-K 89 +/- 12" Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % X C X C C -K 2326 1.0000 --- 99.24 99.57 0 -K 24 0.3412 0.35 0.26 S -K 30 0.0825 0.11 0.04 Si-K 88 0.0805 0.30 0.13 Total 100.00 100.00

220 200-180 160 C 140 o u n 120 t s 100-1 Energy (kev) Column Take-off angle Acquisition type Creation time Livetime Deadtime Channels Channel width Detector type Window type Window thickness Contamination material Contamination thickness File name : HITACHI,GEORGIA TECH 33 eds 98/01/22 10:04 69 27.437 2048 10 0.3 none 0 Accelerating voltage 200 Magni fication 1 Charge 69 Beam current 1 Beam spot size 0 Beam location 0,0 Working distance 13.4 Stage X 0 Stage Y 0 Stage Z 0 Stage tilt 0 Stage rotation 0 Notes: ^3>W O f ) C{ IA Qjc^L P6o ) Refit _0 -K' _0 -K" Refit _Si-K" Thu Jan 22 10:04:51 1998 Chi-sqd - 4.21 Livetime - 69.0 Sec. Standardless Analysis Element Net Error Counts (1-Sigma) C -K 2133 +/- 53 0 -K 2 +/- 23 Cu-K 549 +/- 37 Cu-L 59 +/- 14 S -K 70 +/- 18 Si-K 45 +/- 11

Refit _0 -K' 0 -K" Refit _Si-K" Thu Jan 22 10: 04:51 1998 Chi-sqd = 4.21 Livetime = 69.0 Sec, Standardless Analysis Element Net Error Counts (1-Sigma) C -K 2133 +/- 53 0 -K 2 +/- 23 Cu-K 549 +/- 37 Cu-L 59 +/- 14 S -K 70 +/- 18 Si-K 45 +/- 11 Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % x,c x,c C -K 2133 1.0000 99.55 99.81 0 -K 1 0.3412 0.02 0.01 S -K 70 0.0825 0.27 0.10 Si-K 45 0.0805 0.17 0.07 Total 100.00 100.00

Energy (kev) Column Take-off angle Acquisition type Creation time Livetime Deadtime Channels Channel width Detector type Window type Window thickness Contamination material Contamination thickness File name : Notes: 3 ^ G> / ^ ^ : HITACHI,GEORGIA TECH : 33 Accelerating voltage 200 : eds Magni f ication 1 : 98/01/22 10:16 Charge 71 : 71 Beam current 1 : 27.719 Beam spot size 0 : 2048 Beam location 0,0 10 Working distance 13.4 Stage X 0 Stage Y 0 0.3 Stage Z 0 Refit / Refit _0 -K" _S -K" _Si-K' _Si-K" Thu Jan 22 10:16:57 1998 none Stage tilt 0 0 Stage rotation 0 Chi-sqd - 2.82 Livetime -71.0 Sec. Standardless Analysis Element Net Error Counts (1-Sigma) C -K 983 +/- 39 0 -K 62 +/- 11 Cu-K 488 +/- 33 Cu-L 9 +/- 11 S -K 56 +/- 8 Si-K 201 +/- 14

** Warning ** Undefined detector subtype. Using default value subtype= 2. Ref it Refit _S -K" _Si-K' _Si-K" Thu Jan 22 10:20:19 1998 Chi-sqd = =3.23 " J Livetime = 71.0 Sec, Standardless Analysis Element Net Error Counts (1-Sigma) C -K 992 +/- 38 Cu-K 488 +/- 33 Cu-L 10 +/- 11 S -K 56 +/- 8 Si-K 201 +/- 14 Adjustment Factors Z-Balance: Shell: K 0.0000 1.0000 L 0.0000 1.0000 M 0.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element C -K S -K Si-K 0 -K Total Counts 992 56 201 K-Rel X,C 1.0000 0.0825 0.0805 K-Std x,c Wt % 96.20 0.45 1.57 1.79 100.00 Atom % Formula Compound% Stoichiometry 97.78 0.17 0.68 1.36 100.00 C S Si02 96.20 0.45 3.36 100.00 1720.347 3. 001 12.000 24.000 Stoichiometry results are based upon 24 Oxygen atoms Table Symbols: S wt.% calculated by Stoichiometry

c Column Take-off angle Acquisition type Creation time Livetime Deadtime Channels Channel width Detector type Window type Window thickness Contamination material Contamination thickness File name : HITACHI,GEORGIA TECH 33 Accelerating voltage 200 eds Magnification 1 98/01/22 10:09 Charge 66 66 Beam current 1 26.104 Beam spot size 0 2048 Beam location 0,0 10 Working distance 13.4 Stage X 0 Stage Y 0 0.3 Stage Z 0 none Stage tilt 0 0 Stage rotation 0 Notes: A^^F Q, \ IAX) Refit.0 -K' «0 0 -K" Refit.Si-K" Thu Jan 22 10:09:36 1998 Chi-sqd - 2.69 Livetime - 66.0 Sec. Standardless Analysis Element Net Error Counts (1-Sigma) C -K 1236 +/- 41 0 -K 16 +/- 11 Cu-K 452 +/- 32 Cu-L 30 +/- 11 S -K 59 +/- 17 Si-K 136 +/- 12

Refit _0 -K' _0 -K" Refit _Si-K" Thu Jan 22 10:09:36 1998 Chi-sqd = 2.69 Livetime = 66.0 Sec Standardless Analysis Element Net Error Counts (1-Sigma) C -K 1236 +/- 41 0 -K 16 +/- 11 Cu-K 452 +/- 32 Cu-L 30 +/- 11 S -K 59 +/- -IX.- Si-K 136 +/- 12 Adjustment Factors K L M Z-Balance: 0.0000 0.0000 0.0000 Shell: 1.0000 1.0000 1.0000 Metallurgical and Biological Thin Section Correction Acceleration Voltage =200 kv Take-off Angle = 33.00 deg Element Counts K-Rel K-Std Wt % Atom % x,c x,c C -K 1235 1.0000 98.31 99.15 0 -K 16 0.3412 0.43 0.33 S -K 59 0.0825 0.39 0.15 Si-K 135 0.0805 0.87 0.37 Total 100.00 100.00