Great Lakes Graphite Full Graphite Flake Analysis Prepared by: Stephen Klein Coulometrics, LLC. Prepared for: Great Lakes Graphite Date: November 30, 2016
Great Lakes Graphite Flake Analysis FLAKE ANALYSIS TESTING: Sieve samples to sizes shown in Table below. +50, 50x100, 100x200, 200x400, 400x635, -635 mesh Measure masses to get flake size distribution (Table 1) Tap Density and LOI (Table 2) Measure BET (Table 3) Grind samples to -635 mesh Repeat BET Add BET graph to report with both sieved and sieved/ground BET data Complete XRD Complete ash analysis on materials. Send samples for PIXE Analysis. EChem: Complete slurry, electrodes, coin cells, testing 2
Great Lakes Graphite Sieve Analysis Note: Left out 25g of As Received material. Coulometrics Control # Flake Size (mesh) Particle Size (mm) Mass in Sieve (g) Size Fraction (%) +50 0.300 0 0% 50x100 0.300-0.150 2.02 0.9% G16-0148 100x200 200x400 0.150-0.075 0.074-0.037 22.84 10.2% 98.29 44.2% 400x635 0.037-0.020 65.32 29.4% -635 0.020 34.06 15.3% 3
Great Lakes Graphite Tap & Ash Analysis ID# Flake Size (mesh) Tap Density (g/cc) LOI Ash Content (% carbon) Sample 1 Sample 2 Sample 3 As Received 0.69 94.92 95.14 95.52 +50 Not enough material after sieving G16-0148 50x100 Not enough material after sieving 100x200 0.65 94.42 96.98 97.08 200x400 0.63 96.75 97.51 96.12 400x635 0.58 94.84 94.96 94.83-635 0.55 91.09 91.55 90.91 4
Great Lakes Graphite BET Analysis ID# Flake Size (mesh) Ads. (m 2 /g) BET SA (As Received) BET SA (Grnd to -635) Des. (m 2 /g) Avg. (m 2 /g) Ads. (m 2 /g) Des. (m 2 /g) Avg. (m 2 /g) As Received 3.31 3.69 3.50 4.58 5.23 4.91 +50 Not enough material after sieving G16-0148 50x100 Not enough material after sieving 100x200 2.61 2.55 2.58 5.01 5.00 5.01 200x400 3.00 2.94 2.97 4.81 4.70 4.78 400x635 4.24 4.16 4.20 5.78 5.69 5.72-635 5.15 5.16 5.16 N/A N/A N/A 5
Great Lakes Graphite Surface Area Analysis 6
Great Lakes Graphite As Received, 100x200, 200x400 XRD Data Crystallite size Lc = 189-203 Å La = 190-201 Å 7
Great Lakes Graphite 400x635, -635 XRD Data Crystallite size Lc = 195-286 Å La = 180-203 Å 8
: As Received Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G16-0148 3.07 91.9 Conductive Carbon SFG 6L 0.067 2.0 Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) 0.2031 - Total 0.0124 - PVDF 6.1 Electrode Properties Loading: 12.66 mg/cm 2 Calendered Density: 1.735 g/cc 9
Great Lakes Graphite As Received 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap 344-351 mah/g Irrev. Cap. 40.5-40.8 mah/g Resistance 91.99-93.92 ohm First cycle efficiency 88.5-89.2% 10
: 100x200 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G16-0148 3.52 92.0 Conductive Carbon SFG 6L 0.076 2.0 Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) 0.2294 - Total 0.0139 - PVDF 6.0 Electrode Properties Loading: 12.21 mg/cm 2 Calendered Density: 1.796 g/cc 11
Great Lakes Graphite 100x200 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap 349-351 mah/g Irrev. Cap. 35.0-35.6 mah/g Resistance 105-105.09 ohm First cycle efficiency 89.9-90.9% 12
: 200x400 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G16-0148 3.09 91.9 Conductive Carbon SFG 6L 0.067 2.0 Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) 0.2037 - Total 0.0124 - PVDF 6.1 Electrode Properties Loading: 14.23 mg/cm 2 Calendered Density: 1.714 g/cc 13
Great Lakes Graphite 200x400 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap 350-352 mah/g Irrev. Cap. 33.4-33.7 mah/g Resistance 91.31-102.2 ohm First cycle efficiency 91.0-91.2% 14
: 400x635 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G16-0148 2.50 91.9 Conductive Carbon SFG 6L 0.054 2.0 Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) 0.1671 - Total 0.0101 - PVDF 6.1 Electrode Properties Loading: 11.92 mg/cm 2 Calendered Density: 1.509 g/cc 15
Great Lakes Graphite 400x635 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap 334-355 mah/g Irrev. Cap. 34.5-37.1 mah/g Resistance 83.06-97.73 ohm First cycle efficiency 90.5-90.6% 16
: -635 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G16-0148 3.24 91.9 Conductive Carbon SFG 6L 0.067 2.0 Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) 0.2031 - Total 0.0124 - PVDF 6.1 Electrode Properties Loading: 14.65 mg/cm 2 Calendered Density: 1.776 g/cc 17
Great Lakes Graphite -635 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap 330-338 mah/g Irrev. Cap. 37.6-37.9 mah/g Resistance 95.94-106.95 ohm First cycle efficiency 89.6-89.9% 18
Great Lakes Graphite Electrochemical Data Summary echem Results ID Rev. Capacity (mah/g) Irrev. Capacity (mah/g) Resistance (ohms) First Cycle Efficiency (%) As Received 351 40.5 91.99 89.2 100x200 351 35.0 105.00 90.9 200x400 352 33.4 91.31 91.2 400x635 355 34.5 83.06 90.6-635 338 37.6 95.94 89.9 19
Summary Sample provided is predominantly -100 mesh and was likely screened before shipping. Results show good electrochemical performance of 350 mah/g reversible capacity. Purity drops from 97 to 90% with decreasing flake size. Reversible capacity also drops as a result. Recommendations: Flake should be spheronized and purified for more accurate results 18650 full sized LIBs could then be constructed for accurate performance and life data useful to manufacturers 20