A transmission electron microscope sample rod

Abstract

The present invention discloses a sample holder for a transmission electron microscope, which comprises the following components: a rod body for inserting into the transmission electron microscope and isolating the vacuum degrees inside and outside the transmission electron microscope; a fixing bracket arranged at one end of the rod body located inside the transmission electron microscope and used for fixing a sample; an operating rod arranged in the rod cavity of the rod body and rotatably matched with the rod body; a thimble arranged at the rod end of the operating rod and hinged with the operating rod, the thimble corresponding to the position of the sample and capable of performing in-situ pressing tests on the sample; and an adjusting part for adjusting the axial movement of the operating rod along the rod body and / or adjusting the deflection angle of the thimble. By controlling the axial movement of the operating rod along the rod body in real time and adjusting the deflection angle of the thimble, the present invention realizes the orthogonal double-tilting function of the sample, can perform in-situ mechanical loading observation and research on the specific crystal orientation of a specific area of the sample, and has higher test efficiency.

Description

Technical Field

[0001] The invention relates to the field of material structure analysis, in particular to a transmission electron microscope sample rod. Background Art

[0002] The study of plastic deformation of structural materials has always been a hot topic in academia, and one of the research focuses is the response mode and degree of change of the microstructure of structural materials to external forces. Since the various nanoscale structural defects in the microstructure are extremely small, it is difficult to directly observe them through conventional testing methods. Transmission electron microscopy is a testing method that uses electromagnetic prisms to converge electron beams and use them as probes to detect samples. Since the wavelength of the electron beam is much lower than that of visible light, the theoretical resolution of transmission electron microscopy is much higher than conventional testing methods. It is currently the main testing method for directly observing microscopic crystal defects inside materials and their evolution laws.

[0003] At present, the academic community is not satisfied with using transmission electron microscopes to observe static microscopic crystal defects, but hopes to observe the microstructural response of structural materials during stress in transmission electron microscopes. To this end, it is necessary to implement controllable mechanical loading on the sample in a transmission electron microscope and observe it throughout the process. Due to the small internal space of the transmission electron microscope, only small-sized samples can be used for testing, and the samples are placed in the transmission electron microscope through a special sample rod. Therefore, in order to achieve real-time observation of the sample's stress process in a transmission electron microscope, a sample rod capable of realizing mechanical experiments must be manufactured. However, the existing unidirectional tensile sample rod can only be tilted in one dimension, and it is difficult to obtain a specific crystal orientation in the target area. The test efficiency is low, so it needs to be solved urgently. Summary of the invention

[0004] In order to avoid and overcome the technical problems existing in the prior art, the present invention provides a transmission electron microscope sample holder. The present invention realizes the orthogonal double tilting function of the sample, can perform in-situ mechanical loading observation and research on the specific crystal orientation of a specific area of ​​the sample, and has high test efficiency.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A transmission electron microscope sample holder comprises the following components:

[0007] The rod body is used to be inserted into the transmission electron microscope and isolate the vacuum inside and outside the transmission electron microscope;

[0008] A fixing frame is arranged at one end of the rod body located in the transmission electron microscope and is used to fix the sample;

[0009] An operating rod is arranged in the rod cavity of the rod body and rotatably cooperates with the rod body;

[0010] The ejector pin is arranged at the rod end of the operating rod and is hinged with the operating rod. The ejector pin corresponds to the position of the sample and can perform an in-situ ejection pressure test on the sample.

[0011] An adjusting portion, used for adjusting the axial movement of the operating rod along the rod body and / or adjusting the deflection angle of the ejector pin;

[0012] The rod body includes a rod shaft inserted into the transmission electron microscope and a sealing sleeve for sealing the opening of the rod shaft outside the transmission electron microscope. The sealing sleeve is fixed to the rod shaft by bolts and the contact surface is sealed by a sealing ring. The rod cavity of the rod shaft is an active cavity connected to the transmission electron microscope, and the cylinder cavity of the sealing sleeve is an adjustment cavity connected to the active cavity. The diameter of the adjustment cavity is larger than the diameter of the active cavity and the adjustment part is pre-installed in the adjustment cavity. The operating rod is rotatably matched in the active cavity, and the rod end of the operating rod extends into the adjustment cavity and corresponds to the position of the adjustment part.

[0013] As a further solution of the present invention: an adjustment seat for adjusting the deflection angle of the ejector is fixed on the fixing frame, and an adjustment protrusion is radially protruded on the ejector. After the adjustment protrusion rotates to a predetermined position with the ejector, when the operating rod slides axially along the rod body, the position of the adjustment protrusion and the adjustment seat intersect, so that the adjustment seat can push the adjustment protrusion to adjust the angle between the ejector and the operating rod.

[0014] As a further solution of the present invention, the sample clamp for clamping and fixing the sample is fixed on the fixing frame through a flip shaft, so that it can be fixed after flipping relative to the fixing frame, and the axis of the flip shaft is perpendicular to the hinge axis of the ejector.

[0015] As a further solution of the present invention: the outer ring of the operating rod is provided with a sleeve rod that rotates with the active cavity and the operating rod can slide axially along the sleeve rod cavity; an adjusting rod that is staggered with the movable trajectory of the ejector is convexly provided at the end of the sleeve rod; the adjusting rod abuts against one side of the sample clamp so that the sample clamp can be pushed while the sleeve rod rotates to cause it to flip; a torsion spring that applies elastic force to the other side of the sample clamp is also provided on the fixed frame, and the direction of the elastic force is opposite to the pressure direction of the adjusting rod on the sample clamp; the torsion spring cooperates with the adjusting rod to keep the sample clamp in a balanced state.

[0016] As a further solution of the present invention: the adjusting part includes an adjusting screw which is coaxially arranged with the operating rod and threadedly matched with the rod body, one end of the adjusting screw is located outside the rod body, and the other end is located in the adjusting cavity and abuts against the rod end of the operating rod, thereby being able to produce an axial pushing action on the operating rod.

[0017] As a further solution of the present invention: a transmission gear located in the adjustment cavity is coaxially fixed on the rod body of the operating rod, and a driving source is arranged in the adjustment cavity to drive the transmission gear to rotate;

[0018] The rod body of the operating rod is also sleeved with a return spring, one end of which is in contact with the sleeve rod, and the other end of which is in contact with the transmission gear, so as to apply an elastic force to the operating rod in the direction of the adjusting screw.

[0019] As a further solution of the present invention: the driving source includes a first control worm wheel fixed in the adjustment cavity and meshing with the transmission gear, and a first control worm outside the rod body is inserted into the adjustment cavity and forms a worm gear match with the first control worm wheel.

[0020] As a further solution of the present invention: a second control worm gear located in the adjustment cavity is coaxially fixed outside the sleeve rod, and the second control worm gear located outside the rod body is inserted into the adjustment cavity and forms a worm gear match with the second control worm gear.

[0021] As a further solution of the present invention: a first bearing and a second bearing are respectively fixed at both ends of the movable cavity, and the first bearing and the second bearing are rotatably matched with the outer ring of the sleeve rod to form a two-point support for the sleeve rod.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1. The present invention realizes the orthogonal double tilting function of the sample by real-time controlling the axial movement of the operating rod along the rod body and adjusting the deflection angle of the ejector pin, and can perform in-situ mechanical loading observation and research on the specific crystal orientation of a specific area of ​​the sample, with higher test efficiency.

[0024] 2. The present invention provides an adjusting protrusion radially on the side of the ejector pin. During the rotation of the adjusting protrusion with the ejector pin and the operating rod, the adjusting protrusion intersects with the position of the adjusting seat along the axial direction. At this time, the adjusting protrusion can be abutted and collided with the adjusting seat by pushing the operating rod along the axial direction, thereby adjusting the swing angle of the ejector pin. After the adjustment is completed, the adjusting protrusion and the adjusting seat can be staggered again by rotating the operating rod, thereby adjusting the angle between the ejector pin and the operating rod. The segmented arrangement of the rod body enables the adjusting portion to be pre-assembled in the adjusting cavity of the sealing sleeve, which makes the assembly speed faster and convenient for disassembly and installation during testing.

[0025] 3. The sample clamp of the present invention can be fixed on the fixed frame by a flipping shaft so as to generate a flipping action, thereby adjusting the pitch angle of the sample, and cooperating with the horizontal swing adjustment of the ejector pin, the test area of ​​the sample can be quickly selected; since a sleeve rod that can rotate with the rod body is also sleeved outside the operating rod, the flipping angle of the sample clamp can be adjusted by the adjusting rod when the sleeve rod is rotated, and the sample clamp is also affected by the elastic force of the torsion spring while flipping, which can ensure that the sample clamp can always remain in a balanced state after the flipping angle is adjusted.

[0026] 4. In the present invention, the rotation of the adjusting screw outside the rod body can generate an axial pushing action on the operating rod, causing the thimble to move towards the sample. When the adjusting screw pushes the operating rod forward, the return spring is in a compressed state. When the adjusting screw retracts, the return spring resets and drives the operating rod to reset synchronously, so as to keep the operating rod and the adjusting screw always in contact with each other.

[0027] 5. In the present invention, a transmission gear is coaxially fixed on the body of the operating rod. Through the worm and worm gear transmission, the operating rod can be driven to rotate while the first control worm is rotated outside the rod body, thereby driving the thimble to rotate and change its orientation. The sleeve rod can also be controlled to rotate through the worm and worm gear transmission to adjust the flipping angle of the sample clamp. The cooperation of the first bearing and the second bearing enables the sleeve rod to form two-point stable support for the sleeve rod while rotating and mating with the rod body.

[0028] 6. In the present invention, the cooperation of the first sealing ring, the second sealing ring and the third sealing ring isolates the vacuum degree inside and outside the transmission electron microscope, ensuring the safety and reliability of the test process. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 is a schematic structural diagram of the present invention.

[0030] In the figure:

[0031] 1. Rod body; 11. Adjusting cavity; 12. Moving cavity; 121. First bearing; 122. Second bearing;

[0032] 13. First sealing ring; 14. First control worm; 15. First control worm gear;

[0033] 2. Fixed frame; 21. Sample clamp; 22. Torsion spring; 23. Flipping shaft; 24. Adjusting seat;

[0034] 3. Sleeve rod; 31. Adjusting rod; 32. Second sealing ring;

[0035] 33. Second control worm gear; 34. Second control worm;

[0036] 4. Operating rod; 41. Adjusting screw; 42. Transmission gear; 43. Return spring;

[0037] 44. Thimble; 45. Adjusting protrusion; 46. Third sealing ring. DETAILED DESCRIPTION OF THE INVENTION

[0038] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0039] Please refer to Figure 1 , in an embodiment of the present invention, a sample rod for a transmission electron microscope includes a columnar rod body 1. An adjustment cavity 11 and a movable cavity 12 are sequentially formed in the rod body 1 along the axial direction. After the rod body 1 is inserted into the transmission electron microscope, the movable cavity 12 communicates with the inside of the transmission electron microscope. A first sealing ring 13 is sleeved outside the rod body 1 to seal the gap between the rod body 1 and the transmission electron microscope.

[0040] The rod body 1 is composed of two sections, including a rod body inserted into the transmission electron microscope and a sealing sleeve for closing the opening of the rod body. Here, the opening refers to the opening of the rod body outside the transmission electron microscope. The sealing sleeve is sleeved at the opening of the rod body and fixed to the rod body by bolts. The contact surface between the two is sealed by an annular sealing ring.

[0041] The rod cavity of the rod body is the movable cavity 12 communicating with the transmission electron microscope, and the barrel cavity of the sealing sleeve is the adjustment cavity 11 communicating with the movable cavity 12. The diameter of the adjustment cavity 11 is larger than that of the movable cavity 12 to allow each adjustment component to be pre-loaded therein.

[0042] A first bearing 121 and a second bearing 122 are respectively fixed at both ends of the movable cavity 12. The sleeve rod 3 passes through the inner rings of the first bearing 121 and the second bearing 122 and is rotationally matched with the first bearing 121 and the second bearing 122.

[0043] A second sealing ring 32 sleeved on the outer ring of the sleeve rod 3 is arranged between the first bearing 121 and the second bearing 122 to fill the gap between the sleeve rod 3 and the cavity wall of the movable cavity 12.

[0044] The sleeve rod 3 is a hollow rod. The operating rod 4 passes through the rod cavity of the sleeve rod 3, and a third sealing ring 46 is sleeved outside the operating rod 4 to fill the gap between the operating rod 4 and the rod cavity of the sleeve rod 3. Preferably, two groups of the third sealing rings 46 are arranged symmetrically at both ends of the operating rod 4.

[0045] The first sealing ring 13, the second sealing ring 32, and the third sealing ring 46 cooperate to isolate the internal and external environments of the transmission electron microscope and maintain the vacuum degree during the operation of the electron microscope.

[0046] A fixing frame 2 for fixing the sample is arranged at the end of the rod body 1 inserted into the transmission electron microscope, and the fixing frame 2 can be fixed by bolts. A sample clamp 21 is fixed on the fixing frame 2 through a flip axis 23. The sample is clamped and fixed by the sample clamp 21 and then sent into the transmission electron microscope. The flip axis of the sample clamp 21 is perpendicular to the axis of the rod body 1.

[0047] A torsion spring 22 is fixed to the fixing frame 2 via a spring support shaft. One end of the torsion spring 22 abuts against the fixing frame 2 , and the other end abuts against the upper side of the sample holder 21 .

[0048] An adjusting rod 31 is axially extended from the front end of the sleeve rod 3 , and the end of the adjusting rod 31 abuts against the lower side of the sample clamp 21 , thereby offsetting the elastic force of the torsion spring 22 on the sample clamp 21 , so that the sample clamp 21 is in a balanced state.

[0049] When the sleeve rod 3 rotates, the adjusting rod 31 is driven to rotate synchronously, thereby pushing the sample holder 21 to flip to adjust the flip angle of the sample, and at the same time cooperates with the torsion spring 22 to keep the sample holder 21 in a balanced state. During the rotation process, the adjusting rod 31 is staggered with the active track position of the ejector pin 44 and does not interfere with each other.

[0050] To facilitate the control of the rotation of the sleeve rod 3, a second control worm gear 33 located in the adjustment chamber 11 is coaxially fixed outside the sleeve rod 3, and a second control worm 34 is provided outside the rod body 1, which is threadedly matched with the rod body 1 and extends into the adjustment chamber 11. The second control worm 34 cooperates with the second control worm gear 33, so that when the second control worm 34 rotates outside the rod body 1, the sleeve rod 3 can be driven to rotate synchronously.

[0051] The rod end of the operating rod 4 is hingedly provided with an ejector pin 44 so that the ejector pin 44 can swing horizontally, and the tip of the ejector pin 44 corresponds to the position of the sample.

[0052] The operating rod 4 can be linearly extended and retracted along the rod cavity of the sleeve rod 3. To achieve the extension and retraction process, an adjusting screw 41 is arranged on the rod body 1 along the axial direction of the operating rod 4 and is threadedly matched with the rod body 1. One end of the adjusting screw 41 is located outside the rod body 1, and the other end abuts against the rod end of the operating rod 4 in the adjusting cavity 11. When the adjusting screw 41 is manually rotated, the operating rod 4 can be pushed forward axially.

[0053] To facilitate the resetting of the operating rod 4, a transmission gear 42 is coaxially fixed to the rod end of the operating rod 4, and a return spring 43 is sleeved on the operating rod 4, one end of the return spring 43 abuts against the transmission gear 42, and the other end abuts against the rod end of the sleeve rod 3. When the adjusting screw 41 pushes the operating rod 4 forward, the return spring 43 is in a compressed state, and when the adjusting screw 41 is retracted, the return spring 43 is reset, thereby driving the operating rod 4 to reset synchronously, so as to keep the operating rod 4 and the adjusting screw 41 always in abutment.

[0054] A first control worm gear 15 meshing with the transmission gear 42 is installed in the adjusting chamber 11, and a first control worm 14 is provided outside the rod body 1, which is threadedly matched with the rod body 1 and extends into the adjusting chamber 11. The first control worm 14 cooperates with the first control worm gear 15, so that when the first control worm 14 is rotated outside the rod body 1, the operating rod 4 can be driven to rotate.

[0055] In order to facilitate the adjustment of the deflection angle of the ejector pin 44, an adjustment protrusion 45 is radially protruded on the side of the ejector pin 44, and an adjustment seat 24 is fixed on the fixing frame 2. During the rotation of the adjustment protrusion 45 with the ejector pin 44 and the operating rod 4, there is an intersection with the axial position of the adjustment seat 24. When there is an intersection, the operating rod 4 can be pushed axially to make the adjustment protrusion 45 collide with the adjustment seat 24 to adjust the swing angle of the ejector pin 44. After the adjustment is completed, the operating rod 4 can be rotated again to make the adjustment protrusion 45 and the adjustment seat 24 staggered again.

[0056] The basic principles of the present application are described above in conjunction with specific embodiments. However, it should be noted that the advantages, strengths, effects, etc. mentioned in the present application are only examples and not limitations, and it cannot be considered that these advantages, strengths, effects, etc. are required by each embodiment of the present application. In addition, the specific details disclosed above are only for the purpose of illustration and ease of understanding, not for limitation, and the above details do not limit the present application to being implemented by adopting the above specific details.

[0057] The block diagrams of the devices, apparatuses, equipment, and systems involved in this application are only illustrative examples and are not intended to require or imply that they must be connected, arranged, and configured in the manner shown in the block diagram. As will be appreciated by those skilled in the art, these devices, apparatuses, equipment, and systems can be connected, arranged, and configured in any manner. Words such as "including", "comprising", "having", etc. are open words, referring to "including but not limited to", and can be used interchangeably with them. The words "or" and "and" used here refer to the words "and / or" and can be used interchangeably with them, unless the context clearly indicates otherwise. The words "such as" used here refer to the phrase "such as but not limited to", and can be used interchangeably with them.

[0058] It should also be noted that in the apparatus, device and method of the present application, each component or each step can be decomposed and / or recombined. Such decomposition and / or recombination should be regarded as equivalent solutions of the present application.

[0059] The foregoing description of the disclosed aspects is provided to enable any person skilled in the art to make or use the present application. Various modifications to these aspects will be readily apparent to those skilled in the art, and the general principles defined herein may be applied to other aspects without departing from the scope of the present application. Thus, the present application is not intended to be limited to the aspects shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

[0060] The foregoing description has been presented for purposes of illustration and description. Furthermore, the description is not intended to limit embodiments of the present application to the form disclosed herein. Although several example aspects and embodiments have been discussed above, those skilled in the art will recognize some variations, modifications, alterations, additions, and subcombinations thereof.

Claims

1. A transmission electron microscope sample holder, It is characterized in that It includes the following components: The rod body (1) is used for being inserted into the transmission electron microscope and isolating the vacuum inside and outside the transmission electron microscope; A fixing frame (2) is arranged at one end of the rod body (1) located inside the transmission electron microscope and is used to fix the sample; An operating rod (4) is arranged in the rod cavity of the rod body (1) and is rotatably matched with the rod body (1); An ejector pin (44) is arranged at the rod end of the operating rod (4) and is hingedly matched with the operating rod (4). The ejector pin (44) corresponds to the position of the sample and can perform an in-situ ejection pressure test on the sample. An adjustment portion, used for adjusting the axial movement of the operating rod (4) along the rod body (1) and / or adjusting the deflection angle of the ejector pin (44); The rod body (1) comprises a rod shaft inserted into the transmission electron microscope and a sealing sleeve for sealing an opening of the rod shaft located outside the transmission electron microscope, the sealing sleeve and the rod shaft are fixed by bolts and the contact surface is sealed by a sealing ring, the rod cavity of the rod shaft is an active cavity (12) connected to the transmission electron microscope, the barrel cavity of the sealing sleeve is an adjustment cavity (11) connected to the active cavity (12), the diameter of the adjustment cavity (11) is larger than the diameter of the active cavity (12), and the adjustment part is pre-installed in the adjustment cavity (11), the operating rod (4) is rotatably matched in the active cavity (12), and the rod end of the operating rod (4) extends into the adjustment cavity (11) and corresponds to the position of the adjustment part; An adjusting seat (24) for adjusting the deflection angle of the ejector pin (44) is fixed on the fixing frame (2). An adjusting protrusion (45) is radially protruded on the ejector pin (44). After the adjusting protrusion (45) rotates to a predetermined position along with the ejector pin (44), when the operating rod (4) slides axially along the rod body (1), the positions of the adjusting protrusion (45) and the adjusting seat (24) intersect, so that the adjusting seat (24) can push the adjusting protrusion (45) to adjust the angle between the ejector pin (44) and the operating rod (4).

2. A transmission electron microscope sample holder according to claim 1, It is characterized in that The sample clamp (21) for clamping and fixing the sample is fixed on the fixing frame (2) via a turning shaft (23), so that it can be fixed after turning relative to the fixing frame (2), and the axis of the turning shaft (23) and the hinge axis of the ejector pin (44) are perpendicular to each other.

3. A transmission electron microscope sample holder according to claim 2, It is characterized in that The outer ring of the operating rod (4) is sleeved with a sleeve rod (3) that is rotatably matched with the active cavity (12), and the operating rod (4) can slide axially along the rod cavity of the sleeve rod (3). The end of the sleeve rod (3) is convexly provided with an adjustment rod (31) that is offset from the active track of the ejector pin (44). The adjustment rod (31) is in contact with one side of the sample clamp (21) so that the sample clamp (21) can be pushed while rotating with the sleeve rod (3) to produce a flipping action. A torsion spring (22) that applies elastic force to the other side of the sample clamp (21) is also provided on the fixed frame (2). The direction of the elastic force is opposite to the pressure direction of the adjustment rod (31) on the sample clamp (21). The torsion spring (22) cooperates with the adjustment rod (31) so that the sample clamp (21) is in a balanced state.

4. A transmission electron microscope sample holder according to claim 3, It is characterized in that The adjusting part includes an adjusting screw rod (41) arranged coaxially with the operating rod (4) and in threaded cooperation with the rod body (1). One end of the adjusting screw rod (41) is located outside the rod body (1), and the other end is located inside the adjusting cavity (11) and abuts against the rod end of the operating rod (4) so as to generate an axial pushing action on the operating rod (4).

5. A sample rod for a transmission electron microscope according to claim 4, wherein, a transmission gear (42) located inside the adjusting cavity (11) is coaxially fixed on the rod body of the operating rod (4), and a driving source is arranged inside the adjusting cavity (11) to drive the transmission gear (42) to rotate; A return spring (43) is further sleeved on the rod body of the operating rod (4). One end of the return spring (43) abuts against the sleeve rod (3), and the other end abuts against the transmission gear (42), so as to apply an elastic force to the operating rod (4) in the direction towards the adjusting screw rod (41).

6. A sample rod for a transmission electron microscope according to claim 5, wherein, the driving source includes a first control worm wheel (15) fixed inside the adjusting cavity (11) and meshing with the transmission gear (42). A first control worm (14) located outside the rod body (1) is inserted into the adjusting cavity (11) and forms a worm and worm wheel cooperation with the first control worm wheel (15).

7. A sample rod for a transmission electron microscope according to claim 4, wherein, a second control worm wheel (33) located inside the adjusting cavity (11) is coaxially fixed outside the sleeve rod (3). A second control worm (34) located outside the rod body (1) is inserted into the adjusting cavity (11) and forms a worm and worm wheel cooperation with the second control worm wheel (33).

8. A sample rod for a transmission electron microscope according to claim 4, wherein, a first bearing (121) and a second bearing (122) are respectively fixed at both ends of the movable cavity (12). The first bearing (121) and the second bearing (122) are in rotary cooperation with the outer circle of the sleeve rod (3) so as to form two-point support for the sleeve rod (3).

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