Protected Lithium-Ion Supply Electrode for Oxidation-Stable TEM Analysis
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Solution Overview
Problem
Existing lithium-ion supply electrodes for transmission electron microscopy (TEM) analysis suffer from lithium oxidation due to exposure to air, leading to low lithium-ion conductivity and inaccurate testing conditions, and require expensive liquid holders that are difficult to integrate with sensitive microscopes.
Innovation Solution
A lithium-ion supply electrode with a solid electrolyte layer, a lithium layer, and a protective metal layer is developed, allowing for real-time analysis using a focused ion beam apparatus to prevent lithium oxidation and maintain high conductivity, suitable for use with microscopes sensitive to light and vibration.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If a metal tip is wetted with liquid lithium in a glovebox and loaded into a TEM holder in air, then the electrode can be prepared for TEM analysis, but lithium oxidizes to lithium oxide which has low lithium-ion conductivity causing overvoltage
Solution Approach 1:
The patent applies inert atmosphere by performing the electrode preparation process inside a glovebox filled with inert gas (argon or nitrogen). The metal tip is wetted with liquid lithium and the protective layer is formed in this inert environment, preventing lithium oxidation during the critical preparation phase. This resolves the contradiction by enabling ease of manufacture through controlled inert environment while maintaining reliability by preventing oxidation that would degrade lithium-ion conductivity.
Solution Approach 2:
The patent applies preliminary action by forming the protective layer on the lithium surface immediately after wetting the metal tip with liquid lithium, before the electrode is exposed to air. This preliminary protective coating is deposited while the lithium is still in its fresh, non-oxidized state within the glovebox, creating a barrier that prevents subsequent oxidation during handling and TEM analysis, thus maintaining high lithium-ion conductivity.
2Reliability
If the glovebox is located near the TEM to enable quick loading, then lithium oxidation is prevented, but the TEM cannot be used due to vibrations from the glovebox pump
Solution Approach 1:
The patent applies preliminary action by completing all lithium handling and protective layer formation operations inside the glovebox before transferring the prepared electrode to the TEM holder. The electrode is fully prepared and sealed with its protective layer while still in the inert atmosphere, allowing it to be subsequently handled and loaded into the TEM without requiring the glovebox to be positioned near the microscope, thus eliminating vibration issues while maintaining oxidation prevention.
Solution Approach 2:
The patent applies inert atmosphere by maintaining the lithium in a sealed environment within the glovebox during preparation and protecting it with an inert gas atmosphere. This allows the electrode to be prepared completely within the glovebox without needing immediate transfer to the TEM, enabling the glovebox to be located away from the TEM and avoiding vibration problems while still preventing lithium oxidation through the inert environment.
3Productivity
If a liquid holder is used to provide a liquid environment for real-time charging and discharging tests, then real-time analysis can be performed, but the equipment cost increases and image quality decreases
Solution Approach 1:
The patent applies parameter changes by transitioning from a liquid electrolyte environment to a solid electrolyte environment. This parameter change allows real-time charging and discharging tests to be performed using a solid electrolyte layer that is compatible with vacuum conditions in the TEM. The solid electrolyte maintains ionic conductivity while enabling clear imaging and eliminating the need for expensive liquid holders, thus achieving real-time analysis capability without increased device complexity.
4Productivity
If liquid electrolyte is used on a metal tip for real-time microscopic analysis, then charging and discharging can be tested, but the liquid electrolyte cannot be present in the high vacuum environment and may solidify due to electron beams
Solution Approach 1:
The patent applies parameter changes by changing the physical state of the electrolyte from liquid to solid. The solid electrolyte layer is deposited on the lithium surface while in a liquid state within the glovebox, then cooled to form a solid layer. This solid electrolyte maintains ionic conductivity for real-time charging and discharging testing while being stable in the high vacuum environment of the TEM and resistant to solidification from electron beam exposure, thus resolving the contradiction between productivity and reliability.
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
The electrode enables real-time analysis of lithium secondary battery materials by preventing lithium oxidation and maintaining high conductivity, facilitating structural and interfacial reaction observation without the need for a glove box, thus enhancing testing accuracy and reducing equipment costs.
Implementation Method 1
a solid electrolyte layer including a solid electrolyte
Implementation Method 2
a protective layer formed on the lithium layer and including a metal
Data Source
AI summary
Disclosed are a lithium-ion supply electrode for real-time microscopic analysis and a method of manufacturing same. The lithium-ion supply electrode includes a solid electrolyte layer including a solid electrolyte, a lithium layer formed on the solid electrolyte layer and including lithium, and a protective layer formed on the lithium layer and including a metal. Therefore, lithium in the electrode does not undergo oxidation in a short time. Therefore, the lithium-ion supply electrode can be used for real-time analysis of structural changes and interfacial reactions of lithium secondary battery materials using a transmission electron microscope.