JP5779963B2 - Observation sample sealed container - Google Patents

Description

  The present invention relates to an observation sample sealed container used for microscopic image observation of an observation sample observed in a sealed container.

When acquiring a Raman image using a Raman microscope while controlling the atmosphere around the sample, it is necessary to use an airtight container with an observation window formed of glass that looks through the sample chamber on the stage of the microscope. It is common. In such a sealed container, in order to seal the contact portion between the observation window material and the container body, thermocompression bonding, welding using a metal brazing material, a thermoplastic adhesive, or an O-ring is used. Sometimes.
For example, as an example of attaching an observation window material to a container body and applying thermocompression bonding to ensure hermeticity, there is the following Patent Document 1, which includes an observation window made of quartz with a seal ring interposed therebetween. A technique for thermocompression bonding a material to a container body is disclosed.
Moreover, there exists the following patent document 2 as an example using an O-ring. In this patent document, an observation window material is disposed between an annular flange and a center ring, and the outer peripheral end of the observation window material is sandwiched between the inner peripheral ends of the flange and the center ring. An O-ring is attached between the flange and the center ring, between the observation window member and the flange, and between the observation window member and the center ring.

JP 2001-214973 A JP 2002-66300 A

When sealing the contact portion between the observation window material and the container body using thermocompression bonding, welding using a metal brazing material or adhesion using a thermoplastic adhesive, the observation window material should be used when welding or drying the adhesive. There is a risk of distortion. Further, when an O-ring or the like is used, there is a high possibility that the observation window material is distorted by pressing the observation window material and the container body.
When a Raman microscope image is observed through the observation window material, the thickness of the observation window material is important. If the observation window material is too thick, the spatial resolution is lowered and the image is blurred. Therefore, it is desirable to use an observation window material having a thickness of 1 mm or less.

However, in the observation window material having a thickness of 1 mm or less, the distortion at the time of mounting on the container body described above may occur more greatly. When a Raman microscope image is acquired using a distorted observation window material, there is a problem that the light condensing property on the sample surface is deteriorated and a good Raman image cannot be obtained.
The present invention has been made in view of such circumstances, and provides an inexpensive observation sample sealed container that can eliminate or reduce distortion of an observation window material and can obtain a good Raman image. With the goal.

In order to achieve the above object, an observation sample sealed container according to the present invention includes a flat observation container main body in which a first recess is formed at the center and a second recess is formed at the bottom of the first recess. An observation window member for forming a sample chamber in the second recess and a through-hole for allowing the sample chamber to be seen in the central portion by being accommodated in the first recess and covering the upper portion of the second recess. In the observation sample sealed container comprising a lid member that covers an outer peripheral side end of the observation window member and an outer peripheral side surface of the observation container main body, either one of the surfaces on which the observation container main body and the lid member are in contact with each other Forming a first annular groove on the surface, forming a second annular groove on the surface of the lid member in contact with the observation window material, attaching a first O-ring to the first annular groove, A second O-ring is attached to the second annular groove, and the lid member is overlaid on the observation container body. The between the lid member and the observation container body is sealed by said first O- ring, and between the lid member and the observation window material to seal by said second O- ring, wherein The pressing force applied to the second O-ring at the time of sealing was made smaller than the pressing force applied to the first O-ring .
In the observation sample sealed container, the depth of the second annular groove is made deeper than the depth of the first annular groove, and the pressing force applied to the second O-ring during the sealing is may be small Kusuru so than the pressing force loaded on first O- ring.
In the observation sample sealed container, the thickness of the observation window material may be 1 mm or less.
A tapered surface can be formed in which the through hole of the lid member of the observation sample sealed container is reduced in diameter toward the sample chamber.
With respect to the area where the observation window material and the bottom of the first recess come into contact with each other in the state where the observation window material of the observation sample sealed container is accommodated in the first recess, the area of the observation window material It is preferable to make it 75% or more.

In the observation sample sealed container of the present invention, the pressing force applied to the second O-ring at the time of sealing is made smaller than the pressing force applied to the first O-ring. Since a large load is not applied to the observation window member by the ring, the distortion of the observation window member can be reduced, and the thickness of the observation window member can be reduced to 1 mm or less. As a result, when the observation sample sealed container is used for a Raman microscope, a high-magnification objective lens with a short working distance can be used, and a Raman image with high spatial resolution can be obtained. The light can be correctly collected, and a good Raman image can be obtained.
The hermeticity of the sample chamber is good, and the atmosphere of the sample chamber can be maintained in the initial state for a long time.

It is sectional drawing which cut | disconnected the observation sample airtight container by embodiment of this invention to the up-down direction. It is a disassembled perspective view of the observation sample airtight container by embodiment of this invention. It is the perspective view which looked at the cover member of the observation sample airtight container of FIG. 1 from the downward direction. It is the perspective view which looked at the container main body of the observation sample airtight container of FIG. 1 from the downward direction. FIG. 2 is an exploded cross-sectional view of the observation sample sealed container of FIG. 1 cut in a vertical direction.

Hereinafter, an observation sample sealed container according to an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a cross-sectional view of the observation sample sealed container cut in the vertical direction. 2 is an exploded perspective view of the observation sample sealed container, FIG. 3 is a perspective view of the lid member of the observation sample sealed container as viewed from below, and FIG. 4 is a perspective view of the container body of the observation sample container as viewed from below. FIG. 4 is an exploded cross-sectional view of the observation sample container cut in the vertical direction.
With reference to FIGS. 1 and 2, the observation sample sealed container 1 according to the present embodiment is used for Raman microscope observation, and includes a container body 2, a lid member 3, an observation window material 4, O-rings 5 and 6, and a stopper. Tools 7-9 are provided.
The bolt 7, the wing nut 8 and the washer 9 are collectively referred to as fasteners 7-9.

The container body 2 has a substantially disk shape, and a first recess 11 that is recessed toward the bottom surface (lower surface) 18 is formed at the center of the surface (upper surface) 17. The first recess 11 is a cylindrical space composed of a peripheral wall and a bottom, and a second recess 12 that is recessed toward the bottom surface 18 of the container body 2 is formed at the center of the bottom of the first recess 11. The second recess 12 is also a cylindrical space composed of a peripheral wall and a bottom. The first and second recesses 11 and 12 are formed to be concentric with the container body 2.
The size of the first recess 11 and the second recess 12 (area of the bottom surface) is preferably such that the first recess 11 has an area of 75% or more. The reason will be described later.
Between the 1st recessed part 11 and the outer periphery of the container main body 2, the annular | circular shaped 1st annular groove 13 dented to the bottom face 18 side is formed in the surface 17 of the container main body 2. As shown in FIG. The first annular groove 13 has a quadrangular cross section.

  With reference to FIGS. 3 to 5, an attachment hole 19 that penetrates the container body 2 vertically is formed between the first annular groove 13 and the outer peripheral edge of the container body 2. The mounting hole 19 has a counterbore hole (large diameter hole) 20 that accommodates the head of the bolt 7 on the bottom surface 18 side of the container body 2, and a small diameter hole 21 through which the shaft portion of the bolt 7 is inserted on the surface 17 side. Is forming. The small diameter hole 21 is formed with a female screw that is screwed onto the shaft portion of the bolt 7. In this embodiment, three mounting holes 19 are formed at intervals of 120 degrees in the circumferential direction.

Referring back to FIGS. 1 and 2, the lid member 3 has a substantially disk shape, and a through hole 23 is formed in the center. The through hole 23 is reduced in diameter toward the bottom surface (lower surface) 26 side of the lid member 3. A tapered surface 24 is formed. In addition, a circular step surface 22 that is slightly recessed toward the surface 25 is formed on the bottom surface 26 so as to surround the through hole 23 (see FIG. 3). On the stepped surface 22, an annular second annular groove 14 is formed outside the through-hole 23 and is recessed toward the bottom surface 26 side on the surface (upper surface) 25 side of the lid member 3. The second annular groove 14 has a quadrangular cross section. On the outer peripheral side of the lid member 3, an attachment hole 29 penetrating the lid member 3 up and down is formed between the second annular groove 14 and the outer peripheral edge of the lid member 3.
The step surface 22 may be omitted, and the second annular groove 14 may be formed directly on the bottom surface 26 of the lid member 3.
The attachment holes 29 are formed at positions corresponding to the attachment holes 19 of the container main body 2, and are formed at three locations at intervals of 120 degrees in the circumferential direction, similarly to the attachment holes 19.
The container main body 2 and the lid member 3 are made of a metal material having a heat insulating effect and are formed of SUS304 in the present embodiment, but stainless steel, aluminum, or the like can be used.

The observation window member 4 has a disk shape, has a thickness of 1 mm or less, and has a diameter slightly smaller than the diameter of the first recess 11. The depth of the first recess 11 is formed to be substantially the same as the thickness of the observation window member 4, and when the observation window member 4 is accommodated in the first recess 11, the surface of the observation window member 4 and the container body The two surfaces 17 are preferably flush with each other. Although the thickness of the observation window member 4 is as thin as 1 mm, it is made thicker in the drawing for easy viewing.
As the observation window material, it is preferable to use a material such as quartz, calcium fluoride, and sapphire that emits less light when irradiated with an excitation laser used for Raman measurement. When the intensity of Raman scattering from the sample is sufficiently large, a normal glass material can be used.

  The first O-ring 5 is formed so that the diameter of the ring (hereinafter referred to as the ring diameter) corresponds to the diameter of the first annular groove 13 so as to be attached to the first annular groove 13. The second O-ring 6 is formed so that the ring diameter corresponds to the diameter of the second annular groove 14 so as to be attached to the second annular groove 14. Therefore, the ring diameter of the first O-ring 5 is larger than that of the second O-ring 6. In this embodiment, the O-rings 5 and 6 have the same shaft (cross-sectional) diameter. Materials for the O-rings 5 and 6 are made of silicon rubber, natural rubber, Viton, Teflon (registered trademark), or the like.

Referring to FIG. 5, the depth t1 from the surface 17 of the first annular groove 13 and the depth t2 from the bottom surface 26 of the second annular groove 14 are the first annular groove 13 in this embodiment. The second annular groove 14 is formed to be deeper than that. That is, the relationship of t1> t2 is established. Therefore, when the O-rings 5 and 6 are attached to the first and second annular grooves 13 and 14, respectively, the height at which the first O-ring 5 protrudes from the surface 17 of the container body 2 is the second height. The O-ring 6 is larger than the height protruding from the bottom surface 26 of the lid member 3.
The position where the first annular groove 13 is formed, in other words, the position where the O-ring 5 is mounted is outside the first recess 11 and is between the surface 17 of the container body 2 and the bottom surface of the lid member 3. Seal the gap. The position where the second annular groove 14 is formed, in other words, the position where the O-ring 6 is mounted is outside the through-hole 23 and inside the outer peripheral portion of the observation window member 4, and the step surface of the lid member 3. The space between 22 and the observation window material 4 is sealed. When the step surface 22 is omitted, the space between the bottom surface 26 and the observation window material 4 is sealed.
A sample stage 31 is disposed in the sample chamber 30. The sample table 31 has a cylindrical shape, and several types of stainless steel sample tables 31 having different thicknesses are prepared. The sample stage 31 is used while being appropriately exchanged depending on the size of the sample 32, and the distance between the surface of the sample 32 and the bottom surface (lower surface) of the observation window member 4 is preferably adjusted within 1 mm.

To assemble the observation sample sealed container 1, as an example, the first O-ring 5 is attached to the first annular groove 13 of the container body 2, and the observation window member 4 is accommodated in the first recess 11. Then, after mounting the second O-ring 6 in the second annular groove 14 of the lid member 3, the lid member 3 is overlapped on the container body 2. At this time, the positions of the mounting holes 19 and 29 of the container body 2 and the lid member 3 are matched. In this state, the height at which the first O-ring 5 protrudes from the surface 17 of the container body 2 is larger than the height at which the second O-ring 6 protrudes from the back surface of the lid member 3. The O-ring 5 is relatively abutted against the bottom surface 26 of the lid member 3, but the second O-ring 6 is not in contact with the observation member 4, or is only slightly abutted even when contacted.
In addition, since the internal thread is formed in the small diameter hole 21 of the mounting hole 19 of the container main body 2, if the bolt 7 is attached to the small diameter hole 21 in advance, the operation becomes easy. By setting the bolt 7 in the mounting holes 19 and 29, the shaft of the bolt 7 protrudes from the mounting hole 29 of the lid member 3, so that the washer 9 is inserted into the bolt shaft and each wing nut 8 is tightened. The observation sample sealed container 1 is assembled.
In addition, the bolt 7 and the wing nut 8 are used to assemble the container body 2 and the lid member 3, but other methods such as sandwiching the bottom surface 18 of the container body 2 and the surface 25 of the lid member 3 may be used. Good.

The observation sample sealed container 1 in the present embodiment has the following operational effects.
The first O-ring 5 seals between the surface 17 of the container body 2 and the bottom surface of the lid member 3, blocks air from entering from the outer periphery of the container body 2 and the lid member 3, and the second O- The ring 6 seals the gap between the stepped surface 22 of the lid member 3 and the observation window member 4 and blocks air from entering from the through hole 23 side. In this way, the inside of the sample chamber 30 can be sealed.
As described above, the length of the first O-ring 5 protruding from the surface 17 of the container body 2 is larger than the length of the second O-ring 6 protruding from the bottom surface 26 of the lid member 3. The first O-ring 5 is loaded with a relatively large pressing force on the bottom surface 26 of the lid member 3, while the second O-ring 6 is loaded with a relatively small pressing force to the extent that the sealing performance is not affected. Only. Therefore, the sealing of the sample chamber 30 is ensured, and distortion can be prevented without applying a large pressing force to the observation window material 4.
The first O-ring 5 may be disposed between the observation window member 4 and the bottom surface of the first recess 11, but the first O-ring 5 is the surface 17 of the container body 2. Since the first O-ring 5 is made in non-contact with the observation window member 4 so as to seal between the bottom of the lid member 3 and the load, the load on the observation window member 4 is reduced.

In the observation sample sealed container 1 according to the present embodiment, for example, when a sample is placed in a glove box with a low dew point and the sealing operation is performed, the atmosphere environment in the sample chamber 30 is maintained even after being taken out to the air environment. It is possible to hold for a certain time. It was confirmed that the sample chamber 30 was sealed in an environment with a dew point of −70 ° C., and the dew point of −70 ° C. was maintained for 1 hour after exposure to the atmosphere.
Since the first annular groove 13 is shallower than the second annular groove 14, each O-ring at the time of assembly depends on the difference in depth between the first and second annular grooves 13, 14. A distortion factor of 5 or 6 is appropriate. By the strain rate of the O-ring 6 installed between the observation window member 4 and the lid member 3 being smaller than the strain rate of the O-ring 5 installed between the lid member 3 and the container body 2. Even if the thickness of the observation window member 4 is 1 mm or less, the sample chamber 30 can be sealed without distorting the observation window member 4.
In addition, since conventional heat treatment such as welding is not required, the strain can be maintained in an appropriate range, and various optical window materials can be used.

As described above, the observation window member 4 is in contact with the bottom surface of the first recess 11 at an area that is 75% or more of the area of the observation window member 4 and does not include packings. It becomes easy to make the front (upper) surface of the material 4 parallel to the front (upper) surface of the sample table 31. Further, by increasing the contact area, it is possible to avoid stress concentration at the time of tightening the stoppers 7 to 9 and to keep the observation window member 4 surface parallel to the container body 2 without distorting the observation window member 4. .
When the liquid with high reactivity is put into the sample chamber 30 by denting the first recess 11 toward the bottom surface 18 side, even if the liquid overflows outside the sample chamber 30, the first recess 11 As a result, the liquid does not easily reach the first and second O-rings 5 and 6, and the O-rings 5 and 6 react with the liquid to make it difficult to damage the O-rings 5 and 6.
The through-hole 23 of the container lid 2 has a tapered structure that decreases in diameter toward the sample chamber 30 side. Since the microscope objective lens is often tapered at the tip, the tapered lens structure allows the objective lens to be inserted into the through-hole 23 and closer to the sample surface, and the high-power objective with a short working distance. It can also be used with lenses.

By installing several types of stainless steel cylindrical sample stands 31 having different thicknesses on the bottom surface of the sample chamber 30, the distance between the bottom surface of the observation window member 4 and the surface of the sample 32 is 1 mm or less depending on the thickness of the sample. Can be. In this way, by using the sample stage 31 to set the distance between the bottom surface of the observation window member 4 and the surface of the sample 32 to 1 mm or less, it becomes possible to use a high-power objective lens with a short working distance and high spatial resolution. A Raman image can be acquired.
The bottom surface 18 of the container body 2 has a counterbore 20 for attaching the bolt 7. The counterbore 20 improves the stability of the bolt 7, and the head of the bolt 7 is accommodated in the counterbore 20, so that the bolt 7 does not protrude from the bottom 18. It contacts the surface of the microscope stage 34. By adopting such a structure, the observation window member 4 is not distorted, and the surface, bottom surface, sample table surface, bottom surface 18 of the container body 2 and the surface of the microscope stage 34 are kept parallel to each other. Can be collected more correctly on the sample surface, and a good Raman image can be obtained.

The present invention has been described in detail based on the embodiments with reference to the accompanying drawings. However, the present invention is not limited to the above-described embodiments, and other modifications can be made without departing from the scope of the present invention. Or it can be changed.
For example, in the above embodiment, the shaft diameters of the O-rings 5 and 6 are the same, and the depths of the first annular groove 13 and the second annular groove 14 are changed to load the second O-ring 6. For example, the first and second O-rings have the same shaft diameter, and the first annular groove and the second annular groove have the same depth. The pressing force applied to the second O-ring may be reduced by making the hardness of the material of the O-ring softer than that of the first O-ring.
Further, the first and second O-rings are made of the same material, and the first annular groove and the second annular groove have the same depth, and the shaft diameter of the second O-ring is changed to the first O-ring. The pressing force applied to the second O-ring may be reduced by making it smaller than the shaft diameter of the ring. However, in any case, the airtight action of the second O-ring is maintained.
In the above embodiment, the first annular groove 13 is formed on the surface 17 of the container body 2, but may be formed on the bottom surface 26 of the lid member 3.
Moreover, although the said embodiment demonstrated as an observation sample sealed container for Raman microscopes, you may use it as an observation sample sealed container of another microscope.

DESCRIPTION OF SYMBOLS 1 Observation sample sealed container 2 Container main body 3 Lid member 4 Observation window material 5 1st O-ring 6 2nd O-ring 11 1st recessed part 12 2nd recessed part 13 1st annular groove 14 2nd annular Groove 17, 25 Surface 18, 26 Bottom 23 Through-hole 24 Tapered surface 30 Sample chamber 31 Sample stage 32 Sample

Claims (5)

A flat observation container body in which a first recess is formed at the center and a second recess is formed at the bottom of the first recess;
An observation window material that forms a sample chamber in the second recess by being housed in the first recess and covering the top of the second recess;
In the observation sample sealed container provided with a lid member covering the outer peripheral side end of the observation window member and the outer peripheral side surface of the observation container body, forming a through hole through which the sample chamber can be seen in the center part,
Forming a first annular groove on any one of the surfaces of the observation container body and the lid member contacting each other, forming a second annular groove on the surface of the lid member contacting the observation window member, Mounting a first O-ring in the first annular groove, mounting a second O-ring in the second annular groove;
The lid member is overlaid on the observation container main body, the gap between the lid member and the observation container main body is sealed with the first O-ring, and the gap between the observation window member and the lid member is the first. The observation sample is sealed with two O-rings, and the pressing force applied to the second O-ring at the time of sealing is made smaller than the pressing force applied to the first O-ring. Airtight container. The depth of the second annular groove is made deeper than the depth of the first annular groove, and the pressing force applied to the second O-ring during the sealing is applied to the first O-ring. observation sample sealed container according to claim 1 which is a small Kusuru so than the pressing force of the load.   The observation sample sealed container according to claim 1 or 2, wherein the observation window member has a thickness of 1 mm or less.   The observation sample sealed container according to any one of claims 1 to 3, wherein a through hole of the lid member forms a tapered surface whose diameter decreases toward the sample chamber.   The area where the observation window member and the bottom of the first recess contact with each other in a state where the observation window member is accommodated in the first recess is 75% or more of the area of the observation window member. Item 5. The observation sample sealed container according to any one of Items 1 to 4.

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