JP2022069812A - Sample holder and charged particle beam device including the same - Google Patents

Abstract

To provide a sample holder capable of observing a sample exposed to various gas atmospheres without modifying the housing of a charged particle beam device, and a charged particle beam device including the same.SOLUTION: There is provided a sample holder which holds a sample and is inserted through an existing hole of a charged particle beam device. The sample holder includes: a sample installation part where a sample is installed; a gas sealing chamber where a desired gas is sealed; and a movement mechanism moving the sample installation part between inside and outside the gas sealing chamber. The gas sealing chamber has an opening through which the sample installed in the sample installation part passes, and an airtight part which contacts around the opening to keep air tight is provided at the tip of the sample installation part.SELECTED DRAWING: Figure 2A

Description

The present invention relates to a sample holder used in a charged particle beam device.

A charged particle beam device represented by a transmission electron microscope is a device that irradiates a sample with an electron beam accelerated by a high voltage to obtain an observation image of the sample. In recent years, there has been an increasing demand for observing changes in sample morphology and physical properties in different environments. For example, in a catalyst experiment or the like, a sample that has been shielded from the atmosphere is reduced with hydrogen gas, then observed by a charged particle beam device without exposing the sample to the atmosphere, and the sample after being exposed to various gas atmospheres is obtained. Observed again by a charged particle beam device. Further, it may be necessary to observe not only after being exposed to various gas atmospheres but also in various environments such as heating and voltage application.

Patent Document 1 describes a function of changing the state of a sample from the side facing the sample holding portion that holds the sample in order to enable observation in various environments without taking the sample out of the charged particle beam device. Disclosed is a charged particle beam device in which a detachable reverse side entry portion is inserted.

Japanese Unexamined Patent Publication No. 2015-76147

However, in Patent Document 1, it is necessary to provide a hole into which the reverse side entry portion is inserted, in addition to the hole into which the sample holding portion is inserted. That is, it is necessary to modify the housing of the charged particle beam device.

Therefore, an object of the present invention is to provide a sample holder capable of observing a sample exposed to various gas atmospheres and a charged particle beam device including the sample holder without modifying the housing of the charged particle beam device.

In order to achieve the above object, the present invention is a sample holder that holds a sample and is inserted through an existing hole of a charged particle beam device, in which a sample setting portion on which the sample is placed and a desired gas are enclosed. The gas-filled chamber is provided with a moving mechanism for moving the sample mounting portion between the inside and the outside of the gas-filled chamber, and the gas-filled chamber has an opening through which the sample installed in the sample mounting portion passes. It is characterized in that an airtight portion having contact with the periphery of the opening and maintaining airtightness is provided at the tip of the sample mounting portion.

According to the present invention, it is possible to provide a sample holder capable of observing a sample exposed to various gas atmospheres and a charged particle beam device including the sample holder without modifying the housing of the charged particle beam device.

It is a schematic block diagram of a transmission electron microscope which is an example of a charged particle beam apparatus. It is a side sectional view at the time of observing a sample using the sample holder of Example 1. FIG. It is a side sectional view when the sample is exposed to the gas atmosphere by using the sample holder of Example 1. FIG. It is an upper sectional view at the time of observing a sample using the sample holder of Example 1. FIG. It is an upper sectional view when the sample is exposed to the gas atmosphere by using the sample holder of Example 1. FIG. It is a block diagram of the sample holder of Example 2. It is a block diagram of the sample holder of Example 3. FIG. It is a block diagram of the sample holder of Example 4. FIG. It is a block diagram of the sample holder of Example 5.

Hereinafter, the sample holder of the present invention and the charged particle beam apparatus provided with the sample holder will be described with reference to the drawings. The charged particle beam device is a transmission electron microscope, a scanning electron microscope, a focused ion beam device, or the like that generates an observation image of a sample by irradiating the sample with a charged particle beam such as an electron beam. In the following, a transmission electron microscope will be described as an example of a charged particle beam device. In the following description and the accompanying drawings, components having the same functional configuration are designated by the same reference numerals, so that duplicate description will be omitted. Further, in order to show the orientation of each figure, an XYZ coordinate system is added to each figure.

The transmission electron microscope 1 of Example 1 will be described with reference to FIG. The transmission electron microscope 1 has an electron source 4, a focusing lens 5, an objective lens 6, an imaging lens 7, a fluorescent plate 8, a camera 9, a goniometer 10, and an image display unit 2, and the goniometer 10 has a sample holder of Example 1. 11 is inserted.

The electron source 4 includes a cathode that emits the electron beam 3 and an accelerating tube that accelerates the electron beam 3. The focusing lens 5 and the objective lens 6 are lenses that adjust the size of the electron beam 3 irradiated to the sample 13. The objective lens 6 has an upper magnetic pole piece arranged on the side of the electron source 4 and a lower magnetic pole piece arranged on the side of the camera 9 with respect to the sample 13. The imaging lens 7 is a lens that forms an image of electrons transmitted through the sample 13 on the fluorescent screen 8 or the camera 9. The fluorescent plate 8 is a plate that emits fluorescence when electrons that have passed through the imaging lens 7 are incident. The camera 9 captures the fluorescence emitted by the fluorescent plate 8 and the electrons that have passed through the imaging lens 7. The image display unit 2 is a liquid crystal display or the like that displays an observation image captured by the camera 9.

The goniometer 10 is a mechanism for moving the sample holder 11 or the like to be inserted in the direction of the X-axis or rotating it around an axis parallel to the X-axis. The goniometer 10 is not essential, and instead of the goniometer 10, an insertion hole into which the sample holder 11 or the like is inserted may be provided. The gas supply / exhaust section 15 is connected to the goniometer 10 or the sample holder 11 inserted into the insertion hole via the pipes 14a and 14b. The gas supply / exhaust unit 15 is composed of, for example, a gas cylinder filled with hydrogen gas and a vacuum pump for evacuating. Further, valves 16a and 16b for opening and closing the pipes 14a and 14b, respectively, are provided.

The sample holder 11 of the first embodiment will be described with reference to FIGS. 2A, 2B, 3A, and 3B. 2A and 2B are side sectional views, and FIGS. 3A and 3B are upper sectional views. FIGS. 2A and 3A show the sample 13 when observing the sample 13, and FIGS. 2B and 3B expose the sample 13 to a gas atmosphere. Show the time. The sample holder 11 has a sample mounting portion 12, a central shaft 17, an outer cylinder 18, a grip 21, and a moving knob 22. Hereinafter, each part will be described.

The sample setting portion 12 is a member on which the sample 13 is placed, and a first airtight portion 19 for maintaining airtightness, for example, an O-ring is provided at the tip thereof. The sample setting portion 12 is fixed to the central shaft 17.

The central shaft 17 is a cylindrical member, and the sample mounting portion 12 is provided at the tip thereof, and the pipes 14a and 14b are housed inside. A second airtight portion 20, for example, an O-ring for maintaining airtightness is provided on the outer surface of the tip of the central shaft 17. Further, a screw 23, which is a spiral groove, is provided on a part of the outer surface of the central shaft 17. The screw 23 is combined with the inner circumference of the moving knob 22.

The outer cylinder 18 is a cylindrical member, and the central shaft 17 is arranged inside, and the second airtight portion 20 comes into contact with the inner surface. Further, the tip of the outer cylinder 18 is provided with an opening 30 through which the sample 13 installed in the sample setting portion 12 passes. The size of the opening 30 is smaller than the outer diameter of the first airtight portion 19. Further, a grip 21 is provided on the outer surface of the outer cylinder 18. The outer cylinder 18 and the grip 21 are fixed to the goniometer 10 and the insertion hole.

The moving knob 22 is a mechanism for moving the central shaft 17 in the direction of the X axis with respect to the outer cylinder 18, and is provided so as to be rotatable with respect to the grip 21. When the moving knob 22 is rotated with respect to the grip 21, the center pole 17 moves in the direction of the X axis with respect to the outer cylinder 18 via the screw 23, and the sample mounting portion 12 fixed to the center pole 17 is also included. Moving. That is, by operating the moving knob 22, the sample 13 installed in the sample setting unit 12 can be moved between the inside and the outside of the outer cylinder 18.

An example of a procedure for observing a sample exposed to various gas atmospheres by the sample holder 11 of the first embodiment will be described. First, by operating the moving knob 22, the sample 13 installed in the sample setting unit 12 is moved into the outer cylinder 18. While the central shaft 17 continues to move with respect to the outer cylinder 18, the second airtight portion 20 keeps in contact with the inner surface of the outer cylinder 18 to maintain airtightness. Further, when the state illustrated in FIGS. 2B and 3B is reached, the first airtight portion 19 comes into contact with the periphery of the opening 30 to maintain airtightness. As a result, the outer cylinder 18, the first airtight portion 19, and the second airtight portion 20 form a gas encapsulation chamber 18a capable of encapsulating a desired gas. The valves 16a and 16b are both closed.

Next, the valve 16a for gas exhaust is opened, and the gas filling chamber 18a is evacuated by the gas supply / exhaust unit 15. When the gas filling chamber 18a has a sufficient degree of vacuum, the valve 16a for gas exhaust is closed. Then, the valve 16b for supplying gas is opened, and the desired gas is supplied from the gas supply / exhaust unit 15 to the gas filling chamber 18a, so that the sample 13 is exposed to the gas atmosphere.

Next, the valve 16b for gas supply is closed, the valve 16a for gas exhaust is opened, and the gas filling chamber 18a is evacuated by the gas supply / exhaust unit 15. When the gas filling chamber 18a has a sufficient degree of vacuum, the valve 16a for gas exhaust is closed.

Further, by operating the moving knob 22, the sample 13 installed in the sample setting unit 12 is moved to the outside of the outer cylinder 18, that is, the outside of the gas filling chamber 18a. When the sample mounting portion 12 passes between the upper magnetic pole piece and the lower magnetic pole piece of the objective lens 6 and the sample 13 is arranged at a position as illustrated in FIG. 1, the electron beam from the electron source 4 is sent to the sample 13. 3 is irradiated and an observation image is generated. It is preferable that the thickness of the sample setting portion 12, that is, the size in the Z-axis direction is smaller. If the sample mounting portion 12 becomes thinner, the distance between the upper magnetic pole piece and the lower magnetic pole piece of the objective lens 6 can be narrowed, so that the lens strength of the objective lens can be further improved.

After the observation image is generated, the sample 13 may be moved into the outer cylinder 18 by operating the moving knob 22 again, and the sample 13 may be exposed to a new gas atmosphere. That is, by repeatedly exposing the sample 13 to the gas atmosphere inside the gas filling chamber 18a and observing the sample 13 outside the gas filling chamber 18a, it is possible to observe the samples exposed to various gas atmospheres.

As described above, by inserting the sample holder 11 of Example 1 into the goniometer 10 or the insertion hole provided in advance in the transmission electron microscope 1, the sample 13 exposed to the gas atmosphere can be observed without being exposed to the atmosphere. can do. That is, according to the first embodiment, it is provided a sample holder capable of observing a sample exposed to various gas atmospheres without modifying the housing of a charged particle beam device represented by the transmission electron microscope 1. Can be done.

In the first embodiment, the sample 13 installed in the sample setting portion 12 is moved between the inside and the outside of the gas filling chamber 18a formed by the outer cylinder 18, the first airtight portion 19, and the second airtight portion 20. Thereby, it was described to observe the sample 13 exposed to various gas atmospheres. In Example 2, not only the sample 13 is exposed to the gas atmosphere, but also the observation of the sample 13 during or after heating will be described. The description of the same configuration as that of the first embodiment will be simplified by assigning the same reference numerals.

The sample holder 11 of the second embodiment will be described with reference to FIG. A heater 24a, a heater wiring 24b, a heater power supply 24c, a thermometer 25a, a thermometer wiring 25b, and a temperature display unit 25c are added to the sample holder 11 of the second embodiment with respect to the configuration of the first embodiment. ..

The heater 24a is an element for heating the sample 13, and is provided in the sample setting unit 12. Electric power is supplied to the heater 24a from the heater power supply 24c via the heater wiring 24b. The heater wiring 24b is housed inside the central shaft 17 together with the pipes 14a and 14b, and connects the heater 24a and the heater power supply 24c.

The thermometer 25a is a measuring instrument for measuring the temperature of the heater 24a and the sample 13, for example, a thermocouple. The temperature measured by the thermometer 25a is displayed on the temperature display unit 25c transmitted via the thermometer wiring 25b. The thermometer wiring 25b is housed inside the central shaft 17 together with the pipes 14a and 14b, and connects the thermometer 25a and the temperature display unit 25c. The electric power supplied by the heater power supply 24c may be controlled based on the difference between the preset target temperature and the temperature measured by the thermometer 25a.

An observation example of the sample 13 that is exposed to and heated by various gas atmospheres by the sample holder 11 of the second embodiment will be described. For example, by heating the sample 13 arranged in the gas filling chamber 18a to a predetermined temperature and then introducing the gas into the gas filling chamber 18a, the sample 13 exposed to the gas atmosphere after heating is observed. Alternatively, by introducing gas into the gas filling chamber 18a in which the sample 13 is arranged and then heating the sample 13 with the heater 24a, the sample 13 heated after being exposed to the gas atmosphere is observed. Further, the timing of gas introduction and heating may be patterned in advance. By patterning the timing, the sample 13 can be observed in an environment in which various gas atmospheres and heating cycles are combined.

As described above, by inserting the sample holder 11 of Example 2 into the goniometer 10 or the insertion hole, not only the sample holder 11 is exposed to various gas atmospheres, but also the sample 13 during or after heating is exposed to the atmosphere. Can be observed without. That is, according to the second embodiment, it is possible to provide a sample holder capable of observing the sample 13 exposed to various gas atmospheres and heated without modifying the housing of the charged particle beam device.

In Example 1, observing a sample 13 exposed to various gas atmospheres has been described. In Example 3, not only the sample 13 is exposed to the gas atmosphere, but also the sample 13 to which the voltage is applied is observed. The description of the same configuration as that of the first embodiment will be simplified by assigning the same reference numerals.

The sample holder 11 of the third embodiment will be described with reference to FIG. An electrode 26a, an electric wire 26b, and a power supply 26c are added to the sample holder 11 of the third embodiment with respect to the configuration of the first embodiment. The sample 13 is in contact with the tip of the electrode 26a, and a voltage is applied to the sample 13 from the power supply 26c via the electric wire 26b and the electrode 26a. The electric wire 26b is housed inside the central shaft 17 together with the pipes 14a and 14b.

With the sample holder 11 of Example 3, it is possible to observe the sample 13 to which a voltage is applied as well as being exposed to various gas atmospheres. For example, by applying a voltage while exposing the sample 13 arranged in the gas filling chamber 18a to the gas atmosphere, the sample 13 to which the voltage is applied while being exposed to the gas atmosphere is observed. Alternatively, the sample 13 may be moved to a position where the electron beam 3 is irradiated without exposing the sample 13 to the gas atmosphere, and the sample 13 in a state where a voltage is applied may be observed.

As described above, by inserting the sample holder 11 of Example 3 into the goniometer 10 or the insertion hole, not only is the sample holder 11 exposed to various gas atmospheres, but also the sample 13 to which the voltage is applied is not exposed to the atmosphere. Can be observed. That is, according to the third embodiment, it is possible to provide a sample holder capable of observing the sample 13 exposed to various gas atmospheres and to which a voltage is applied without modifying the housing of the charged particle beam device. ..

In Example 1, observing a sample 13 exposed to various gas atmospheres has been described. In Example 4, observing the sample 13 while monitoring the pressure when the sample 13 is exposed to the gas atmosphere will be described. The description of the same configuration as that of the first embodiment will be simplified by assigning the same reference numerals.

The sample holder 11 of the fourth embodiment will be described with reference to FIG. A pressure gauge 27a, a pressure gauge wiring 27b, and a pressure display unit 27c are added to the sample holder 11 of the fourth embodiment with respect to the configuration of the first embodiment.

The pressure gauge 27a is a measuring instrument for measuring the pressure in the gas filling chamber 18a. The pressure measured by the pressure gauge 27a is displayed on the pressure display unit 27c transmitted via the pressure gauge wiring 27b. The pressure gauge wiring 27b is housed inside the center shaft 17 together with the pipes 14a and 14b, and connects the pressure gauge 27a and the pressure display unit 27c. The operation of the gas supply / exhaust unit 15 and the opening / closing of the valves 16a and 16b may be controlled based on the difference between the preset target pressure and the pressure measured by the pressure gauge 27a.

The sample holder 11 of the fourth embodiment not only exposes the sample to various gas atmospheres, but also allows the sample 13 to be observed while keeping the pressure of the gas filling chamber 18a constant. That is, it is possible to provide a sample holder capable of observing the sample 13 exposed to various gas atmospheres maintained at a constant pressure without modifying the housing of the charged particle beam device.

In Example 1, it has been described that the sample holder 11 is inserted into the transmission electron microscope 1 and used. The sample holder 11 may be used by being inserted into a device other than the transmission electron microscope 1. In Example 5, the sample holder 11 is inserted into a focused ion beam device for processing and observing a sample by irradiating it with an ion beam, and the sample holder 11 will be described. The description of the same configuration as that of the first embodiment will be simplified by assigning the same reference numerals.

The sample holder 11 of Example 5 will be described with reference to FIG. 7. An attachment 28 is added to the sample holder 11 of the fifth embodiment with respect to the configuration of the first embodiment. The attachment 28 is an instrument attached to the outer surface of the outer cylinder 18 of the sample holder 11, and is inserted into the insertion port 29 of the focused ion beam device. Further, the sample holder 11 mounted on the attachment 28 is rotatably supported by the attachment 28 with an axis parallel to the X axis as a rotation axis. That is, the direction when the sample 13 is processed or observed by the focused ion beam device can be arbitrarily switched.

With the sample holder 11 of Example 5, not only the sample 13 exposed to various gas atmospheres can be observed, but also the sample 13 processed by the focused ion beam device can be observed. That is, it is possible to provide a sample holder capable of observing the sample 13 exposed to various gas atmospheres and switching the direction of the sample 13 without modifying the housing of the charged particle beam device.

The plurality of examples of the present invention have been described above. The present invention is not limited to the above embodiment, and the components can be modified and embodied without departing from the gist of the invention. In addition, a plurality of components disclosed in the above examples may be appropriately combined. For example, all the components of Examples 2 to 5 may be combined together. Further, some components may be deleted from all the components shown in the above embodiment.

1: Transmissive electron microscope, 2: Image display unit, 3: Electron beam, 4: Electron source, 5: Focusing lens, 6: Objective lens, 7: Imaging lens, 8: Fluorescent plate, 9: Camera, 10: Goniometer , 11: Sample holder, 12: Sample mounting part, 13: Sample, 14a: Piping, 14b: Piping, 15: Gas supply / exhaust section, 16a: Valve, 16b: Valve, 17: Central shaft, 18: Outer cylinder, 19: 1st airtight part, 20: 2nd airtight part, 21: grip, 22: moving knob, 23: screw, 24a: heater, 24b: heater wiring, 24c: heater power supply, 25a: thermometer, 25b: thermometer Wiring, 25c: Temperature display, 26a: Electron, 26b: Electric wire, 26c: Power supply, 27a: Pressure gauge, 27b: Pressure gauge wiring, 27c: Pressure display, 28: Attachment, 29: Insertion port, 30: Opening

Claims (9)

A sample holder that holds a sample and is inserted through an existing hole in a charged particle beam device.
The sample installation section where the sample is installed and the sample installation section
A gas encapsulation chamber in which the desired gas is encapsulated, and
A moving mechanism for moving the sample mounting portion between the inside and the outside of the gas filling chamber is provided.
The gas encapsulation chamber has an opening through which the sample installed in the sample installation portion passes.
A sample holder characterized in that an airtight portion that contacts the periphery of the opening to maintain airtightness is provided at the tip of the sample mounting portion. The sample holder according to claim 1.
The moving mechanism includes a cylindrical outer cylinder, a center pole provided with a sample mounting portion at the tip and arranged in the outer cylinder, a grip fixed to the hole together with the outer cylinder, and the center pole. It has a moving knob that rotates with respect to the grip while being combined with a screw provided on a part of the outer surface.
The sample setting portion is a sample holder characterized in that the moving knob is moved by rotating with respect to the grip. The sample holder according to claim 2.
The gas-filled chamber is a sample holder formed when the sample mounting portion moves into the outer cylinder and the airtight portion comes into contact with the periphery of the opening. The sample holder according to claim 1.
A sample holder characterized in that a heater for heating the sample is provided in the sample setting portion. The sample holder according to claim 4.
A sample holder characterized in that a thermometer for measuring the temperature of the sample is provided in the sample setting portion. The sample holder according to claim 1.
A sample holder characterized in that an electrode for applying a voltage to the sample is provided in the sample setting portion. The sample holder according to claim 1.
A sample holder characterized in that the sample setting portion is provided with a vacuum gauge for measuring the pressure in the gas filling chamber. The sample holder according to claim 2.
A sample holder characterized in that an attachment that rotatably supports the outer cylinder is attached to the outer surface of the outer cylinder. A charged particle beam device that generates an observation image of a sample by irradiating the sample with an electron beam from an electron source.
A charged particle beam device comprising the sample holder according to claim 1.

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