Sample bracket

Abstract

The invention discloses a sample bracket, and relates to the technical field of scanning electron microscopes, the sample bracket provided by the invention comprises a mounting base, a clamping base, an inclination angle sample seat, a carrying net and a positioning device, the mounting base can be fixed on a vacuum transfer device; the clamping base is fixedly arranged on the mounting base, and a plurality of fixed mounting positions and at least one adjusting mounting position are arranged on the clamping base; the plurality of inclination angle sample seats are respectively arranged at the fixed mounting position and the adjusting mounting position, and the inclination angle of the inclination angle sample seat at the adjusting mounting position can be adjusted; the carrying net is used for carrying a sample and is arranged on the inclination angle sample seat; the positioning device can abut against the side, away from the dip angle sample base, of the carrying net so that the carrying net can be fixed to the dip angle sample base. According to the sample bracket provided by the invention, the dip angle of the dip angle sample seat at the mounting position can be adjusted, the sample bracket is adaptive to a scanning electron microscope vacuum transfer device, and the dip angle of the sample can be flexibly adjusted according to different crystal orientation requirements.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of scanning electron microscopy, in particular to a sample holder. BACKGROUND

[0002] With the rapid development of nanomaterial science and electron microscopy technology, the research demand for air-sensitive materials (such as lithium metal battery electrodes and perovskite semiconductors) is increasing. Such materials are easily oxidized, decomposed or structurally damaged when exposed to air or humidity, making it difficult to characterize their intrinsic properties. In the traditional scanning electron microscope (SEM) focused ion beam (FIB) sample preparation process, the sample needs to be transferred to different devices multiple times, and it is difficult to avoid short-term exposure during the process, which seriously restricts the accurate preparation and structural analysis of sensitive materials. In the current technology, although a vacuum transfer device has been used to reduce sample contamination, the functions of the sample holder still have significant deficiencies. The existing sample holder is designed with a fixed inclination angle, which cannot be adjusted flexibly for different crystal orientation requirements, resulting in low efficiency of crystal band axis alignment and affecting the atomic resolution characterization under the transmission electron microscope (TEM).

[0003] Therefore, there is an urgent need to design a technical solution that is suitable for a scanning electron microscope vacuum transfer device and allows flexible adjustment of the inclination angle of the sample for different crystal orientation requirements. SUMMARY

[0004] The purpose of the present application is to provide a sample holder to solve the problems existing in the prior art, which is suitable for a scanning electron microscope vacuum transfer device and allows flexible adjustment of the inclination angle of the sample for different crystal orientation requirements.

[0005] To achieve the above-mentioned purpose, the present application provides the following solutions: The present application provides a sample holder, comprising: a mounting base capable of being fixed to a vacuum transfer device; a clamping base fixed to the mounting base, the clamping base being provided with a plurality of fixed mounting positions and at least one adjustable mounting position; a plurality of inclination sample holders respectively arranged at the fixed mounting positions and the adjustable mounting position, and the inclination of the inclination sample holder arranged at the adjustable mounting position being adjustable; a carrier net for carrying a sample and arranged on the inclination sample holder; and a positioning device capable of abutting against the side of the carrier net away from the inclination sample holder to fix the carrier net on the inclination sample holder.

[0006] Preferably, a plurality of grooves and at least one strip-shaped groove are formed at the position close to the top of one side of the clamping base, the grooves forming the fixed mounting positions, and the strip-shaped groove forming the adjustable mounting position.

[0007] Preferably, an angle pin shaft is arranged on the clamping base and penetrates the side wall of the groove and the side wall of the strip-shaped groove, and the angle sample seat is movably arranged on the angle pin shaft; the groove can limit the position of the angle sample seat, and the strip-shaped groove can provide the adjusting space required by the angle sample seat during the adjustment of the angle.

[0008] Preferably, an angle adjusting screw is threadedly connected to one side of the clamping base away from the strip-shaped groove, one end of the angle adjusting screw penetrates into the strip-shaped groove and can abut against the angle sample seat in the strip-shaped groove, and the position where the angle adjusting screw abuts against the angle sample seat is below the angle pin shaft.

[0009] Preferably, a rectangular groove is arranged below the groove and the strip-shaped groove respectively, the lower part of the positioning device is arranged in the rectangular groove, and the upper part of the positioning device can abut against one side of the carrier net at the corresponding position.

[0010] Preferably, the positioning device comprises a clamping jaw, the lower part of the clamping jaw is rotatably connected in the rectangular groove, and the top of the clamping jaw is provided with an extension rod, and the end of the extension rod can abut against one side of the carrier net.

[0011] Preferably, a clamping jaw pin shaft is arranged on the clamping base and penetrates the side wall of the rectangular groove, and the lower part of the clamping jaw is rotatably sleeved on the clamping jaw pin shaft; an elastic member is arranged in the rectangular groove, one end of the elastic member abuts against the inner wall of the rectangular groove away from the opening end, and the other end abuts against the inner side wall below the clamping jaw pin shaft.

[0012] Preferably, a threaded through hole is arranged at the position below the clamping jaw pin shaft, an adjusting screw is threadedly connected in the threaded through hole, one end of the adjusting screw penetrates through the threaded through hole and penetrates into the elastic member.

[0013] Preferably, the mounting base comprises an integrally formed upper base and a lower base, the width dimension of the upper base is greater than the width dimension of the lower base; the clamping base is fixedly installed on the upper base through a sample seat fixing screw; and the lower base is fixedly connected with the vacuum transfer device.

[0014] Preferably, protection holes are arranged at both ends of the upper base in the length direction, mounting holes coaxial with the protection holes are arranged at both ends of the lower base in the length direction, the inner diameter of the mounting hole is smaller than the inner diameter of the protection hole, an installation screw is threadedly connected in the mounting hole, the top end of the installation screw is located in the protection hole, the end of the installation screw penetrates through the mounting hole and is fixedly connected with the vacuum transfer device.

[0015] The present application has the following technical effects compared with the prior art: The tilt sample holder of this invention, located at the adjustable mounting position, can swing up and down and tilt, thereby adjusting the angle of the tilt sample holder. This causes the fixed carrier and sample on it to be adjusted synchronously to the set angle, thereby obtaining a specific crystal orientation. This allows for flexible adjustment to meet different crystal orientation requirements, improving zone axis alignment efficiency and reducing the impact on atomic-level resolution characterization under transmission electron microscopy (TEM). Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the overall structure of the sample holder in one or more embodiments of the present invention; Figure 2 This is a schematic diagram of the structure of the sample holder after the angle of the tilt sample seat at the adjustment mounting position is adjusted in one or more embodiments of the present invention. Figure 3 This is an exploded view of the sample holder in one or more embodiments of the present invention; Figure 4 This is a cross-sectional view of the sample holder in one or more embodiments of the present invention; Figure 5 This is a schematic diagram illustrating the process of installing the sample holder into the vacuum transfer device in one or more embodiments of the present invention; Figure 6 This is a schematic diagram of the sample holder located on the vacuum transfer device in one or more embodiments of the present invention; Figure 7 for Figure 6 Enlarged view of point A; Figure 8 This is a schematic diagram showing the state of the sample holder when it is sealed by a vacuum transfer device in one or more embodiments of the present invention.

[0018] In the figure: 100-sample holder; 1-mounting base; 2-clamping base; 3-adjusting screw; 4-gripper; 5-tilt sample holder; 6-tilt pin; 7-carrying net; 8-tilt adjustment screw; 9-gripper pin; 10-adjusting spring; 11-sample holder fixing screw; 12-mounting screw; 200-vacuum transfer device. Detailed Implementation

[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] The purpose of this invention is to provide a sample holder to solve the problems existing in the prior art, which is compatible with the vacuum transfer device of a scanning electron microscope and facilitates flexible adjustment of the tilt angle of the sample to meet different crystal orientation requirements.

[0021] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0022] In existing technologies, although vacuum transfer devices exist to reduce sample contamination, their accompanying sample holders can only process 1-2 samples per batch, resulting in low efficiency. They also lack multi-angle adjustment capabilities, making it difficult to meet the needs of preparing complex crystal orientations. Furthermore, the fixed design limits sample positioning accuracy, increasing the difficulty of subsequent TEM characterization calibration. To address this issue, this invention provides a sample holder, referencing... Figures 1-8As shown, the device includes a mounting base 1, a clamping base 2, multiple tilt sample holders 5, multiple carrier nets 7, and multiple positioning devices. The mounting base 1 can be fixed on the vacuum transfer device 200. The clamping base 2 is fixedly mounted on the mounting base 1 and has multiple fixed mounting positions and at least one adjustable mounting position. The multiple tilt sample holders 5 are respectively located at the fixed mounting positions and the adjustable mounting positions, and the tilt angle of the tilt sample holder 5 located at the adjustable mounting position can be adjusted. The carrier net 7 is used to carry the sample and is set on the tilt sample holder 5. The positioning device can abut against the side of the carrier net 7 away from the tilt sample holder 5 to fix the carrier net 7 on the tilt sample holder 5. This invention features multiple tilt sample holders 5 arranged in parallel, supporting the concurrent preparation of multiple samples. Combined with the vacuum transfer device 200, it significantly shortens the air exposure time of sensitive samples, reducing the risk of oxidation. Secondly, by dynamically adjusting the tilt angle of the tilt sample holders 5 at the mounting position (within ±15° range), the zone axis orientation of the sample can be directly optimized during FIB sample preparation, providing an ideal crystallographic orientation for high-resolution TEM observation. Finally, the overall device adopts a modular design, compatible with mainstream electron microscope sample stages and the vacuum transfer device 200. The sample holder 100 of this invention, used in conjunction with the vacuum transfer device 200, enables FIB preparation of air-sensitive samples. Simultaneously, the sample angle can be adjusted, facilitating flexible adjustment of materials to meet different crystal orientation requirements. This compensates for the tilt angle of the FIB sample stage, aligning the zone axis of the transferred material for observation of specific orientations under a transmission electron microscope, providing reliable and convenient sample preparation support for further fine structural characterization under TEM.

[0023] In one embodiment, two grooves and a strip groove are formed near the top on one side of the clamping base 2. The grooves serve as fixed mounting positions, and the strip groove serves as adjustable mounting positions, allowing three samples to be prepared simultaneously using FIB. The sample located at the adjustable mounting position can have its tilt angle adjusted to obtain a specific crystal orientation.

[0024] In one embodiment, the clamping base 2 is provided with an angle pin 6 that passes through the side wall of the groove and the side wall of the strip groove. The angle sample holder 5 is movably mounted on the angle pin 6. The groove can limit the angle sample holder 5 at its location, and the strip groove can provide the adjustment space required for the angle sample holder 5 at its location to adjust its angle. The angle sample holder 5 located in the groove is abutted and limited by the side wall of the groove, so it is in a fixed position and cannot adjust its angle. The angle sample holder 5 located in the strip groove can rotate around the angle pin 6 at a set angle in the strip groove, thereby adjusting its angle. The direction of adjustment of the angle is defined as the β direction. To facilitate tilt angle adjustment and ensure that the adjusted angle is maintained, in this embodiment, a tilt angle adjusting screw 8 is threadedly connected to the side of the clamping base 2 away from the slot. One end of the tilt angle adjusting screw 8 passes through the slot and abuts against the tilt sample holder 5 located within the slot. The position where the tilt angle adjusting screw 8 abuts against the tilt sample holder 5 is below the tilt pin 6. By turning the tilt angle adjusting screw 8, it moves axially, thereby causing the end of the tilt angle adjusting screw 8 to push the lower part of the tilt sample holder 5 to rotate around the tilt pin 6, thus achieving adjustment of the overall angle of the tilt sample holder 5. A positioning platform is provided on the outside of the tilt sample holder 5, and the positioning platform is used to attach and fix the sample carrier 7, so that the angle of the carrier 7 can be adjusted synchronously during the tilt sample holder 5 angle adjustment. The carrier 7 is a key consumable for focused ion beam (FIB) technology, mainly used to support and fix the sample. In this embodiment, the carrier 7 is made of copper.

[0025] In one embodiment, rectangular grooves are provided below both the groove and the strip groove. The lower part of the positioning device is located in the rectangular groove. The positioning device includes a gripper 4. The lower part of the gripper 4 is rotatably connected to the rectangular groove. One end of the lower part of the gripper 4 extends away from the rectangular groove and extends to the outside of the rectangular groove. A vertical connecting rod is provided at the lower end of the gripper 4 located outside the rectangular groove. The top of the vertical connecting rod is the top of the gripper 4. An extension rod is provided at the top position, extending towards the side of the tilted sample holder 5. The end of the extension rod can abut against one side of the carrier net 7. To increase the fixing force of the gripper 4 on the carrier net 7, the clamping base 2 in this embodiment is provided with a gripper pin 9 that penetrates the sidewalls of multiple rectangular slots. The lower part of the gripper 4 is rotatably sleeved on the gripper pin 9. An elastic element is provided in the rectangular slot. One end of the elastic element abuts against the inner wall of the rectangular slot away from the opening end, and the other end abuts against the inner sidewall of the gripper 4 located below the gripper pin 9. In this embodiment, the elastic element is an adjusting spring 10. When the adjusting spring 10 is in a compressed state, under the action of the restoring force of the adjusting spring 10, it can push the lower part of the gripper 4 to rotate around the gripper pin 9 in a direction away from the tilted sample holder 5, thereby causing the end of the extension rod at the top of the gripper 4 to rotate in a direction closer to the tilted sample holder 5, thereby causing the end of the extension rod to be fixedly abutted against the carrier net 7 on the tilted sample holder 5, and having a certain abutting force to prevent slippage.

[0026] In one embodiment, the gripper 4 has a threaded through hole located below the gripper pin 9. An adjusting screw 3 is threaded into the threaded through hole. Before installing the gripper 4, the adjusting spring 10 needs to be placed in the rectangular groove of the clamping base 2. One end of the adjusting screw 3 passes through the threaded through hole and is inserted into the adjusting spring 10. When the end of the extension rod abuts against the carrier 7, the adjusting screw 3 is turned so that the end of the adjusting screw 3 abuts against the inner wall of the rectangular groove away from the opening. This keeps the gripper 4 in this position, thereby further improving the fixing effect of the gripper 4 on the carrier 7 and ensuring that the sample on the carrier 7 does not shake.

[0027] In one embodiment, the mounting base 1 includes an integrally formed upper base and a lower base, the width of the upper base being greater than the width of the lower base; the clamping base 2 is fixedly mounted on the upper base by sample holder fixing screws 11; protective holes are provided at both ends of the upper base along its length, and mounting holes coaxial with the protective holes are provided at both ends of the lower base along its length, the inner diameter of the mounting holes being smaller than the inner diameter of the protective holes, mounting screws 12 are threaded into the mounting holes, the top of the mounting screws 12 is located inside the protective holes, the end of the mounting screws 12 passes through the mounting holes and is fixedly connected to the vacuum transfer device 200, the protective holes can prevent the upper part of the screws from interfering with other equipment. The sample holder 100 of the present invention can hold three carrier nets 7, two with fixed angles and one that can be tilted, allowing three samples to be prepared simultaneously using FIB. In use, in a glove box filled with inert gas, the sample to be prepared is taken out, the sample is loaded onto the carrier nets 7 of the sample holder 100, two carrier nets 7 are loaded onto the fixed mounting positions of the sample holder 100, and the other carrier net 7 is loaded onto the adjustable mounting position and its angle is adjusted. Both the vacuum transfer device 200 and the glove box are mature technologies. Inside the glove box, the vacuum transfer device 200 is activated to seal the sample. Then, the vacuum transfer device 200 is removed from the glove box and installed into the FIB scanning electron microscope. Once the vacuum level of the FIB scanning electron microscope reaches the required operating temperature, the vacuum transfer device 200 is activated, allowing the sample holder 100 to leak out. The FIB scanning electron microscope is then operated to complete sample preparation. The vacuum transfer device 200 is then closed to seal the sample. Next, the vacuum transfer device 200 is removed from the FIB scanning electron microscope and placed back into the glove box. Inside the glove box, the vacuum transfer device 200 is activated, and the sample-containing grid 7 is transferred to the TEM-specific vacuum transfer rod. Finally, the sample is subjected to microscopic study using a TEM.

[0028] Specific examples have been used to illustrate the principles and implementation methods of this invention. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of this invention. Furthermore, those skilled in the art will recognize that, based on the ideas of this invention, there will be changes in the specific implementation methods and application scope. Therefore, the content of this specification should not be construed as a limitation of this invention.

Claims

1. A sample holder, characterized in that: include: The mounting base can be fixed to the vacuum transfer device; A clamping base is fixedly mounted on the mounting base, and the clamping base is provided with multiple fixed mounting positions and at least one adjustable mounting position; Multiple tilt sample holders are respectively located at the fixed mounting position and the adjustable mounting position, and the tilt angle of the tilt sample holder located at the adjustable mounting position can be adjusted; A sample carrier net is used to support the sample and is placed on the tilted sample holder; as well as The positioning device is capable of contacting the side of the carrier net away from the tilted sample holder to fix the carrier net onto the tilted sample holder.

2. The sample holder according to claim 1, characterized in that: The clamping base has multiple grooves and at least one strip groove on one side near the top. The grooves form the fixed mounting position, and the strip groove forms the adjustable mounting position.

3. The sample holder according to claim 2, characterized in that: The clamping base is provided with an angle pin that passes through the side wall of the groove and the side wall of the strip groove. The angle sample holder is movably mounted on the angle pin. The groove can limit the angle sample holder at its position, and the strip groove can provide the adjustment space required for adjusting the angle of the angle sample holder at its position.

4. The sample holder according to claim 3, characterized in that: The clamping base is threaded with an angle adjustment screw on the side away from the strip groove. One end of the angle adjustment screw passes through the strip groove and can abut against the angle sample holder located in the strip groove. The position where the angle adjustment screw abuts against the angle sample holder is below the angle pin.

5. The sample holder according to claim 2, characterized in that: A rectangular groove is provided below each of the grooves and strip grooves. The lower part of the positioning device is located in the rectangular groove, and the upper part of the positioning device can abut against one side of the net at the corresponding position.

6. The sample holder according to claim 5, characterized in that: The positioning device includes a gripper, the lower part of which is rotatably connected to the rectangular groove, and the top of the gripper is provided with an extension rod, the end of which can abut against one side of the carrier net.

7. The sample holder according to claim 6, characterized in that: The clamping base is provided with a jaw pin that passes through the sidewalls of the multiple rectangular slots. The lower part of the jaw is rotatably sleeved on the jaw pin. An elastic element is provided in the rectangular slot. One end of the elastic element abuts against the inner wall of the rectangular slot away from the opening end, and the other end abuts against the inner sidewall of the jaw located below the jaw pin.

8. The sample holder according to claim 7, characterized in that: The gripper has a threaded through hole located below the gripper pin. An adjusting screw is threaded into the threaded through hole, with one end of the adjusting screw passing through the threaded through hole and inserted into the elastic element.

9. The sample holder according to claim 1, characterized in that: The mounting base includes an integrally formed upper base and a lower base, the width of the upper base being greater than the width of the lower base; the clamping base is fixedly mounted on the upper base by sample holder fixing screws; the lower base is fixedly connected to the vacuum transfer device.

10. The sample holder according to claim 9, characterized in that: The upper base has protective holes at both ends along its length, and the lower base has mounting holes at both ends along its length that are coaxial with the protective holes. The inner diameter of the mounting holes is smaller than that of the protective holes. Mounting screws are threaded into the mounting holes, with the top of the mounting screws located inside the protective holes and the end of the mounting screws passing through the mounting holes and being fixedly connected to the vacuum transfer device.

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