Sample preparation mold and preparation method of positive electrode material observation sample
By designing a sample making mold containing prismatic convexity, the problems of inconsistent shape and low repeatability in traditional sample making methods are solved, and efficient and uniform specifications of the observation sample preparation of positive electrode material is achieved.
Patent Information
- Application Number
- CN202311544421.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-20
- Publication Date
- 2025-05-20
AI Technical Summary
The traditional method of sample making of positive electrode materials is greatly affected by human factors during the cutting process, resulting in inconsistent shape and size of the observation surface and low repeatability.
A sample making mold is designed, including the mold body and prismatic projection. By adding the positive electrode material and embedding agent to the sample filling groove and curing it, a sample with prismatic depression is formed, and the bottom edge of the prismatic depression is cut to ensure that each sample preparation is obtained with uniform specifications.
By using this sample making mold, a uniform observation surface with high repeatability can be obtained, the testing efficiency can be improved, and the stability of sample making quality can be improved.
Smart Images
Figure CN120020538A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the technical field of electron microscopy sample preparation, and particularly to a sample preparation mold and a method for preparing an observation sample of a cathode material. Background Art
[0002] In the field of cathode material research and development, in order to observe the morphological characteristics inside the material, the resin embedding method is usually used to prepare samples of cathode materials. The general process of the resin embedding method is as follows: epoxy resin is mixed with cathode material powder, then cured to form a resin block, and finally the resin block is cut by means of tools to form an observation surface, completing the preparation of the observation sample. The traditional sample preparation method is greatly affected by human factors during cutting, the shape and size of the obtained observation surfaces are not uniform, and the repeatability of the observation sample preparation is low. Summary of the Invention
[0003] Based on this, it is necessary to provide a sample preparation mold and a method for preparing an observation sample of a cathode material. When using this sample preparation mold to prepare an observation sample of the cross-section of cathode material particles, an observation surface with uniform specifications can be obtained with high repeatability, thereby improving the testing efficiency.
[0004] In a first aspect, this application provides a sample preparation mold, including: a mold body and a prismatic protrusion; a sample adding groove is provided on the mold body, the prismatic protrusion is arranged inside the sample adding groove, one side surface of the prismatic protrusion is arranged on the bottom of the sample adding groove, and one side edge of the prismatic protrusion faces the notch of the sample adding groove.
[0005] In some embodiments, the height from the notch of the sample adding groove to the side edge of the prismatic protrusion facing the notch of the sample adding groove is 5 mm to 11 mm.
[0006] In some embodiments, the depth of the sample adding groove is 8 mm to 12 mm.
[0007] In some embodiments, the height difference between the side edge of the prismatic protrusion facing the notch of the sample adding groove and the side surface arranged on the bottom of the sample adding groove is 1 mm to 3 mm.
[0008] In some embodiments, the diameter of the bottom surface of the sample adding groove is 8 mm to 12 mm or the side length of the bottom surface of the sample adding groove is 8 mm to 12 mm.
[0009] In some embodiments, the width of the narrowest part of the side surface of the prismatic protrusion arranged on the bottom of the sample adding groove is 2 mm to 4 mm.
[0010] In some embodiments, the two bottom surfaces of the prismatic protrusion are respectively attached to the two opposite side walls of the sample adding groove.
[0011] In some embodiments, the sample preparation mold further includes a support member disposed at the bottom of the sample addition groove, and one side surface of the prismatic protrusion is disposed on the surface of the support member.
[0012] In some embodiments, each side surface of the support member is in close contact with the groove wall of the sample addition groove.
[0013] In some embodiments, the thickness of the support member is 4 mm to 6 mm.
[0014] In some embodiments, the sample preparation mold further includes a through-hole member detachably connected to the surface of the mold body provided with the sample addition groove. A through-hole is provided on the through-hole member, and the through-hole communicates with the sample addition groove.
[0015] In some embodiments, the thickness of the through-hole member is 2 mm to 4 mm.
[0016] In some embodiments, the cross-section of the through-hole has the same shape and size as the notch of the sample addition groove.
[0017] In a second aspect, the present application provides a method for preparing an observation sample of a positive electrode material, using the sample preparation mold according to any one of the above, including the following steps:
[0018] Add the positive electrode material and the embedding agent into the sample addition groove and submerge the prismatic protrusion;
[0019] Cure the positive electrode material and the embedding agent to prepare a cured sample, and the cured sample has a prismatic depression;
[0020] Take out the cured sample and cut the cured sample along the bottom edge of the prismatic depression.
[0021] In the above sample preparation mold, a sample addition groove is provided on the mold body, a prismatic protrusion with one side surface located at the bottom of the groove is provided at the bottom of the sample addition groove, and one side edge of the prismatic protrusion faces the notch of the sample addition groove. When using this sample preparation mold to prepare a sample for observing the cross-section of positive electrode material particles, after adding the raw materials into the sample addition groove and curing, a sample with a prismatic depression can be obtained. The bottom edge of the prismatic depression can be used as a cutting guide. Cutting the sample along the bottom edge of the prismatic depression can make the observation surface obtained each time have a relatively high degree of approximation. When using this sample preparation mold to prepare a sample for observing the cross-section of positive electrode material particles, an observation surface with uniform specifications can be obtained with high repeatability, thereby improving the test efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 is a schematic structural diagram of a sample preparation mold provided by an embodiment of the present application;
[0023] Figure 2Schematic diagram of the prismatic protrusion provided by an embodiment of the present application;
[0024] Figure 3 Schematic diagram of the prismatic protrusion provided by another embodiment of the present application;
[0025] Figure 4 Schematic diagram of the prismatic protrusion provided by another embodiment of the present application;
[0026] Figure 5 Schematic diagram of the sample preparation mold provided by another embodiment of the present application;
[0027] Figure 6 Flow chart of the preparation method of the positive electrode material observation sample provided by an embodiment of the present application;
[0028] Figure 7 Flow chart of the preparation method of the positive electrode material observation sample provided by another embodiment of the present application;
[0029] Figure 8 Field emission electron microscope image of the cross-section sample preparation of the positive electrode material particles in Example 1;
[0030] Figure 9 Field emission electron microscope image of the cross-section sample preparation of the positive electrode material particles in Example 2.
[0031] Explanation of reference numerals
[0032] 10. Mold body; 20. Sample addition groove; 30. Prismatic protrusion; 40. Support member; 50. Through-hole member. Detailed implementation manners
[0033] To make the above objects, features, and advantages of the present application more obvious and understandable, the following will describe the detailed implementation manners of the present application in conjunction with the accompanying drawings. Many specific details are set forth in the following description to facilitate a thorough understanding of the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present application. Therefore, the present application is not limited by the specific embodiments disclosed below.
[0034] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.
[0035] In the description of the present application, it should be understood that the orientation or positional relationships indicated by the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. are based on the orientation or positional relationships shown in the drawings. These are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, they should not be construed as limiting the present application.
[0036] In addition, the terms "first" and "second" are only used for descriptive purposes and should not be construed as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In the description of the present application, the meaning of "a plurality" is at least two, such as two, three, etc., unless otherwise specifically and clearly defined.
[0037] In the present application, unless otherwise clearly specified and limited, the terms "mounted", "connected", "coupled", "fixed", etc. should be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or integrated; it may be a mechanical connection or an electrical connection; it may be directly connected or indirectly connected through an intermediate medium, and it may be the internal communication of two elements or the interaction relationship between two elements, unless otherwise clearly limited. For those of ordinary skill in the art, the specific meanings of the above terms in the present application can be understood according to specific circumstances.
[0038] Referring to Figure 1 , an embodiment of the present application provides a sample preparation mold, including: a mold body 10 and a prismatic protrusion 30; a sample addition groove 20 is provided on the mold body 10, the prismatic protrusion 30 is disposed inside the sample addition groove 20, one side surface of the prismatic protrusion 30 is disposed on the bottom of the sample addition groove 20, and one side edge of the prismatic protrusion 30 faces the notch of the sample addition groove 20.
[0039] In the above sample preparation mold, a sample adding groove 20 is provided on the mold body 10. A prismatic protrusion 30 with one side surface located at the bottom of the sample adding groove 20 is provided at the bottom of the sample adding groove 20. One side edge of the prismatic protrusion 30 faces the notch of the sample adding groove 20. When using this sample preparation mold to prepare a sample for observing the cross-section of the positive electrode material particles, after adding the raw material into the sample adding groove 20 and curing it, a sample with a prismatic depression can be obtained. This prismatic depression can be used as a cutting guide. Cutting the sample along the bottom edge of the prismatic depression can result in an observation surface with a relatively high degree of approximation each time. When using this sample preparation mold to prepare a sample for observing the cross-section of the positive electrode material particles, an observation surface with a unified specification can be obtained with a relatively high repeatability, thereby improving the testing efficiency. It can be understood that the bottom edge of the prismatic depression corresponds to the side edge of the prismatic protrusion 30 that faces the notch of the sample adding groove 20.
[0040] It can be understood that this sample preparation mold is applicable to the preparation of samples for observing the cross-section of particulate materials for electron microscopy. Further, this sample preparation mold is applicable to the preparation of samples for observing the cross-section of positive electrode material particles for electron microscopy. Exemplarily, this sample preparation mold is applicable to the preparation of samples for observing the cross-section of positive electrode material particles by field emission electron microscopy.
[0041] In some embodiments, the prismatic protrusion 30 is a prism with an odd number of side edges, or a prism with an even number of side edges and a bottom surface that is not a regular polygon.
[0042] Refer to Figure 2 As shown, as an example, Figure 2 is a schematic three-dimensional structure diagram of the prismatic protrusion 30 in the shape of a triangular prism. Among them, the X direction is the height direction of the prismatic protrusion 30, that is, the depth direction of the sample adding groove 20. The Y direction is the width direction of the side surface of the prismatic protrusion 30 provided at the bottom of the sample adding groove 20, and the Z direction is the length direction of the side surface of the prismatic protrusion 30 provided at the bottom of the sample adding groove 20. It can be understood that in other embodiments, the prismatic protrusion 30 can also be a pentagonal prism, a heptagonal prism, a quadrangular prism with a bottom surface that is not a square, and a hexagonal prism with a bottom surface that is not a regular hexagon, etc. Refer to Figure 3 and Figure 4 As shown, Figure 3 and Figure 4 respectively show other implementable embodiments of the prismatic protrusion 30.
[0043] In some embodiments, the height from the notch of the sample loading groove 20 to the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 is 5 mm to 11 mm. Optionally, the height from the notch of the sample loading groove 20 to the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 is 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, 10 mm, or 11 mm. Alternatively, the height from the notch of the sample loading groove 20 to the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 can also be within the range between any two of the above heights. Exemplarily, referring to Figure 1 as shown, Figure 1 in which a is the height from the notch of the sample loading groove 20 to the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20.
[0044] In some embodiments, the two bottom surfaces of the prismatic protrusion 30 are respectively attached to the two opposite side walls of the sample loading groove 20. When the two bottom surfaces of the prismatic protrusion 30 are respectively attached to the two opposite side walls of the sample loading groove 20, when using this sample preparation mold for sample preparation, a through prismatic depression can be formed on the surface of the sample, which is convenient for cutting.
[0045] In some embodiments, the depth of the sample loading groove 20 is 8 mm to 12 mm. Within this depth range of the sample loading groove 20, the sample cross-section of the positive electrode material observation sample has a suitable side length. Optionally, the depth of the sample loading groove 20 is 8 mm, 8.2 mm, 8.4 mm, 8.6 mm, 8.8 mm, 9 mm, 9.2 mm, 9.4 mm, 9.6 mm, 9.8 mm, 10 mm, 10.2 mm, 10.4 mm, 10.6 mm, 10.8 mm, 11 mm, 11.2 mm, 11.4 mm, 11.6 mm, 11.8 mm, or 12 mm. Alternatively, the depth of the sample loading groove 20 can also be within the range between any two of the above depths. Exemplarily, referring to Figure 1 as shown, Figure 1 in which b is the depth of the sample loading groove 20.
[0046] In some embodiments, the height difference between the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 and the side surface provided at the bottom of the sample loading groove 20 is 1 mm to 3 mm. Optionally, the height difference between the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 and the side surface provided at the bottom of the sample loading groove 20 is 1 mm, 1.2 mm, 1.4 mm, 1.6 mm, 1.8 mm, 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm, or 3 mm. Alternatively, the height difference between the side edge of the prismatic protrusion 30 facing the notch of the sample loading groove 20 and the side surface provided at the bottom of the sample loading groove 20 can also be within the range between any two of the above height differences. Exemplarily, referring to Figure 1 as shown, Figure 1Wherein c is the height difference between the side edge of the prism-shaped protrusion 30 facing the notch of the sample addition groove 20 and the side surface provided at the bottom of the sample addition groove 20.
[0047] In some embodiments, the bottom surface of the sample addition groove 20 is circular. That is, the sample addition groove 20 is a cylindrical sample addition groove 20.
[0048] In some embodiments, the diameter of the bottom surface of the sample addition groove 20 is 8 mm to 12 mm. Within this diameter range of the bottom surface of the sample addition groove 20, the sample cross-section of the positive electrode material particle cross-section preparation has a suitable side length. Optionally, the diameter of the bottom surface of the sample addition groove 20 is 8 mm, 8.2 mm, 8.4 mm, 8.6 mm, 8.8 mm, 9 mm, 9.2 mm, 9.4 mm, 9.6 mm, 9.8 mm, 10 mm, 10.2 mm, 10.4 mm, 10.6 mm, 10.8 mm, 11 mm, 11.2 mm, 11.4 mm, 11.6 mm, 11.8 mm or 12 mm. Alternatively, the diameter of the bottom surface of the sample addition groove 20 can also be within the range between any two of the above diameters. It can be understood that when the bottom surface of the sample addition groove 20 is circular, the two bottom surfaces of the prism-shaped protrusion 30 can be arc surfaces to fit the groove wall of the sample addition groove.
[0049] In some embodiments, the bottom surface of the sample addition groove is polygonal.
[0050] In some embodiments, the side length of the bottom surface of the sample addition groove 20 is 8 mm to 12 mm. Further, the bottom surface of the sample addition groove 20 is a regular polygon. As an example, the bottom surface of the sample addition groove 20 can be a square, that is, the sample addition groove 20 is a cuboid-shaped sample addition groove 20. Within this side length range of the bottom surface of the sample addition groove 20, the sample cross-section of the positive electrode material particle cross-section preparation has a suitable side length. Optionally, the side length of the bottom surface of the sample addition groove 20 is 8 mm, 8.2 mm, 8.4 mm, 8.6 mm, 8.8 mm, 9 mm, 9.2 mm, 9.4 mm, 9.6 mm, 9.8 mm, 10 mm, 10.2 mm, 10.4 mm, 10.6 mm, 10.8 mm, 11 mm, 11.2 mm, 11.4 mm, 11.6 mm, 11.8 mm or 12 mm. Alternatively, the side length of the bottom surface of the sample addition groove 20 can also be within the range between any two of the above side lengths.
[0051] In some embodiments, the width of the side surface of the prismatic protrusion 30 disposed on the bottom of the sample addition groove 20 is 2 mm to 4 mm. The width of the side surface of the prismatic protrusion 30 disposed on the bottom of the sample addition groove 20 can control the opening size of the prismatic depression of the sample within a suitable range. Optionally, the width of the side surface of the prismatic protrusion 30 disposed on the bottom of the sample addition groove 20 is 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm, 3 mm, 3.2 mm, 3.4 mm, 3.6 mm, 3.8 mm, or 4 mm. Alternatively, the width of the side surface of the prismatic protrusion 30 disposed on the bottom of the sample addition groove 20 can also be within the range between any two of the above widths. Exemplarily, referring to Figure 1 as described above, Figure 1 where d is the width of the side surface of the prismatic protrusion 30 disposed on the bottom of the sample addition groove 20.
[0052] In some embodiments, the prismatic protrusion 30 is a straight prismatic protrusion 30.
[0053] In some embodiments, the prismatic protrusion 30 is a regular prismatic protrusion 30.
[0054] Referring to Figure 5 , in some embodiments, the sample preparation mold further includes a support member 40. The support member 40 is disposed on the bottom of the sample addition groove 20, and one side surface of the prismatic protrusion 30 is disposed on the surface of the support member 40. By providing the support member 40 and disposing one side surface of the prismatic protrusion 30 on the surface of the support member 40, it is convenient to adjust the thickness of the cured sample. It can be understood that the support member 40 can be fixedly connected or detachably connected to the bottom of the sample addition groove 20, and the prismatic protrusion 30 can be fixedly connected or detachably connected to the surface of the support member 40.
[0055] In some embodiments, each side surface of the support member 40 is disposed in contact with the groove wall of the sample addition groove 20.
[0056] In some embodiments, the thickness of the support member 40 is 4 mm to 6 mm. Optionally, the thickness of the support member 40 in the depth direction of the sample addition groove 20 is 4 mm, 4.2 mm, 4.4 mm, 4.6 mm, 4.8 mm, 5 mm, 5.2 mm, 5.4 mm, 5.6 mm, 5.8 mm, or 6 mm. Alternatively, the thickness of the support member 40 can also be within the range between any two of the above thicknesses. It can be understood that the thickness of the support member 40 refers to the thickness of the support member 40 in the depth direction of the sample addition groove 20. By selecting support members 40 with different thicknesses, the thickness of the prepared sample can be adjusted.
[0057] In some embodiments, the sample preparation mold further includes a through-hole member 50. The through-hole member 50 is detachably connected to the surface of the mold body 10 where the sample addition groove 20 is provided. A through-hole is formed in the through-hole member 50, and the through-hole communicates with the sample addition groove 20. The provision of the through-hole member 50 enables the addition amount of the sample preparation raw material to exceed the notch of the sample addition groove 20 when adding the raw material. After the raw material is cured, the through-hole member 50 is removed, which facilitates the removal of the cured sample.
[0058] In some embodiments, the cross-section of the through-hole has the same shape and size as the notch of the sample addition groove 20.
[0059] In some embodiments, the projection of the through-hole in the horizontal direction coincides with the projection of the notch in the horizontal direction.
[0060] In some embodiments, the through-hole member 50 includes a first component and a second component, and the first component and the second component can be combined to form a complete through-hole member 50. The through-hole member 50 composed of the first component and the second component is more convenient for the disassembly of the through-hole member 50.
[0061] In some embodiments, the thickness of the through-hole member 50 is 2 mm to 4 mm. Optionally, the thickness of the through-hole member 50 is 2 mm, 2.2 mm, 2.4 mm, 2.6 mm, 2.8 mm, 3 mm, 3.2 mm, 3.4 mm, 3.6 mm, 3.8 mm or 4 mm. Alternatively, the thickness of the through-hole member 50 can also be within the range between any two of the above thicknesses. It can be understood that the thickness of the through-hole member 50 refers to the thickness of the through-hole member 50 in the depth direction of the sample addition groove 20.
[0062] In some embodiments, the height of the mold body is 25 mm to 35 mm. Optionally, the height of the mold body is 25 mm, 26 mm, 27 mm, 28 mm, 29 mm, 30 mm, 31 mm, 32 mm, 33 mm, 34 mm or 35 mm. Alternatively, the height of the mold body can also be within the range between any two of the above heights. Exemplarily, referring to Figure 1 as shown, Figure 1 where e is the height of the mold body.
[0063] In some embodiments, the mold body is cylindrical.
[0064] In some embodiments, the bottom surface diameter of the mold body is 25 mm to 35 mm. Optionally, the bottom surface diameter of the mold body is 25 mm, 26 mm, 27 mm, 28 mm, 29 mm, 30 mm, 31 mm, 32 mm, 33 mm, 34 mm or 35 mm. Alternatively, the bottom surface diameter of the mold body can also be within the range between any two of the above diameters. Exemplarily, referring to Figure 1 as shown, Figure 1 where f is the bottom surface diameter of the mold body.
[0065] In some embodiments, the material of the mold body includes at least one of stainless steel, polyvinyl chloride, polyethylene, and random copolymerized polypropylene.
[0066] In some embodiments, the material of the prismatic protrusion 30 is the same as that of the mold body.
[0067] In some embodiments, the material of the support member 40 is the same as that of the mold body.
[0068] In some embodiments, the material of the through-hole member 50 is the same as that of the mold body.
[0069] Referring to Figure 6 , another embodiment of the present application provides a method for preparing a positive electrode material observation sample, using the sample preparation mold of any one of the above, including the following steps:
[0070] S100: Add the positive electrode material and the embedding agent into the sample addition groove 20 and submerge the prismatic protrusion 30;
[0071] S110: Cure the positive electrode material and the embedding agent to prepare a cured sample, and the cured sample has a prismatic depression;
[0072] S120: Take out the cured sample and cut the cured sample along the bottom edge of the prismatic depression.
[0073] In the above method for preparing the positive electrode material observation sample, the above sample preparation mold is used for sample preparation. When using the sample preparation mold to prepare a cross-section of the positive electrode material particles, the raw materials are added to the sample addition groove 20 and the prismatic protrusion 30 is submerged. After curing, a cured sample with a prismatic depression can be obtained. The prismatic depression can be used as a cutting guide, and cutting the sample along the bottom edge of the prismatic depression can make the observation surface have a high degree of approximation each time. The method for preparing the positive electrode material observation sample can repeatedly obtain observation surfaces with uniform specifications, thereby improving the test efficiency.
[0074] In some embodiments, cutting the sample along the bottom edge of the prismatic depression includes: cutting the sample along the bottom edge of the prismatic depression, and the cutting direction is along the thickness direction of the sample. It can be understood that the thickness direction of the sample corresponds to the depth direction of the sample addition groove 20.
[0075] In some embodiments, after adding the positive electrode material and the embedding agent into the sample addition groove 20, the following steps are further included: performing a degassing treatment on the positive electrode material and the embedding agent.
[0076] In some embodiments, performing a degassing treatment on the positive electrode material and the embedding agent includes: placing the sample preparation mold in a vacuum drying oven for degassing treatment.
[0077] In some embodiments, the time for degassing treatment is 2 h to 4 h. Optionally, the time for degassing treatment is 2 h, 2.2 h, 2.4 h, 2.6 h, 2.8 h, 3 h, 3.2 h, 3.4 h, 3.6 h, 3.8 h, or 4 h. Alternatively, the time for degassing treatment can also be within the range between any two of the above times.
[0078] In some embodiments, adding the positive electrode material and the embedding agent into the sample adding groove 20 includes: adding the positive electrode material and the embedding agent into the sample adding groove 20 and controlling the upper surface of the raw material to be located between the notch of the sample adding groove 20 and the surface of the through-hole member 50 away from the mold body.
[0079] In some embodiments, before adding the positive electrode material and the embedding agent into the sample adding groove 20, it further includes applying a release agent to the inner wall of the sample adding groove 20, the surface of the support member 40, the surface of the prismatic protrusion 30, and the surface of the through-hole member 50 facing the notch of the sample adding groove 20.
[0080] In some embodiments, the release agent includes at least one of fatty acid soap, fatty acid, paraffin, glycerol, petrolatum, silicone oil, and polyethylene glycol.
[0081] In some embodiments, the curing temperature is 60°C to 80°C. Optionally, the curing temperature is 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, 68°C, 69°C, 70°C, 71°C, 72°C, 73°C, 74°C, 75°C, 76°C, 77°C, 78°C, 79°C, or 80°C. Alternatively, the curing temperature can also be within the range between any two of the above temperatures.
[0082] In some embodiments, the curing time is 30 min to 90 min. Optionally, the curing time is 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, 65 min, 70 min, 75 min, 80 min, 85 min, or 90 min. Alternatively, the curing time can also be within the range between any two of the above times.
[0083] Refer to Figure 7 , in some embodiments, for the method for preparing a positive electrode material observation sample, using the sample preparation mold of any one of the above, it includes the following steps:
[0084] S200: Mix the positive electrode material and the embedding agent to obtain a sample preparation raw material;
[0085] S210: Apply a release agent to the inner wall of the sample adding groove 20, the surface of the support member 40, the surface of the prismatic protrusion 30, and the surface of the through-hole member 50 facing the notch of the sample adding groove 20;
[0086] S220: Add the sample preparation raw material into the sample loading groove 20 and control the upper surface of the sample preparation raw material to be between the notch of the sample loading groove 20 and the surface of the through-hole member 50 away from the mold body;
[0087] S230: Perform a defoaming treatment on the sample preparation raw material;
[0088] S240: Cure the sample preparation raw material to obtain a cured sample, and the cured sample has a prismatic depression;
[0089] S250: Remove the through-hole member 50, take out the cured sample, and cut the cured sample along the bottom edge of the prismatic depression.
[0090] In some embodiments, the method for preparing a positive electrode material observation sample, using the sample preparation mold of any one of the above, comprises the following steps:
[0091] (1) Mix the positive electrode material and the embedding agent to obtain a sample preparation raw material;
[0092] (2) Apply a release agent to the inner wall of the sample loading groove 20, the surface of the support member 40, the surface of the prismatic protrusion 30, and the surface of the through-hole member 50 facing the notch of the sample loading groove 20;
[0093] (3) Add the sample preparation raw material into the sample loading groove 20 and control the upper surface of the sample preparation raw material to be between the surface of the notch of the sample loading groove 20 and the surface of the through-hole member 50 away from the mold body;
[0094] (4) Perform a defoaming treatment on the sample preparation raw material;
[0095] (5) Cure the sample preparation raw material to obtain a cured sample, and the cured sample has a prismatic depression;
[0096] (6) Remove the through-hole member 50, take out the cured sample, and cut the cured sample along the bottom edge of the prismatic depression.
[0097] The following are specific embodiments
[0098] Example 1
[0099] Sample preparation mold:
[0100] In this embodiment, the sample preparation mold includes a mold body, a support member 40, and a through-hole member 50. The mold body is a cylinder with a bottom diameter of 30 mm and a height of 30 mm. A cylindrical sample addition groove 20 is provided on the top surface of the mold body. The depth of the sample addition groove 20 is 10 mm, and the bottom diameter of the sample addition groove 20 is 10 mm. The support member 40 is a cylindrical support member 40, the bottom surface of which is slightly smaller than the notch of the sample addition groove 20 and can move along the depth direction of the sample addition groove 20 within the sample addition groove 20. The height of the support member 40 is 5 mm. A prismatic protrusion 30 is provided on one bottom surface of the support member 40, and one side surface of the prismatic protrusion 30 is connected to the bottom surface of the support member 40. The height of the prismatic protrusion 30 is 2 mm, and the width of the side surface of the prismatic protrusion 30 provided on the support member 40 is 3 mm. The through-hole member 50 is an annular cylinder with a thickness of 3 mm, a bottom diameter of 30 mm, and an inner hole diameter of 10 mm. The through-hole member 50 can be disassembled into two semi-annular shapes with the same shape and size.
[0101] Preparation method of the positive electrode material observation sample:
[0102] In this embodiment, the preparation method of the positive electrode material observation sample uses the above sample preparation mold for sample preparation, including the following steps:
[0103] Step 1: Take an appropriate amount of epoxy resin embedding agent mother liquor (GATAN Resin-G2) and curing agent (GATAN Hardener-G2), and mix them evenly on a glass slide according to a volume ratio of 10:1;
[0104] Step 2: Take 20 mg of the ternary positive electrode material solid powder sample, add it to the mixed resin embedding agent, and stir for 5 minutes to make it evenly mixed;
[0105] Step 3: Place the support member 40 into the sample addition groove 20 with the surface provided with the prismatic protrusion 30 facing the notch of the sample addition groove 20; place the through-hole member 50 on the surface of the mold provided with the sample addition groove 20;
[0106] Step 4: Dip a cotton swab in a small amount of vaseline (Huilide petrolatum white vaseline analytical pure), evenly apply it on the groove wall of the sample addition groove 20, the surface of the support member 40, the surface of the prismatic protrusion 30, and the surface of the through-hole member 50 facing the notch of the sample addition groove 20. Use a blade or spatula to scrape an appropriate amount of the resin embedding agent mixed with the sample and put it into the sample addition groove 20 until the upper surface of the sample is slightly higher than the notch of the sample addition groove 20;
[0107] Step 5: Place the mold in a vacuum drying oven and keep it in a vacuum state at room temperature for 2 h to remove air bubbles;
[0108] Step 6: After removing the air bubbles, use a spatula to scrape the excess resin on the upper surface of the mold flat, and place the mold in a vacuum drying oven to cure at 80 °C for 30 min;
[0109] Step 7: Take out the mold, remove the through-hole part 50, pick out the cured sample with tweezers or a knife, and cut the sample preparation raw material along the depth direction of the conical depression to obtain a sample cross-section.
[0110] The sample prepared in Example 1 was observed. The observation method was as follows: The sample was adhered to a special sample stage for field emission electron microscopy with conductive glue (RH731-5, Nisshin EM Co., Ltd.) and placed in the sample chamber of a field emission electron microscope (Thermo Fisher Apreo 2) for observation. The observation results of the cross-section of the positive electrode material particles in Example 1 are as Figure 8 shown. Among them, the circular region located in the middle of the picture is the cross-sectional image of the positive electrode material particles without polishing. From Figure 8 it can be seen that the sample preparation mold in this application is suitable for preparing observation samples of the cross-section of positive electrode material particles for field emission electron microscopy observation. Using the sample preparation mold in this application for sample preparation can obtain a positive electrode material observation sample with good sample preparation effect and convenient for observation.
[0111] Example 2
[0112] Sample preparation mold:
[0113] The mold in this example is the same as that in Example 1.
[0114] Method for preparing positive electrode material observation sample:
[0115] In this example, the method for preparing the positive electrode material observation sample uses the above-mentioned sample preparation mold for sample preparation, including the following steps:
[0116] Step 1: Take an appropriate amount of epoxy resin embedding agent mother liquor (GATAN Resin-G2) and curing agent (GATAN Hardener-G2), and mix them evenly on a glass slide according to a volume ratio of 10:1;
[0117] Step 2: Take 30 mg of the ternary positive electrode material solid powder sample, add it to the mixed resin embedding agent, and stir for 5 minutes to make it evenly mixed;
[0118] Step 3: Place the support member 40 in the sample addition groove 20 with the side provided with the prismatic protrusion 30 facing the notch of the sample addition groove 20; place the through-hole part 50 on the surface of the mold provided with the sample addition groove 20;
[0119] Step 4: Dip a cotton swab in a small amount of vaseline (Huilide mineral white vaseline, analytical pure), evenly apply it to the groove wall of the sample addition groove 20, the surface of the support member 40, the surface of the prismatic protrusion 30, and the surface of the through-hole part 50 facing the notch of the sample addition groove 20. Use a blade or a spatula to scrape an appropriate amount of the resin embedding agent mixed with the sample and put it into the sample addition groove 20 until the upper surface of the sample is slightly higher than the notch of the sample addition groove 20;
[0120] Step 5: Place the mold in a vacuum drying oven and maintain a vacuum state at room temperature for 4 h to remove air bubbles.
[0121] Step 6: After removing the air bubbles, use a spatula to scrape the excess resin on the upper surface of the mold flat, and place the mold in a vacuum drying oven to cure at 60 °C for 90 min.
[0122] Step 7: Take out the mold, remove the through-hole part 50, use tweezers or a knife to pick out the cured sample, cut the sample preparation raw material along the depth direction of the conical depression, and control the cutting direction to pass through the vertex of the conical depression to obtain a sample cross-section.
[0123] The sample preparation obtained in Example 2 was observed. The observation method was as follows: Place the sample preparation section upward, use conductive adhesive (RH731-5 of Nissin EM Co., Ltd.) to stick the sample on a special sample stage for argon ion polishing to polish the section, and place it in an argon ion polisher (GATAN Ilion+Ⅱ MODEL697); Select the single-beam mode on the operation interface, and set the polishing program as follows: polish for 2 hours under the condition of 5 KeV and polish for 2 hours under the condition of 4 KeV. After polishing, take out the sample and place it in the sample chamber of a field emission electron microscope for observation. The observation results of the cross-section of the positive electrode material particles in Example 2 are as Figure 9 shown. Figure 9 It is an electron microscope image of a partial method of the observation surface of the observation sample of the positive electrode material prepared in Example 2. Among them, the circular region located in the middle of the picture is the polished cross-section image of the positive electrode material particles. From Figure 9 it can be seen that the sample preparation mold in this application is suitable for the sample preparation of the cross-section of the positive electrode material particles for field emission electron microscope observation. Using the sample preparation mold in this application for sample preparation can obtain a positive electrode material observation sample with good sample preparation effect and convenient for observation.
[0124] Comparative Example 1
[0125] Example of conventional sample preparation method:
[0126] Step 1: Take a glass slide (SM101 of Xingwei Optics), clean the surface with absolute ethanol, and keep it clean and dust-free.
[0127] Step 2: Take an appropriate amount of epoxy resin embedding agent mother liquor (GATAN Resin-G2) and curing agent (GATANHardener-G2), and mix them evenly on the glass slide according to a volume ratio of 10:1.
[0128] Step 3: Take 20 mg of the ternary positive electrode material solid powder sample, add it to the mixed resin embedding agent, and stir for 5 minutes to make it evenly mixed.
[0129] Step 4: Dip a lint-free cloth in a small amount of alcohol and wipe off the excess powder, leaving only the resin embedding agent mixed with the positive electrode material on the glass slide.
[0130] Step 5: Place the glass slide with the sample into a vacuum drying oven (Faithful DZ-1BCⅡ 24L), and place it under vacuum for 2 hours to remove the air bubbles in the resin.
[0131] Step 6: Take another clean and lint-free glass slide and cover the surface of the resin embedding agent mixed with the positive electrode material, covering it slowly to avoid mixing in air bubbles; support objects approximately the same thickness as the glass slide can be inserted on both sides between the two glass slides for support.
[0132] Step 7: Place the above sample into the vacuum drying oven and cure it at 60 °C for 90 min.
[0133] Step 8: Take out the above sample, and pry the resin block off the glass slide with a knife or forceps.
[0134] Step 9: Cut the resin block with pliers to form a cross-section.
[0135] The traditional method for preparing the cross-section of positive electrode material particles uses a glass slide as the sample carrier, and after fixing and curing with a support object and the glass slide, the shape and size of the sample are greatly affected by human factors. It is difficult to control the sample preparation quality and the repeatability of sample preparation is poor. At the same time, the sample prepared by the traditional sample preparation method has no indentation of the sample prepared by using the mold in this application, and there is no cutting guide, making it difficult to control the cutting quality of the cross-section.
[0136] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.
[0137] The above-described embodiments only represent several implementation manners of this application. Their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of this application, several modifications and improvements can still be made, and these all belong to the protection scope of this application. Therefore, the protection scope of the patent of this application should be subject to the appended claims, and the specification and drawings can be used to explain the content of the claims.
Claims
1. A sample making mold, characterized in that: include: A mold body and a prismatic protrusion; the mold body is provided with a sample adding groove, the prismatic protrusion is arranged inside the sample adding groove, one side of the prismatic protrusion is arranged at the bottom of the sample adding groove, and one side edge of the prismatic protrusion is arranged toward the notch of the sample adding groove.
2. The sample making mold according to claim 1, characterized in that: The height of the notch of the sample adding groove from the side edge of the prismatic protrusion facing the notch of the sample adding groove is 5 mm to 11 mm.
3. The sample making mold according to claim 1, characterized in that: The depth of the sample loading groove is 8 mm to 12 mm; and / or, The height difference between the side edge of the prismatic protrusion facing the notch of the sample loading groove and the side surface arranged at the bottom of the sample loading groove is 1 mm to 3 mm; and / or, The diameter of the bottom surface of the sample adding groove is 8 mm to 12 mm or the side length of the bottom surface of the sample adding groove is 8 mm to 12 mm; and / or, The width of the side surface of the prism-shaped protrusion arranged on the bottom of the sample adding groove is 2 mm to 4 mm.
4. The sample making mold according to claim 1, characterized in that: The two bottom surfaces of the prism-shaped protrusion are respectively arranged in contact with the two opposite side walls of the sample adding groove.
5. The sample making mold according to any one of claims 1 to 4, characterized in that: The sample preparation mold further comprises a support member, wherein the support member is arranged at the bottom of the sample adding groove, and a side surface of the prism-shaped protrusion is arranged on the surface of the support member.
6. The sample making mold according to claim 5, characterized in that: Each side surface of the support member is arranged in close contact with the groove wall of the sample adding groove.
7. The sample making mold according to claim 5, characterized in that: The thickness of the support member is 4 mm to 6 mm.
8. The sample making mold according to any one of claims 1 to 4 and 6 to 7, characterized in that: The sample preparation mold further comprises a through-hole component, which is detachably connected to the surface of the mold body provided with the sample adding groove, and the through-hole component is provided with a through hole, which is communicated with the sample adding groove.
9. The sample making mold according to claim 8, characterized in that: The thickness of the through-hole member is 2 mm to 4 mm; and / or, The cross section of the through hole is the same in shape and size as the notch of the sample adding slot.
10. A method for preparing a positive electrode material observation sample, characterized in that: Using the sample preparation mold according to any one of claims 1 to 9 comprises the following steps: Adding positive electrode material and embedding agent into the sample adding groove and submerging the prismatic protrusion; Curing the positive electrode material and the embedding agent to prepare a cured sample, wherein the cured sample has a prismatic depression; The cured sample is taken out and cut along the bottom edge of the prism-shaped recess.