The present invention relates to a specimen cryo holder used with a charged-particle system (for example, focused ion beam system (FIB system), transmission electron microscope (TEM), or scanning transmission electron microscope (STEM)). In addition, the present invention relates also to a dewar which is suitably mounted to a specimen cryo holder.
An FIB system is a system capable of processing a specimen into an arbitrary shape by irradiating the specimen with a focused beam of charged particles. In particular, an FIB system having a microprobe is capable of extracting a minute specimen from an arbitrary site of a specimen. This technique of extraction is called an FIB microsampling method. The FIB microsampling method is a method suitable for producing a specimen needed when analysis of a state or structure on the order of several nanometers is performed by use of an electron microscope or the like, with such analysis being a subject of research in nanotechnology (Patent Document 1).
Meanwhile, when a thin film specimen produced is observed under an electron microscope, an effect of an electron beam may raise the temperature of the specimen so as to make it difficult to analyze the intrinsic state or structure of the specimen. Especially, a specimen susceptible to thermal damage is generally low in thermal conductivity, so that charge-up and thermal conduction properties of the specimen contribute greatly to the thermal damage. As a countermeasure against this problem, there has been proposed a method of cooling a specimen under observation (Patent Document 2). A specimen cryo holder proposed in Patent Document 2, however, is unable to efficiently transfer the heat of a cooling source to a specimen, but is only able to barely cool the specimen.
Besides, in order to observe a thin film specimen under an electron microscope, irradiation with the electron beam should be performed perpendicularly to the thin film surface. Therefore, this kind of specimen cryo holder generally needs a mechanism by which the orientation of the specimen can be tilted. For instance, an observation of a crystalline specimen needs a tilting mechanism with respect to at least one axis. In the case of existing specimen cryo holders, however, a vessel in which a cooling source (for example, liquid nitrogen) is contained (the vessel will hereinafter be referred to as “dewar”) is fixed to the tilting mechanism. Therefore, a tilting of the specimen cryo holder causes the vessel to be also tilted, and the free surface level of liquid nitrogen in the vessel is changed, resulting in boiling (bubbling). Vibrations due to the boiling are propagated through the specimen cryo holder to the specimen, rendering the observation of the specimen difficult. Accordingly, there is a need for a specimen cryo holder equipped with a tilting mechanism such that a specimen having a low thermal conductivity can be observed with efficient cooling thereof.
Note that during processing by use of an FIB system, the specimen temperature may rise depending on the processing conditions. Especially Where the object of processing is a thermally weak resin, a low-melting-point metal, a low-temperature phase change matter or the like, it is preferable to process the specimen while cooling the specimen.
In general, part of the energy of charged particles colliding on a processing position is used for sputtering, but the rest of the energy is taken into the inside of the specimen and transformed into thermal energy. The thermal energy is propagated through the inside of the specimen to diffuse to a cooling region, and, after a predetermined period of time, the specimen temperature is stabilized in the vicinity of a target temperature.
However, where the thermal energy given by the irradiation with charged particles surpasses the quantity of heat transferred from the cooling source to the cooling region, the specimen temperature would be raised. In order to process a specimen by charged particles while cooling the specimen, therefore, it is necessary to appropriately control the cooling temperature, charged-particle irradiation conditions and the like, taking into account the heat transfer characteristics and the form of the specimen. In the existing specimen cryo holders, however, the quantity of heat transferred is very small, as aforementioned, so that the control itself is difficult to achieve.
Besides, in processing by an FIB system, the processing should be carried out while radiating an ion beam from a parallel direction to a thin film surface. In the existing specimen cryo holders, however, the vessel containing the cooling source (for example, liquid nitrogen) is fixed to the tiling mechanism, as aforementioned, so that a tilting of the specimen cryo holder would cause the vessel to be tilted together. This results in boiling (bubbling) of the liquid nitrogen, and the resulting vibrations are propagated to the specimen to be processed. Accordingly, in the cases of FIB systems, also, there is a need for realization of a specimen cryo holder equipped with a tilting function such that a specimen having a low thermal conductivity can be processed simultaneously with efficient cooing thereof.
The present invention has been made in consideration of the above-mentioned problem. Accordingly, it is an object of the invention to provide a specimen cryo holder equipped with a tiling function such that a specimen can be cooled during processing or observation thereof, and a dewar for the same.
For solving the above problem, a specimen cryo holder according to the present invention has a mechanism capable of cooling a specimen while maintaining the posture of a dewar in a fixed direction even when the specimen is tilted into a direction suitable for processing or observation thereof. In addition, a dewar according to the present invention has a vacuum maintenance mechanism on an outer vessel by which an inner vessel holding a cooling source therein is vacuum-insulated from outside air.
According to the specimen cryo holder of the present invention, a specimen can be tilted into a direction suitable for processing or observation thereof using charged particles, while efficiently cooling the specimen. The use of the dewar according to the present invention makes it possible to enhance vacuum insulation performance during observation or processing, and to maintain cooling of a specimen by use of a cooling source for a long time. Other problems, configurations and effects than the aforementioned will become clear upon reading the description of an embodiment that follows.
Now, a mode for carrying out the present invention will be described below, based on the drawings. Note that the way in which the present invention is embodied is not limited to the exemplary mode described below, and various modifications are possible within the scope of the technical idea of the invention.
First, a difference between the positional relationship between, charged particles and a specimen at the time of processing the specimen and that at the time of observing the specimen will be described.
A specimen 1 is a minute specimen produced, for example, by an FIB microsampling method. A processing/observation region 2 with which the specimen 1 is provided is not greater than 10 μm square, in the cases of normal processing or observation. Note that the specimen 1 is adhered directly to a cryo specimen base 3, which is cooled by a cooling source.
At the time of processing (
Note that during observation. (
The specimen cryo holder 13 includes: a shutter 19 constituting an outer tube; a heat shield 18 constituting an inner tube; an L-shaped cooling rod 14 of which a part is accommodated in the inner tube; and a dewar mounting part 15 which holds the heat shield 18 such that the heat shield 18 is rotatable and holds the cooling rod 14. The dewar mounting part 15 holds the cooling rod 14, with a part of the cooling rod 14 inserted in an opening provided in a lower-side portion thereof. The part of the cooling rod 14 protrudes from a lower surface of the dewar mounting part 15 so that when a dewar is mounted to the lower surface of the dewar mounting part 15, the part of the rod makes contact with a cooling source 16.
Here, the cooling rod 14 is not fixed to either the inside of the heat shield 18 or the inside of the dewar mounting part 15. When it is desired to fix the cooling rod 14 to the inside of the heat shield 18, a locking mechanism 26 is used. The locking mechanism 26 in this embodiment locks the cooling rod 14 by pressing the cooling rod 14 against the inside of the heat shield 18 when pressed in; when pressed in again, the locking mechanism 26 unlocks the cooling rod 14.
As will be described later, the dewar is fixedly mounted to the dewar mounting part 15 via a screw or screws or the like. Incidentally, the dewar mounting part 15 and the heat shield 18 are rotatably mounted to each other through O-rings 20. The shutter 19 is so mounted as to be reciprocally movable along a surface of the heat shield 18, by way of the O-rings 20.
In this embodiment, a tip portion (a portion on the specimen attaching side) of the heat shield 18 is partly cut so that opposed two arms protrude in the axial direction so that a cryo specimen base support 10 can be held between the two arms. Here, the cryo specimen base support 10 and the cooling rod 14 are linked to each other via a flexible cooling transfer member (for example, a tubular metallic mesh) 17. The flexible cooling transfer member 17 is a freely deformable member. Therefore, the cryo specimen base support 10 is separated from the cooling rod 14, and only the cryo specimen base support 10 can be tilted (rotated in the axial direction of the heat shield 18) independently of the cooling rod 14.
The cryo specimen base 3 with the specimen 1 mounted thereto is mounted to the cryo specimen base support 10. Therefore, that the cryo specimen base support 10 can be tilted independently of the cooling rod 14 means that the specimen 1 can be tilted independently of the cooling rod 14. A process up to fixation of the specimen 1 to the cryo specimen base 3 has already been known (Non-patent Document 1). Accordingly, description of this process is omitted here.
Since the cryo specimen base support 10 is fixed to the heat shield 18 as aforementioned, rotating the heat shield 18 relative to the dewar mounting part 15 causes the cryo specimen base support 10 to rotate together with the heat shield 18, whereby the orientation of the specimen 1 is rotated. The reason why the cryo specimen base support 10 and the heat shield 18 can be rotated lies in that the cryo specimen base support 10 and the cooling rod 14 are linked to each other via the flexible cooling transfer member 17, as aforementioned.
The cryo specimen base 3 can be detached from the cryo specimen base support 10 after processing/observation is finished. Naturally, when processing/observation is to be performed again, the cryo specimen base 3 can be mounted to the cryo specimen base support 10. A structure for detachably mounting the cryo specimen base 3 to the cryo specimen base support 10 will be described later.
In addition, a holder tip shield 9 and a holder tip shield retainer 8 are sequentially attached to a tip portion of the heat shield 18. The holder tip shield 9 is a member for hermetically sealing the inside of the shutter 19 by making secure contact with an end portion of the shutter 19 when the shutter 19 is slid, toward the tip of the heat shield 18 along the axis of the heat shield 18. Besides, the holder tip shield retainer 8 is a member for preventing the holder tip shield 9 from falling off.
The dewar has a double vessel structure composed of an inner dewar 23 which holds the cooling source (e.g., liquid nitrogen) 16 therein, and an outer dewar 21 which accommodates the inner dewar 23, with a heat shield 22 therebetween. The heat shield 22 is maintained in a vacuum state. Therefore, the inner dewar 23 is perfectly thermally insulated from the exterior of the outer dewar 21 by the heat shield 22.
An upper surface of the inner dewar 23 is formed with two openings. The cooling rod 14 is inserted in one of the two openings, and the other of the two openings is used for introducing the cooling source 16.
In this embodiment, a lower surface of the outer dewar 21 is formed with an evacuation port 24, to which is attached a vacuum maintenance cap 25. The evacuation port 24 is used for evacuating the heat shield 22. The vacuum maintenance cap 25 is used for maintaining the heat shield 22 evacuated in a high vacuum state. As aforementioned, the dewar is detachably mounted to the specimen cryo holder by a screw or screws or the like.
<Orientation of Specimen in Use>
In an FIB system for producing a thin film specimen, as shown in
In this instance, the cooling rod 14 is in an unlocked state. Since the cooing rod 14 is kept unlocked, even if a tilt angle of the specimen 1 is changed (namely, even if the heat shield 18 is rotated about a center axis of the cooling rod 14), the cooling rod 14 would not rotate together with the heat shield 18, and the dewar would not rotate together with the dewar mounting part 15. In other words, the cooling source 16 held in the dewar is kept as it is in a horizontal state. Even if bubbling is generated in the cooling source 16 by an external cause or the like, the resulting vibration is propagated wholly through the flexible cooling transfer member 17 and is attenuated. Therefore, the accuracy of processing/observation can be effectively prevented from being lowered.
In an electron microscope for observation of the thin film specimen produced, as shown in
In the electron microscope, observation using a transmission wave or the like is performed with the specimen 1 in a cooled state. A signal 7 (e.g., characteristic X-rays) emitted from the specimen 1 passes a space 4 (not shown), and is detected efficiently by a detector, to be utilized for specimen evaluation. For the observation here, the specimen 1 having a crystalline structure has to be tilted into a vertical (up-and-down) and in-plane direction in regard of the sheet surface of the drawing, as has been mentioned above. Therefore, the rotation (tilting) of the shutter 19 and the heat shield 18 (or only the heat shield 18) may be carried out using a tilting mechanism for a system stage which holds the specimen cryo holder 13, or may be carried out manually.
Naturally, at the time of observation, also, the locking mechanism 26 is set in an unlocking state. This ensures that the cooling source 16 held in the inner dewar 23 can be kept in a horizontal state, irrespectively of the processing/observation direction for the thin film specimen.
<Shutter Function>
In the next place, an example of use of the shutter 19 will be described. The shutter 19 is provided for avoiding damaging or contamination of the specimen during transport of the specimen cryo holder 13 between systems. Use Example (a) shown at the top in
<Mounting Structure for Cryo Specimen Base>
Here, using
Note that a straight-line-shaped slot formed in the head of the fixing screw 27 is not formed to extend to opposite end edges of the screw head but is composed of a slot which is so formed that, as depicted in
In addition, as illustrated in
<Dewar>
The upper surface of the inner dewar 23 is formed with two openings, and cylindrical pipes are so mounted as to extend upward from the two openings. One-side ends of the two pipes are connected respectively to holes of the same shape which are formed in the outer dewar 21. This connection ensures that a space defined by the inner dewar 23 and the outer dewar 21 forms the heat shield 22. Note that one of the two openings is used as a cooling rod insertion port 31a in which to insert the cooling rod 14, and the other is used as a cooling source introduction port 31b for introduction of the cooling source 16. Note that the designations of the cooling rod insertion port 31a and the cooling source introduction port 31b are merely expedient ones, so that either of the two ports may be used for insertion of the cooling rod 14 and the other for introduction of the cooling source 16.
In addition, the lower surface of the outer dewar 21 is formed with the evacuation port 24, and the vacuum maintenance cap 25 is attached to the evacuation port 24. The evacuation port 24 is used for evacuating the heat shield 22. The vacuum maintenance cap 25 is used for maintaining the heat shield 22 evacuated in a high vacuum state.
<Summary>
As has been described above, the use of the specimen cryo holder 13 ensures that the orientation of the dewar mounted to the dewar mounting part 15 of the specimen cryo holder 13 can always be maintained in the direction of gravity even when the orientation (tilt) of the specimen is changed for processing or observation. Therefore, where the specimen cryo holder 13 is used, bubbling of liquid nitrogen, liquid helium or the like used as the cooling source 16 would not occur even upon a change in the orientation (tilt) of the specimen. As a result, propagation of bubbling-induced vibrations to the specimen 1 is obviated, so that the accuracy of observation and processing can be enhanced.
Naturally, the temperature of the cooling source 16 is propagated to the specimen 1 by way of the cooling rod 14, the flexible cooling transfer member 17, the cryo specimen base support 10 and the cryo specimen base 3. Therefore, observation/processing with cooling of the specimen 1 can also be performed. Note that the flexible cooling transfer member 17 is excellent in thermal conductivity and, therefore, a sufficient quantity of heat can be propagated therethrough to the specimen 1.
The aforementioned technical effects are realized because the specimen cryo holder has the following characteristic features.
The features are:
(1) that the specimen 1 and the cryo specimen base support 10 on which to mount the cryo specimen base 3 are linked to each other by way of the cooling rod 14 deformable at least in twisting directions, and the specimen 1 can be rotated (tilted) independently of the cooling rod 14; and
(2) that the cooling rod 14 is not fixed to the heat shield 18 constituting the inner tube or the dewar mounting part 15.
In addition, the dewar according to this embodiment is attachable to and detachable from the specimen cryo holder 13 (specifically, the dewar mounting part 15). Where it is unnecessary to cool the specimen 1, therefore, the dewar can be detached from the specimen cryo holder 13. Besides, in the dewar according to this embodiment, the outer dewar 21 constituting the outer tube is provided with the vacuum maintenance cap 25, which ensures that if evacuation is carried, out each time observation or processing is performed, the observation and processing can be carried out under a high degree of vacuum at all times. This makes it possible to maintain the temperature of the cooling source for a long period of time, and to perform a continuous operation for a long time. Besides, since a continuous operation can thus be performed, a total operation time necessary for processing and observation can be greatly shortened. As a result, a rapid development of materials analysis and research can be realized. In particular, a wide range of application can be expected in the fields of materials analysis and research involving anisotropy.
1 . . . Specimen, 2 . . . Processing/observation region, 3 . . . Cryo specimen base, 4 . . . Space, 5 . . . Charged particles, 6 . . . Charged particles, 7 . . . Signal, 8 . . . Holder tip shield retainer, 9 . . . Holder tip shield, 10 . . . Cryo specimen base support, 11 . . . Holder receiving part, 12 . . . O-ring, 13 . . . Specimen cryo holder, 14 . . . Cooling rod (Second heat conduction member), 15 . . . Dewar mounting part, 16 . . . Cooling source, 17 . . . Flexible cooling transfer member (First heat conduction member), 18 . . . Heat shield (First tubular member), 19 . . . Shutter (Second tubular member), 20 . . . O-ring, 21 . . . Outer dewar, 22 . . . Heat shield, 23 . . . inner dewar, 24 . . . Evacuation port, 25 . . . Vacuum maintenance cap, 26 . . . Locking mechanism, 27 . . . Fixing screw, 28 . . . Evacuation port, 29 . . . Cryo specimen base presser, 30 . . . Cone point part, 31a . . . Cooling rod insertion port, 31b . . . Cooling source introduction port.
Number | Date | Country | Kind |
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2012-145599 | Jun 2012 | JP | national |
Filing Document | Filing Date | Country | Kind |
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PCT/JP2013/065427 | 6/4/2013 | WO | 00 |
Publishing Document | Publishing Date | Country | Kind |
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WO2014/002700 | 1/3/2014 | WO | A |
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Number | Date | Country | |
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20150340199 A1 | Nov 2015 | US |