JP2009080005A - Sample storage device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample storage device capable of easily preserving samples after preparing cross-section, etc. under vacuum environment and conveying while preserving under vacuum environment. <P>SOLUTION: The sample storage device 1 includes a main case 2 fixed and attached to a processing chamber 21 of a sample preparing device 20 and a detachable case 10. Inner side of a sample preserving chamber 5 and the detachable case 10 can communicate with the processing chamber 21 through a vacuum gate valve. A sample can be preserved under vacuum environment by inserting the sample into the preserving chamber 5 and/or the detachable case 10 and evacuating the processing chamber 21 using an evacuation device equipped by the sample preparing device 20 under a condition opening the vacuum gate valve. When the vacuum gate valve is closed, the sample can be taken out after opening to atmosphere. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

  The present invention relates to a sample storage device for storing a sample that has been irradiated with a charged particle beam to produce a cross section or a sample that is irradiated with a charged particle beam to observe and / or analyze a surface.

  As an apparatus for preparing a sample to be observed with a scanning electron microscope (SEM) or a transmission electron microscope (TEM), for example, a sample preparation apparatus as described in JP 2005-37164 A is known. . This sample preparation apparatus prepares a sample cross section by arranging a shielding material having a linear edge on the sample and etching the sample with an ion beam that passes through the side of the edge and irradiates the sample. be able to. An evacuation apparatus is connected to the processing chamber for producing the cross section so that the evacuation can be performed for the ion beam.

  Some samples may be oxidized or denatured by absorbing moisture in the atmosphere when exposed to the atmosphere for a long time. It may take time until the sample prepared by the ion beam is used for actual observation. Since the sample irradiated with the ion beam has a high temperature and tends to oxidize quickly, it is desirable that the sample be cut off from the atmosphere as soon as possible after the sample is taken out from the processing chamber.

  For example, Japanese Patent Application Laid-Open No. 2003-121322 discloses a technique in which a sample to be observed with a TEM is stored while being vacuum-dried and can be observed in a short time after being mounted on the TEM. .

  Japanese Patent Application Laid-Open No. 2001-171751 discloses a technique related to a portable desiccator that is used for the purpose of moving a small amount of sample under reduced pressure or oxygen-free conditions.

JP-A-2005-37164 JP 2003-121322 A JP 2001-171751 A

  A medium-sized or large-sized desiccator that has been commercially available from the past and a desiccator disclosed in Japanese Patent Application Laid-Open No. 2003-121322 of Patent Document 2 are difficult to carry because they are assumed to be used stationary. In addition, a large vacuum desiccator that collectively stores a large number of samples has the inconvenience that the entire room must be opened to the atmosphere even when a single sample is taken out.

  The portable desiccator disclosed in Japanese Patent Application Laid-Open No. 2001-171751 of Patent Document 3 is a general-purpose small desiccator. For example, when carrying a small amount of sandy sample from a mineral collection site to a laboratory. Is suitable. Therefore, it is necessary to prepare a separate exhaust device that is used to decompress the interior of the portable desiccator.

  On the other hand, since a specific cross section of the sample manufactured by the sample manufacturing apparatus disclosed in Japanese Patent Application Laid-Open No. 2005-37164 of Patent Document 1 is used for observation, it is necessary to store the sample so as to protect the surface. In addition, it is desirable that the sample can be stored in a vacuum immediately after the sample is prepared by the operator.

  The present invention has been made to solve the above-mentioned problems, and its purpose is to minimize the time for exposing a sample, which has been subjected to cross-section preparation using an ion beam, to the atmosphere, and easily in a vacuum environment. It is an object of the present invention to provide a sample storage device that can be stored in a vacuum environment and stored in a place where an observation device such as an SEM or TEM is provided as necessary.

In order to solve the above problem, the invention according to claim 1
A sample storage device for storing a sample to be observed and / or analyzed by irradiation with a charged particle beam,
A main case having a space capable of being evacuated to communicate with an evacuation unit evacuated by an evacuation device;
A detachable case having an internal space for sample storage,
The main case is a plug that incorporates a mechanism for performing a vacuum partition between the evacuation part and the space that can be evacuated, and a first vacuum check valve mechanism for connecting the removable case to the main case. Have a mouth,
The detachable case has a tube opening incorporating a second vacuum check valve mechanism,
The main case can be evacuated via the first vacuum check valve mechanism and the second vacuum check valve mechanism by inserting the cylindrical port of the removable case into the insertion port of the main case. It is characterized in that it communicates with various spaces.

The invention according to claim 2
The space where the main case can be evacuated is communicated with a evacuation unit of a device different from the sample storage device.

The invention according to claim 3
In the first vacuum check valve mechanism and the second vacuum check valve mechanism, when the tube port is inserted into the insertion port, the inside of the removable case and the space where the main case can be evacuated communicate with each other. When the cylindrical port is pulled out from the insertion port in a state where the internal space of the removable case is evacuated, the vacuum of the internal space of the main case is removed by the first vacuum check valve mechanism. And a mechanism that operates so that the internal space of the detachable case is held in a vacuum with respect to the outside by the second vacuum check valve mechanism.

The invention according to claim 4
When the inside of the removable case removed from the main case is in a depressurized state, the atmosphere is brought into the removable sample storage case by pressing the atmosphere side end of the second vacuum check valve mechanism. It is characterized by including a mechanism to be introduced.

The invention according to claim 5
The main case further includes a sample storage space that can be evacuated and opened to the atmosphere.

The invention according to claim 6
A leak mechanism capable of introducing the atmosphere into the sample storage space while the vacuum partitioning mechanism is closed when the sample storage space of the main case is in a decompressed state; It is characterized by providing.

The invention according to claim 7 provides
The main case includes a plurality of insertion ports for inserting the cylindrical ports of the removable case.

The invention according to claim 8 provides
The space for storing the sample of the main case has a lid using a transparent material such as glass or plastic, and when the inside of the space for storing the sample is in a decompressed state, the lid is a vacuum sealing material. It is characterized by being sealed by.

The invention described in claim 9
The detachable case has a lid made of a transparent material such as glass or plastic, and when the inside of the detachable case is decompressed, the lid is sealed with a vacuum sealing material. It is characterized by that.

  According to the present invention, a sample prepared using an ion beam can be immediately stored in a vacuum case, so that a sample that is easily oxidized or a sample that is hygroscopic can be quickly stored. Moreover, since the exhaust system of the existing apparatus can be used as a vacuum exhaust system for obtaining a vacuum environment, an extra installation space is not required and the installation cost can be reduced. In addition, the main case that is fixedly attached to the sample preparation device is combined with the removable case so that the sample can be transported away from the sample preparation device. . In addition, by preparing a plurality of removable cases, each sample can be individually stored in a vacuum environment, and each sample can be individually taken out as an observation sample.

  Embodiments of the present invention will be described below with reference to the drawings. However, the technical scope of the present invention is not limited by this illustration. In each figure, the same reference numerals are given to the same or similar operations, and detailed description is not repeated.

  1 and 2 are perspective views showing an example in which the sample storage device of the present invention is used by being attached to a sample preparation device using an ion beam. In FIG. 1, an ion gun 23 and a stage 24 are incorporated in a processing chamber 21 in a sample preparation device 20, and the inside of the processing chamber 21 can be evacuated and opened to the atmosphere by a vacuum exhaust device and a leak valve (not shown). .

  The sample storage device 1 includes a main case 2 fixedly attached to a sample preparation device 20 and a removable case 10 that can be attached to and detached from the main case 2. FIG. 1 shows a state where the removable case 10 is connected to the main case 2, and FIG. 2 shows a state where the removable case 10 is removed from the main case 2.

  The main case 2 is attached to the opening provided on the outer wall of the processing chamber 21 of the sample preparation device 20 using the adapter 3. The main case 2 is provided with a vacuum gate valve between the processing chamber 21 and the sample storage device 1, and the vacuum gate valve can be opened and closed by operating the open / close knob 4a.

  The main case 2 is provided with a sample storage chamber 5 and can be evacuated through the exhaust hole 5a. The sample storage chamber 5 can be vacuum-sealed by a transparent lid 6 and an O-ring 7. Further, the leak mechanism 8 can be operated to open the atmosphere from the leak hole 5b. The removable case 10 can be vacuum-sealed by a transparent lid 11 and an O-ring 12. The removable case 10 is connected to the main case 2 by inserting the tube port 13 into the insertion port 9. When the tube port 13 is inserted into the insertion port 9, the tip end portion 14a of the leak valve 14 is pushed in the direction of arrow A in FIG. 2, and the vacuum check valve mechanism 15 is opened. When the tube port 13 is pulled out from the insertion port 9, the tip end portion 14 a returns to its original position, and the inside of the removable case 10 is shut off from the outside by the vacuum check valve mechanism 15.

  FIG. 3 is a drawing for explaining the structure of the sample storage device of the present invention in more detail. FIG. 3A is a plan view showing a state in which the main case 2 and the removable case 10 are connected. FIG. 3B is a cross-sectional view showing a BB cross section of FIG. FIG. 3A is a plan view seen from the direction of the arrow D in FIG. FIG. 3C is a cross-sectional view of the removable case 10 corresponding to the CC cross section of FIG. The detachable case 10 shown in FIG. 3A is a plan view seen from the direction of arrow E in FIG.

  In FIG. 3A, a vacuum check valve 9 a is provided in the back of the insertion port 9 of the main case 2. When the tube port 13 of the removable case 10 is inserted into the insertion port 9, the inside of the main case 2 and the inside 10a of the removable case 10 communicate with each other via the vacuum check valve 9a. In addition, when the inside of the main case 2 is in a reduced pressure state and the tube port 13 is pulled out from the insertion port 9, the inside of the main case 2 is held in vacuum with respect to the outside by the vacuum check valve 9a.

In FIG. 3 (c), when the interior 10 a of the removable case 10 is vacuum-sealed, the tip end portion 14 a of the leak valve 14 slightly protrudes from the tube port 13. When the removable case 10 is inserted into the insertion port of the main case 2, the distal end portion 14a of the leak valve 14 is pressed against the abutting portion 9b inside the main case 2, and moves to the position 14a '. That is, when the distal end portion 14a of the leak valve 14 is at the position 14a ', the inside 10a of the removable case 10 is in communication with the outside. Therefore, when the inside 10a of the removable case 10 is in a decompressed state, if the tip portion 14a is pressed, the inside 10a is released to the atmosphere, and if the pressure is stopped, the tip portion 14a is moved from the position 14a 'to the original position by the action of the elastic body. It comes to return to the position.

  Next, a usage example when the sample storage device of the present invention is attached to a sample preparation device will be described.

  When sample preparation is completed in the sample preparation apparatus 20, the processing chamber 21 is opened to the atmosphere, the stage 24 is pulled out, and the sample is taken out. When the prepared sample is put into the sample storage chamber 5 of the main case 2, the lid 6 is opened and the sample is put. At this time, if the sample storage chamber 5 is in a vacuum, the lid 6 is opened after the leak mechanism 8 releases the atmosphere. When storing in the removable case 10, the lid 11 is opened and the sample is placed in the interior 10a. When the inside 10 a of the removable case 10 is evacuated, it is connected to the main case 2. The leak mechanism 8 is closed and the vacuum gate valve 4 is opened.

  If there is a sample for the next sample preparation, it is set in the sample preparation apparatus, the stage 24 is closed, and the processing chamber 21 is evacuated. If there is no sample for subsequent sample preparation or if it is desired to prioritize storing the prepared sample in a vacuum environment, the stage 24 is immediately closed and the processing chamber 21 is evacuated without setting the next sample. Needless to say, you can do it. When the processing chamber 21 is sufficiently evacuated, the vacuum gate valve 4 is closed.

  By the above procedure, the sample placed in the sample storage chamber 5 and the removable case 10 of the main case 2 can be easily stored in a vacuum environment. Further, if necessary, the inside of the removable case 10 can be separated from the main case 2 while keeping the vacuum inside, and only the removable case 10 can be carried to a desired place.

  In the above description, the number of insertion ports provided in the main case 2 is one. However, the main case may be elongated to provide a plurality of insertion ports.

  In the above description, the case where the sample storage device of the present invention is attached to the sample preparation device has been described as an example. However, vacuum evacuation such as SEM, TEM, FIB (focused ion beam device), EPMA (electronic probe microanalyzer), etc. It can also be used by being attached to a vacuum exhaust system of a device having the device, and belongs to the technical scope of the present invention. Furthermore, a dedicated evacuation device may be attached to the sample storage device of the present invention.

The perspective view which shows the example by which the sample storage apparatus of this invention is attached to the sample preparation apparatus. The perspective view which shows the removable case of the state removed from the main case. The figure which shows the detailed structure of the sample storage apparatus of this invention.

Explanation of symbols

(Those that perform the same or similar operations are denoted by a common reference.)
DESCRIPTION OF SYMBOLS 1 Sample storage apparatus 2 Main case 3 Adapter 4 Vacuum gate valve 4a Opening / closing knob 5 Sample storage chamber 5a Exhaust hole 5b Leak hole 6,11 Lid 7,12 O-ring 8 Leak mechanism 9 Insert 9a Vacuum check valve 9b Part 10 Detachable case 13 Tube port 14 Leak valve 14a Tip 15 Vacuum check valve mechanism 20 Sample preparation device 21 Processing chamber 23 Ion gun 24 Stage

Claims (9)

A sample storage device for storing a sample to be observed and / or analyzed by irradiation with a charged particle beam,
A main case having a space capable of being evacuated to communicate with an evacuation unit evacuated by an evacuation device;
A detachable case having an internal space for sample storage,
The main case is a plug that incorporates a mechanism for performing a vacuum partition between the evacuation part and the space that can be evacuated, and a first vacuum check valve mechanism for connecting the removable case to the main case. Have a mouth,
The detachable case has a tube opening incorporating a second vacuum check valve mechanism,
The main case can be evacuated via the first vacuum check valve mechanism and the second vacuum check valve mechanism by inserting the cylindrical port of the removable case into the insertion port of the main case. A sample storage device characterized in that it communicates with a large space. 2. The sample storage device according to claim 1, wherein the vacuum evacuable space of the main case is communicated with a vacuum exhaust unit of a device different from the sample storage device. In the first vacuum check valve mechanism and the second vacuum check valve mechanism, when the tube port is inserted into the insertion port, the inside of the removable case and the space where the main case can be evacuated communicate with each other. When the cylindrical port is pulled out from the insertion port in a state where the internal space of the removable case is evacuated, the vacuum of the internal space of the main case is removed by the first vacuum check valve mechanism. And a mechanism that operates so that the internal space of the detachable case is vacuum-maintained with respect to the outside by the second vacuum check valve mechanism. 2. The sample storage device according to item 1. When the inside of the removable case removed from the main case is in a depressurized state, the atmosphere is brought into the removable sample storage case by pressing the atmosphere side end of the second vacuum check valve mechanism. The sample storage device according to claim 1, further comprising a mechanism to be introduced. The sample storage device according to any one of claims 1 to 3, wherein the main case further includes a space for storing a sample that can be evacuated and opened to the atmosphere. A leak mechanism capable of introducing the atmosphere into the sample storage space while the vacuum partitioning mechanism is closed when the sample storage space of the main case is in a decompressed state; The sample storage device according to claim 5, further comprising: 3. The sample storage device according to claim 1, wherein the main case includes a plurality of insertion ports into which the cylindrical ports of the detachable case are inserted. The space for storing the sample of the main case has a lid using a transparent material such as glass or plastic, and when the inside of the space for storing the sample is in a decompressed state, the lid is a vacuum sealing material. The sample storage device according to any one of claims 5 and 6, wherein the sample storage device is sealed. The detachable case has a lid made of a transparent material such as glass or plastic, and when the inside of the detachable case is decompressed, the lid is sealed with a vacuum sealing material. The sample storage device according to any one of claims 1 to 4, wherein the sample storage device is provided.

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