The Lithium Ion Conductive Glass Ceramics (EQ-CGCS) i) Main Feature ii) General Properties iii) Composition & Structure iv) Manufacturing Process

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1 Lithium Ion Conductive Glass Ceramics: Properties and Application in Lithium Metal Batteries MTI Corp. 860 South 9th St., CA

2 Lithium Ion Conductive Glass Ceramics: Properties and Application in Lithium Metal Batteries The Lithium Ion Conductive Glass Ceramics (EQ-CGCS) i) Main Feature ii) General Properties iii) Composition & Structure iv) Manufacturing Process 2

3 - Glass & Gllass-ceramics Composition Engineering Expertise - Homogeneous Glass production know-how - Precision Metrology technologies - Precision Plano Plano Grinding / Polishing & Cleaning technologies - Precision Cleaning technologies for Glass substrates 3

4 - Glass-ceramics Technology - Composition / Structure: Nono-scale aggregates of poly-crystalline particles are dispersed among amorphous glass matrix In t e n c it y /A.U. 100nm θ/ - Benefits: Added properties (values) to the original glass, with Improved Mechanical Strength and Processability dl/l ( x ) SiO2 Glass Ultra Low Expansion Glass Temperature (degree C) *at OHARA Measurement 2mm 4

5 - Glass-ceramics, to have isotropically dispersed Lithium-Ion Conductive Crystal particles and an amorphous glass phase 0 - Features -> Top level Ionic Conductivity among Inorganic Materials (In the order of 10-4 S/cm at RT) -> Thermally Stable up to 600, Nonflammable. -> Can be Handled in Air. -> No Through Hole (No H 2 O Penetration) Lo g σ(scm -1 ) /T (K -1 ) The Arrhenius plot (Original Powder Material) 7

6 Presently the supply of EQ-CGCS is basically concentrated in membrane form. melted & polished plates Li 2 O-Al 2 O 3 -SiO 2 -P 2 O 5 -TiO 2 -GeO 2 Conductivity : ~ 1 x 10-4 S/cm at 25 C Proved seawater stability (>2 years*) Membrane in Dia.2 x250um thickness

7 Main Feature (Where does EQ-CGCS positions in Lithium-Ion Conductive Inorganic Materials?) (Original Powder Material) 0 LISICON (Li ZnGe O ) Li β-alumina (Li 2 O 11Al 2 O 3, Line Data) (Membrane) Logσ (Scm -1 ) LiI (Single Crystal) T=727 T=394 T=227 T=127 T=60 T= /T (K -1 ) β-lialsio 4 L 2 S-P 2 S 5 (Point Data) Li 1.5 Al 0.3 Ti 1.7 P 3 O 12 Li 3.5 V 0.5 Ge 0.5 O 4 Li 2 Ti 3 O 7 Li 3 N (Powder) 9

8 Thermally Stable up to 600 Thermogravimetry TG /% No Weight Change is detected at heating to 600. No Exothermal Reaction is detected at heating to 600. Measured up to 600 in Air Differential Thermal Analysis DTA /(uv/mg) exo Temperature / C Nonflammable, Can be Handled in Air. Stable against Flame Stable in Water

9 Blocking moisture penetration (Moisture Permeability Measurement) 6.00 Moisture permiability (g m -2 -day) Mocon Permatran 3/ Time(hour)

10 ii) General Properties Chemical Properties Mechanical Properties Water Resistance in Powder form (RW(P) in JOGIS Class) Class 1 Acid Resistance in Powder form (RW(P) in JOGIS Class) Class 1 4 Point Bending Strength 140N/mm 2 Knoop Hardness (Hk) 590 Specific Gravity 3.05 Thermal Properties Coefficient of Thermal Expansion 94 x 10-7 /degree C (30 ~ 350degree C) 82 x 10-7 /degree C (350 ~ 600degree C)

11 iii) Composition & Structure Main Crystal Phase: Li 1+x Al x Ge y Ti 2-x-y P 3 O 12 (NASICON type crystals) Sub Crystal Phase: Li 1+x+3z Al x (Ge,Ti) 2-x (Si z PO 4 ) 3 (NASICON type crystals) Li 1+x+3z Al x (Ti,Ge) 2-x Si 3z P 3-z O 12 Sub Crystal Phase: AlPO 4

12 iii) Composition & Structure - X-Ray Diffraction 2000 (113) LiTi 2 P 3 O 12 Intenstity(counts) (014) (024) AlPO (012) (116) (300) (211) (223) (134) (042) (2110) (410) (202) (137) (312) ( 220) (0012) θ Cu Kα

13 iii) Composition & Structure - TEM & EDX Li 1+x Al x Ge y Ti 2-x-y P 3 O 12 AlPO 4 Li 1+x+3z Al x (Ge,Ti) 2-x (Si z PO 4 ) 3

14 iii) Composition & Structure - Microstructure & Compositional distribution Observations by Low Acceleration Scanning Microscope for the cross-section of EQ-CGCS plate Secondary Electron Imaging (SEI, x20k) Backscattered Electron Imaging (BEI, x20k) AlPO 4 (Dark Grey Spot) Li 1+x Al x Ge y Ti 2-x-y P 3 O 12 (Light Grey Back Ground) Li 1+x+3z Al x (Ge,Ti) 2-x (Si z PO 4 ) 3 (White Spot)

15 iii) Composition & Structure - Li Ion Conduction Mechanism in the material: Vacancy Diffusion (Ti,Ge)O 6 PO 4 (Ti,Ge)O 6 C-axis Li(filled) Li(vacancy)

16 iii) Composition & Structure Complex Impedance plot for EQ-CGCS (Original Powder Material) Rb: Attributed to Grain Boundary Rg: Attributed to Bulk of Grain

17 iv) Manufacturing Process Mixing Raw Materials (Li 2 CO 3, Al(PO 3 ) 3, SiO 2, H 3 PO 4, TiO 2, GeO 2 ) Melting Glass Drawing & Forming Crystallization Mechanical Processing Lithium-Ion Conductive Glass-ceramics *Efficient mfg Process (Tape Cast & Sintered Plating) is now under development. The process realize a near-net shape and yields lesser removal

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