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• W3206159519 abstract "In order to meet the increasing need for energy storage systems in consumer devices,electric vehicles and stationary energy storage devices, the existing battery technologiesare constantly being further developed. An important criterion for the performance ofthe battery is its energy density. Even if the cathode accounts mostly for the weight ofa lithium ion battery cell, there is a promising possibility of weight saving on the anodeside by replacing graphite with pure lithium metal. To this end, an electrolyte needs tobe developed that is stable against the potential of the pure metal. Liquid electrolytescannot meet this requirement and also involve safety risks as ammability. Solid-state electrolytes are supposed to enable the use of a lithium-metal electrode.Additionally, due to the scarcity of resources for lithium, sodium-based technologies arebeing developed for use as stationary energy storage devices.Thiophosphates feature the highest ionic conductivities among all solid electrolytes. Inmany cases, amorphous thiophosphates offer even higher conductivities than their crystallineanalogues and their structure can differ, too. A structural investigation of amorphouscompounds may not be possible with a standard X-ray analysis. However theirlocal structure has to be enlightened so that a reproducible synthesis can take place.The solid electrolyte Na2P2S6 was synthesized via ball milling in an amorphous statewith subsequent crystallization. The structure of the crystalline phase differs markedlycompared to the corresponding amorphous phase. A combination of XRD-PDF analysisand 23Na/31P MAS NMR spectroscopy measurements indicate that single PS30-4 tetrahedraand corner-sharing tetrahedra are transformed to edge-sharing-tetrahedra duringcrystallization of amorphous Na2P2S6 to crystalline Na2P2S6. Impedance spectroscopyshows that amorphous Na2P2S6 has a conductivity of 5.710-8 S cm-1 which is threeorders of magnitude higher than crystalline Na2P2S6 (2.6 10-11 S cm-1). The higherconductivity can also be recovered by ball milling crystalline Na2P2S6, inducing a reamorphization.Lithium Lanthanum Zirconium oxide (LLZO) exhibits a high ionic conductivity andstability against lithium metal and is therefore a promising candidate as solid state electrolyte.Yet, specifcations on its conductivity are often not reliable and spread widely.Attempts are made to attribute the differences in reported conductivities to the differentsubstituents, sintering times or surface passivations. A microstructural comparison offour differently substituted samples is performed to elucidate the reasons for the differentconductivities.X-ray diffraction revealed that commercial LLZO samples crystallize in the hydrogarnetstructure (space group No. 220), which is described for the first time with a substituent on Zr and La sites. Ball milling of Al3+, Nb5+, Ta5+ and W6+ substituted LLZO resultsin a phase transformation from the garnet structure into the hydrogarnet structurewith a lower symmetry. The distribution of lithium ions in the hydrogarnet structurediffers from that in the garnet structure which was investigated with 6Li MAS NMR andneutron diffraction. A targeted conversion of the hydrogarnet structure into the garnetstructure is proved by calcining the material at 1100 °C for 10 h. With high-temperatureX-ray diffraction, an low thermal expansion of the hydrogarnet unit cell is observed incomparison to the greater expansion of the garnet unit cell. The ionic mobility of Liions in the hydrogarnet structure is examined by means of NMR, in particular line shapeanalysis, relaxometry and pulsed-field gradient NMR. This combination of techniquesshows that the mobility of lithium is significantly reduced on small length scales. Incombination with the structural analysis, this can be traced back to the high occupancyof the Li3 position in the hydogarnet structure, blocking long-range lithium diffusion.However, it was not possible to access the long-range mobility of Li in the hydrogarnetstructure (at 25 °C).Therefore, the contribution of the ceramic component to the total ionic conductivityof polymer composite electrolytes is evaluated. The question whether the long-rangelithium mobility in the hydrogarnet structure is lower compared to the garnet structureis assessed without the necessity for sintering the LLZO to pellets. Impedance spectroscopyshows a conductivity of 1.2 10-6 S cm-1 for a composite electrolyte with ahydrogarnet structure and 3.4 10-6 S cm-1 for a composite electrolyte with a garnetstructure. The higher Li mobility of the garnet-based composite electrolyte comparedto the hydrogarnet-based electrolyte is verified with PFG-NMR measurements of thediffusion coeffcient: 6.1 10-14 m2 s-1 (garnet), resp. 1.1 10-14 m2 s-1 (hydrogarnet).The measured activation energy of dffusion is also higher in the hydrogarnet composite.The conductivity results measured with impedance spectroscopy are compared withcommercial composite electrolytes; a SiO2-ceramic-polymer and a purely polymer-basedelectrolyte.The next step from optimizing a solid state electrolyte in terms of ionic conductivity isto look at its compatibility with the electrodes, here the cathode. It is tested whetherball milling of LLZO with the established cathode material Lithium Nickel Cobalt Manganeseoxide (NCM) results in a good contact of the two materials and consequently alow Li ion diffusion barrier.The interface between LLZO and NCM is investigated by X-ray diffraction, 6Li MASNMR and transmission electron microscopy. A model system consisting of LLZO andNCM is characterized with impedance spectroscopy for a lithium diffusion barrier sandwichedbetween an auxiliary electrolyte in order to separate the ionic conductivity fromthe electrical. An evaluation of only the ionic conductivity apart from the electricalconductivity is not possible due to the high electrical conductivity of the auxiliary electrolyte.The electrolyte Lithium Aluminum Titanium Phosphate (LATP) is examined crystallographicallyagainst the background of upscaling of the synthesis. If the process isupscaled, local inhomogeneities of the educts can be expected in a way that varyingeduct contents have an effect on the product. This applies especially to phosphoric acid,the concentration of which cannot be specified precisely due to its hygroscopy. A Rietveldrefinement analysis against X-ray diffraction data of LATP with varying phosphoric acidcontent during synthesis is performed. An excess of phosphoric acid leads to the formationof AlPO4, which impedes the ionic conductivity. Insufficient phosphoric acid causesthe formation LiTiOPO4. TiO2 is formed in this material after a second sintering step.The findings in this work contribute the understanding of structural changes in solidelectrolytes during processing and thus contribute to the improvement of future solidstatebatteries." @default.
• W3206159519 created "2021-10-25" @default.
• W3206159519 creator A5002107081 @default.
• W3206159519 date "2021-01-01" @default.
• W3206159519 modified "2023-09-23" @default.
• W3206159519 title "Microstructural characterization and multiscale ionic conductivity in lithium and sodium-based solid state electrolytes" @default.
• W3206159519 doi "https://doi.org/10.5445/ir/1000133273" @default.
• W3206159519 hasPublicationYear "2021" @default.
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