Attachment device for lid of sample tube

Abstract

Provided is an attachment device for a lid of a sample tube that enables a lid of a sample tube to be properly fitted in an atmosphere with a small amount of gas. The present invention is a lid attachment device 10 for attaching a lid 102 to an opening of a cylindrical sample tube body 101. The lid attachment device 10 comprises: a device body part 20 having a sealed internal space S; a lid holder 30 for holding the lid 102 in the internal space S; a sample tube body holder 40 for holding the sample tube body 101 in the internal space S; an observation window 22 provided to the device body part 20 for viewing the internal space S from the outside; an introduction port provided to the device body for introducing gas into the internal space S; and a linear introduction machine 60 that is provided on one side of the lid holder 30 and relatively moves the sample tube body holder 40 toward the other side. In the internal space S, the lid 102 moves relative to the sample tube body 101, so that the lid 102 is attached to the sample tube body 101.

Description

Sample tube lid mounting device

[0001] The present invention relates to a sample tube lid mounting device.

[0002] NMR (nuclear magnetic resonance) instruments are used to observe molecular structure and amorphous (disordered) states. When the sample is a solution (liquid), the molecules move at high speed in the solution, averaging chemical shift anisotropy and resulting in peaks appearing in the NMR spectrum. On the other hand, when the sample is a solid, powdered material with low molecular mobility is used, so chemical shift anisotropy is not canceled out, and peaks from molecules of all orientations overlap, resulting in a significantly broadened peak width in the NMR spectrum. For this reason, the MAS (magic angle spinning) method is used when measuring the NMR spectrum of a solid sample. In the MAS method, the sample tube is tilted at approximately 54.7 degrees (the magic angle) relative to the direction of the static magnetic field and rotated at high speed at frequencies ranging from several thousand to several tens of thousands of Hz in order to improve the resolution of the NMR spectrum and reduce anisotropic interactions.

[0003] Generally, sample tubes used in NMR measurements include a cylindrical body having an opening at one end and containing a sample therein, a lid that fits over the opening of the cylindrical body, and blades at the other end of the cylindrical body for rotating the sample tube. For example, the sample tube disclosed in Patent Document 1 further includes an insert that contains the sample and is fitted into the hollow portion of the cylindrical body.

[0004] Japanese Patent Application Publication No. 9-178829

[0005] Sample tubes used in NMR measurements are typically very small, with diameters of 4 mm, 3.2 mm, or 1 mm. Furthermore, the process of filling sample tubes with samples and gases is carried out in a glove box. A glove box is an airtight container designed to allow work to be performed in an environment isolated from the outside air, with only one arm allowed inside. Because sample tubes are small and delicate, filling the cylindrical body of the sample tube with gas and sample and fitting a lid onto the cylindrical body inside such a glove box is extremely difficult.

[0006] Furthermore, NMR measurements require filling the sample tube with gas, but in order to fill the sample tube with gas, the entire interior of the glove box must be filled with gas before the lid is fitted, which poses the problem that a large amount of gas is required even though the volume of the sample tube itself is small.

[0007] The present invention has been made in view of the above-mentioned problems, and has as its object to provide a sample tube lid mounting device that can properly fit a sample tube lid in an atmosphere with a small amount of gas.

[0008] To achieve the above object, the present invention includes the following subject matter.

[0009] Item 1: A lid attachment device for attaching a lid to the opening of a cylindrical sample tube body, comprising: a device main body having a sealed internal space; a lid holder that holds the lid within the internal space; a sample tube body holder that holds the sample tube body within the internal space; an observation window provided in the device main body for viewing the internal space from the outside; an inlet provided in the device main body for introducing gas into the internal space; and linear movement means provided on one of the sample tube body holder and the lid holder for moving one of the sample tube body holder and the lid holder relatively towards the other, wherein the lid attachment device moves the lid relative to the sample tube body within the internal space by the linear movement means, and the lid is attached to the sample tube body.

[0010] Item 2: The lid mounting device described in Item 1 further comprises a position adjustment means provided on the other of the sample tube body holder and the lid holder, which adjusts the position of the other of the sample tube body holder and the lid holder in the vertical and horizontal directions.

[0011] Item 3: The lid attachment device according to item 1 or 2, wherein the observation window is provided on at least one of the upper and lower sides of the device body and at least one of the left and right sides of the device body.

[0012] Item 4: The lid body holder comprises a holder main body portion and a lid body holding portion that is connected to one side of the holder main body portion by a ball joint so as to be able to swing freely, and an end face on one side of the lid body holding portion is a lid body mounting portion to which the lid body is attached. This is a lid body mounting device described in any one of Items 1 to 3.

[0013] Item 5: The lid attachment device according to any one of items 1 to 4, further comprising a holder provided within the sample tube body holder for holding the sample tube body.

[0014] Item 6: The lid attachment device according to Item 1, further comprising a heating device provided within the sample tube body holder.

[0015] According to the present invention, it is possible to provide a sample tube lid mounting device that can properly fit a sample tube lid in an atmosphere with a small amount of gas.

[0016] FIG. 1 is a plan view showing the overall schematic configuration of a lid mounting device according to one embodiment of the present invention. FIG. 2 is a plan view showing the schematic configuration of a linear feeder and a lid holder. FIG. 3 is a perspective view of a sample tube body holder. FIG. 4 is a cross-sectional view of a sample tube body holder. FIG. 5 is a perspective view of a holder. FIG. 6 is a cross-sectional view of a holder. (A) is a perspective view of another example of a holder, and (B) is an exploded perspective view of (A). FIG. 7 is a perspective view of a lid holder. FIG. 8 is a cross-sectional view of a lid holder. FIG. 9 is a plan view showing the internal space as seen through an upper observation window. FIG. 10 is a plan view showing the internal space as seen through an upper observation window. (A) is a perspective view and (B) is a cross-sectional view of a sample tube. FIG. 11 is a cross-sectional view showing another example of a sample tube body holder.

[0017] A lid attachment device 10 of this embodiment is used to attach lids 102 and 103 to a sample tube body 101 of a sample tube 100. The lid attachment device 10 is a lid attachment device for attaching lids 102 and 103 to a sample tube body 101 of a sample tube 100.

[0018] (Sample Tube 100) The sample tube 100 used in the lid attachment device 10 of this embodiment will now be described. As shown in Figures 12(A) and 12(B), the sample tube 100 comprises a cylindrical sample tube body 101 having openings 101a at both ends, and lids 102 and 103 that close the openings 101a. Each lid 102 and 103 comprises a cylindrical lid body 102b and 103b, respectively, and a cylindrical protrusion 102a and 103a that is provided on one end surface of the lid body 102b and 103b and has a smaller diameter than the lid body 102b and 103b. The protrusions 102a and 103a are fitted into the openings 101a at both ends of the sample tube body 101. The other side of the lid body 103b of one of the lids 103 further comprises a blade 103c for rotating the test tube 100 during NMR measurement. The test tube body 101 is also called a sleeve. The lid 103 having the blades 103c is also called a spinning cap, and the lid 102 having no blades 103c is also called a bottom cap.

[0019] When the lids 102 and 103 are fitted to the sample tube body 101, the axis Pa of the sample tube body 101 and the axis Pb of the lids 102 and 103 are on the same axis. By moving the lids 102 and 103 relatively toward the sample tube body 101, the outer surfaces of the protrusions 102a and 103b are pressed into the inner surface of the sample tube body 101 while sliding against it, and the lids 102 and 103 are fitted to the sample tube body 101.

[0020] The lid attachment device 10 of this embodiment allows the lids 102 and 103 to be press-fit into the respective openings 101a of the sample tube body 101. The sample tube 100 for which the lid attachment device 10 is used is, for example, a JEOL model with model number NM-05401ST1. With the lids 102 and 103 fitted to the sample tube body 101, the axial (longitudinal) length (total length) is approximately 6 mm, the outer diameter of the sample tube body 101 is approximately 1 mm, and the inner diameter is approximately 0.5 mm. The sample tube body 101 may be made of any material hard enough to withstand the force applied to the sample tube body 101 when fitting the lids 102 and 103. Examples of suitable materials include ceramic, preferably zirconia, which has a Mohs hardness of approximately 8 to 8.5 and a Vickers hardness (HV) of 11 to 13 GPa. The material forming the lids 102 and 103 is, for example, a synthetic resin such as polyimide resin, and may be the same material as that of the holder 70 described later.

[0021] However, the sample tube 100 is not limited to the embodiment shown in FIG. 12 , and any known sample tube suitable for NMR measurement can be used. For example, a sample tube 100 with a total length of 3.2 mm, 4 mm, or the like may be used. The caps 102 and 103 may also be cylindrical without the protrusions 102 a and 103 a. In this case, the outer surface of the cylinder slides against the inner surface of the sample tube body 101 while being pressed into place. The sample tube 100 may also be a screw tube. A screw tube has, for example, threads on the outer surface of the protrusions 102 a and 103 a of the caps 102 and 103, and a thread on the outer surface of the sample tube body 101 facing the opening 101 a. The threads rotate and engage with each other, allowing the caps 102 and 103 to fit together.

[0022] Furthermore, the test tube body 101 of the test tube 100 may be open on one side and closed on the other side. In this case, an opening 101a is formed on only one side, and either the lid 102 or the lid 103 is fitted into the opening 101a.

[0023] The sample to be subjected to fixed NMR measurement, that is, the sample filled in the sample tube 100, may be, for example, a porous material, a battery material, or a functional material such as a catalyst.

[0024] (Overall Configuration of Lid Attachment Device 10) As shown in Figure 1, the lid attachment device 10 comprises an apparatus main body 20 having a sealed internal space S (Figures 10 and 11), a lid holder 30 that holds a lid 102 within the internal space S, a sample tube body holder 40 that holds a sample tube body 101 within the internal space S, an XY stage 50 (position adjustment means) that holds the sample tube body holder 40, and a linear feeder 60 (linear movement means) that linearly moves the lid holder 30. The lid attachment device 10 is arranged in this order: the XY stage 50, the apparatus main body 20, a hollow extension tube 11 that connects the apparatus main body 20 and the linear feeder 60, and the linear feeder 60. The direction in which these components are arranged in this order is referred to as the longitudinal direction of the lid attachment device 10.

[0025] In the following description, the longitudinal direction of the lid attachment device 10 is also referred to as the Z direction. The front joint 21A, rear joint 21B, lid holder 30, and linear feedthrough 60 of the device main body 20 are arranged on the same axis P1 parallel to the longitudinal direction, and the movement direction of the lid holder 30 is parallel to the longitudinal direction. Along the longitudinal direction, the side on which the XY stage 50 is located across the device main body 20 is referred to as the front side, and the side on which the linear feedthrough 60 is located is referred to as the rear side. The direction perpendicular to the front-to-rear direction is referred to as the up-down direction or X direction, and the direction perpendicular to the up-down direction and the front-to-rear direction is referred to as the left-to-right direction or Y direction. In the following description, an example is described in which the lid 102 of the test tube 100 is fitted into the test tube body 101, but the lid 103 may also be fitted into the test tube body 101.

[0026] (Device Main Body 20) The device main body 20 is a hexagonal pipe having an internal space S and joints 21A to 21F provided in six directions, i.e., up, down, left, right, front, and rear. Of the two front and rear joints 21A and 21B along the length direction, an XY stage 50 is connected to the front joint 21A, and a linear feedthrough 60 is provided to the rear joint 21B via a hollow extension pipe 11. In this embodiment, a hexagonal pipe with model number ICF-34-6W manufactured by Kitano Seiki Co., Ltd. is used as the device main body 20.

[0027] Observation windows 22 are attached to at least one of the upper joint 21C or the lower joint 21D, and at least one of the right joint 21E or the left joint 21F. In this embodiment, two observation windows 22 are provided, one in the upper joint 21C and one in the right joint 21E. The operator can view the sample tube body 101 and the cover 102 disposed in the internal space S from the outside through the observation windows 22. The observation windows 22 are transparent windows made of glass, transparent synthetic resin, or the like, and are attached to the joints 21C and 21E in an airtight manner using O-rings or the like. The observation windows 22 may be attached to both the upper and lower joints 21C and 21D, or both the left and right joints 21F and 21E.

[0028] The left-side joint 21F functions as a gas inlet, and is connected to a gas supply pipe 12. A pressure gauge and a valve (not shown) are connected to the gas supply pipe 12, and gas is introduced from a gas supply source (not shown) through the gas supply pipe 12 into the internal space S. The gas inlet may be any of the joints 21A to 21F of the apparatus main body 20.

[0029] Gases used for fixed NMR measurements include, for example: １３ C isotope-substituted CO ２ , １３ C isotope-substituted CH4.

[0030] (XY stage 50) The XY stage 50 holds the sample tube main body holder 40 and moves the sample tube main body holder 40 in the vertical direction (X direction) or the horizontal direction (Y direction), adjusting the XY position of the sample tube main body holder 40 within the front joint 21A. In this embodiment, the XY stage 50 used is model KXY-34 manufactured by Kitano Seiki Co., Ltd., but is not limited to this.

[0031] 3 and 4, the sample tube body holder 40 comprises a cylindrical holder body 41 and a flange 42 provided on one side of the holder body 41. A screw hole 42a is provided in the flange 42, and the flange 42 is attached to the front side of the XY stage 50 with a screw, thereby supporting the sample tube body holder 40 on the XY stage 50.

[0032] A recess 41b with a circular cross section is formed in the end face at the rear end of the holder main body 41, and the holder 70 of the sample tube body 101 is fitted into the recess 41b. A threaded hole 41c that passes through to the recess 41b is provided in the outer peripheral surface of the rear end 41a of the holder main body 41, and the holder 70 is held in the recess 41b with a screw. Note that if the outer diameter of the holder 70 is set to be approximately the same as the inner diameter of the recess 41b and the holder 79 is fitted tightly into the recess 41b, the holder 70 will be firmly held in the recess 41b, and the threaded hole 41c and screw do not need to be provided. The cross section of the recess 41b is not limited to being circular, and may have any shape that can hold the holder 70 by abutting against it or by means of the threaded hole 41c and screw.

[0033] As shown in FIG. 13 , a heating device for heating the sample to a temperature suitable for measurement is provided inside the front end of the holder main body 41. The shape of the heating device is not particularly limited, but in this embodiment, a rod-shaped heater 43 is used as the heating device. The rod-shaped heater 43 is composed of a base 43a including a heating circuit and wiring, and a heater section 43b, which is a heat-generating section and has an outer diameter smaller than that of the base 43a, and is positioned so that the heater section 43b is located on the recess 41b side. The holder main body 41 is formed with a holder hollow 41d shaped to accommodate the rod-shaped heater 43. The holder hollow 41d is open at the front end surface, and the rod-shaped heater 43 can be inserted through the opening. The shape of the rod-shaped heater 43 is not limited to the above, and any existing rod-shaped heater may be used.

[0034] The holder main body 41 passes through the XY stage 50 and the front joint 21A of the device main body 20, and the tip (rear end) 41a of the holder main body 41 is located in the internal space S of the device main body 20. The sample tube main body holder 40 can be moved up and down and left and right by the XY stage 50. Figures 10 and 11 show the internal space S as seen from the upper observation window 22, with the rear end of the holder main body 41 of the sample tube main body holder 40 moving left and right.

[0035] (Holder 70 for Sample Tube Body 101) As shown in Figures 5 and 6, the holder 70 for the sample tube body 101 has a substantially cylindrical main body 74, which has a first hollow section 71 and a second hollow section 72 formed therein. The first hollow section 71 is located at one end (rear end) of the holder 70 and is open at one end face. The second hollow section 72 is continuous with the first hollow section 71 and has a larger inner diameter than the first hollow section 71, and is closed at the other end. The overall shape of the main body 74 is sufficient as long as it can be fitted into the recess 41b formed in the rear end face of the holder main body 41 and corresponds to the shape of the recess 41b. The cross-sectional shape of the recess 41b and the cross-sectional shape of the holder 70 may be any shape, such as circular, rectangular, or chamfered rectangular.

[0036] As shown in Figure 6, the first hollow section 71 holds the sample tube body 101. The first hollow section 71 has a circular cross section, and its diameter is set to be approximately the same as the diameter of the sample tube body 101. The sample tube body 101 is inserted into the first hollow section 71 through its opening. The sample tube body 101 is held in place by the inner surface of the first hollow section 71 abutting against the outer surface of the sample tube body 101. The sample tube body 101 is held in the first hollow section 71 so that its opening 101a protrudes slightly outward from one end of the holder 70, i.e., beyond the opening of the first hollow section 71.

[0037] Grooves 73 are provided around the circumference of the outer periphery of holder 70 at two locations along the length. Grooves 73 are used by an operator to grip holder 70 with tweezers, allowing the tip of the tweezers to engage with grooves 73 and grip holder 70 stably.

[0038] 7A and 7B, the main body 74 of the holder 70 may be composed of two identically shaped halves 70A and 70B. The halves 70A and 70B are formed by splitting the holder 70 in half along the length. When holding the sample tube body 101 in the first hollow portion 71, the sample tube body 101 is placed on the portion of one half 70A that forms the first hollow portion 71, and then the other half 70B is aligned with the first hollow portion 71. This allows the sample tube body 101 to be held in the first hollow portion 71 of the holder 70 without applying a force to push the sample tube body 101 through the opening of the first hollow portion 71, making the sample tube body 101 less likely to be damaged.

[0039] The holder 70 may be divided into multiple parts along its length. For example, it may be divided into a part including the first hollow section 71 and a part including the remaining portion. Furthermore, if the inner diameter of the first hollow section 71 is larger than the outer diameter of the sample tube body 101, and the inner surface of the first hollow section 71 cannot abut against the outer surface of the sample tube body 101, the holder 70 may be equipped with a spacer. In this case, the spacer is provided between the first hollow section 71 and the sample tube body 101, and the sample tube body 101 is held in the first hollow section 71 by the spacer.

[0040] The material of the holder 70 is not limited, and may be a metal such as aluminum or a synthetic resin (ABS resin, PLA resin, ASA resin, PP (polypropylene) resin, PET resin, etc.), but it is preferable that the holder 70 be made of a material with lower fracture toughness than the sample tube body 101 so as not to damage the sample tube body 101. For example, if the sample tube body 101 is made of zirconia, the material of the holder 70 should have a fracture toughness of approximately 15 MPa.m 1 / 2 It is preferable that the material of the holder 70 is smaller than 100°C. Furthermore, since the holder 70 may be heated by the rod-shaped heater 43 or the like, it is preferable that the material is heat-resistant and has a glass transition point of 150°C or higher. The material of the holder 70 is preferably, for example, super engineering plastic, such as polyamideimide or polyethersulfone. In this embodiment, Vespel (registered trademark), a polyimide resin from DuPont, is used.

[0041] When holder 70 is composed of multiple parts divided along the length direction, each part may be made of a different material. Also, when a spacer is provided, the spacer may be made of super engineering plastic, and the other parts of holder 70 may be made of metal such as aluminum or synthetic resin (ABS resin, PLA resin, ASA resin, PP (polypropylene) resin, PET resin, etc.).

[0042] When using a sample tube body 101 with a different outer diameter, if a holder 70 having a first hollow portion 71 with a diameter that matches the outer diameter of the sample tube body 101 is prepared, the same sample tube body holder 40 can be used and there is no need to replace the entire sample tube body holder 40.

[0043] The lid attachment device 10 may not be provided with the holder 70, and the sample tube body 101 may be held directly by the sample tube body holder 40. In this case, the sample tube body holder 40 may be provided with a clip or the like that can hold the sample tube body 101.

[0044] In addition, when the lid 102 is fitted to both ends of the test tube body 101 of the test tube 100, the lid 102 is fitted in advance to the other end of the test tube body 101. The lid 102 fitted to the other end is positioned in the second hollow portion 72, and the sample tube body 101 is held by the holder 70. This prevents deformation of the lid 102 due to the application of force to the lid 102 fitted to the other end when fitting the lid 102 to one end of the test tube body 101.

[0045] (Linear feedthrough 60) The linear feedthrough 60 holds the lid holder 30 and moves it longitudinally toward the sample tube body holder 40. The linear feedthrough 60 transmits linear motion from the atmosphere side into the sealed space, and as shown in FIG. 2, is composed of a drive unit 61 and a shaft 62 that protrudes from the drive unit 61 and can move forward or backward relative to the drive unit 61. The lid holder 30 is held at the tip of the shaft 62. The movable distance of the shaft 62 is approximately 25 mm. In this embodiment, the linear feedthrough 60 used is model KML-34 manufactured by Kitano Seiki Co., Ltd., but is not limited to this.

[0046] (Lid holder 30) As shown in Figures 8 and 9, the lid holder 30 comprises a cylindrical body portion 31 (holder main body portion) and a cylindrical lid holding portion 32 that is freely rotatably connected to the front side (one side) of the cylindrical body portion 31 by a ball joint 33.

[0047] A shaft recess 31a that is open at the rear end face is formed along the length at the rear end of the cylindrical body portion 31. The front end of the shaft 62 of the linear feedthrough 60 is inserted into the shaft recess 31a. The inner diameter of the shaft recess 31a and the outer diameter of the shaft 62 of the linear feedthrough 60 are set to be approximately the same, and the inner surface of the shaft recess 31a and the shaft 62 come into contact, and the shaft recess 31a and the shaft 62 are locked together by the frictional force acting therebetween.

[0048] As shown in FIG. 9 , a spherical protrusion 34 is provided at the center of the front end surface of the cylindrical body 31. A socket portion 32a having a circular cross section and a concave shape is formed at the center of the rear end surface of the lid body holder 32. The spherical protrusion 34 is slidably housed inside the socket portion 32a. When the spherical protrusion 34 is housed in the socket portion 32a, the inner surface of the socket portion 32a abuts against the surface of the spherical protrusion 34, and the spherical protrusion 34 is locked to the socket portion 32a by friction between the inner surface of the socket portion 32a and the surface of the spherical protrusion 34. A spherical body or spring may be provided at the bottom of the socket portion 32a, functioning as an elastic body between the apex of the spherical protrusion 34 and the socket portion 32a of the lid body holder 32. The spherical protrusion 34 and the socket portion 32a form a ball joint 33, and the lid body holder 32 is freely swingable relative to the cylindrical body 31 via the ball joint 33. In other words, the front end surface 32b of the lid holder 32 can be positioned parallel to a plane perpendicular to the length direction, and can also be positioned inclined relative to the plane perpendicular to the length direction.

[0049] A circumferential groove 32c is formed around the socket 32a, sandwiching the wall portion. The socket 32a and the groove 32c are formed concentrically. Due to the rigidity of the wall portion, the groove 32c functions as an elastic body.

[0050] The lid 102 of the sample tube 100 is attached to the center of the front end face 32b of the lid holder 32 using an attachment means (not shown) such as double-sided tape. That is, the front end face 32b functions as a lid attachment portion. A circle or the like may be provided in the center of the front end face 32b as a mark for attaching the lid 102 of the sample tube 100.

[0051] (Method of Using the Lid Mounting Device 10) The method of using the lid mounting device 10 will be described. First, preparations for mounting the lid are performed. The operator fits and locks the shaft 62 of the linear feedthrough 60 into the shaft recess 31a at the rear end of the lid holder 30. Then, double-sided tape is applied to the center of the front surface of the lid holding portion 32 of the lid holder 30, and the lid 102 of the sample tube 100 is attached to the double-sided tape. At this time, it is preferable to align the axis P2 of the lid holder 30 with the axis Pb of the lid 102. Next, the extension tube 11 is attached to the joint 21B on the rear side of the device main body 20, and the lid holder 30 is inserted from the rear end of the extension tube 11 toward the internal space S of the device main body 20, and the drive unit 61 of the linear feedthrough 60 is attached to the rear end of the extension tube 11.

[0052] Next, the sample tube body 101 filled with the sample to be measured is placed in the first hollow portion of the holder 70 for the sample tube body 101. At this time, the sample tube body 101 is placed so that the opening 101a of the sample tube body 101 protrudes from the holder 70. It is preferable that the axis Pa of the sample tube body 101 and the axis P3 of the holder 70 are aligned. Then, the holder 70 holding the sample tube body 101 is inserted into the recess 41b of the sample tube body holder 40, and the holder 70 is screwed in place. At this time, it is preferable that the holder 70 is held in the sample tube body holder 40 so that the axis P3 of the holder 70 and the axis P4 of the sample tube body holder 40 are aligned.

[0053] The XY stage 50 is attached to the joint 21A on the front side of the device main body 20. The holder body 41 of the sample tube main body holder 40 is inserted via the XY stage 50 toward the internal space S of the device main body 20, and the flange 42 of the sample tube main body holder 40 is screwed to the XY stage 50. A microscope (not shown) is attached to at least one of the observation windows 22. With the above preparation work, the internal space S of the device main body 20 is sealed. Note that microscopes may be attached to all of the multiple observation windows 22, or the operator may change microscopes each time they look into a different observation window 22. Alternatively, the positions of the cover 102 and the sample tube main body 101 may be adjusted visually from the observation window 22 without attaching a microscope to the observation window 22.

[0054] Next, the lid 102 is attached. First, the operator evacuates the internal space S of the device main body 20 and fills the internal space S with a predetermined gas. At this time, the sample tube body 101 may be heated by a heating device while being evacuated so that the sample reaches an appropriate temperature (e.g., 80 to 120 degrees) depending on the sample.

[0055] The operator then adjusts the position of the sample tube body 101 in the XY direction, i.e., its position on the XY plane, using the XY stage 50 to align it with the position on the XY plane of the lid 102. At this time, the operator adjusts the position of the sample tube body 101 in the Y direction by looking into the internal space S through the upper observation window 22, and adjusts the position of the sample tube body 101 in the X direction by looking into the internal space S through the right or left observation window 22.

[0056] When the axes Pa and P3 of the sample tube body 101 and the holder 70 are aligned, and the axes P3 and P4 of the holder 70 and the sample tube body holder 40 are aligned, the axis P4 of the sample tube body holder 40 is parallel to the longitudinal direction of the lid attachment device 10, i.e., the axis P2 of the device 10. Furthermore, the axis of the lid 102 attached to the front end face 32b of the lid holder 30 is assumed to be parallel to the longitudinal direction. In this case, by adjusting the position of the sample tube body holder 40 in the X and Y directions using the XY stage 50, the axis Pb of the lid 102 and the axis Pa of the sample tube body 101 are aligned. With the axis Pb of the lid 102 aligned with the axis Pa of the sample tube body 101, the lid holder 30 is moved forward using the linear feedthrough 60, and the lid 102 is fitted into the opening 101a of the sample tube body 101 without tilting ( FIG. 11 ). At this time, the inside of the sample tube body 101 is filled with the gas that fills the internal space S of the main body of the apparatus.

[0057] On the other hand, when the sample tube body 101 is held in the holder 70, the axis Pa of the sample tube body 101 may be obliquely misaligned with the axis P3 of the holder 70, or when the holder 70 is held in the sample tube body holder 40, the axis P3 of the holder 70 may be obliquely misaligned with the axis P4 of the sample tube body holder 40. Furthermore, the axis P2 of the lid holder 30 may be misaligned with the axis Pb of the lid 102, causing the lid 102 to be attached at an angle to the front end surface 32b of the lid holder 30. In this case, the axis Pb of the lid 102 and the axis Pa of the sample tube body 101 are not coaxial. If the lid holder 30 is moved forward in this state, the lid 102 will be inserted obliquely into the opening of the sample tube body 101, preventing the lid 102 from fitting properly. However, because the lid holder 30 on which the lid 102 is mounted is provided with a ball joint 33, when the lid 102 mounted on the lid holder 32 or the front end surface 32b of the lid holder 30 abuts against the sample tube body 101, the lid holder 32 swings, and the axes Pa and Pb of the sample tube body 101 and the lid 102 coincide with each other. As a result, the lid 102 fits into the sample tube body 101 without tilting.

[0058] According to the above embodiment, an observation window 22 is provided in the device main body 20, so that the operator can adjust the position of the sample tube body 101 and the lid 102 while visually checking them, and can easily perform the work of fitting the lid 102 onto the sample tube 100.

[0059] Furthermore, by providing observation windows 22 in at least two locations on the device main body 20 in different directions, light can be introduced into the internal space S of the device main body 20 from the observation window 22 on the side that the operator is not looking into, making it easier to see the positions of the lid body 102 and the sample body main body.

[0060] Furthermore, since gas is filled only in the internal space S of the device main body 20 and the lid 102 is fitted into the sample tube main body 101 in this internal space S, the lid 102 of the sample tube 100 can be fitted in a small amount of gas atmosphere.

[0061] Furthermore, even if there is a relative positional misalignment in the XY plane between the sample tube body 101 and the lid body 102 in the internal space S of the device main body 20, the position can be fine-tuned by providing an XY stage 50, which is a position adjustment means, and the positions of the sample tube body 101 and the lid body 102 on the XY plane can be aligned.

[0062] Furthermore, by providing the lid holding portion 32 of the lid holder 30 with a ball joint 33, even if the axis Pb of the lid 102 and the axis Pa of the sample tube body 101 do not coincide, the lid 102 can be fitted to the sample tube body 101 without tilting. This is because when the front end face of the lid 102 or the lid holder 30 provided on the lid holding portion 32 abuts against the sample tube body 101, the lid holding portion 32 swings due to the ball joint 33.

[0063] 1, the lid holder 30 is connected to the linear feeder 60, and the sample tube body holder 40 is connected to the XY stage 50, but the sample tube body holder 40 may be connected to the linear feeder 60, and the lid holder 30 may be connected to the XY stage 50. Even in this case, by adjusting the position of the lid holder 30 on the XY plane, the lid 102 can be fitted into the sample tube body 101 without tilting.

[0064] If the sample tube 100 is a screw tube in which the cover 102 is fitted to the sample tube body 101 while rotating, a linear / rotary feedthrough may be used instead of the linear feedthrough 60 .

[0065] Although one embodiment of the present invention has been described above, the present invention is not limited to the above embodiment, and various modifications are possible without departing from the spirit of the present invention. The dimensions, materials, shapes, and relative arrangements of components described as embodiments or shown in the drawings are merely illustrative examples and are not intended to limit the scope of the present invention. Expressions expressing the same state of things, such as "in a certain direction," "along a certain direction," "the same," "identical," "equal," and "homogeneous," not only refer to strict equality, but also to tolerances or differences to the extent that the same function is achieved. Expressions expressing triangular, rectangular, and circular shapes not only refer to shapes in the strict geometric sense, but also to shapes including irregularities, chamfers, etc., to the extent that the same effect is achieved. Expressions referring to one component as "comprising," "comprises," "equips," "includes," or "has" do not exclude the presence of other components. "Parallel" and "orthogonal" mean substantially "parallel" and "orthogonal," and include not only strict "parallel" and "orthogonal" states, but also include an error of several degrees. In addition, expressions such as "part" are sometimes used, such as "end part." For example, "end part" means a part with a certain range that includes the "end." The same applies to other expressions that include "part."

[0066] REFERENCE SIGNS LIST 10 Lid attachment device 20 Device main body 21A Front joint 21B Rear joint 21C Upper joint 21E Right joint 21F Left joint (gas inlet) 22 Observation window 30 Lid holder 33 (34, 32a) Ball joint 34 Spherical protrusion 40 Sample tube main body holder 41 Holder main body 42 Flange 50 XY stage (position adjustment means) 60 Linear feeder (linear movement means) 70 Holder 71 First hollow section 72 Second hollow section 100 Sample tube 101 Sample tube main body 102 Lid S Internal space

Claims

1. A lid attachment device for attaching a lid to the opening of a cylindrical sample tube body, comprising: a device main body having a sealed internal space; a lid holder that holds the lid within the internal space; a sample tube body holder that holds the sample tube body within the internal space; an observation window provided in the device main body for viewing the internal space from the outside; an inlet provided in the device main body for introducing gas into the internal space; and linear movement means provided on one of the sample tube body holder and the lid holder for moving one of the sample tube body holder and the lid holder relatively towards the other, wherein the lid attachment device moves the lid relative to the sample tube body within the internal space by the linear movement means, and the lid is attached to the sample tube body.

2. A lid mounting device as described in claim 1, further comprising a position adjustment means provided on the other of the sample tube body holder and the lid holder, for adjusting the position of the other of the sample tube body holder and the lid holder in the vertical and horizontal directions.

3. A lid mounting device according to claim 1, wherein the observation window is provided on at least one of the upper and lower sides of the device body and at least one of the left and right sides of the device body.

4. The lid body mounting device according to claim 1, wherein the lid body holder comprises a holder main body and a lid body holding part that is connected to one side of the holder main body by a ball joint so as to be able to swing freely, and the end face on one side of the lid body holding part is a lid body mounting part to which the lid body is attached.

5. The lid attachment device according to claim 1, further comprising a holder provided within said sample tube body holder for holding said sample tube body.

6. The lid attachment device according to claim 1, further comprising a heating device provided within said sample tube body holder.

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