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Electrochemical analysis in-situ cell for X-ray diffraction and testing method

A technology of electrochemical analysis and in-situ cell, which is applied in the direction of material analysis, measuring electricity, and measuring devices using radiation diffraction. It can solve the problems of crystal structure changes and difficulties in real-time detection, and achieve low cost, good airtightness, and enhanced signal. The effect of intensity

Inactive Publication Date: 2015-05-06
PULEAD TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using this in-situ cell, the X-beam generated by the X-ray diffractometer passes through the beryllium window to detect and analyze the crystal structure of the positive electrode material in real time, effectively solving the problem that the crystal structure change of the battery material is difficult to detect in real time during the charging and discharging process. question

Method used

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  • Electrochemical analysis in-situ cell for X-ray diffraction and testing method
  • Electrochemical analysis in-situ cell for X-ray diffraction and testing method
  • Electrochemical analysis in-situ cell for X-ray diffraction and testing method

Examples

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Effect test

specific Embodiment 1

[0030] Specific embodiment 1: study LiFePO 4 Phase transition of battery materials during charge and discharge

[0031] Assembling the battery steps: first fix the Be plate, turn the in-situ cell upside down, and put LiFePO on the beryllium window 4 Cathode pole piece, diaphragm, counter electrode piece, electrolyte solution, counter electrode column, and insulated tweezers are used to prevent short circuit of the in-situ cell. During the assembly process, pay attention to the subassembly sequence.

[0032] Place the in-situ cell on the sample stage of the X-ray powder diffractometer and connect the electrodes and counter electrode leads. The start-up conditions of the in-situ cell: charge and discharge according to the corresponding rate respectively, and collect points after discharging, and the battery is static for 7 minutes during the point collection process. X-ray powder diffractometer test conditions: Cu target, voltage 40Kv, current 40mA, scanning range: 28-42°, sc...

specific Embodiment 2

[0034] Specific Example 2: Studying the phase transition of three-element battery materials in the charging and discharging process

[0035] The start-up conditions of the in-situ cell: charge and discharge at 0.2C, charge and discharge to the corresponding voltage, stand still for 17 minutes, and test. X-ray powder diffractometer test conditions: Cu target, voltage 40Kv, current 40mA, scanning range: 35-70°, scanning rate: 2° / min, using automatic sampling programming software, sampling points every 45 minutes, sampling time It is 17min.

[0036] The data tested above is to use the in situ cell test to study the phase transition of NCM battery materials during the charging and discharging process. The test results are as follows: Figure 4As shown, the results show that NCM can realize the reversible transformation of the crystal phase. During the charging process, the H1 phase gradually transforms into the H2 phase, and when the voltage is 4.5V, the H3 phase begins to appear...

specific Embodiment 3

[0037] Specific embodiment 3: Study the phase transition of high voltage LCO battery material charge and discharge process

[0038] The start-up conditions of the in-situ cell: charge and discharge at 0.2C, charge to the corresponding voltage and rest for 17 minutes. X-ray powder diffractometer test conditions: Cu target, voltage 40Kv, current 40mA, scanning range: 35-70°, scanning rate: 2° / min, using automatic sampling programming software, sampling points every 45 minutes, sampling time It is 17min.

[0039] The data tested above is to use the in-situ cell test to study the phase transition of LCO battery materials during high-voltage charging and discharging. The test results are as follows: Figure 5 As shown, the results show that when the voltage is higher than 4.5V, the LCO material will appear O1a and O1 crystal phases during the charging process, and the appearance of these crystal phases is not conducive to the layered structure of the material. The phase has compl...

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Abstract

The invention relates to an electrochemical analysis in-situ cell for X-ray diffraction and a testing method. The combination of an X-ray diffractometer and a battery charging / discharging tester can be realized. The in-situ cell comprises an upper flange and a lower flange which are fixedly connected together, a cavity formed in the middle of the lower flange, a counter electrode column extending into the cavity, and a positioning device connected with the counter electrode column; a hole is formed in the middle of the upper flange; a beryllium sheet covers the hole to form a beryllium window; an electrode slice, a diaphragm and a counter electrode slice are arranged in the cavity; the upper flange is connected with an electrode lead; the counter electrode column is connected with a counter electrode lead. According to the electrochemical analysis in-situ cell, the X-beam generated by the X-ray diffractometer passes through the beryllium window to detect and analyze the crystal structure of a positive electrode material in real time, and therefore, the problem of difficult real-time detection on the change of the crystal structure in the charging and discharging process of the battery material is effectively solved; the electrochemical analysis in-situ cell is ingenious in design, simple to operate, and low in cost.

Description

technical field [0001] This technology belongs to the in-situ X-ray diffraction analysis and testing technology of lithium-ion batteries, and is especially suitable for studying the crystal structure changes of positive and negative electrode materials during the charging and discharging process of lithium-ion batteries. This device is an indispensable device for studying the performance of lithium-ion batteries. Background technique [0002] People's demand for mobile electronic devices is getting higher and higher, and lithium-ion batteries are required to have higher capacity, long life, and high safety. Therefore, it is imperative to continuously improve the level of analysis and testing technology for research on lithium-ion batteries. It is well known that X-ray diffractometer can analyze the crystal structure of materials and analyze the properties of materials from the atomic structure level. Lithium-ion battery charge and discharge tester is one of the key equipment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/20G01R31/36
Inventor 庞占永姜晓瑞周恒辉
Owner PULEAD TECH IND
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