Transmission electron microscope magnetic sample processing device, adjustment method and processing method

Abstract

The present application relates to a processing device, adjustment method, and processing method for magnetic samples for transmission electron microscopy. The processing device comprises a base provided with a three-dimensional displacement platform; a cover tube fixedly connected to the three-dimensional displacement platform and capable of moving in the X, Y, and Z directions driven by the three-dimensional displacement platform; a Halbach magnet fixed within the cover tube and having a central channel; a flushing mechanism including a nozzle; a sliding mechanism including a slide rail provided on the base and a sliding member slidably engaged with the slide rail; and a mounting seat for restraining a sample rod. The mounting seat is connected to the sliding member and, driven by the sliding member, moves toward or away from the Halbach magnet in the Y direction, thereby allowing the front end of the sample rod arranged along the Y direction to be inserted into the channel, with the nozzle opening directed toward the transmission electron microscope magnetic sample at the front end of the sample rod. This device can remove weak links in the magnetic sample under transmission electron microscopy that could potentially harm the transmission electron microscope, thereby extending the service life of the transmission electron microscope.

Description

Technical Field

[0001] The present application relates to the technical field of transmission electron microscopy testing and characterization of instruments and meters, and in particular to a processing device, an adjustment method, and a processing method for transmission electron microscopy magnetic samples. Background Art

[0002] Transmission electron microscopy (TEM) uses high-energy electron beams to observe the microstructure of materials. Similar to how optical microscopes use convex and concave glass lenses to constrain the propagation path of light, TEMs use magnetic lenses to constrain the propagation of high-energy electron beams. Specifically, the magnetic field surrounding TEM samples is greater than 1 Tesla. TEM magnetic samples are typically obtained through focused ion beams, ion thinning, electrolytic double spraying, and ultrathin carbon film / microgrid preparation. Therefore, TEM magnetic samples contain weakly connected areas. When observing magnetic materials, TEM magnetic samples can be attracted to the pole piece due to static magnetostatic forces, causing damage to the microscope.

[0003] Magnetic materials are classified into bulk and powder forms. Bulk magnetic materials are typically prepared into transmission electron microscopy (TEM) samples through ion thinning, electrolytic double spraying, and focused ion beam techniques. The prepared TEM samples often contain some weakly connected portions to the overall TEM sample. These weakly connected portions can escape from the TEM magnetic field and become adsorbed on the surface of the TEM pole piece. To remove these weakly connected portions, the TEM sample is typically subjected to ultrasonic oscillation or mechanical separation using needle tip manipulation. However, these methods can also damage other safe areas of the TEM sample suitable for observation. Powder samples are typically prepared into double-networked carbon film samples through ultrasonic dispersion. However, the two layers of double-networked carbon film can severely reduce the imaging quality of spherical aberration-corrected TEMs. Magnetic powder samples still need to be prepared into conventional ultrathin carbon film / microgrid samples. However, when the carbon support film on the ultrathin carbon film / microgrid does not have sufficient adsorption capacity for the magnetic powder particles, these particles can escape and become adsorbed on the pole piece surface. Summary of the Invention

[0004] Based on this, it is necessary to provide a transmission electron microscope magnetic sample processing device that can reliably remove the weakly connected parts in the magnetic sample.

[0005] The present application provides a device for processing magnetic samples for transmission electron microscopy, comprising a base, a top surface of which is provided with a three-dimensional displacement platform; a cover tube fixedly connected to the three-dimensional displacement platform and capable of moving in the X, Y, and Z directions under the drive of the three-dimensional displacement platform; a Halbach magnet fixed in the cover tube, the center of the Halbach magnet having a channel extending along the Y direction; a flushing mechanism provided on the cover tube and comprising a nozzle for blowing air into the channel; a sliding mechanism provided on the top surface of the base and arranged in sequence with the Halbach magnet along the Y direction, the sliding mechanism comprising a slide rail provided on the base and a sliding member slidably engaged with the slide rail in the Y direction; a mounting seat for constraining a sample rod, the mounting seat being connected to the sliding member and driven by the sliding member to approach or move away from the Halbach magnet along the Y direction, thereby allowing the front end of the sample rod arranged along the Y direction to be inserted into the channel, the front end of the sample rod being used to mount a magnetic sample for transmission electron microscopy, and the nozzle of the nozzle facing the front end of the sample rod.

[0006] In one embodiment, the mounting seat is provided with a limiting groove for the sample rod to be inserted along the X direction, and the mounting seat can be rotatably constrained on the sliding member around an axis extending along the Z direction, so that the sample rod has a mounting position arranged along the X direction and a pre-processing position arranged along the Y direction. When the sample rod is in the mounting position, the mounting seat is located at the end of the slide rail away from the Halbach magnet.

[0007] In one embodiment, the mounting seat includes an upper pressing member and a lower supporting seat arranged in sequence from top to bottom. The upper pressing member is arranged to be able to move along the Z direction relative to the lower supporting seat, and the limiting groove is formed together with the lower supporting seat.

[0008] In one embodiment, a positioning groove for positioning the sample rod is provided on the lower support seat.

[0009] In one embodiment, the base includes a first bottom plate extending along the Y direction and a second bottom plate extending along the X direction, one end of the first bottom plate is connected to one end of the second bottom plate, the cover tube and the sliding mechanism are both arranged on the first bottom plate, and the cover tube is fixed to an end of the first bottom plate away from the second bottom plate, when the sample rod is in the installation position, the mounting seat is located at an initial position of the first bottom plate close to the second bottom plate, and part of the sample rod is located above the second bottom plate.

[0010] In one embodiment, the cover tube includes a first cover shell and a second cover shell connected in sequence along the Y direction, at least a portion of the first cover shell is located between the second cover shell and the mounting seat, a first opening is opened at a position corresponding to the channel, the opening of the second cover shell at the position corresponding to the channel is defined as a second opening, the first opening is located between the channel and the mounting seat, and the nozzle extends into the channel through the second opening.

[0011] In one embodiment, the Halbach magnet is composed of 12 NdFeB magnets spliced ​​together in sequence along its circumference. The magnetization direction of the NdFeB magnet is along the radial direction of the Halbach magnet, and the magnetization directions of two adjacent NdFeB magnets are 30° to each other. The maximum magnetic field in the channel is 1.2 T, and the direction of the maximum magnetic field is along the radial direction of the channel.

[0012] In one embodiment, the position where the magnetic field intensity in the channel of the Halbach magnet is the largest is defined as the first position, and the front end of the sample rod can move to the first position.

[0013] The present application also provides an adjustment method, using the transmission electron microscope magnetic sample processing device described in the above embodiment, to determine the position in the Halbach magnet channel where the magnetic field intensity is the largest, and define it as a first position; the adjustment method is used to adjust the front end of the sample rod to the first position, and includes the following steps:

[0014] S1, installing the sample rod on the mounting base, at this time, the sample rod is in the mounting position;

[0015] S2, rotating the mounting base until the sample rod is in the pretreatment position;

[0016] S3, the sliding member moves along the slide rail toward the Halbach magnet until the front end of the sample rod enters the channel, and the relative position of the front end of the sample rod and the Halbach magnet is adjusted by the three-dimensional displacement platform until the front end of the sample rod is located at the first position.

[0017] The present application also provides a processing method, including the adjustment method, and in step S1, when the sample holder is in the installation position, the transmission electron microscope magnetic sample is installed at a designated position on the front end of the sample holder and assembled in place;

[0018] The flushing mechanism includes an air pipe for communicating with an air source, an air outlet end of the air pipe is connected to the nozzle, and an electromagnetic valve for controlling the on / off of the air pipe is provided on the air pipe. The processing method further includes step S4 located after step S3, wherein:

[0019] In step S4, a DC voltage is applied to the solenoid valve, the solenoid valve opens, and timing begins. Compressed gas is ejected from the nozzle to flush the TEM magnetic sample at the front end of the TEM sample holder. After a period of time, the DC voltage is disconnected, the solenoid valve is closed, and the gas flushing ends. The sample holder is then driven by the sliding member to return to its initial position away from the Halbach magnet, and the sample holder is placed in the installation position. The sample holder is then removed.

[0020] Compared with the prior art, in the TEM magnetic sample processing device provided in the present application, with the cooperation of the magnetic field in the channel of the Halbach magnet and the gas purge, the weak connection part of the TEM magnetic sample on the front end of the sample rod that is potentially harmful to the TEM can be removed, thereby preventing the TEM magnetic sample from being adsorbed to the pole shoe under the action of static magnetostatic force when observing the TEM magnetic sample, thereby extending the service life of the TEM. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the conventional technology, the following briefly introduces the drawings required for use in the embodiments or the conventional technology descriptions. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0022] Figure 1 A perspective view of a device for processing magnetic samples for a transmission electron microscope according to an embodiment of the present application;

[0023] Figure 2 This is a schematic structural diagram of a sample rod according to an embodiment of the present application;

[0024] Figure 3 This is a schematic structural diagram of a mounting base according to an embodiment of the present application;

[0025] Figure 4 for Figure 1 Structural diagram of the sliding mechanism;

[0026] Figure 5 Schematic diagram of the structure of Halbach magnet;

[0027] Figure 6 for Figure 5 A schematic diagram of the structure from another angle (with magnetization direction marked);

[0028] Figure 7 This is a three-dimensional exploded view of the cover cylinder, Halbach magnet and part of the flushing mechanism after assembly;

[0029] Figure 8 for Figure 1A schematic diagram of a structure in which a sample rod is installed and in an installed position;

[0030] Figure 9 for Figure 1 A schematic diagram of a structure in which a sample rod is installed and is in a pretreatment position;

[0031] Figure 10 for Figure 1 Schematic diagram of the structure in which a sample rod is installed and inserted into the channel.

[0032] Figure numerals: 1. base; 11. first bottom plate; 12. second bottom plate; 2. three-dimensional displacement platform; 3. cover cylinder; 31. first cover shell; 311. first opening; 32. second cover shell; 321. second opening; 4. Halbach magnet; 40. channel; 41. NdFeB magnet; 5. flushing mechanism; 51. nozzle; 52. gas pipe; 53. solenoid valve; 6. sliding mechanism; 61. slide rail; 62. sliding part; 7. sample rod; 8. mounting seat; 80. limiting groove; 81. upper pressure piece; 82. lower support seat; 821. positioning groove; 83. assembly seat. DETAILED DESCRIPTION

[0033] To make the above-mentioned objects, features, and advantages of the present application more clearly understood, the specific embodiments of the present application are described in detail below with reference to the accompanying drawings. The following description sets forth many specific details to facilitate a full understanding of the present application. However, the present application can be implemented in many other ways than those described herein, and those skilled in the art can make similar improvements without violating the scope of the present application. Therefore, the present application is not limited to the specific embodiments disclosed below.

[0034] It should be noted that when a component is referred to as being "fixed to" or "set on" another component, it may be directly on the other component or there may also be a central component. When a component is considered to be "connected to" another component, it may be directly connected to the other component or there may be a central component at the same time. The terms "vertical", "horizontal", "up", "down", "left", "right", "side", "top", "bottom" and similar expressions used in the specification of this application are only used to describe the various example structural parts and elements of this application, but these terms are used here for the purpose of convenience of explanation and are determined based on the example orientations shown in the accompanying drawings, and do not represent the only implementation method. Since the embodiments disclosed in the application can be set in different directions, these terms indicating directions are only for illustration and should not be regarded as limitations. For example, "up" and "down" are not necessarily limited to directions opposite to or consistent with the direction of gravity.

[0035] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of such features. Throughout the description of this application, "plurality" means at least two, for example, two, three, etc., unless otherwise specifically defined.

[0036] In this application, unless otherwise expressly specified or limited, when a first feature is "above" or "below" a second feature, it can mean that the first feature is directly in contact with the second feature, or the first feature and the second feature are indirectly in contact through an intermediary. Furthermore, when a first feature is "above," "above," or "above" a second feature, it can mean that the first feature is directly above or diagonally above the second feature, or simply means that the first feature is higher in level than the second feature. When a first feature is "below," "below," or "below" a second feature, it can mean that the first feature is directly below or diagonally below the second feature, or simply means that the first feature is lower in level than the second feature.

[0037] It should be noted that "axial arrangement" means that the overall arrangement direction is along the axial direction, including but not limited to axial extension, and may form an angle with the axial direction.

[0038] Unless otherwise defined, all technical and scientific terms used in the specification of this application have the same meaning as commonly understood by those skilled in the art to which this application belongs. The terms used in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used in the specification of this application includes any and all combinations of one or more of the relevant listed items.

[0039] like Figures 1 to 10 As shown, the present application discloses a magnetic sample processing device for transmission electron microscopy. The device comprises a base 1, a cover 3, a Halbach magnet 4, a flushing mechanism 5, a sliding mechanism 6, and a mounting base 8. A three-dimensional displacement platform 2 is disposed on the top surface of the base 1. The cover 3 is fixedly connected to the three-dimensional displacement platform 2 and, driven by the three-dimensional displacement platform 2, can move in the X, Y, and Z directions.

[0040] It should be noted that the three-dimensional displacement platform 2 can be an existing three-dimensional displacement platform 2, as long as the cover tube 3 can move in the three directions of X, Y, and Z. For example, the three-dimensional displacement platform 2 is composed of three one-dimensional displacement platforms: up and down, left and right, and front and back, and the three one-dimensional displacement platforms are connected by screws. The X direction can be the front-to-back direction or the left-to-right direction, the Z direction is the up-down direction, and the Y direction is the direction at an angle to the X direction.

[0041] like Figures 5 to 10As shown, the Halbach magnet 4 is fixed in the housing 3 , and a channel 40 extending along the Y direction is provided at the center of the Halbach magnet 4 .

[0042] like Figure 1 、 Figures 7 to 10 As shown, the flushing mechanism 5 is disposed on the housing 3 and includes a nozzle 51 for blowing air into the channel 40. In this embodiment, the flushing mechanism 5 also includes a gas pipe 52 for communicating with a gas source. The gas outlet of the gas pipe 52 is connected to the nozzle 51, and the gas pipe 52 is provided with a solenoid valve 53 for controlling the on / off of the gas pipe 52. The gas source is a compressed gas, such as nitrogen or argon.

[0043] Thus, under the control of the solenoid valve 53, compressed gas is delivered to the nozzle 51 through the gas pipe 52 and ejected from the nozzle 51. That is, gas enters from one end, and after a DC voltage is input, the solenoid valve 53 opens and the gas is ejected from the nozzle 51. The gas source is usually stored in a gas cylinder, so the gas inlet end of the gas pipe 52 is connected to the gas cylinder.

[0044] like Figure 1 、 Figures 8 to 10 As shown, the sliding mechanism 6 is provided on the top surface of the base 1 and is arranged in sequence with the Halbach magnet 4 along the Y direction. The sliding mechanism 6 includes a slide rail 61 provided on the base 1 and a slide member 62 that slides with the slide rail 61 in the Y direction. Therefore, the slide rail 61 extends along the Y direction.

[0045] The mounting base 8 is used to constrain the sample rod 7. The mounting base 8 is connected to the sliding member 62 and is driven by the sliding member 62 to move closer to or away from the Halbach magnet 4 along the Y direction, so that the front end of the sample rod 7 arranged along the Y direction is inserted into the channel 40. The front end of the sample rod 7 is used to mount the magnetic sample of the transmission electron microscope, and the nozzle of the nozzle 51 is facing the front end of the sample rod 7.

[0046] TEM magnetic samples are typically obtained through focused ion beam, ion thinning, electrolytic double spraying, and ultrathin carbon film / microgrid preparation. Therefore, TEM magnetic samples contain weakly connected portions. Furthermore, channel 40 allows for the insertion and removal of the front end of sample holder 7.

[0047] It is understandable that, with the combined effect of the magnetic field and gas purge within the channel 40 of the Halbach magnet 4, the weakly connected portion of the TEM magnetic sample at the front end of the sample rod 7 that is potentially harmful to the TEM can be removed, thereby preventing the TEM magnetic sample from being adsorbed to the pole piece under the action of static magnetostatic force when observing the TEM magnetic sample, thereby extending the service life of the TEM.

[0048] The position where the magnetic field intensity is the highest in the channel 40 of the Halbach magnet 4 is defined as the first position, to which the front end of the sample rod 7 can move. The position where the magnetic field intensity is the highest in the channel 40 of the Halbach magnet 4 is typically determined using a Gauss meter probe.

[0049] It is understood that when the TEM magnetic sample at the front end of the sample holder 7 is pushed into the strong magnetic position (i.e., the first position) of the channel 40, the TEM magnetic sample is subjected to the strong magnetic field static magnetometry and purge force. For samples prepared by focused ion beam, ion thinning, or electrolytic double spray, weakly connected portions will experience stretching, bending, and ultimately fracture and detachment under the strong magnetic field static magnetometry and high-speed gas purge. For microgrid and ultrathin carbon film samples, particles with insufficient physical and chemical adsorption to the underlying carbon film will escape from the carbon film under the attraction of the strong magnetic field static magnetometry and gas purge. This ensures that weakly connected portions of the TEM magnetic sample that could potentially harm the TEM are completely removed, eliminating potential damage to the TEM from the magnetic sample and extending the life of the TEM.

[0050] Further, such as Figure 5 and Figure 6 As shown, the Halbach magnet 4 is cylindrical in shape and is composed of 12 NdFeB magnets 41 spliced ​​together along its circumference. The channel 40 is located at the center of the NdFeB magnets 41. The NdFeB magnets 41 are fan-shaped, with a central angle of 30°.

[0051] In this embodiment, if Figure 6 As shown, the magnetizing direction A of the NdFeB magnet 41 is along the radial direction of the Halbach magnet 4, and the magnetizing directions A of the two adjacent NdFeB magnets 41 are 30° to each other. The maximum magnetic field in the channel 40 is 1.2 T, and the direction of the maximum magnetic field is along the radial direction of the channel 40. In this way, a unique maximum magnetic field can be generated at the channel 40 at the center of the Halbach magnet 4. In this embodiment, the maximum magnetic field is a strong magnetic field of 1.2 T. Moreover, at room temperature (20°C~30°C), the maximum magnetic field in the channel 40 can be maintained for a long time. Schematically, the brand of the NdFeB magnet 41 is N50. The magnetizing direction A (i.e., magnetization direction) of the NdFeB magnet 41 is specifically referred to Figure 6 The direction indicated by the arrow.

[0052] like Figure 1 、 Figure 7 and Figure 8As shown, the cover 3 includes a first cover shell 31 and a second cover shell 32 connected in sequence along the Y direction. The first cover shell 31 and the second cover shell 32 are detachably connected by a connector, such as a screw or bolt. This facilitates the installation of the Halbach magnet 4 in the space enclosed by the first cover shell 31 and the second cover shell 32. In addition, at least a portion of the first cover shell 31 is located between the second cover shell 32 and the mounting base 8.

[0053] like Figure 7 and Figure 8 As shown, the first housing 31 has a first opening 311 at a position corresponding to the channel 40, and the second housing 32 has a second opening 321 at a position corresponding to the channel 40. The first opening 311 is located between the channel 40 and the mounting base 8, and the nozzle 51 extends into the channel 40 through the second opening 321. This prevents the nozzle 51 from interfering with the sample rod 7 entering the channel 40 through the first opening 311.

[0054] In order to prevent the nozzle 51 from shaking when spraying, the nozzle 51 is fixed on the cover tube 3.

[0055] like Figure 1 and Figure 3 As shown, the mounting seat 8 is provided with a retaining groove 80 for inserting the sample holder 7 along the X-direction. The mounting seat 8 is rotatably constrained on the slide 62, thereby enabling the sample holder 7 to have an installation position arranged along the X-direction and a pretreatment position arranged along the Y-direction. When the sample holder 7 is in the installation position, the mounting seat 8 is located at the end of the slide rail 61 away from the Halbach magnet 4. The rotation axis of the mounting seat 8 extends along the Z-direction, that is, the mounting seat 8 rotates about the axis extending along the Z-direction.

[0056] In this way, the rotatable mounting base 8 rotates, thereby enabling the sample holder 7 to switch between the mounting position and the pre-processing position. In other words, the transmission electron microscope magnetic sample processing device is integrated with a loading function for mounting the sample holder 7 .

[0057] In other embodiments, a snap-fit ​​structure can be used to snap the sample rod 7 onto the limiting groove 80 of the mounting seat 8. Figure 3As shown, the mounting base 8 includes an upper pressing member 81 and a lower support base 82 arranged sequentially from top to bottom. The upper pressing member 81 is arranged to move relative to the lower support base 82 in the Z direction (i.e., the vertical direction) and forms a limiting groove 80 with the lower support base 82. Thus, by adjusting the position between the upper pressing member 81 and the lower support base 82, sample rods 7 of different diameters can be installed. Furthermore, the upper pressing member 81 is secured to the sliding member 62 or the lower support base 82 via fasteners, thereby securing the position of the upper pressing member 81. Furthermore, the mounting base 8 also includes an assembly base 83 located below the lower support base 82. The lower support base 82 is fixed to the assembly base 83, and the assembly base 83 is rotationally constrained to the sliding member 62.

[0058] The three-dimensional displacement platform 2 is used to adjust the relative position between the center of the Halbach magnet 4 and the front end of the sample rod 7, ensuring that the front end of the sample rod 7 is at the strongest magnetic field when the diameter of the sample rod 7 is different.

[0059] In order to better restrict the sample rod 7 and reduce the possibility of the sample rod 7 moving, a positioning groove 821 for positioning the sample rod 7 is provided on the lower support seat 82. In this embodiment, the positioning groove 821 is an arc-shaped groove that matches the corresponding position of the sample rod 7.

[0060] In addition, if Figure 1 、 Figures 8 to 10 As shown, the base 1 includes a first base plate 11 extending along the Y direction and a second base plate 12 extending along the X direction. One end of the first base plate 11 is connected to one end of the second base plate 12. The cover tube 3 and the sliding mechanism 6 are both disposed on the first base plate 11, and the cover tube 3 is fixed to the end of the first base plate 11 away from the second base plate 12. When the mounting base 8 is in its initial position, with the first base plate 11 close to the second base plate 12, and the sample rod 7 is mounted on the mounting base 8, the sample rod 7 is in the installed position, with a portion of the sample rod 7 located above and parallel to the second base plate 12.

[0061] After loading, the sample holder 7 is rotated 90° counterclockwise until it is parallel to the first base plate 11. The sample holder 7 is now in the pre-treatment position. By pushing the mounting base 8 in the Y direction toward the Halbach magnet 4, the front end of the sample holder 7 enters the channel 40 of the Halbach magnet 4.

[0062] In this embodiment, the base 1 is made of aluminum alloy, and may also be made of other metal materials.

[0063] The present application provides an adjustment method using the aforementioned processing device, for determining the position of the maximum magnetic field strength in the channel 40 of the Halbach magnet 4. The adjustment method is used to adjust the front end of the sample holder 7 to a first position, and the adjustment method includes the following steps:

[0064] S1, install the sample rod 7 on the mounting base 8. At this time, the sample rod 7 is in the installation position. Figure 8 As shown;

[0065] S2, rotating the mounting seat 8 until the sample holder 7 is in the pre-processing position;

[0066] S3, the sliding member 62 moves along the slide rail 61 toward the Halbach magnet 4 until the front end of the sample holder 7 enters the channel 40, see Figure 9 and Figure 10 As shown, the relative position of the front end of the sample rod 7 and the Halbach magnet 4 is adjusted by the three-dimensional displacement platform 2 until the front end of the sample rod 7 is located at the first position.

[0067] Thus, the front end of the sample rod 7 can be positioned at the first position of the maximum magnetic field by the above adjustment method, that is, the front end of the sample rod 7 is placed in a strong magnetic environment. The entire adjustment method is convenient and easy to operate.

[0068] In addition, the present application also provides a method for processing a magnetic sample for a transmission electron microscope, including the above-mentioned adjustment method, and the processing method sequentially comprises the following steps:

[0069] S1, install the sample rod 7 on the mounting base 8. At this time, the sample rod 7 is in the installation position. Figure 8 As shown; when the sample holder 7 is in the installation position, the transmission electron microscope magnetic sample is installed at the specified position of the front end of the sample holder 7 and assembled into place; when installing the sample holder 7, first lift the upper pressing piece 81 and place the sample holder 7 into the positioning groove 821 of the lower support seat 82, then move the upper pressing piece 81 downward so that the upper pressing piece 81 is pressed on the sample holder 7, and then fix the upper pressing piece 81 with fasteners.

[0070] S2, rotate the mounting base 8 until the sample holder 7 is in the pre-treatment position, see Figure 9 As shown;

[0071] S3, the sliding member 62 moves along the slide rail 61 toward the Halbach magnet 4 until the front end of the sample rod 7 enters the channel 40, and the relative position of the front end of the sample rod 7 and the Halbach magnet 4 is adjusted by the three-dimensional displacement platform 2 until the front end of the sample rod 7 is in the first position, see Figure 10 As shown;

[0072] In step S4, a DC voltage is applied to the solenoid valve 53, the solenoid valve 53 opens, and timing begins. A compressed gas source, such as nitrogen or argon, is ejected from the nozzle 51 to flush the TEM magnetic sample at the front end of the TEM sample holder 7. After a period of time, the DC voltage is disconnected, the solenoid valve 53 is closed, and the gas flushing ends. Subsequently, the sample holder 7 is driven by the sliding member 62 to return to its initial position away from the Halbach magnet 4, and the sample holder 7 is placed in the installation position. The sample holder 7 is then removed.

[0073] The sample holder 7 is removed from the mounting base 8 in the reverse order of the installation process, which will not be described in detail in this embodiment. The removed sample holder 7 can then be inserted into the goniometer stage of the transmission electron microscope.

[0074] The on / off of the purge flow and the purge time are controlled by the electromagnetic valve 53. The DC voltage and the flushing time are selected according to actual needs. For example, if the DC voltage is 12V, the flushing time is 1 minute, 2 minutes or more than 2 minutes.

[0075] It is understandable that the mounting base 8 can be moved along the Y direction toward the Halbach magnet 4 by pushing the sliding member 62 of the sliding mechanism 6 or the mounting base 8 until the front end of the sample rod 7 on the mounting base 8 extends into the strong magnetic field. The high-purity inert gas is controlled by the solenoid valve 53 to be ejected from the nozzle 51 to purge the TEM magnetic sample at the front end of the sample rod 7, and finally the weak connection part of the TEM magnetic sample is removed.

[0076] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0077] The above-described embodiments merely represent several implementation methods of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that a person of ordinary skill in the art may make various modifications and improvements without departing from the spirit of the present application, all of which fall within the scope of protection of the present application. Therefore, the scope of patent protection for the present application shall be determined by the appended claims.

Claims

1. A device for processing magnetic samples for transmission electron microscopy, characterized in that: include: A base, wherein a three-dimensional displacement platform is provided on the top surface of the base; The cover cylinder is fixedly connected to the three-dimensional displacement platform and can move along the X direction, Y direction and Z direction under the drive of the three-dimensional displacement platform; A Halbach magnet is fixed in the housing, and a channel is provided in the center of the Halbach magnet extending along the Y direction; a flushing mechanism, disposed on the cover cylinder and comprising a nozzle for blowing air into the channel; a sliding mechanism disposed on the top surface of the base and arranged in sequence with the Halbach magnet along the Y direction, the sliding mechanism comprising a slide rail disposed on the base and a sliding member slidably engaged with the slide rail in the Y direction; A mounting seat, for restraining the sample rod, connected to the sliding member, and driven by the sliding member to move closer to or away from the Halbach magnet along the Y direction, so that the front end of the sample rod arranged along the Y direction is inserted into the channel. The front end of the sample rod is used to mount a magnetic sample for a transmission electron microscope, and the nozzle of the nozzle faces the front end of the sample rod; The mounting seat is provided with a limiting groove for the sample rod to be inserted along the X direction, and the mounting seat can be rotatably constrained on the sliding member around an axis extending along the Z direction, so that the sample rod has an installation position arranged along the X direction and a pre-processing position arranged along the Y direction. When the sample rod is in the installation position, the mounting seat is located at the end of the slide rail away from the Halbach magnet.

2. The processing device according to claim 1, characterized in that The mounting seat includes an upper pressing member and a lower supporting seat arranged in sequence from top to bottom. The upper pressing member is arranged to be able to move along the Z direction relative to the lower supporting seat, and the limiting groove is formed together with the lower supporting seat.

3. The processing device according to claim 2, characterized in that The lower support seat is provided with a positioning groove for positioning the sample rod.

4. The processing device according to claim 1, characterized in that The base includes a first bottom plate extending along the Y direction and a second bottom plate extending along the X direction, one end of the first bottom plate is connected to one end of the second bottom plate, the cover tube and the sliding mechanism are both arranged on the first bottom plate, and the cover tube is fixed to one end of the first bottom plate away from the second bottom plate, when the sample rod is in the installation position, the mounting seat is located at an initial position of the first bottom plate close to the second bottom plate, and part of the sample rod is located above the second bottom plate.

5. The processing device according to claim 1, characterized in that The cover tube includes a first cover shell and a second cover shell connected in sequence along the Y direction, at least part of the first cover shell is located between the second cover shell and the mounting seat, the first cover shell has a first opening at a position corresponding to the channel, and the second cover shell has a second opening at a position corresponding to the channel, the first opening is located between the channel and the mounting seat, and the nozzle extends into the channel through the second opening.

6. The processing device according to claim 1, characterized in that The Halbach magnet is composed of 12 NdFeB magnets spliced ​​together in sequence along its circumference. The magnetization direction of the NdFeB magnet is along the radial direction of the Halbach magnet, and the magnetization directions of two adjacent NdFeB magnets are 30° to each other. The maximum magnetic field in the channel is 1.2 T, and the direction of the maximum magnetic field is along the radial direction of the channel.

7. The processing device according to any one of claims 1 to 6, characterized in that The position where the magnetic field intensity in the channel of the Halbach magnet is the largest is defined as a first position, and the front end of the sample rod can move to the first position.

8. A method of regulation, characterized in that: Using the transmission electron microscope magnetic sample processing device according to any one of claims 1 to 6, determining the position where the magnetic field intensity is the largest in the Halbach magnet channel, and defining it as the first position; The adjustment method is used to adjust the front end of the sample rod to the first position, and includes the following steps: S1, installing the sample rod on the mounting base, at this time, the sample rod is in the mounting position; S2, rotating the mounting base until the sample rod is in the pretreatment position; S3, the sliding member moves along the slide rail toward the Halbach magnet until the front end of the sample rod enters the channel, and the relative position of the front end of the sample rod and the Halbach magnet is adjusted by the three-dimensional displacement platform until the front end of the sample rod is located at the first position.

9. A processing method, characterized in that: The method includes the adjustment method according to claim 8, and in step S1, when the sample holder is in the installation position, the transmission electron microscope magnetic sample is installed at a designated position on the front end of the sample holder and assembled into place; The flushing mechanism includes an air pipe for communicating with an air source, an air outlet end of the air pipe is connected to the nozzle, and an electromagnetic valve for controlling the on / off of the air pipe is provided on the air pipe. The processing method further includes step S4 located after step S3, wherein: In step S4, a DC voltage is applied to the solenoid valve, the solenoid valve opens, and timing begins. Compressed gas is ejected from the nozzle to flush the TEM magnetic sample at the front end of the TEM sample holder. After a period of time, the DC voltage is disconnected, the solenoid valve is closed, and the gas flushing ends. The sample holder is then driven by the sliding member to return to its initial position away from the Halbach magnet, and the sample holder is placed in the installation position. The sample holder is then removed.

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