JP2023182490A - Atmosphere cut-off device and atmosphere non-exposed conveyance method - Google Patents

Abstract

To provide a deformable and compact atmosphere cut-off device which can reduce an influence on a sample holder due to an atmospheric pressure variation and disturbance in an atmosphere, and when moving a sample to an another place, cut-off the atmosphere in each sample holder to conveyance it so as to have less oxygen and water.SOLUTION: An atmosphere cut-off device is constructed by: a chamber part 6 that cut-offs a sample holder 3 from an atmosphere; and a connection part 5 that adheres and connects the chamber part to a sample mounting part 2 of an observation and analysis device 1, and can deform a whole structure so that a lid 10, a vacuum valve, a gas introduction valve, and a gate valve can be detached and attached. By freely combining parts, the device becomes an atmosphere cut-off cover that cuts off a device outer exposure part of the sample holder 3 from an atmosphere at the time of the observation and an analysis. In the case where the sample is moved to an another location from the observation and analysis device, the sample holder is just cut off from the atmosphere, and it can be conveyed between globe boxes in a state of less oxygen and water. The lid 10 having a connector 11 can be exchanged in accordance with necessary.SELECTED DRAWING: Figure 1

Description

Patent Act Article 30, Paragraph 2 application filed Date of sale: March 31, 2020 Place of sale: National Institute for Materials Science, National Institute for Materials Science

The present invention relates to a device for sealing part or the whole of a sample holder attached to an observation/analysis device to isolate it from the atmosphere, and a transportation method without exposure to the atmosphere.

The sample held in the sample holder is transported through the atmosphere, inserted into the appropriate position in the observation/analysis device, and irradiated with a beam of charged particles such as electrons and ions.The charged particles generated from the sample after being irradiated are It is now possible to measure the shape and composition of a sample by detecting radiation such as X-rays and X-rays. The following problems occur in the process of sample measurement.

1. Instability of the position of observation and analysis points The air inside the laboratory is affected by the opening and closing of doors and air conditioning. Because part of the sample holder is exposed to the atmosphere when the observation/analysis device is attached, the sample holder may be pushed or pulled by fluctuations in the atmospheric pressure or movement of air in the room, making the sample position unstable. Observation and analysis points move.

2. Deterioration of samples due to moisture and oxygen in the atmosphere during transportation Many samples absorb oxygen and moisture contained in the atmosphere, causing sample contamination. In addition, there are many materials that easily react with oxygen and moisture, and in such cases, observation and analysis results will be different from those of the original material.

In this way, in the observation/analysis device, the sample holder with the sample attached is transported in the atmosphere, and only the tip of the sample holder is inserted into the observation/analysis device. When using the manufacturer's standard sample holder, observation and analysis equipment of the type that seals the part of the sample holder exposed to the atmosphere has begun to appear, but special sample holders with heating functions, etc. These sample holders are not compatible with the device manufacturer's sealing function.

JP2020-27716 JP2012-138233

As for blocking the atmosphere from the exposed portion of the sample holder, a dedicated cover provided by an observation/analysis device manufacturer or a third party is known (Patent Document 1). However, this cover has the function of a cover specialized for reducing atmospheric fluctuations, noise, and vibration, and is not expandable, and may not be usable depending on the shape of the connector for supplying power to the sample holder. be. Furthermore, since the cover has a single function, it cannot have the function of blocking the entire sample holder from the atmosphere and removing it from the apparatus and transporting it.

Although there is a type of sample holder that does not expose only the sample holding part of the sample holder to the atmosphere, it is not possible for the user to use the sample holder by shielding the entire sample holder from the atmosphere (Patent Document 2). Furthermore, since the entire sample holder cannot be shielded from the atmosphere, it is not compatible with the atmosphere shielding cover, and a cover must be prepared separately.

The atmospheric non-exposed transport device according to the present invention is an atmospheric shielding device that is attached to the sample holder mounting portion of an observation/analysis device and serves as a cover, and can be tightly connected and fixed to the sample holder mounting portion of the observation/analysis device. It is composed of a connecting part, a chamber part that can be tightly connected and fixed to the connecting part, and a lid that can be detached from the chamber part, and the connecting part, the chamber part, and the lid can each be separated. It is characterized by

Further, the connecting portion, the chamber portion, and the lid are characterized in that they do not interfere with parts and accessories that are pre-installed in the observation/analysis device.

Furthermore, the lid has a connector that allows power to be supplied to a connecting cable attached to the sample holder of the observation/analysis device.

In addition, the connection part, the chamber part, and the lid do not interfere with parts and accessories that are pre-installed in the observation/analysis device, and the lid can be connected to the connection cable attached to the sample holder of the observation/analysis device. It is characterized by having a connector that enables power supply.

In addition, the non-atmospheric transport according to the present invention is an atmospheric shielding device that serves as a transport device when transporting a sample holder from an observation/analysis device to another location, and includes the connection portion and the connection portion that is closely connected and connected to the connection portion. It consists of a gate valve that can be fixed, a chamber part that can be closely connected and fixed to the gate valve, and a lid that can be attached to and detached from the chamber part, and the entire sample holder is housed in the chamber part, shielded from the atmosphere. It has transportable characteristics.

Further, the connecting portion, the chamber portion, the gate valve, and the lid are characterized in that they do not interfere with parts and accessories that are pre-installed in the observation/analysis device.

Further, in the method for transporting the atmospheric shielding device according to the present invention, when transporting the sample holder from the observation/analysis device to another location, an atmospheric shielding type glove is attached to a part of the chamber section, and the glove is used to hold the specimen holder. After pulling out the specimen from the experimental container or observation/analysis device and placing the entire sample holder inside the chamber, the gate valve was closed and the chamber was evacuated or replaced with an inert gas to remove oxygen and moisture as much as possible. The device is characterized in that it can be separated from observation and analysis equipment and carried while shielded from the atmosphere.

According to the atmospheric isolation device of the present invention, by using the exposed part of the sample holder attached to the observation/analysis device as a cover to isolate it from the atmosphere, changes in the atmospheric pressure in the room and movement of the atmosphere can be transmitted to the sample holder. can be reduced.

According to the atmospheric isolation device of the present invention, it can be used for any sample holder by replacing the lid with multiple types of connectors according to the specifications of the connector of the connection cable attached to the sample holder. .

According to the atmospheric isolation device of the present invention, by installing a gate valve between the connection part and the chamber part, the entire sample holder is housed in the chamber and is isolated from the atmosphere, and oxygen and moisture are removed by vacuum evacuation or gas replacement. It is possible to carry the sample while maintaining a state where it is excluded as much as possible, and it is possible to reduce deterioration of the sample due to oxygen and water components contained in the atmosphere.

According to the atmosphere blocking method of the present invention, a sample held in a sample holder in a glove box is attached to the goniometer of an analyzer without coming into contact with the atmosphere, and the sample can be placed inside the analyzer without coming into contact with the atmosphere. It has the effect of enabling analysis without deterioration due to oxygen and water components contained in the atmosphere.

is an atmospheric isolation device that isolates the exposed external part of the heated sample holder attached to the observation/analysis device from the atmosphere, and also supplies power from an external power source to the connector that can be connected to the power supply cable attached to the heated holder. It is a figure showing an example of a device.

1 is a diagram illustrating an example of an atmosphere blocking device for transporting the entire sample holder, which allows the sample holder to be transported from the glove box to the analyzer without exposing the sample held in the sample holder to the atmosphere. FIG.

The atmospheric shielding device of the present invention can be closely connected to the observation/analysis device, and is composed of parts that can be separated, and can be freely deformed, so that the sample holder can be attached to the observation/analysis device. When the sample holder is exposed outside the device, the exposed part of the sample holder can be used as a cover to block the atmosphere.Also, when transporting the sample without exposing it to the atmosphere, the entire sample holder can be stored inside the device. It can be used as a device for transporting from an observation/analysis device to another location by shutting off the atmosphere. Therefore, the atmospheric isolation device of the present invention reduces the influence of atmospheric pressure and air fluctuations in the laboratory during measurements, and reduces contamination and deterioration due to oxygen and water components contained in the atmosphere during sample transport. In the creation of reproducible data, it enables highly reliable and stable analysis, and is useful in a wide range of fields including research and development.

Referring to FIG. 1, in the atmospheric blocking device of the present invention, a sample holder 3 is attached to a sample holder attachment part 2 of an observation/analysis device 1, and a sample 4 is held at an appropriate position inside the observation/analysis device 1. After that, the connection part 5 of the atmospheric isolation device consisting of the connection part 5, the chamber part 6, and the lid 7 is brought into close contact with the sample holder attachment part 2, and fixed with the fixture 8, so that the sample holder 3 can be removed from the apparatus. Insulate exposed areas from the atmosphere.

Referring to FIG. 1, in the atmospheric blocking device of the present invention, a cable 9 for supplying power to a heater 14 at the tip of a sample holder 3 is connected from the inside to a connector 11 attached to a lid 10, and a power source 13 is connected to the The output cable 12 is connected to the connector 11 from the outside, and the cable 9 and the cable 12 are electrically connected. With the part of the heated sample holder 3 exposed outside the apparatus cut off from the atmosphere, current is passed from the power supply 13 to the heater 14, and the sample is heated. It is possible to heat 4.

In the atmosphere shielding device of the present invention, referring to FIG. 2, a glove 16 is attached to the chamber portion 15 via a flange 17. The evacuation valve 24 is connected to a vacuum pump, and the gas introduction valve 25 is connected to an arbitrary gas cylinder such as an inert gas. After the gate valve 21 of the gate valve 22 is closed by the drive rod 23 and the inside of the chamber section 15 is sealed, the vacuum evacuation and gas replacement inside the chamber section 15 are controlled by opening and closing the evacuation valve 24 and the gas introduction valve 25. to eliminate oxygen and moisture.

The evacuation valve 19 is connected to a vacuum pump, and the gas introduction valve 20 is connected to an arbitrary gas cylinder such as an inert gas. The connecting part 5 is closely connected and fixed to the sample holder attachment part 2 of the observation/analysis device 1 by the fixture 8, and the inside of the connecting part 5 is evacuated and gas replaced by opening and closing the vacuum evacuation valve 19 and the gas introduction valve 20. control to eliminate oxygen and moisture.

With the connection part 5 tightly connected to the sample holder attachment part 2 of the observation/analysis device 1 by the fixture 8, the inside of the connection part 5 is evacuated and gas replaced by opening and closing the vacuum evacuation valve 21 and the gas introduction valve 21. control and eliminate oxygen and moisture.
With the connection part 5 and chamber part 15 filled with replacement gas at the same pressure, open the gate valve 21 with the drive rod 23 of the gate valve part 22, grasp the holder grip 7 of the sample holder 3 with the gloves 16, and remove the sample holder. The sample holder 3 is pulled out from the attachment part 2 and moved into the chamber part 15. The sample holder 3 is placed and held on the pedestal 18, the gate valve 21 is closed by the drive rod 23, and the connection part 5 is separated from the sample holder attachment part 2. In this way, the sample 4 in the sample holder 3 can be removed from the observation/analysis apparatus 1 without coming into contact with the atmosphere, and can be transported to any desired location.

The sample holder 3, which has been transported after being shut off from the atmosphere in the reverse order of steps [0025] to [0027], can be inserted into the observation/analysis apparatus 1 without coming into contact with the atmosphere.

If the glove box is provided with a flange having the same shape as the sample holder attachment part 2, the sample can be inserted into the glove box without being exposed to the atmosphere. Conversely, the sample can be taken out of the glove box and transported to any location without exposing it to the atmosphere. That is, by using this device, the sample can be moved between the observation/analysis device 1 and the glove box without coming into contact with the atmosphere.

If the chamber 3 is made of a transparent material such as glass or resin, the inside can be observed and, for example, the state of the sample holder can be confirmed.

1 Observation/analysis device 2 Sample holder attachment part 3 Sample holder 4 Sample 5 Connection part 6 Chamber part 7 Holder grip 8 Fixture 9 Cable 10 Lid 11 Connector 12 Output cable 13 Power supply 14 Heater 15 Chamber part 16 Gloves 17 Flange 18 Pedestal 19 Vacuum valve 20 Gas introduction valve 21 Gate valve 22 Gate valve part 23 Drive rod 24 Vacuum valve 25 Gas introduction valve

Claims (7)

An atmospheric shielding device that is attached to the sample holder attachment part of an observation/analysis device and serves as a cover,
A connection part that can be tightly connected and fixed to the sample holder attachment part of an observation/analysis device,
a chamber part that can be closely connected and fixed to the connection part;
a removable lid to the chamber section;
an atmosphere blocking device, characterized in that the connecting portion, the chamber portion, and the lid are each separable. The connecting portion, the chamber portion, and the lid do not interfere with parts and accessories that are pre-installed in the observation/analysis device;
The atmosphere blocking device according to claim 1, characterized in that: The lid has a connector that allows power to be supplied to a connection cable attached to a sample holder of an observation/analysis device.
The atmosphere blocking device according to claim 1, characterized in that: The connection portion, the chamber portion, and the lid do not interfere with parts and accessories that are pre-installed in the observation/analysis device, and
The lid has a connector that allows power to be supplied to a connection cable attached to a sample holder of an observation/analysis device.
The atmosphere blocking device according to claim 1, characterized in that: An atmosphere blocking device that serves as a transport device when transporting a sample holder from an observation/analysis device to another location,
The connection part;
a gate valve that can be closely connected and fixed to the connection part;
a chamber part that can be tightly connected and fixed to the gate valve;
a removable lid to the chamber section;
An atmosphere shielding device comprising: an atmosphere shielding device, which is characterized in that the entire sample holder can be stored in the chamber section, shielded from the atmosphere, and transported. The connection part, the chamber part, the gate valve, and the lid do not interfere with parts and decorations that are pre-installed in the observation/analysis device;
The atmosphere blocking device according to claim 5, characterized in that: When transporting the sample holder from the observation/analysis device to another location,
Attaching air-blocking type gloves to a part of the chamber part,
Using the above gloves, pull out the sample holder from the experimental container or observation/analysis equipment.
After installing the entire sample holder inside the chamber section,
The gate valve is closed, and the chamber is evacuated or replaced with an inert gas to remove oxygen and moisture as much as possible,
It can be separated from observation and analysis equipment and carried while shielded from the atmosphere.
A method for transporting an atmospheric isolation device characterized by

Images