Method and device for comprehensive detection of interface characteristics of ionic battery

Abstract

The present disclosure relates to the technical field of ion battery interface characteristic measurement, and particularly relates to an ion battery interface characteristic comprehensive detection method and device. The method comprises the following steps: determining a to-be-detected interface corresponding to a to-be-detected ion battery sample; determining a working state corresponding to the to-be-detected ion battery sample; and determining an ion battery interface characteristic corresponding to the to-be-detected interface based on the working state by using a dual-wavelength photoelectric combined Raman method. The present disclosure can realize comprehensive detection of ion battery interface reaction and energy carrier transport.

Description

TECHNICAL FIELD

[0001] The present disclosure relates to the technical field of ion battery interface property measurement, and particularly relates to an ion battery interface property comprehensive detection method and device. BACKGROUND

[0002] Due to the advantages of high environmental protection, high safety and high energy density, ion batteries represented by lithium ion batteries have broad application prospects and great application value in the fields of energy storage, transportation power, mobile communication and aerospace. However, in ion batteries, the interface compatibility between the electrolyte and the electrode will directly affect the transport of ions and electrons at the interface, and then affect the cycle characteristics and rate performance of the battery. In addition, the chemical reaction at the electrode-electrolyte interface and the growth of lithium dendrites during the cycle process will further affect the transport and conversion performance of the energy carriers, and then lead to the increase of interface impedance, the attenuation of battery capacity and even short circuit failure. Therefore, the interface problem has become a bottleneck restricting the further development of ion batteries, and improving the transport, conversion and chemical reaction characteristics of the energy carriers at the interface is of great significance to the performance improvement of ion batteries.

[0003] However, the in-situ and real-time detection means of the interface reaction characteristics and the transport and conversion characteristics of the energy carriers still need to be developed. Therefore, how to realize the comprehensive detection of the interface reaction and the transport of the energy carriers of ion batteries has become the focus of attention. SUMMARY

[0004] The present disclosure provides an ion battery interface property comprehensive detection method and device, and the main purpose is to realize the comprehensive detection of the interface reaction and the transport of the energy carriers of ion batteries.

[0005] According to an aspect of the present disclosure, an ion battery interface property comprehensive detection method is provided, comprising:

[0006] determining a to-be-detected interface corresponding to a to-be-detected ion battery sample;

[0007] determining a working state corresponding to the to-be-detected ion battery sample;

[0008] determining an ion battery interface property corresponding to the to-be-detected interface based on the working state by using a dual-wavelength photoelectric combined Raman method.

[0009] Optionally, in an embodiment of the present disclosure, the ion battery interface property includes dynamic interface reaction characteristics, energy carrier transport characteristics and static interface reaction characteristics, and the determination of the to-be-detected interface corresponding to the to-be-detected ion battery sample comprises:

[0010] determining that the to-be-tested interface is a positive electrode interface, a negative electrode interface, or an electrolyte separator interface of the to-be-tested ion battery sample when the dynamic interfacial reaction characteristic, the energy carrier transport characteristic, and the static interfacial reaction characteristic corresponding to the to-be-tested ion battery sample are determined;

[0011] The ion battery interface characteristic includes a lithium dendrite growth characteristic, and the determining the to-be-tested interface corresponding to the to-be-tested ion battery sample includes:

[0012] The to-be-tested interface is determined to be a negative electrode interface of the to-be-tested ion battery sample when the lithium dendrite growth characteristic corresponding to the to-be-tested ion battery sample is determined.

[0013] Optionally, in an embodiment of the present disclosure, the ion battery interface characteristic includes a dynamic interfacial reaction characteristic, an energy carrier transport characteristic, and a lithium dendrite growth characteristic, and the determining the working state corresponding to the to-be-tested ion battery sample includes:

[0014] The working state corresponding to the to-be-tested ion battery sample is determined to be a charging and discharging state when the dynamic interfacial reaction characteristic, the energy carrier transport characteristic, and the lithium dendrite growth characteristic corresponding to the to-be-tested ion battery sample are determined.

[0015] The ion battery interface characteristic includes a static interfacial reaction characteristic, and the determining the working state corresponding to the to-be-tested ion battery sample includes:

[0016] The working state corresponding to the to-be-tested ion battery sample is determined to be a non-charging and discharging state when the static interfacial reaction characteristic corresponding to the to-be-tested ion battery sample is determined.

[0017] Optionally, in an embodiment of the present disclosure, the ion battery interface characteristic includes a dynamic interfacial reaction characteristic and an energy carrier transport characteristic, and the determining the ion battery interface characteristic corresponding to the to-be-tested interface based on the working state by using the dual-wavelength photoelectric coupling Raman method includes:

[0018] The first-wavelength laser is controlled to be focused on a first surface coordinate corresponding to the to-be-tested ion battery sample and to excite a first Raman spectrum, and the second-wavelength laser is controlled to be focused on a second surface coordinate corresponding to the to-be-tested ion battery sample and to excite a second Raman spectrum, wherein the first surface coordinate and the second surface coordinate are located on the same side of the to-be-tested interface, the first surface coordinate and the second surface coordinate are not coincident, a line connecting the first surface coordinate and the second surface coordinate is perpendicular to the to-be-tested interface, a distance between the first surface coordinate and the second surface coordinate is a preset coordinate distance, a distance between the first surface coordinate and the to-be-tested interface is smaller than a distance between the second surface coordinate and the to-be-tested interface, and a wavelength of the first-wavelength laser is greater than a wavelength of the second-wavelength laser.

[0019] based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time, to synchronously determine the change trend of the battery working signal, the first Raman spectrum and the second Raman spectrum with time;

[0020] According to the change trend of the battery working signal, the first Raman spectrum, the second Raman spectrum with time and the preset coordinate interval, the dynamic interface reaction characteristic and the energy carrier transport characteristic are determined.

[0021] Optionally, in an embodiment of the present disclosure, the ion battery interface characteristic includes a lithium dendrite growth characteristic, and the ion battery interface characteristic corresponding to the interface to be measured is determined based on the working state by using the dual-wavelength photoelectric combined Raman method, including:

[0022] A measurement area is determined, the first wavelength laser is controlled to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite a third Raman spectrum, and the second wavelength laser is controlled to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite a fluorescence spectrum, wherein the third surface coordinate is located in the measurement area, and the wavelength of the first wavelength laser is greater than the wavelength of the second wavelength laser;

[0023] based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement area, and the fluorescence spectrum corresponding to the measurement area at the same time, to synchronously determine the change trend of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time;

[0024] According to the change trend of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time, the lithium dendrite growth characteristic is determined.

[0025] Optionally, in an embodiment of the present disclosure, the ion battery interface characteristic includes a static interface reaction characteristic, and the ion battery interface characteristic corresponding to the interface to be measured is determined based on the working state by using the dual-wavelength photoelectric combined Raman method, including:

[0026] control the first wavelength laser to focus on a fourth surface coordinate corresponding to the ion battery sample to be measured and excite a fourth Raman spectrum, and control the second wavelength laser to focus on a fifth surface coordinate corresponding to the ion battery sample to be measured and excite a fifth Raman spectrum, wherein the fourth surface coordinate and the fifth surface coordinate are located on the same side of the interface to be measured, the fourth interface coordinate and the fifth interface coordinate are not coincident, the line connecting the fourth interface coordinate and the fifth interface coordinate is perpendicular to the interface to be measured, the distance between the fourth interface coordinate and the fifth interface coordinate is a preset coordinate distance, the distance between the fourth interface coordinate and the interface to be measured is less than the distance between the fifth interface coordinate and the interface to be measured, and the wavelength of the first wavelength laser is greater than the wavelength of the second wavelength laser;

[0027] based on the working state, using time synchronization, recording the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate at the same time, to synchronously determine the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time;

[0028] According to the change trend of the fourth Raman spectrum, the fifth Raman spectrum with time and the preset coordinate distance, the static interface reaction characteristic is determined.

[0029] According to another aspect of the present disclosure, there is provided an ion battery interface characteristic comprehensive detection device, characterized in that it comprises a dual-wavelength spectral measurement system, a charge-discharge control system, an environment regulation system and a data synchronization analysis system; wherein,

[0030] The environment regulation system is configured to determine an interface to be measured corresponding to an ion battery sample to be measured.

[0031] The charge-discharge control system is configured to determine a working state corresponding to the ion battery sample to be measured.

[0032] The data synchronization analysis system is configured to determine, by the dual-wavelength spectral measurement system, an ion battery interface characteristic corresponding to the interface to be measured by using a dual-wavelength photoelectric combined Raman method based on the working state.

[0033] Optionally, in an embodiment of the present disclosure, the environment regulation system comprises a sample cavity, a temperature control platform, an atmosphere regulation platform and a displacement platform; wherein,

[0034] The sample cavity is configured to place the ion battery sample to be measured.

[0035] The temperature control platform is connected with the sample cavity and is configured to control the temperature in the sample cavity.

[0036] The atmosphere regulation platform is connected with the sample cavity and is used for controlling the atmosphere environment in the sample cavity.

[0037] The displacement platform is connected with the sample cavity and is used for adjusting the position of the ion battery to be tested.

[0038] Optionally, in an embodiment of the present disclosure, the dual-wavelength spectral measurement system comprises a first continuous laser, a second continuous laser, a first narrow-band pass filter, a second narrow-band pass filter, a scanning galvanometer, a selective lens, an objective lens, a first filter, a second filter, a spectral detection device, and at least one mirror.

[0039] The first continuous laser is used for generating first-wavelength continuous probe laser.

[0040] The second continuous laser is used for generating second-wavelength continuous probe laser.

[0041] The first narrow-band pass filter is used for improving the beam quality of the first-wavelength continuous probe laser to obtain first-wavelength laser.

[0042] The second narrow-band pass filter is used for improving the beam quality of the second-wavelength continuous probe laser to obtain second-wavelength laser.

[0043] The scanning galvanometer is used for receiving the first-wavelength laser and reflecting the first-wavelength laser.

[0044] The selective lens is used for receiving the first-wavelength laser reflected by the scanning galvanometer and receiving the second-wavelength laser.

[0045] The objective lens is used for receiving the first-wavelength laser and the second-wavelength laser emitted by the selective lens, focusing the first-wavelength laser and the second-wavelength laser on the ion battery sample to be tested, and receiving the Raman spectrum excited by the first-wavelength laser and the second-wavelength laser.

[0046] The first filter is used for eliminating Rayleigh scattering excited by the first-wavelength laser in the Raman spectrum.

[0047] The second filter is used for eliminating Rayleigh scattering excited by the second-wavelength laser in the Raman spectrum.

[0048] The spectral detection device is used for receiving the filtered Raman spectrum and fluorescence spectrum, and performing spectral detection on the filtered Raman spectrum and the fluorescence spectrum.

[0049] The at least one mirror is used for constructing an optical path.

[0050] Optionally, in one embodiment of the present disclosure, the charge and discharge control system comprises a battery test platform and an electrochemical workstation, the data synchronous analysis system comprises a time synchronization control module and a data analysis module, the time synchronization control module comprises an instrument synchronization control submodule and a timing recording submodule; wherein,

[0051] The battery test platform is configured to control the charge and discharge state of the ion battery sample to be tested and record the battery working signal of the ion battery sample to be tested, wherein the charge and discharge state comprises a constant current charging state, a constant voltage charging state, a constant current discharging state and a static state.

[0052] The electrochemical workstation is connected to the battery test platform and configured to detect the impedance spectrum of the ion battery sample to be tested in situ.

[0053] The instrument synchronization control submodule is connected to the battery test platform and the dual-wavelength spectral measurement system, respectively, and configured to synchronize the detection time of the battery test platform and the dual-wavelength spectral measurement system.

[0054] The timing recording submodule is connected to the instrument synchronization control submodule and configured to record the battery working signal of the ion battery sample to be tested recorded by the battery test platform, the spectral signal recorded by the dual-wavelength spectral measurement system, and the detection time corresponding to the battery working signal and the spectral signal.

[0055] The data analysis module is connected to the timing recording submodule and configured to analyze the spectral signal and the battery working signal corresponding to the detection time, and determine the ion battery interface characteristics corresponding to the interface to be tested.

[0056] According to another aspect of the present disclosure, an ion battery interface characteristic comprehensive detection device is provided, comprising:

[0057] at least one processor; and

[0058] a memory connected to the at least one processor in communication; wherein,

[0059] The memory stores instructions executable by the at least one processor, and the instructions are executed by the at least one processor to enable the at least one processor to execute the method of any one of the preceding aspects.

[0060] According to another aspect of the present disclosure, a non-transitory computer readable storage medium storing computer instructions is provided, wherein the computer instructions are used to make the computer execute the method of any one of the preceding aspects.

[0061] According to another aspect of the present disclosure, a computer program product is provided, comprising a computer program which, when executed by a processor, implements the method of any one of the preceding aspects.

[0062] In one or more embodiments of the present disclosure, by determining a to-be-tested interface corresponding to a to-be-tested ion battery sample; determining a working state corresponding to the to-be-tested ion battery sample; and utilizing a dual-wavelength photoelectric combined Raman method to determine an ion battery interface characteristic corresponding to the to-be-tested interface based on the working state. Therefore, by utilizing the dual-wavelength photoelectric combined Raman method to determine the ion battery interface characteristic corresponding to the to-be-tested interface, comprehensive detection of ion battery interface reactions and energy carrier transport can be realized.

[0063] Additional aspects and advantages of the present disclosure will be in part apparent and in part pointed out hereinafter. BRIEF DESCRIPTION OF DRAWINGS

[0064] The above and / or additional aspects and advantages of the present disclosure will become apparent and be readily appreciated from the following description, including the appended drawings, wherein:

[0065] Figure 1 A flowchart illustrating a first ion battery interface characteristic comprehensive detection method provided by an embodiment of the present disclosure is shown;

[0066] Figure 2 A flowchart illustrating a second ion battery interface characteristic comprehensive detection method provided by an embodiment of the present disclosure is shown;

[0067] Figure 3 A flowchart illustrating a preparation process of a to-be-tested ion battery sample provided by an embodiment of the present disclosure is shown;

[0068] Figure 4 A structural diagram of a sample cavity provided by an embodiment of the present disclosure is shown;

[0069] Figure 5 A design diagram of laser focusing provided by an embodiment of the present disclosure is shown;

[0070] Figure 6 A schematic diagram of a measurement principle of a dynamic interface reaction and energy carrier transport process provided by an embodiment of the present disclosure is shown;

[0071] Figure 7 A schematic diagram of a relationship between a Raman characteristic peak position and peak intensity reflecting ion concentration at a positive electrode interface and ion concentration provided by an embodiment of the present disclosure is shown;

[0072] Figure 8 A flowchart illustrating a third ion battery interface characteristic comprehensive detection method provided by an embodiment of the present disclosure is shown;

[0073] Figure 9 Fig. 1 shows a schematic diagram of a measurement principle of lithium dendrite growth provided by an embodiment of the present disclosure;

[0074] Figure 10 Fig. 2 shows a schematic diagram of a fluorescence signal scanning imaging characterization of lithium dendrite growth provided by an embodiment of the present disclosure;

[0075] Figure 10 Fig. 3 shows a schematic diagram of a fluorescence-Raman signal scanning imaging characterization of lithium dendrite growth environment provided by an embodiment of the present disclosure;

[0076] Figure 11 Fig. 4 shows a flowchart of a fourth ion battery interface property comprehensive detection method provided by an embodiment of the present disclosure;

[0077] Figure 12 Fig. 5 shows a structural schematic diagram of a first ion battery interface property comprehensive detection method provided by an embodiment of the present disclosure;

[0078] Figure 13 Fig. 6 shows a structural schematic diagram of a second ion battery interface property comprehensive detection method provided by an embodiment of the present disclosure;

[0079] Figure 14 Fig. 7 is a block diagram of an ion battery interface property comprehensive detection device for implementing the ion battery interface property comprehensive detection method of the embodiments of the present disclosure. DETAILED DESCRIPTION

[0080] Embodiments of the present disclosure are described in detail below with reference to the accompanying drawings. The embodiments described below are examples for explaining the present disclosure and are not intended to limit the present disclosure. On the contrary, embodiments of the present disclosure include all changes, modifications and equivalents falling within the spirit and scope of the appended claims.

[0081] According to some embodiments, in the related art, the characterization methods used by the in-situ and real-time detection means of interface reaction properties and energy carrier transport and conversion properties are mainly aimed at the overall performance of the battery or the interface properties before and after cycling, and lack in-situ and real-time detection of reaction interface layer evolution and ion-electron transport and conversion properties during charging and discharging. On this basis, the interface multi-factor coupling mechanism still needs to be studied: ion transport and electron transport exist at the interface at the same time, existing research focuses on ion transport properties, but the influence of ion and electron coupled transport on the overall performance of the battery has not been explained; the mechanism of lithium dendrite growth is not clear, and the process of ion and electron coupled conversion into lithium atoms needs to be further characterized; in addition, the influence of interface chemical reaction on ion-electron coupling also needs to be studied.

[0082] In some embodiments, Raman spectroscopy, as an in-situ non-destructive characterization method, has been applied to lithium-ion battery research. However, existing methods have not yet achieved in-situ, real-time detection of interface layer evolution and ion-electron coupling transport and conversion during charging and discharging. Furthermore, traditional Raman methods can only detect the properties of a single point in the electrolyte at any given time, failing to characterize the carrier transport process at the interface and making it difficult to determine the rate of interface reaction layer expansion. Since different degrees of interface reaction can significantly affect carrier transport characteristics, a breakthrough method must be developed to achieve multi-factor, in-situ, real-time detection of interface characteristics during charging and discharging.

[0083] In some embodiments, fluorescence methods, as optical means, have been used to characterize the morphology of lithium dendrite growth in situ. However, fluorescence can only reflect the dendrite morphology and cannot provide information on other material components in the lithium dendrite growth environment, making it difficult to determine the influence of interfacial reactions on lithium dendrite growth. Raman spectroscopy holds promise for obtaining information on environmental materials, but compared to fluorescence signals, Raman signals are extremely weak. When fluorescence is excited by laser, the corresponding Raman information is overwhelmed by the fluorescence signal and difficult to measure. Therefore, to reveal the mechanism of lithium dendrite growth, a breakthrough method must be proposed to achieve simultaneous detection of fluorescence and Raman spectroscopy at the interface.

[0084] It is easy to understand that existing methods for measuring interface characteristics cannot achieve comprehensive detection of interfacial reactions and carrier transport in ion batteries, which has become a problem that urgently needs to be solved in the field of ion battery measurement.

[0085] The present disclosure will now be described in detail with reference to specific embodiments.

[0086] In the first embodiment, such as Figure 1 As shown, Figure 1 This diagram illustrates a flowchart of a first method for comprehensive detection of interface characteristics of ion batteries according to an embodiment of the present disclosure. This method can be implemented using a computer program and can run on a device for comprehensive detection of interface characteristics of ion batteries. The computer program can be integrated into an application or run as a standalone utility application.

[0087] Specifically, the comprehensive detection method for the interface characteristics of ion batteries includes:

[0088] S11, Determine the interface to be tested corresponding to the ion battery sample to be tested;

[0089] According to some embodiments, ion batteries are also called lithium-ion batteries. Lithium-ion batteries refer to a general term for batteries that use lithium-ion intercalation compounds as the positive electrode material. Lithium-ion batteries use carbon materials as the negative electrode and lithium-containing compounds as the positive electrode; no metallic lithium is present, only lithium ions.

[0090] In some embodiments, the ion battery sample to be tested refers to an ion battery that needs to be subjected to comprehensive detection of ion battery interface characteristics. The ion battery sample to be tested does not refer to a fixed sample. The ion battery sample to be tested includes, but is not limited to, a full solid-state ion battery, a semi-solid ion battery, a liquid ion battery, and the like.

[0091] In some embodiments, the interface to be tested refers to an interface used when the ion battery sample to be tested is subjected to comprehensive detection of ion battery interface characteristics. The interface to be tested does not refer to a fixed interface. The interface to be tested includes, but is not limited to, a positive electrode interface of the ion battery sample to be tested, a negative electrode interface, and the like.

[0092] It is easy to understand that when the ion battery interface characteristics are comprehensively detected, the interface to be tested corresponding to the ion battery sample to be tested can be determined.

[0093] S12, determining a working state corresponding to the ion battery sample to be tested;

[0094] According to some embodiments, the working state corresponding to the ion battery sample to be tested does not refer to a fixed state. For example, the working state can be a charging and discharging state, and the working state can also be a non-charging and discharging state.

[0095] It is easy to understand that when the ion battery interface characteristics are comprehensively detected, the working state corresponding to the ion battery sample to be tested can be determined.

[0096] S13, determining ion battery interface characteristics corresponding to the interface to be tested based on the working state by using a dual-wavelength photoelectric combined Raman method.

[0097] According to some embodiments, the dual-wavelength photoelectric combined Raman method refers to an optical analysis method for performing spectrum analysis according to Raman effect by using two lasers with different wavelengths. The dual-wavelength photoelectric combined Raman method does not refer to a fixed method. For example, when the ion battery interface characteristics change, the dual-wavelength photoelectric combined Raman method can also change. When the ion battery sample to be tested changes, the dual-wavelength photoelectric combined Raman method can also change.

[0098] In some embodiments, the ion battery interface characteristics do not refer to a fixed characteristic. The ion battery interface characteristics include, but are not limited to, dynamic interface reaction characteristics, carrier energy sub-transport characteristics, lithium dendrite growth characteristics, and static interface reaction characteristics, and the like.

[0099] It is easy to understand that when the working state corresponding to the ion battery sample to be tested is determined, the dual-wavelength photoelectric combined Raman method can be used to determine the ion battery interface characteristics corresponding to the interface to be tested based on the working state corresponding to the ion battery sample to be tested.

[0100] To sum up, the method provided by the embodiments of the present disclosure determines the to-be-tested interface corresponding to the to-be-tested ion battery sample; determines the working state corresponding to the to-be-tested ion battery sample; and determines the ion battery interface characteristics corresponding to the to-be-tested interface based on the working state by using the dual-wavelength photoelectric combined Raman method. Therefore, the comprehensive detection of the ion battery interface reaction and the energy carrier sub-transport can be realized by determining the ion battery interface characteristics corresponding to the to-be-tested interface by using the dual-wavelength photoelectric combined Raman method.

[0101] Please refer to Figure 2 , Figure 2 A flowchart of a second ion battery interface characteristic comprehensive detection method provided by the embodiments of the present disclosure is shown.

[0102] Specifically, the ion battery interface characteristic comprehensive detection method comprises the following steps:

[0103] S21, determining a to-be-tested ion battery sample;

[0104] According to some embodiments, Figure 3 A preparation flowchart of a to-be-tested ion battery sample provided by the embodiments of the present disclosure is shown. As shown in Figure 3 When the to-be-tested ion battery is a full-solid-state lithium ion battery, the full-solid-state lithium ion battery can be formed by die pressing, and then demolded by a demolding machine. Then, a flat side surface of the full-solid-state lithium ion battery, on which the positive electrode interface-electrolyte-negative electrode interface can be observed, is selected as a measurement section. The measurement section can be directly formed by pressing or obtained by cutting a flat section.

[0105] In some embodiments, Figure 3 The preparation flowchart of the to-be-tested ion battery sample shown is not limited to full-solid-state ion batteries, and semi-solid-state ion batteries and liquid-state ion batteries can also be used.

[0106] According to some embodiments, since a plurality of to-be-tested ion battery samples are sensitive to water and oxygen environment, when the ion battery interface characteristic comprehensive detection is performed, the to-be-tested ion battery sample needs to be placed in a sample chamber with controllable environmental atmosphere for charge and discharge cycles to perform the ion battery interface characteristic comprehensive detection. A temperature control platform for maintaining the external environment of the sample and an atmosphere control platform can be integrated with the sample chamber, so that the sample chamber can realize temperature and atmosphere control, and be placed on a displacement platform to control the coordinates of the to-be-tested ion battery sample by the displacement platform. Meanwhile, the sample chamber can be provided with an optical measurement window to expose the positive electrode interface, electrolyte and negative electrode interface of the to-be-tested ion battery sample under the optical measurement window.

[0107] In some embodiments, Figure 4 A structural schematic diagram of a sample chamber provided by the embodiments of the present disclosure is shown. As shown in Figure 4As shown, the optical measurement window can be a silicon dioxide SiO2 visible window, which can be used to transmit the probe laser, the material of the clamping device clamping the ion battery sample to be measured can be stainless steel, which can be directly used as the positive / negative electrode current collector, and the pressure of the clamping device can be adjusted by a nut; the air pump is used to maintain the atmospheric environment in the sample chamber; and the temperature controller can be used to regulate the ambient temperature of the ion battery sample to be measured.

[0108] It is easy to understand that when the dynamic interfacial reaction characteristic and the carrier transport characteristic are detected, the ion battery to be measured can be processed to obtain the ion battery sample to be measured, which can observe the positive electrode interfacial-electrolyte-negative electrode interfacial section.

[0109] S22, determining the interface to be measured corresponding to the ion battery sample to be measured as the positive electrode interface, the negative electrode interface or the electrolyte separator interface of the ion battery sample to be measured;

[0110] According to some embodiments, when the ion battery sample to be measured is a liquid ion battery, the liquid ion battery has a separator and the like structure. Therefore, the interface formed by the electrolyte and other structures such as the separator can also be used as the interface to be measured corresponding to the ion battery sample to be measured, i.e., the electrolyte separator interface.

[0111] It is easy to understand that when the dynamic interfacial reaction characteristic and the carrier transport characteristic are detected, the interface to be measured corresponding to the ion battery sample to be measured can be determined as the positive electrode interface, the negative electrode interface or the electrolyte separator interface of the ion battery sample to be measured.

[0112] S23, determining the working state corresponding to the ion battery sample to be measured as a charging and discharging state;

[0113] According to some embodiments, when the ion battery sample to be measured is placed in the sample chamber, the ion battery sample to be measured can be connected with an external charging and discharging control system. Further, when the working state corresponding to the ion battery sample to be measured is determined as the charging and discharging state, the ion battery sample to be measured can be controlled to be in the charging and discharging state by controlling the charging and discharging control system to be turned on.

[0114] In some embodiments, when the charging and discharging control system is turned on and controls the ion battery sample to be measured to be in the charging and discharging state, the charging and discharging current, the charging and discharging voltage and the charging and discharging cycle number corresponding to the ion battery sample to be measured can be adjusted.

[0115] It is easy to understand that when the dynamic interfacial reaction characteristic and the carrier transport characteristic are detected, the working state corresponding to the ion battery sample to be measured can be determined as the charging and discharging state.

[0116] S24, control the first wavelength laser to focus on the first surface coordinate corresponding to the ion battery sample to be measured and excite the first Raman spectrum, and control the second wavelength laser to focus on the second surface coordinate corresponding to the ion battery sample to be measured and excite the second Raman spectrum;

[0117] According to some embodiments, Figure 5 A design schematic diagram of laser focusing is shown. As shown in Figure 5 The first wavelength laser with wavelength λ1 is reflected by the scanning galvanometer and then converges with the second wavelength laser with wavelength λ2 through the selective lens. Then, the first wavelength laser is focused on the first surface coordinate (position 1) above the ion battery sample to be measured placed on the displacement platform through the same objective lens, and the second wavelength laser is focused on the second surface coordinate (position 2) above the ion battery sample to be measured placed on the displacement platform.

[0118] In some embodiments, the wavelength λ1 of the first wavelength laser is not equal to the wavelength λ2 of the second wavelength laser, and specifically, the wavelength λ1 of the first wavelength laser is greater than the wavelength λ2 of the second wavelength laser.

[0119] In some embodiments, by adjusting the displacement platform, the first surface coordinate and the second surface coordinate can be changed as a whole. By adjusting the angle of the scanning galvanometer, the first surface coordinate can be adjusted alone without changing the second surface coordinate. Therefore, the separate regulation of the first surface coordinate and the second surface coordinate can be realized.

[0120] In some embodiments, as shown in Figure 5 When detecting the dynamic interfacial reaction characteristics and the energy carrier transport characteristics, the first surface coordinate and the second surface coordinate can be regulated to be located on the same side of the interface to be measured, the first surface coordinate and the second surface coordinate can be regulated not to coincide, the line connecting the first surface coordinate and the second surface coordinate can be regulated to be perpendicular to the interface to be measured, the distance between the first surface coordinate and the second surface coordinate can be regulated to be a preset coordinate distance l, and the distance between the first surface coordinate and the interface to be measured can be regulated to be less than the distance between the second surface coordinate and the interface to be measured.

[0121] In some embodiments, as shown in Figure 5 The first surface coordinate and the second surface coordinate can be selected in the region where the electrolyte is close to the interface to be measured. That is, the first surface coordinate and the second surface coordinate are selected in the region where the distance between the electrolyte and the interface to be measured is less than the electrolyte-interface distance threshold. The electrolyte-interface distance threshold does not refer to a fixed threshold. For example, when a threshold modification instruction for the electrolyte-interface distance threshold is obtained, the threshold of the electrolyte-interface distance threshold can be changed.

[0122] It is easy to understand that when the working state corresponding to the ion battery sample to be measured is determined to be the charging and discharging state and the interface to be measured, the first wavelength laser can be controlled to focus on the first surface coordinate corresponding to the ion battery sample to be measured and excite the first Raman spectrum, and the second wavelength laser can be controlled to focus on the second surface coordinate corresponding to the ion battery sample to be measured and excite the second Raman spectrum.

[0123] S25, based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time, to synchronously determine the change trend of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time;

[0124] According to some embodiments, the battery working signal is not specific to a fixed signal. The battery working signal includes but is not limited to the voltage signal and the current signal when the ion battery sample to be measured is charged, the voltage signal and the current signal when the ion battery sample to be measured is discharged, and the like.

[0125] In some embodiments, when the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time are recorded using time synchronization to synchronously determine the change trend of the voltage signal and the current signal when the ion battery sample to be measured is charged and discharged, the first Raman spectrum, and the second Raman spectrum with time, the time when the ion battery sample to be measured is first charged can be taken as the initial 0 time when the charging and discharging control system is turned on. Then, using the time synchronization control module, after starting measurement, the time t1 when the measurement starts is recorded, and the voltage signal and the current signal of the ion battery sample to be measured during the charging process or the discharging process at the measurement time t1 are recorded. At the same time, at time t1, the first wavelength laser and the second wavelength laser are used to excite the spectrum signal of the ion battery sample to be measured respectively to obtain the first Raman spectrum information corresponding to the first surface coordinate and the second Raman spectrum information corresponding to the second surface coordinate at the measurement time t1. Finally, the measurement step is repeated to further obtain the voltage signal and the current signal of the ion battery sample to be measured during charging and discharging, and the first Raman spectrum information and the second Raman spectrum information at times t2, t3, t4, t5, etc., to obtain the change trend of the voltage signal and the current signal of the ion battery sample to be measured during charging and discharging, the first Raman spectrum, and the second Raman spectrum with time.

[0126] In some embodiments, when the first Raman spectrum information and the second Raman spectrum information are acquired, the first Raman spectrum information and the second Raman spectrum information will pass through the objective lens at the same time and be collected on the same spectrum by the charge-coupled device (CCD). However, since the wavelength λ1 of the first wavelength laser and the wavelength λ2 of the second wavelength laser are different, the Raman spectra excited by the first wavelength laser and the second wavelength laser also have different absolute wavelengths, that is, the absolute wavelength of the Raman characteristic peak in the measured Raman spectrum can be used to determine whether it is the first Raman spectrum information of the first surface coordinate or the second Raman spectrum information of the second surface coordinate. In order to avoid the overlap of the spectrum signals of the first Raman spectrum information and the second Raman spectrum information, the difference between the wavelength λ1 and the wavelength λ2 can be controlled to be greater than 100 nm.

[0127] It is easy to understand that when it is determined that the working state corresponding to the ion battery sample to be measured is the charging and discharging state, the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time can be recorded based on the charging and discharging state by using the time synchronization control module, so as to synchronously determine the change trend of the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate with time.

[0128] S26, determining the dynamic interfacial reaction characteristic and the energetic carrier transport characteristic according to the change trend of the battery working signal, the first Raman spectrum, the second Raman spectrum with time, and the preset coordinate interval.

[0129] According to some embodiments, when the dynamic interfacial reaction characteristic is determined, the characteristic peaks of the interfacial reaction products corresponding to the first surface coordinate and the second surface coordinate can be identified according to the change trend of the first Raman spectrum and the second Raman spectrum with time, respectively, to obtain the time when the interfacial reaction product characteristic peaks appear at the first surface coordinate and the second surface coordinate, respectively. Then, the change trend of the interfacial reaction product concentration corresponding to the first surface coordinate and the interfacial reaction product concentration corresponding to the second surface coordinate with the measurement time can be determined based on the characteristic peak intensity analysis of the interfacial reaction product characteristic peaks, respectively. Finally, the dynamic interfacial reaction speed and the reaction interface layer expansion speed corresponding to the ion battery sample to be measured, that is, the dynamic interfacial reaction characteristic, can be determined in combination with the preset coordinate interval l.

[0130] In some embodiments, the characteristic peaks of interfacial reaction products do not specifically refer to a particular peak. These characteristic peaks include, but are not limited to, characteristic peaks of known interfacial reaction products of the battery, characteristic peaks of interfacial products calculated and analyzed based on the positive electrode material, negative electrode material, and electrolyte material, and new characteristic peaks of other non-electrolyte material characteristic peaks that appear at the interface during static placement or charge / discharge processes, etc.

[0131] In some embodiments, Figure 6 This diagram illustrates the measurement principle of a dynamic interface reaction and carrier transport process provided in an embodiment of this disclosure. Figure 6 As shown, the negative electrode interface of the ion battery sample is identified as the test interface. During the charging and discharging process, the negative electrode material reacts with the electrolyte, generating new reactants, which in turn produce new characteristic peaks in the Raman spectrum. Since the first surface coordinate is closer to the negative electrode interface than the second surface coordinate, the characteristic peak of the interface reaction product first appears at the first surface coordinate at time t2. As the measurement time increases and the reaction proceeds, the concentration of the interface reaction product at the first surface coordinate continuously increases, and the peak intensity of the characteristic peak of the interface reaction product increases. Based on the pre-calibrated relationship between the interface reaction product and the peak intensity of the characteristic peak, combined with the measurement time, the dynamic interface reaction rate can be determined. Simultaneously, as the measurement time increases, the reaction interface layer continuously expands, and at time t3, the characteristic peak of the interface reaction product also appears at the second surface coordinate. Based on the times t2 and t3 when the characteristic peak of the interface reaction product appears, combined with the distance l between the first and second surface coordinates, the expansion rate of the reaction interface layer during the dynamic process can be determined.

[0132] In some embodiments, in actual measurements, in addition to the peak intensity of the characteristic peak, changes in the concentration of the interfacial reaction products may also cause changes in information such as the peak position and full width at half maximum (FWHM) of the characteristic peak. The above-mentioned relationship can be obtained not only through pre-experimental calibration and first-principles calculations, but also by comparing the impedance spectrum measurement results before and after the reaction to determine the content of the dynamic interfacial reaction products, thereby obtaining the correspondence between the peak intensity, peak position, FWHM of the characteristic peak of the reaction products and the concentration of the reaction products.

[0133] According to some embodiments, when determining the carrier transport characteristics, characteristic peaks related to conductive ions in the electrolyte corresponding to the first and second surface coordinates can be identified based on the changing trends of the first and second Raman spectra over time. Then, based on the peak intensity, peak position, and full width at half maximum (FWHM) of the characteristic peaks related to these conductive ions, the changing trends of the ion concentrations corresponding to the first and second surface coordinates over time can be analyzed. Next, the changing trend of ion transport information over time can be determined by combining a preset coordinate spacing l. Finally, the ion-electron coupling transport process can be analyzed based on the changing trends of ion transport information, voltage signal, and current signal over time to obtain the carrier transport characteristics.

[0134] In some embodiments, ion transport information does not refer to a specific fixed piece of information. This ion transport information includes, but is not limited to, ion transport rate, changes in interfacial ion concentration, etc.

[0135] In some embodiments, such as Figure 6 As shown, time t1 to time t3 represents the charging process. During this time, lithium ions move from the positive electrode interface to the negative electrode interface. The lithium ion concentration at the second surface coordinate, which is farther from the negative electrode interface, increases first, leading to an increase in the intensity of the characteristic peak representing lithium ions. Then, as the charging time increases, lithium ions further move to the first surface coordinate, and the intensity of the characteristic peak representing lithium ions at the first surface coordinate also begins to increase. Next, by combining the delay time of the increase in the characteristic peak intensity representing lithium ions and the preset coordinate spacing l, the migration speed of lithium ions during the charging process can be determined. Finally, by combining the trends of the voltage and current signals with the measurement time, the ion-electron coupling transport process can be determined. Time t3 to time t5 represents the discharging process; similarly, the migration speed of lithium ions and the ion-electron coupling transport process during the discharging process can be obtained.

[0136] In some embodiments, during actual measurements, in addition to the peak intensity of the characteristic peak representing lithium ions, changes in the concentration of conductive ions in the electrolyte can also cause changes in information such as the peak position and full width at half maximum (FWHM) of the characteristic peak. Figure 7 This diagram illustrates the relationship between the position and intensity of the Raman characteristic peaks reflecting ion concentration at the positive electrode interface, as provided in an embodiment of this disclosure, and the variation of ion concentration. For example... Figure 7 As shown, during the charging process, lithium ions move from the negative electrode interface to the positive electrode interface, increasing the lithium ion concentration at the positive electrode interface, resulting in a continuous increase in Raman peak intensity and a red shift in peak position. Conversely, during the discharging process, the lithium ion concentration at the positive electrode interface decreases, and the peak intensity and peak position exhibit the opposite changes.

[0137] In some embodiments, the peak position and peak intensity of the Raman characteristic peak reflecting the ion concentration at the positive electrode interface change with the ion concentration, which can be obtained by pre-experiment calibration, first-principle calculation, or by calculating and analyzing the voltage signal and current signal measured during the charging and discharging dynamic process.

[0138] In some embodiments, when the peak position and peak intensity of the Raman characteristic peak reflecting the ion concentration at the positive electrode interface change with the ion concentration are determined by calculating and analyzing the voltage signal and current signal measured during the charging and discharging dynamic process, the total amount of lithium ion migration (i.e., the charging and discharging electric quantity) can be calculated based on the voltage and current signals, and then the lithium ion concentration distribution in the electrolyte can be determined in combination with the charging and discharging time and the electrolyte size, and then the corresponding relationship between the characteristic peak intensity, peak position, half-width, etc. of the Raman characteristic peak reflecting the ion concentration at the positive electrode interface and the lithium ion concentration can be obtained.

[0139] In some embodiments, when the content of the dynamic interfacial reaction product is determined by comparing the impedance spectrum measurement results before and after the reaction, the battery impedance spectrum of the ion battery sample to be measured can be measured before the charging and discharging test to determine the impedance information inside the ion battery sample to be measured before charging and discharging. Then, the battery impedance spectrum of the ion battery sample to be measured is measured after the charging and discharging test to determine the impedance information inside the ion battery sample to be measured after charging and discharging. Finally, the content of the dynamic interfacial reaction product can be determined according to the impedance information inside the ion battery sample to be measured before charging and discharging and the impedance information inside the ion battery sample to be measured after charging and discharging.

[0140] According to some embodiments, when the dynamic interfacial reaction characteristics and the carrier energy sub-transport characteristics are determined according to the variation trends of the battery working signal, the first Raman spectrum, the second Raman spectrum with time, and the preset coordinate interval, the battery impedance spectrum corresponding to the ion battery sample to be measured can be measured before and after the variation trends of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time. Then, the dynamic interfacial reaction characteristics and the carrier energy sub-transport characteristics can be measured and analyzed together according to the variation trends of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time before and after charging and discharging.

[0141] As can be easily understood, when the variation trends of the battery working signal, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate with time are determined, the dynamic interfacial reaction characteristics and the carrier energy sub-transport characteristics can be determined according to the variation trends of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time and the preset coordinate interval.

[0142] To sum up, the method provided in the embodiments of the present disclosure determines the ion battery sample to be measured; determines the interface to be measured corresponding to the ion battery sample to be measured as the positive electrode interface, the negative electrode interface or the electrolyte separator interface of the ion battery sample to be measured; determines the working state corresponding to the ion battery sample to be measured as the charging and discharging state; controls the first wavelength laser to focus on the first surface coordinate corresponding to the ion battery sample to be measured, and controls the second wavelength laser to focus on the second surface coordinate corresponding to the ion battery sample to be measured; determines the change trend of the battery working signal, the first Raman spectrum corresponding to the first surface coordinate and the second Raman spectrum corresponding to the second surface coordinate with time based on the working state; and determines the dynamic interface reaction characteristic and the energy carrier transport characteristic according to the change trend of the battery working signal, the first Raman spectrum and the second Raman spectrum with time and the preset coordinate distance. Therefore, by using the dual-wavelength photoelectric combined Raman method, the synchronous acquisition of the multi-position photo-electric signals is realized, and the signals of different measurement positions are distinguished by the two lasers with different wavelengths. In combination with the relative distance between the two measurement positions and the delay time of the Raman characteristic peak change, the micro-scale in-situ characterization of the ion transport speed and the interface reaction speed can be realized, and the coupling effect of the interface reaction degree and the energy carrier transport performance can be confirmed in real time. The interface reaction process and the ion transport process are measured at the same time, and the influence of the interface reaction process on the ion-electron coupling transport process can be further determined in-situ and in real time by combining data analysis, the influence effect of different interface reaction products on ion transport is revealed, and the comprehensive measurement and research of the battery characteristics under the charging and discharging dynamic conditions can be realized. In addition, since different substances have different Raman characteristic peaks, this method can also be used to find new chemical reactions and new interface reaction products occurring under different environmental conditions and in the charging and discharging process.

[0143] Please refer to Figure 8 , Figure 8 A flowchart of a third ion battery interface characteristic comprehensive detection method provided by the embodiments of the present disclosure is shown.

[0144] Specifically, the ion battery interface characteristic comprehensive detection method comprises:

[0145] S31, determining the interface to be measured corresponding to the ion battery sample to be measured as the negative electrode interface of the ion battery sample to be measured;

[0146] The specific process is as described above, which will not be repeated here.

[0147] It is easy to understand that when the lithium dendrite growth characteristic detection is performed, the interface to be measured corresponding to the ion battery sample to be measured can be determined as the negative electrode interface of the ion battery sample to be measured.

[0148] S32, determining the working state corresponding to the ion battery sample to be measured as the charging and discharging state;

[0149] The specific process is as above, which will not be repeated here.

[0150] S33, dropping a target fluorescent reagent on the surface of the ion battery sample to be measured;

[0151] According to some embodiments, the target fluorescent reagent refers to a fluorescent reagent that can have a fluorescence quenching reaction with active lithium and is stable to electrolyte. The target fluorescent reagent is not a fixed reagent. For example, the target fluorescent reagent can change when the ion battery sample to be measured changes. For example, the main light-emitting wavelength of the fluorescent reagent can be λ f .

[0152] In some embodiments, dropping the target fluorescent reagent on the surface of the ion battery sample to be measured can enable rapid dynamic imaging of the ion battery sample to be measured by fluorescence detection.

[0153] It is easy to understand that when it is determined that the interface to be measured is the negative electrode interface of the ion battery sample to be measured, and it is determined that the working state corresponding to the ion battery sample to be measured is the charging and discharging state, the target fluorescent reagent can be dropped on the surface of the ion battery sample to be measured.

[0154] S34, determining a measurement area, controlling the first-wavelength laser to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite a third Raman spectrum, and controlling the second-wavelength laser to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite a fluorescence spectrum;

[0155] The specific process is as above, which will not be repeated here.

[0156] According to some embodiments, the measurement area is not a fixed area. For example, the measurement area can be selected in the area where the electrolyte is close to the negative electrode interface. That is, the measurement area is selected in the area where the distance between the electrolyte and the negative electrode interface is less than the electrolyte-interface-to-be-measured distance threshold.

[0157] In some embodiments, the third surface coordinate refers to a coordinate located in the measurement area. The third surface coordinate is not a fixed coordinate. For example, the third surface coordinate can change when the measurement area changes.

[0158] According to some embodiments, the first-wavelength laser focuses on the third surface coordinate corresponding to the ion battery sample to be measured, for exciting a Raman spectrum. The second-wavelength laser focuses on the third surface coordinate corresponding to the ion battery sample to be measured, for fluorescence in-situ detection.

[0159] In some embodiments, the wavelength λ1 of the first-wavelength laser is not equal to the wavelength λ2 of the second-wavelength laser. Specifically, the wavelength λ1 of the first-wavelength laser is greater than the wavelength λ2 of the second-wavelength laser.

[0160] It is easy to understand that when the target fluorescent reagent is dropped on the surface of the ion battery sample to be measured, the measurement area can be determined, and the first wavelength laser is controlled to focus on the third surface coordinates corresponding to the ion battery sample to be measured and excite the third Raman spectrum, and the second wavelength laser is controlled to focus on the third surface coordinates corresponding to the ion battery sample to be measured and excite the fluorescence spectrum.

[0161] S35, based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement area, and the fluorescence spectrum corresponding to the measurement area at the same time, to synchronously determine the change trend of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time;

[0162] According to some embodiments, when the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement area, and the fluorescence spectrum corresponding to the measurement area at the same time are recorded using time synchronization to synchronously determine the change trend of the voltage signal and the current signal of the ion battery sample to be measured during discharge, the third Raman spectrum and the fluorescence spectrum with time, the time synchronization control module can be used to record the measurement time t1, and the voltage signal and the current signal of the battery discharge process at the measurement time t1 are recorded, and the first wavelength laser with a wavelength of λ1 and the second wavelength laser with a wavelength of λ2 are used to synchronously scan and obtain the third Raman spectrum and the fluorescence spectrum corresponding to the measurement area at the measurement time t1. Finally, the measurement step is repeated to further obtain the voltage signal and the current signal of the ion battery sample to be measured during discharge, the third Raman spectrum and the fluorescence spectrum information at the time t2, t3, t4, t5 and the like, to obtain the change trend of the voltage signal and the current signal of the ion battery sample to be measured during discharge, the third Raman spectrum and the fluorescence spectrum with time.

[0163] In some embodiments, when the first wavelength laser with a wavelength of λ1 and the second wavelength laser with a wavelength of λ2 are used to synchronously scan and obtain the third Raman spectrum and the fluorescence spectrum corresponding to the measurement area at the measurement time t1, the wavelength λ1 of the first wavelength laser is greater than the main light-emitting wavelength λ f of the target fluorescent reagent. The wavelength λ2 of the second wavelength laser is less than the main light-emitting wavelength λ f of the target fluorescent reagent. Therefore, the first wavelength laser cannot excite sample fluorescence, and its Raman characteristic peak (Stokes peak, wavelength greater than λ1) will not be submerged by the fluorescence signal λ f of the fluorescence spectrum, and the second wavelength laser can be used for in-situ fluorescence detection.

[0164] In some embodiments, when the main light-emitting wavelength λ f of the target fluorescent reagent does not coincide with the second Raman spectrum excited by the second wavelength laser with a wavelength of λ2, the wavelength λ2 is less than the wavelength λ fThe second wavelength laser can also be used to realize simultaneous measurement of Raman spectrum and fluorescence spectrum.

[0165] In some embodiments, the signals of the measurement region can be obtained by multi-point scanning imaging, line imaging, surface imaging, etc. When the signals of the measurement region are obtained by multi-point scanning imaging and line imaging, the initial 0 time can be the time when the scanning starts.

[0166] It is easy to understand that when the first wavelength laser is controlled to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite the third Raman spectrum, and the second wavelength laser is controlled to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite the fluorescence spectrum, the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement region, and the fluorescence spectrum corresponding to the measurement region at the same time can be recorded based on the working state by using the time synchronization control module, so as to synchronously determine the change trend of the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement region, and the fluorescence spectrum corresponding to the measurement region with time.

[0167] S36, determining the lithium dendrite growth characteristics according to the change trend of the battery working signal, the third Raman spectrum, and the fluorescence spectrum with time.

[0168] According to some embodiments, Figure 9 A schematic diagram of a measurement principle of a lithium dendrite growth process is shown. As shown in Figure 9 When determining the lithium dendrite growth characteristics, the fluorescence spectrum of the measurement region can be identified, and the growth process of the lithium dendrite can be dynamically imaged by the fluorescence spectrum, as shown in Figure 10 (a). Then, the ion species and distribution in the lithium dendrite growth environment can be measured in combination with the third Raman spectrum, and the linear relationship between the fluorescence signal intensity and the lithium dendrite concentration can be quantitatively calibrated, so as to dynamically detect the lithium deposition process.

[0169] According to some embodiments, as shown in Figure 9 When determining the lithium dendrite growth characteristics, the change trend of the metal lithium content at different positions in the measurement region with the measurement time can be analyzed based on the fluorescence generation and fluorescence intensity information, and the lithium dendrite information can be determined according to the change of the lithium dendrite morphology at different times in the measurement region. In addition, the influence of the changes of other ions and substances in the lithium dendrite growth environment on the lithium dendrite growth can be determined in combination with the change trend of the third Raman spectrum in the measurement region with time, as shown in Figure 10 (b).

[0170] In some embodiments, the change trend of the third Raman spectrum with time includes but is not limited to the change of the Raman characteristic peak intensity, and the generation and disappearance of the characteristic peak.

[0171] In some embodiments, the lithium dendrite information does not refer to a fixed information. The lithium dendrite information includes, but is not limited to, growth conditions and growth rate of the lithium dendrite.

[0172] According to some embodiments, when determining the lithium dendrite growth characteristics according to the trends of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time, the battery impedance spectrum corresponding to the ion battery sample to be measured can be measured before and after the trends of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time are obtained. Then, the lithium dendrite growth characteristics can be measured and analyzed according to the trends of the battery impedance spectrum before and after the measurement and the trends of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time.

[0173] It is easy to understand that when determining the trends of the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement area and the fluorescence spectrum corresponding to the measurement area with time, the lithium dendrite growth characteristics can be determined according to the trends of the battery working signal, the third Raman spectrum and the fluorescence spectrum with time.

[0174] To sum up, the method provided by the embodiments of the present disclosure determines the to-be-tested interface corresponding to the to-be-tested ion battery sample as the negative electrode interface of the to-be-tested ion battery sample, determines the working state corresponding to the to-be-tested ion battery sample as the charging and discharging state, determines the measurement region, controls the first-wavelength laser to focus on the third surface coordinate corresponding to the to-be-tested ion battery sample, controls the second-wavelength laser to focus on the third surface coordinate corresponding to the to-be-tested ion battery sample, drops the target fluorescent reagent on the surface of the to-be-tested ion battery sample, determines the battery working signal corresponding to the to-be-tested ion battery sample, the third Raman spectrum corresponding to the measurement region, and the change trend of the fluorescence spectrum corresponding to the measurement region with time based on the working state, and determines the lithium dendrite growth characteristics according to the change trend of the battery working signal, the third Raman spectrum, and the fluorescence spectrum with time. Therefore, by using the charging and discharging control system and the dual-wavelength photoelectric combined Raman method, in-situ characterization of the lithium dendrite growth morphology and the change of the growth environment at the negative electrode interface during the charging process can be achieved. By scanning the fluorescence signal, the growth process of the lithium dendrite can be imaged in real time, and by quantitatively calibrating the relationship between the fluorescence signal intensity and the lithium dendrite concentration, the amount of lithium deposition can be dynamically detected according to the fluorescence intensity. In addition, by scanning the Raman signal, the ion components and concentration in the lithium dendrite growth environment can be reflected, and the lithium dendrite growth mechanism can be studied. At the same time, by simultaneously obtaining the fluorescence signal and the Raman signal by using dual-wavelength, the short-wavelength laser measures the fluorescence signal, and the long-wavelength laser measures the Raman signal, the mutual interference of the fluorescence detection and the Raman detection can be avoided, the fluorescence and Raman signals at the same position can be quickly separated and obtained, the in-situ, comprehensive, and real-time detection of the ion battery interface performance can be achieved, the in-situ detection of the material component distribution in the lithium dendrite growth environment can be achieved, the influence of the environment on the lithium dendrite growth can be revealed, and the method for inhibiting the lithium dendrite growth can be developed and verified, which has important significance for revealing the lithium dendrite growth mechanism, improving the ion battery life and stability. Moreover, the real-time influence of the interface reaction on the ion transport characteristics and the lithium dendrite growth can be coupled and analyzed, which has important significance for accurately characterizing the ion battery interface characteristics, breaking through the interface bottleneck, and improving the battery performance.

[0175] See Figure 11 , Figure 11 A flowchart of a fourth ion battery interface characteristic comprehensive detection method provided by the embodiments of the present disclosure is shown.

[0176] Specifically, the ion battery interface characteristic comprehensive detection method comprises the following steps.

[0177] S41, determining the to-be-tested interface corresponding to the to-be-tested ion battery sample as the positive electrode interface, the negative electrode interface, or the electrolyte separator interface of the to-be-tested ion battery sample;

[0178] The specific process is as described above, which will not be repeated here.

[0179] S42, determine that the working state of the ion battery sample to be tested is a non-charging and discharging state;

[0180] The specific process is as described above, which will not be repeated here.

[0181] It is easy to understand that when the static interface reaction characteristic detection is performed, the ion battery sample to be tested is in a static process, that is, a standing process when the ion battery sample to be tested is in a non-charging and discharging state. Therefore, the working state of the ion battery sample to be tested can be controlled to be a non-charging and discharging state by controlling the charging and discharging control system to be closed.

[0182] S43, control the first wavelength laser to focus on the fourth surface coordinate corresponding to the ion battery sample to be tested and excite the fourth Raman spectrum, and control the second wavelength laser to focus on the fifth surface coordinate corresponding to the ion battery sample to be tested and excite the fifth Raman spectrum;

[0183] The specific process is as described above, which will not be repeated here.

[0184] According to some embodiments, when the first wavelength laser is controlled to focus on the fourth surface coordinate corresponding to the ion battery sample to be tested and the second wavelength laser is controlled to focus on the fifth surface coordinate corresponding to the ion battery sample to be tested, the fourth surface coordinate and the fifth surface coordinate can be regulated to be located on the same side of the interface to be tested, the fourth interface coordinate and the fifth interface coordinate are regulated not to coincide, the line connecting the fourth interface coordinate and the fifth interface coordinate is regulated to be perpendicular to the interface to be tested, the distance between the fourth interface coordinate and the interface to be tested is regulated to be less than the distance between the fifth interface coordinate and the interface to be tested, and the distance between the fourth interface coordinate and the fifth interface coordinate is regulated to be the preset coordinate distance l.

[0185] In some embodiments, the wavelength λ1 of the first wavelength laser is not equal to the wavelength λ2 of the second wavelength laser, and specifically, the wavelength λ1 of the first wavelength laser is greater than the wavelength λ2 of the second wavelength laser.

[0186] It is easy to understand that when the static interface reaction characteristic detection is performed, the first wavelength laser can be controlled to focus on the fourth surface coordinate corresponding to the ion battery sample to be tested and excite the fourth Raman spectrum, and the second wavelength laser can be controlled to focus on the fifth surface coordinate corresponding to the ion battery sample to be tested and excite the fifth Raman spectrum.

[0187] S44, based on the working state, record the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate at the same time by using time synchronization, to synchronously determine the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time;

[0188] The specific process is as described above, which will not be repeated here.

[0189] According to some embodiments, when the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate are recorded at the same time instant by using time synchronization, the change trend of the fourth Raman spectrum and the fifth Raman spectrum with the time instant can be determined synchronously. When the charging and discharging control system is turned off, the time instant when the first measurement of the ion battery sample to be measured is performed can be taken as the initial 0 time instant, or the time instant when the ion battery sample to be measured is obtained can be selected as the initial 0 time instant. Then, by using the time synchronization control module, the time instant t1 when the measurement is started is recorded after the measurement is started, and at the time instant t1, the spectral signal of the ion battery sample to be measured is excited by using the first wavelength laser and the second wavelength laser respectively to obtain the fourth Raman spectrum information corresponding to the fourth surface coordinate and the fifth Raman spectrum information corresponding to the fifth surface coordinate at the time instant t1. Finally, the measurement step is repeated to further obtain the fourth Raman spectrum information and the fifth Raman spectrum information at the time instants t2, t3, t4, t5, etc. to obtain the change trend of the fourth Raman spectrum and the fifth Raman spectrum with the time instant.

[0190] It is easy to understand that when the first wavelength laser is controlled to focus on the fourth surface coordinate corresponding to the ion battery sample to be measured and the second wavelength laser is controlled to focus on the fifth surface coordinate corresponding to the ion battery sample to be measured, the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate can be recorded at the same time instant by using the time synchronization control module based on the non-charging and discharging state to synchronously determine the change trend of the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate with the time instant.

[0191] S45, determining the static interfacial reaction characteristic according to the change trend of the fourth Raman spectrum and the fifth Raman spectrum with the time instant and the preset coordinate interval.

[0192] The specific process is as described above, which will not be repeated here.

[0193] According to some embodiments, when the change trend of the fourth Raman spectrum and the fifth Raman spectrum with the time instant is obtained, the characteristic peaks of the interfacial reaction products corresponding to the fourth surface coordinate and the fifth surface coordinate can be identified respectively according to the change trend of the fourth Raman spectrum and the fifth Raman spectrum with the time instant to obtain the time instants when the characteristic peaks of the interfacial reaction products appear at the fourth surface coordinate and the fifth surface coordinate respectively. Then, the change trend of the interfacial reaction product concentration corresponding to the fourth surface coordinate and the interfacial reaction product concentration corresponding to the fifth surface coordinate with the measurement time instant can be determined respectively based on the peak intensity analysis of the characteristic peaks of the interfacial reaction products. Finally, the static interfacial reaction speed and the reaction interfacial layer expansion speed corresponding to the ion battery sample to be measured, i.e. the static interfacial reaction characteristic, can be determined in combination with the preset coordinate interval l.

[0194] In some embodiments, during the static process, the positive electrode material or the negative electrode material reacts with the electrolyte to produce new reactants. Then, new characteristic peaks can appear in the Raman spectrum. Since the fourth surface coordinate is closer to the interface to be measured, the characteristic peaks of the interface reaction products will first appear at the fourth surface coordinate. As the measurement time increases and the reaction proceeds, the concentration of the interface reaction products at the fourth surface coordinate increases, and the peak intensity of the characteristic peaks of the interface reaction products increases. Finally, based on the pre-calibrated relationship between the concentration of the reactants and the peak intensity of the characteristic peaks, combined with the measurement time, the static interface reaction rate can be determined. At the same time, as the measurement time increases, the reaction interface layer expands, and the characteristic peaks of the interface reaction products also appear at the fifth surface coordinate. Combined with the preset distance l between the coordinates and the time difference of the appearance of the interface reaction products, the expansion rate of the reaction interface layer in the static process can be determined.

[0195] In some embodiments, in actual measurement, in addition to the peak intensity of the characteristic peaks, the concentration change of the static interface reaction products can also cause changes in the peak position, half-width, etc. The above change relationship can be obtained not only by pre-experiment calibration and first-principle calculation, but also by comparing the impedance spectrum measurement results before and after the reaction to determine the content of the static interface reaction products, and then obtaining the corresponding relationship between the peak intensity, peak position, half-width, etc. of the characteristic peaks of the static interface reaction products and the concentration of the reaction products.

[0196] According to some embodiments, when determining the static interface reaction characteristics according to the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time and the preset distance between the coordinates, the battery impedance spectrum corresponding to the ion battery sample to be measured can be measured before and after the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time is obtained. Then, the static interface reaction characteristics can be measured and analyzed according to the change trend of the battery impedance spectrum before and after the reaction and the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time.

[0197] It is easy to understand that when determining the change trend of the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate with time, the static interface reaction characteristics can be determined according to the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time and the preset distance between the coordinates.

[0198] To sum up, the method provided in the embodiments of the present disclosure determines the to-be-tested interface corresponding to the to-be-tested ion battery sample as the positive electrode interface, the negative electrode interface or the electrolyte separator interface of the to-be-tested ion battery sample; determines the working state corresponding to the to-be-tested ion battery sample as the non-charging and discharging state; controls the first wavelength laser to focus on the fourth surface coordinate corresponding to the to-be-tested ion battery sample, and controls the second wavelength laser to focus on the fifth surface coordinate corresponding to the to-be-tested ion battery sample; determines the change trend of the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate with time based on the working state; and determines the static interface reaction characteristic according to the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time and the preset coordinate distance. By using the dual-wavelength photoelectric combined Raman method, the synchronous acquisition of the multi-position light-electricity signals is realized, and the signals of different measurement positions are distinguished by the two lasers with different wavelengths. In combination with the relative distance between the two measurement positions and the delay time of the Raman characteristic peak change, the comprehensive measurement and research of the battery characteristics in the static process can be realized. In addition, since different substances have different Raman characteristic peaks, this method can also be used to find new chemical reactions and new interface reaction products occurring in different environmental conditions in the static process.

[0199] In the technical solutions of the present disclosure, the collection, storage, use, processing, transmission, provision and disclosure of user personal information involved in the technical solutions comply with relevant laws and regulations and do not violate public order and good customs.

[0200] The following is an embodiment of the device of the present disclosure, which can be used to execute the method embodiments of the present disclosure. For details not disclosed in the device embodiments of the present disclosure, please refer to the method embodiments of the present disclosure.

[0201] Please refer to Figure 12 which shows the structure schematic diagram of the first ion battery interface characteristic comprehensive detection device provided by the embodiments of the present disclosure.

[0202] Specifically, the ion battery interface characteristic comprehensive detection device comprises a dual-wavelength spectrum measurement system, a charging and discharging control system, an environment regulation system and a data synchronous analysis system; wherein,

[0203] The environment regulation system is configured to determine the to-be-tested interface corresponding to the to-be-tested ion battery sample.

[0204] The charging and discharging control system is configured to determine the working state corresponding to the to-be-tested ion battery sample.

[0205] The data synchronous analysis system is configured to determine the ion battery interface characteristic corresponding to the to-be-tested interface by the dual-wavelength spectrum measurement system using the dual-wavelength photoelectric combined Raman method based on the working state.

[0206] In the embodiments of the present disclosure, Figure 13A structure schematic diagram of a second ion battery interface property comprehensive detection device provided by an embodiment of the present disclosure is shown. As shown in Figure 13 The environmental regulation system includes a sample cavity 400, a temperature control platform 401, an atmosphere regulation platform 402, and a displacement platform 403; wherein,

[0207] The sample cavity 400 is used for placing an ion battery sample to be tested 000.

[0208] The temperature control platform 401 is connected with the sample cavity 400, and is used for controlling the temperature in the sample cavity 400.

[0209] The atmosphere regulation platform 402 is connected with the sample cavity 400, and is used for controlling the atmosphere environment in the sample cavity 400.

[0210] The displacement platform 403 is connected with the sample cavity 400, and is used for adjusting the position of the ion battery sample to be tested 000.

[0211] In the embodiment of the present disclosure, as shown in Figure 13 The dual-wavelength spectrum measurement system includes a first continuous laser 101, a second continuous laser 102, a first narrow-band pass filter 010, a second narrow-band pass filter 011, a scanning galvanometer 030, a selective lens 040, an objective lens 050, a first filter 012, a second filter 013, a spectrum detection device 500, and at least one mirror 020; wherein,

[0212] The first continuous laser 101 is used for generating first-wavelength continuous detection laser.

[0213] The second continuous laser 102 is used for generating second-wavelength continuous detection laser.

[0214] The first narrow-band pass filter 010 is used for improving the beam quality of the first-wavelength continuous detection laser, to obtain first-wavelength laser.

[0215] The second narrow-band pass filter 020 is used for improving the beam quality of the second-wavelength continuous detection laser, to obtain second-wavelength laser.

[0216] The scanning galvanometer 030 is used for receiving the first-wavelength laser and reflecting the first-wavelength laser.

[0217] The selective lens 040 is used for receiving the first-wavelength laser reflected by the scanning galvanometer and receiving the second-wavelength laser.

[0218] The objective lens 050 is used for receiving the first-wavelength laser and the second-wavelength laser incident by the selective lens, focusing the first-wavelength laser and the second-wavelength laser on the ion battery sample to be tested, and receiving the Raman spectrum excited by the first-wavelength laser and the second-wavelength laser.

[0219] A first filter 012 is configured to eliminate Rayleigh scattering of the first wavelength laser in the Raman spectrum.

[0220] A second filter 013 is configured to eliminate Rayleigh scattering of the second wavelength laser in the Raman spectrum.

[0221] A spectral detection device 500 is configured to receive the filtered Raman spectrum and fluorescence spectrum, and perform spectral detection on the filtered Raman spectrum and fluorescence spectrum.

[0222] At least one mirror 020 is configured to construct an optical path.

[0223] According to some embodiments, the displacement platform 403 can be adjusted together with the scanning galvanometer 030 to adjust the focusing position of the first wavelength laser and the second wavelength laser on the ion battery sample 000 to be measured.

[0224] In some embodiments, the first filter 010 and the second filter 020 can be notch filters.

[0225] In some embodiments, the selective lens 040 can include a half-transmission half-reflection mirror, a partial-transmission partial-reflection mirror with a preset ratio, and a 45-degree cutoff filter. The cutoff wavelength of the 45-degree cutoff filter is λ2.

[0226] In the embodiments of the present disclosure, as shown in Figure 13 The charge-discharge control system includes a battery test platform 200 and an electrochemical workstation 201, the data synchronization analysis system includes a time synchronization control module and a data analysis module 700, the time synchronization control module includes an instrument synchronization control submodule 300 and a timing recording submodule 600; wherein,

[0227] The battery test platform 200 is configured to control the charge-discharge state of the ion battery sample to be measured, and record the battery working signal of the ion battery sample to be measured, wherein the charge-discharge state includes a constant current charging state, a constant voltage charging state, a constant current discharging state, and a static state.

[0228] The electrochemical workstation 201 is connected with the battery test platform 200, and is configured to detect the impedance spectrum of the ion battery sample to be measured in situ.

[0229] The instrument synchronization control submodule 300 is connected with the battery test platform 200 and the dual-wavelength spectral measurement system, and is configured to synchronize the detection time of the battery test platform 200 and the dual-wavelength spectral measurement system.

[0230] The timing recording submodule 600 is connected with the instrument synchronization control submodule 300, and is configured to record the battery working signal of the ion battery sample to be measured recorded by the battery test platform, the spectral signal recorded by the dual-wavelength spectral measurement system, and the detection time corresponding to the battery working signal and the spectral signal.

[0231] The data analysis module 700 is connected with the timing recording sub-module 600, and is configured to analyze the spectrum signal and the battery working signal corresponding to the detection time, and determine the ion battery interface characteristic corresponding to the interface to be detected.

[0232] According to some embodiments, the electrochemical workstation 201 can realize in-situ detection of the impedance spectrum of the ion battery sample to be detected during the measurement process and before and after the measurement.

[0233] In some embodiments, when the data analysis module 700 analyzes the spectrum signal and the battery working signal corresponding to the detection time, and determines the ion battery interface characteristic corresponding to the interface to be detected, the data analysis module 700 can also process and analyze the Raman spectrum signal and the fluorescence signal, the voltage signal, the current signal, the alternating current impedance spectrum information and the time information excited by the first wavelength laser and the second wavelength laser at the same time.

[0234] In the embodiments of the present disclosure, the data analysis module 700 includes a static interface reaction data analysis sub-module, a dynamic interface reaction and energy carrier sub-transport process data analysis sub-module, and a lithium dendrite growth process data analysis sub-module; wherein,

[0235] The static interface reaction data analysis sub-module is configured to analyze the static interface reaction speed and the reaction interface layer expansion speed.

[0236] The dynamic interface reaction and energy carrier sub-transport process data analysis sub-module is configured to analyze the dynamic interface reaction speed, the reaction interface layer expansion speed and the ion-electron coupling transport process.

[0237] The lithium dendrite growth process data analysis sub-module is configured to analyze the growth of the lithium dendrite, the growth speed, and the changes of other ions and substances in the environment of the lithium dendrite growth.

[0238] It should be noted that the ion battery interface characteristic comprehensive detection device provided in the above embodiments is only used as an example for the division of the above functional modules when the ion battery interface characteristic comprehensive detection method is executed. In actual applications, the above functions can be completed by different functional modules according to needs, that is, the internal structure of the device is divided into different functional modules to complete all or part of the functions described above. In addition, the ion battery interface characteristic comprehensive detection device and the ion battery interface characteristic comprehensive detection method provided in the above embodiments belong to the same concept, and the implementation process is described in detail in the method embodiments. Therefore, it is not repeated here.

[0239] The serial numbers of the above embodiments of the present disclosure are only for description, and do not represent the advantages and disadvantages of the embodiments.

[0240] In summary, the apparatus proposed in this disclosure determines the interface to be tested for the ion battery sample through an environmental control system; determines the operating state of the ion battery sample through a charge-discharge control system; and determines the interface characteristics of the ion battery corresponding to the interface to be tested based on the operating state through a dual-wavelength spectral measurement system using a dual-wavelength photoelectric Raman method. Therefore, the dual-wavelength spectral measurement system, charge-discharge control system, and data synchronization analysis system enable simultaneous detection of multi-position Raman spectroscopy, fluorescence spectroscopy, voltage signals, and current signals. Furthermore, the data synchronization analysis system enables automated processing of optical signals, electrical signals, AC impedance spectroscopy information, and time information. Simultaneously, combined with the environmental control system, the ambient temperature and atmosphere of the sample can be controlled. Furthermore, combined with impedance spectroscopy detection, in-situ measurements of the ion battery interface reaction characteristics, ion-electron coupling transport characteristics, and lithium dendrite growth characteristics under multi-factor coupling can be achieved, revealing the coupling effects between various factors and realizing comprehensive, in-situ, and real-time measurement of the ion battery interface characteristics.

[0241] The acquisition, storage, and application of user personal information involved in the technical solution disclosed herein comply with the provisions of relevant laws and regulations and do not violate public order and good morals.

[0242] According to embodiments of this disclosure, this disclosure also provides a comprehensive detection device for the interface characteristics of ion batteries, a readable storage medium, and a computer program product.

[0243] Figure 14 A schematic block diagram of an example ion battery interface characteristic comprehensive detection device 1400 that can be used to implement embodiments of the present disclosure is shown. The components shown herein, their connections and relationships, and their functions are merely examples and are not intended to limit the implementation of the present disclosure described and / or claimed herein.

[0244] like Figure 14 As shown, the ion battery interface characteristic comprehensive testing device 1400 includes a computing unit 1401, which can perform various appropriate actions and processes according to a computer program stored in a read-only memory (ROM) 1402 or a computer program loaded from a storage unit 1408 into a random access memory (RAM) 1403. The RAM 1403 can also store various programs and data required for the operation of the ion battery interface characteristic comprehensive testing device 1400. The computing unit 1401, ROM 1402, and RAM 1403 are interconnected via a bus 1404. An input / output (I / O) interface 1405 is also connected to the bus 1404.

[0245] The plurality of components in the ion battery interface property comprehensive detection apparatus 1400 are connected to the I / O interface 1405, including: an input unit 1406, such as a keyboard, a mouse, and the like; an output unit 1407, such as various types of displays, speakers, and the like; a storage unit 1408, such as a magnetic disk, an optical disk, and the like; and a communication unit 1409, such as a network card, a modem, a wireless communication transceiver, and the like. The communication unit 1409 allows the ion battery interface property comprehensive detection apparatus 1400 to exchange information / data with other devices through a computer network, such as the Internet, and / or various telecommunication networks.

[0246] The computing unit 1401 can be various general and / or special-purpose processing components with processing and computing capabilities. Some examples of the computing unit 1401 include, but are not limited to, a central processing unit (CPU), a graphics processing unit (GPU), various special-purpose artificial intelligence (AI) computing chips, various computing units running machine learning model algorithms, a digital signal processor (DSP), and any appropriate processor, controller, microcontroller, and the like. The computing unit 1401 performs various methods and processes described above, such as the ion battery interface property comprehensive detection method. For example, in some embodiments, the ion battery interface property comprehensive detection method can be implemented as a computer software program, which is tangibly embodied in a machine-readable medium, such as the storage unit 1408. In some embodiments, part or all of the computer program can be loaded and / or installed onto the ion battery interface property comprehensive detection apparatus 1400 via the ROM 1402 and / or the communication unit 1409. When the computer program is loaded onto the RAM 1403 and executed by the computing unit 1401, one or more steps of the ion battery interface property comprehensive detection method described above can be performed. Alternatively, in other embodiments, the computing unit 1401 can be configured to perform the ion battery interface property comprehensive detection method by any other appropriate means, such as by means of firmware.

[0247] Various implementations of the systems and techniques described above can be realized in digital electronic circuitry, integrated circuitry, a field programmable gate array (FPGA), an application specific integrated circuit (ASIC), a system on a chip (SOC), a programmable logic device (CPLD), computer hardware, firmware, software, and / or combinations thereof. These various implementations can include implementation in one or more computer programs that are executable and / or interpretable on a programmable system including at least one programmable processor, which can be special or general purpose, coupled to receive data and instructions from, and to transmit data and instructions to, a storage system, at least one input device, and at least one output device.

[0248] Program code for carrying out methods of the present disclosure can be written in any combination of one or more programming languages. The program code can be provided to a processor or controller of a general purpose computer, special purpose computer, or other programmable data processing apparatus to produce a machine, such that the program code, when executed by the processor or controller, produces the functions / operations specified in the flowcharts and / or block diagrams. The program code can be executed entirely on a machine, partially on a machine, partially on a machine as a stand-alone software package, or entirely on a remote machine or off-the-shelf battery interface characteristics comprehensive detection device.

[0249] In the context of the present disclosure, a machine-readable medium can be a tangible medium that can contain or store program for use by or in connection with an instruction execution system, apparatus, or device. The machine-readable medium can be a machine-readable signal medium or a machine-readable storage medium. Machine-readable storage medium can include, without limitation, electronic, magnetic, optical, electromagnetic, infrared, or semiconductor system, apparatus, or device, or any suitable combination of the foregoing. More specific examples of the machine-readable storage medium will include one or more lines of electrical connections, portable computer disks, hard disk, random access memory (RAM), read-only memory (ROM), erasable programmable read-only memory (EPROM or Flash memory), optical fibers, portable compact disc read-only memory (CD-ROM), optical storage device, magnetic storage device, or any suitable combination of the foregoing.

[0250] To provide for interaction with a user, the systems and techniques described here can be implemented on a computer having a display device (e.g., a CRT (cathode ray tube) or LCD (liquid crystal display) monitor) for displaying information to the user and a keyboard and a pointing device (e.g., a mouse or a trackball) by which the user can provide input to the computer. Other kinds of devices can be used to provide for interaction with a user as well; for example, feedback provided to the user can be any form of sensory feedback (e.g., visual feedback, auditory feedback, or tactile feedback); and input from the user can be received in any form, including acoustic, speech, or tactile input.

[0251] The systems and techniques described here can be implemented in a computing system that includes a back end component (e.g., as a data ion battery interface characteristic comprehensive detection apparatus), or that includes a middleware component (e.g., an application ion battery interface characteristic comprehensive detection apparatus), or that includes a front end component (e.g., a user computer having a graphical user interface or a Web browser through which a user can interact with an implementation of the systems and techniques described here), or any combination of such back end, middleware, or front end components. The components of the system can be interconnected by any form or medium of digital data communication (e.g., a communication network). Examples of communication networks include a local area network (LAN), a wide area network (WAN), the Internet, and a blockchain network.

[0252] The computer system can include clients and ion battery interface characteristic comprehensive detection apparatuses. The clients and ion battery interface characteristic comprehensive detection apparatuses are generally remote from each other and typically interact through a communication network. The relationship of the clients and ion battery interface characteristic comprehensive detection apparatuses with each other is often through a computer program running on each computer and having a client-ion battery interface characteristic comprehensive detection apparatus relationship to the other computers. The ion battery interface characteristic comprehensive detection apparatus can be a cloud ion battery interface characteristic comprehensive detection apparatus, also known as a cloud computing ion battery interface characteristic comprehensive detection apparatus or a cloud host, which is a host product in the cloud computing service system to solve the defects of large management difficulty and weak business scalability in traditional physical hosts and VPS services ("Virtual Private Server", or simply "VPS"). The ion battery interface characteristic comprehensive detection apparatus can also be a distributed system ion battery interface characteristic comprehensive detection apparatus or a blockchain combined ion battery interface characteristic comprehensive detection apparatus.

[0253] It should be understood that various forms of flow shown above can be used to reorder, add, or delete steps. For example, each step described in the present disclosure can be executed in parallel, sequentially, or in a different order, as long as the desired results of the technical solutions disclosed in the present disclosure can be achieved, and the present disclosure is not limited herein.

[0254] The above detailed description does not constitute a limitation on the protection scope of the present disclosure. Those skilled in the art should understand that various modifications, combinations, sub-combinations, and substitutions can be made according to design requirements and other factors. Any modifications, equivalent replacements, and improvements made within the spirit and principles of the present disclosure shall be included in the protection scope of the present disclosure.

Claims

1. A method for comprehensive detection of ion battery interface characteristics, characterized in that, The method comprises the following steps: determining a to-be-tested interface corresponding to a to-be-tested ion battery sample; determining a working state corresponding to the to-be-tested ion battery sample; determining an ion battery interface characteristic corresponding to the to-be-tested interface based on the working state by using a dual-wavelength photoelectric combined Raman method; the ion battery interface characteristic comprises a dynamic interface reaction characteristic, a carrier energy sub-transport characteristic, a static interface reaction characteristic, and a lithium dendrite growth characteristic; when the dynamic interface reaction characteristic and the carrier energy sub-transport characteristic are determined, the method comprises the following steps: controlling a first-wavelength laser to focus on a first surface coordinate corresponding to the to-be-tested ion battery sample and to excite a first Raman spectrum, and controlling a second-wavelength laser to focus on a second surface coordinate corresponding to the to-be-tested ion battery sample and to excite a second Raman spectrum; the first surface coordinate and the second surface coordinate are located on the same side of the to-be-tested interface, the first surface coordinate and the second surface coordinate are not coincident, a line connecting the first surface coordinate and the second surface coordinate is perpendicular to the to-be-tested interface, a distance between the first surface coordinate and the second surface coordinate is a preset coordinate distance, a distance between the first surface coordinate and the to-be-tested interface is smaller than a distance between the second surface coordinate and the to-be-tested interface, and a wavelength of the first-wavelength laser is greater than a wavelength of the second-wavelength laser; based on the working state, recording a battery working signal corresponding to the to-be-tested ion battery sample, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time by using time synchronization, so as to synchronously determine variation trends of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time; determining the dynamic interface reaction characteristic and the carrier energy sub-transport characteristic according to the variation trends of the battery working signal, the first Raman spectrum, and the second Raman spectrum with time and the preset coordinate distance; when the lithium dendrite growth characteristic is determined, the method comprises the following steps: dropping a target fluorescent reagent on a surface of the to-be-tested ion battery sample; determining a measurement region, controlling a first-wavelength laser to focus on a third surface coordinate corresponding to the to-be-tested ion battery sample and to excite a third Raman spectrum, and controlling a second-wavelength laser to focus on the third surface coordinate corresponding to the to-be-tested ion battery sample and to excite a fluorescent spectrum; the third surface coordinate is located in the measurement region, and a wavelength of the first-wavelength laser is greater than a wavelength of the second-wavelength laser; based on the working state, recording a battery working signal corresponding to the to-be-tested ion battery sample, the third Raman spectrum corresponding to the measurement region, and the fluorescent spectrum corresponding to the measurement region at the same time by using time synchronization, so as to synchronously determine variation trends of the battery working signal, the third Raman spectrum, and the fluorescent spectrum with time; determining the lithium dendrite growth characteristic according to the variation trends of the battery working signal, the third Raman spectrum, and the fluorescent spectrum with time.

2. The method of claim 1, wherein, The method for determining the to-be-tested interface corresponding to the to-be-tested ion battery sample comprises the following steps: determining the working state of the ion battery sample to be tested when the dynamic interfacial reaction characteristic, the carrier energy sub-transport characteristic and the static interfacial reaction characteristic corresponding to the ion battery sample to be tested are determined; determining the negative electrode interface of the ion battery sample to be tested when the lithium dendrite growth characteristic corresponding to the ion battery sample to be tested is determined.

3. The method of claim 1, wherein, The determination of the working state of the ion battery sample to be tested comprises: determining the working state of the ion battery sample to be tested as a charging and discharging state when the dynamic interfacial reaction characteristic, the carrier energy sub-transport characteristic and the lithium dendrite growth characteristic corresponding to the ion battery sample to be tested are determined; determining the working state of the ion battery sample to be tested as a non-charging and discharging state when the static interfacial reaction characteristic corresponding to the ion battery sample to be tested is determined.

4. The method of claim 1, wherein, In the determination of the static interfacial reaction characteristic, it comprises: controlling the first wavelength laser to focus on the fourth surface coordinate corresponding to the ion battery sample to be tested and excite the fourth Raman spectrum, and controlling the second wavelength laser to focus on the fifth surface coordinate corresponding to the ion battery sample to be tested and excite the fifth Raman spectrum, wherein the fourth surface coordinate and the fifth surface coordinate are located on the same side of the interface to be tested, the fourth surface coordinate and the fifth surface coordinate do not coincide, the line connecting the fourth surface coordinate and the fifth surface coordinate is perpendicular to the interface to be tested, the distance between the fourth surface coordinate and the fifth surface coordinate is a preset coordinate distance, the distance between the fourth surface coordinate and the interface to be tested is less than the distance between the fifth surface coordinate and the interface to be tested, and the wavelength of the first wavelength laser is greater than the wavelength of the second wavelength laser; based on the working state, using time synchronization, recording the fourth Raman spectrum corresponding to the fourth surface coordinate and the fifth Raman spectrum corresponding to the fifth surface coordinate at the same time, to synchronously determine the change trend of the fourth Raman spectrum and the fifth Raman spectrum with time; determining the static interfacial reaction characteristic according to the change trend of the fourth Raman spectrum, the fifth Raman spectrum with time and the preset coordinate distance.

5. An ion battery interface property comprehensive detection device, characterized in that, It comprises: a dual-wavelength spectral measurement system, a charging and discharging control system, an environment control system and a data synchronization analysis system; wherein the environment control system is used to determine the interface to be tested corresponding to the ion battery sample to be tested; the ion battery interface characteristics include dynamic interfacial reaction characteristic, carrier energy sub-transport characteristic and static interfacial reaction characteristic and lithium dendrite growth characteristic; the charging and discharging control system is used to determine the working state of the ion battery sample to be tested; the data synchronization analysis system is used to determine the ion battery interface characteristics corresponding to the interface to be tested by the dual-wavelength spectral measurement system using the dual-wavelength photoelectric combined Raman method based on the working state; the ion battery interface characteristics include dynamic interfacial reaction characteristic, carrier energy sub-transport characteristic and static interfacial reaction characteristic and lithium dendrite growth characteristic; In the determination of the dynamic interfacial reaction characteristic, the carrier energy sub-transport characteristic, it comprises: control the first wavelength laser to focus on a first surface coordinate corresponding to the ion battery sample to be measured and excite a first Raman spectrum, and control the second wavelength laser to focus on a second surface coordinate corresponding to the ion battery sample to be measured and excite a second Raman spectrum, wherein the first surface coordinate and the second surface coordinate are located on the same side of the interface to be measured, the first surface coordinate and the second surface coordinate are not coincident, the line connecting the first surface coordinate and the second surface coordinate is perpendicular to the interface to be measured, the distance between the first surface coordinate and the second surface coordinate is a preset coordinate distance, the distance between the first surface coordinate and the interface to be measured is less than the distance between the second surface coordinate and the interface to be measured, and the wavelength of the first wavelength laser is greater than the wavelength of the second wavelength laser; based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the first Raman spectrum corresponding to the first surface coordinate, and the second Raman spectrum corresponding to the second surface coordinate at the same time, to determine the change trend of the battery working signal, the first Raman spectrum and the second Raman spectrum with time synchronously; determine the dynamic interface reaction characteristic and the energy carrier transport characteristic according to the change trend of the battery working signal, the first Raman spectrum, the second Raman spectrum with time and the preset coordinate distance; when determining the lithium dendrite growth characteristic, the method comprises: dropping a target fluorescent reagent on the surface of the ion battery sample to be measured; determining a measurement region, controlling the first wavelength laser to focus on a third surface coordinate corresponding to the ion battery sample to be measured and excite a third Raman spectrum, and controlling the second wavelength laser to focus on the third surface coordinate corresponding to the ion battery sample to be measured and excite a fluorescent spectrum, wherein the third surface coordinate is located in the measurement region, and the wavelength of the first wavelength laser is greater than the wavelength of the second wavelength laser; based on the working state, using time synchronization, recording the battery working signal corresponding to the ion battery sample to be measured, the third Raman spectrum corresponding to the measurement region, and the fluorescent spectrum corresponding to the measurement region at the same time, to determine the change trend of the battery working signal, the third Raman spectrum and the fluorescent spectrum with time synchronously; determine the lithium dendrite growth characteristic according to the change trend of the battery working signal, the third Raman spectrum and the fluorescent spectrum with time.

6. The apparatus of claim 5, wherein, The environment regulation system comprises a sample cavity, a temperature control platform, an atmosphere regulation platform and a displacement platform; wherein, the sample cavity is used to place the ion battery sample to be measured; the temperature control platform is connected with the sample cavity and is used to control the temperature in the sample cavity; the atmosphere regulation platform is connected with the sample cavity and is used to control the atmosphere environment in the sample cavity; the displacement platform is connected with the sample cavity and is used to adjust the position of the ion battery to be measured.

7. The apparatus of claim 5, wherein, The dual-wavelength spectral measurement system comprises a first continuous laser, a second continuous laser, a first narrow-band pass filter, a second narrow-band pass filter, a scanning galvanometer, a selective lens, an objective lens, a first filter, a second filter, a spectral detection device, and at least one mirror. The first continuous laser is configured to generate first-wavelength continuous probe laser. The second continuous laser is configured to generate second-wavelength continuous probe laser. The first narrow-band pass filter is configured to improve the beam quality of the first-wavelength continuous probe laser to obtain first-wavelength laser. The second narrow-band pass filter is configured to improve the beam quality of the second-wavelength continuous probe laser to obtain second-wavelength laser. The scanning galvanometer is configured to receive the first-wavelength laser and reflect the first-wavelength laser. The selective lens is configured to receive the first-wavelength laser reflected by the scanning galvanometer and the second-wavelength laser. The objective lens is configured to receive the first-wavelength laser and the second-wavelength laser transmitted by the selective lens, focus the first-wavelength laser and the second-wavelength laser on the ion battery sample to be measured, and receive Raman spectrum excited by the first-wavelength laser and the second-wavelength laser. The first filter is configured to eliminate Rayleigh scattering excited by the first-wavelength laser in the Raman spectrum. The second filter is configured to eliminate Rayleigh scattering excited by the second-wavelength laser in the Raman spectrum. The spectral detection device is configured to receive the filtered Raman spectrum and fluorescence spectrum, and perform spectral detection on the filtered Raman spectrum and the fluorescence spectrum. The at least one mirror is configured to construct an optical path.

8. The apparatus of claim 5, wherein, The charge and discharge control system comprises a battery test platform and an electrochemical workstation, the data synchronous analysis system comprises a time synchronization control module and a data analysis module, and the time synchronization control module comprises an instrument synchronization control submodule and a timing recording submodule. The battery test platform is configured to control the charge and discharge state of the ion battery sample to be measured and record the battery working signal of the ion battery sample to be measured, wherein the charge and discharge state comprises a constant-current charging state, a constant-voltage charging state, a constant-current discharging state, and a standing state. The electrochemical workstation is connected with the battery test platform and is configured to detect the impedance spectrum of the ion battery sample to be measured in situ. The instrument synchronization control submodule is connected with the battery test platform and the dual-wavelength spectral measurement system, respectively, and is configured to synchronize the detection time of the battery test platform and the dual-wavelength spectral measurement system. The timing recording submodule is connected with the instrument synchronization control submodule and is configured to record the battery working signal of the ion battery sample to be measured recorded by the battery test platform, the spectral signal recorded by the dual-wavelength spectral measurement system, and the detection time corresponding to the battery working signal and the spectral signal. The data analysis module is connected with the timing recording submodule, and is configured to analyze the spectrum signal and the battery operation signal corresponding to the detection time, and determine the ion battery interface characteristic corresponding to the interface to be measured.

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