JP2726541B2 - Electron microscope or similar device - Google Patents

Description

The present invention relates to an electron microscope or similar device for preparing or processing a sample in a chamber separated from a sample exchange chamber and transferring it to the sample chamber.

[Prior Art] When observing and analyzing minute substances contained in exhaust gas with an electron microscope, conventionally, the following has been performed. That is, the sample holder is arranged in a sample supply chamber provided separately from the sample exchange chamber, and the minute substance contained in the exhaust gas sent to the supply chamber is collected on a sample collection film attached to the sample holder. After that, take out into the atmosphere. When a sample collection membrane is used, the membrane is attached to a sample holder in the atmosphere. Next, the lid of the sample exchange chamber of the electron microscope is opened, the sample holder is inserted into the exchange chamber, and the exchange chamber is further evacuated. After that, the gate valve is opened, the sample holder is inserted into the sample chamber, and the speculum is positioned. It is arranged to be.

[Problem to be Solved by the Invention] In such a conventional apparatus, the sample must be exposed to the atmosphere before the sample is inserted into the sample chamber of the electron microscope. It reacts and is polluted by trace substances in the atmosphere. Therefore, the sample could not be observed without being affected by the atmosphere. Recently, electron microscopes have been developed to respond to such problems by supplying or processing samples in a chamber separated from the sample exchange chamber and observing them without being affected by the atmosphere. .

However, after introducing a gas from a gas supply source located far from the place where the electron microscope is installed and reacting with the vapor-deposited sample, the sample is set at a microscope position such as an electron microscope without being exposed to the air at all. The sample could not be observed.

An object of the present invention is to provide an electron microscope or similar device that can solve such a conventional problem.

[Means for Solving the Problems] According to a first aspect of the present invention, a sample exchange chamber connected to a sample chamber via a first gate valve and a sample holder inserted into the exchange chamber are provided inside the sample chamber. An electronic device comprising: a transfer mechanism for transferring the sample to an observation position; and a sample processing chamber detachably connected to the exchange chamber via a second gate valve and having a holding unit for holding the sample holder therein. A microscope or a similar device, means for introducing an atmospheric gas into the sample processing chamber, means for heating a sample mounting portion of a sample holder held in the sample processing chamber, and means for depositing a sample on the sample mounting portion. It is characterized in that a vapor deposition means is provided.

According to a second aspect of the present invention, a laser transmission window is provided in the sample processing chamber, a sample is irradiated with a laser beam through the window, and the sample is evaporated by heating the laser beam to be deposited on the mounting portion. 1 characterized by an electron microscope or similar device.

A third aspect of the present invention is characterized in that an ion gun or a vapor deposition source is detachably provided on a wall of the sample processing chamber so as to look at a sample surface of a sample holder held in the sample chamber.

[Example] Hereinafter, an example of the present invention will be described in detail with reference to the drawings.

FIG. 1 is a diagram for explaining an embodiment of the present invention, and FIG.
The figure is an enlarged view of a main part of the present invention.

In FIG. 1, 1 is a lens barrel of an electron microscope, 2 is a sample chamber, 3 is a sample stage having a hole 4 for inserting a sample holder, and 5 is an objective lens. The lens barrel 1 is provided with a sample transfer chamber 6 that can communicate with the sample chamber 2 via a gate valve 7. The sample transfer chamber 6 is connected to a vacuum exhaust system (not shown) via an exhaust pipe 8. 9 is a vacuum valve. Ten
Is a transfer rod of the sample holder, and a claw 11 for holding the sample holder is attached to the tip of the transfer rod 10. Transfer rod
An operation shaft 12 is passed through the inside of 10, so that the claw 11 can be opened and closed. Reference numeral 13 denotes a sample processing chamber having a holder 22 for holding a sample holder 21 therein. Reference numeral 14 denotes a sample holder insertion / removal opening of the sample processing chamber. An exhaust pipe 16 is attached to the sample processing chamber 13, and a vacuum valve 17 is attached to the exhaust pipe 16. Further, the gas introduction pipe 37 connected to the gate valve 36 can be connected to the gas supply chamber by a connector (not shown). Reference numeral 18 denotes a connection opening formed in the sample transfer chamber wall for connecting the sample processing chamber 13. FIG. 1 shows a state in which the sample holder insertion / removal opening 14 of the sample processing chamber 13 is joined to the connection opening 18. A concave portion 19 is provided in the chamber 13, and a stopper 20 is attached to the chamber wall of the sample transfer chamber 6.

The internal structure of the sample processing chamber 13 will be described with reference to FIG. 2 (an enlarged view of a main part) in which the same components as those in FIG.

A sample holder 21 is accommodated in a sample holder holding section 22 inside the sample processing chamber 13. Further, around the speculum sample mounting portion 23 at one end of the sample holder 21,
A cylindrical sample heater 24 is attached to the sample holder holder 22 via a thermal insulator 25. 26 is the sample mounting part
A thermocouple attached to contact 23. An evaporation sample table 27 is provided at a position facing the speculum sample mounting section 23, and the evaporation sample table 27 can be heated by a sample heating heater 28 on the back surface thereof. A thermocouple 29 is attached to the evaporation sample stage 27 for measurement. Further, a shutter 30 operable from the outside of the sample processing chamber 13 is mounted between the evaporation stage 27 and the sample mounting portion 23.

In addition, a laser transmission window 31 is provided on the side wall of the sample processing chamber 13 so as to look into the central portion of the evaporation sample table 27. The holding section 22 is integrally fixed to a transfer rod 32 for transferring the sample holder. Transfer rod 32 is O-ring 33
The heating lead wire 34 and the thermocouple lead wire 35 are buried inside. The gas introduction pipe 37 connected to the gate valve 36 can be connected to the gas supply chamber by a connector (not shown).

In such a configuration, first, in a state where the sample processing chamber 13 is separated from the sample transfer chamber 6, the speculum sample mounting portion 23
After the sample holder 21 having the sample support membrane through which the electron beam can pass is attached to the holder 22, the gate valve 15 is closed. Then, the vacuum valve 17 is opened, and the inside of the sample processing chamber 13 is evacuated by a vacuum pump (not shown) connected to the exhaust pipe 16. After that, the gate valve 36 for gas pressure adjustment connected to the gas supply source
Is adjusted to introduce, for example, exhaust gas into the sample processing chamber 13. Next, power is supplied to the sample heater 24, and the temperature of the sample supporting film is adjusted using the thermocouple 26. A sample for evaporation is previously mounted on a central portion of the sample table 27 for evaporation. Note that this sample was placed on the evaporation stage 27 with the laser transmission window 31 removed in advance. The sample is heated and evaporated by a laser beam emitted from a laser oscillator (not shown) through the laser transmission window 31.

A part of the substance evaporated by the heating adheres to the support film, and the amount (film thickness) of the substance adheres to an arbitrary value by a shutter 30 provided between the evaporating sample stage 27 and the sample mounting part 23. Can be controlled. Here, the sample heating heater 28 can be used as a heating source of the sample for evaporation.

As a result, the evaporated sample reacts with the gas introduced into the sample processing chamber 13 at a desired temperature and is deposited on the support film to produce a sample for a microscope.

After the preparation of the sample, the gate valve 36 is closed and the vacuum valve 17 is opened. After the inside of the sample processing chamber 13 is sufficiently evacuated, the vacuum valve 17 is closed. Next, with the sample holder insertion opening 14 of the sample processing chamber 13 connected to the connection opening 18 of the sample transfer chamber 6,
Is turned into the recess 19, and the sample processing chamber 13 is moved to the sample transfer chamber 6.
Airtightly through an O-ring 38. Then, the vacuum valve 9 is opened, and the inside of the sample transfer chamber 6 is evacuated through the exhaust pipe 8. When the degree of vacuum in the sample transfer chamber 6 rises, the gate valve
15 is opened, the sample transfer rod 32 is raised, and the sample holder 21 is inserted into the sample transfer chamber 6. Then, after operating the operating shaft 12 to clamp the sample holder 21 with the claw 11, the gate valve 7 is opened, and the sample holder 21 is moved by the transfer rod 10 to the sample stage 3.
Carry it up and set it at the microscope position.

In this way, a gas is introduced from a gas supply source located away from the installation place of the electron microscope, etc., and reacted with the deposited sample, and then moved to the microscopic position of the electron microscope without being exposed to the atmosphere at all. Because a sample can be set,
The vapor deposition sample can be observed by causing a gas reaction in a state not affected by the atmosphere or the like.

Note that the above-described embodiment is merely an embodiment of the present invention, and can be modified and implemented.

For example, the above-described embodiment shows an example in which the evaporated substance is coated on the heated sample support film to a required thickness, but the sample previously placed on the sample mounting portion is heated to a high temperature to react with the gas. The present invention can be similarly applied to a case where a sample on which a process such as etching is performed on a sample surface is observed without being affected by the atmosphere. In the present invention, a laser irradiation method using a laser transmission window and a resistance heating method using a laser transmission window as a heating source for the evaporated sample can be used. In addition, it is possible to evaporate from a very small area, and it becomes possible to select the evaporating substance. Here, the sample processing chamber 13
If an ion gun 39 and an evaporation source (not shown) are detachably provided on the sample processing chamber wall so as to look at the sample surface of the sample holder 21 held therein, the sample is already deposited on the sample support film by evaporation or the like. The sample that has been formed can be subjected to ion etching, ion implantation, deposition of another substance, or the like.

Furthermore, an adapter that allows the sample holder for the electron microscope in the above-described example apparatus to be mounted as it is is provided on a sample holding device of a scanning electron microscope or an Auger electron spectrometer, and the sample holder inserted into the exchange chamber is attached to the adapter. By providing a transfer mechanism for transferring the sample to the sample holding device via the sample exchange chamber and detachably connecting the sample processing chamber to the sample exchange chamber, the same sample can be scanned and scanned by an electron microscope or an Auger after the observation by the electron microscope. It can be observed or analyzed by an electron spectroscope.

[Effects of the Invention] As is clear from the above description, according to the first aspect of the present invention, the sample exchange chamber connected to the sample chamber via the first gate valve, and the sample inserted into the exchange chamber A sample having a transfer mechanism for transferring a holder to an observation position in the sample chamber, and a holding unit for holding the sample holder in an interior detachably connected to the exchange chamber via a second gate valve. An electron microscope or a similar device having a processing chamber, means for introducing an atmospheric gas into the sample processing chamber, means for heating a sample mounting portion of a sample holder held in the sample processing chamber, and the sample mounting portion Since a vapor deposition means for vapor-depositing the sample is provided, a gas is introduced from a gas supply source located at a location remote from an electron microscope or the like to react with the vapor-deposited sample. Microscope, etc. A vapor-deposited sample that has undergone a gas reaction can be set at a speculum position for observation.

Further, according to the second aspect of the present invention, the sample processing chamber is provided with a laser transmission, the sample is irradiated with a laser beam through the window, the sample is evaporated by heating the laser beam, and the sample is evaporated on the mounting portion. Therefore, only the sample processing room was moved to the installation room of the heating laser facility, which was far from the installation site of the electron microscope, etc., and the microscope sample was evaporated by the laser. After introducing a gas from the gas supply source in the above to the sample processing chamber and reacting with the deposition metal, set the deposition sample that has undergone the gas reaction at the microscope position such as an electron microscope without exposing it to the atmosphere at all. This sample can be observed.

Further, according to the third aspect of the present invention, an ion gun or a vapor deposition source is detachably provided on a wall of the sample processing chamber so as to look into a sample surface of a sample holder held in the sample chamber, so that a sample supporting film is provided. Immediately after vapor deposition of the sample, ion etching, ion implantation, vapor deposition of another substance, or the like can be performed on the sample already formed thereon.

[Brief description of the drawings]

FIG. 1 is a view showing a main part of an embodiment of the present invention, and FIG. 2 is a view showing a state where a sample processing chamber is connected to a sample supply chamber. 1: barrel, 2: sample chamber 3: sample stage, 4: hole 5: objective lens, 6: sample transfer chamber 7, 15: gate valve, 8, 16: exhaust pipe 9, 17: vacuum valve, 10: transfer Bar 11: Claw, 12: Operation shaft 13: Sample processing chamber 14: Sample holder insertion / removal opening 18: Connection opening 19: Concave, 20: Clamp 21: Sample holder 22: Sample holder holder 23: Microscope sample holder 24: Sample heater 25: Thermal insulator, 26, 29: Thermocouple 27: Sample evaporator 28: Sample heater 30: Shutter, 31: Laser transmission window 32: Transfer rod, 33, 38: O-ring 34 : Lead wire for heater 35: Lead wire for thermocouple 36: Gate valve for adjusting gas pressure 37: Gas inlet tube 39: Ion gun 40: Screw

 ──────────────────────────────────────────────────続 き Continuing from the front page Examiner Naoyuki Nakamura (56) References Japanese Utility Model Sho-59-152560 (JP, U) Japanese Utility Model Sho 50-157152 (JP, U)

Claims (3)

(57) [Claims] A sample exchange chamber connected to the sample chamber via a first gate valve; a transfer mechanism for transferring a sample holder inserted into the exchange chamber to an observation position in the sample chamber;
An electron microscope or a similar device having a sample processing chamber detachably connected to the exchange chamber via a second gate valve and having a holding portion for holding the sample holder therein, Means for introducing atmospheric gas;
An electron microscope or a similar device, comprising: means for heating a sample mounting portion of a sample holder held in the sample processing chamber; and vapor deposition means for vapor depositing a sample on the sample mounting portion. 2. A laser transmission window is provided in said sample processing chamber,
2. An electron microscope or a similar device according to claim 1, wherein the sample is irradiated with a laser beam through the window, and the sample is evaporated by heating the laser beam to be deposited on the sample mounting portion. 3. An ion gun or a vapor deposition source is detachably provided on a wall of the sample processing chamber so as to look into a sample surface of a sample holder held in the sample chamber.
Or an electron microscope or similar device according to 2.