In-situ synchrotron radiation transmission-type XAS battery testing device

Abstract

The utility model relates to an in-situ synchrotron radiation transmission type XAS battery testing device, which comprises a battery mould, the battery mould comprises a sealing cover, a main shell and a base, the sealing cover comprises a sleeve part inserted into the main shell, a first beryllium window is arranged at the lower end of the sleeve part, the base is fixedly arranged at the lower end of the main shell, and a second beryllium window is arranged in the middle of the base. A sealed space for containing the battery assembly is formed among the sleeve part, the main shell and the base, the upper side of the battery assembly is provided with a negative electrode making contact with the first beryllium window, and the lower side of the battery assembly is provided with a positive electrode making contact with the second beryllium window. And the base is provided with a positive lead connected with the charge-discharge instrument. According to the in-situ synchrotron radiation transmission-type XAS testing device, the combination of an electrochemical performance test and an in-situ synchrotron radiation transmission-type XAS test is realized, and the negative lead and the positive lead are respectively connected to the limiting flange part at the upper end of the sealing cover and the base, so that the sealing performance of an internal electrochemical cell cannot be damaged.

Description

TECHNICAL FIELD

[0001] The utility model relates to in situ electrochemistry reaction pool and in situ test technical field, concretely in situ synchrotron transmission type XAS battery test device. BACKGROUND

[0002] Developing high energy density, high safety lithium ion battery is one of key problems to meet the rapid development of electric vehicle industry, and the specific capacity of the anode material is too low to cause the main reason of the lithium ion battery energy density cannot be improved. In recent years, researchers have developed a series of NiCoMn ternary materials and lithium-rich manganese-based anode materials to meet the demand of people for large capacity, high rate battery, however, research found that the battery composed of these anode materials exhibits short cycle life, poor rate performance, low coulomb efficiency and other shortcomings in the test process, and in order to solve the above defects of the anode material, it is necessary to clarify the structure-activity relationship between the material properties and the electrochemical performance evolution of the anode material, and reveal the influence relationship between the anode material properties such as chemical composition, material morphology, lattice structure, element distribution, ion transport characteristics and apparent electrochemical performance of the anode material during the battery charging and discharging process, in order to develop targeted material property improvement and improvement strategy to further improve the battery performance.

[0003] Synchrotron X-ray absorption spectroscopy (X-ray absorption spectroscopy) technology is a characterization method for studying material structure and specific element valence, which continuously collects the signal of X-ray transmitted through the sample before and after the specific element absorption edge, and records the relationship between transmitted light intensity and incident light energy, so that the absorption spectrum of the specific element can be obtained, and because the absorption edge of the element corresponds to the energy of the inner level electron of the element, the technology can also be used to identify the element species, in addition, the absorption spectrum will shift with the change of the element valence, accordingly, the change of the element valence can be characterized, the two-dimensional spectral imaging technology formed by further combining the technology with X-ray two-dimensional imaging technology can obtain two-dimensional distribution information of element and valence at the same time.

[0004] But the structure of the in-situ electrochemical cell matched with the synchrotron radiation XAS technology in the prior art still needs to be further optimized, for example, the in-situ electrochemical electrolytic cell suitable for the synchrotron radiation XAS test disclosed in CN212646538U mainly comprises a first end cover, a second end cover and a light-transmitting assembly, the first end cover and the second end cover are oppositely arranged to form a working electrode groove and a counter electrode groove, etc., however, the electrochemical cell does not arrange an electrode current collector, and is not suitable for testing sheet-shaped electrode materials. For another example, the electrochemical reaction cell for X-ray in-situ two-dimensional imaging disclosed in CN210863593U mainly comprises an upper pressing head, a lower pressing head and an electrode assembly, although the electrochemical cell arranges a circular titanium foil and a ring-shaped copper foil as the current collector, however, the two electrode leads are directly led out from the sealing ring between the upper pressing head and the lower pressing head, which to some extent damages the sealing performance of the electrochemical cell. Practical new type content

[0005] The utility model discloses a kind of in-situ synchrotron radiation transmission type XAS cell test devices, which realizes the combination of electrochemical performance test and in-situ synchrotron radiation transmission type XAS test, and negative pole lead and positive pole lead are respectively connected on the limiting flange portion of the upper end of sealing cover and base, without damaging the sealing performance of internal electrochemical cell.

[0006] The utility model discloses a kind of in-situ synchrotron radiation transmission type XAS cell test devices, which realizes the combination of electrochemical performance test and in-situ synchrotron radiation transmission type XAS test, and negative pole lead and positive pole lead are respectively connected on the limiting flange portion of the upper end of sealing cover and base, without damaging the sealing performance of internal electrochemical cell.

[0007] The utility model discloses a kind of in-situ synchrotron radiation transmission type XAS cell test devices, including battery mould, and the battery mould includes sealing cover, main shell and base, wherein sealing cover includes sleeve portion inserted into main shell, and the lower end middle part of the sleeve portion is equipped with first beryllium window, the base is fixed to the lower end of the main shell and is equipped with second beryllium window in middle part, the sleeve portion, main shell and base form the sealed space of accommodating battery assembly between, and the negative pole of battery assembly upper side is contacted with first beryllium window, the positive pole of lower side is contacted with second beryllium window, the sleeve portion upper end is equipped with the limiting flange portion located in the upper side of main shell, and the limiting flange portion is equipped with negative pole lead and is connected with charge-discharge instrument, the base is equipped with positive pole lead and is connected with charge-discharge instrument.

[0008] The circumferential outer side of the lower end of the sleeve portion is equipped with the first sealing ring between the main shell, and the upper side of the base is equipped with the second sealing ring between the lower end surface of the main shell.

[0009] The inner wall of the through hole for the sleeve portion to insert in the main shell is equipped with the first sealing groove for installing the first sealing ring, the lower end surface of the main shell is equipped with the second sealing groove for installing the second sealing ring, and the upper surface of the base is equipped with the third sealing groove for installing the second sealing ring.

[0010] The base is fixed to the lower end of the main shell by bolt.

[0011] The lower end of the sleeve part is provided with a lower sealing platform, and the lower sealing platform comprises a window positioning ring, the first beryllium window is arranged in the window positioning ring, and the window positioning ring is fixedly connected with the sleeve part.

[0012] The battery mold is arranged in a battery mold support, the battery mold support comprises a mounting sleeve for accommodating the battery mold, and the mounting sleeve is provided with fastening bolts on the circumferential wall, and the lower side of the mounting sleeve is provided with a supporting rod.

[0013] The utility model discloses the advantages and positive effects are:

[0014] 1. The utility model discloses the combination of electrochemical performance test and in-situ synchrotron radiation transmission type XAS test can realize the characterization of positive material element distribution, valence state evolution and microstructure in the process of battery charging and discharging, and dynamically tracks the failure evolution process of positive material, and the negative lead and the positive lead are connected on the limiting flange part on the upper end of the sealing cover and the base respectively, and the sealing performance of the internal electrochemical cell is not damaged.

[0015] 2. The utility model discloses that the positive pole and the negative pole of electrode assembly are contacted with corresponding beryllium window with low X ray absorption ability, which not only eliminates the use of additional current collector, improves the penetration ability of X ray to obtain high-quality characterization results, but also eliminates additional electrode lead in the battery, and thus makes it possible to directly lead out the electrode lead outside the battery mold and connect with the charging and discharging instrument. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is the use state schematic diagram of the utility model,

[0017] Figure 2 It is Figure 1 The structural section view of battery mold,

[0018] Figure 3 It is Figure 2 The structural schematic diagram of sealing cover,

[0019] Figure 4 It is Figure 3 The structural schematic diagram of lower sealing platform,

[0020] Figure 5 It is Figure 2 The structural schematic diagram of main shell,

[0021] Figure 6 It is Figure 2 The structural top view of base,

[0022] Figure 7 It is Figure 2Structure diagram of middle battery assembly,

[0023] Figure 8 For Figure 1 Structure diagram of middle battery mold support.

[0024] Wherein, 1 is a battery mold, 101 is a sealing cover, 1011 is a lower sealing table, 10111 is a first beryllium window, 10112 is a window positioning ring, 1012 is a negative lead, 1013 is a ray channel, 1014 is a limiting flange part, 1015 is a sleeve part, 102 is a main shell, 1021 is a through hole, 1022 is a first sealing groove, 1023 is a second sealing groove, 1024 is a screw hole, 103 is a base, 1031 is a second beryllium window, 1032 is a positive lead, 1033 is a third sealing groove, 104 is a battery assembly, 1041 is a negative electrode, 1042 is a diaphragm, 1043 is a positive electrode, 2 is a battery mold support, 201 is a fastening bolt, 202 is a mounting sleeve, 203 is a support rod, 3 is a charge-discharge instrument, 4 is an X-ray, 5 is a first sealing ring, 6 is a second sealing ring, 7 is a bolt. DETAILED DESCRIPTION

[0025] The utility model will be further described in connection with the drawings.

[0026] As Figures 1-8 shown, the utility model includes battery mold 1, and as Figures 2-7 shown, battery mold 1 includes sealing cover 101, main shell 102 and base 103, wherein sealing cover 101 includes sleeve part 1015 inserted into main shell 102, and the lower end middle part of sleeve part 1015 is equipped with first beryllium window 10111, base 103 is fixed to the lower end of main shell 102 and is equipped with second beryllium window 1031 in the middle part, a sealing space is formed between sleeve part 1015, main shell 102 and base 103, and battery assembly 104 is arranged in the sealing space, as Figure 2 and Figure 7 shown, the upper side of battery assembly 104 is equipped with negative electrode 1041 and contacts first beryllium window 10111, and the lower side is equipped with positive electrode 1043 and contacts second beryllium window 1031, the upper end of sleeve part 1015 is equipped with limiting flange part 1014 located in the upper side of main shell 102, and limiting flange part 1014 is equipped with negative lead 1012 and is connected with charge-discharge instrument 3, and base 103 is equipped with positive lead 1032 and is connected with charge-discharge instrument 3.

[0027] When the utility model works, as Figures 1-2As shown, the sleeve part 1015 is formed with a radiation channel 1013 for the X-ray 4 to pass through, and the X-ray 4 sequentially passes through the first beryllium window 10111, the battery assembly 104 and the second beryllium window 1031, and the charge-discharge instrument 3 cooperates with the battery assembly 104 to carry out in-situ XAS test for charging and discharging. Since the negative electrode lead 1012 and the positive electrode lead 1032 are respectively connected to the limiting flange part 1014 on the upper end of the sealing cover 101 and the base 103, the sealing space formed between the sleeve part 1015, the main shell 102 and the base 103 is not affected, that is, the sealing performance of the electrochemical cell is not damaged. In addition, the first beryllium window 10111 and the second beryllium window 1031 are made of beryllium material with low X-ray absorption rate, which can improve the penetration ability of the X-ray 4 on the one hand, and the beryllium window is conductive, which not only eliminates the use of additional current collectors, but also eliminates additional electrode leads inside the battery, thereby making it possible to directly lead out the electrode lead outside the battery mold 1 and connect it to the charge-discharge instrument 3.

[0028] In the embodiment, the sealing cover 101 and the base 103 are made of stainless steel material, the main shell 102 is made of polyether ether ketone material with high mechanical strength, good chemical stability and easy mechanical processing, and the sleeve part 1015 of the sealing cover 101 is screw-inserted into the through hole 1021 of the main shell 102 and fixed.

[0029] As shown in the drawings, Figures 1-8 In the embodiment, the lower end of the sleeve part 1015 is provided with a first sealing ring 5 between the outer side and the main shell 102, and the upper side of the base 103 is provided with a second sealing ring 6 between the lower end surface of the main shell 102. The sleeve part 1015, the main shell 102 and the base 103 form a sealed space through the sealing effect of the first sealing ring 5 and the second sealing ring 6. In the embodiment, the first sealing ring 5 and the second sealing ring 6 are made of butyronitrile rubber or perfluorinated rubber material with good chemical stability, wear resistance and aging resistance.

[0030] As shown in the drawings, Figure 5 In the embodiment, the through hole 1021 of the main shell 102 for inserting the sleeve part 1015 is provided with a first sealing groove 1022 on the inner wall for installing the first sealing ring 5, and the lower end surface of the main shell 102 is provided with a second sealing groove 1023 for installing the second sealing ring 6, as shown in the drawings, Figure 6 The upper surface of the base 103 is provided with a third sealing groove 1033 for installing the second sealing ring 6.

[0031] As shown in the drawings, Figure 2 and Figure 5As shown in the drawings, in the embodiment, the base 103 is fixed to the lower end of the main shell 102 by the bolt 7, and the lower end surface of the main shell 102 is provided with a threaded hole 1024 for the threaded insertion of the bolt 7.

[0032] As shown in the drawings, Figure 2 and 4 As shown in the drawings, in the embodiment, the lower end of the sleeve part 1015 is provided with a lower sealing platform 1011, and the lower sealing platform 1011 comprises a window positioning ring 10112, the first beryllium window 10111 is arranged in the window positioning ring 10112, and the window positioning ring 10112 is fixedly connected with the sleeve part 1015.

[0033] As shown in the drawings, Figure 7 As shown in the drawings, in the embodiment, the battery assembly 104 comprises a negative electrode 1041, a diaphragm 1042 and a positive electrode 1043 arranged in sequence from top to bottom, wherein the diaphragm 1042 insulates the electrical contact between the negative electrode 1041 and the positive electrode 1043.

[0034] As shown in the drawings, Figure 1 and Figure 8 As shown in the drawings, the battery mold 1 of the utility model can be arranged in a battery mold support 2 during use, the battery mold support 2 comprises a mounting sleeve 202 for accommodating the battery mold 1, the mounting sleeve 202 is provided with a fastening bolt 201 on the circumferential wall to lock and fix the main shell 102 part of the battery mold 1, the negative electrode lead 1012 and the positive electrode lead 1032 are respectively led out from the front and rear sides of the battery mold support 2 and then connected with the charge-discharge instrument 3, and the mounting sleeve 202 is provided with a supporting rod 203 on the lower side to realize supporting and fixing.

[0035] The working principle of the utility model is as follows:

[0036] During assembly, the positive electrode slurry is first directly coated onto the second beryllium window 1031 in the middle of the base 103. After the positive electrode slurry is dried, it forms the positive electrode 1043 of the battery assembly 104. Then, the main housing 102 is placed in the base 103, and the second sealing ring 6 is placed between the third sealing groove 1033 on the upper side of the base 103 and the second sealing groove 1023 at the lower end of the main housing 102. Then, the base 103 is fixed to the lower end face of the main housing 102 using bolts 7. At this time, the second sealing groove 1023 and the third sealing groove 1033 press the second sealing ring 6 to ensure a seal. Then, the separator 1042 and the negative electrode 1 of the battery assembly 104 are connected. 041 is inserted sequentially along the through hole 1021 inside the main housing 102 and falls onto the positive electrode 1043. Then, a certain amount of liquid electrolyte is added to wet the positive electrode 1043, negative electrode 1041 and separator 1042. Then, the first sealing ring 5 is placed in the first sealing groove 1022 on the inner wall of the through hole 1021 of the main housing 102. Then, the sleeve portion 1015 of the sealing cover 101 is threaded into the through hole 1021 of the main housing 102, and the first beryllium window 10111 at the lower end of the sleeve portion 1015 abuts against the negative electrode 1041 of the battery assembly 104. At the same time, the sealing cover 101 and the main housing 102 are also fixed by threads.

[0037] After the battery mold 1 is assembled, it is placed into the mounting sleeve 202 in the battery mold bracket 2, and the battery mold 1 is locked and fixed in the mounting sleeve 202 using fastening bolts 201. Then, the support rod 203 of the battery mold bracket 2 is fixed on the sample stage, so that the X-ray 4 can be accurately injected into the X-ray channel 1013 of the battery mold 1. Finally, the negative electrode lead 1012 and the positive electrode lead 1032 are electrically connected to the charge and discharge instrument 3 to realize in-situ XAS testing during battery charging and discharging.

Claims

1. An in-situ synchrotron transmission XAS battery testing apparatus, characterized by: The battery mold (1) comprises a sealing cover (101), a main shell (102) and a base (103), wherein the sealing cover (101) comprises a sleeve part (1015) inserted into the main shell (102), and a first beryllium window (10111) is arranged at the middle of the lower end of the sleeve part (1015); the base (103) is fixed to the lower end of the main shell (102) and is provided with a second beryllium window (1031) at the middle of the lower end; the sleeve part (1015), the main shell (102) and the base (103) form a sealed space for accommodating a battery assembly (104), and a negative electrode (1041) at the upper side of the battery assembly (104) is in contact with the first beryllium window (10111), and a positive electrode (1043) at the lower side is in contact with the second beryllium window (1031); a limiting flange part (1014) is arranged at the upper end of the sleeve part (1015) and located at the upper side of the main shell (102), and the limiting flange part (1014) is provided with a negative electrode lead (1012) connected with a charge and discharge instrument (3); and the base (103) is provided with a positive electrode lead (1032) connected with the charge and discharge instrument (3).

2. The in-situ synchrotron transmission XAS battery test device of claim 1, wherein: A first sealing ring (5) is arranged between the outer side of the lower end of the sleeve part (1015) and the main shell (102), and a second sealing ring (6) is arranged between the upper side of the base (103) and the lower end surface of the main shell (102).

3. The in-situ synchrotron transmission XAS battery test device of claim 2, wherein: A first sealing groove (1022) for mounting the first sealing ring (5) is arranged on the inner wall of a through hole (1021) for inserting the sleeve part (1015) in the main shell (102), and a second sealing groove (1023) for mounting the second sealing ring (6) is arranged on the lower end surface of the main shell (102), and a third sealing groove (1033) for mounting the second sealing ring (6) is arranged on the upper surface of the base (103).

4. The in-situ synchrotron transmission XAS battery test device of claim 1, wherein: The base (103) is fixed to the lower end of the main shell (102) by a bolt (7).

5. The in-situ synchrotron transmission XAS battery test device of claim 1, wherein: A lower sealing platform (1011) is arranged at the lower end of the sleeve part (1015), and the lower sealing platform (1011) comprises a window positioning ring (10112), and the first beryllium window (10111) is arranged in the window positioning ring (10112), and the window positioning ring (10112) is fixed to the sleeve part (1015).

6. The in-situ synchrotron transmission XAS battery test device of claim 1, wherein: The battery mold (1) is arranged in a battery mold support (2), and the battery mold support (2) comprises a mounting sleeve (202) for accommodating the battery mold (1), and a fastening bolt (201) is arranged on the circumferential wall of the mounting sleeve (202), and a supporting rod (203) is arranged at the lower side of the mounting sleeve (202).

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