JP7238695B2 - Mirror for observing inside of device, method for preparing analysis sample, and method for observing sample - Google Patents

Description

TECHNICAL FIELD The present invention relates to a mirror for observation inside an apparatus, a method for preparing an analysis sample, and a method for observing a sample.

When performing chemical analysis or observation with an electron microscope, a sample may be preprocessed into a form suitable for the analysis method or observation method. For example, since a powder sample cannot be used for analysis or observation as it is, it is made into a resin-embedded sample for analysis or observation. The resin-embedded sample is prepared by injecting resin into a container for resin-embedded sample preparation in which the powder sample is placed, performing defoaming treatment by vacuuming, and heating at a predetermined temperature for a predetermined time (for example, 12 hours). It is produced by curing the resin by (See Patent Documents 1 and 2, for example).

JP 2016-50918 A JP 2013-167525 A

By the way, in sample processing, it is important to grasp the state of the sample during processing. For example, when preparing a resin-embedded sample, the resin is dried in a processing device such as a vacuum dryer. Poor impregnation of the resin into the powder sample may occur due to volatilization or insufficient pressure reduction in the atmosphere. Therefore, it is important to carefully perform heating and depressurization while checking the state of the sample.

To confirm the state of the sample, for example, it is conceivable to observe the sample through a window provided on the opening/closing door of the processing apparatus. However, since the size of the window is generally small, it is difficult to grasp in detail the state of the sample stored in a container such as a vat from the outside of the processing apparatus.

SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a technique for easily observing the state of a sample being processed in a processing apparatus from the outside.

A first aspect of the present invention is
a pedestal member;
a mirror member fixed to the base member so as to be inclined with respect to a horizontal plane;
When placed in a processing apparatus having a processing space in which the front side is open and a sample is accommodated and processed, at least a A mirror for observing the inside of a device is provided which can bridge between a pair of guide rails and can adjust the position of the pair of guide rails in the depth direction.

A second aspect of the present invention is, in the first aspect,
The angle of inclination of the mirror surface member with respect to the horizontal plane is within a range of ±10° around 45°.

A third aspect of the present invention is, in the first or second aspect,
The processing equipment is a vacuum dryer or a decompressor.

A fourth aspect of the present invention is, in the first to third aspects,
The mirror member is a SUS mirror-polished plate.

A fifth aspect of the present invention is, in the first to fourth aspects,
The base member is a metal square bar.

A sixth aspect of the present invention is, in the first to fifth aspects,
The mirror surface member is screwed to the base member.

A seventh aspect of the present invention is, in the first to sixth aspects,
A protective film is provided on the surface of the mirror surface member.

An eighth aspect of the present invention is
A method of processing a sample to produce an analytical sample, comprising:
A main body portion having an opening on the front side and having a processing space in which a sample is stored and processed, an opening/closing door for opening and closing the opening of the main body portion, and a depth toward the back wall on each of the left and right side walls inside the main body portion. a step of preparing a processing apparatus comprising at least one pair of guide rails provided extending in a direction and an observation window provided in the open/close door;
A pedestal member and a mirror surface member fixed to the pedestal member so as to be inclined with respect to a horizontal plane, capable of bridging between the pair of guide rails, wherein the depth in the pair of guide rails A step of preparing a mirror for observing the inside of the device, the position of which can be adjusted in a direction;
placing the sample in the processing space;
The apparatus interior observation mirror is arranged above the sample by bridging between the pair of guide rails, and its position is changed according to the position of the sample within the processing apparatus. adjusting the guide rail in the depth direction;
and processing the sample,
A method for preparing an analysis sample is provided, wherein, in the step of processing the sample, an image of the sample viewed from above, which is reflected on the mirror surface member during processing, is observed from outside the processing apparatus through the observation window. be done.

A ninth aspect of the present invention is
A method for observing the state of a sample placed in a processing apparatus, comprising:
A main body portion having an opening on the front side and having a processing space in which a sample is stored and processed, an opening/closing door for opening and closing the opening of the main body portion, and a depth toward the back wall on each of the left and right side walls inside the main body portion. a step of preparing a processing apparatus comprising at least one pair of guide rails provided extending in a direction and an observation window provided in the open/close door;
a pedestal member and a mirror surface member fixed to the pedestal member so as to be inclined with respect to a horizontal plane, the pedestal member being capable of bridging between the pair of guide rails in the processing apparatus; a step of preparing a mirror for observing the inside of the device, the position of which can be adjusted in the depth direction on the pair of guide rails;
placing the sample in the processing space;
The apparatus interior observation mirror is arranged above the sample by bridging between the pair of guide rails, and its position is changed according to the position of the sample within the processing apparatus. adjusting the guide rail in the depth direction;
Observing an image of the sample viewed from above, which is reflected on the mirror surface member, from outside the processing apparatus through the observation window.

According to the present invention, it is possible to easily observe the state of the sample being processed in the processing apparatus from the outside.

FIG. 1 is a perspective view of an apparatus internal observation mirror according to an embodiment of the present invention. FIG. 2 is a schematic cross-sectional view of an in-apparatus observation mirror according to an embodiment of the present invention. FIG. 3 is a diagram for explaining a case in which a mirror for observing the inside of the apparatus is installed, and is a cross-sectional view of the processing space. FIG. 4 is a diagram for explaining a case where the mirror for observing the inside of the apparatus is installed, and is a front view when viewed from the front side. FIG. 5 is a front view of the processing apparatus as seen from the front side.

<One embodiment of the present invention>
An embodiment of the present invention will be described below. In the following, first, the schematic configuration of the processing apparatus will be described, and then the mirror for observing the inside of the apparatus according to the present embodiment and the method of preparing an analysis sample using the same will be described with reference to the drawings.

FIG. 1 is a perspective view of an apparatus internal observation mirror according to an embodiment of the present invention. FIG. 2 is a schematic cross-sectional view of an in-apparatus observation mirror according to an embodiment of the present invention. FIG. 3 is a diagram for explaining a case where a mirror for observing the inside of the apparatus is installed, and is a cross-sectional view of the processing apparatus. FIG. 4 is a diagram for explaining a case where the mirror for observing the inside of the apparatus is installed, and is a front view when viewed from the front side. FIG. 5 is a front view of the processing apparatus as seen from the front side, showing a state in which the opening/closing door is opened to open the processing space. In this specification, as shown in FIGS. 3 to 5, the horizontal direction is indicated by XX', the vertical direction by YY', and the front-to-rear direction (depth direction) by ZZ'.

(Processing device)
First, a schematic configuration of a processing apparatus using the in-apparatus observation mirror of the present embodiment will be described.

The processing apparatus 100 includes a main body 110, an opening/closing door 120, a pair of guide rails 130, 130, and an observation window 140, as shown in FIG. The main body part 110 has a processing space 111 which is open on the front side and accommodates and processes a sample. The body part 110 is provided with an opening/closing door 120 for opening and closing the opening of the main body part 110 to seal the processing space 111 . At least one pair of guide rails 130, 130 extending in the depth direction toward the back wall 110b is provided on the left and right side walls 110a inside the body portion 110. As shown in FIG. The pair of guide rails 130, 130 are provided to support, for example, a shelf member, and are arranged at the same predetermined height from the bottom surface inside the main body 110 to support the shelf member horizontally. is configured as The opening/closing door 120 is provided with an observation window 140 for observing the processing space 111 from the outside of the processing apparatus 100 .

The processing apparatus 100 is not particularly limited, but includes, for example, a vacuum dryer and a decompressor. In the vacuum dryer and the decompressor, heating means (not shown) and pressure reducing means (not shown) are connected to the main body 110 so as to heat and reduce the pressure in the processing space 111 .

When a sample is processed by the processing apparatus 100, the sample is introduced into the processing space 111 and placed inside the main body 110, and the processing is performed with the opening/closing door 120 closed and the processing space 111 sealed. During this process, the sample in the processing space 111 is observed through the observation window 140 . However, the size of the observation window 140 is small, and it may be difficult to grasp the state of the sample in detail. In general, the sample is housed in the container 20 and placed in the processing space 111 as shown in FIG. may not be observable.

(mirror for observing inside the device)
In this embodiment, the apparatus internal observation mirror 10 shown in FIGS. 1 and 2 is used in order to easily observe the state of the sample in the sealed processing space 111 from the outside.

As shown in FIG. 1, the apparatus interior observation mirror 10 of the present embodiment includes a base member 11 and a mirror surface member 12 fixed to the base member 11 while being inclined with respect to a horizontal plane.

The pedestal member 11 is an elongated rod-like member having a length capable of bridging between the pair of guide rails 130 , 130 . The length is not particularly limited, and may be changed as appropriate according to the distance between the pair of guide rails 130,130. From the viewpoint of stably fixing the mirror surface member 12, the base member 11 preferably has a weight that prevents the tilted and fixed mirror surface member 12 from falling over, and preferably has a rectangular cross section. It preferably consists of a square bar. Further, by forming the base member 11 from metal, corrosion during processing can be suppressed. The width and thickness of the pedestal member 11 can be appropriately changed according to the size of the processing space 111, but it is preferable to have a size that allows the position of the inside observation mirror 10 to be freely adjusted in the depth direction of the guide rail 130. . Note that the width of the base member 11 indicates the size in the horizontal direction in FIG. 2, and the thickness indicates the size in the vertical direction.

The base member 11 has a trapezoidal cross section from the viewpoint of tilting and fixing the mirror surface member 12, and is inclined so that the width becomes narrower from the top surface to the bottom surface. is preferred. The angle of the inclined surface 11a may be appropriately changed according to the angle at which the mirror surface member 12 is inclined. 1 and 2 illustrate the case where the base member 11 has one inclined surface 11a on one long side, another inclined surface with a different angle of inclination is provided on the other long side. may have. Thereby, the angle of the mirror surface member can be changed by one base member. For example, by forming slanted surfaces with different angles such that one slanted surface is 45° and the other slanted surface is 60°, the mirror surface member 12 can be tilted according to the angle at which the mirror surface member 12 is tilted. You can choose an inclined surface to attach the

The mirror surface member 12 is fixed to the base member 11 so as to be inclined with respect to the horizontal plane. Specifically, the mirror surface member 12 is fixed to the inclined surface 11a on the long side of the base member 11, and is fixed in a state of being inclined with respect to the horizontal plane. The mirror surface member 12 mirrors the sample placed in the processing space 111 of the processing apparatus 100 so that the sample can be observed from the outside. The tilt angle of the mirror surface member 12 is not particularly limited as long as the image 30 of the sample viewed from above can be observed from the outside of the processing apparatus 100 through the observation window 140 . From the viewpoint of making the sample observable more reliably, the inclination angle of the mirror surface member 12 with respect to the horizontal plane is preferably within a range of ±10° around 45°.

As the mirror member 12, when the processing apparatus 100 is a vacuum dryer or a decompressor, it is preferable to use a mirror-polished plate made of SUS. A mirror-polished SUS plate can suppress corrosion and breakage even when the processing space 111 is heated or decompressed, so that the sample can be observed.

Fixation of the mirror surface member 12 to the pedestal member 11 is not particularly limited, but is preferably fixed with a screw 13 as shown in FIG. Fixing the mirror surface member 12 with the screws 13 facilitates attachment and detachment of the mirror surface member 12 to and from the base member 11 , thereby improving work efficiency such as cleaning the mirror surface member 12 .

As shown in FIG. 4, the specular member 12 is preferably provided with a protective film 14 on its inclined surface 11a. The protective film 14 protects the mirror member 12 by covering the surface of the mirror member 12 , especially the inclined surface 11 a facing the container 20 . The protective film 14 is detachable and can be replaced as required. In the processing apparatus 100 , for example, when the mixture 21 of the powder sample and the liquid resin is dried in a vacuum, the mixture 21 may scatter due to foaming and adhere to the mirror surface member 12 . The adhering mixture 21 is hard to remove because it is fixed by drying. In this respect, by providing the protective film 14 on the surface of the mirror surface member 12 , the mixture 21 can be prevented from directly adhering to the mirror surface member 12 . Moreover, when a solid matter adheres to the protective film 14, the solid matter can be easily removed by removing and replacing it.

The area covered with the protective film 14 on the mirror surface member 12 may be a partial area where the container 20 is reflected as shown in FIG. 4, or may be the entire surface of the inclined surface 11a.

The material of the protective film 14 is not particularly limited as long as it is transparent and does not easily deteriorate at high temperature or in a vacuum. As the protective film 14, for example, a stretch film or the like can be used.

(Method for preparing analysis sample)
Next, a method for preparing an analysis sample using the in-apparatus observation mirror 10 will be described. The manufacturing method of this embodiment includes a sample observation method. In the present embodiment, a case will be described in which a powder sample as a sample is impregnated with resin, and a resin-embedded sample in which the powder sample is embedded in resin is prepared as an analysis sample.

First, a powder sample is prepared as a sample. This powder sample is mixed with a liquid resin, and the mixture 21 is placed in a heat-resistant container 20 .

Subsequently, as shown in FIGS. 3 and 4, the container 20 containing the mixture 21 is introduced into the processing space 111 of the processing apparatus 100 and placed in the center of the main body 110 .

1 and 2 is introduced into the processing space 111, and as shown in FIG. It is placed above the container 20 (sample 21). Then, the position of the inside observation mirror 10 is appropriately adjusted according to the position of the container 20 . Specifically, as shown in FIG. 3, the inside observation mirror 10 is slid in the depth direction (ZZ') toward the back wall 110b of the main body 110, and the mirror surface member 12 is viewed through the observation window 140. The position of the inside observation mirror 10 is adjusted so that the image 30 seen from the upper side of the container 20 is reflected on the mirror surface member 12 when the container 20 is closed.

Subsequently, the opening/closing door 120 of the processing apparatus 100 is closed to seal the processing space 111 . After that, the mixture 21 is processed by evacuating the processing space 111 with the depressurizing means and heating the processing space 111 with the heating means. The heating temperature may be changed according to the type of liquid resin, and may be, for example, 20°C to 80°C.

By observing the mirror surface member 12 in the processing space 111 through the observation window 140 during the processing of the mixture 21, the state of the mixture 21 (the state of the sample contained in the mixture 21) is grasped from the image 30 reflected there. In this embodiment, after confirming that the liquid resin is dried, the operation of the processing apparatus 100 is stopped.

As described above, a resin-embedded sample in which a powder sample is embedded in a resin is obtained as an analysis sample.

The apparatus interior observation mirror 10 of this embodiment bridges between a pair of guide rails 130 , 130 and is configured to be slidable in the depth direction of the guide rails 130 within the processing apparatus 100 . Therefore, the position within the processing apparatus 100 can be freely adjusted according to the position where the container 20 containing the sample is placed. In addition, since the mirror member 12 is tilted and fixed to the mirror 10 for observing the inside of the apparatus, the mirror member 12 can project an image 30 of the sample viewed from above. By viewing from the outside through 140, the state of the sample in the processing space 111 can be grasped from the outside. Therefore, according to the apparatus internal observation mirror 10 of the present embodiment, the state of the sample being processed in the processing apparatus 100 can be easily observed from the outside of the processing apparatus 100 .

In addition, by treating the sample while observing it using the mirror 10 for observing the inside of the apparatus, the state of the sample can be grasped while the sample is being processed. This makes it possible to check for signs of abnormal sample conditions, such as scattering of powder samples due to rapid evaporation of solvent components, poor resin impregnation due to volatilization of curing agents or insufficient pressure reduction, etc. By stopping the operation of the processing apparatus 100, it is possible to prevent abnormal states from occurring. That is, the analytical sample can be produced more efficiently.

Although the embodiments of the present invention have been described above, the present invention is not limited to the above-described embodiments, and can be modified in various ways without departing from the gist of the present invention.

10 Inside observation mirror 11 Base member 12 Mirror surface member 13 Screw 14 Protective film 20 Container 21 Mixture 30 Image 100 Processing device 110 Main unit 111 Processing space 120 Open/close door 130 Guide rail 140 Observation window

Claims (9)

a pedestal member;
a mirror member fixed to the base member so as to be inclined with respect to a horizontal plane;
When placed in a processing apparatus having a processing space in which the front side is open and a sample is accommodated and processed, at least a A mirror for observing the inside of a device that can bridge between a pair of guide rails and can adjust the position of the pair of guide rails in the depth direction. The angle of inclination of the mirror surface member with respect to the horizontal plane is within a range of ±10° centered on 45°.
The mirror for observing inside the device according to claim 1 . The processing equipment is a vacuum dryer or a pressure reducer,
The mirror for observing the inside of the device according to claim 1 or 2. wherein the mirror surface member is a SUS mirror-polished plate;
The mirror for observing inside a device according to any one of claims 1 to 3. The base member is a metal square bar,
The mirror for observing inside a device according to any one of claims 1 to 4. The mirror surface member is screwed to the base member,
The mirror for observing inside a device according to any one of claims 1 to 5. A protective film is provided on the surface of the mirror surface member,
The mirror for observing inside a device according to any one of claims 1 to 6. A method of processing a sample to produce an analytical sample, comprising:
A main body portion having an opening on the front side and having a processing space in which a sample is stored and processed, an opening/closing door for opening and closing the opening of the main body portion, and a depth toward the back wall on each of the left and right side walls inside the main body portion. a step of preparing a processing apparatus comprising at least one pair of guide rails provided extending in a direction and an observation window provided in the open/close door;
A pedestal member and a mirror surface member fixed to the pedestal member so as to be inclined with respect to a horizontal plane, capable of bridging between the pair of guide rails, wherein the depth in the pair of guide rails A step of preparing a mirror for observing the inside of the device, the position of which can be adjusted in a direction;
placing the sample in the processing space;
The apparatus interior observation mirror is arranged above the sample by bridging between the pair of guide rails, and its position is changed according to the position of the sample within the processing apparatus. adjusting the guide rail in the depth direction;
and processing the sample,
A method for preparing an analysis sample, wherein, in the step of processing the sample, an image of the sample viewed from above, which is reflected on the mirror surface member during processing, is observed from outside the processing apparatus through the observation window. A method for observing the state of a sample placed in a processing apparatus, comprising:
A main body portion having an opening on the front side and having a processing space in which a sample is stored and processed, an opening/closing door for opening and closing the opening of the main body portion, and a depth toward the back wall on each of the left and right side walls inside the main body portion. a step of preparing a processing apparatus comprising at least one pair of guide rails provided extending in a direction and an observation window provided in the open/close door;
a pedestal member and a mirror surface member fixed to the pedestal member so as to be inclined with respect to a horizontal plane, the pedestal member being capable of bridging between the pair of guide rails in the processing apparatus; a step of preparing a mirror for observing the inside of the device, the position of which can be adjusted in the depth direction on the pair of guide rails;
placing the sample in the processing space;
The apparatus interior observation mirror is arranged above the sample by bridging between the pair of guide rails, and its position is changed according to the position of the sample within the processing apparatus. adjusting the guide rail in the depth direction;
and observing an image of the sample viewed from above, which is reflected on the mirror surface member, from the outside of the processing apparatus through the observation window.

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