Powder sample preparation device for scanning electron microscope

Abstract

The utility model provides a powder sample preparation device for a scanning electron microscope, and belongs to the technical field of lithium battery test equipment. The device comprises a sample preparation box body and a sample preparation assembly, wherein a cabin door is arranged on the sample preparation box body. The sample preparation assembly comprises an air inlet pipe, an air outlet pipe, a feeding port, a blocking part and a sample preparation conductive adhesive, the air inlet pipe is arranged in the horizontal direction, one end of the air inlet pipe penetrates through the sample preparation box body, the other end of the air inlet pipe is used for being connected with an air source, the feeding port is formed in the top of the sample preparation box body and connected with the air inlet pipe, and the blocking part is arranged in the sample preparation box body and right faces one end of the air inlet pipe; the sample preparation conductive adhesive is installed at the bottom of the sample preparation box and located between the blocking part and one end of the air inlet pipe, and the air outlet pipe is arranged on the other side wall of the sample preparation box in a penetrating mode. Cross contamination interference between sample tests can be avoided, meanwhile, powder materials are quantitatively controlled to be scattered on the conductive adhesive, and accurate and efficient sample preparation is achieved.

Description

Technical Field

[0001] The utility model relates to the technical field of lithium battery test equipment, and particularly relates to a powder sample preparation device for a scanning electron microscope. Background Art

[0002] A scanning electron microscope (SEM) is a large-scale precision instrument for high-resolution micro-area morphology analysis, which is widely used in the field of lithium battery materials. It can be used to analyze the morphology, composition, structure, etc. of the positive and negative electrode powder materials of lithium batteries. The physical and chemical and electrochemical properties of the positive and negative electrode materials of the battery are related to the performance of the final battery. Correct and efficient use of the scanning electron microscope to study lithium battery materials helps materials development, process development, and product development engineers analyze the positive and negative electrode materials of lithium batteries, thereby improving the comprehensive performance of lithium batteries.

[0003] In the related art, when using a scanning electron microscope to photograph the positive and negative electrode powder samples of lithium batteries, the sample preparation is generally carried out by a staff member using a cotton swab or a toothpick-like tool to dip a small amount of powder and scatter it on the fixed area of the conductive adhesive, then blow off the excess powder sample, and then move it to the electron microscope to complete the test.

[0004] Adopting the sample preparation method in the related art, by manually dipping a small amount of powder and scattering it on the conductive adhesive, the dipping amount is not easy to be artificially controlled, and there is often sample accumulation and uneven scattering on the conductive adhesive. At the same time, when batch sample tests are required, blowing off the powder scattered on the experimental table and in the air is likely to cause cross-contamination between samples. Operating directly in the air will also cause dust to fill the air in the sample room, which is harmful to the test personnel and equipment. Summary of the Utility Model

[0005] The embodiment of the utility model provides a powder sample preparation device for a scanning electron microscope, which can avoid cross-contamination interference between sample tests and quantitatively control the scattering of powder materials on the conductive adhesive to achieve accurate and efficient sample preparation. The technical solution is as follows:

[0006] A powder sample preparation device for a scanning electron microscope includes: a sample preparation box body and a sample preparation assembly.

[0007] A hatch door is arranged on the sample preparation box body.

[0008] The sample preparation assembly includes an air inlet pipe, an air outlet pipe, a feed inlet, a blocking part, and a sample preparation conductive adhesive. The air inlet pipe is arranged horizontally and one end thereof penetrates into the sample preparation box body, and the other end is used for connecting a gas source. The feed inlet is arranged at the top of the sample preparation box body and is connected to the air inlet pipe. The blocking part is arranged in the sample preparation box body and is arranged opposite to one end of the air inlet pipe. The sample preparation conductive adhesive is installed at the bottom of the sample preparation box body and is located between the blocking part and one end of the air inlet pipe. The air outlet pipe penetrates through the other side wall of the sample preparation box body.

[0009] Optionally, the blocking part is an impact sphere, and the blocking part is hoisted on the top wall of the sample preparation box body.

[0010] Optionally, a narrow pipe section is arranged between one end of the air inlet pipe and the inner side wall of the sample preparation box body. The diameter of the narrow pipe section is smaller than the diameters of both ends of the air inlet pipe, and the feed inlet is connected to the narrow pipe section.

[0011] Optionally, a screen is arranged at the feed inlet.

[0012] Optionally, it further includes a feed pipe and an infrared heating device. The feed inlet is connected to the narrow pipe section through the feed pipe, and the infrared heating device is arranged around the feed inlet and the feed pipe.

[0013] Optionally, it further includes a vibration block, and the vibration block is connected to the feed inlet.

[0014] Optionally, the sample preparation conductive adhesive is in a plate shape, including a sample preparation area and an edge area arranged around the sample preparation area, and a tape is pasted on the edge area.

[0015] Optionally, the gas source is a nitrogen source.

[0016] Optionally, the height of one end of the air inlet pipe is higher than the height of one end of the air outlet pipe located inside the sample preparation box body.

[0017] Optionally, it further includes a guide rail and a tray. The tray is slidably mounted on the guide rail through a moving motor. One end of the guide rail is connected to the hatch, and the other end of the guide rail is located between the blocking part and one end of the air inlet pipe. The sample preparation conductive adhesive is arranged on the tray.

[0018] The beneficial effects brought by the technical solution provided by the embodiment of the present invention at least include:

[0019] By using the powder sample preparation device for a scanning electron microscope provided by the embodiment of the present invention, a sample preparation space isolated from the outside is provided for the lithium-ion positive and negative electrode powder samples by setting the sample preparation box body. During sample preparation, the experimental powder sample is introduced through the feed inlet, and an external gas source is connected through the air inlet pipe to provide fluid power. By adjusting the flow rate of the carrier gas, the injection amount of the powder sample, and the horizontal and vertical distances between the sample preparation conductive adhesive 25 and the blocking part 24, the powder sample is evenly dispersed on the sample preparation conductive adhesive 25 without being affected by human factors. After opening the door to take the sample, the inside of the sample preparation box body 1 can also be purged and the residual dust can be discharged through the air inlet pipe 21 and the air outlet pipe 22 to prepare for the next sample preparation environment. It can avoid cross-contamination interference in the sample test room while quantitatively controlling the scattering of the powder material on the conductive adhesive, realizing accurate and efficient sample preparation. Description of the Drawings

[0020] To more clearly illustrate the technical solutions in the embodiments of the present invention, the following will briefly introduce the accompanying drawings required for the description of the embodiments. Obviously, the accompanying drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other accompanying drawings can be obtained based on these drawings.

[0021] Figure 1 is a schematic three-dimensional structure diagram of a powder sample preparation device for a scanning electron microscope provided by an embodiment of the present invention;

[0022] Figure 2 is a schematic internal structure diagram of a powder sample preparation device for a scanning electron microscope provided by an embodiment of the present invention;

[0023] Figure 3 is Figure 2 a cross-sectional schematic diagram at A-A in

[0024] Figure 4 is a schematic structure diagram of a conductive adhesive provided by an embodiment of the present invention.

[0025] In the figure: 1 - sample preparation box body; 2 - sample preparation assembly; 3 - guide rail; 4 - tray; 11 - hatch door; 21 - intake pipe; 22 - exhaust pipe; 23 - feed inlet; 24 - blocking part; 25 - conductive adhesive; 25a - sample preparation area; 25b - edge area; 211 - narrow pipe section; 231 - sieve mesh; 232 - feed pipe; 233 - infrared heating device; 234 - vibration block; a - gas source. Detailed implementation manners

[0026] To make the objectives, technical solutions, and advantages of the present invention clearer, the following will further describe the embodiments of the present invention in detail in conjunction with the accompanying drawings.

[0027] Figure 1 is a schematic three-dimensional structure diagram of a powder sample preparation device for a scanning electron microscope provided by an embodiment of the present invention; Figure 2 is a schematic internal structure diagram of a powder sample preparation device for a scanning electron microscope provided by an embodiment of the present invention; Figure 3 is Figure 2 a cross-sectional schematic diagram at A-A in Figure 4 is a schematic structure diagram of a conductive adhesive provided by an embodiment of the present invention. As Figures 1 to 4 shown, an embodiment of the present invention provides a powder sample preparation device for a scanning electron microscope, including: a sample preparation box body 1 and a sample preparation assembly 2.

[0028] Among them, a hatch door 11 is provided on the sample preparation box body 1.

[0029] The sample preparation component 2 includes an air inlet pipe 21, an air outlet pipe 22, a feed port 23, a blocking portion 24 and a sample preparation conductive adhesive 25. The air inlet pipe 21 is arranged in the horizontal direction and one end is passed through the sample preparation box 1, and the other end is used to connect to the air source a. The feed port 23 is arranged at the top of the sample preparation box 1 and connected to the air inlet pipe 21. The blocking portion 24 is arranged in the sample preparation box 1 and is arranged opposite to one end of the air inlet pipe 21. The sample preparation conductive adhesive 25 is installed at the bottom of the sample preparation box 1 and is located between the blocking portion 24 and one end of the air inlet pipe 21. The air outlet pipe 22 is passed through the other side wall of the sample preparation box 1.

[0030] In the embodiment of the utility model, when powder sample preparation is required, a plate-shaped or sheet-shaped conductive glue 25 is placed at a designated position in the sample preparation box 1, and the hatch 11 is closed. The positive and negative electrode powders of the lithium battery are added through the feed port 23, and the external gas source a is started to pass inert gas into the air inlet pipe 21. The added powders collide with each other in the air inlet pipe 21, disperse and mix with the gas, and are ejected from one end of the air inlet pipe 21 to the inside of the sample preparation box 1 under the pressure of the gas source a. After being ejected, the gas-solid mixture will contact the blocking part 24 arranged at intervals opposite to the outlet. Under the obstruction of the blocking part 24, the gas-solid mixture will be further dispersed after the collision and scattered on the sample preparation conductive glue 25 arranged at the bottom under the action of gravity. After the material is unloaded, the carrier gas of the gas source a is turned off, and the preset time is continued to be waited. After the powder is completely scattered on the sample preparation conductive glue 25, the hatch 11 can be opened to take out the sample preparation conductive glue 25, and it can be moved to the relevant equipment for on-machine testing. At the same time, before preparing and testing the next sample, a vacuum cleaner can be connected to the air outlet pipe 22, and inert gas can be blown in conjunction with the gas source a to extract the powder floating inside the sample preparation box 1 and scattered in other locations from the sample preparation box 1, thereby ensuring that the sample preparation device removes environmental dust.

[0031] The powder sample preparation device for scanning electron microscope provided by the embodiment of the utility model is adopted, and the sample preparation box 1 is provided to provide a sample preparation space isolated from the outside world for the positive and negative electrode powder samples of lithium battery. During sample preparation, the experimental powder sample is lowered through the feed port, and the fluid power is provided by the external gas source a through the air inlet pipe 21. By adjusting the flow rate of the carrier gas, the sample injection amount of the powder sample, and the horizontal and vertical distance between the sample preparation conductive glue 25 and the blocking part 24, the powder sample is evenly dispersed on the sample preparation conductive glue 25 without being affected by human factors. After opening the door for sampling, the residual dust in the sample preparation box 1 can also be purged and discharged through the air inlet pipe 21 and the air outlet pipe 22 to prepare the sample preparation environment for the next time. While avoiding cross-contamination interference between sample tests, it can quantitatively control the powder material scattered on the conductive glue to achieve accurate and efficient sample preparation.

[0032] Optionally, the blocking portion 24 is an impact sphere, and the blocking portion 24 is hoisted on the top wall of the sample preparation box body 1. Exemplarily, in the embodiment of the present invention, the blocking portion 24 is arranged to be hoisted on the inner top wall of the sample preparation box body 1 and is coaxially and spaced from the air inlet pipe 21. The impact sphere-shaped blocking portion 24 has a smooth outer surface as a whole when contacting the gas-solid mixture. Since the arc surface positions of the contact are different, the trajectories and final positions of the powder sample when encountering resistance and falling are more dispersed, so that the powder sample can fall more evenly on the underlying sample preparation conductive adhesive 25, further improving the sample preparation yield. At the same time, it can also reduce the probability of the powder sample adhering and staying on the surface of the blocking portion 24, which is convenient for cleaning.

[0033] Optionally, a narrow pipe section 211 is provided between one end of the air inlet pipe 21 and the inner side wall of the sample preparation box body 1. The diameter of the narrow pipe section 211 is smaller than the diameters of both ends of the air inlet pipe 21, and the feed inlet 23 is connected to the narrow pipe section 211. Exemplarily, in the embodiment of the present invention, by providing a narrow pipe section 211 with a relatively smaller overall pipe diameter with respect to the air inlet pipe 21 at the connection position between the air inlet pipe 21 and the feed inlet 23, and the diameter of the narrow pipe section 211 is one-third of the pipe diameters of the wider pipe sections at both ends of the air inlet pipe 21, the air inlet pipe 21 as a whole forms a Venturi tube structure. According to the Venturi effect, the flow rate of a fluid (gas or liquid) will increase in the narrowed part of the pipe. According to Bernoulli's law, the increase in flow rate will lead to a decrease in fluid pressure. This decrease in pressure forms a low-pressure area near the fluid, that is, an adsorption effect will be generated in the narrow pipe section 211 area, sucking the powder sample fed from the feed inlet 23 into the air inlet pipe 21 sufficiently and introducing it into the sample preparation box body 1 through the carrier gas sufficiently, ensuring the sample preparation accuracy and sample preparation efficiency.

[0034] Optionally, a screen 231 is provided at the feed inlet 23. Exemplarily, in the embodiments of the present invention, by providing a screen 231 at the feed inlet 23, such as using a 200-mesh screen, large agglomerated particles in the fed powder sample can be blocked to avoid affecting the final sample preparation. Further, in cooperation with the operation of the screen 231, a vibration block 234 structure driven by a motor can also be provided at the feed inlet 23 to apply a certain amplitude of vibration to the screen 231 when the material is falling onto the screen 231, further helping the powder material to disperse and smoothly enter the sample preparation box body 1 from the screen 231, reducing the deposition and blockage of large agglomerated particles, and further improving the sample preparation efficiency.

[0035] Optionally, it further includes a feed pipe 232 and an infrared heating device 233. The feed port 23 is connected to the narrow pipe section 211 through the feed pipe 232, and the infrared heating device 233 is arranged around the feed port 23 and the feed pipe 232. Exemplarily, in the embodiment of the present invention, by arranging the infrared heating device 233 around the feed port 23 and the feed pipe 232, infrared heating can be performed during the process of the powder sample leading to the intake pipe 21 to dry the residual moisture that may exist in the powder material, further improving the sample preparation yield.

[0036] Optionally, the sample preparation conductive adhesive 25 is in a plate shape, including a sample preparation area 25a and an edge area 25b arranged around the sample preparation area 25a, and a tape is pasted on the edge area 25b. Exemplarily, in the embodiment of the present invention, by pasting a tape on the edge area 25b at the edge of the sample preparation conductive adhesive 25, the falling powder sample will only be scattered and adhered in the sample preparation area 25a required in the middle. After the sample preparation is completed, tearing off the excess tape can make the powder sample only disperse in the area required for the experiment.

[0037] Optionally, the gas source a is a nitrogen gas source a. Exemplarily, in the embodiment of the present invention, using an inert gas as the carrier gas has a low price and will not cause pollution, avoiding harm to the physical health of experimental personnel.

[0038] Optionally, one end of the intake pipe 21 is higher than one end of the outlet pipe 22 located inside the sample preparation box body 1. Exemplarily, in the embodiment of the present invention, during the internal purging operation, the gas introduced through the intake pipe 21 with a higher height will cooperate with the suction negative pressure of the outlet pipe 22 with a lower height to form an air flow from top to bottom inside the sample preparation box body 1, so as to blow down and discharge the possible dust inside as a whole. At the same time, the lower setting of the outlet pipe 22 can also facilitate the more smooth suction of the powder sample deposited at the bottom by the suction negative pressure, effectively improving the purging efficiency.

[0039] Optionally, it further includes a guide rail 3 and a tray 4. The tray 4 is slidably installed on the guide rail 3 through a moving motor. One end of the guide rail 3 is connected to the hatch 11, and the other end of the guide rail 3 is located between the blocking part 24 and one end of the intake pipe 21. The sample preparation conductive adhesive 25 is arranged on the tray 4. Exemplarily, in the embodiment of the present invention, when placing the sample preparation conductive adhesive 25 and taking and preparing samples, the movable tray 4 can be moved along the guide rail 3 to convey the sample preparation conductive adhesive 25 between the sample taking and placing position and the preparation position. The staff can open the hatch 11 to perform the operation without going deep into the sample preparation box body 1, reducing contact with the possible powder sample and further avoiding harm to the physical health of experimental personnel.

[0040] Unless otherwise defined, technical or scientific terms used herein shall have the ordinary meanings as understood by those of ordinary skill in the art to which this utility model pertains. The terms "first", "second" and similar terms used in the description and claims of this utility model patent application do not denote any order, quantity or importance, but are only used to distinguish different components. Similarly, terms such as "a" or "an" do not denote a quantity limitation, but rather indicate the presence of at least one. The terms "comprising" or "including" and similar terms mean that the elements or items appearing before "comprising" or "including" cover the elements or items listed after "comprising" or "including" and their equivalents, and do not exclude other elements or items. The terms "connected" or "coupled" and similar terms are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. The terms "upper", "lower", "left", "right" etc. are only used to indicate relative positional relationships, and when the absolute position of the object being described changes, the relative positional relationships may also change accordingly.

[0041] The above are only optional embodiments of this utility model and are not intended to limit this utility model. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of this utility model shall be included within the protection scope of this utility model.

Claims

1. A powder sample preparation device for a scanning electron microscope, characterized in that, Including: A sample preparation box body (1) and a sample preparation component (2), A hatch door (11) is provided on the sample preparation box body (1); The sample preparation component (2) includes an air inlet pipe (21), an air outlet pipe (22), a feed inlet (23), a blocking part (24) and a sample preparation conductive adhesive (25). The air inlet pipe (21) is arranged horizontally and one end thereof penetrates into the sample preparation box body (1), and the other end is used for connecting to an air source (a). The feed inlet (23) is arranged at the top of the sample preparation box body (1) and is connected to the air inlet pipe (21). The blocking part (24) is arranged in the sample preparation box body (1) and is arranged opposite to one end of the air inlet pipe (21). The sample preparation conductive adhesive (25) is installed at the bottom of the sample preparation box body (1) and is located between the blocking part (24) and one end of the air inlet pipe (21). The air outlet pipe (22) penetrates through another side wall of the sample preparation box body (1).

2. The powder sample preparation device for a scanning electron microscope according to claim 1, wherein, The blocking part (24) is an impact ball, and the blocking part (24) is hoisted on the top wall of the sample preparation box body (1).

3. The powder sample preparation device for a scanning electron microscope according to claim 1, characterized in that, A narrow pipe section (211) is arranged between one end of the air inlet pipe (21) and the inner side wall of the sample preparation box body (1). The diameter of the narrow pipe section (211) is smaller than the diameters of both ends of the air inlet pipe (21). The feed inlet (23) is connected to the narrow pipe section (211).

4. A powder sample preparation device for a scanning electron microscope according to claim 3, characterized in that, A screen mesh (231) is provided at the feed inlet (23).

5. A powder sample preparation device for a scanning electron microscope according to claim 3, characterized in that, It further includes a feed pipe (232) and an infrared heating device (233). The feed inlet (23) is connected to the narrow pipe section (211) through the feed pipe (232). The infrared heating device (233) is arranged around the feed inlet (23) and the feed pipe (232).

6. The powder sample preparation device for a scanning electron microscope according to claim 3, characterized in that, It further includes a vibration block (234), and the vibration block (234) is connected to the feed inlet (23).

7. A powder sample preparation device for a scanning electron microscope according to any one of claims 1 to 6, characterized in that, The sample preparation conductive adhesive (25) is in a plate shape and includes a sample preparation area (25a) and an edge area (25b) arranged around the sample preparation area (25a). A tape is pasted on the edge area (25b).

8. A powder sample preparation device for a scanning electron microscope according to any one of claims 1 to 6, characterized in that, The air source (a) is a nitrogen gas source (a).

9. A powder sample preparation device for a scanning electron microscope according to any one of claims 1 to 6, characterized in that, The height of one end of the air inlet pipe (21) is higher than the height of one end of the air outlet pipe (22) located in the sample preparation box body (1).

10. A powder sample preparation device for a scanning electron microscope according to any one of claims 1 to 6, characterized in that, It further includes a guide rail (3) and a tray (4). The tray (4) is slidably installed on the guide rail (3) through a moving motor. One end of the guide rail (3) is connected to the hatch door (11), and the other end of the guide rail (3) is located between the blocking part (24) and one end of the air inlet pipe (21). The sample preparation conductive adhesive (25) is arranged on the tray (4).

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