In-situ battery device for soft X-ray microscopic imaging

Abstract

The invention relates to an in-situ battery device for soft X-ray microscopic imaging. The in-situ battery device comprises an upper silicon wafer and a lower silicon wafer, the upper silicon wafer and the lower silicon wafer are respectively provided with an upper observation window and a lower observation window, and two sides of the upper observation window are respectively provided with a liquid extraction and injection port; a liquid pool is formed in the lower silicon wafer, so that the width of the liquid pool is larger than the distance between the two liquid pumping and injecting openings; two electrodes are manufactured on the lower silicon wafer, one ends of the two electrodes are oppositely arranged in the liquid pool and keep a certain gap, the gap is located in the area covered by the view of the upper observation window and the view of the lower observation window, only single-layer electrode particles are reserved after the electrode area in the liquid pool is impressed by the PDMS block, and the other ends of the two electrodes extend out of the liquid pool; and at least one upper through hole and at least one lower through hole are respectively formed in corresponding positions around the upper and lower observation windows. According to the in-situ battery device and the imaging method provided by the invention, the applicability is relatively wide, the single-layer electrode particles are adopted, a relatively large distance exists between the electrode particles under soft X-rays, and accurate high-resolution soft X-ray imaging of the single-layer electrode particles can be realized.

Description

technical field [0001] The invention relates to the field of synchrotron radiation CT imaging and in-situ devices, in particular to an in-situ battery device for soft X-ray microscopic imaging. Background technique [0002] In the field of energy materials, with the explosive growth of portable devices and electric vehicles, the need to develop next-generation batteries with excellent performance and high safety is becoming more and more urgent. The development of such advanced batteries requires the optimization of existing materials, as well as the discovery and utilization of new battery materials with better electrochemical performance. At present, most of the commonly used battery materials are micron-sized particles. During characterization, the mixed information of multi-particle signal superposition will be obtained at the same time, and it is impossible to accurately characterize single particles. In order to elucidate the reaction and degradation mechanism of batt...

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Problems solved by technology

[0003] Although ex situ imaging techniques can provide a lot of valuable information about battery materials, the test results are not necessarily completely accurate because they cannot be tested in a real reaction environment

For example, during the charge-discharge cycle, the non-equilibrium process and the transient process of the reaction, i.e., the mesophase and possibly the metastable phase, are hardly observed

And since the ex situ characterization of a single particle requires disassembly of the battery, it is technically very difficult to track the same particle over multiple repeated charge-discharge cycles.

In addition, due to the high sensitivity of some electrode materials to oxygen and moisture, which may be contaminated, irreversibly changed when handling, transferring samples, these results may mislead the understanding of the reaction and degradation mechanism

[0004] Soft X-ray imaging technology is a non-destructive testing technology with high resolution and strong penetrability. Compared with electron microscopy, soft X-ray has higher penetration ability to electrode particles and electrolyte and less radiation damage. However, when hard X-rays are used to observe single particles with high light element content or small thickness (about 1 micron), the imaging contrast is poor, so the effect of tracking the spatial evolution of the same micron-sized particle and the solid-liquid interface in the liquid not good

[0005] At present, the in situ imaging technology based on soft X-rays is still in its infancy. Due to the limitation of imaging conditions (working distance, ultra-high vacuum, sample stage size, soft X-ray penetration ability, etc.), the in situ imaging technology of micron-sized single particles can be realized. Bit imaging is very difficult

At present, only Lim et al. of Stanford University have designed an in-situ battery device for STXM (scanning transmission X-ray microscope), but the overall device structure is complex; and the processing requirements for microfluidic chips and battery devices are relatively high, and the price is relatively high. expensive

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