JPH02160351A - Electron microscope - Google Patents

Abstract

PURPOSE:To make it possible to observe a sample without being affected by the atmosphere by supplying or processing a sample in a chamber separated from a sample exchanging chamber. CONSTITUTION:A vacuum frame 13 which is equipped with a holding part so as to hold said sample holder 17, a gate valve 16, an exhaust pipe 20, a vacuum valve 21, an opening 22 for connection and a sample transfer rod 18, etc., are provided in an electron microscope so that a sample is set and observed at a sample observation position without being exposed to the atmosphere at all after the sample supplied from a sample supply chamber is collected to a sample holder 17 in a vacuum frame 13. In this way, a sample can be observed under such a condition that the sample is not affected by the atmosphere.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an electron microscope in which a sample is supplied or processed in a chamber separate from the sample exchange chamber and then transferred to the sample chamber.

[Prior Art] When observing and analyzing minute substances contained in exhaust gas using an electron microscope, the conventional method was as follows.

That is, a sample holder is placed in a sample supply chamber provided separately from the sample exchange chamber, and the minute substances contained in the exhaust gas sent to this supply chamber are collected onto a sample collection membrane attached to the sample holder. After that, take the sample holder out into the atmosphere. Next, open the lid of the sample exchange chamber of the electron microscope, insert the sample holder into the exchange chamber, and after preliminary evacuation of the exchange chamber, open the gate valve, insert the sample holder into the sample chamber, and position the microscope. I am trying to place it in

[Three problems to be solved by the invention] In such conventional devices, the sample must be exposed to the atmosphere before being inserted into the sample chamber of the electron microscope, and as a result, the sample is exposed to oxygen, water, etc. in the atmosphere. They may react with water or be contaminated by trace substances in the atmosphere.

Therefore, it was not possible to observe the sample without being affected by the atmosphere.

The purpose of the present invention is to solve these problems and provide an electron microscope that can observe a sample supplied or processed in a chamber separate from the sample exchange chamber without being affected by the atmosphere. There is.

[Means for Solving the Problems] Therefore, the present invention provides a sample exchange chamber connected to a sample chamber via a gate valve, and a sample holder inserted into the sample exchange chamber that is moved to five observation positions within the sample chamber. The electron microscope is equipped with a vacuum casing having a holding part for holding the sample holder therein, and a vacuum casing for isolating the inside of the casing from external space when the casing is closed. A gate valve provided near the insertion and dislocation of the sample holder, an exhaust pipe attached to the casing so that the inside of the casing can be connected to a vacuum pump, a vacuum valve provided on the exhaust pipe, and the sample exchanger. a connection opening bored in the chamber, and a mechanism for detachably attaching the casing to the sample exchange chamber while maintaining airtightness with the insertion/removal port of the casing being joined to the connection opening; A transfer mechanism provided in the housing for transferring the sample holder held by the holding part in the attached state into the sample exchange chamber through the insertion/ejection port, and a transfer mechanism provided separately from the sample exchange chamber. A supply/processing chamber for processing or supplying a sample, and the housing is airtightly connected to the supply/processing chamber with the insertion/removal port of the housing connected to the connection opening provided in the supply/processing chamber. It is characterized by having a mechanism for maintaining and removably attaching it.

[Example] Embodiments of the present invention will be described in detail below based on the drawings.

FIG. 1 is a diagram showing essential parts of an embodiment of the present invention, and FIG. 2 is a diagram showing a state in which a vacuum casing is connected to a sample supply chamber.

In Figure 1, 1 is the lens barrel of the electron microscope, 2 is the sample chamber,
3 is a sample stage having a hole 4 for inserting a sample holder, and 5 is an objective lens.

A sample exchange chamber 6 that can communicate with the sample chamber 2 via a gate valve 7 is attached to the lens barrel 1 . The sample exchange chamber 6 is connected to a vacuum exhaust system (not shown) via an exhaust pipe 8. 9 is a vacuum valve. Reference numeral 10 denotes a transfer rod for the sample holder, and a claw 11 for holding the sample holder is attached to the tip of the transfer rod 10.

An operating shaft 12 is passed through the transfer rod 10, and the claw 1
1 can be opened and closed. Reference numeral 13 denotes a vacuum casing having a holding portion 14 for holding a sample holder 17 therein. Reference numeral 15 denotes a sample holder insertion/extraction port of the vacuum casing, and a gate valve 1 is provided in the vacuum casing 15 to control opening/closing of the insertion/extraction port.
6 is installed. The holding portion 14 is integrally fixed to a transfer rod 18 for transferring the sample holder.

The transfer rod 18 can be moved while maintaining a vacuum by an O-ring 19. An exhaust pipe 20 is attached to the vacuum casing 13, and a vacuum valve 21 is attached to the exhaust pipe 20. A cylindrical body constituting the sample holder 14 is provided with a communication hole 14a. Reference numeral 22 denotes a connection opening bored in the wall of the sample exchange chamber for connecting the vacuum housing 13. With the sample holder insertion/removal port 15 of the vacuum case 13 connected to the connection opening 22, the vacuum case 13 is inserted into the sample exchange chamber 6.
A recess 23 is provided in the vacuum housing 13 in order to detachably attach the
is provided, and a stopper 24 is attached to the wall of the sample exchange chamber 6.

In FIG. 2, in which the same components as in FIG. 1 are given the same numbers, 25 is a sample supply chamber. A connection opening 26 is bored in the wall of the chamber 25.
With the sample holder insertion and dislocation of the vacuum housing connected to the
In order to detachably attach the vacuum housing 13 to the sample supply chamber 25, a fastener 27 is attached to the wall of the sample supply chamber 25. The exhaust pipe 20 can be connected to an exhaust pipe 30 connected to a vacuum pump 29 through a connector 28. In Figures 1 and 2, 31, 32° 33.34
is 0-ringsinyl.

In such a configuration, first, in a state where the vacuum housing 13 is separated from the sample exchange chamber 6 and the sample supply chamber 25,
The gate valve 16 is opened, the sample holder 17 is inserted into the vacuum housing 13, and the sample holder 17 is held in the holding part 14. After that, the gate valve 16
is closed, and with the sample holder insertion/removal port 15 of the vacuum housing 13 connected to the connection opening 26 of the sample supply chamber 25, turn the stopper 27 to insert it into the recess 23, and place the vacuum housing 13 into the sample supply chamber 25. Install airtight. Next, the exhaust pipes 20 and 30 are connected by the connector 28, the vacuum valve 21 is opened, and the inside of the vacuum casing 13 is evacuated by the vacuum pump 29. After the air, etc. in the vacuum housing 13 is exhausted and the air, etc. in the sample supply chamber 25 is exhausted by the same operation, exhaust gas containing trace substances that will become the sample is introduced into the sample supply chamber 25, and the partition is closed. Open valve 16. As a result, the exhaust gas passes through the vacuum housing 13 and heads to the vacuum pump 29 via the exhaust pipes 20 and 30. During this process, some of the trace substances contained in the exhaust gas adhere to the sample collection adhesive film (not shown) attached to the tip of the sample holder 17 and are collected. After closing the valve 16 and sufficiently evacuating the inside of the vacuum housing 13, the vacuum valve 21 is closed. And exhaust pipe 20
and 30, and move the vacuum housing 13 to the sample supply chamber 25.
Remove from. Next, with the sample holder insertion/removal port 15 of the vacuum housing 13 connected to the connection opening 22 of the sample exchange chamber 6, turn the stopper 24 and insert it into the recess 23, and move the vacuum housing 13 into the sample exchange chamber 6. Attach airtight to.

Then, the vacuum valve 9 is opened and the sample exchange chamber 6 is passed through the exhaust pipe 8.
Exhaust the inside. When the degree of vacuum in the sample exchange chamber 6 increases, the gate valve 16 is opened, the sample transfer rod 18 is raised, and the sample holder 17 is inserted into the sample exchange chamber 6. Therefore,
After operating the operation shaft 12 to clamp the sample holder 17 between the claws 11, the gate valve 7 is opened, and the transfer rod 10 carries the sample holder 17 onto the sample stage 3 and sets it at the microscope position.

In this way, after the sample supplied from the sample supply chamber 25 is collected in the sample holder 17 inside the vacuum housing 13,
Since the sample is set at the sample observation position and observed without being exposed to the atmosphere, the sample can be observed without being affected by the atmosphere.

It should be noted that the above-described embodiment is only one embodiment of the present invention, and can be modified and implemented.

For example, the above embodiment was an example in which the vacuum housing was connected to the sample supply chamber, but the sample may be subjected to a gas reaction, the sample may be broken, the sample surface may be etched, the sample surface may be coated, etc. The present invention can be similarly applied to cases in which vacuum casings are connected to various sample processing chambers in which processed samples are observed without being affected by the atmosphere.

[Effect of the invention] As is clear from the above explanation, the present invention has the following effects:
a vacuum casing including a holding part for holding the sample holder inside; a gate valve provided near the sample holder insertion/extraction opening of the casing to isolate the inside of the casing from an external space when the casing is closed; an exhaust pipe attached to the housing to enable connection of the inside of the housing with a vacuum pump; a vacuum valve provided on the exhaust pipe; and a connection opening bored in the sample exchange chamber;
a mechanism for removably attaching the casing to the sample exchange chamber while maintaining airtightness with the insertion/removal port of the casing being joined to the connection opening; a transfer mechanism provided in the housing for transferring the sample holder into the sample exchange chamber through the insertion/removal port; and a supply for processing or supplying the sample provided separately from the sample exchange chamber. /Processing chamber and its supply/
The present invention includes a mechanism for removably attaching the housing to the supply/processing chamber while maintaining airtightness with the insertion/removal port of the housing connected to the connection opening provided in the processing chamber. This makes it possible to observe samples without being affected by the atmosphere, and it becomes possible to observe samples that are not contaminated by trace substances in the atmosphere before they react with oxygen, water, etc. in the atmosphere.

[Brief explanation of the drawing]

FIG. 1 is a diagram showing essential parts of an embodiment of the present invention, and FIG. 2 is a diagram showing a state in which a vacuum casing is connected to a sample supply chamber. 1: Lens tube 2: Sample chamber 3: Sample stage 4 Two holes 5: Objective lens 6: Sample exchange chamber 7.16: Gate valve 8, 20, 30: Exhaust pipe 9.21: Vacuum valve
10: Transfer rod 11: Claw 12: Operation shaft 13: Vacuum housing 14: Holding section 14a: Hole 15: Sample holder insertion/extraction port 17: Sample holder 18: Transfer rod 19.31, 32, 33, 34; 0 ring 22 .26:
Connection opening 23: Recess 24, 27: Stopper 25: Sample supply chamber 28: Connection 29: Vacuum pump throat

Claims (1)

[Claims] An electron microscope equipped with a sample exchange chamber connected to a sample chamber via a gate valve, and a transfer mechanism for transferring a sample holder inserted into the sample exchange chamber to an observation position in the sample chamber. A vacuum housing including a holding part for holding the sample holder, a gate valve provided near the sample holder insertion/extraction opening of the housing to isolate the inside of the housing from external space when the vacuum housing is closed, and the housing. an exhaust pipe attached to the casing so that the inside can be connected to a vacuum pump, a vacuum valve provided on the exhaust pipe, a connection opening bored in the sample exchange chamber, and an insertion hole in the casing. a mechanism for removably attaching the casing to the sample exchange chamber while maintaining airtightness in a state where the ejection port is joined to the connection opening; a transfer mechanism provided in the casing for transferring the sample into the sample exchange chamber through the insertion/ejection port; a supply/processing chamber provided separately from the sample exchange chamber for processing or supplying the sample; An electronic device having a mechanism for removably attaching the housing to the supply/processing chamber while maintaining airtightness with the insertion/removal port of the housing connected to a connection opening provided in the supply/processing chamber. microscope.