JP2004342401A - Sample exchanging device in transmission electron microscope - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a sample exchanging device of a transmission electron microscope capable of simply and precisely mounting a sample cartridge on a sample holder. <P>SOLUTION: When an inside of a main exhaust chamber 5 is exhausted up to a given high degree of vacuum, a gate valve 6 is opened for exchange of a sample, and a control circuit 26 recognizes by an operation of a microswitch 9 that the gate valve 6 is opened. When the control circuit 26 recognizes the opening of the gate valve 6, a goniometer drive circuit 25 is controlled to a tilt angle of the sample toward a direction of a position X from among sample exchanging positions X, Y, Z memorized and sets the sample holder 2 at the tip of the goniometer on the sample exchanging position. Later, a conveying rod 17 is pushed out into an inside of a lens-barrel 1, an end of the sample cartridge 15 is inserted into an opening at the tip of the sample holder 2, and the sample cartridge is fixed to the sample holder 2. After the sample cartridge is fixed to the sample holder 2, the conveying rod 17 releases chucking of the sample cartridge and pulls back the conveying rod alone into the main exhaust chamber 5. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a sample exchange device in a transmission electron microscope in which a sample cartridge having a sample mounted thereon is transported from the atmosphere and is attached to and detached from a tip of a sample holder in a lens barrel maintained in a vacuum.
[0002]
[Prior art]
FIG. 1 shows a sample exchange device in a conventional transmission electron microscope. FIG. 1 shows a cross section of a lens barrel of an electron microscope to which a sample exchange mechanism is attached. In the figure, reference numeral 1 denotes a lens barrel, and an electron beam generated and accelerated by an electron gun (not shown) is irradiated to a sample attached to the sample holder 2 from a direction perpendicular to the plane of the drawing.
[0003]
The sample holder 2 is fixed to a goniometer 3 provided in a part of the lens barrel 1, and although not shown in detail, the sample mounted on the tip of the sample holder 2 is parallel to the paper surface by the goniometer 3. It is configured to be movable in a suitable XY direction and a Z direction perpendicular to the paper surface. Further, the sample is configured so that it can be tilted by the goniometer 3.
[0004]
The sample exchange mechanism 4 is mounted at a position symmetrical to the mounting position of the goniometer 3 of the lens barrel 1. The sample exchange mechanism 4 has a main exhaust chamber 5 communicating with the inside of the lens barrel 1, and a first gate valve 6 is provided between the main exhaust chamber 5 and the inside of the lens barrel 1. Therefore, by opening the first gate valve 6, the main exhaust chamber 5 and the inside of the lens barrel 1 communicate with each other, and by closing the first gate valve 6, the main exhaust chamber 6 and the inside of the lens barrel 1 are evacuated. It becomes an independent state.
[0005]
A preliminary exhaust chamber 7 is attached to one end of the main exhaust chamber 5. A second gate valve 8 is provided between the preliminary exhaust chamber 7 and the main exhaust chamber 5. Therefore, by opening the second gate valve 8, the main exhaust chamber 5 communicates with the inside of the preliminary exhaust chamber 7, and by closing the second gate valve 8, the main exhaust chamber 6 and the inside of the preliminary exhaust chamber 7 communicate with each other. Are made vacuum independent. A micro switch 9 is attached to the gate valve 6 so that the valve OPEN / CLOSE of the gate valve 6 can be identified.
[0006]
The main exhaust chamber 5 is provided with an exhaust pipe 11 connected to a diffusion pump (not shown), and the interior of the main exhaust chamber 5 is maintained at a relatively high degree of vacuum by the diffusion pump. The preliminary exhaust chamber 7 is provided with an exhaust pipe 12 connected to a rotary pump (not shown), and the inside of the preliminary exhaust chamber 7 is maintained at a relatively low vacuum by the rotary pump.
[0007]
A transfer holder 13 is provided in the preliminary exhaust chamber 7, and a sample cartridge 15 on which a sample 14 is mounted is mounted on the transfer holder 13. The transfer holder 13 on which the sample cartridge 15 is placed is movable by a rod 16 in the vertical direction of the drawing. In the main exhaust chamber 5, a transport rod 17 for chucking the sample cartridge 15 and moving the sample cartridge 15 in a direction parallel to the paper surface is provided.
[0008]
In order to move the transfer holder 13 and the transport rod 17 from outside the vacuum into the main exhaust chamber 5 and the preliminary exhaust chamber 7 that are evacuated to vacuum, for example, an opening portion of the main exhaust chamber 5 where the transport rod 17 moves. An O-ring seal 18 is attached to an opening of the transfer chamber 13 and the transfer chamber 13 in the pre-evacuation chamber 7. This prevents the degree of vacuum in the main exhaust chamber 5 and the preliminary exhaust chamber 7 from being reduced. The transport rod 17 is movable while always being thermally connected to a heat conductive member 20 thermally connected to a tank 19 in which liquid nitrogen is sealed. The operation of such a configuration will now be described.
[0009]
First, a procedure for transporting the sample 14 to the sample holder 2 in the lens barrel 1 for microscopy will be described. First, the gate valves 8 and 6 are set in the CLOSE state, and the transfer holder 13 on which the sample cartridge 15 on which the sample 14 is mounted is loaded into the preliminary exhaust chamber 7. Thereafter, the inside of the preliminary exhaust chamber 7 is exhausted by the rotary pump through the exhaust pipe 12. The degree of vacuum in the preliminary exhaust chamber 7 is monitored, and when the degree of vacuum reaches a predetermined degree, the gate valve 8 is set to the OPEN state, and the transfer holder 13 is introduced into the main exhaust chamber 5 using the rod 16.
[0010]
The inside of the main exhaust chamber 5 is maintained at a relatively high degree of vacuum by a diffusion pump. After the transfer holder 13 is moved to a predetermined position, the movement of the transfer rod 17 is controlled such that the transfer rod 17 is moved so that the tip of the transfer rod 17 reaches the transfer position of the transfer holder 13. In this state, the sample cartridge 15 is held at the tip of the transport rod 17 by an appropriate chuck mechanism at the tip of the transport rod 17. After the sample cartridge 15 is held at the tip of the transport rod, the transfer holder 13 is pulled back into the preliminary exhaust chamber 7, and the gate valve 8 is set to CLOSE.
[0011]
When the gate valve 8 is in the CLOSE state, the inside of the main exhaust chamber 5 is evacuated to a higher degree of vacuum by a diffusion pump (not shown) via the exhaust pipe 19. At this time, the transport rod 17 is cooled via the heat conducting member 20 connected to the tank 19 containing liquid nitrogen. As a result, the sample cartridge 15 and the sample 14 are also cooled to the liquid nitrogen temperature.
[0012]
When the degree of vacuum inside the main exhaust chamber 5 is exhausted to a predetermined high vacuum degree, the gate valve 6 is opened, and the transport rod 17 is inserted into the lens barrel 1. A sample cartridge 15 with a sample 14 held at the tip of a transport rod 17 in the lens barrel 1 is mounted on a sample holder 2 fixed to the goniometer 3. The transport of the sample cartridge 15 and the mounting of the sample cartridge 15 on the sample holder 2 are performed while manually controlling the transport rod of the sample exchange mechanism 4.
[0013]
Conversely, when taking out the sample whose microscope has been completed to the outside from the lens barrel 1, the transport rod 17 is inserted to the position of the sample holder 2 at the tip of the goniometer 3, and the sample cartridge 15 is chucked at the tip of the rod 17. Thereafter, the transport rod is pulled out of the lens barrel 1 and the gate valve 6 is closed. Thereafter, the gate valve 8 is opened, and the transfer holder 13 is introduced into the main exhaust chamber 5. Then, the sample cartridge 15 that has been chucked by the transport rod 17 is placed on the transfer holder 13, and by pulling out the rod 16 of the transfer holder 13, the sample 14 is taken out into the preliminary exhaust chamber 7. When the transfer holder 13 is returned into the preliminary exhaust chamber 7, the gate valve 8 is manually closed to maintain the degree of vacuum in the main exhaust chamber 5.
[0014]
The details of a method for introducing such a sample into a sample holder attached to the goniometer by introducing it from the opposite side of the goniometer are described in detail in, for example, Patent Document 1.
[0015]
[Patent Document 1]
JP-A-11-185686
[0016]
[Problems to be solved by the invention]
In the method of exchanging the sample with the configuration shown in FIG. 1, the sample exchange position in the lens barrel 1 and the optimum image observation position are often different, and each time the sample exchange is performed, the sample holder 2 is moved to the sample exchange position. It must be moved and then moved to the optimal position for image observation. Such an operation is troublesome, and there are cases where the sample exchange position and the optimal image observation position are incorrect.
Further, the sample cartridge insertion opening of the sample holder 2 is narrowed in consideration of the fixation of the sample cartridge 15, so that the goniometer cannot be removed unless the goniometer is accurately moved to the sample replacement position. If the sample cartridge 15 is to be mounted on the sample holder 2 when the goniometer is not moved to the sample exchange position, in the worst case, the sample holder 2 is damaged or the sample cartridge 15 is moved to the lens barrel 1. Drop inside. Further, if the sample cartridge 15 is to be removed from the sample holder 2 when the goniometer has not moved to the sample replacement position, the sample holder 2 will be damaged in the worst case.
[0017]
The present invention has been made in view of such a point, and an object of the present invention is to eliminate a risk of breakage of a sample holder and to easily and accurately mount a sample cartridge on a sample holder by using a sample exchange of a transmission electron microscope. The realization of the device.
[0018]
[Means for Solving the Problems]
A sample exchange device in a transmission electron microscope according to the invention according to claim 1, wherein the sample holder is inserted into the lens barrel from one of the lens barrels and the sample mounted on the sample holder is moved at least in the X, Y, and Z directions. And a sample exchange mechanism provided in a lens barrel portion facing the goniometer, and a sample transport rod for transporting a sample to be observed from the sample exchange mechanism onto a sample holder. In the apparatus, a goniometer is operated to obtain a sample exchange position, a storage means for storing the position data, a gate valve for separating the exhaust chamber and the barrel included in the sample exchange mechanism, and data for opening and closing the gate valve. Opening / closing data generating means for supplying the sample exchange position data and gate valve opening / closing data, and controlling the position of the goniometer based on the gate valve opening / closing data. And a control device for automatically moving the sample position of the goniometer to the sample exchange position. By accurately obtaining and storing the sample exchange position in advance, the goniometer is accurately moved to the sample exchange position. The sample exchange can be performed accurately without damaging the sample holder.
[0019]
According to a second aspect of the present invention, there is provided a sample exchange apparatus for a transmission electron microscope according to the first aspect, wherein the goniometer is operated to determine an optimal image observation position and store the position data. After the sample is set in the sample holder, the goniometer is controlled by the control device, and the sample is automatically moved to the optimal position for image observation, so that sample exchange can be performed accurately and image observation can be performed. The sample can be accurately and automatically moved to the optimum position.
[0020]
According to a third aspect of the present invention, there is provided a sample exchange apparatus for a transmission electron microscope. A main exhaust chamber connected thereto; and a preliminary exhaust chamber connected to the main exhaust chamber and the second gate valve in a vacuum manner. A sample cartridge in which a sample is set is first introduced into the preliminary exhaust chamber. After evacuating the preliminary exhaust chamber to a predetermined degree of vacuum, the second gate valve is opened, the sample cartridge is introduced into the main exhaust chamber, the second gate valve is closed, and the main exhaust chamber is evacuated to a high vacuum; After the evacuation chamber is evacuated to a predetermined degree, the first gate valve is opened, and the sample cartridge is transported to the sample holder position of the goniometer that has been moved to the sample exchange position. As a result, the sample can be exchanged while maintaining the vacuum in the lens barrel at a high level, and the inside of the lens barrel can be maintained in a clean environment.
[0021]
According to a fourth aspect of the present invention, there is provided a sample exchange device in a transmission electron microscope according to the third aspect of the present invention, wherein a sample cartridge is attached to a tip of a transport rod in the exhaust chamber, and a first gate valve is opened at the time of sample exchange. The transfer rod is moved to move the sample cartridge to the sample exchange position, and a part of the transfer rod is supported by a heat conducting member to cool the heat conducting member. . As a result, it becomes possible to observe the sample in a state where it is cooled to the temperature of liquid nitrogen.
[0022]
According to a fifth aspect of the present invention, there is provided a sample exchange apparatus in a transmission electron microscope according to the first to fourth aspects of the present invention, wherein the opening and closing data generating means for the gate valve is provided by opening and closing a gate valve for partitioning between the main exhaust chamber and the lens barrel. It is characterized by using a microswitch for generating a signal.
[0023]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. FIG. 2 shows an example of a sample exchange device in an electron microscope according to the present invention, and the same or similar components as those in the conventional device in FIG. 1 are denoted by the same reference numerals. In FIG. 2, reference numeral 1 denotes a lens barrel, and an electron beam generated and accelerated by an electron gun (not shown) is irradiated to the sample holder 2 in a direction perpendicular to the plane of the drawing.
[0024]
The sample holder 2 is fixed to a goniometer 3 provided in a part of the lens barrel 1, and although not shown in detail, the sample mounted on the tip of the sample holder 2 is parallel to the paper surface by the goniometer 3. It is configured to be movable in a suitable XY direction and a Z direction perpendicular to the paper surface. Further, the sample is configured so that it can be tilted by the goniometer 3. The goniometer 3 is connected to a goniometer drive circuit 25 that drives the goniometer 3, moves the sample in the sample holder 2 in the X, Y, and Z directions, and drives the sample to tilt in the X direction.
[0025]
The drive circuit 25 is connected to a control circuit 26 for controlling the operation of the drive circuit. The control circuit 26 is connected with a personal computer 27, a CRT 28, and an input device 29 such as a mouse and a keyboard as a human interface for exchanging information, data, and the like with an operator, and instructing operations.
[0026]
By the operation from the input device 29, the positions in the X, Y, and Z directions, which are the sample exchange positions, and the inclination angles of the sample in the X direction are stored, and when the sample cartridge 15 is mounted on the sample holder 2, Reads out the sample exchange position stored in the personal computer 27, that is, the position in the X, Y, and Z directions, and the tilt angle of the sample in the X direction by the control circuit 26, and based on the read data, the goniometer The drive circuit 25 is controlled to move the sample to the sample exchange position.
[0027]
The image observation optimum position (Z-direction position) is also stored by the operation from the input device 29. After the sample is mounted on the sample holder 2, the control circuit 26 controls the goniometer drive circuit 25 via the goniometer drive circuit 25. , The goniometer 2 is driven, and the sample moves to the Z direction position, which is the optimal position for image observation.
[0028]
The sample exchange mechanism 4 is mounted at a position symmetrical to the mounting position of the goniometer 3 of the lens barrel 1. The sample exchange mechanism 4 has a main exhaust chamber 5 communicating with the inside of the lens barrel 1, and a first gate valve 6 is provided between the main exhaust chamber 5 and the inside of the lens barrel 1. Therefore, by opening the first gate valve 6, the main exhaust chamber 5 communicates with the inside of the lens barrel 1, and by closing the first gate valve 6, the main exhaust chamber 5 and the inside of the lens barrel 1 become vacuum. It becomes an independent state.
[0029]
The first gate valve 6 is provided with a microswitch 9 that operates in OPEN / CLOSE of the gate valve 6. The microswitch 9 is connected to a control circuit 26, and the control circuit 26 is configured to recognize OPEN / CLOSE of the gate valve 6. On the other hand, the position of the sample 14 is stored in the control circuit 26 by storing the position of the goniometer when the operation for storing the position is performed from the input device 29 together with the sample exchange position and the optimal image observation position.
[0030]
When an operation for storing the sample exchange position is performed from the input device 29, the sample position at that time in the X, Y, and Z directions and the inclination angle of the sample in the X direction are stored in the control circuit 26 as the sample exchange position. You. When an operation for storing the sample exchange position is performed from the input device 29, the data of the sample exchange position in the X, Y, and Z directions and the tilt angle of the sample in the X direction stored by the control circuit 26 are stored in the goniometer drive circuit 25. And the goniometer 3 is driven to set the sample 14 attached to the sample holder 2 at the tip of the goniometer 3 at the sample exchange position.
[0031]
When an operation for storing the optimal image observation position is performed from the input device 29, the sample position Z at that time is stored in the control circuit 26 as the optimal image observation position. When an operation for moving the sample 14 to the optimum image observation position is performed by the input device 29, the control circuit 26 controls the goniometer driving circuit 25 to the optimum image observation position Z stored, and the sample 3 at the tip of the goniometer 3 is imaged. Set to the optimal position for observation.
[0032]
A preliminary exhaust chamber 7 is attached to one end of the main exhaust chamber 5. A second gate valve 8 is provided between the preliminary exhaust chamber 7 and the main exhaust chamber 5. Therefore, by opening the second gate valve 8, the main exhaust chamber 5 communicates with the inside of the preliminary exhaust chamber 7, and by closing the second gate valve 8, the main exhaust chamber 6 and the inside of the preliminary exhaust chamber 7 communicate with each other. Are made vacuum independent.
[0033]
The main exhaust chamber 5 is provided with an exhaust pipe 11 connected to a diffusion pump (not shown), and the interior of the main exhaust chamber 5 is maintained at a relatively high degree of vacuum by the diffusion pump. The preliminary exhaust chamber 7 is provided with an exhaust pipe 12 connected to a rotary pump (not shown), and the inside of the preliminary exhaust chamber 7 is maintained at a relatively low vacuum by the rotary pump.
[0034]
A transfer holder 13 is provided in the preliminary exhaust chamber 7, and a sample cartridge 15 on which a sample 14 is mounted is mounted on the transfer holder 13. The transfer holder 13 on which the sample cartridge 15 is placed is movable by a rod 16 in the vertical direction of the drawing. In the main exhaust chamber 5, a transport rod 17 for chucking the sample cartridge 15 and moving the sample cartridge 15 in a direction parallel to the paper surface is provided.
[0035]
In order to move the transfer holder 13 and the transport rod 17 from outside the vacuum into the main exhaust chamber 5 and the preliminary exhaust chamber 7 that are evacuated to vacuum, for example, an opening portion of the main exhaust chamber 5 where the transport rod 17 moves. An O-ring seal 18 is attached to an opening of the transfer chamber 13 and the transfer chamber 13 in the pre-evacuation chamber 7. This prevents the degree of vacuum in the main exhaust chamber 5 and the preliminary exhaust chamber 7 from being reduced. The transport rod 17 is movable while always being thermally connected to a heat conductive member 20 thermally connected to a tank 19 in which liquid nitrogen is sealed. The operation of such a configuration will now be described.
[0036]
First, a case where the sample cartridge 15 in the atmosphere is mounted on the sample holder 2 provided in the lens barrel 1 having a relatively high vacuum degree and an image observation is performed will be described. That is, a procedure for transporting the sample 14 to the sample holder 2 in the lens barrel 1 for microscopy will be described. First, the transfer holder 13 on which the sample cartridge 15 on which the sample 14 is mounted is loaded into the preliminary exhaust chamber 7. Thereafter, the inside of the preliminary exhaust chamber 7 is exhausted by the rotary pump through the exhaust pipe 12. The degree of vacuum in the preliminary exhaust chamber 7 is monitored, and when the degree of vacuum reaches a predetermined degree, the gate valve 8 is set to the OPEN state, and the transfer holder 13 is introduced into the main exhaust chamber 5 using the rod 17.
[0037]
The inside of the main exhaust chamber 5 is maintained at a relatively high degree of vacuum by a diffusion pump. After the transfer holder 13 is moved to a predetermined position, the movement of the transfer rod 17 is controlled such that the transfer rod 17 is moved so that the tip of the transfer rod 17 reaches the transfer position of the transfer holder 13. In this state, the sample cartridge 15 is held at the tip of the transport rod 17 by an appropriate chuck mechanism at the tip of the transport rod 17. After the sample cartridge 15 is held at the tip of the transport rod, the transfer holder 13 is pulled back into the preliminary exhaust chamber 7, and the gate valve 8 is set to CLOSE.
[0038]
When the gate valve 8 is in the CLOSE state, the interior of the main exhaust chamber 5 is evacuated to a higher degree of vacuum by a diffusion pump (not shown) via the exhaust pipe 11. At this time, the transport rod 17 is cooled via the heat conducting member 20 connected to the tank 19 containing liquid nitrogen. As a result, the sample cartridge 15 and the sample 14 are also cooled to the liquid nitrogen temperature.
[0039]
When the degree of vacuum inside the main exhaust chamber 5 is exhausted to a predetermined high vacuum degree, the gate valve 6 is opened for sample exchange. When the gate valve 6 opens, the control circuit 26 recognizes that the gate valve 6 has opened by the operation of the attached microswitch 9.
[0040]
When the control circuit 26 recognizes that the gate valve 6 has been opened, the control circuit 26 controls the goniometer drive circuit 25 to the stored sample exchange positions in the X, Y, and Z directions and the tilt angle of the sample in the X direction, thereby controlling the goniometer. The tip sample holder 2 is set at the sample exchange position. Thereafter, the transport rod 17 is pushed into the lens barrel 1, one end of the sample cartridge 15 is inserted into the opening at the tip of the sample holder 2, and the sample cartridge 15 is fixed to the sample holder 2.
[0041]
After fixing the sample cartridge to the sample holder 2, the transport rod 17 releases chucking of the sample cartridge, and only the transport rod is pulled back into the main exhaust chamber 5. Thereafter, the gate valve 6 is closed. When the gate valve 6 is closed, the control circuit 26 recognizes that the gate valve 6 is closed and confirms that the sample cartridge 15 is mounted on the sample holder 2 by the operation of the microswitch 9, and then the goniometer driving circuit 25 uses the goniometer drive circuit 25. 3 is controlled so that the sample 14 attached to the sample holder 2 is arranged at the optimum position for image observation. At this stage, the sample is irradiated with an electron beam to observe an image.
[0042]
Next, a procedure for removing the sample cartridge 15 from the sample holder 2 will be described. First, image observation is stopped, irradiation of the sample with the electron beam is stopped, and then the gate valve 6 is opened. When the gate valve 6 opens, the control circuit 26 recognizes that the gate valve 6 has opened by the operation of the attached microswitch 9.
[0043]
When the control circuit 26 recognizes that the gate valve 6 is opened, the control circuit 26 drives the goniometer drive circuit 25 to the stored sample exchange positions in the X, Y, and Z directions and the tilt angle of the sample in the X direction, and the goniometer Is set at the sample exchange position. Thereafter, the transport rod 17 of the sample exchange mechanism 4 is moved from the main exhaust chamber 5 into the lens barrel 1, the sample cartridge 15 is chucked, and the sample cartridge 15 is pulled out from the sample holder 2. Then, the transport rod 17 is pulled back to the left side in the figure, and transports the sample cartridge 15 into the main exhaust chamber 5 for sample replacement. When the sample cartridge 15 is transported to a predetermined position in the main exhaust chamber 5, the gate valve 6 is closed.
[0044]
The transport method of the sample cartridge between the main exhaust chamber 5 and the inside of the lens barrel 1 has been described above. Next, the transport of the sample cartridge 15 between the main exhaust chamber 5 and the preliminary exhaust chamber 7 will be described. explain. When observing a new sample, the transfer holder 13 on which the sample cartridge 15 to which the sample 14 is attached is placed is introduced into the preliminary exhaust chamber 7. Thereafter, the inside of the preliminary exhaust chamber 7 is exhausted by the rotary pump through the exhaust pipe 12. The degree of vacuum in the preliminary exhaust chamber 7 is monitored, and when the degree of vacuum reaches a predetermined degree, the gate valve 8 is set to the OPEN state, and the transfer holder 13 is introduced into the main exhaust chamber 5 using the rod 17.
[0045]
The inside of the main exhaust chamber 5 is maintained at a relatively high degree of vacuum by a diffusion pump. After the transfer holder 13 is moved to a predetermined position, the movement of the transfer rod 17 is controlled such that the transfer rod 17 is moved so that the tip of the transfer rod 17 reaches the transfer position of the transfer holder 13. In this state, the sample cartridge 15 is held at the tip of the transport rod 17 by an appropriate chuck mechanism at the tip of the transport rod 17. After the sample cartridge 15 is held at the tip of the transport rod, the transfer holder 13 is pulled back into the preliminary exhaust chamber 7, and the gate valve 8 is set to CLOSE.
[0046]
When the gate valve 8 is in the CLOSE state, the interior of the main exhaust chamber 5 is evacuated to a higher degree of vacuum by a diffusion pump (not shown) via the exhaust pipe 11. When the degree of vacuum inside the main exhaust chamber 5 is exhausted to a predetermined high vacuum degree, the gate valve 6 is opened, and the sample cartridge 14 is set at a desired position in the lens barrel 1 in the above-described manner.
[0047]
Conversely, when taking out the sample for which the microscopic examination has been completed from the lens barrel 1, the sample cartridge 15 is returned into the main exhaust chamber 5 by the above-described method, and the gate valve 6 is closed. Thereafter, the gate valve 8 is opened, and the transfer holder is introduced into the main exhaust chamber 5. Therefore, the sample cartridge 15 that has been chucked by the transport rod 17 is placed on the transfer holder 13, and the rod 14 of the transfer holder 13 is pulled out, whereby the sample 14 is taken out into the preliminary exhaust chamber 7. When the transfer holder 13 is returned into the preliminary exhaust chamber 7, the gate valve 8 is manually closed to maintain the degree of vacuum in the main exhaust chamber 5.
[0048]
Although the embodiment of the present invention has been described above, the present invention is not limited to this embodiment, and various modifications can be made. For example, the sample exchange mechanism 4 is not limited to the above-described method, and another method may be used.
[0049]
【The invention's effect】
As described above, the sample exchange device in the transmission electron microscope according to the first aspect of the present invention inserts the sample holder into the lens barrel from one of the lens barrels and moves the sample attached to the sample holder into at least X, Y , A goniometer for moving in the Z-direction, and a sample exchange mechanism provided in a lens barrel portion facing the goniometer, and a sample transport rod for transporting a sample to be observed from the sample exchange mechanism onto a sample holder. In a sample exchange device in a transmission electron microscope, a goniometer is operated to determine a sample exchange position and store the position data, a gate valve that separates an exhaust chamber included in the sample exchange mechanism from the inside of the lens barrel, and a gate. Opening / closing data generating means for generating data of opening / closing of the valve, and the sample exchange position data and the opening / closing data of the gate valve are supplied, and based on the gate valve opening / closing data It has a control device that controls the position of the niometer and automatically moves the sample position of the goniometer to the sample exchange position.By accurately finding and storing the sample exchange position in advance, the goniometer can be accurately sampled. The sample can be moved to the exchange position, and the sample exchange can be performed accurately without fear of damaging the sample holder.
[0050]
According to a second aspect of the present invention, there is provided a sample exchange apparatus for a transmission electron microscope according to the first aspect, wherein the goniometer is operated to determine an optimal image observation position and store the position data. After the sample is set in the sample holder, the goniometer is controlled by the control device, and the sample is automatically moved to the optimal position for image observation, so that sample exchange can be performed accurately and image observation can be performed. The sample can be automatically moved to the optimal position.
[0051]
According to a third aspect of the present invention, there is provided a sample exchange apparatus for a transmission electron microscope. A main exhaust chamber connected thereto; and a preliminary exhaust chamber connected to the main exhaust chamber and the second gate valve in a vacuum manner. A sample cartridge in which a sample is set is first introduced into the preliminary exhaust chamber. After evacuating the preliminary exhaust chamber to a predetermined degree of vacuum, the second gate valve is opened, the sample cartridge is introduced into the main exhaust chamber, the second gate valve is closed, and the main exhaust chamber is evacuated to a high vacuum; After the evacuation chamber is evacuated to a predetermined degree, the first gate valve is opened, and the sample cartridge is transported to the sample holder position of the goniometer that has been moved to the sample exchange position. As a result, the sample can be exchanged while maintaining the vacuum in the lens barrel at a high level, and the inside of the lens barrel can be maintained in a clean environment.
[0052]
According to a fourth aspect of the present invention, there is provided a sample exchange device in a transmission electron microscope according to the third aspect of the present invention, wherein a sample cartridge is attached to a tip of a transport rod in the exhaust chamber, and a first gate valve is opened at the time of sample exchange. The transfer rod is moved to move the sample cartridge to the sample exchange position, and a part of the transfer rod is supported by a heat conducting member to cool the heat conducting member. . As a result, it is possible to observe the sample in a cooled state.
[Brief description of the drawings]
FIG. 1 is a diagram showing a conventional sample exchange device.
FIG. 2 is a diagram showing one embodiment of a sample exchange device based on the present invention.
[Explanation of symbols]
1 lens barrel
2 Sample holder
3 Goniometer
4 Sample exchange mechanism
5 exhaust chamber
6, 8 gate valve
7 Spare exhaust chamber
9 Micro switch
11, 12 Exhaust pipe
13 Transfer holder
14 samples
15 Sample cartridge
16 rod
17 Transfer rod
19 Liquid nitrogen tank
20 Heat conductive members
25 Goniometer drive circuit
26 Control circuit
27 Personal Computer
28 CRT
29 Input device

Claims (5)

A goniometer that inserts the sample holder into the lens barrel from one of the lens barrels and moves the sample attached to the sample holder in at least the X, Y, and Z directions, and a sample exchange mechanism provided in the lens barrel facing the goniometer. And a sample exchange device in a transmission electron microscope having a sample transport rod for transporting a sample to be observed from a sample exchange mechanism onto a sample holder, by operating a goniometer to obtain a sample exchange position and determining the position. Storage means for storing data; a gate valve for separating an exhaust chamber and a lens barrel included in the sample exchange mechanism; opening / closing data generating means for generating data for opening / closing the gate valve; Valve opening / closing data is supplied, and the goniometer position is controlled based on the gate valve opening / closing data, and the goniometer sample position is automatically moved to the sample exchange position. Sample changer in the transmission electron microscope having a control device. Operate the goniometer to determine the optimal image observation position and store the position data.After the sample is set in the sample holder of the goniometer, the goniometer is controlled by the controller and the sample is automatically moved to the optimal image observation position. 2. The sample exchange device in a transmission electron microscope according to claim 1, wherein the sample exchange device is configured to cause the sample exchange. The sample exchange mechanism includes a main exhaust chamber that is vacuum-connected to the inside of the lens barrel by a first gate valve, and a preliminary exhaust chamber that is vacuum-connected to the main exhaust chamber by a second gate valve. The sample cartridge in which the sample is set is first introduced into the preliminary exhaust chamber, and after exhausting the preliminary exhaust chamber to a predetermined degree of vacuum, the second gate valve is opened and the sample cartridge is introduced into the main exhaust chamber. The second gate valve is closed, the main exhaust chamber is evacuated to a high vacuum, and after the main exhaust chamber is evacuated to a predetermined degree of vacuum, the first gate valve is opened and the sample cartridge is moved to the sample exchange position. 3. The sample exchange device in a transmission electron microscope according to claim 1, wherein the sample exchange device is configured to be transported to a sample holder position of a goniometer. In this exhaust chamber, the sample cartridge is attached to the tip of the transport rod, and when exchanging the sample, the first gate valve is opened and the transport rod is moved to transport the sample cartridge to the sample exchange position. 4. The sample exchange device in a transmission electron microscope according to claim 3, wherein a part of the rod is supported by a heat conductive member, and the heat conductive member is cooled. The sample exchange in the transmission electron microscope according to any one of claims 1 to 4, wherein the gate valve opening / closing data generating means is a microswitch that generates a signal by opening / closing the gate valve that separates between the main exhaust chamber and the lens barrel. apparatus.

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