A staining device for a sample of an electron microscope

Abstract

The application relates to a staining device for a sample of an electron microscope, which comprises a first container, a first partition, a first cover plate, a connecting rod, a second cover plate and a sample holder, the first container is provided with a first cavity, the top of the first cavity is provided with a first opening, the first partition divides the first cavity into a first chamber and a second chamber, the second chamber is provided with a second opening; the first cover plate is provided with the connecting rod, the end of the connecting rod is further provided with the second cover plate, the sample holder is arranged on the second cover plate, when the first cover plate is covered on the first opening, the second cover plate can be covered on the second opening under the driving of the connecting rod, so that the sample holder protrudes into the second chamber, the sample on the sample holder can be dyed by the dye, the dye or the toxic gas evaporated by the dye can be absorbed by the absorbent in the first chamber, and cannot overflow to the outside of the first cavity, safe dyeing of the sample is realized, and the operation is facilitated.

Description

Technical Field

[0001] This invention relates to the field of mechanics, and more specifically to a staining apparatus for samples used in an electron microscope. Background Technology

[0002] Lithium-ion batteries mainly consist of four parts: positive electrode material, negative electrode material, electrolyte, and separator. The binder is one of the important auxiliary functional materials in lithium-ion batteries, and it is the main source of the mechanical properties of the entire electrode, having a significant impact on the electrode manufacturing process and the electrochemical performance of the battery. The binder in lithium-ion battery electrodes usually adheres to the active material and is mostly a polymer material; the distribution of its various components is a key focus of analysis. Electron microscopy sample metal staining techniques are particularly useful for analyzing the structure of lithium battery electrodes, including the structure of the positive and negative electrode materials and the components adsorbed by the binder, thereby determining the quality and lifespan of the lithium battery. Electron microscopy imaging relies on the difference in electron penetration or reflection to create contrast. Optical color staining is meaningless in electron microscopy observation, and electron beams have poor penetration of heavy elements such as metals, resulting in darker colors. Therefore, heavy metal staining is often used on polymers or organic materials that are mainly composed of light elements.

[0003] Staining agents used in lithium batteries are toxic. For example, osmium tetroxide (OsO4) can fix the morphology of lipids and is commonly used as a fixative and staining agent for cells and tissues. Osmium tetroxide is also used to stain polymer materials. Osmium tetroxide binds to unsaturated double bond functional groups in molecular structures: Os staining is used to distinguish the arrangement of different components in mixed polymer materials. The vapors generated during osmium tetroxide fumigation or staining are toxic to the respiratory tract and eyes, requiring operation in a fume hood, which is inconvenient. Currently, there is no dedicated staining equipment for staining positive and negative electrode materials or binders of lithium batteries. Summary of the Invention

[0004] In view of the above problems, the present invention provides a staining device for samples for electron microscopes, which solves the problem of inconvenient staining operations of existing lithium battery positive and negative electrode materials or binders.

[0005] To achieve the above objectives, the present invention provides a staining apparatus for samples used in an electron microscope, comprising a first container, a first partition, a first cover plate, a connecting rod, a second cover plate, and a sample holder; the first container has a first cavity with a first opening at the top; the first partition is disposed within the first cavity, dividing the first cavity into an adjacent first chamber and a second chamber, the second chamber having a second opening at the top; the first chamber contains an absorbent, and the second chamber contains a stain; the first cover plate closes the first opening; the connecting rod passes through the first cover plate and is movable up and down relative to the first cover plate; the second cover plate is disposed at the end of the connecting rod, and closes the second opening under the action of the connecting rod; the sample holder is disposed on the second cover plate, and a sample is disposed on the sample holder, which protrudes into the second chamber when the second cover plate closes the second opening to stain the sample.

[0006] In some embodiments, a second partition is further included, which is circumferentially disposed along the edge of the second cover plate. When the second cover plate closes the second opening, the second partition forms a first gas passage to introduce the vapor of the dye evaporated by heating into the absorbent.

[0007] In some embodiments, a heater is also included, disposed at the bottom of the second chamber, for heating the dye.

[0008] In some embodiments, a heat insulation element is also included, which is disposed at the bottom of the first partition and is also disposed in the circumferential direction of the heater.

[0009] In some embodiments, the system further includes a second gas passage and a first gas pump, wherein the first chamber is connected to one end of the second gas passage and the first gas pump is connected to the other end of the second gas passage to extract gas from the first chamber.

[0010] In some embodiments, a second container is also included, the second cavity having a second cavity, the top of the second cavity having a third opening, the second cavity containing cleaning fluid, and the first cover plate can also be used to cover the third opening so that the sample on the sample holder is immersed in the cleaning fluid.

[0011] In some embodiments, the bottom of the second cavity is further provided with a drain outlet, and the dyeing apparatus further includes a first filter screen disposed at the drain outlet of the second cavity.

[0012] In some embodiments, the second container is further provided with an infusion line that communicates with the second cavity to deliver the cleaning fluid into the second cavity.

[0013] In some embodiments, a limiting member is also included, which is disposed at the end of the connecting rod away from the second cover plate. The limiting member is used to engage with the connection between the connecting rod and the first cover plate so that the sample on the second cover plate is suspended in the second cavity.

[0014] In some embodiments, a third cover plate is also included, the size of which is adapted to the size of the first opening, and the third cover plate can be used to cover the first opening.

[0015] Unlike existing technologies, in the above technical solution, the dyeing device includes a first container, a first partition, a first cover plate, a connecting rod, a second cover plate, and a sample holder. The first container has a first cavity with a first opening at the top. The first partition divides the first cavity into a first chamber and a second chamber, with the second chamber having a second opening. The second chamber is used to hold the dye, and the first chamber is used to hold the absorbent, which can adsorb harmful substances in the dye. The first cover plate has a connecting rod, and the end of the connecting rod has a second cover plate. The second cover plate has a sample holder. When the first cover plate is closed... When the first opening is open, the second cover plate can be closed at the second opening under the action of the connecting rod, so that the sample holder protrudes into the second chamber, allowing the sample on the sample holder to be stained with dye. When the first cover plate is closed at the first opening, the first cavity becomes a sealed cavity. During the staining process, the dye or the toxic gas evaporated by the dye will be absorbed by the absorbent in the first chamber and will not overflow to the outside of the first cavity. When removing the sample, the first cover plate, connecting rod, second cover plate and sample holder can be removed from the first cavity as a whole for sample drying. This achieves safe staining of the sample and is convenient to operate.

[0016] The above description of the invention is merely an overview of the technical solution of the present invention. In order to enable those skilled in the art to better understand the technical solution of the present invention and to implement it based on the description and drawings, and to make the above-mentioned objectives and other objectives, features and advantages of the present invention easier to understand, the following description is provided in conjunction with the specific embodiments and drawings of the present invention. Attached Figure Description

[0017] The accompanying drawings are only used to illustrate the principles, implementation methods, applications, features, and effects of specific embodiments of the present invention and other related contents, and should not be considered as limitations on the present invention.

[0018] In the accompanying drawings of the instruction manual:

[0019] Figure 1 This is a schematic diagram of the specific structure of the fume extractor described in the background art;

[0020] Figure 2 This is a schematic diagram of the specific structure of the staining apparatus for an electron microscope as described in the specific embodiment.

[0021] Figure 3 This is a schematic diagram of the specific structure of the sample fixing assembly described in the specific implementation method;

[0022] Figure 4 This is a schematic diagram illustrating the structure in which the connecting rod moves upward relative to the first cover plate in a specific embodiment.

[0023] Figure 5 This is a schematic diagram of the sample fixing assembly placed upside down in a specific embodiment;

[0024] Figure 6 This is a schematic diagram of the flow path of the first gas passage in a specific implementation embodiment;

[0025] Figure 7 This is a schematic diagram of the flow path of the second gas passage in a specific implementation embodiment;

[0026] Figure 8 This is a schematic diagram of the specific structure of the staining apparatus for electron microscope samples in use, as described in the specific embodiment.

[0027] Figure 9 This is a schematic diagram showing another usage state of the staining apparatus for electron microscopes described in the specific embodiment.

[0028] Figure 10 This is a schematic diagram of the staining apparatus for electron microscope samples in a non-use state, as described in the specific embodiment.

[0029] The reference numerals used in the above figures are explained as follows:

[0030] 1. First container;

[0031] 11. First cavity;

[0032] 111. The first opening;

[0033] 112. First partition;

[0034] 113. First chamber;

[0035] 114. Second chamber;

[0036] 115. Second opening;

[0037] 116. Absorbent;

[0038] 117. Dyes;

[0039] 12. Heater;

[0040] 13. Thermal insulation components;

[0041] 2. Sample fixing components;

[0042] 21. First cover plate;

[0043] 22. Connecting rod;

[0044] 23. Second cover plate;

[0045] 24. Sample rack;

[0046] 241. Sample;

[0047] 25. Second partition;

[0048] 251. Flow guide hole;

[0049] 26. Limiting components;

[0050] 3. Second container;

[0051] 31. Second cavity;

[0052] 311. Cleaning solution;

[0053] 312. The third opening;

[0054] 313. Drainage outlet;

[0055] 314. First filter screen;

[0056] 32. Infusion tubing;

[0057] 4. Third cover plate. Detailed Implementation

[0058] To illustrate the possible application scenarios, technical principles, implementable specific solutions, and achievable objectives and effects of this invention in detail, the following description, in conjunction with the listed specific embodiments and accompanying drawings, provides a detailed explanation. The embodiments described herein are merely illustrative of the technical solutions of this invention and are therefore intended only as examples, not as limiting the scope of protection of this invention.

[0059] In this document, the term "embodiment" means that a specific feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of the invention. The term "embodiment" appearing in various places throughout the specification does not necessarily refer to the same embodiment, nor does it specifically limit its independence or connection with other embodiments. In principle, in this invention, as long as there are no technical contradictions or conflicts, the technical features mentioned in each embodiment can be combined in any way to form corresponding implementable technical solutions.

[0060] Unless otherwise defined, the technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains; the use of related terms herein is merely for the purpose of describing particular embodiments and is not intended to limit the invention.

[0061] In the description of this invention, the term "and / or" is used to describe the logical relationship between objects, indicating that three relationships can exist. For example, A and / or B means: A exists, B exists, and A and B exist simultaneously. Additionally, the character " / " generally indicates that the preceding and following objects have an "or" logical relationship.

[0062] In this invention, terms such as “first” and “second” are used merely to distinguish one entity or operation from another, and do not necessarily require or imply any actual quantity, hierarchy, or order between these entities or operations.

[0063] Without further limitations, the use of terms such as “comprising,” “including,” “having,” or other similar open-ended expressions in this invention is intended to cover non-exclusive inclusion, which does not exclude the presence of additional elements in a process, method, or product that includes the stated elements, such that a process, method, or product that includes a list of elements may include not only those defined elements but also other elements not expressly listed, or elements inherent to such a process, method, or product.

[0064] Similar to the understanding in the Examination Guidelines, in this invention, expressions such as "greater than," "less than," and "exceeding" are understood to exclude the stated number; expressions such as "above," "below," and "within" are understood to include the stated number. Furthermore, in the description of the embodiments of this invention, "multiple" means two or more (including two), and similar expressions related to "multiple" are also understood in this way, such as "multiple groups" and "multiple times," unless otherwise explicitly specified.

[0065] In the description of the embodiments of the present invention, the spatial related expressions used, such as "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "vertical," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the specific embodiments or drawings. They are only for the purpose of describing the specific embodiments of the present invention or for the reader's understanding, and do not indicate or imply that the device or component referred to must have a specific position, a specific orientation, or be constructed or operated in a specific orientation. Therefore, they should not be construed as limitations on the embodiments of the present invention.

[0066] Unless otherwise explicitly stated or limited, the terms "installation," "connection," "linking," "fixing," and "setting," as used in the description of the embodiments of this invention, should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral arrangement; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal connection of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this invention according to the specific circumstances.

[0067] Unless otherwise explicitly stated or limited, the terms "installation," "connection," "linking," "fixing," and "setting," as used in the description of the embodiments of this invention, should be interpreted broadly. For example, "connection" can be a fixed connection, a detachable connection, or an integral arrangement; it can be a mechanical connection, an electrical connection, or a communication connection; it can be a direct connection or an indirect connection through an intermediate medium; it can be the internal connection of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in the embodiments of this invention according to the specific circumstances.

[0068] It should be noted that the dye 117 shown in this application has two commonly used staining methods. One is immersion staining: soaking in a 2% OsO4 solution, or directly immersing in osmium tetroxide to react with it; the other is fumigation staining: bulk polymer materials are often stained using fumigation, where the sample 241 is stained with the vapor produced by heating dye 117. The sectioning effect after staining is better than that after sectioning, such as... Figure 1 In the prior art, bulk osmium tetroxide crystals are placed at the bottom of a container, and the bottom container is heated to generate vapor, which is then evaporated into the sample 241 suspended at the top of the container to stain the sample 241.

[0069] In this application, sample 241 can be a binder. Lithium-ion battery binders are materials used to firmly bond various components together within the battery. These binders typically need to possess good adhesion, strength, and high-temperature resistance, making them a crucial structure affecting electrode quality. The particle size, shape, material distribution, and microstructure of the binder all influence electrode quality and are commonly analyzed using SEM. Typical SEM images can observe the appearance of the binder and active materials, revealing information such as particle size and uniformity. The binder adheres to the active material and is mostly a polymer; the distribution of various substances is a key focus of the analysis. Since visual identification is not possible, ESB mode is used to distinguish materials. ESB enhances the ability to differentiate between carbon (C) and phosphorus (F). Another component, CMC, shares similar elemental composition with SBR (C, H, O), making it difficult to distinguish using general component analysis methods. The characteristic of OsO4 intercalating with C double bonds is used to calibrate SBR; Os staining allows for tracking the distribution of Os.

[0070] Among them, the sample 241 after being soaked or fumigated needs to be further cleaned to remove excess dye 117. For example, it can be soaked in pure water for 15 minutes, three times in total, and then the sample 241 is placed in a drying oven to dry for subsequent use.

[0071] Based on the above principles, this embodiment provides a staining device for a sample 241 of an electron microscope, including a first container 1, a first partition 112, a first cover plate 21, a connecting rod 22, a second cover plate 23, and a sample holder 24; the first container 1 has a first cavity 11, and the top of the first cavity 11 is provided with a first opening 111; the first partition 112 is disposed in the first cavity 11, and the first partition 112 is used to divide the first cavity 11 into an adjacent first chamber 113 and a second chamber 114, the top of the second chamber 114 is provided with a second opening 115, and the first chamber 113 is located within... An absorbent 116 is provided, and a dye 117 is provided in the second chamber 114. A first cover plate 21 is used to cover the first opening 111. A connecting rod 22 passes through the first cover plate 21 and can move up and down relative to the first cover plate 21. A second cover plate 23 is provided at the end of the connecting rod 22 and is used to cover the second opening 115 under the action of the connecting rod 22. A sample holder 24 is provided on the second cover plate 23 and a sample 241 is provided on the sample holder 24. The sample holder 24 is used to extend into the second chamber 114 when the second cover plate 23 covers the second opening 115 to dye the sample 241.

[0072] In this embodiment, the shape of the first partition 112 varies, resulting in different shapes for the first chamber 113 and the second chamber 114 formed by it. Preferably, the first partition 112 is annular, and it is disposed within the first cavity 11, dividing the first cavity 11 into annular first chamber 113 and cylindrical second chamber 114. The second chamber 114 is located at the center of the annular structure of the first chamber 113, meaning that the first chamber 113 and the second chamber 114 are coaxially arranged. The difference between the first opening 111 and the second opening 115 is that the first opening 111 is the opening of the first cavity 11, and the second opening 115 is the opening of the second chamber 114, specifically as follows: Figure 2 As shown, when the first cover plate 21 closes the first opening 111, both the first chamber 113 and the second chamber 114 in the first cavity 11 are sealed chambers.

[0073] It should be noted that the first cover plate 21 and the first opening 111 shown in this embodiment are sealed together, and the connection between the connecting rod 22 and the first cover plate 21 is also sealed. This method can effectively prevent harmful substances from overflowing through the gap between the first opening 111 and the first cover plate 21 during the dyeing process, thereby improving the operational safety of the entire device.

[0074] In some preferred embodiments, the edge of the first opening 111 is recessed downward by a certain distance to form a stepped structure. When the first cover plate 21 is closed on the first opening 111, the edge of the first cover plate 21 matches the stepped structure. This method facilitates the position calibration of the first cover plate 21 and avoids gaps when the first cover plate 21 is closed on the first opening 111. Especially when the first opening 111 is a circular opening, this method enables the first cover plate 21 to be coaxially closed with the first opening 111, which is convenient for use.

[0075] In this embodiment, the position or specific structure of the connecting rod 22 on the first cover plate 21 can be set according to actual conditions. When the first cover plate 21 is circular, the connecting rod 22 is preferably located at the center of the first cover plate 21. Optionally, the connection between the connecting rod 22 and the first cover plate 21 can be sealed by setting a soft silicone seal. The end of the connecting rod 22 is provided with a second cover plate 23. The shape of the second cover plate 23 is adapted to the shape of the second opening 115. When the second chamber 114 and the first chamber 113 are coaxially arranged and the second opening 115 is circular, the second cover plate 23 can be coaxially arranged with the connecting rod 22, so that the second cover plate 23 is subjected to more uniform force.

[0076] Please see Figures 2 to 5In this embodiment, the connecting rod 22 can move up and down relative to the first cover plate 21. The normal operating state is when the first cover plate 21 closes the first opening 111. The second cover plate 23 is located at the downward end of the connecting rod 22, that is, below the first cover plate 21. A sample holder 24 is also provided on the bottom surface of the second cover plate 23. The sample holder 24 can be an existing sample holder structure, and samples 241 are placed on the sample holder 24. It should be noted that the sample 241 shown in this embodiment can be any kind of item, preferably an adhesive sample 241 made of polymer material. This sample 241 can be a sample 241 before slicing or a sample 241 after slicing, preferably a sample 241 after slicing. Staining with dye 117 after slicing will make the staining of the sample 241 more complete. Multiple sets of samples 241 can be fixed on the sample holder 24. Specific methods of fixing the sample 241 include sticking, hanging, clamping, snapping, adsorption, etc., which are not limited in this embodiment.

[0077] In this embodiment, the first cover plate 21, the connecting rod 22, the second cover plate 23, and the sample holder 24 form a movable integral structure, which is referred to as the sample fixing assembly 2 for ease of description. The sample fixing assembly 2 shown in this embodiment can be removed from the first cavity 11 and placed upside down. This upside-down placement can be understood as placing the first cover plate 21 at the bottom, so that the second cover plate 23 on the connecting rod 22 is placed above the first cover plate 21, and the sample holder 24 on the second cover plate 23 is placed in an upright position. Specifically, as shown... Figure 5 As shown, this method facilitates placing the sample fixing component 2 directly in a drying oven or indoors for air drying or baking, and also facilitates removing the sample 241 from the sample rack 24.

[0078] In this embodiment, the first chamber 113 contains an absorbent 116, and the second chamber 114 contains a dye 117. The absorbent 116 is a liquid used to absorb toxic substances in the dye 117. Optionally, the dye 117 can be an OsO4 (or RuO4) solution, and its specific concentration can be set according to actual needs. The absorbent 116 can be NaHSO3. The dye 117 in the second chamber 114 can be used to immerse or fumigate the sample 241 on the sample holder 24, and the specific concentration can be adjusted according to actual needs.

[0079] The specific usage procedure of the dyeing device in this embodiment is as follows: place the dye 117 in the second chamber 114 and the absorbent 116 in the first chamber 113. Set the liquid level of the dye 117 in the second chamber 114 according to the different dyeing methods. Grab the sample fixing component 2 and cover the first cover plate 21 at the first opening 111. Note that when the first cover plate 21 is covered at the first opening 111, the second cover plate 23 is aligned with the second opening 115 and closed. The sample holder 24 and the sample 241 on the second cover plate 23 can extend into the second chamber 114. When using immersion dyeing, it is necessary to ensure that the liquid level in the second chamber 114 can fully wet the sample 241. When using fumigation dyeing, it is necessary to ensure that the liquid level in the second chamber 114 is lower than the lowest point of the sample 241 so as to fully fumigate the sample 241. It should be noted that when the second cover plate 23 of this embodiment closes the second opening 115, a gap may be left to facilitate the absorbent 116 to fully absorb the toxic substances in the second chamber 114 and reduce the toxic concentration when the first opening 111 is opened and closed.

[0080] The dyeing apparatus shown in this embodiment can be used to dye polymer materials, especially binders in lithium batteries. These binders are made of polymer materials and require the use of OsO4, a toxic substance, as dye 117. Slight carelessness can lead to safety risks. The dyeing apparatus shown in this application has a first chamber 113 and a second chamber 114 in the first cavity 11. The dye 117 is placed in the second chamber 114, and the absorbent 116 is placed in the first chamber 113. The second opening 115 on the second chamber 114 is covered by a second cover plate 23, which seals and isolates the dye 117 from the external environment during the dyeing process. Furthermore, the absorbent 116 absorbs the dye 117 to prevent it from overflowing from the first cavity 11, thus improving the operational safety of the entire dyeing process. The entire apparatus is easy to use, safe, and portable.

[0081] Please see Figure 6 In some embodiments, a second partition 25 is also included, which is arranged circumferentially along the edge of the second cover plate 23. When the second cover plate 23 is closed on the second opening 115, the second partition 25 forms a first gas passage to introduce the vapor of the dye 117 evaporated by heating into the absorbent 116.

[0082] In this embodiment, the second partition 25 is disposed around the edge of the second cover plate 23. When the second cover plate 23 is closed over the second opening 115, the second partition 25 can form a sealed cavity around the edge of the second opening 115. In this sealed cavity, the overflowing dye 117 or dye 117 vapor cannot flow directly to the first opening 111, but can only react with the absorbent 116 solution in the sealed cavity. Specifically, when using a fumigation method, the dye 117 vapor overflows from the gap at the connection between the second cover plate 23 and the second opening 115 into this sealed cavity, and then reacts with the absorbent 116. The first gas passage shown in this embodiment is also the vapor flow path, specifically as follows: Figure 6 As shown by the middle arrow, this method can further reduce the risk of toxic gas spills.

[0083] In a preferred embodiment, a plurality of flow guide holes 251 may be provided at the bottom of the second partition 25 to allow the absorbent 116 to flow sufficiently between the second partition 25 and the first partition 112, thereby maintaining the concentration of the absorbent 116.

[0084] In some embodiments, a heater 12 is also included, which is disposed at the bottom of the second chamber 114 and is used to heat the dye 117.

[0085] The heater 12 shown in this embodiment can be a heating coil. The heater 12 can be integrated into the bottom of the first container 1, specifically embedded in the bottom of the second chamber 114, so as to fully heat the dye 117 in the second chamber 114.

[0086] In some embodiments, a heat insulation element 13 is also included. The heat insulation element 13 is disposed at the bottom of the first partition 112 and is also disposed around the heater 12. It should be noted that the heat insulation element 13 being disposed at the bottom of the first partition 112 can be understood as being disposed at the junction of the first chamber 113 and the second chamber 114, and does not strictly refer to the bottom surface of the first partition 112. The specific size of the heat insulation element 13 can be set according to actual needs. For example, the heat insulation element 13 can also be annularly disposed on the outer circumference of the second chamber 114 to fully absorb the heat of the heating element, reduce the impact of the heat of the heating element on the temperature of the absorbent 116, and maintain the concentration of the absorbent 116.

[0087] In some embodiments, the system further includes a second gas passage and a first air pump, wherein the first chamber 113 is connected to one end of the second gas passage and the first air pump is connected to the other end of the second gas passage to extract gas from the first chamber 113.

[0088] In this embodiment, the second gas passage is connected to the first chamber 113, and is specifically located near the top of the first chamber 113. This prevents the absorbent 116 from entering the second gas passage. The other end of the second gas passage is connected to a first air pump, which can use the second gas passage to extract gas from the first chamber 113, preventing toxic gas overflowing from the second chamber 114 from escaping through the first opening 111. It should be noted that this embodiment also includes a third gas passage, which can be connected to an external gas source and is also connected to the first chamber 113. This helps maintain pressure balance within the first chamber 113. Optionally, the third gas passage and the second gas passage are positioned opposite each other on opposite sides of the first chamber 113, as shown below. Figure 7 As indicated by the middle arrow, this better matches the gas flow characteristics and improves pumping efficiency.

[0089] Please see Figures 8 to 10 In some embodiments, a second container 3 is also included, the second container 3 having a second cavity 31, the top of the second cavity 31 having a third opening 312, the second cavity 31 having a cleaning solution 311, and the first cover plate 21 can also be used to cover the third opening 312 so that the sample 241 on the sample holder 24 is immersed in the cleaning solution 311.

[0090] This embodiment also includes a second container 3, which has a second cavity 31. It should be noted that the second container 3 and the first container 1 can be integrated into a single unit; that is, the first container 1 and the second container 3 can refer to two areas of a single component. Alternatively, the second container 3 and the first container 1 can be two independent components. This embodiment does not impose any limitations on this. For example, when staining sample 241 in the first cavity 11, cleaning solution 311 can be simultaneously added to the second cavity 31 for cleaning sample 241, thereby improving staining efficiency.

[0091] The second cavity 31 contains a cleaning solution 311. The cleaning solution 311 can be pure water or other solutions with cleaning functions. This embodiment does not limit this, and the specific type of cleaning solution 311 can be set according to actual needs. The top of the second cavity 31 is also provided with a third opening 312. The size of the third opening 312 can be the same as the size of the first opening 111, so that the first cover plate 21 can directly cover the third opening 312. Preferably, the edge of the third opening 312 can also be provided with a downwardly recessed stepped structure. This method facilitates the rapid alignment of the first cover plate 21 when closing the third opening 312.

[0092] After staining, the sample 241 on the sample holder 24 needs to be cleaned in the cleaning solution 311 a certain number of times for observation. The second cavity 31 shown in this embodiment is used to hold the stained sample 241. When using it, the sample fixing component 2 can be moved from the first cavity 11 to the second cavity 31. The operation is simple.

[0093] In some embodiments, the bottom of the second cavity 31 is further provided with a drain outlet 313, and the staining apparatus also includes a first filter screen 314, which is disposed at the drain outlet 313 of the second cavity 31. The first filter screen 314 can prevent the sample 241 from being directly discharged from the drain outlet 313 after falling. Optionally, the drain outlet 313 can be funnel-shaped to guide the washing liquid 311 during the discharge process, so that the washing liquid 311 can be discharged more fully.

[0094] In some embodiments, the second container 3 is further provided with an infusion line 32, which communicates with the second cavity 31 to deliver the cleaning solution 311 into the second cavity 31. Optionally, a one-way valve may also be provided at the connection between the infusion line 32 and the second cavity 31 to prevent the cleaning solution 311 in the second cavity 31 from flowing back.

[0095] In some embodiments, a limiting member 26 is also included. The limiting member 26 is disposed at the end of the connecting rod 22 away from the second cover plate 23. The limiting member 26 is used to engage at the connection between the connecting rod 22 and the first cover plate 21, so that the sample 241 on the second cover plate 23 is suspended in the second cavity 31.

[0096] In this embodiment, the limiting member 26 is disposed at the other end of the connecting rod 22, and the limiting member 26 is used to limit the connecting rod 22 in the vertical direction. Optionally, the limiting member 26 can be disc-shaped, and the edge of the limiting member 26 can extend outward to increase the gripping area of ​​the connecting rod 22. When adjusting the connecting rod 22, the user can directly grasp the limiting member 26 for adjustment.

[0097] In some preferred embodiments, the connection between the first cover plate 21 and the connecting rod 22 is also provided with a downwardly recessed groove. This method makes it easy to hide the limiting member 26 in the groove when the entire sample fixing assembly 2 is inverted. When the entire sample fixing assembly 2 is inverted, the bottom surface of the first cover plate 21 is used as the supporting contact surface, making the entire sample fixing assembly 2 less likely to tip over and easier to place.

[0098] In some embodiments, a third cover plate 4 is also included, the size of which is adapted to the size of the first opening 111. The third cover plate 4 can be used to cover the first opening 111. In this embodiment, the third cover plate 4 can directly cover the first opening 111 or the third opening 312 when the dyeing device is not used, to prevent external dust from entering the first cavity 11 or the second cavity 31.

[0099] Specifically, the entire dyeing apparatus can be used in the following steps:

[0100] (1) A suitable amount of dye 117OsO4 solution is loaded into the second chamber 114, and absorbent 116NaHSO3 solution is loaded into the first chamber 113.

[0101] (2) A complex array of test pieces (i.e., sample 241) is placed on the sample holder 24 of the sample fixing assembly 2 and placed into the second chamber 114.

[0102] (3) Turn on the air extraction equipment (i.e., the first air pump) and the heating equipment (i.e., the heating element) to generate OsO4 vapor.

[0103] (4) After the vapor deposition has been completed for a period of time, turn off the heating element, take out the sample fixing component 2, and cover it with the third cover plate 4.

[0104] (5) Place the sample holder 24 into the second cavity 31, and after several cycles of the cleaning process, remove it.

[0105] (6) Place the sample fixing component 2 upside down in a drying oven to air dry. After drying, the sample can be observed under an electron microscope.

[0106] In the above technical solution, the dyeing device includes a first container 1, a first partition 112, a first cover 21, a connecting rod 22, a second cover 23, and a sample holder 24. The first container 1 has a first cavity 11, and the top of the first cavity 11 is provided with a first opening 111. The first partition 112 divides the first cavity 11 into a first chamber 113 and a second chamber 114. The second chamber 114 has a second opening 115. The second chamber 114 is used to place the dye 117, and the first chamber 113 is used to place the absorbent 116. The absorbent 116 can adsorb harmful substances in the dye 117. The first cover 21 is provided with a connecting rod 22, and the end of the connecting rod 22 is also provided with a second cover 23. The second cover 23 is provided with a sample holder 24. When the first cover 21 is closed, the sample holder 24 is placed on the second cover 23. When the first opening 111 is in place, the second cover plate 23 can be closed at the second opening 115 under the action of the connecting rod 22, so that the sample holder 24 protrudes into the second chamber 114, allowing the sample 241 on the sample holder 24 to be dyed by the dye 117. When the first cover plate 21 is closed at the first opening 111, the first cavity 11 becomes a sealed cavity. During the dyeing process, the dye 117 or the toxic gas evaporated by the dye 117 will be absorbed by the absorbent 116 in the first chamber 113 and will not overflow to the outside of the first cavity 11. When removing the sample, the first cover plate 21, the connecting rod 22, the second cover plate 23 and the sample holder 24 can be removed from the first cavity 11 as a whole for the drying of the sample 241, thus achieving safe dyeing of the sample 241 and facilitating operation.

[0107] Finally, it should be noted that although the above embodiments have been described in the description and drawings of this invention, this should not limit the scope of patent protection of this invention. Any technical solutions that are based on the essential concept of this invention, utilize the content described in the description and drawings of this invention to make equivalent structural or procedural substitutions or modifications, as well as the direct or indirect application of the technical solutions of the above embodiments to other related technical fields, are all included within the scope of patent protection of this invention.

Claims

1. A staining apparatus for samples used in an electron microscope, characterized in that, include: A first container has a first cavity, and the top of the first cavity has a first opening; A first partition is disposed within the first cavity. The first partition is used to divide the first cavity into a first chamber and a second chamber that are arranged adjacently. The top of the second chamber is provided with a second opening. An absorbent is disposed in the first chamber and a dye is disposed in the second chamber. A first cover plate is used to close the first opening; A connecting rod passes through the first cover plate and can move up and down relative to the first cover plate; A second cover plate is disposed at the end of the connecting rod, and the second cover plate is used to cover the second opening under the action of the connecting rod; A sample holder is disposed on the second cover plate, and the sample is disposed on the sample holder. The sample holder is used to extend into the second chamber when the second cover plate closes the second opening to stain the sample.

2. The staining apparatus for samples used in an electron microscope according to claim 1, characterized in that, Also includes: The second partition is arranged circumferentially along the edge of the second cover plate. When the second cover plate is closed on the second opening, the second partition forms a first gas passage to introduce the vapor of the dye evaporated by heating into the absorbent.

3. The staining apparatus for samples used in an electron microscope according to claim 1, characterized in that, Also includes: A heater is disposed at the bottom of the second chamber, and the heater is used to heat the dye.

4. The staining apparatus for samples used in an electron microscope according to claim 3, characterized in that, Also includes: A heat insulation element is disposed at the bottom of the first partition plate, and the heat insulation element is also disposed in the circumferential direction of the heater.

5. The staining apparatus for samples used in an electron microscope according to claim 1, characterized in that, Also includes: A second gas passage, wherein the first chamber is connected to one end of the second gas passage; A first air pump is connected to the other end of the second gas passage to extract gas from the first chamber.

6. The staining apparatus for samples used in an electron microscope according to claim 1, characterized in that, Also includes: The second container has a second cavity, the top of which has a third opening. The second cavity contains a cleaning solution. The first cover plate can also be used to close the third opening so that the sample on the sample holder is immersed in the cleaning solution.

7. The staining apparatus for samples used in an electron microscope according to claim 6, characterized in that, The bottom of the second cavity is also provided with a drain outlet, and the dyeing device further includes: The first filter screen is located at the drain outlet of the second cavity.

8. The staining apparatus for samples used in an electron microscope according to claim 6, characterized in that, The second container is also provided with an infusion line, which is connected to the second cavity to deliver the cleaning solution into the second cavity.

9. The staining apparatus for samples used in an electron microscope according to claim 6, characterized in that, Also includes: A limiting member is provided at the end of the connecting rod away from the second cover plate. The limiting member is used to engage at the connection between the connecting rod and the first cover plate, so that the sample holder on the second cover plate is suspended in the second cavity.

10. The staining apparatus for samples used in an electron microscope according to claim 6, characterized in that, Also includes: A third cover plate, the size of which is adapted to the size of the first opening, is used to cover the first opening.

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