Great Lakes Graphite Full Graphite Flake Analysis

Transcription

1 Great Lakes Graphite Full Graphite Flake Analysis Prepared by: Stephen Klein Coulometrics, LLC. Prepared for: Great Lakes Graphite Date: November 30, 2016

2 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

3 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 (%) % 50x % G x x % % 400x % % 3

4 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 Not enough material after sieving G x100 Not enough material after sieving 100x x x

5 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 Not enough material after sieving G x100 Not enough material after sieving 100x x x N/A N/A N/A 5

6 Great Lakes Graphite Surface Area Analysis 6

7 Great Lakes Graphite As Received, 100x200, 200x400 XRD Data Crystallite size Lc = Å La = Å 7

8 Great Lakes Graphite 400x635, -635 XRD Data Crystallite size Lc = Å La = Å 8

9 : As Received Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G Conductive Carbon SFG 6L Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) Total PVDF 6.1 Electrode Properties Loading: mg/cm 2 Calendered Density: g/cc 9

10 Great Lakes Graphite As Received 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap mah/g Irrev. Cap mah/g Resistance ohm First cycle efficiency % 10

11 : 100x200 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G Conductive Carbon SFG 6L Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) Total PVDF 6.0 Electrode Properties Loading: mg/cm 2 Calendered Density: g/cc 11

12 Great Lakes Graphite 100x200 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap mah/g Irrev. Cap mah/g Resistance ohm First cycle efficiency % 12

13 : 200x400 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G Conductive Carbon SFG 6L Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) Total PVDF 6.1 Electrode Properties Loading: mg/cm 2 Calendered Density: g/cc 13

14 Great Lakes Graphite 200x400 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap mah/g Irrev. Cap mah/g Resistance ohm First cycle efficiency % 14

15 : 400x635 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G Conductive Carbon SFG 6L Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) Total PVDF 6.1 Electrode Properties Loading: mg/cm 2 Calendered Density: g/cc 15

16 Great Lakes Graphite 400x635 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap mah/g Irrev. Cap mah/g Resistance ohm First cycle efficiency % 16

17 : -635 Mesh Electrode Preparation Electrode Mixing Information: Material ID Mass (g) Composition (dry wt%) Active Material G Conductive Carbon SFG 6L Binder Kynar HSV900/NMP (6.1wt% solid PVDF, balance NMP) Total PVDF 6.1 Electrode Properties Loading: mg/cm 2 Calendered Density: g/cc 17

18 Great Lakes Graphite -635 Mesh 1M LiPF 6 in EC/DEC (1:1) Additives: None C/20 cycling Rev. Cap mah/g Irrev. Cap mah/g Resistance ohm First cycle efficiency % 18

19 Great Lakes Graphite Electrochemical Data Summary echem Results ID Rev. Capacity (mah/g) Irrev. Capacity (mah/g) Resistance (ohms) First Cycle Efficiency (%) As Received x x x

20 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 full sized LIBs could then be constructed for accurate performance and life data useful to manufacturers 20