JPH11201920A - Sample observing and analyzing method by vacuum system observing and analyzing device, and sample box for same device - Google Patents

Abstract

PROBLEM TO BE SOLVED: To enable highly accurate and high-quality observation and analysis while preventing the oxidization and moisture absorption of a sample in the observation and analysis of a sample such as metal lithium prepared by a sample preparing device and placed in the observa tion room of a vacuum observing analyzing device. SOLUTION: In a sample box 20, a lid plate 22 maintains closing air tightness at a recessed sample pocket 23 by the difference between the inner pressure and outer pressure of the pocket 23, and the lid plate 22 can be automatically opened by the energizing force of a spring by the equilibrium between the inner pressure and outer pressure of the pocket 23. The sample box 20 is placed in the glove box 5 of an atmosphere of inert gas of a sample preparing device 2 to house a sample 3 in the pocket 23. Continuously, the inside of the pocket 23 is brought into a vacuum state to set the pocket 23 at a closing hermetic state in which the lid 22 is adhered to the pocket 23. Then the sample box 20 is transferred to the observation room 9 of a vacuum system observing and analyzing device 1 and is set on a sample platform 11, and the observation room is brought into a vacuum state. By this, the lid 22 is brought into an automatically opened state, and the sample 3 in the pocket 23 is irradiated with an electron beam 12 and observed and analyzed characteristically in this observing and analyzing method and the sample box 20.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for observing and analyzing a sample of metallic lithium or the like by irradiating it with a particle beam or an electromagnetic wave in a vacuum observation / analysis apparatus such as a scanning electron microscope or an electron beam microanalyzer. And a sample box used in the vacuum observation / analysis apparatus.

[0002]

2. Description of the Related Art When observing the surface state (irregularity) of a super-oxidizing and super-hygroscopic sample such as metallic lithium, alkali metal and alkaline earth metal and measuring the amount of elements on the sample surface, a scanning electron microscope is required. (In the case of elemental measurement, a detector for elemental analysis is attached). That is, a sample is set in the observation / analysis room of the scanning electron microscope, and the observation / analysis room is set in a substantially vacuum state (0.001 Pa or less) and irradiated with an electron beam to perform observation / analysis. Then, the sample is prepared in a sample room of a sample preparation device having working gloves, which can be set in a vacuum atmosphere and an inert gas atmosphere such as an argon gas atmosphere, and is moved to the observation analysis room of the scanning electron microscope. It is.

[0003]

The above-described conventional method for observing and analyzing a sample by using a scanning electron microscope employs a method in which a sample carefully prepared in an inert gas atmosphere of a separate sample preparation device is used.
Since it comes into contact with the atmosphere in the transition course before setting it in the observation analysis room of the electron microscope, the super-oxidizing and super-hygroscopic sample surface such as metallic lithium becomes oxidized and absorbed by moisture, making it difficult to perform accurate observation analysis. There is.

In order to prevent the oxidation and moisture absorption, even if a sample prepared in a sample room is put into a sample container which can be set to a vacuum state and transferred to an electron microscope,
Since the sample taken out of the sample container for the transfer is in contact with the atmosphere even in a short time, it is not an effective measure to prevent oxidation and moisture absorption, and the observation and analysis room of the electron microscope and the sample preparation equipment Vacuum atmosphere by connecting the sample room
Even if it is intended to transfer the sample in an inert atmosphere, it becomes impractical because the equipment becomes huge and the equipment becomes extremely expensive.
There is a need in the art for measures to prevent oxidation and moisture absorption of samples that are inexpensive and excellent in practicality.

[0005] The present invention solves the above-mentioned disadvantages of the prior art, and at the same time, observes and observes a sample that meets the technical requirements of the relevant field.
An analysis method and a sample box are provided.

[0006]

According to the present invention, a sample is prepared in an inert gas atmosphere room, and the sample is provided in a sample pocket of a separate sample box in the inert gas atmosphere room. The sample is stored, then the sample pocket is evacuated and the lid closed and locked in an airtight state, and then the sample box is moved to the observation / analysis room of a vacuum observation / analysis apparatus, and the observation / analysis room is evacuated. A vacuum observation / analysis characterized by irradiating the sample pocket within the sample pocket with a particle beam / electromagnetic wave and observing / analyzing the sample pocket by opening the sample pocket into an open form with a lid automatically opened. Method for observing and analyzing samples using an analyzer ”

[0007] A sample pocket having an exhaust valve with a check valve and recessed in the upper surface of the box body, and a lid plate having an open biasing spring and capable of closing the upper opening of the sample pocket with an airtight seal are provided. , The inside of the sample pocket is generally in a vacuum state,
And, in the pressure relationship where the outside of the sample pocket is approximately 1 atm and the lid plate maintains a closed airtight state, and the pressure relationship between the inside and outside of the sample pocket is approximately balanced,
A sample box for a vacuum system observation / analysis device is characterized in that the lid plate is configured to be automatically opened by the urging force of the urging spring.

That is, according to the observation / analysis method of the present invention, a sample for observation / analysis prepared in an inert gas atmosphere of a sample preparation device is stored in a sample pocket of a separate sample box in the inert gas atmosphere. Then, the inside of the pocket is set and locked in a vacuum-tight state, transferred to the observation / analysis device, and the observation / analysis room of the observation / analysis device is evacuated to automatically open the lid for observation / analysis. It features a process. Then, the sample box of the present invention has a “exhaust valve with a biasing spring and a check valve” and a “cover plate configuration in which a lid plate in a hermetically closed state can be automatically opened according to a pressure difference condition between the inside and outside of the pocket”. It allows for conservative transfer.

[0009]

According to the above-described observation and analysis method using the vacuum observation and analysis apparatus of the present invention, the sample to be transferred and set from the inert gas atmosphere room of the sample preparation device to the observation and analysis room of the observation and analysis device is kept in a vacuum atmosphere. Thereafter, since the sample is exposed and observed / analyzed in the vacuum atmosphere of the observation / analysis room, the sample in a series of processes from sample preparation to observation / analysis is completely shut off from contact with the atmosphere. Therefore, oxidation and moisture absorption of the super-oxidizable and super-hygroscopic sample can be prevented in a perfect form. The sample box of the present invention can maintain the lid closed airtight state and automatically open the lid plate depending on the pressure conditions of the inside and outside of the sample pocket, so that the above-described operation of the observation and analysis method of the present invention can be smoothly achieved with a compact and simple structure. .

[0010]

Embodiments of the present invention will be described below. First, an embodiment of a sample box for an observation / analysis device according to the present invention will be described with reference to FIG. That is, in the sample box 20 of the present invention, a sample pocket 23 (hereinafter simply referred to as a pocket 23) is recessed in the upper surface of the front half of the box body 21 of the rectangular parallelepiped metal block. An exhaust valve 25 with a check valve at the end of an exhaust hole 26 communicating with the exhaust port 26 and a lid plate 22 whose upper opening can be closed and opened. And the lid plate 22
It is hinged and movable via a link bar 24 connected between the side wall of the block body 21 and the side edge of the lid plate 22, so that the upper opening of the pocket 23 can be closed or placed on the rear half of the box body 21. The pocket 23 can be opened by being set. A seal ring 31 is attached to the upper surface of the box body 21 on the periphery of the pocket 23 so as to be joined to the cover plate 22 in a closed position and to seal the pocket 23 in an airtight manner.

Further, in the link bar 24 of the moving mechanism of the cover plate 22, a coil spring 27 of an urging spring is fitted on a connecting pin 30 to the box body 21.
7 has one end 28 fixed to the link bar 24 and the other end 29 fixed to the box body 21. And
When the cover plate 22 with the pocket 23 closed is lightly pressed with a fingertip and sucked and exhausted from the exhaust valve 25 to make the inside of the pocket 23 substantially in a vacuum state, the pressing pressure of the cover plate 22 is generated by the atmospheric pressure outside the pocket 23, Even when the fingertip is released, the lid plate 22 is directly adsorbed and covered on the pocket 23 to maintain the vacuum state of the pocket 23 airtight, and when the sample box 20 in that state is placed in a vacuum atmosphere, the inner and outer pressures of the pocket 23 are balanced. The pressing force of the cover plate 22 disappears, and the coil spring 2
The cover plate 22 is automatically moved by the urging force of the box body 2.
1, the cover plate 22 is closed and opened under the urging force condition in which the pocket 23 is opened by moving to the rear half portion of the cover plate 1.

The above-mentioned sample box 20 is placed in a preparation room of a sample preparation device to be described later to store a sample 3 of metallic lithium or the like.
Is stored in an inert gas atmosphere, and the pocket 23 is evacuated to a vacuum-tight state.
Is automatically opened in a vacuum atmosphere to observe and analyze the sample.

Next, an embodiment of a sample observation / analysis method using the vacuum observation / analysis apparatus of the present invention will be described with reference to FIG. That is, the sample 3 of metallic lithium which is an observation / analysis sample required in the inert gas atmosphere of the sample preparation device 2 is prepared.
Is transferred to a vacuum observation / analysis device 1 to observe the surface condition of the sample 3, and the sample preparation device 2 is referred to as a “glove room 5 having working gloves 4 whose ends are fixed to the room wall” and a “material / tool Preparation Room 6 ”is communicated via door 8
A sample is observed by the following procedure / method using a two-chamber structure that can be shut off.

That is, as shown in FIG. 2, the sample box 20 with the cover plate 22 opened and a material for producing the sample 3 such as material, manual suction pump, tweezers, conductive tape (not shown), and the door 7 are opened. And put it in preparation room 6 and door 7
Is closed, and the preparation room 6 is evacuated by the vacuum pump 17, and then argon gas is supplied from the argon cylinder 16 to make the preparation room 6 an atmosphere of one atmosphere of inert gas.

Subsequently, the door 8 is opened, and the sample box 20 and the material tools in the preparation room 6 are moved to the glove room 5 under an atmosphere of 1 atmosphere of argon gas, and the sample 3 is prepared using the material tools described above. A conductive tape is laid as needed in the pocket 23 of the sample box 20 with the plate open, and the sample 3 is put thereon, and the sample 3 is set in the pocket 23. Subsequently, a manual suction pump is connected to the exhaust valve 25 of the sample box 20, and the cover plate 22 is pressed with a fingertip to cover the cover plate 2.
2 is closed, suction is evacuated, the inside of the pocket 23 is evacuated, the cover plate 22 is set and locked in a closed airtight state,
The sample box 20 in the set lock state is taken out to the atmosphere via the preparation room 6.

Thereafter, the sample box 20 is connected to the vacuum observation / analysis device 1 of another device (the device of this embodiment is
The sample stage 11 is placed on the sample stage 11 from the sample entrance 10 of a scanning electron microscope using an electron beam, which is one of the particle beams. The observation room 9 is evacuated by closing and sucking and exhausting from the intake hole 15, and the lid plate 22 of the sample box 20 is automatically opened to open the pocket 23. Thereafter, the sample 3 in the pocket 23 is irradiated with the electron beam 12 and the sample stage 11 is moved and adjusted in three axial directions while observing the image with the cathode ray tube to set the sample box 20 at an appropriate observation position. The surface state of the sample 3 is observed.

The observation and analysis method according to the above-described embodiment has the above-mentioned effects. In a series of processes from the preparation of the sample 3 to the observation of electron beam irradiation, the sample 3 is completely shut off from contact with the atmosphere. Super oxidizing and super hygroscopic sample 3
Oxidation and moisture absorption are completely prevented, enabling high-precision observation and analysis. The sample box 20, which enables high-precision observation and analysis, has a practical advantage that it can be manufactured easily and inexpensively with a simple and compact structure that does not have a motor for opening and closing the cover plate.

Note that the present invention is not limited to the above-described embodiment, but includes an electron beam microanalyzer, an X-ray photoelectron spectrometer,
The present invention is applied to other vacuum observation / analysis devices such as an Auger electron spectrometer and a secondary ion mass spectrometer. Further, as shown in FIG. In some cases, the lid plate 22 is connected to the cover plate 22 with a hinge 32 to automatically raise the lid plate 22 or open it 180 °. In FIG. 3, the box body 21 can be downsized.

[0019]

As described above, the sample observation / analysis method and the sample box using the vacuum system observation / analysis apparatus of the present invention are used in a series of processes from sample preparation to observation / analysis to bring the sample into contact with the atmosphere. , Which makes observation and analysis of super-oxidizing and super-hygroscopic samples extremely accurate and enables high-quality observation and analysis, as well as small, compact, easy-to-use and inexpensive samples. The box has the effect of meeting the needs of the technical field with high practicality that can achieve high quality observation and analysis.

[Brief description of the drawings]

FIG. 1 shows the procedure of an embodiment of the observation / analysis method of the present invention.
Illustration of the method

FIG. 2 shows an embodiment of the sample box of the present invention,
(A) is a perspective view of a cover plate opened state, (B) is a perspective view of a cover plate closed state, (C) is a side view of a main part showing a spring biasing mechanism of the cover plate, and (D) is a view of (B). Cross section

FIG. 3 is a side view of another embodiment of the sample box of the present invention.

[Explanation of symbols]

 REFERENCE SIGNS LIST 1 vacuum observation / analysis device 2 sample preparation device 3 sample 4 work gloves 5 glove room 6 preparation room 9 observation analysis room 11 sample stage 12 electron beam 13 detector 20 sample box 21 box body 22 lid plate 23 sample pocket 24 link bar 25 Exhaust Valve 26 Exhaust Hole 27 Coil Spring 30 Connecting Pin 31 Seal Ring 32 Hinge

Claims (2)

[Claims] 1. A sample is prepared in an inert gas atmosphere room, the sample is stored in a sample pocket of a separate sample box in the inert gas atmosphere room, and then the sample pocket is evacuated. The lid closed and locked in an airtight state, and then the sample box was moved to an observation / analysis room of a vacuum system observation / analysis apparatus, and the observation / analysis room was evacuated to open the sample pocket automatically. A method for observing and analyzing a sample using a vacuum system observation and analysis apparatus, characterized in that the sample in the sample pocket is irradiated with a particle beam or electromagnetic wave to observe and analyze the sample. 2. A sample pocket having an exhaust valve with a check valve and recessed in the upper surface of the box body, and a lid plate having an open biasing spring and capable of closing the upper opening of the sample pocket in an airtight manner. Provided, the inside of the sample pocket is generally in a vacuum state,
And, in the pressure relationship where the outside of the sample pocket is approximately 1 atm and the lid plate maintains a closed airtight state, and the pressure relationship between the inside and outside of the sample pocket is approximately balanced,
A sample box for a vacuum observation / analysis apparatus, wherein the lid plate is configured to be automatically opened by the urging force of the urging spring.