CT sample preparation tool and method for battery material in inert atmosphere

Abstract

The invention discloses a CT sample preparation tool and method for a battery material in an inert atmosphere, and the tool comprises a sample preparation tube which is used for collecting a sample; the sample collection tube is used for collecting the sample collected by the sample preparation tube, sealing and storing for inspection; the demolding rod is used for pushing the sample from the sample preparation tube into the sample collection tube; the sample preparation method comprises the following steps: preparing a sample; preparing a sample; feeding a sample into a tube; and packaging the sample and testing the sample. According to the CT sample preparation tool and method for the battery material under the inert atmosphere, inert atmosphere protection is achieved in the whole process from sample loading and packaging to CT scanning, air is isolated in the whole process, and material degradation is avoided; x-ray attenuation and artifact interference are reduced, submicron resolution is ensured, and the problem that in a traditional method, a sample is prone to pollution due to long contact time with air in the transfer process is effectively solved; and moreover, the battery pack can be compatible with various types of batteries, the universality is higher, and the application range is wider.

Description

Technical Field

[0001] The present invention relates to the technical field of batteries, and particularly to a CT sample preparation tooling and a sample preparation method for battery materials under an inert atmosphere. Background Art

[0002] With the rapid development of new energy technologies, the research on high-performance energy storage devices such as lithium-ion liquid batteries and solid-state batteries has become the core direction. During long-term cycling, the microstructure of battery materials (such as electrode particle morphology, pore distribution, crack evolution, etc.) directly affects their electrochemical performance (such as cycle life, energy density, safety). Therefore, it is crucial to perform high-precision and non-destructive three-dimensional structure characterization on battery materials. High-resolution computed tomography (CT) technology has become an effective means for analyzing the internal structure of materials due to its non-destructive imaging and sub-micron resolution characteristics. Although common industrial high-resolution CT technology has significant advantages, it still faces the following challenges in battery material analysis: ① Limited resolution: Conventional test tooling is prone to introducing artifacts or blocking key areas due to poor X-ray penetrability or oversized sample preparation size, affecting the quality of CT imaging, and it is difficult to achieve sub-micron resolution. ② Sample contamination problem: Battery materials (such as lithium metal, sulfide solid electrolytes, etc.) are sensitive to air, and exposure to oxygen or moisture can cause oxidation, passivation, or structural deterioration. It is difficult to completely isolate air during the traditional sample preparation process, resulting in damage to the authenticity of the sample. ③ Low sample preparation efficiency: Existing inert atmosphere protection devices have poor compatibility with CT equipment, and the sample loading, sealing, and atmosphere maintenance processes are cumbersome, taking up to several hours, making it difficult to meet the requirements for rapid and high-throughput analysis in research and development. Summary of the Invention

[0003] Aiming at the problems in the prior art, the present invention aims to solve at least one of the technical problems in the related art to a certain extent. Therefore, the present invention discloses a CT sample preparation tooling and a sample preparation method for battery materials under an inert atmosphere, realizing full-process inert atmosphere protection from sample loading, encapsulation to CT scanning, completely isolating air to avoid material deterioration; reducing X-ray attenuation and artifact interference, ensuring sub-micron resolution, and effectively solving the problem that existing samples are contaminated during the acquisition process due to the influence of the existing tooling structure and long sampling time, resulting in affected resolution.

[0004] The present invention is realized through the following technical solutions:

[0005] The present invention first provides a CT sample preparation tooling for battery materials under an inert atmosphere, including

[0006] A sample preparation tube for collecting samples;

[0007] A sample collection tube for collecting the samples collected by the sample preparation tube, sealing them, and then sending them for inspection;

[0008] Ejecting rod, which is used to push the sample from the sample preparation tube into the sample collection tube.

[0009] As a further solution, the ejecting rod is cylindrical.

[0010] As a further solution, the ejecting rod is a solid cylindrical structure.

[0011] As a further solution, the ejecting rod is a hollow cylindrical structure with a sealed bottom.

[0012] As a further solution, the sample preparation tube includes a body, a cutter head and a collection end that are connected in sequence from top to bottom. The collection end is used to collect samples, the cutter head is used for fixed connection with the sample collection tube. The sample preparation tube is provided with a central through hole for sleeving the ejecting rod, and the length of the sample preparation tube is less than the length of the ejecting rod.

[0013] As a further solution, both the body and the cutter head are hollow cylindrical structures. There is a central through hole in the body, a central through hole in the cutter head, and a sampling central hole in the collection end. The inner diameter of the central through hole in the body is greater than or equal to the inner diameter of the central through hole in the cutter head. The inner diameters of the central through hole in the cutter head and the central hole in the collection end are the same. After the three central holes are connected, a central through hole is formed.

[0014] As a further solution, the top of the central through hole in the body is a funnel-shaped structure.

[0015] As a further solution, the upper part of the body is a chamfered structure.

[0016] As a further solution, the upper part of the sample collection tube is a chamfered structure.

[0017] As a further solution, the inner diameter of the central through hole in the body is greater than or equal to the inner diameter of the central through hole in the cutter head.

[0018] As a further solution, the sample preparation tube is an integral structure.

[0019] As a further solution, the body and the cutter head are an integral structure or welded, and the cutter head and the collection end are an integral structure.

[0020] As a further solution, the cutter head and the collection end are threadedly connected.

[0021] As a further solution, the outer diameter of the body is greater than the outer diameter of the cutter head.

[0022] As a further solution, the collection end is a wedge-shaped or inverted frustum structure.

[0023] As a further solution, the sample collection tube includes an upper part and a lower part with a sealed bottom. The upper part is a hollow cylindrical structure. The upper part is detachably connected to the cutter head. The lower part is a sealed structure for holding samples. When the sample enters the sample collection tube, the opening of the upper part is sealed.

[0024] As a further solution, a limiting part is provided between the upper part and the lower part, and the shape of the limiting part matches the shape of the collection end.

[0025] As a further solution, the form of the hermetic encapsulation is direct heat sealing or sealing with paraffin or epoxy resin.

[0026] As a further solution, the sample collection tube is of an integral structure.

[0027] As a further solution, the lower part is semi-circular arc-shaped, inverted conical or cylindrical.

[0028] As a further solution, the limiting part is an annular protrusion, an annular step or a clamping platform.

[0029] As a further solution, the material of the demolding rod is titanium metal, molybdenum metal or stainless steel.

[0030] As a further solution, the material of the sample preparation tube is titanium metal, molybdenum metal or stainless steel.

[0031] As a further solution, the material of the sample collection tube is any one or a combination of polyether ether ketone (PEEK), polytetrafluoroethylene (PTFE), polyethylene (PE), polyethylene (PE), polycarbonate (PC) or polystyrene (PS) that can penetrate the X-rays emitted by the CT device.

[0032] As a further solution, the outer diameter of the sample preparation tube is larger than the outer diameter of the cutter head, and the inner diameter of the central through hole is less than 1 mm.

[0033] As a further solution, the cutter head is clamped with the sample collection tube.

[0034] As a further solution, a buckle is provided on the outer part of the cutter head, and a clamping groove matching the buckle is provided on the inner wall of the upper part; when the cutter head needs to be clamped with the sample collection tube, the buckle can be clamped with the clamping groove.

[0035] As a further solution, in order to further improve the sealing performance when the cutter head is connected with the sample collection tube, a rubber layer is provided inside the clamping groove, and the rubber layer is heat-sealed or pasted on the clamping groove.

[0036] As a further solution, an annular protrusion is provided on the outer wall of the cutter head, the material of the annular protrusion is rubber, and an annular groove for placing the annular protrusion is provided on the sample collection tube. When the buckle is connected with the clamping groove, the annular protrusion is located in the annular groove.

[0037] As a further solution, the clamping groove is located above the annular groove.

[0038] The present invention also provides a CT sample preparation method for battery materials under an inert atmosphere, including the following steps:

[0039] S1. Prepare the sample: Disassemble the battery and take out the electrode sheet under the conditions of room temperature and a full inert gas atmosphere.

[0040] S2. Make the sample: Place the electrode sheet horizontally and put the sample preparation tube above the electrode sheet. Apply pressure to the cutting head of the sample preparation tube to punch the electrode sheet to collect the sample, and the range of the punching pressure is 0 N to 5000 N.

[0041] S3. Put the sample into the tube: After fixing the cutting head with the collected sample to the sample collection tube, push the sample into the sample collection tube through the die ejector rod.

[0042] S4. Package the sample: Package the sample in the sample collection tube.

[0043] S5. Test the sample: Place the packaged sample collection tube in a CT tester for testing.

[0044] As a further solution, the method of packaging the sample in the sample collection tube in S4 is direct heat sealing, using paraffin or epoxy resin for gluing.

[0045] The present invention can be widely applied to the high-precision CT sample preparation tests of common solid and liquid batteries in various organic and aqueous systems.

[0046] The features and beneficial effects of the present invention are as follows:

[0047] A CT sample preparation tooling for battery materials under an inert atmosphere:

[0048] (1) The CT sample preparation tooling for battery materials under an inert atmosphere of the present invention has a simple structure and a small size, realizing a "one-stop" sample preparation process from sampling, sample preparation to packaging, simplifying the operation process, shortening the sample preparation time, greatly improving the sample preparation efficiency, and effectively solving the problem that the sample is easily contaminated due to the long contact time with air during the sample transfer process in the traditional method.

[0049] (2) The CT sample preparation tooling for battery materials under an inert atmosphere of the present invention controls the sample size by designing the tooling size, thereby improving the imaging resolution.

[0050] (3) The CT sample preparation tooling for battery materials under an inert atmosphere of the present invention supports the general adaptation of solid-state battery powder electrode sheets, soft-pack battery slices and liquid battery electrode sheets, and is compatible with mainstream high-resolution CT models, with strong versatility.

[0051] A CT sample preparation method for battery materials under an inert atmosphere:

[0052] (1) The CT sample preparation method for battery materials in an inert atmosphere according to the present invention realizes the whole-process inert atmosphere protection from sample loading, encapsulation to CT scanning, isolates air throughout the process, and avoids material deterioration; reduces X-ray attenuation and artifact interference, ensuring sub-micron resolution; and is particularly suitable for highly active materials such as lithium metal and sulfide solid electrolytes.

[0053] (2) The CT sample preparation method for battery materials in an inert atmosphere according to the present invention realizes a "one-stop" sample preparation process from sampling, sample preparation to encapsulation, simplifies the operation process, shortens the sample preparation time, and greatly improves the sample preparation efficiency.

[0054] (3) The CT sample preparation method for battery materials in an inert atmosphere according to the present invention supports the sample preparation of solid-state battery powder electrodes, soft-pack battery slices and liquid battery electrodes, and has strong versatility. Description of the Drawings

[0055] In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the drawings required for use in the embodiments or the description of the prior art. Obviously, the following drawings are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative efforts.

[0056] Figure 1 It is a cross-sectional view of the CT sample preparation tooling for battery materials in an inert atmosphere according to the embodiments of the present invention;

[0057] Figure 2 It is a positional relationship diagram of the demolding rod and the sample preparation tube according to the embodiments of the present invention;

[0058] Figure 3 It is a positional relationship diagram of the cutter head and the acquisition end according to the embodiments of the present invention;

[0059] Figure 4 It is a cross-sectional view of the sample collection tube according to the embodiments of the present invention;

[0060] Figure 5 It is a flow chart of the CT sample preparation method for battery materials in an inert atmosphere according to the embodiments of the present invention;

[0061] Figure 6 It is a spatial resolution measurement diagram of CT testing on battery materials according to the embodiments of the present invention;

[0062] Figure 7 It is a reconstructed diagram of CT testing on battery materials according to the embodiments of the present invention;

[0063] Figure 8 It is a front view of the CT test result of battery materials according to the embodiments of the present invention;

[0064] Figure 9 This is the top view of the CT test results for the battery material described in the embodiments of the present invention;

[0065] Figure 10 This is the top view of the CT test results for the soft-pack battery material described in the embodiments of the present invention;

[0066] Figure 11 This is the front view of the CT test results for the soft-pack battery material described in the embodiments of the present invention.

[0067] Explanation of reference numerals

[0068] 1 - Demolding rod; 2 - Sample preparation tube; 21 - Body; 211 - Central through-hole of the body; 22 - Tool bit; 221 - Central through-hole of the tool bit; 23 - Collection end; 231 - Central hole of the collection end; 3 - Sample collection tube; 31 - Upper part; 32 - Lower part; 33 - Limiting part; 34 - Internal thread. Detailed implementation manners

[0069] To facilitate the understanding of the present invention, the present invention will be described more comprehensively below. Embodiments of the present invention are given, but the scope of the present invention is not limited thereby.

[0070] Unless otherwise defined, all technical and scientific terms used in this application have the same meaning as commonly understood by those skilled in the technical field to which this application belongs; the terms used in this application are only for the purpose of describing specific embodiments and are not intended to limit this application; the terms "including" and "having" and any variations thereof in the description and claims of this application and the above accompanying drawings are intended to cover non-exclusive inclusion. In the description of this application, it should be understood that the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus cannot be understood as a limitation of the present invention. In addition, the terms "first", "second", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. Thus, the features defined with "first", "second", etc. may explicitly or implicitly include one or more of such features. In the description of the present invention, unless otherwise stated, "a plurality" means two or more.

[0071] In the description of the present invention, it should be noted that unless otherwise clearly specified and defined, the terms "installation", "connection", and "coupling" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific situations.

[0072] Glossary:

[0073] CT: Computed Tomography technology.

[0074] One-stop: It means concentrating all the services, information, or processes required by customers on a single platform or site, so that users can complete all their needs without having to switch between multiple channels. Its essence is the integration and consolidation of services, aiming to improve efficiency and experience. In this article, it means that the sample preparation process of sampling, sample preparation, and encapsulation is completed on the sample preparation tooling platform without the need for an additional platform.

[0075] A CT sample preparation tooling under an inert atmosphere for battery materials, the battery materials include liquid battery slurry electrodes, solid battery powder electrodes, and dry electrodes; the inert atmosphere refers to the argon atmosphere in the glove box; the high-resolution CT sample preparation tooling refers to improving the CT test resolution by standardizing the sample size through the tooling, such as Figures 1 to 4 as shown, including

[0076] A sample preparation tube 2 for collecting samples;

[0077] A sample collection tube 3 for collecting the samples collected by the sample preparation tube 2 and sealing and storing them;

[0078] A demolding rod 1 for pushing the sample from the sample preparation tube 2 into the sample collection tube 3.

[0079] The sample preparation tooling of the present application realizes the whole process of inert atmosphere protection from sample loading, encapsulation to CT scanning, solves the problem of sample transfer pollution in traditional methods, and is especially suitable for highly active materials such as lithium metal and sulfide solid electrolytes. It supports the general adaptation of multiple samples (such as solid battery powder electrodes, soft-pack battery slices, and liquid battery electrodes), is compatible with mainstream high-resolution CT models, and greatly shortens the sample preparation time.

[0080] The demolding rod 1 provided by the present invention is cylindrical.

[0081] In an embodiment provided by the present invention, the demolding rod 1 is a solid cylindrical structure. This structure has low requirements for processing tools, can be mass-produced, is not easily damaged, and has a long service life.

[0082] In another embodiment provided by the present invention, the demolding rod 1 is a hollow cylindrical structure with a sealed bottom. This structure can reduce the weight of the demolding rod 1, save materials, and effectively reduce the cost of raw materials.

[0083] The material of the demolding rod 1 provided by the present invention is titanium metal, molybdenum metal or stainless steel.

[0084] The sample preparation tube 2 includes a main body 21, a cutter head 22 and a collection end 23 connected in sequence from top to bottom. The cutter head 22 is provided with an external thread 24 connected to the sample collection tube 3. The sample preparation tube 2 is also provided with a central through hole for sleeving the demolding rod 1, and its length is less than that of the demolding rod 1, so that the demolding rod 1 can directly push the sample into the sample collection tube without the aid of external tools.

[0085] In the present invention, both the main body 21 and the cutter head 22 are hollow cylindrical structures. The main body 21 is internally provided with a main body central through hole 211, the cutter head 22 is internally provided with a cutter head central through hole 221, the collection end 23 is internally provided with a collection end central hole 231, and the collection end is internally provided with a sampling central hole. The inner diameter of the main body central through hole is greater than or equal to the inner diameter of the cutter head central through hole. The inner diameters of the cutter head central through hole and the collection end central hole are the same. After the three central holes are connected, a central through hole is formed. Preferably, the outer diameter of the main body 21 is greater than the outer diameter of the cutter head 22. On the one hand, it is for the aesthetic design, and on the other hand, it is convenient for the cutter head 22 to cooperate with the sample collection tube.

[0086] In an embodiment provided by the present invention, the top of the main body central through hole 211 is a funnel-shaped structure, which is convenient for the demolding rod 1 to enter.

[0087] In an embodiment provided by the present invention, the upper part of the main body 21 is a chamfered structure, which can effectively prevent the damage caused by the collision between the demolding rod 1 and the sample preparation tube 2 during the operation, and extend the service life of the sample preparation tooling.

[0088] In an embodiment provided by the present invention, the upper part of the sample collection tube 3 is a chamfered structure, which can effectively prevent the damage caused by the collision between the collection end 23 and the upper part of the sample collection tube 3 during the operation, and extend the service life of the sample preparation tooling.

[0089] In an embodiment provided by the present invention, in order to facilitate the demolding rod 1 to enter the cutter head central through hole 221, the inner diameter of the main body central through hole 211 can be set to be greater than or equal to the inner diameter of the cutter head central through hole 221.

[0090] In an embodiment provided by the present invention, the collection end 23 is a wedge shape provided with a collection end central hole 231. The setting of the wedge shape can enhance the stamping and cutting performance through the sharpening treatment of the edge sharpness.

[0091] In another embodiment provided by the present invention, the collection end 23 has a frustum structure with a central hole 231 at the collection end. This structure enables the collected samples to gather at the bottom and can be easily pushed directly into the sample collection tube 3 through the ejection rod 1.

[0092] In one embodiment provided by the present invention, the sample preparation tube 2 is an integral structure, which is convenient for injection molding in one piece and improves production efficiency.

[0093] In another embodiment provided by the present invention, the main body 21 and the cutter head 22 are welded into shape, and the cutter head 22 and the collection end 23 are threadedly connected, which is convenient for maintenance and replacement. When one of the components is damaged, only the damaged component needs to be replaced instead of replacing all of them, effectively reducing the loss cost.

[0094] The material of the sample preparation tube 2 provided by the present invention is titanium metal, molybdenum metal or stainless steel.

[0095] The sample collection tube 3 includes an upper part 31 and a lower part 32 connected below it. The upper part is a hollow cylindrical structure. The upper part 31 is provided with an internal thread 34 that matches the external thread 24. The lower part 32 is a sealed structure for holding samples. When the sample enters the sample collection tube 3, the opening of the upper part 31 is sealed.

[0096] In the present invention, the form of the sealed package is direct heat sealing or sealing with paraffin or epoxy resin glue.

[0097] In one embodiment provided by the present invention, in order to prevent the collection end 23 from reaching too low a position in the lower part 32 when the thread connection teeth cannot engage, a limiting part 33 is provided between the upper part 31 and the lower part 32. The limiting part 33 is used to limit the collection end 23, and the shape of the limiting part 33 matches the shape of the collection end 23.

[0098] In one embodiment provided by the present invention, the sample collection tube 3 is an integral structure, which is convenient for injection molding in one piece, improves production efficiency, and effectively ensures the sealing performance at the same time.

[0099] In one or more embodiments, the lower part 32 is in a semi-circular arc shape, an inverted conical shape or a cylindrical shape, and the specific shape can be set according to actual needs.

[0100] In one or more embodiments, the limiting part 32 is an annular protrusion, an annular step or a clamping platform, and the specific shape can be set according to actual needs.

[0101] In the present invention, the material of the sample collection tube 3 is any one or a combination of polyether ether ketone (PEEK), polytetrafluoroethylene (PTFE), polyethylene (PE), polyethylene (PE), polycarbonate (PC) or polystyrene (PS) that can penetrate the X-rays emitted by the CT test equipment.

[0102] In an embodiment provided by the present invention, the cutter head 22 is snap-connected to the sample collection tube 3.

[0103] In an embodiment provided by the present invention, a snap is provided outside the cutter head 22, and a card slot matching the snap is provided on the inner wall of the upper part 21; when the cutter head 22 needs to be snap-connected to the sample collection tube 3, the snap can be snap-connected to the card slot.

[0104] In an embodiment provided by the present invention, in order to further improve the sealing performance when the cutter head 22 is connected to the sample collection tube 3, a rubber layer is provided inside the card slot, and the rubber layer is heat-sealed or pasted on the card slot.

[0105] In an embodiment provided by the present invention, in order to further improve the sealing performance when the cutter head 22 is connected to the sample collection tube 3, an annular protrusion is provided on the outer wall of the cutter head 22, the material of the annular protrusion is rubber, and an annular groove for placing the annular protrusion is provided on the sample collection tube 3. When the snap is connected to the card slot, the annular protrusion is located in the annular groove, effectively playing a role in isolating air. Preferably, the card slot is located above the annular groove. Setting such a positional relationship is that when the snap and the card slot are snap-connected, the card slot is located above the annular groove, which is convenient for the staff to observe whether the snap connection is intact, and while ensuring the sealing performance, it will not block the line of sight.

[0106] In the present invention, the outer diameter of the sample preparation tube 2 is larger than the outer diameter of the cutter head, and the inner diameter of the central through hole is less than 1 mm. Preferably, the inner diameter of the central through hole is 0.8 mm. At this size, the accuracy achieved by mold processing is the highest.

[0107] In an embodiment provided by the present invention, the length of the body 21 is 50 mm, the outer diameter is 6 mm, the length of the cutter head 22 is 10 mm, the outer diameter is 3 mm, the collection end 23 is a frustum structure, the inner diameter of the central through hole is 0.8 mm, the outer diameter of the demolding rod 1 is 0.7 mm, and the inner diameter of the sample collection tube 3 matches the outer diameter of the cutter head 22, that is, the two are tightly fitted after being threadedly connected. The present invention controls the sample size by designing the tooling size, thereby improving the imaging resolution.

[0108] The working principle of a CT sample preparation tooling for battery materials under an inert atmosphere is as follows:

[0109] Place the sample preparation tooling above the pole piece and align it with the battery pole piece to be collected. Under the action of an external force, the collection end 23 punches and collects the sample from the battery pole piece. After collecting the pole piece sample, insert the cutter head 22 of the sample preparation tube 2 into the sample collection tube 3 and threadedly connect the two. Then insert the demolding rod 1 through the central through hole until the demolding rod 1 pushes the sample on the collection end 23 into the sample collection tube 3. Then take out the demolding rod 1, and seal the sample inside the sample collection tube 3 by direct heat sealing or with paraffin or epoxy resin glue.

[0110] A method for preparing CT samples of battery materials under an inert atmosphere, as follows Figures 5 to 11 shown, includes the following steps:

[0111] S1. Prepare the sample: At room temperature, inside a glove box filled with argon inert gas, disassemble the battery and take out the electrode sheet; Protect the whole process in an inert atmosphere: Isolate the air from sample preparation to CT scanning to avoid material deterioration;

[0112] S2. Make the sample: Place the electrode sheet horizontally, place the sample preparation tube 2 above the electrode sheet so that the collection end 23 is aligned with the battery electrode sheet, manually or use a press to apply pressure to the cutter head 22 of the sample preparation tube 2 so that the collection end 23 punches the electrode sheet to collect the sample, and the range of the externally applied pressure is 0 N to 5000 N;

[0113] S3. Put the sample into the tube: Connect the sample collection tube 3 to the cutter head 22 of the sample preparation tube by thread, insert the demolding rod 1 into the sample preparation tube 2 until the sample is pushed into the sample collection tube 3;

[0114] S4. Package the sample: Use direct heat sealing, paraffin or epoxy resin glue to package the sample collection tube 3; It can reduce X-ray attenuation and artifact interference and ensure sub-micron resolution;

[0115] S5. Test the sample: Place the packaged sample collection tube 3 in a CT tester for testing.

[0116] Using the sample preparation method of the present invention, a "one-stop" sample preparation process from sampling, sample preparation to packaging is realized, which simplifies the operation process, shortens the sample preparation time, and greatly improves the sample preparation efficiency; At the same time, it is compatible with mainstream CT equipment and has stronger compatibility.

[0117] Example 1

[0118] A method for preparing CT samples of battery materials under an inert atmosphere, includes the following steps:

[0119] X1. Prepare the sample: At room temperature, inside a glove box filled with argon inert gas, disassemble the solid-state battery to remove the mold and take out the silicon negative electrode sheet and sulfide solid electrolyte;

[0120] X2. Make the sample: Place the silicon negative electrode sheet and sulfide solid electrolyte horizontally, place the sample preparation tube 2 above the electrode sheet so that the collection end 23 is aligned with the battery electrode sheet, manually or use a press to apply pressure to the cutter head 22 of the sample preparation tube 2 so that the collection end 23 punches the electrode sheet to collect the sample, and the range of the pressure is 0 N to 5000 N;

[0121] X3. Put the sample into the tube: Connect the sample collection tube 3 to the cutter head 22 of the sample preparation tube by thread, insert the demolding rod 1 into the sample preparation tube 2 until the sample is pushed into the sample collection tube 3;

[0122] X4. Encapsulate the sample: Encapsulate the sample collection tube 3 by heating method;

[0123] X5. Test the sample: Place the encapsulated sample collection tube 3 in a CT tester for testing.

[0124] The test results are as Figures 6 to 9 shown. Analyze and measure the spatial resolution by the edge response method, calibrate at 5 points, and the resolutions are 0.50, 0.44, 0.47, 0.45 and 0.48 μm respectively, and the average resolution is 0.468 μm. As shown in Table 1, Table 1 is the measurement result of the spatial resolution of the CT test on the battery material of the present invention.

[0125] Table 1

[0126] Edge point selection 1 2 3 4 5 Average value Spatial resolution (μm) 0.50 0.44 0.47 0.45 0.48 0.468

[0127] It can be directly seen from Table 1 that after using the CT sample preparation method for battery materials in an inert atmosphere of the present invention, the minimum resolution is 0.5 μm, the maximum resolution is 0.44 μm, and the average value is 0.468 μm, which is smaller than 1 μm in the prior art. It shows that after using the CT sample preparation method for battery materials in an inert atmosphere of the present invention, the resolution of the sample in the CT detector is greatly improved, thereby indicating that the X-ray attenuation and artifact interference are reduced, and effectively solving the problem that the resolution is easily affected by contamination due to the long contact time with air during the sample transfer process in the traditional method.

[0128] Example 2

[0129] A CT sample preparation method for battery materials in an inert atmosphere, comprising the following steps:

[0130] Y1. Prepare the sample: Under room temperature conditions, in a glove box filled with argon inert gas, disassemble and demold the liquid soft-pack battery, and take out the lithium iron phosphate electrode sheet;

[0131] Y2. Make the sample: Place the battery electrode sheet horizontally, place the sample preparation tube 2 on the electrode sheet so that the collection end 23 is aligned with the battery electrode sheet, and manually or use a press to apply pressure to the cutter head 22 of the sample preparation tube 2 so that the collection end 23 punches the electrode sheet to collect the sample, and the pressure range is 0 N to 5000 N;

[0132] Y3. Put the sample into the tube: Connect the sample collection tube 3 and the cutter head 22 of the sample preparation tube by thread, insert the demolding rod 1 into the sample preparation tube 2 until the sample is pushed into the sample collection tube 3;

[0133] Y4. Encapsulate the sample: Encapsulate the sample collection tube with paraffin or epoxy resin glue;

[0134] Y5. Test the sample: Place the encapsulated sample collection tube 3 in a CT tester for testing.

[0135] The test results, such as Figure 10 and Figure 11 shown. The spatial resolution was analyzed by the edge response method. Five points were selected for calibration, and the resolutions were 0.48, 0.45, 0.47, 0.46, and 0.49 μm respectively. The average resolution was 0.47 μm, as shown in Table 2. Table 2 is the measurement result of the spatial resolution of the CT test on the pouch cell material of the present invention.

[0136] Table 2

[0137] Edge point selection 1 2 3 4 5 Average value Spatial resolution (μm) 0.48 0.45 0.47 0.46 0.49 0.47

[0138] It can be directly seen from Table 2 that after using the CT sample preparation method for the battery material of the present invention in an inert atmosphere, the minimum resolution of the collected sample is 0.49 μm, the maximum resolution is 0.45 μm, and the average value is 0.47 μm, which is smaller than 1 μm in the prior art. This shows that after using the CT sample preparation method for the battery material of the present invention in an inert atmosphere, the resolution of the sample in the CT detector is greatly improved, thereby indicating that the X-ray attenuation and artifact interference are reduced, and the problem that the resolution is easily affected by contamination due to the long contact time with air during the sample transfer process in the traditional method is effectively solved.

[0139] In summary, the CT sample preparation tooling and method for battery materials provided by the present invention realize the whole process of inert atmosphere protection from sample loading, encapsulation to CT scanning, isolate air throughout the process, and avoid material deterioration; reduce X-ray attenuation and artifact interference, ensure sub-micron resolution, and effectively solve the problem that the sample is easily contaminated due to the long contact time with air during the sample transfer process in the traditional method.

[0140] It should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A CT sample preparation tooling for battery materials under an inert atmosphere, characterized in that including a sample preparation tube for collecting samples; a sample collection tube for collecting the samples collected by the sample preparation tube, sealing them and then sending them for inspection; a demolding rod for pushing the sample from the sample preparation tube into the sample collection tube.

2. The CT sample preparation tooling for battery materials in an inert atmosphere according to claim 1, characterized in that, The sample preparation tube includes a body, a cutter head and a collection end connected in sequence from top to bottom. The collection end is used for collecting samples, and the cutter head is used for fixedly connecting with the sample collection tube. The sample preparation tube is provided with a central through hole for sleeving the demolding rod, and the length of the sample preparation tube is less than that of the demolding rod.

3. A CT sample preparation tooling for battery materials in an inert atmosphere according to claim 2, characterized in that, Both the body and the cutter head are hollow cylindrical structures. There is a body central through hole inside the body, and a cutter head central through hole inside the cutter head. The collection end is a wedge-shaped or inverted frustum structure with a sampling central hole inside. The inner diameter of the body central through hole is greater than or equal to the inner diameter of the cutter head central through hole. The inner diameters of the cutter head central through hole and the collection end central hole are the same. The three central holes are connected to form a central through hole.

4. A CT sample preparation tooling for battery materials under an inert atmosphere according to claim 1, characterized in that, The sample collection tube includes an upper part and a lower part with a sealed bottom. The upper part is a hollow cylindrical structure. The upper part is detachably connected to the cutter head. The lower part is a sealed structure for holding samples. When the sample enters the sample collection tube, the opening of the upper part is sealed and encapsulated.

5. A CT sample preparation tooling for battery materials under an inert atmosphere according to claim 4, characterized in that, A limiting part is arranged between the upper part and the lower part, and the shape of the limiting part matches the shape of the collection end.

6. The CT sample preparation tooling for battery materials under an inert atmosphere according to claim 5, wherein The materials of the demolding rod and the sample preparation tube are both titanium metal, molybdenum metal or stainless steel, and the material of the sample collection tube is any one or a combination of polyetheretherketone, polytetrafluoroethylene, polyethylene, polyethylene, polycarbonate or polystyrene that can penetrate the X-rays emitted by the CT device.

7. The CT sample preparation tooling for a battery material under an inert atmosphere according to claim 3, characterized in that The outer diameter of the sample preparation tube is greater than the outer diameter of the cutter head, and the inner diameter of the central through hole is less than 1 mm.

8. A method for preparing a CT sample of a battery material under an inert atmosphere, characterized in that, Applying a CT sample preparation tooling under an inert atmosphere for a battery material according to any one of claims 1 to 7 includes the following steps: S1. Prepare the sample: Under the condition of an inert gas, disassemble the battery and take out the electrode sheet; S2. Make the sample: Place the electrode sheet horizontally, place the sample preparation tube above the electrode sheet, apply pressure to the cutter head of the sample preparation tube to punch the electrode sheet to collect the sample, and the range of the punching pressure is 0 N to 5000 N; S3. Put the sample into the tube: After fixing the cutter head with the collected sample to the sample collection tube, push the sample into the sample collection tube through the demolding rod; S4. Package the sample: Package the sample in the sample collection tube; S5. Test the sample: Place the packaged sample collection tube in a CT tester for testing.

9. A method for CT sample preparation of a battery material under an inert atmosphere according to claim 8, characterized in that, The method of packaging the sample in the sample collection tube in S4 is direct heat sealing, using paraffin or epoxy resin for sealing.

10. A CT sample preparation tooling and method for battery materials under an inert atmosphere, characterized in that, It can be widely applied to the high-precision CT sample preparation tests of common solid and liquid batteries in various organic systems and aqueous systems.

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