A scanning electron microscope sample protection device for air-sensitive samples and its use method

Abstract

The present invention discloses a scanning electron microscope sample injection protection device for air-sensitive samples and its use method. The device consists of a sleeve, a sleeve screw cap, a spring chamber, a compression spring, a sample chamber, a fork-shaped baffle, a fixed base and other parts. The sample chamber is sealed in the sleeve with the help of a resistance rubber plug that can achieve good airtightness. The sample chamber is provided with a sample chamber for loading the sample to be tested; the fork-shaped baffle is used to ensure that the sample chamber is in a static sealed state during the preparation stage. Before testing, the various components of the sleeve are assembled in a glove box, and then the fixed base and sleeve are fixed to the electron microscope sample stage. Before the electron microscope is evacuated, the fork-shaped baffle is quickly pulled out, and the sample chamber will slowly move toward the observation window on the sleeve under the drive of the spring, while remaining in a sealed state. When the electron microscope is in a high vacuum, the sample chamber moves into place and is fully exposed inside the electron microscope. This injection method can ensure that the sample is always kept away from air, thereby achieving non-destructive injection of air-sensitive samples in a simple and effective way.

Description

Technical Field

[0001] The present invention relates to the technical field of scanning electron microscopes, and in particular to a scanning electron microscope sample feeding protection device for air-sensitive samples and a use method thereof. Background Art

[0002] Scanning electron microscopy (SEM) is a widely used instrumental analytical method for observing the microscopic morphology of materials and determining the composition of micro-areas. The testing process generally includes three parts: sample preparation, sample transfer, and SEM analysis. Sample transfer refers to the process of transferring the sample to be tested into the SEM sample chamber. For conventional samples, this process has no effect on the sample. However, for air-sensitive samples, such as metal elements such as lithium and sodium that are extremely easily oxidized in air, or samples that are very deliquescent, such as calcium chloride, this step will inevitably expose the sample to air. Although the exposure time can be shortened to a few seconds, it will still cause irreversible damage to the sample and may even make it impossible to obtain valid test results. Summary of the Invention

[0003] In order to overcome the defects of the above-mentioned prior art, the technical problem to be solved by the present invention is to provide a simple and highly operable sample protection device to ensure that the sample will never come into contact with air during the transfer process to the scanning electron microscope, thereby eliminating the possibility of sample deterioration; the sample protection device does not require external force to drive, and does not require any modification to the electron microscope sample chamber. The use process is simple and reliable, and can be widely used in scanning electron microscopes of various manufacturers / models, with strong applicability.

[0004] In order to achieve the above-mentioned purpose of the invention, the present invention provides a scanning electron microscope sampling protection device for air-sensitive samples, wherein the sleeve is a cylindrical hollow cylinder with a sealed bottom end and a sleeve screw cap connected to the top end by a thread; a plurality of through-holes are provided on the sleeve screw cap to keep the spring chamber in the sleeve connected to the external atmosphere and maintain the air pressure balance on both sides of the sample chamber sealed in the sleeve when vacuuming. A hollow area with a rectangular projection is provided on the side wall near the bottom end of the sleeve, which serves as an observation window; a sample chamber is sealed in the sleeve, and resistance plugs are respectively adhered to the circular cross-sections at both ends of the sample chamber, and the outer edge of the resistance plug is surrounded by several circles of annular plug protrusions; a rectangular cavity is provided inside the sample chamber, which serves as a sample chamber, and the opening direction of the sample chamber is perpendicular to the long axis of the sleeve, and a sample stage is fixedly placed therein; a plurality of baffle holes are provided at the position where the observation window contacts the sample chamber, and a fork-shaped baffle is clamped on the baffle hole; a spring chamber is provided between the sample chamber and the sleeve screw cover, and a compression spring is provided in the spring chamber; two protruding slide rail grooves are provided on the upper surface of the fixed base, which are used for sliding and fixing two sheet-like legs extending obliquely downward and provided below the outer side wall of the sleeve.

[0005] The sleeve has an outer diameter of 25-50mm, a length of 50-80mm, a side wall thickness of 2-3mm, and a bottom thickness of 1-2mm. It is made of aluminum or copper. The sleeve is provided with an external sleeve thread on the outer wall at the top opening. The thread width of the external sleeve thread is 2-4mm, and is used to screw together with the sleeve screw cap. The sleeve screw cap is a circular metal cover made of aluminum or copper. The inner edge of the annular protrusion of the sleeve screw cap has a diameter consistent with the outer diameter of the sleeve and is provided with an internal screw cap thread with a thread width of 2-4mm, which can be screwed together and sealed with the external sleeve thread provided on the outer wall of the sleeve. The annular protrusion of the sleeve screw cap is 2mm thick, the protrusion height is 3-5mm, and the thickness of the circular cap top is 1-2mm.

[0006] The main body of the sample capsule is a metal cylinder with a hollowed-out middle and a diameter consistent with the inner diameter of the sleeve, a length of 12-20 mm, and a material of aluminum or copper; the hollowing direction of the sample capsule is perpendicular to the longitudinal axis of the cylinder of the sleeve, and the hollow part with a rectangular shape after hollowing is the sample chamber, the width of the sample chamber is less than 90% of the diameter of the sample capsule, the length is 10-18 mm, the depth does not exceed 75% of the diameter of the sample capsule, and the remaining thickness at both ends of the capsule body is 1-1.5 mm; the size of the observation window is comparable to the size of the sample chamber in the sample capsule.

[0007] The resistance rubber plug is a thin, circular rubber sheet 2-4 mm thick, with a diameter equal to the inner diameter of the sleeve and the diameter of the sample chamber. The thickness of the rubber plug near the observation window is greater than that at the end in contact with the compression spring. The annular protrusion on the rubber plug is 0.5 mm high and 1 mm wide. The resistance rubber plug is used to ensure good airtightness between the sample chamber and the sleeve, increase the friction coefficient of the sample chamber moving within the sleeve, and provide sufficient protection for the sample inside the chamber.

[0008] A sample stage socket is provided at the center of the bottom of the sample chamber. The sample stage socket is a round hole with a depth of 2-4 mm and a diameter of 2-3 mm, which is used to insert and fix the sample stage. The sample stage includes a surface-type sample stage, a cross-sectional sample stage and a hybrid sample stage, and is made of aluminum or copper. The base of the sample stage is a rectangular parallelepiped, and the length and width are exactly the same as the size of the sample chamber. The height varies according to the sample, ensuring that the sample fixed thereon is 1-5 mm away from the observation window. Nail legs are provided under the base of the sample stage, and the diameter and length of the nail legs match the sample stage socket, so that the sample stage can be fully fitted and firmly placed in the sample chamber.

[0009] The spring chamber is a cavity within the sleeve that houses the compression spring, located between the sample chamber and the sleeve's screw cap. The compression spring's outer diameter matches the sleeve's inner diameter, and its length ranges from 20 to 60 mm. The spring wire has a diameter of less than 1.6 mm. When compressed, one end of the compression spring presses against the sample chamber's resistance plug, while the other end presses against the tightened sleeve's screw cap.

[0010] The fork-shaped baffle is located between the observation window and the sample chamber. It is a baffle with several long, strip-shaped protruding ends, with a thickness of 2-3 mm and a width not exceeding the diameter of the sleeve. It is made of titanium or aluminum. The long, strip-shaped protruding ends of the fork-shaped baffle extend in the same direction as the direction in which the baffle is inserted or removed, and the upper portion is fixed to a horizontal, straight bar. The fork-shaped baffle is inserted along the baffle insertion hole position preset on the side wall of the sleeve. When fully inserted, its long, strip-shaped protruding ends fit neatly into the insertion hole at the bottom of the inner wall of the sleeve. A disc-shaped fork-shaped baffle handle is provided on the bar above the fork-shaped baffle to facilitate the insertion and removal of the fork-shaped baffle. The fork-shaped baffle is inserted perpendicular to the long axis of the sleeve and close to one side of the sample chamber to prevent the sample chamber from moving under the action of spring pressure. It is manually pulled out before the electron microscope sample chamber is evacuated.

[0011] The fixed base is a rectangular metal sheet made of aluminum or copper. It is 40-70 mm long, 30-60 mm wide, and 2-3 mm thick. Two upward-extending slide rail slots are provided on its upper surface for receiving two sheet-like legs extending obliquely downward from the bottom of the sleeve. The slide rails of the slide rail slots are 40-70 mm long, with a slot spacing of 30-60 mm. The sheet-like legs are long and 30-60 mm long, with a leg thickness of 1-2 mm and a leg spacing of 30-60 mm. The width of the portion of the sheet-like legs that fits within the slide rail slots is 2-3 mm. The shape of the slide rail slots matches the sheet-like legs of the sleeve, ensuring that the sleeve is firmly fixed on the electron microscope sample stage. After fixation, the bottom of the sleeve should be in close contact with the surface of the fixed base.

[0012] A method for using the above-mentioned scanning electron microscope sample protection device for air-sensitive samples comprises the following steps:

[0013] a. Assembly of the sampling protection device: Under the protection of the glove box atmosphere, secure the sample to be tested on the sample stage of the protection device. Then, insert the nail legs below the sample stage base into the sample stage sockets at the bottom of the sample chamber. The sample stage is firmly placed in the sample chamber located within the sample chamber. Slowly push the sample chamber from one end of the sleeve opening until it is close to the observation window. Insert the fork-shaped baffle into the baffle socket provided on the sleeve to block the sample chamber from the observation window. Install the compression spring from one side of the sleeve opening and tighten the sleeve cap so that the compression spring is compressed and sealed in the spring chamber. This completes the assembly of the sampling protection device.

[0014] b. Securing the Sleeve to the SEM Stage: Remove the sample protection device assembled in step a from the glove box and prepare to transfer it to the SEM. Before transfer, seal the device in a thick, argon-filled ziplock bag to further protect the sample. Use conductive tape to secure the mounting base to the SEM stage. Push the tab-shaped feet at the bottom of the sleeve into the slide rail slots on the base to secure the sleeve to the SEM stage.

[0015] c. The sample chamber moves within the sleeve toward the observation window: Quickly pull out the fork-shaped baffle, close the electron microscope sample chamber door, and quickly evacuate the chamber. Without the fork-shaped baffle, the sample chamber will slowly move toward the observation window driven by the compression spring. By adjusting the resistance plug and the relevant parameters of the compression spring, the movement speed is controlled so that the sample chamber communicates with the electron microscope sample chamber atmosphere through the observation window, and a high vacuum state is achieved within the electron microscope sample chamber.

[0016] d. Perform electron microscopy observation: The sample chamber is finally moved to the sealed side of the sleeve, and the sample inside is completely exposed under the observation window, and then normal electron microscopy testing can be carried out.

[0017] The sampling protection device of the present invention is composed of main parts such as a sleeve, a sleeve screw cap, a spring chamber, a compression spring, a sample cabin, a sample chamber, a resistance rubber plug, a fork-shaped baffle, an observation window and a fixed base. The sample cabin and the spring chamber are sealed in the sleeve, and the sample cabin with a sample chamber designed inside is located in front of the spring chamber. By tightening the sleeve screw cap to the open end of the sleeve, that is, one end of the spring chamber, the spring placed in the spring chamber is in a compressed state. At this time, one end of the compression spring is against one side of the sample cabin, providing a driving force for the movement of the sample cabin in the sleeve toward the observation window. During the assembly stage of the sampling protection device, the sample cabin is sealed in the sleeve in the glove box, and good airtightness is achieved in the sample cabin with the help of the resistance rubber plug to ensure that the sample is always under argon protection. By arranging a fork-shaped baffle at one end of the sample cabin close to the observation window, the sample cabin is prevented from moving toward the observation window before being transferred to the electron microscope.

[0018] After the entire device is placed in the scanning electron microscope sample chamber and fixed, pull out the fork-shaped baffle, quickly close the electron microscope sample chamber door and start vacuuming. During this process, the sample chamber in a closed state will slowly move toward the observation window under the self-drive of the spring; by adjusting the movement speed of the sample chamber, the sample chamber is moved to the point where the observation window and the electron microscope sample chamber atmosphere are connected. The electron microscope sample chamber is already in a high vacuum state, thereby achieving electron microscope sampling without air contact throughout the process. When the sample chamber finally reaches the top of the sleeve and is completely exposed under the observation window, normal electron microscope observation can be carried out. In order to ensure that the sleeve is stably fixed on the electron microscope sample stage during the entire process, the device is designed with a fixed base that can be fixed on the electron microscope sample stage. The sleeve and the fixed base are connected and fixed by a slide rail.

[0019] Compared with the existing technology, the present invention has the following beneficial effects: the compression spring autonomously drives the sample chamber to move within the sleeve, effectively and controllably achieving non-destructive sampling of air-sensitive samples in a scanning electron microscope, ensuring that the sample is never exposed to air during transfer and vacuuming of the electron microscope sample chamber. The resistance plug design on both sides of the sample chamber not only ensures the airtightness of the sample chamber within the chamber, but also increases the movement resistance, extending the sample protection time. The protection time can be controlled by adjusting the plug resistance and the compression spring parameters. The clever use of the driving force of the compression spring eliminates the need for external force and modification of the electron microscope sample chamber, making it simple and convenient to use, suitable for electron microscopes of various brands and models, and highly practical. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 A perspective view of the internal structure of the scanning electron microscope sample feeding protection device of the present invention;

[0021] Figure 2 A cross-sectional view of the scanning electron microscope sample feeding protection device of the present invention;

[0022] Figure 3 This is an appearance diagram of the scanning electron microscope sample feeding protection device of the present invention;

[0023] Figure 4 This is the appearance of the sleeve;

[0024] Figure 5 A perspective view of the sleeve capping;

[0025] Figure 6 is a side view of the sample chamber;

[0026] Figure 7 This is a cross-sectional view of the sample chamber;

[0027] Figure 8 is a schematic diagram of the sample stage;

[0028] Figure 9 is a cross-sectional view of a forked baffle;

[0029] Figure 10 It is a side view of the fixed base;

[0030] In the figure: 1-sleeve; 2-sleeve screw cap; 3-observation window; 4-baffle socket; 5-fork-shaped baffle; 501-fork-shaped baffle handle; 6-sleeve external thread; 7-flaky support foot; 8-screw cap internal thread; 9-screw cap circular hole; 10-sample chamber; 11-resistance rubber plug; 12-ring-shaped protrusion of rubber plug; 13-sample chamber; 14-sample stage socket; 15-sample stage; 1501-surface type sample stage; 1502-section type sample stage; 1503-hybrid type sample stage; 16-spring chamber; 17-compression spring; 18-fixed base; 19-slide rail slot. DETAILED DESCRIPTION

[0031] The present invention will be further described below with reference to specific examples, but the present invention is not limited thereto in any way.

[0032] The present invention provides the following Figure 1-10 The present invention shows a scanning electron microscope sampling protection device for air-sensitive samples, wherein the sleeve 1 is a cylindrical hollow cylinder with a sealed bottom end and a sleeve screw cap 2 connected to the top end by a thread. The sleeve screw cap 2 is provided with a plurality of through screw cap holes 9; a rectangular hollow portion is provided on the side wall of the sleeve 1 near the bottom end, which serves as an observation window 3; a sample chamber 10 is sealed in the sleeve 1, and resistance plugs 11 are adhered to both ends of the sample chamber 10, and the outer edge of the resistance plug 11 is surrounded by a plurality of ring-shaped plug protrusions 12; a rectangular parallelepiped is provided inside the sample chamber 10. The cavity is a sample chamber 13, the opening direction of the sample chamber 13 is perpendicular to the long axis of the sleeve 1, and a sample stage 15 is fixedly placed inside the sample chamber 13; a plurality of baffle holes 4 are provided at the position where the observation window 3 contacts the sample chamber 10, and a fork-shaped baffle 5 is clamped on the baffle hole 4; a spring chamber 16 is provided between the sample chamber 10 and the sleeve screw cover 2, and a compression spring 17 is provided in the spring chamber 16; the upper surface of the fixed base 18 is provided with two protruding slide rail grooves 19, which are used for sliding and fixing the two sheet-like legs 7 extending obliquely downward and provided at the bottom of the outer side wall of the sleeve 1.

[0033] A method for using the above-mentioned scanning electron microscope sample protection device for air-sensitive samples comprises the following steps:

[0034] a. Assembly of the sampling protection device: Under the protection of the glove box atmosphere, fix the sample to be tested on the sample stage 15 of the protection device, then insert the nail legs under the base of the sample stage 15 into the sample stage sockets 14 at the bottom of the sample chamber 13, and firmly place the sample stage 15 in the sample chamber 13 located in the sample capsule 10; slowly push the sample chamber 10 from the open end of the sleeve 1 until it is close to the observation window 3; insert the fork-shaped baffle 5 into the baffle socket 4 provided on the sleeve 1 to block the sample chamber 10 from the outside of the observation window 3; install the compression spring 17 from the open side of the sleeve 1 and tighten the sleeve screw cover 2 so that the compression spring 17 is in a compressed state and sealed in the spring chamber 16, thereby completing the assembly of the sampling protection device;

[0035] b. Securing the Sleeve to the Electron Microscope Stage: Remove the sample protection device assembled in step a from the glove box and prepare to transfer it to the SEM. Before transfer, seal the device in a thick, argon-filled ziplock bag to further protect the sample. Use conductive tape to secure the mounting base 18 to the electron microscope stage. Push the tab-shaped support legs 7 at the bottom of the sleeve 1 into the slide rail slots 19 on the base to secure the sleeve 1 to the electron microscope stage.

[0036] c. The sample chamber moves within the sleeve toward the observation window: Quickly pull out the forked baffle 5, close the electron microscope sample chamber door, and quickly evacuate the chamber. Without the forked baffle 5, the sample chamber 10 will slowly move toward the observation window 3 under the self-drive of the compression spring 17. By adjusting the resistance plug 11 and the relevant parameters of the compression spring 17, the movement speed is controlled so that the sample chamber 13 communicates with the electron microscope sample chamber atmosphere through the observation window 3, and a high vacuum state is achieved within the electron microscope sample chamber.

[0037] d. Conduct electron microscopy observation: The sample chamber 10 will eventually move to the sealed side of the sleeve 1, and the sample inside will be completely exposed below the observation window 3, and then normal electron microscopy testing can be carried out.

[0038] The preferred embodiments of the present invention are described in detail below with reference to the accompanying drawings. However, the present invention is not limited to the specific details in the following embodiments. Within the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, and these simple modifications all fall within the scope of protection of the present invention.

[0039] Example 1

[0040] The sleeve 1 has an outer diameter of 30mm, a length of 50mm, and a sidewall thickness of 2mm. Made of copper, the bottom seal is 2mm thick. The projected dimensions of the observation window 3 are 20mm long and 14mm wide. Four sets of upper and lower baffle holes 4 are designed on the sidewall of the sleeve 1, where the observation window 3 and its projected portion meet the sample chamber 10. These holes are square, 2mm in length, and are positioned to align with the long, protruding ends of the forked baffles 5. The outer tabs 7 of the sleeve 1 are 40mm long and 1mm thick, with a spacing of 36mm. The width of the portion of the sleeve 1 that fits within the slide rail slot 19 on the base is 2mm. Once secured to the base, the bottom of the sleeve 1 should rest firmly against the surface of the fixed base 18. The width of the sleeve 1's external threads is 3mm.

[0041] The material of the sleeve screw cap 2 is metal copper, the diameter of the inner edge of its annular raised part is 30mm, and a thread is designed on one side of the inner edge with a width of 3mm, which can be tightened and sealed with the open end of the sleeve 1 with an external thread; the annular raised part of the sleeve screw cap 2 is 2mm thick, the raised height is 4mm, and the thickness of the circular cover top is 1mm; the sleeve screw cap 2 is designed with four screw cap circular holes 9 on the top surface of the cover, with a hole diameter of 2mm.

[0042] The sample chamber 10 is 12 mm long and 26 mm in diameter. It is made of metal aluminum. A hollow part in the shape of a rectangular parallelepiped is hollowed out perpendicular to the longitudinal axis of the sample chamber 10. The width is 10 mm, the length is 20 mm, and the depth is 12 mm. The remaining thickness at both ends of the chamber is 1 mm.

[0043] The resistance rubber plug 11 has a diameter of 26 mm. The side in contact with the compression spring 17 is 2 mm thick, and the other side is 3 mm thick. It is adhered flatly to the circular cross-sections at both ends of the sample chamber 10 with strong glue. The 3 mm thick plug has two annular protrusions 12 surrounding its outer edge, while the 2 mm thick plug has a single annular protrusion, 0.5 mm high and 1 mm wide.

[0044] Sample chamber 13 is the hollowed-out portion of sample capsule 10. A circular hole, 3mm deep and 2mm in diameter, is designed at the center of its bottom to accommodate the fixed sample stage 15. Sample stage 15 is available in surface, cross-section, or hybrid types. Made of aluminum, it has a rectangular base measuring 20mm in length, 10mm in width, and 12mm in height. It has legs measuring 2mm in diameter and 3mm in length.

[0045] The spring chamber 16 is a cavity located in the sleeve 1 and has a length of 14 mm to accommodate a compression spring 17. The compression spring 17 is a spring with an outer diameter of 26 mm, made of 304 stainless steel, a length of 30 mm, and a spring wire diameter of 1.2 mm.

[0046] The fork-shaped baffle 5 is made of metal aluminum with a thickness of 2mm. The upper straight horizontal bar is 20mm long and is designed with four equally spaced long strip-shaped protruding ends. The cross-section of each protruding end is square with a side length of 2mm and a length of 13mm. The fork-shaped baffle handle 501 on the baffle straight horizontal bar is semicircular with a diameter of 10mm.

[0047] The material of the fixed base 18 is copper, 50mm long, 42mm wide and 2mm thick. The slide rail slot 19 on its upper surface is 40mm long, 36mm apart, 1mm thick and 2mm wide.

[0048] Inside the glove box, a cross-sectional sample of a lithium-ion battery composite electrode is prepared and attached to a dedicated cross-sectional sample stage 1502. Sample stage 1502 is securely positioned within sample chamber 10, which is then slowly pushed from the open side of sleeve 1 until it is near observation window 3. A forked baffle 5 is inserted into baffle receptacle 4 on sleeve 1 to secure the position of sample chamber 10. A compression spring 17 is inserted through the open end of sleeve 1, and sleeve cap 2 is pressed against the spring protruding from the sleeve. Slowly apply force until the cap 2 is fully tightened onto sleeve 1. The assembled sleeve 1 is sealed in a thick, ziplock bag and removed from the glove box.

[0049] Observation was carried out using a Japanese electronic scanning electron microscope JSM-7900F. First, the fixed base 18 was fixed to the sample stand of the electron microscope with conductive tape, and then the sleeve 1 was fixed to the base through the slide rail slot 19; the vacuum of the scanning electron microscope sample exchange chamber was broken, and the electron microscope sample stand with the sleeve 1 and the fixed base 18 fixed was installed. The fork-shaped baffle 5 was pulled out, the exchange chamber door was quickly closed and vacuum was started. The vacuuming time was expected to be about 1 minute, and the sample chamber moving time was also set to about 1 minute through preliminary adjustment.

[0050] After the sample exchange chamber is vacuumed and the sample chamber in the sleeve is moved to the bottom of the observation window, the sample stand is pushed into the electron microscope sample chamber, and the Oxford Extreme windowless energy spectrometer is used to perform component surface distribution analysis of the lithium element on the cross-section sample.

[0051] Example 2

[0052] The sleeve 1 has an outer diameter of 40mm, a length of 60mm, and a sidewall thickness of 2mm. Made of aluminum, the bottom seal is 2mm thick. The projected dimensions of the observation window 3 are 20mm long and 18mm wide. Five upper and lower sets of baffle holes 4 are designed on the sidewall of the sleeve 1, where the observation window 3 and its projected portion meet the sample chamber. These holes are rectangular, 3mm long and 2mm wide, and their positions align with the long, protruding ends of the forked baffles 5. The long, flat legs 7 on the outside of the sleeve 1 are 40mm long and 2mm thick, with a spacing of 48mm. The width of the portion of the legs that engages the slide rail slot 19 on the base is 2mm. Once secured to the base, the bottom of the sleeve 1 should rest closely on the surface of the fixed base 18. The width of the sleeve 1's external threads is 3mm.

[0053] The material of the sleeve screw cap 2 is metal aluminum, the diameter of the inner edge of its annular raised part is 40mm, and a thread is designed on one side of the inner edge with a width of 3mm, which can be tightened and sealed with the open end of the sleeve 1 with an external thread; the annular raised part of the sleeve screw cap 2 is 2mm thick, the raised height is 4mm, and the thickness of the circular cover top is 2mm; the sleeve screw cap 2 is designed with four screw cap circular holes 9 on the top surface of the cover, with a hole diameter of 3mm.

[0054] The sample chamber 10 is 15 mm long and 36 mm in diameter. It is made of metal aluminum. A hollow part in the shape of a rectangular parallelepiped is hollowed out perpendicular to the longitudinal axis of the sample chamber 10. The width is 13 mm, the length is 30 mm, and the depth is 15 mm. The remaining thickness at both ends of the chamber is 1 mm.

[0055] The resistance rubber plug 11 has a diameter of 36 mm. The side in contact with the compression spring 17 is 2 mm thick, and the other side is 4 mm thick. It is adhered flatly to the circular cross-sections at both ends of the sample chamber 10 with strong glue. The 4 mm thick plug has three annular protrusions 12 surrounding its outer edge, while the 2 mm thick plug has a single annular protrusion, 0.5 mm high and 1 mm wide.

[0056] Sample chamber 13 is the hollowed-out portion of sample capsule 10. A circular hole, 4mm deep and 3mm in diameter, is designed at the center of its bottom to accommodate the fixed sample stage 15. Sample stage 15 is available in surface, cross-section, or hybrid types. Made of aluminum, it has a rectangular base measuring 30mm in length, 13mm in width, and 15mm in height. It has legs measuring 3mm in diameter and 4mm in length.

[0057] Spring chamber 16 is a 15mm-long cavity within sleeve 1 that houses compression spring 17. Compression spring 17 is a 32mm-long spring with an outer diameter of 36mm, made of 304 stainless steel, and a 1.4mm-diameter spring wire. To accommodate the electron microscope's requirement that magnetic samples be excluded, the spring is demagnetized.

[0058] The fork-shaped baffle 5 is made of titanium with a thickness of 2 mm. The upper straight bar is 30 mm long and has five equally spaced long strip-shaped protruding ends. The cross-section of each protruding end is a rectangle with a length of 3 mm, a width of 2 mm, and a length of 28 mm. The fork-shaped baffle handle 501 on the baffle straight bar is semicircular with a diameter of 15 mm.

[0059] The fixed base 18 is made of aluminum and has a length of 60 mm, a width of 55 mm and a thickness of 3 mm. The slide rail slots 19 on the upper surface thereof are 40 mm long, 48 mm apart, 2 mm thick and 2 mm wide.

[0060] Inside the glove box, prepare a fresh surface for the magnesium-aluminum alloy sample and adhere it to a dedicated hybrid sample stage 1503. Securely secure sample stage 1503 within sample chamber 10, then slowly push sample chamber 10 from the open side of sleeve 1 until it is near observation window 3. Insert fork-shaped baffle 5 into baffle receptacle 4 on sleeve 1 to secure sample chamber 10. Install compression spring 17 through the open end of sleeve 1. Press sleeve cap 2 against the spring's protruding end and slowly apply force until cap 2 is fully tightened onto sleeve 1. Seal the assembled sleeve 1 in a thick, ziplock bag and remove from the glove box.

[0061] Observation was carried out using a JSM-7610F scanning electron microscope from Japan. First, the fixed base 18 was fixed to the sample stand of the electron microscope with conductive tape, and then the sleeve 1 was fixed to the fixed base 18 through the slide rail slot 19. The vacuum of the scanning electron microscope sample exchange chamber was broken, and the sample stand with the sleeve 1 and the fixed base 18 fixed was installed. The fork-shaped baffle 5 was pulled out, the exchange chamber door was quickly closed, and vacuuming was started. The estimated vacuuming time was about 1 minute, and the sample chamber moving time was also set to about 1 minute through preliminary adjustment.

[0062] After the sample exchange chamber is vacuumed and the sample chamber in the sleeve is moved to the bottom of the observation window, the sample stand is pushed into the electron microscope sample chamber, the electron beam high voltage is turned on for morphology analysis, and the oxygen content in the sample is analyzed using the Oxford X-MAX energy spectrometer.

[0063] Example 3

[0064] Sleeve 1 has an outer diameter of 50mm, a length of 80mm, and a sidewall thickness of 3mm. Made of copper, the bottom seal is 2mm thick. The projected dimensions of the observation window 3 are 30mm long and 22.5mm wide. Six upper and lower sets of baffle holes 4 are designed on the sidewall of sleeve 1, where the observation window 3 and its projected portion contact the sample chamber. The projected baffle holes 4 are squares with sides of 3mm, and their positions match the long, extended ends of the forked baffles 5. The sheet-like legs 7 on the outside of sleeve 1 are 60mm long and 2mm thick, with a spacing of 60mm. The width of the portion of the legs that fits within the slide rail slots 19 on the fixed base 18 is 3mm. Once secured to the fixed base 18, the bottom of the sleeve 1 should rest closely against the surface of the fixed base 18. The width of the sleeve 1's external threads is 4mm.

[0065] The material of the sleeve screw cap 2 is metal copper, the diameter of the inner edge of its annular raised part is 50mm, and a thread is designed on one side of the inner edge with a width of 4mm, which can be tightened and sealed with the open end of the sleeve 1 with an external thread; the annular raised part of the sleeve screw cap 2 is 2mm thick, the raised height is 5mm, and the thickness of the circular cover top is 2mm; the sleeve screw cap 2 is designed with four screw cap circular holes 9 on the top surface of the cover, with a hole diameter of 3mm.

[0066] The sample chamber 10 is 20 mm long and 44 mm in diameter. It is made of metallic copper. A hollow part in the shape of a rectangular parallelepiped is hollowed out perpendicular to the longitudinal axis of the sample chamber 10. The width is 17 mm, the length is 30 mm, and the depth is 20 mm. The remaining thickness at both ends of the chamber is 1.5 mm.

[0067] The resistance rubber plug 11 has a diameter of 44 mm. The side in contact with the compression spring 17 is 3 mm thick, and the other side is 4 mm thick. It is adhered flatly to the circular cross-sections at both ends of the sample chamber 10 with strong glue. The 4 mm thick plug has three rings of annular protrusions 12 around its outer edge, while the 3 mm thick plug has two rings of protrusions, each 0.5 mm high and 1 mm wide.

[0068] Sample chamber 13 is the hollowed-out portion of sample capsule 10. A circular hole, 4mm deep and 3mm in diameter, is designed at the center of its bottom to accommodate the fixed sample stage 15. Sample stage 15 is available in surface, cross-section, or hybrid types. Made of copper, it has a rectangular base measuring 30mm in length, 17mm in width, and 20mm in height. It has legs measuring 3mm in diameter and 4mm in length.

[0069] The spring chamber 16 is a cavity in the sleeve 1 that contains a compression spring and has a length of 23.5 mm. The compression spring 17 is a spring with an outer diameter of 44 mm, made of 304 stainless steel, a length of 48 mm, and a spring wire diameter of 1.4 mm.

[0070] The fork-shaped baffle 5 is made of titanium with a thickness of 3mm. The upper straight horizontal bar is 30mm long and is designed with six equally spaced long strip-shaped protruding ends. The cross-section of each protruding end is square with a side length of 3mm and a length of 35mm. The fork-shaped baffle handle 501 on the baffle straight horizontal bar is semicircular with a diameter of 15mm.

[0071] The fixed base 18 is made of copper and has a length of 70 mm, a width of 70 mm and a thickness of 3 mm. The slide rail slots 19 on the upper surface thereof are 70 mm long, 60 mm apart, 2 mm thick and 3 mm wide.

[0072] Inside the glove box, prepare a sample containing highly hygroscopic calcium chloride particles on a dedicated surface sample stage 1501. Securely secure sample stage 1501 within sample chamber 10, then slowly push sample chamber 10 from the open side of sleeve 1 until it is near observation window 3. Insert fork-shaped baffle 5 into baffle receptacle 4 on the sleeve to secure sample chamber 10. Install compression spring 17 through the open end of sleeve 1, press sleeve cap 2 against the spring protruding from the sleeve, and slowly apply force until cap 2 is fully tightened onto sleeve 1. Seal the assembled sleeve 1 in a thick, ziplock bag and remove from the glove box.

[0073] Observation was performed using a Hitachi scanning electron microscope SU5000. First, the fixed base 18 was fixed to the sample stand of the electron microscope with conductive tape, and then the sleeve 1 was fixed to the base through the slide rail slot 19. The fork-shaped baffle 5 was pulled out, the sample chamber door was quickly closed, and vacuuming was started. The movement of the sample injection device and the sample chamber 10 was observed in real time through the camera in the sample chamber. The vacuuming time was estimated to be about 3 minutes, and the sample chamber movement time was also set to about 3 minutes through preliminary adjustment.

[0074] After the electron microscope sample chamber is vacuumed and the sample chamber in the sleeve is moved to the bottom of the observation window, the electron beam high voltage is turned on to analyze the sample surface morphology. After avoiding the influence of moisture absorption, the sample can show its original morphology.

[0075] Anyone skilled in the art will be able to utilize the above-disclosed technical content to make many possible changes and modifications to the technical solution of the present invention, or to modify it into equivalent embodiments with equivalent changes, without departing from the scope of the technical solution of the present invention. Therefore, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention that do not depart from the content of the technical solution of the present invention shall still fall within the scope of protection of the technical solution of the present invention.

Claims

1. A method for using a scanning electron microscope sample protection device for air-sensitive samples, characterized in that: The method comprises the following steps: a. Assembly of the sampling protection device: fix the sample to be tested on the sample stage (15) of the scanning electron microscope sampling protection device under the protection of the glove box atmosphere, and then insert the nail legs under the base of the sample stage (15) into the sample stage socket (14) at the bottom of the sample chamber (13), and the sample stage (15) is firmly placed in the sample chamber (13) located in the sample chamber (10); slowly push the sample chamber (10) from one end of the opening of the sleeve (1) to the vicinity of the observation window (3); insert the fork-shaped baffle (5) into the baffle socket (4) provided on the sleeve (1) to block the sample chamber (10) from the outside of the observation window (3); install the compression spring (17) from the side of the opening of the sleeve (1) and tighten the sleeve screw cover (2) so that the compression spring (17) is in a compressed state and is sealed in the spring chamber (16), thereby completing the assembly of the sampling protection device; b. Fixing the sleeve on the electron microscope sample stage: Take out the sample protection device assembled in step a from the glove box and prepare to transfer it to the scanning electron microscope. Before the transfer, the device can be sealed in a thick self-sealing bag filled with argon to further protect the sample; Use conductive tape to firmly fix the fixed base (18) on the scanning electron microscope sample stage, push the sheet-like support foot (7) at the bottom of the sleeve (1) into the slide rail slot (19) on the base to complete the fixing of the sleeve (1) on the scanning electron microscope sample stage; c. The sample chamber moves toward the observation window in the sleeve: quickly pull out the fork-shaped baffle (5), close the door of the scanning electron microscope sample chamber and quickly evacuate the sample chamber. At this time, the sample chamber (10) without the fork-shaped baffle (5) will slowly move toward the observation window (3) under the self-drive of the compression spring (17). By adjusting the relevant parameters of the resistance plug (11) and the compression spring (17), the moving speed is controlled so that when the sample chamber (13) is connected to the atmosphere of the electron microscope sample chamber through the observation window (3), the electron microscope sample chamber has reached a high vacuum state; d. Conduct electron microscope observation: The sample chamber (10) is finally moved to the sealed side of the sleeve (1), and the sample to be tested inside is completely exposed below the observation window (3), and then normal electron microscope testing can be carried out.

2. The method of use according to claim 1, characterized in that: The scanning electron microscope sample protection device for air-sensitive samples comprises a sleeve (1) and a fixed base (18); the sleeve (1) is a cylindrical hollow cylinder with a sealed bottom end and a sleeve screw cap (2) connected to the top end by a thread, and the sleeve screw cap (2) is provided with a plurality of through screw cap holes (9); a hollow portion projected as a rectangle is provided on the side wall of the sleeve (1) near the bottom end, which serves as an observation window (3); a sample chamber (10) is sealed in the sleeve (1), and resistance rubber plugs (11) are respectively adhered to the circular cross-sections at both ends of the sample chamber (10), and the outer edge of the resistance rubber plug (11) is surrounded by a plurality of ring-shaped rubber plug protrusions (12); a long The cube-shaped cavity is a sample chamber (13), the opening direction of the sample chamber (13) is perpendicular to the long axis of the sleeve (1), and a sample stage (15) is fixedly placed therein; a plurality of baffle holes (4) are provided at the side wall of the sleeve (1) where the observation window (3) contacts the sample chamber (10), and a fork-shaped baffle (5) is clamped on the baffle hole (4); a spring chamber (16) is provided between the sample chamber (10) and the sleeve screw cover (2), and a compression spring (17) is placed in the spring chamber (16); the upper surface of the fixed base (18) is provided with two protruding slide rail grooves (19), which are used for sliding and fixing two sheet-like legs (7) extending obliquely downward and provided below the outer side wall of the sleeve (1).

3. The method of use according to claim 2, wherein: The sleeve (1) has an outer diameter of 25-50 mm, a length of 50-80 mm, a side wall thickness of 2-3 mm, a bottom thickness of 1-2 mm, and is made of aluminum or copper. The sleeve (1) is provided with a sleeve external thread (6) on the outer wall at the top opening, and the thread width of the sleeve external thread (6) is 2-4 mm, which is used for screwing together with the sleeve screw cap (2).

4. The method of use according to claim 3, wherein: The sleeve screw cap (2) is a circular metal cover made of aluminum or copper; the diameter of the inner edge of the annular protruding portion of the sleeve screw cap (2) is consistent with the outer diameter of the sleeve (1), and is provided with an inner screw cap thread (8) with a thread width of 2-4 mm, which can be screwed and sealed with the outer sleeve thread (6) provided on the outer wall of the sleeve (1); the thickness of the annular protruding portion of the sleeve screw cap (2) is 2 mm, the protrusion height is 3-5 mm, and the thickness of the circular cover top is 1-2 mm.

5. The method of use according to claim 4, wherein: The main body of the sample capsule (10) is a metal cylinder with a hollowed-out middle and a diameter consistent with the inner diameter of the sleeve, a length of 12-20 mm, and a material of aluminum or copper; the hollowing direction of the sample capsule (10) is perpendicular to the longitudinal axis of the cylinder of the sleeve (1), and the hollow part of the hollowed-out rectangular parallelepiped is the sample chamber (13), the width of the sample chamber (13) is less than 90% of the diameter of the sample capsule (10), the length is 10-18 mm, and the depth does not exceed 75% of the diameter of the sample capsule (10); the remaining thickness of the sample capsule (10) at both ends is 1-1.5 mm; the size of the observation window (3) is comparable to the size of the sample chamber (13) in the sample capsule (10).

6. The method of use according to claim 5, wherein: The resistance rubber plug (11) is a thin, circular rubber sheet with a thickness of 2-4 mm and a diameter equal to the inner diameter of the sleeve (1) and the diameter of the sample chamber (10), wherein the thickness of the rubber plug near the observation window (3) is greater than the thickness of the rubber plug at the end in contact with the compression spring (17); the protrusion height of the annular protrusion (12) of the rubber plug is 0.5 mm and the width is 1 mm.

7. The method of use according to claim 6, wherein: A sample stage socket (14) is provided at the center of the bottom of the sample chamber (13). The sample stage socket (14) is a round hole with a depth of 2-4 mm and a diameter of 2-3 mm, which is used to insert and fix the sample stage (15); the sample stage (15) includes a surface-type sample stage (1501), a cross-sectional sample stage (1502) and a mixed-type sample stage (1503), and is made of one of aluminum and copper. The base of the sample stage (15) is a rectangular parallelepiped, and its length and length are exactly the same as those of the sample chamber (13). The height varies depending on the sample, ensuring that the sample fixed thereon is 1-5 mm away from the observation window (3); nail legs are provided under the base of the sample stage (15), and the diameter and length of the nail legs match those of the sample stage socket (14).

8. The method of use according to claim 7, wherein: The outer diameter of the compression spring (17) is consistent with the inner diameter of the sleeve (1), the length is 20-60 mm, and the diameter of the spring steel wire is less than 1.6 mm.

9. The method of use according to claim 8, wherein: The fork-shaped baffle (5) is located between the observation window (3) and the sample chamber (10), and is a baffle with several long strip-shaped protruding ends, with a thickness of 2-3 mm and a width not exceeding the diameter of the sleeve (1), and is made of titanium or aluminum; the direction of the long strip protrusion of the fork-shaped baffle (5) is consistent with the direction of insertion or extraction of the baffle, and its upper part is fixed on a horizontal straight bar; the fork-shaped baffle (5) is inserted along the baffle socket (4) preset on the side wall of the sleeve, and after being fully inserted, its long strip-shaped protruding end is just stuck in the socket at the bottom of the inner wall of the sleeve (1); the size and distribution of the baffle socket (4) match the long strip-shaped protruding end of the fork-shaped baffle (5); a circular fork-shaped baffle handle (501) is designed on the upper bar of the fork-shaped baffle (5).

10. The method of use according to claim 9, wherein: The fixed base (18) is a metal sheet with a main body of a rectangular parallelepiped, and the material is one of aluminum or copper; its length is 40-70 mm, width is 30-60 mm, and thickness is 2-3 mm, and its upper surface is designed with two upwardly extending slide rail slots (19); the slide rail length of the slide rail slot (19) is 40-70 mm, and the slot spacing is 30-60 mm; the sheet-like support leg (7) is a long sheet, with a length of 30-60 mm, a support leg thickness of 1-2 mm, and a support leg spacing of 30-60 mm; the width of the portion of the sheet-like support leg (7) stuck in the slide rail slot (19) is 2-3 mm.

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