Case study of failure analysis of oxide-based all-solid-state batteries

It has high safety and can be used in various environments! Consistent analysis is possible.

We will introduce a case where a series of analyses, from identifying failure points to cross-sectional observation, was conducted on an oxide-based all-solid-state battery that was destroyed during reliability testing. Heat generation analysis revealed a strong tendency for heat generation on the side, and X-ray transmission observation showed a white linear contrast anomaly near the boundary where heat generation was observed in the X-ray transmission image. It is suspected that some abnormality is occurring in the white line area. When CP cross-sectional SEM observation was performed on the area where the anomaly was visible, layer delamination was observed. It is inferred that delamination occurred between the current collector and electrolyte layers due to the positive (negative) electrode layer expanding and contracting repeatedly during reliability testing. 【Case Overview】 ■ Sample Information: Oxide-based all-solid-state battery that experienced degradation due to charge and discharge testing ■ Heat Generation Analysis Result: A strong tendency for heat generation was observed on the side ■ Other Analysis Contents: - X-ray transmission observation - CP cross-sectional observation and elemental analysis using SEM *For more details, please refer to the PDF document or feel free to contact us.

• Contract Analysis

The purity of the electrolyte greatly affects the performance of the battery! It suppresses the volatility of sulfur components and converts them into a form that can be detected by IC.

We would like to introduce an example of analyzing the purity of phosphorus pentasulfide using ion chromatography for the composition analysis of raw materials for all-solid-state batteries. Phosphorus pentasulfide is one of the raw materials used in the production of electrolytes for sulfide-based all-solid-state batteries. As a pretreatment for IC measurement, the powder of phosphorus pentasulfide was dissolved in alkaline water and converted into phosphate and sulfide salts. Subsequently, sulfide ions were oxidized to sulfate ions to prepare the IC measurement solution. For more details, please refer to the published catalog. 【Solid Electrolytes (Partial)】 ■Li3PS4 ■Li7P3S11 ■Li6PS5Cl ■Li6PS5Br *For more information, please refer to the PDF materials or feel free to contact us.

• Analytical Equipment and Devices

It is possible to perform non-destructive testing from fault location identification to internal observation! High-precision identification of heat generation areas can be achieved.

Thermal analysis is a method for identifying defective areas by detecting heat generated at leak points due to applied voltage using a high-sensitivity InSb camera. By detecting the weak heat generated from shorts and leaks with a high-sensitivity InSb camera, it is possible to non-destructively identify the failure points of electronic components such as semiconductors. Furthermore, non-destructive observation can also be performed using X-ray inspection equipment. 【Features】 ■ Identifying defective areas by detecting heat generated at leak points with a high-sensitivity InSb camera ■ Analyzing samples in a non-destructive state, and also capable of analyzing electronic components that are difficult to analyze with OBIRCH or emission methods ■ Using the lock-in function to acquire phase information allows for high-precision identification of heat generation points *For more details, please refer to the PDF document or feel free to contact us.

• Contract Analysis

Cracks that couldn't be detected visually might be found with X-rays!

When stress such as warping, bending, or twisting is applied to the printed circuit board, cracks may occur inside the MLCC (Multi-Layer Ceramic Chip Capacitor). Additionally, cracks that occur internally are often hidden by the electrodes, making it difficult to detect them from the exterior. In such cases, how about checking with X-rays? [Observation Details] ■ Oblique CT Observation It is possible to perform CT without destroying the printed circuit board, in its original state. ■ Orthogonal CT Observation It is possible to observe the shape of the components in their original state. *For more details, please refer to the PDF document or feel free to contact us.

• Other inspection equipment and devices
• X-ray inspection equipment

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The "Mechanical Stitching Method" by Nichinichisui Road Machinery Co., Ltd. is a new technique that allows for the repair of metal cracks without the application of heat. By using special bolts and reinforcement plates, cracks are physically removed without causing any thermal impact on the base material. Repairs can be made even in environments where open flames cannot be used. Since no heat is applied, the disassembly of equipment is minimized. ◎ For more details, please contact us. ◎ If a detailed technical explanation is needed, please contact us.

The "Mechanical Stitching Method" by Nichinichisui Road Machinery Co., Ltd. is a new technique that allows for the repair of metal cracks without the application of heat. By using special bolts and reinforcement plates, cracks are physically removed, and repairs are made without causing any thermal impact on the base material. Repairs can be carried out even in environments where open flames cannot be used. Since no heat is applied, the disassembly of equipment is minimized. ◎ For more details, please contact us. ◎ If a detailed technical explanation is needed, please contact us.

● This is a leak testing device for small electronic components that does not use fluorinated inert liquids (PFAS-free). ● There is no longer a need for unstable visual confirmation through liquid immersion testing. It adopts a quantitative testing method that allows for stable pressure leak testing. ● It is a tabletop leak testing device specifically for gross leaks, with accuracy equal to or greater than that of liquid immersion testing. ● The detectable range is approximately 1×10⁻² Pa·m³/s to 1×10⁻⁶ Pa·m³/s (varies depending on the target product). ● It is suitable for sealed structures ranging from a few millimeters to a maximum of 80 × 70 mm. Please feel free to contact us for more information!

Fukuda Co., Ltd. has been pursuing leak detection for 60 years and is committed to advancing the future of leak testing. 【 Supporting Various Leak Tests: Air Leak Test / Gas Leak Test (Hydrogen Gas, Helium Gas) 】 We develop, manufacture, and sell leak testing equipment to inspect airtightness and sealing properties. We will propose the appropriate testers and devices for each inspection target. 【 Target Industries and Examples of Inspection Targets 】 - Automotive Industry: Engines, FC components, valves and piping, various parts - Electronic Components Industry: Smartphones, keyless switches, various small sensors - Pharmaceuticals / Food / Cosmetics Industry: Bottle containers, syringes, vials, eye drop containers, pillow packaging, PTP packaging We will propose the most suitable leak testers for each industry. 【 ISO Certification 】JIS Q 9001:2015 (ISO 9001:2015)