Method and sample shelf for X-ray diffraction in-situ test

An in-situ test and X-ray technology, applied in the preparation of test samples, material analysis using radiation diffraction, etc., can solve the problems of electrolyte volatilization, single electrode active material, etc., and achieve simple processing, easy acquisition, and easy Achieved effect

Active Publication Date: 2012-05-02
DONGGUAN AMPEREX TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both ZL200610025206.5 and ZL200820239263.8 proposed an X-ray diffraction in-situ test device with an open hole structure, but the sealing methods are all mechanical seals with sealing rings or inert gas protection, which can realize long-term charge-discharge in-situ test in the air Under such circumstances, there is a hidden danger of electrolyte volatilization
And the above-mentioned in-situ test device can only obtain the in-situ X-ray diffraction spectrum of a single electrode active material on the basis of one-time sample preparation

Method used

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  • Method and sample shelf for X-ray diffraction in-situ test
  • Method and sample shelf for X-ray diffraction in-situ test
  • Method and sample shelf for X-ray diffraction in-situ test

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] According to the above method, the processing is completed to manufacture the X-ray diffraction in-situ test sample holder. Make a slurry with LiNi0.33Mn0.33Co0.33O2 as the cathode active material and natural graphite as the anode active material, and apply the slurry on the aluminum foil with a porosity of 40% and the copper foil with a porosity of 35% according to the above method, and roll Made into pole pieces. Cut the cathode pole piece into small pieces of 33mm*48mm, cut the anode pole piece into small pieces of 34mm*50mm, and keep the tabs. Cut the isolation film into a small piece of 36mm*52mm, stack the above three, and fix it with positioning glue. Wrap the prepared bare cell with 0.025mm polyethylene film, seal the top and one side, inject electrolyte, and vacuum seal the other side after standing for 1 hour. Use a small current such as 0.5mA to charge the battery for the first time and form it. If there is gas that affects the flatness of the surface of t...

Embodiment 2

[0034] According to the above method, the processing is completed to manufacture the X-ray diffraction in-situ test sample holder. Made with LiCoO 2 As the cathode active material, use natural graphite as the slurry of the anode active material, and apply it on the aluminum foil with a porosity of 50% and the copper foil with a porosity of 30% according to the above method, and then roll it into a pole piece . Cut the cathode pole piece into small pieces of Ф = 10mm, cut the anode pole piece into small pieces of Ф = 12mm, and keep the tabs. Cut the isolation film into a small piece of Ф=16mm, stack the above three, and fix it with positioning glue. Wrap the prepared bare cell with a 0.040mm polypropylene film, seal the top and one side of the packaging area 7, inject electrolyte, and vacuum seal the other side after standing for 1 hour. Use a small current such as 0.1mA to charge the battery for the first time and form it. If there is gas that affects the flatness of the s...

Embodiment 3

[0036] According to the above method, the processing is completed to manufacture the X-ray diffraction in-situ test sample holder. Make a slurry with graphite as the active material of the electrode to be tested, and apply it on copper foil with a porosity of 60% according to the above method, and then roll it into a pole piece, and cut it into Ф = 10mm Small pieces, keep the tabs 10. Using a metal lithium sheet as a reference electrode, cut it into small pieces with Ф=12mm, and press them tightly with the tab 10. Cut the isolation film 11 into a small piece with Ф=16mm, stack the above three, and fix it with positioning glue. Wrap the prepared bare cell with a 0.1mm polystyrene film, seal the top and one side of the packaging area 7, and inject electrolyte, and then vacuum-seal the other side after standing for 1 hour, and pass Clamping and standing improves the flatness of the surface. Clamp the reshaped battery cell test side up on the charging and discharging test chann...

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Abstract

The invention relates to the field of a test method and a test device and particularly relates to a sample shelf and a test method for an X-ray diffraction in-situ test. The sample shelf comprises a sample shelf base frame with a sample slot, a positioning plate, a charge-discharge test channel and a conducting wire, wherein the positioning plate is jointed on the sample shelf base frame; the charge-discharge test channel is riveted on the sample shelf base frame; and the conducting wire is welded on the charge-discharge test channel. In the sample shelf provided by the invention, an X-ray powder diffractometer is free from any structural reformation or an operation of adding a functional component, and a polymeric membrane material, which is environmentally-friendly, non-toxic, easily obtained and simply processed, is used as an X-ray transmission window as well as a packaging material of a sample core, thereby realizing the observation and monitoring for crystal structural change of a cathode active material and an anode active material under different voltages during a charge-discharge process and a process of repeating for different times on the basis of preparing the sample core for the X-ray diffraction in-situ test.

Description

technical field [0001] The present invention relates to the field of testing equipment and testing methods, in particular to a testing method and device for in-situ testing of X-ray diffraction, in particular to an X-ray diffraction test of a lithium-ion battery under different voltages during charging and discharging and during different cycles. Test method and sample holder for in-situ testing. Background technique [0002] With the miniaturization and thinning of mobile devices such as mobile phones, digital cameras, notebook computers and portable DVDs, the market demand for mobile energy is increasing. attention. Not only in the consumer electronics market with strong demand for energy density, but also in the green and clean energy market represented by electric vehicles and energy storage power stations, lithium-ion battery products have more stable performance and longer life. Therefore, the development and research of lithium-ion battery electrode material systems...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/20G01N1/28
Inventor 吴梦尧郭佳丽
Owner DONGGUAN AMPEREX TECH
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