JP5437612B2 - Sample holder for electron microscope - Google Patents

Description

  The present invention relates to a sample holder for an electron microscope, and more particularly to a sample holder for an electron microscope that can introduce gas into a sample chamber in which a sample is placed.

  Since an electron microscope observes a sample using an electron beam, the sample is often placed in a vacuum. However, there are cases where the electron microscope is observed while the sample is exposed to gas, such as when the reaction process of the sample is observed with an electron microscope. In such a case, the sample is placed in the sample chamber, and gas is introduced into the sample chamber from the outside of the housing of the electron microscope.

  FIG. 1 is a schematic diagram showing a sample holder 10 arranged in a transmission electron microscope. As shown in FIG. 1, the inside of the housing 64 of the electron microscope 60 is evacuated. When the electron beam 62 passes through a sample (not shown) in the sample chamber 20, the sample can be observed. Gas is supplied to the sample chamber 20 from the gas supply unit 52. Further, the gas is exhausted from the sample chamber 20 by the vacuum pump 54. The gas adjusting unit 50 adjusts the gas flow rate and pressure. The O-ring 68 is provided between the housing 64 and the sample holder 10 in order to keep the inside of the housing 64 in a vacuum.

Patent Document 1 describes an electron microscope sample holder that introduces liquid helium into a sample cooling holder of an electron microscope.
JP 2000-251819 A

  As shown in FIG. 1, a sample chamber 20 in which a sample for observation with an electron microscope is placed is placed in a vacuum. From the viewpoint of maintaining a vacuum, the sample holder 10 is preferably inserted into the housing 64 through a small hole. For this reason, since the gas is introduced into and discharged from the sample chamber 20, the introduction pipe and the discharge pipe cannot be made thick. Therefore, the conductance for introducing and discharging the gas into the sample chamber 20 is large, and the gas flow rate cannot be ensured.

  The present invention has been made in view of the above problems, and an object of the present invention is to provide an electron microscope holder capable of increasing the conductance of gas introduction into and discharge from a sample chamber.

In the present invention, any one of a sample chamber in which a sample to be irradiated with an electron beam is arranged, an introduction tube for introducing gas into the sample chamber, and a discharge tube for discharging gas from the sample chamber is A gas guide / exhaust pipe provided so as to surround the other periphery of the introduction pipe and the exhaust pipe, and all the spaces other than the other of the introduction pipe and the exhaust pipe of the gas guide / exhaust pipe are all The sample holder for an electron microscope is the one of the introduction pipe and the discharge pipe . According to the present invention, the cross section of the introduction pipe and the discharge pipe can be increased, and therefore the conductance for introducing and discharging the gas can be increased.

In the above configuration, configured the gas guiding exhaust pipe in the region connected to said sample chamber, said inlet pipe and said one of said discharge pipe that surrounds the periphery of the other of the exhaust pipe and the inlet pipe It can be. According to this configuration, the conductance of gas introduction / discharge can be further increased.

In the above configuration, the sample is disposed in the sample chamber, and windows for transmitting the electron beam are provided above and below the sample in the sample chamber, and the window separates a gas atmosphere in the sample chamber from a vacuum. it can be configured to have. According to this configuration, the conductance of gas introduction / discharge can be further increased.

In the above configuration, the diameter of said one of said inlet pipe and said discharge pipe is larger at the opposite side to the sample chamber from the sample chamber, the other diameter of the exhaust pipe and the inlet pipe, said sample chamber It can be set as a larger structure on the opposite side . According to this configuration, the conductance of gas introduction / discharge can be further increased.

In the above configuration, the sample chamber has a cavity in which the gas guide cannula is formed from one surface to be connected, the other of the exhaust pipe and the inlet pipe is inserted into the cavity, said inlet pipe wherein one of the exhaust pipe may be a configuration that is connected so as to surround the cavity in said one surface. According to this configuration, the conductance of the gas in the sample chamber can be increased.

In the above configuration, the other of said exhaust pipe and said inlet pipe is said inlet, said inlet tube and said one of said discharge pipe can have a structure wherein a discharge pipe.

  The said structure WHEREIN: It can be set as the structure from which the direction in which gas is introduce | transduced into the said inlet pipe differs from the direction in which gas is discharged | emitted from the said exhaust pipe. According to this configuration, the conductance of the gas introduced into the introduction pipe and the gas discharged from the discharge pipe can be ensured.

In the above structure, the gas from a direction different from the extending direction of the gas Shirubehai pipe the one than thicker between the inlet pipe and the exhaust pipe on the opposite side of the one of said sample chamber and said exhaust pipe and said inlet pipe A buffer chamber for introducing or discharging can be provided.

The said structure WHEREIN: It can be set as the structure by which the said gas is introduce | transduced or discharged | emitted from the extending | stretching direction of the said gas guiding / exhausting pipe to the said other of the said introduction pipe and the said discharge pipe.

  According to the present invention, the cross section of the introduction pipe and the discharge pipe can be increased, and therefore the conductance for introducing and discharging the gas can be increased.

  FIG. 2 is a cross-sectional view of a sample holder 10a according to a comparative example. FIG. 3 is a cross-sectional perspective view of the vicinity of the sample chamber 20a. As shown in FIGS. 2 and 3, the sample holder 10 a includes a sample chamber 20 a, an introduction tube 12 a, a discharge tube 14 a, and a cover 56. An upper window 36 and a lower window (not shown) are provided in the sample chamber 20a. The upper window 36 and the lower window transmit an electron beam and separate the gas atmosphere in the sample chamber 20a from the vacuum in the housing 64. A gas is supplied to the introduction pipe 12a from the gas supply unit 52 through the tube 82a. The introduction pipe 12a introduces gas into the sample chamber 20a. The discharge pipe 14a is connected to the vacuum pump 54 via the tube 84a, and discharges gas from the sample chamber 20a. The cover 56 protects the introduction pipe 12a and the discharge pipe 14a. As shown in FIGS. 2 and 3, in the comparative example, the introduction pipe 12a and the discharge pipe 14a are provided in parallel.

  FIG. 4 is a cross-sectional view of the sample holder 10 according to the first embodiment, and FIG. 5 is a cross-sectional perspective view of the vicinity of the sample chamber 20. As shown in FIGS. 4 and 5, the sample holder 10 includes the sample chamber 20, the gas guide / exhaust pipe 11, and the cover 56. In the gas guide / exhaust pipe 11, a discharge pipe 14 is provided so as to surround the periphery of the introduction pipe 12. A discharge pipe 14 is formed between the cover 56 and the introduction pipe 12. Thus, the introduction pipe 12 and the discharge pipe 14 form a coaxial structure. The introduction tube 12 is directly connected to the sample chamber 20. The width of the gas guide / exhaust tube 11 is small on the sample chamber 20 side, and the width of the introduction tube 12 is also small on the sample chamber 20 side.

  A buffer chamber 16 is provided on the opposite side of the gas conduit 11 from the sample chamber 20 side. The buffer chamber 16 is wider than the discharge pipe 14 and buffers the gas discharged from the discharge pipe 14. A tube 84 is provided in the buffer chamber 16 in a direction different from the extending direction of the discharge pipe 14 (downward in FIG. 4). Thereby, the gas in the buffer chamber 16 is discharged in a direction different from the extending direction of the discharge pipe 14. On the other hand, gas is introduced into the introduction pipe 12 through the tube 82 from the extending direction of the introduction pipe 12. The introduction pipe 12, the discharge pipe 14, the buffer chamber 16, and the cover 56 are made of a metal such as SUS or an insulator, for example.

  FIG. 6A to FIG. 6D are diagrams showing the sample chamber 20, and respectively show a top view, a BB sectional view, a CC sectional view, and a DD sectional view. Referring to FIGS. 6A to 6D, the sample chamber 20 is made of a nonmagnetic metal. Holes 26 and 24 for providing an upper window and a lower window are formed in the upper and lower surfaces of the sample chamber 20, respectively. A cavity 22 is formed in the sample chamber 20 from the surface to which the gas guide / exhaust pipe 11 is connected.

  7A to 7E are views showing the sample chamber 20 to which the gas guide / exhaust pipe 11 is connected, and are a top view, a BB sectional view, a CC sectional view, and a DD, respectively. Sectional drawing and EE sectional drawing are shown. 7A to 7E, an upper window 36 and a lower window 34 are provided in the holes 26 and 24 of the sample chamber 20, respectively. The upper window 36 and the lower window 34 are made of a material that can withstand a pressure difference between a vacuum and a gas and transmit an electron beam. For example, a C or BN thin film can be used. The upper window 36, the sample 40, and the lower window 34 are arranged linearly. Thereby, the electron beam transmitted through the upper window 36 is irradiated to the sample 40. The electron beam that has passed through the sample 40 passes through the lower window 34. The introduction pipe 12 of the gas guide / exhaust pipe 11 is inserted into the cavity 22 of the sample chamber 20. The tip of the introduction tube 12 is inserted to the vicinity of the sample 40. The discharge pipe 14 is fixed to one surface of the sample chamber 20. Thus, the periphery of the introduction pipe 12 inserted into the cavity 22 is surrounded by the cavity 22 and connected to the space of the cavity 22 and the discharge pipe 14.

  The introduction pipe 12 introduces gas to the vicinity of the sample 40 in the sample chamber 20. After the gas is introduced to the vicinity of the sample 40, the gas is discharged through the region other than the introduction pipe 12 of the cavity 22 and the discharge pipe 14. As the gas, for example, oxygen, air, CO or the like is used, and can be appropriately used depending on the object to be observed.

  FIG. 8A and FIG. 8B are other examples of the sample chamber 20. With reference to FIGS. 8A and 8B, the introduction tube 12 is in contact with the inner surface of the sample chamber 20 above and below the sample chamber 20. Thus, the cavity 22 may not completely surround the introduction tube 12.

  FIG. 9 is a detailed cross-sectional view of the vicinity of the sample 40, and is a cross-sectional view taken along line FF in FIG. As shown in FIG. 9, the sample chamber 20 includes an upper plate 70, a lower plate 72, a sample support plate 74, and a spacer 76. A lattice 71 for reinforcing the upper window 36 is formed in the hole 26 formed in the upper plate 70, and the upper window 36 is provided in the lattice 71. Similarly, a lattice 73 for reinforcing the lower window 34 is provided in the hole 24. A lattice 75 is formed on the sample support plate 74, and the sample 40 is disposed near the lattice 75. Thereby, the electron beam passes through the holes 78 formed by the lattice 75. Gas can also pass through the holes 78. The sample 40 may be disposed between the upper window 36 and the lower window 34. For example, the sample 40 may be disposed directly on the upper window 36 or the lower window 34 without using the sample support plate 75. The thickness of the spacer 76 can be changed as appropriate.

  According to the first embodiment, as shown in FIGS. 4 and 5, in the gas guide / exhaust pipe 11, the exhaust pipe 14 is provided so as to surround the periphery of the introduction pipe 12. Thereby, compared with the introduction pipe 12a and the discharge pipe 14a of the comparative example as shown in FIG. 2 and FIG. 3, the cross sections of the introduction pipe 12 and the discharge pipe 14 can be increased, and therefore the conductance for introducing and discharging the gas can be increased. . The introduction pipe 12 may be provided so as to surround the periphery of the discharge pipe 14. Moreover, since Example 1 is a coaxial structure, the magnitude | size of the cross-sectional area of the introduction pipe 12 and the discharge pipe 14 can be designed arbitrarily. Therefore, the conductance of either the introduction pipe 12 or the discharge pipe 14 can be made larger than the other as necessary. For example, if the conductance of the introduction tube 12 is increased, the pressure in the sample chamber 20 can be easily set higher, and if it is reversed, the pressure in the sample chamber 20 can be easily set lower.

  Referring to FIG. 1, a gasket and an O-ring are provided between the housing 64 and the sample holder 10 to keep airtightness. For this reason, it is preferable that the cross section of the sample holder 10 is circular. In the comparative example of FIGS. 2 and 3, a cover 56 is provided to make the cross section of the sample holder 10 circular. On the other hand, in Example 1, the outer wall of the discharge pipe 14 is the outer wall of the sample holder 10. That is, a space other than the introduction pipe 12 of the gas guide / exhaust pipe 11 can be used as the exhaust pipe 14. Therefore, the conductance of gas introduction and discharge can be further increased.

  For example, in the comparative example of FIGS. 2 and 3, if the diameter of the cover 56 is 8 mm and the wall thickness is 1 mm, the diameters of the introduction pipe 12 and the discharge pipe 14 can be secured only 3 mm or less. Will have an inner diameter of 1-2 mm. on the other hand. 4 and 5, the outer shape of the discharge pipe 14 can be 8 mm and the inner diameter can be 6 mm. Therefore, the outer diameter of the introduction tube 12 can be 4.5 mm and the inner diameter can be 3.5 mm.

  Further, as shown in FIGS. 7A to 7E, the discharge pipe 14 can surround the introduction pipe 12 in a region where the gas guide / discharge pipe 11 is connected to the sample chamber 20. Thereby, the conductance of gas discharge can be further increased.

  Further, as shown in FIG. 4, the diameter of the introduction pipe 12 is set according to the diameter of the gas guide / exhaust pipe 11 (sample holder). For example, the thickness of the gas conduit 11 is larger on the gas introduction / exhaust side than on the sample chamber 20 side. Therefore, the thickness of the introduction tube 12 is also made larger on the gas introduction / discharge side than on the sample chamber 20 side. Thereby, the introduction pipe | tube 12 can be thickened and conductance can be enlarged.

  As shown in FIGS. 7A to 7E, the sample chamber 20 has a cavity 22 formed from one surface to which the gas guide / discharge tube 11 is connected. The introduction pipe 12 is inserted into the cavity 22, and the discharge pipe 14 is connected to the one surface so as to surround the cavity 22. As a result, a structure that increases the gas conductance can be easily formed even in the sample chamber 20.

  If the conductance of the gas in and out of the sample holder 10 can be increased, the conductance of the gas to and from the sample holder 10 affects the conductance of the entire gas. As shown in FIG. 2, if the gas is introduced into and discharged from the sample holder 10 from the same direction, the tubes 82 a and 84 a for introducing and discharging the gas to the sample holder 10 cannot be thickened. Therefore, the conductance is lowered. Therefore, as shown in FIG. 4, the direction in which the gas is introduced into the introduction pipe 12 is different from the direction in which the gas is discharged from the discharge pipe 14. Thereby, the tubes 82 and 84 can be made thick and conductance can be ensured.

  Further, a buffer chamber 16 thicker than the discharge pipe 14 is provided on the exhaust side of the discharge pipe 14 (on the side opposite to the sample chamber 20). Thereby, gas can be discharged | emitted in the direction different from the extending | stretching direction of the gas guide / exhaust pipe 11. FIG. Further, gas is introduced into the introduction pipe 12 from the extending direction of the gas guide / exhaust pipe 11. Thereby, the tubes 82 and 84 can be made thick and conductance can be ensured. When the introduction pipe is provided around the discharge pipe, a buffer layer thicker than the introduction pipe may be provided on the introduction side of the introduction pipe. In this case, the gas may be introduced from a direction different from the extending direction of the gas guiding / exhausting pipe, and the gas may be discharged from the extending direction of the gas guiding / exhausting pipe.

  The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific embodiments, and various modifications and changes can be made within the scope of the gist of the present invention described in the claims. It can be changed.

FIG. 1 is a schematic diagram showing a sample holder arranged in a transmission electron microscope. FIG. 2 is a cross-sectional view of a sample holder according to a comparative example. FIG. 3 is a cross-sectional perspective view of the vicinity of the sample chamber. FIG. 4 is a cross-sectional view of the sample holder according to the first embodiment. FIG. 5 is a cross-sectional perspective view of the vicinity of the sample chamber. FIG. 6A to FIG. 6D are diagrams showing the sample chamber. FIG. 7A to FIG. 7E are diagrams showing a sample chamber to which a gas guide / exhaust pipe is connected. FIG. 8A and FIG. 8B are other examples of the sample chamber. FIG. 9 is a detailed cross-sectional view of the vicinity of the sample.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Sample chamber 11 Gas conducting / exhausting tube 12 Introducing tube 14 Exhaust tube 16 Buffer chamber 20 Sample chamber 22 Cavity 24, 26 Hole 34, 36 Window 40 Sample

Claims (8)

A sample chamber in which a sample to be irradiated with an electron beam is placed;
One of the introduction pipe for introducing gas into the sample chamber and the discharge pipe for discharging gas from the sample chamber is provided so as to surround the other of the introduction pipe and the discharge pipe. Gas exhaust pipe,
Comprising
All the spaces other than the other of the introduction pipe and the discharge pipe of the gas guide / exhaust pipe are the one of the introduction pipe and the discharge pipe ,
The sample is disposed in the sample chamber, and windows for transmitting the electron beam are provided above and below the sample in the sample chamber, and the window separates a gas atmosphere in the sample chamber from a vacuum. Sample holder for electron microscope. A sample chamber in which a sample to be irradiated with an electron beam is placed;
One of the introduction pipe for introducing gas into the sample chamber and the discharge pipe for discharging gas from the sample chamber is provided so as to surround the other of the introduction pipe and the discharge pipe. Gas exhaust pipe,
Comprising
All the spaces other than the other of the introduction pipe and the discharge pipe of the gas guide / exhaust pipe are the one of the introduction pipe and the discharge pipe,
The one diameter of the introduction tube and the discharge tube is larger on the opposite side of the sample chamber than the sample chamber, and the other diameter of the introduction tube and the discharge tube is on the opposite side of the sample chamber A sample holder for an electron microscope , characterized in that it is large. A sample chamber in which a sample to be irradiated with an electron beam is placed;
One of the introduction pipe for introducing gas into the sample chamber and the discharge pipe for discharging gas from the sample chamber is provided so as to surround the other of the introduction pipe and the discharge pipe. Gas exhaust pipe,
Comprising
All the spaces other than the other of the introduction pipe and the discharge pipe of the gas guide / exhaust pipe are the one of the introduction pipe and the discharge pipe,
Unlike the direction in which gas is introduced into the introduction pipe and the direction in which gas is discharged from the discharge pipe,
The sample holder for an electron microscope is thicker than the one of the introduction tube and the discharge tube on the opposite side of the one of the introduction chamber and the discharge tube, and is different from the extending direction of the gas guide / discharge tube. A sample holder for an electron microscope comprising a buffer chamber for introducing or discharging gas from a direction. In the region where the gas guide / exhaust pipe is connected to the sample chamber, the one of the introduction pipe and the discharge pipe surrounds the other of the introduction pipe and the discharge pipe. The sample holder for electron microscopes as described in any one of Claim 1 to 3 . The sample chamber has a cavity formed from one surface to which the gas conduit pipe is connected,
The other of the introduction pipe and the discharge pipe is inserted into the cavity, and the one of the introduction pipe and the discharge pipe is connected to the one surface so as to surround the cavity. The sample holder for electron microscopes as described in any one of Claim 1 to 4 .   6. The other of the introduction pipe and the discharge pipe is the introduction pipe, and the one of the introduction pipe and the discharge pipe is the discharge pipe. The sample holder for an electron microscope as described. 7. The sample holder for an electron microscope according to claim 1 , wherein a direction in which gas is introduced into the introduction pipe is different from a direction in which gas is discharged from the discharge pipe. . The sample holder for an electron microscope according to claim 3, wherein the gas is introduced into or discharged from the other of the introduction tube and the discharge tube from the extending direction of the gas guide / discharge tube.

Images