Sample holder tip and sample holder

Abstract

[Problem] The purpose of the present invention is to provide a sample holder that enables various forms of observation. [Solution] A sample holder tip according to the present invention is characterized by comprising: a sample stage on which a sample and / or a sample grid is mounted; a slit part which is mounted to the sample stage and which can tilt the sample stage; a frame part which holds the sample stage; and a guide part which guides the frame part. Moreover, a preferred embodiment of the sample holder tip according to the present invention is characterized in that there are a plurality of the sample stages.

Description

Sample holder tip and sample holder

[0001] The present invention relates to a sample holder tip and a sample holder used for sample visualization, image formation, analysis, etc., and more particularly to a sample holder tip and a sample holder used for sample observation under vacuum.

[0002] The need to observe and analyze samples at the molecular and atomic level has led to the need for electron microscopy, which combines highly accurate imaging and analytical techniques under harsh conditions. For example, transmission electron microscopes (TEMs) are used to observe samples under ultra-high or high vacuum.

[0003] As a sample holder for positioning a sample at an observation position of a TEM, for example, a sample holder for a transmission electron microscope is known (Patent Document 1), which comprises: a sample holder body having a first opening with a step formed therein; a sample holding member that is rotatably housed within the first opening by having a portion of its periphery supported by the step and has a second opening in its center for holding the sample; and a cover member that has an amorphous material film that covers the second opening except for at least a portion of the second opening.

[0004] Also known is a cryogenic sample holder for storing, cooling, and positioning a sample in at least one imaging and analysis device, characterized in that it includes a container for storing and holding the sample, a storage container for storing a liquid cooling medium having a collection point for the liquid cooling medium, a thermal conductor that is in thermal contact with the liquid cooling medium and the container regardless of the amount of the liquid cooling medium in the container and the spatial orientation of the storage container, the thermal conductor being in adjacent surface contact with the liquid cooling medium at the collection point, and an elongated barrel attached between the storage container and the container to position the sample at a preselected location in at least one of the imaging and analysis devices (Patent Document 2).

[0005] JP 2007-179805 A JP 2013-537689 A

[0006] In conventional TEM sample holders, including the one disclosed in Patent Document 1, it is necessary to isolate the atmosphere side from the vacuum side so that the vacuum does not leak through the holder inside the TEM.

[0007] Recently, semiconductor observation has become increasingly integrated, reaching areas that cannot be observed with the resolution of an SEM, and there has been a shift from SEM to TEM for defect analysis, confirmation of structural integrity, etc. This requires processing a large amount of semiconductor analysis, but unlike SEM, analysis takes time, so previous throughput cannot be achieved, and even if observation and analysis are continued around the clock, it is not completed, resulting in an increase in waiting times for observation.

[0008] In order to solve the above problems, an object of the present invention is to provide a sample holder that allows various observations.

[0009] In order to achieve the above object, the present inventors have conducted extensive research into the tip of a sample holder, and as a result have come up with the present invention.

[0010] That is, the tip of the sample holder of the present invention is characterized by having a sample pedestal on which the sample and / or sample mesh is placed, a slit portion that is placed on the sample pedestal and that can tilt the sample pedestal, a frame portion that holds the sample pedestal, and a guide portion that guides the frame portion.

[0011] In a preferred embodiment of the tip of the sample holder of the present invention, the sample holder tip comprises a plurality of sample pedestals.

[0012] In a preferred embodiment of the tip of the sample holder of the present invention, the sample pedestal has a support portion that slides the slit portion.

[0013] In a preferred embodiment of the sample holder tip of the present invention, the sample and / or sample mesh is fixed to the sample pedestal by a fixing member.

[0014] In a preferred embodiment of the tip of the sample holder of the present invention, the fixing member is ring-shaped.

[0015] In a preferred embodiment of the tip of the sample holder of the present invention, it is further characterized by having an offset cam mechanism.

[0016] The sample holder of the present invention is characterized by having the sample holder tip of the present invention.

[0017] In addition, in a preferred embodiment of the sample holder of the present invention, the sample holder further comprises a sample holder shaft having the sample holder tip, an outer cylinder capable of storing the sample holder shaft, and a sample holder handle installed on the sample holder shaft on the opposite side from the sample holder tip, and is characterized in that the sample holder shaft is rotatable around the sample holder shaft.

[0018] In addition, in a preferred embodiment of the sample holder of the present invention, the rotation is characterized in that the sample can be rotated around the axis of the sample holder shaft portion or around an axis perpendicular to the axial direction of the sample holder shaft portion.

[0019] In a preferred embodiment of the sample holder of the present invention, the axis of the sample holder moves back and forth relative to the longitudinal direction of the sample holder, thereby changing the position of the sample pedestal.

[0020] In a preferred embodiment of the sample holder of the present invention, there are a plurality of sample pedestals.

[0021] In a preferred embodiment of the sample holder of the present invention, the rotation of the sample holder shaft about an axis perpendicular to the axial direction thereof is performed via an offset cam mechanism.

[0022] The sample holder tip of the present invention has the advantageous effect of being useful for processing a large number of samples. The sample holder tip of the present invention also has the advantageous effect of simplifying sample attachment, thereby eliminating losses due to attachment errors. The sample holder of the present invention also has the advantageous effect of significantly reducing the time required to insert and remove a sample into a TEM, thereby improving the observation speed.

[0023] FIG. 1 is a diagram showing a side cross-sectional view of a sample holder in one embodiment of the present invention. FIG. 2 is a diagram showing a perspective view of the tip of a sample holder in one embodiment of the present invention. FIG. 3 is a diagram showing a side cross-sectional view of the tip of a sample holder in one embodiment of the present invention. FIG. 4 is a diagram showing a perspective view of the tip of a sample holder in one embodiment of the present invention. FIG. 5 is a diagram showing a state in which all sample pedestals are presented. FIG. 6 is a diagram showing a perspective view of a sample holder in one embodiment of the present invention. FIG. 6 is a diagram showing a state in which some sample pedestals are stored in the outer cylindrical portion.

[0024] The sample holder tip of the present invention is characterized by comprising a sample pedestal on which the sample and / or sample mesh is placed, a slit portion placed on the sample pedestal and capable of tilting the sample pedestal, a frame portion for holding the sample pedestal, and a guide portion for guiding the frame portion. In the present invention, the sample pedestal on which the sample and / or sample mesh is placed is not particularly limited, and may be a sample pedestal on which only the sample is placed and mounted. The fixing portion for fixing the sample and / or sample mesh to the sample pedestal is also not particularly limited, and may be any portion capable of fixing the sample, etc. to the sample holder tip. As described below, a clamp can be used, and if the sample is carried using a tip or cartridge, the tip, etc. may be used for fixing the sample.

[0025] In a preferred embodiment of the sample holder tip of the present invention, the sample holder tip has a plurality of sample pedestals. The presence of a plurality of sample pedestals makes it possible to reduce the time required to insert and remove the sample holder, thereby improving the speed of sample observation.

[0026] In a preferred embodiment of the sample holder tip of the present invention, the sample pedestal has a support portion that slides the slit portion. In the present invention, there are no particular limitations as long as the sample pedestal can be tilted by sliding the slit portion. For example, a support portion can be provided and the slit portion can be slid on the support portion.

[0027] In a preferred embodiment of the sample holder tip of the present invention, the sample and / or sample mesh is fixed to the sample pedestal by a fixing member. In a preferred embodiment of the sample holder tip of the present invention, the fixing member is ring-shaped. In the present invention, for example, the ring-shaped fixing member can be placed above the sample or the like and rotated to clamp the sample or the like, making it possible to easily fix the sample or the like. To prevent the sample or the like from slipping, a slip prevention member may be placed between the ring-shaped fixing member and the sample pedestal, in a groove cut in the sample pedestal.

[0028] Furthermore, a preferred embodiment of the specimen holder tip of the present invention is characterized by further comprising an offset cam mechanism. In the present invention, the offset cam mechanism is not particularly limited, and a conventional mechanism can be used. The specimen holder tip of the present invention is equipped with a camshaft, and by rotating the specimen holder shaft, the camshaft also rotates, and the specimen stage can be tilted. By rotating the camshaft, the specimen can be rotated around an axis perpendicular to the axial direction of the specimen holder shaft. The specimen holder shaft can also be rotated by rotating the handle.

[0029] The sample holder of the present invention is characterized by having the sample holder tip of the present invention. The above description can be referred to for the sample holder tip that can be used for the sample holder of the present invention.

[0030] In a preferred embodiment of the sample holder of the present invention, the sample holder further comprises a sample holder shaft having the sample holder tip, an outer cylinder capable of storing the sample holder shaft, and a sample holder handle attached to the sample holder shaft on the opposite side from the sample holder tip, the sample holder shaft being rotatable about the sample holder shaft. The above description of the sample holder tip that can be used in the sample holder of the present invention can be referred to.

[0031] In addition, in a preferred embodiment of the sample holder of the present invention, the rotation is characterized in that the sample can be rotated around the axis of the sample holder shaft portion or around an axis perpendicular to the axial direction of the sample holder shaft portion.

[0032] In a preferred embodiment, the sample holder shaft can be made rotatable around the sample holder shaft. This is also called X-axis tilt, α-tilt, or uniaxial tilt. Generally, this can be performed using a device on the TEM side, but in the present invention, X-axis tilt is also possible on the sample holder side. By making the sample holder rotatable around the shaft, the sample and / or sample mesh mounting part can also be made rotatable around the shaft, making it possible to observe the sample while it is rotated. Rotation can be performed by any conventional method and is not particularly limited. More specifically, for example, rotation can be performed using the handle part of the sample holder.

[0033] In a preferred embodiment of the present invention, the rotation allows the sample and / or sample mesh mounting portion to rotate around the axis of the sample holder shaft portion as described above, as well as around an axis perpendicular to the axial direction of the sample holder shaft portion. The mechanism for allowing rotation around an axis perpendicular to the axial direction of the sample holder shaft portion may be a conventional mechanism and is not particularly limited. In a preferred embodiment, the rotation around the axis perpendicular to the axial direction of the sample holder shaft portion may be performed via an offset cam mechanism.

[0034] In a preferred embodiment of the sample holder of the present invention, the axis of the sample holder moves back and forth relative to the longitudinal direction of the sample holder, thereby changing the position of the sample pedestal. This change in the position of the sample pedestal allows for fine adjustment of the sample position, and in the case of multiple sample pedestals, it is possible to set the center of observation on each sample pedestal. In other words, the center of each sample can be switched with a single operation. As described above, the present invention allows for rotation around the axis of the sample holder shaft, as well as around an axis perpendicular to the axial direction of the sample holder shaft. This makes it possible to align the crystal orientation of the sample, thereby broadening the scope of analysis. In other words, the present invention makes it possible to realize a sample holder that can hold one or more samples, and further uses a sample pedestal with a tilting function for aligning the crystal orientation, and that allows for easy sample attachment.

[0035] In a preferred embodiment of the sample holder of the present invention, the sample holder is characterized in that a plurality of sample pedestals are provided. The presence of a plurality of sample pedestals in the present invention makes it possible to process a large number of samples. Furthermore, the present invention also significantly reduces the time required to load and unload samples from a TEM, thereby improving the observation speed.

[0036] In a preferred embodiment of the present invention, the rotation of the sample holder shaft about an axis perpendicular to the axial direction of the sample holder shaft is performed via an offset cam mechanism. For details about the offset cam mechanism, please refer to the description of the tip of the sample holder described above.

[0037] While examples of the sample holder of the present invention will be described below with reference to the drawings, the present invention is not limited to these examples and can, of course, be modified as needed without departing from the spirit and scope of the present invention.

[0038] Figure 1 shows a side cross-sectional view of a sample holder according to one embodiment of the present invention. In Figure 1, 1 denotes a sample cradle, 2 denotes an offset cam mechanism, 3 denotes a sample holder shaft, 4 denotes an outer cylinder, 5 denotes a camshaft, 6 denotes a handle, and 7 denotes a motor. This example includes three tiltable cradles 1. 2 denotes an offset cam mechanism. Rotation of the sample holder shaft connected to the motor 7 and the camshaft connected to the sample holder shaft causes the cradle 1 to rotate. The camshaft is connected to the motor 7 via the sample holder shaft 3. The sample holder shaft 3 not only has a rotation function but also a retraction function for sample switching. The motor 7 is connected to the sample holder shaft 3 and thus to the camshaft, but the handle 6 also functions as a sample switcher. The handle can be moved back and forth along the longitudinal direction of the sample holder to switch samples. In this example, the camshaft is connected to the motor 7, creating a so-called two-axis tilt sample holder.

[0039] Next, Figure 2 is a perspective view of the tip of a sample holder in one embodiment of the present invention. In Figure 2, 10 denotes a reference frame, 11 denotes an offset cam mechanism, 12 denotes a reference frame guide rail (a guide portion that guides the frame portion), and 13 denotes a sample pedestal holding frame (a frame portion that holds the sample pedestal). The reference frame 10 can function as a frame for ensuring stable movement of the sample pedestal and other components. 13 denotes the sample pedestal holding frame, which allows sample switching and retraction. The reference frame 10 can have guide rails 12. The reference frame guide rails 12 serve as guide grooves, allowing the sample pedestal holding frame 13 to move. That is, the sample pedestal holding frame can move back and forth in the longitudinal direction of the sample holder along the reference frame guide rails 12. This allows sample switching. Furthermore, for atomic-resolution observation, the reference frame guide rails can also contribute to vibration prevention.

[0040] Next, Figure 3 shows a side cross-sectional view of the tip of a sample holder in one embodiment of the present invention. In Figure 3, 20 denotes a slit (slit portion), 21 denotes a pin A (support portion), 22 denotes a sample pedestal, 23 denotes a pin B (support portion), 24 denotes a camshaft slit, 25 denotes an offset cam mechanism, 26 denotes a reference frame, and 27 denotes a camshaft. In this example, three sample pedestals 22 are provided. The slits at the ends of the sample pedestal can contact the support portions of adjacent sample pedestals. The slits and support portions are slidable, thereby enabling the sample pedestal to be tilted as shown. In this example, support portions are used at both ends of the central sample pedestal. However, any combination of slits and support portions is not particularly limited, and the sample pedestal can be tilted. Such an embodiment can also be considered as an aspect of the present invention. That is, it is sufficient for the sample pedestal to have either a slit or a support (pin). If multiple pedestals exist, it is sufficient for there to be a combination of slits and support between adjacent sample pedestals. The rotation of the camshaft 27 activates the offset cam mechanism 25, tilting the sample pedestal 22. Camshaft slits 24 are provided at the ends of adjacent sample pedestals on the offset cam mechanism 25. These camshaft slits convert the rotational motion of the offset cam mechanism 25 into tilting motion of the sample pedestal. In summary, to tilt the three cradles 22 simultaneously, the central cradle serves as the reference, and pins AB (21, 23) are fixed. The adjacent sample pedestals 22 are mounted on slit tables so that the central pins AB (21, 23) slide. Furthermore, the sample pedestal 22 is slit-shaped, allowing the pins to slide with the rotation of the camshaft 27, enabling it to rotate.

[0041] Figure 4 is a perspective view of the tip of a sample holder in one embodiment of the present invention. In Figure 4, reference numeral 30 denotes an anti-slip ring, 31 denotes a clamp ring (fixing member), 32 denotes a state in which the sample is fixed by rotation, 33 denotes a reference frame, 34 denotes the center of the rotation axis, 35 denotes a groove, 36 denotes a sample pedestal holding frame, and 37 denotes a reference frame guide rail. The clamp ring (fixing member) 31 can be used to fix the sample. The anti-slip ring 30 can serve to prevent the clamp ring 31 and, ultimately, the sample from moving. The anti-slip ring 30 has a shape that matches the groove 35, allowing it to be fixed to the sample pedestal. The sample can be fixed to the sample pedestal by rotating the clamp ring (fixing member) 31. In this example, the sample can be clamped by placing a ring-shaped fixing member on top and rotating it, making it easy to fix the sample.

[0042] Reference numeral 34 denotes the center of rotation axis, and the sample stage can rotate and tilt around this center.

[0043] 5 is a perspective view of a sample holder in one embodiment of the present invention, showing all sample pedestals in place.

[0044] Fig. 6 is a perspective view of a sample holder according to an embodiment of the present invention, showing a state in which a part of the sample pedestal is stored in the outer cylinder. The position of the sample pedestal can be changed by moving the handle back and forth in the direction of the arrow in Fig. 6.

[0045] The sample holder of the present invention is suitable for use under high vacuum conditions and is expected to be useful in a wide range of fields.

[0046] 1 Specimen base (cradle) 2 Offset cam mechanism 3 Specimen holder shaft 4 Outer cylinder 5 Camshaft 6 Handle 7 Motor 10 Reference frame 11 Offset cam mechanism 12 Reference frame guide rail (guide part that guides the frame part) 13 Specimen base holding frame (frame part that holds the specimen base) 20 Slit 21 Pin A 22 Specimen base 23 Pin B 24 Slit for camshaft 25 Offset cam mechanism 26 Reference frame 27 Camshaft 30 Anti-slip ring 31 Clamp ring 32 Specimen fixed by rotation 33 Reference frame 34 Center of rotation axis 35 Groove 36 Specimen base holding frame 37 Reference frame guide rail

Claims

1. A sample holder tip characterized by having a sample pedestal on which the sample and / or sample mesh is placed, a slit portion placed on the sample pedestal and capable of tilting the sample pedestal, a frame portion for holding the sample pedestal, and a guide portion for guiding the frame portion.

2. The tip of the sample holder according to claim 1, characterized in that there are a plurality of said sample pedestals.

3. The tip of the sample holder according to claim 2, wherein said sample pedestal has a support portion that slides said slit portion.

4. A sample holder tip as claimed in any one of claims 1 to 3, characterized in that the sample and / or sample mesh is fixed to the sample pedestal by a fixing member.

5. The tip of the sample holder according to claim 4, wherein said fixing member is ring-shaped.

6. The tip of a sample holder according to any one of claims 1 to 5, further comprising an offset cam mechanism.

7. A sample holder having a sample holder tip according to any one of claims 1 to 6.

8. A sample holder as described in claim 7, further comprising a sample holder shaft having said sample holder tip, an outer cylinder capable of storing said sample holder shaft, and a sample holder handle attached to said sample holder shaft on the opposite side to said sample holder tip, wherein said sample holder shaft is rotatable about said sample holder shaft.

9. A sample holder according to claim 8, characterized in that said rotation allows the sample to be rotated about the axis of said sample holder shank or about an axis perpendicular to the axial direction of said sample holder shank.

10. The sample holder according to claim 8 or 9, characterized in that the axis of the sample holder moves back and forth relative to the longitudinal direction of the sample holder to change the position of the sample pedestal.

11. The sample holder according to any one of claims 8 to 10, characterized in that there are a plurality of said sample pedestals.

12. The specimen holder according to claim 9, wherein the rotation of said specimen holder shaft portion about an axis perpendicular to the axial direction is effected via an offset cam mechanism.

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