BATTERY CHEMISTRY RESEARCH IN KOKKOLA Jorma Uusitalo PROFESSOR ULLA LASSI 14.11.2013
BATTERY CHEMISTRY RESEARCH IN KOKKOLA Research group Juho Välikangas, M.Sc.(Eng.) Janne Keränen, M.Sc.(Eng.) Toni Kauppinen, B.Sc. (Eng.) Minna Jokinen, M.Sc. (-15.8.2013) Pekka Tanskanen, M.Sc. (Geol.) Siru Tuomaala, M.Sc. (-30.6.2013) Maarit Myllykoski, since 1.9.2013 Tao Hu, D.Sc. (Eng.) Samuli Räsänen, D.Sc. (Freeport) Pekka Tynjälä, D.Sc. (Chem) Ulla Lassi, D.Sc.(Eng.) Preparation of electrode materials Characterization of battery chemicals Recovery of valuable metals -LCO, LFP, LTO, NMC, graphite -Different methods applied -Characterization of physical and chemical properties -Electrochemical testing -Metals recovery from process solutions, battery recycling, catalysts
BATTERY CHEMISTRY RESEARCH IN KOKKOLA Main research areas include Preparation of battery chemicals Characterisation of chemicals Applications
MAIN RESEARCH PROJECTS ON THE TOPIC LITIUM/funded by Tekes and companies, 2008-2010 IMPOLI/funded by Tekes and companies, 2010-2012 Improved properties of lithium ion battery chemicals (with Aalto University) NANOLI/Teknologiateollisuus foundation, 2010-2013 Nanostructured materials for lithium ion batteries NOFALI/Tekes 2012-2014 Novel Electrode Fabrication Methods for Lithium Ion Battery (with Aalto University) LITIUM, 2013-2015 (High-temperature process) for the preparation of Li-ion battery chemicals REMETAL, 2013-2015 Recovery of valuable metals from industrial secondary flows, recycling of batteries and catalysts SCEMAB/Academy of Finland (under evaluation, with University of Eastern Finland) Several projects on-going with industry
BATTERY research laboratory Active electrode material + binder + carbon + solvent Mixing, Determination of slurry properties (e.g. viscosity) Preparation of electrode material Electrode coating on Al (cathode) or Cu (anode) foil Drying Calendering Pressing
BATTERY research laboratory Electrode cutting Testing
Battery testing Battery recycling University Consortium Chydenius First lithium mine in Europe [spodumene] Li-ion battery manufacturing TiO2 & Li4Ti5O12 Battery chemicals Coating of electrodes A! ytisrevnuoala rsyitmehcfonapd End-user of batteries Li-ion battery material research
NOFALI Novel electrode fabrication methods for lithium ion battery 2012-2014 To develop safer, cheaper and environmentally-friendlier materials and processes for Li-ion battery (For large-scale applications) Anode/cathode combination: Li4Ti5O12 / LiFePO4 (Not yet used in commercial applications) Several work packages : (1) anode materials (2) cathode materials (3) binder materials (4) fabrication techniques (5) characterization Commercialization of Sachtleben s LTO anode material and a new water-based printing process for Liion battery manufacturing (Sachtleben, Sunchemical and Walki) To increase battery know-how in Finland (As long-term success in battery production in Finland is NOT possible without basic battery research at universities) To learn from our very top-end foreign collaborators (By sending our PhD students to work in these laboratories for long enough periods)
RESEARCH OF ANODE MATERIALS Li4Ti5O12 Al foil was coated with LTO (84%) slurry Water-based binder was used in the LTO slurry Different electrode thicknesses (wet 150 and 200 µm) were used Some other anodes, such as magnetite* and Ag/Li4Ti5O12** are also studied Tuomaala, Räsänen & Lassi, 2013, unpublished data *NANOLI and IMPOLI projects **In collaboration with prof. Jokiniemi s group Theoretical capacity of LTO is 175 mah/g Half-cells Li/ Li4Ti5O12 Several parallel cells Pouch cells Li4Ti5O12/LCO (results not shown)
RESEARCH OF CATHODE MATERIALS LiFePO4-CNT composites LiFePO4 nanoparticles grown on the MWCNTs array XRD pattern shows orthorhombic LiFePO4 TEM images of LiFePO4-CNT composites Lassi, Hu, Pohjalainen, Kallio, Kordas, Jantunen (2013) Int. J. of Material Science, in press. Hu, Pohjalainen, Lassi, Kallio, Kordas, Jantunen (2011) EICOON Workshop NANOLI (Nanostructured materials for lithium ion batteries) project, 2010-2013
RESEARCH OF CATHODE MATERIALS LiFePO4-CNT composites The charging/discharging curve and specific capacity as a function of cycling for LFP-CNT LiFePO4-MWCNTs composites prepared by coprecipitation Effect of surfactant was also studied Lassi, Hu, Pohjalainen, Kallio, Kordas, Jantunen (2013) Int. J. of Material Science, in press. Hu, Pohjalainen, Lassi, Kallio, Kordas, Jantunen (2011) EICOON Workshop NANOLI project 2010-2013
RESEARCH OF CATHODE MATERIALS Lithium mixed oxides (NMC) NMC M5JU 6000 LiOH 2H LiOH 2H O 2O 2 LiLi 2CO 33 2CO 5000 Lin (Counts) NiNi CoyMn (OH)2 2 x xco z z(oh) ymn Wet Wetgrinding grinding Variable: Variable:Grinding Grindingtime time Dry Drygrinding grinding Variable: Variable:Grinding Grindingtime time 4000 3000 2000 1000 Synthesis Synthesis(high (hightemperature) temperature) Different times and temperatures Different times and temperaturesapplied applied LiNixMnyCozO2 0 15 20 30 40 2-Theta - Scale s. 4e: m i t pe ts - 0 5 0. : pe ts- 0 0. 0 7: d n E- 0 0. 5 1: t ra ts- ed cko l h T / h T 2e: p y T- w a r. U J 5 M M C Ne: l i F t r o p m s I : n o i t a er p O - 2 O ) 3 3. 0 i N 3 3. 0 o C 3 3. 0 n M ( i L - e d i x O e l k c i es N n ag n a M t l a b o C m u i h t i - L ) * ( 7 4 1-0 6 5-0 0 Grinding Grindingand andsieving sieving Screen underflow below Screen underflow below44 44µm µm XRD, XRD,SEM SEM Half cells, Li/Li(Ni Co0,20,2 Mn )O2 2 Half cells, Li/Li(Ni Mn 0,50,5Co 0,30,3)O Pouch Pouchcells cellsli(ni Li(Ni CoMn Mn)O2/graphite )O2/graphite xco x yy zz Juho s slides? Synthesis of Li(NixCoyMnz)O2 Välikangas, Palovaara, Tanskanen, Räsänen, Hu & Lassi, 2013, unpublished data IMPOLI project 2010-2012, LITIUM project 2013-2015 50 60 70
RESEARCH OF CATHODE MATERIALS Li(NixCoyMnz)O2 Materials are tested with three parallel half cells Li/Li(Ni0,5Co0,2Mn0,3)O2 Välikangas, Palovaara, Tanskanen, Räsänen, Hu & Lassi, 2013, unpublished data IMPOLI project 2010-2012, LITIUM project 2013-2015
RESEARCH OF CATHODE MATERIALS Li(NixCoyMnz)O2 Välikangas, Palovaara, Tanskanen, Räsänen, Hu & Lassi, 2013, unpublished data IMPOLI project 2010-2012, LITIUM project 2013-2015 Välikangas, Palovaara, Tanskanen, Räsänen, Hu & Lassi, 2013, unpublished data IMPOLI project 2010-2012, LITIUM project 2013-2015
OPTIMIZATION OF CELL PREPARATION Coin cells and pouch cells Slurry: Composition, NMP concentration, Viscosity, Mixing process, particle size Foil coating: Coating speed, Blade thickness Drying process: Temperature, Time Calendering pressures Assembling of cells Surface and cross section of the LCO cathode
Effects of slurry properties on the electrode coating Variables: - e.g. slurry composition - NMP concentration - viscosity of slurry - mixing process We aimed to have optimal viscosity for the coating process Finally, optimized conditions can be evaluated only based on the results of electrochemical testing (specific capacity, cyclability, rate performance)!!
LITHIUM VALUE CHAIN Mining industry Spodumene Ilmenite Chemical industry Bulk chemicals: Li carbonate TiO2 Co chemicals Zn products Special chemicals: Battery chemicals Catalysts Applications Batteries, Functional surfaces, Catalysts, Other applications Raw minerals Chemical processing Applications Recovery/ Recycling of metals Recycling of batteries Recycling of catalysts Revovery of valuable metals Recycling and reuse Reseach and process development, innovations Keliber OMG (Freeport Cobalt) Nordic Mining Sachtleben Pigments Talvivaara Sun Chemical Cove Resources Boliden Yara Akkuser RecAlkaline Crisolteq Walki Cargotec
Thanks to. Lisätietoja: www.chydenius.fi/yksikot/luonnontieteet Lisätietoja: www.chydenius.fi/yksikot/soveltava-kemia
Thank You for Your attention! Lisätietoja: www.chydenius.fi/yksikot/luonnontieteet Lisätietoja: www.chydenius.fi/yksikot/soveltava-kemia Yhteystiedot: Prof. Ulla Lassi, University of Oulu /Kokkola University Consortium Chydenius, email: ulla.lassi@oulu.fi, Tel: +358 400 294 090