CN115143893A - Method for detecting internal strain in-situ of solid-state lithium battery through fiber grating sensor - Google Patents

Method for detecting internal strain in-situ of solid-state lithium battery through fiber grating sensor Download PDF

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Publication number
CN115143893A
CN115143893A CN202210677985.6A CN202210677985A CN115143893A CN 115143893 A CN115143893 A CN 115143893A CN 202210677985 A CN202210677985 A CN 202210677985A CN 115143893 A CN115143893 A CN 115143893A
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battery
solid
fiber
grating sensor
lithium metal
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朱孔军
郭君
吴奇
武猛
梁彭花
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Nanjing University of Aeronautics and Astronautics
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Nanjing University of Aeronautics and Astronautics
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/16—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge
    • G01B11/18—Measuring arrangements characterised by the use of optical techniques for measuring the deformation in a solid, e.g. optical strain gauge using photoelastic elements
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses an in-situ detection system for internal strain of a solid-state lithium metal battery, which comprises a fiber bragg grating demodulator, a fiber bragg grating sensor and a data analysis module, wherein the fiber bragg grating sensor is embedded into the solid-state lithium metal battery, and the solid-state lithium metal battery is connected with a blue charging system and an electrochemical workstation for relevant tests. The invention provides a method for decoupling the relation between the electrochemical behavior in the solid lithium metal battery and the strain of an electrode material by adopting an optical fiber grating sensor for the first time, and the strain in-situ detection is realized by acquiring strain information and tracking the expansion condition of the internal volume of the battery through an embedded optical fiber sensor. Provides a technical means for deeply exploring the mechanical properties of each electrode material, has important significance for further selecting high-performance electrode materials, and has application value of battery safety detection. Meanwhile, the fiber grating sensor can realize the on-line remote detection of the sensor on multiple objects and parameters, and is convenient for forming a multi-form intelligent fiber sensing network.

Description

Method for detecting internal strain in-situ of solid-state lithium battery through fiber grating sensor
Technical Field
The invention belongs to the field of lithium battery detection, and particularly relates to a method for detecting internal strain in situ of a solid-state lithium battery through a fiber grating sensor.
Background
All materials in the solid-state lithium metal battery use solid materials and do not contain liquid. Compared with liquid lithium ion battery, it has good safety performance and high energy density (specific energy)>500Wh/kg, energy density>1500 Wh/L) and long cycle life. The development of the solid lithium metal battery has important significance for the popularization and the application of electric automobiles, and can also actively promote the development of the short-distance electric aviation industry. However, the interface problem between the solid electrolyte and each electrode in the solid-state lithium metal battery includes: the interface resistance between the electrode and the electrolyte is large, the interface compatibility is poor, and the reaction between the lithium metal cathode and the electrolyte is not solved at present. And Li under the charge-discharge cycle conditions + The uneven deposition and stripping of the lithium-ion battery can cause volume expansion of electrode materials and growth of lithium dendrites, and the stress of a negative electrode is increased sharply and irreversible volume expansion and volume continuous change occur due to the formation of porous lithium and dead lithium, so that the cycle life of the battery is greatly influenced. At the present stage, the conventional sensor used for detecting the internal strain of the battery, such as a strain gauge, has a large influence on the chemical performance of the battery after being embedded in the battery due to a large volume, so that in-situ detection is difficult to realize. Often, a detection method which is tightly attached to the surface is adopted, the strain in the battery is difficult to detect quickly and accurately, detection dimensionality needs to be expanded urgently, and a new online detection method for the solid-state lithium metal battery is provided.
Disclosure of Invention
The invention aims to: the invention aims to provide an in-situ detection method for internal strain of a solid lithium metal battery of an implanted fiber grating sensor, and aims to solve the problem that the internal strain of the solid lithium metal battery is difficult to detect in situ.
The technical scheme is as follows: the invention discloses a method for detecting internal strain in-situ of a solid-state lithium battery through a fiber grating sensor, which comprises the following steps:
step 1, presetting a detection system and a solid lithium metal battery, wherein the detection system comprises a fiber grating demodulator, a fiber grating sensor and a data analysis module;
step 2, drilling a hole at one side of a stainless steel positive electrode shell of the solid-state lithium metal battery, and embedding a metal capillary in the hole;
step 3, penetrating through the metal capillary tube to implant the fiber bragg grating sensor into the middle of a positive plate and a gasket of the solid-state lithium metal battery in parallel;
step 4, sequentially assembling the components of the solid-state lithium metal battery in a glove box;
and 5, packaging the battery by using a small-sized hydraulic button battery sealing machine, sealing the drilled hole by using epoxy resin, solidifying the battery for 12-24 hours in a glove box, taking out the battery, connecting the battery with a blue charging system and an electrochemical workstation for testing, connecting bare optical fibers outside the solid-state lithium metal battery with the input end of an optical fiber grating demodulator, converting the change of the acquired optical signals into electric signals by the optical fiber grating demodulator, and analyzing and processing the data by a data processing module.
Further, in step 1, the Fiber Bragg Grating sensor is a Fiber Bragg Grating (FBG) sensor, and includes a Fiber Bragg Grating region, a Fiber coating layer, and a Fiber core.
Further, in step 1, the solid-state lithium metal battery is a CR2032 button battery.
Further, in step 2, the diameter of the drilled hole is 200-300 μm.
Further, in step 2, the metal capillary has a length of 5-10mm and an inner diameter of 300-500 μm.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
(1) According to the invention, the fiber bragg grating sensor is embedded into the solid-state lithium metal battery, so that the accurate measurement of the internal strain of the lithium metal battery is realized. The anode of the solid lithium metal battery is in solid-solid contact with the traditional solid polymer electrolyte at room temperature, so that the ion transmission is limited, the testing environment of the solid lithium metal battery is usually a high-temperature environment at present, and the fiber grating sensor provided by the invention has the advantages of small volume, corrosion resistance and easiness in embedding into the battery. According to the technical scheme provided by the invention, the fiber bragg grating sensor is implanted into the solid-state lithium metal battery for strain measurement, so that the accurate measurement of the internal strain behavior of the solid-state lithium metal battery is realized, and experimental verification is carried out on the internal strain behavior; electrolyte does not exist in the solid-state lithium metal battery, and the corrosion influence of the electrolyte on the fiber grating sensor does not need to be considered; the influence on the cycle performance of the lithium metal battery is small after the lithium metal battery is implanted, and the fiber grating sensor can be cycled for 100 circles after being implanted into the solid-state lithium metal battery in the early-stage test.
(2) Compared with the traditional sensor, the fiber grating sensor uses light as a carrier of sensitive information, adopts optical fiber as a medium for transmitting the sensitive information, and has the characteristic of optical measurement. The battery has less influence on the performance of the battery after being embedded due to the small volume. The high-sensitivity electromagnetic interference-resistant high-voltage power supply has the advantages of good electrical insulation performance, strong electromagnetic interference resistance, high sensitivity, easiness in realizing remote monitoring of a detected signal, convenience in connection with a computer and the like.
Drawings
FIG. 1 is a system for detecting internal strain in a solid state lithium metal battery;
FIG. 2 shows the specific position of the fiber grating sensor;
FIG. 3 is a diagram of a fiber Bragg grating sensor structure;
FIG. 4 is a curve of impedance change after a solid-state lithium metal battery is embedded in a fiber grating sensor;
FIG. 5 is a graph of the change in capacity of a solid-state lithium metal battery 80 cycles before cycling;
fig. 6 is a strain variation curve of the solid-state lithium metal battery during charge and discharge cycles.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
The FBG sensor is a fiber grating sensor with the highest use frequency and the widest use range. When the grating is subjected to an external physical field (such as strain, temperature and the like), the grating pitch of the grating area is changed, so that the wavelength of the reflection spectrum is changed. And determining the change of the corresponding physical quantity of the part to be detected according to the difference value of the wavelength change. Of all the external factors that cause wavelength shift of the grating, the most direct parameters are temperature and strain. The invention selects the environment of 60 ℃ for detection. Therefore, the heat generated by the internal material of the battery is not considered in the test process, the fiber grating sensor is not packaged, and only the strain is considered to be the parameter causing the central wavelength change of the fiber grating sensor.
The present embodiment provides a system for measuring internal strain of a solid-state lithium metal battery, as shown in fig. 1, including: the system comprises an electrochemical workstation or battery testing system 1, a solid-state lithium metal battery 2, a fiber grating sensor 3, a fiber grating demodulator 4 and a data processing module 5. And the battery testing system and the electrochemical workstation 1 are used for carrying out charge-discharge cycle testing on the solid-state lithium metal battery, the bare fiber outside the solid-state lithium metal battery 2 is connected with the input end of the fiber grating demodulator 4, and the demodulator 4 converts the change of the acquired optical signal into an electric signal. And finally, the data processing module 5 is adopted to analyze and process the data.
Since the fiber bragg grating sensor 3 is embedded in the solid-state lithium metal battery 2 and is introduced by foreign matters, different implantation positions of the sensors can affect the performance of the battery. In order to avoid the influence of the implantation of the fiber grating sensor 3 on the activity of the electrode material, the fiber grating region is fixed inside the solid-state lithium metal battery (between the stainless steel gasket 10 and the anode shell 11) through a previous-stage correlation test, and the electrochemical cycle performance of the battery is stable when the sensor is at the position. Meanwhile, referring to fig. 5, the fiber bragg grating sensor 3 is implanted, the solid-state lithium metal battery 2 circulates at a certain charge-discharge rate, and the capacity attenuation is small, so that the detection method has certain feasibility.
The original state of the solid-state lithium metal battery to be measured in this embodiment is a state without charge-discharge cycles. The solid-state lithium metal battery used in the present invention, see fig. 2, includes: a stainless steel negative electrode shell 6, a lithium metal sheet 7, a Polyethylene oxide (PEO) based solid electrolyte 8, a positive electrode material 9, a stainless steel gasket 10, a positive electrode shell 11, a fiber grating sensor 12, a sensor implantation hole 13 and a capillary tube 14. The solid-state lithium metal battery is selected in the embodiment, and V is used 6 O 13 Is a positive electrode material and is a positive electrode material,the lithium sheet is a negative electrode material, and PEO-based polyvinylidene fluoride (Poly (1,1-difluoroethylene), PVDF) is a solid electrolyte. The specific structure of the fiber grating sensor is shown in fig. 3, which includes: a fiber grating region 15, a fiber coating layer 16 and a fiber core 17. The sensor 3 is implanted in the middle of the positive plate 9 and the gasket 10 in parallel through the hole 13 and the capillary 14, and because no active substance exists in the position, the influence of the implantation position of the fiber grating sensor 3 on the performance of the battery is minimum, and when the volume expansion occurs in the battery, the sensor 3 can also quickly detect the internal strain condition of the battery. After the fiber bragg grating sensor is fixed, the bare optical fiber is led out of the lithium metal battery shell, and in order to prevent the optical fiber from being broken due to friction and shearing in the operation process, the metal capillary 14 and the optical fiber coating layer 16 can improve the mechanical strength of the optical fiber. The drilled hole 13 is encapsulated with epoxy resin in a glove box and cured for a certain time, and then the solid-state lithium metal battery 2 is taken out for a relevant test.
First, the electrochemical workstation 1 was used to test its impedance change, see fig. 4, for a high temperature test (constant temperature in the incubator of 60 ℃). Compared with the battery without the fiber bragg grating sensor 3, the battery impedance change after the fiber bragg grating sensor is embedded is small, which shows that the influence of the implantation of the fiber bragg grating sensor on the battery performance change is small, and the impedance is only increased by 9.5 omega. Next, the solid-state lithium metal battery 2 was subjected to a plurality of charge-discharge cycle tests using the battery test system 1. The grating demodulator 4 is a detection instrument for real-time measurement of the central wavelength of a sensitive element in various FBG sensors, and the main principle is as follows: lambda [ alpha ] B ＝2n eff And Λ. Wherein n is eff Is the effective refractive index of the fiber core, and Λ is the period of the fiber grating. When the environmental temperature, strain or other physical quantity of the fiber grating changes, the period or fiber core refractive index of the grating changes, so that the central wavelength of the reflected light shifts, and the central wavelength of the reflected light changes before and after the central wavelength changes (delta lambda) B ) And analyzing to obtain the change condition of the physical quantity to be measured. Finally, referring to fig. 6, after the fiber grating sensor is implanted into the solid-state lithium metal battery, the strain and charge-discharge chemistry inside the battery are performed under certain cycle conditionsIn order to have certain relation, the two curves have similar changing trends. The invention detects the internal strain behavior of the battery through the optical sensor, provides the possibility of researching the correlation between the electrochemical behavior and the internal strain behavior of the battery in the charging and discharging processes, and can deeply analyze the mechanical failure problems of the solid lithium battery in the charging and discharging processes, including the cracking/breaking of electrode materials/solid electrolytes, the contact loss of the electrodes and the electrolytes, the short circuit of the battery caused by the growth of lithium dendrites, and the like.

Claims (5)

1. A method for detecting internal strain in situ of a solid-state lithium battery through a fiber grating sensor is characterized by comprising the following steps:
step 1, presetting a detection system and a solid lithium metal battery, wherein the detection system comprises a fiber grating demodulator, a fiber grating sensor and a data analysis module;
step 2, drilling a hole at one side of a stainless steel positive electrode shell of the solid-state lithium metal battery, and embedding a metal capillary tube into the hole;
step 3, penetrating through the metal capillary tube to implant the fiber bragg grating sensor into the middle of a positive plate and a gasket of the solid-state lithium metal battery in parallel;
step 4, sequentially assembling the components of the solid-state lithium metal battery in a glove box;
and 5, packaging the battery by using a small-sized hydraulic button battery sealing machine, sealing the drilled hole by using epoxy resin, solidifying the battery for 12-24 hours in a glove box, taking out the battery, connecting the battery with a blue charging system and an electrochemical workstation for testing, connecting bare optical fibers outside the solid-state lithium metal battery with the input end of an optical fiber grating demodulator, converting the change of the acquired optical signals into electric signals by the optical fiber grating demodulator, and analyzing and processing the data by a data processing module.
2. The method for detecting the strain in-situ inside the lithium solid-state battery by the Fiber Bragg Grating sensor according to claim 1, wherein in the step 1, the Fiber Bragg Grating sensor is a Fiber Bragg Grating (FBG) sensor, and comprises a Fiber Bragg Grating region, a Fiber coating layer and a Fiber core.
3. The method for detecting the internal strain in situ of the lithium solid state battery through the fiber grating sensor as claimed in claim 1, wherein in step 1, the solid state lithium metal battery is a CR2032 button type battery.
4. The method for detecting the strain in-situ inside the lithium solid-state battery through the fiber bragg grating sensor as claimed in claim 1, wherein in the step 2, the diameter of the drilled hole is 200-300 μm.
5. The method for detecting the strain in situ in the lithium solid state battery through the fiber bragg grating sensor as claimed in claim 1, wherein in the step 2, the metal capillary tube has a length of 5-10mm and an inner diameter of 300-500 μm.
CN202210677985.6A 2022-06-16 2022-06-16 Method for detecting internal strain in-situ of solid-state lithium battery through fiber grating sensor Pending CN115143893A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116915181A (en) * 2023-07-19 2023-10-20 武汉理工大学 Perovskite solar cell health state online in-situ monitoring system and method
CN117233104A (en) * 2023-11-16 2023-12-15 宁德时代新能源科技股份有限公司 Battery lithium separation detection method and device based on optical fiber sensor

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116915181A (en) * 2023-07-19 2023-10-20 武汉理工大学 Perovskite solar cell health state online in-situ monitoring system and method
CN116915181B (en) * 2023-07-19 2024-03-05 武汉理工大学 Perovskite solar cell health state online in-situ monitoring system and method
CN117233104A (en) * 2023-11-16 2023-12-15 宁德时代新能源科技股份有限公司 Battery lithium separation detection method and device based on optical fiber sensor
CN117233104B (en) * 2023-11-16 2024-04-05 宁德时代新能源科技股份有限公司 Battery lithium separation detection method and device based on optical fiber sensor

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