JP5304011B2 - Focused ion beam device with local region temperature measuring device and local region temperature measuring method - Google Patents

Description

The present invention enables a substantial temperature measurement of an observation site when observing a tissue change at a high temperature using a heating stage by being attached to a focused ion beam apparatus for the purpose of microstructural observation and microfabrication. Also, the present invention relates to a focused ion beam device equipped with a device for measuring a local temperature change generated by ion beam irradiation when a sample is subjected to focused ion beam microfabrication, and a temperature measurement method using this device. is there.

  The microfabrication technology using the focused ion beam method is linked with the recent micromachining (MEMS) technology as a technology for manufacturing ultra-small machine parts such as small coils, springs, and motors of several tens of μm. Expected. In addition, the position as a sample preparation technique for a transmission electron microscope has been fixed, and a focused ion beam processing method has been widely applied from metals to semiconductors to insulators and organic materials. In particular, the technique for producing a thin-section sample for a transmission electron microscope is further advanced. For example, as disclosed in Patent Document 1, first, a sample site to be thinned from a test piece having a size of several mm is extracted from a tissue. Identify while observing, introduce the manipulator into the focused ion beam device, take out a plate-shaped micro area with a width of less than 10 μm using ion beam processing and adhesion technology to the manipulator, and then prepare separately A technique is also disclosed in which a plate-shaped micro sample is mounted on a 3 mmφ half-moon sample stage for an electron microscope and thinned by an ion beam processing technique to such a thickness that an electron beam can pass through the sample. .

  By the way, the principle of this processing method is a method in which gallium (Ga) ions are accelerated at an acceleration voltage of tens of thousands of V and irradiated onto a sample, and fine processing is performed while repelling atoms by the principle of ion sputtering. In particular, there is a concern about a local temperature rise of the material being processed by the ion beam.

  A technique for in-situ observation of a tissue change when a sample is heated is well known, but generally only an indirect temperature measurement method using a thermocouple attached to a heating stage.

  For example, Patent Document 2 discloses a technique for measuring the temperature of a local region using a very small thermocouple. Here, in order to avoid thermal point contact between the thermocouple contact part and the local area measurement part, the ion beam deposition function part is attached to the focused ion beam processing apparatus, and the thermocouple contact part and the measurement part are deposited. Technology that integrates with technology is shown. Also, in the old days, Patent Document 3 discloses a technique that attempts to measure the temperature of a local region within a scanning electron microscope for the purpose of inspecting a local temperature rise portion such as a semiconductor circuit. However, at that time, there was no ion beam processing or manipulator technology, and no specific technology of temperature measurement technology corresponding to the current micromachining technology was shown, such as manually operating the temperature measurement unit from the outside.

  Next, looking at the technology of small thermocouples, the ultrathin thermocouple wire used for measuring the temperature in a minute region in the semiconductor field, etc. is 12.5-50 μm thick, but it is thin and weak, so it is difficult to handle There is a problem that it is easy to cut immediately. Therefore, a 100-300 μm coated thermocouple wire with high strength is used as the main line, and an ultrafine thermocouple wire having a thickness of 12.5-100 μm is joined at once with the same material, and the tip is spherically joined, or spherical Patent Document 4 discloses a technique of rolling after joining and making a disk-shaped contact portion.

Japanese Patent Laid-Open No. 5-180739 JP 2002-25494 A Japanese Patent Laid-Open No. 51-25960 JP 2003-344178 A

  When trying to measure the temperature rise in the tens of μm region and the surrounding temperature distribution at the time of microfabrication in the focused ion beam device, the tip of the tip is 12.5 μm even if a conventional ultrafine thermocouple is used. In the case where the ends of the strands of the wire are spherically bonded or rolled, the diameter of the contact portion is about 25 μm, which is almost the same as the measurement target region or smaller than the measurement target region, and the heat reverse flow phenomenon It was found that accurate temperature measurement was not possible. Therefore, it was reconfirmed that in order to accurately measure the temperature in the minute region near the observation field, it is essential to integrate a very small thermocouple by vapor deposition technology.

  However, only by inserting a very small thermocouple wire into the focused ion beam device, a nozzle that emits a gas for adhering to the observation region or processing region of the target sample in the vicinity of the μm order by beam assist deposition. Thermocouple wires are often intertwined, and the temperature measurement method is not necessarily excellent in workability. Furthermore, when the surface of the temperature measurement target is not smooth and there are severe irregularities such as an aggregate of particles, it is not always easy to measure the temperature in the vicinity of the target particle.

  In addition, if the opportunity to observe the tissue changes dynamically when the sample is heated increases, not only the relatively low temperature range of several hundred degrees Celsius, but also the need for measuring the tissue changes at high temperatures of 1000 degrees Celsius or higher. Increasingly, a structure that can easily change the type of the smallest thermocouple has been required.

  Furthermore, instead of indirectly measuring the temperature with the thermocouple attached to the heating stage, the target thermometer can be directly attached to the observation field, and the target temperature can be measured directly. It has been desired to improve the fine movement operation for accurately connecting the tip of the thermocouple to the location.

  Accordingly, the present invention provides a local region temperature measuring apparatus and a local region temperature measuring method for a focused ion beam device that can solve the above-described problems and can accurately measure a minute region in the vicinity of an observation field. With the goal.

In order to achieve the above object, the inventor of the present application has intensively studied the form and configuration of the tip of the extremely small thermocouple attached to the inside of the focused ion beam processing apparatus, etc. As a result, the following new local region temperature measuring apparatus has been developed. It led to the development of a focused ion beam equipment with.

(1) A focused ion beam device having a local region temperature measurement function and a beam-assisted deposition function, wherein the local region temperature measurement device, an ion gun that emits an ion beam, and fine processing or irradiation while irradiating the ion beam A sample chamber for installing a sample to be subjected to tissue observation, and a gas discharge nozzle for beam-assisted deposition for jetting a deposition gas to be reacted with an ion beam into the sample chamber, The region temperature measuring device and the beam assist deposition gas discharge nozzle are arranged at positions opposed to each other centering on an irradiation axis of the ion beam irradiated from the ion gun toward the sample. The apparatus includes a contact-type temperature measurement unit provided at a holder tip of the local region temperature measurement device, and the contact An insulating guide for protecting the mold temperature measuring unit, and the fine motion control unit for exposing the contact temperature measuring portion from the insulating guides, at least Bei example, a gradient of 45 ° or more with respect to the insulating guide holder shaft It has the contact temperature measuring unit, characterized in that exposed by moving along the insulating guide, the focused ion beam apparatus having a local region temperature measuring device.
(2) the contact temperature measuring part, Ri Do from the thermocouple, the thermal contact portions of the thermocouples, is processed by a focused ion beam, localized according to a diameter of less rod-shaped 50 [mu] m (1) A focused ion beam device equipped with a region temperature measuring device.
( 3 ) The focused ion beam device including the local region temperature measuring device according to (1) or (2) , wherein the contact-type temperature measuring unit has a structure that can be attached to and detached from the tip of the holder by an insertion method.
( 4 ) Local in a focused ion beam apparatus that measures the temperature of a temperature measurement object during processing by the focused ion beam apparatus including the local region temperature measuring apparatus according to any one of (1) to ( 3 ). A temperature measurement method for a region, wherein a contact-type temperature measurement unit is moved and exposed from an insulating guide by a fine movement drive control unit, and the temperature measurement is performed by the beam assist deposition function in the vicinity of the observation region of the temperature measurement object. After bonding the object and the contact-type temperature measuring unit, the ground is taken through the temperature measuring object, and the observation region of the temperature measuring object is measured while the temperature of the temperature measuring object is measured. A predetermined shape is processed by a processing method, and after the processing is completed, the bonded portion between the temperature measurement object and the contact-type temperature measurement unit is separated by a focused ion beam processing method. Temperature measurement method of a local region in the focused ion beam apparatus characterized.
( 5 ) A focused ion beam device including the local region temperature measurement device according to any one of (1) to ( 3 ), wherein the temperature of the temperature measurement object during heating is measured in the focused ion beam device. It is a temperature measurement method for a local region, and after taking the ground through the temperature measurement object, observe the state change of the observation region while heating and cooling the temperature measurement object to a predetermined temperature, at an arbitrary temperature, A contact-type temperature measurement unit is moved and exposed from the insulating guide by the fine movement drive control unit, and in the vicinity of the observation region of the temperature measurement object, the temperature-measurement object and the contact-type temperature measurement unit are After the temperature measurement is completed, the bonded portion between the temperature measurement object and the contact-type temperature measurement unit is separated by a focused ion beam processing method. Temperature measurement method of the local area during sample heating within a focused ion beam apparatus characterized by.
( 6 ) The local region temperature measurement method according to ( 4 ) or ( 5 ), wherein the position where the contact-type temperature measurement unit is bonded is in the range of 0.01 to 50 μm from the observation region.

  ADVANTAGE OF THE INVENTION According to this invention, the local temperature rise amount at the time of ion beam processing of the sample within a focused ion beam apparatus can be measured. In addition, in the heating in-situ observation experiment using the heating stage, it is possible to directly measure the temperature of the observation field in the environment where the observation ion beam is irradiated.

  Exemplary embodiments of the present invention will be described below in detail with reference to the accompanying drawings. In addition, in this specification and drawing, about the component which has the substantially same function structure, duplication description is abbreviate | omitted by attaching | subjecting the same code | symbol.

  This is a focused ion beam device having a beam assist deposition function to which this device is applied. This ion beam unit emits an ion beam accelerated to 30,000 to 40,000 V, and the emitted ion beam is A focusing lens system, a sample chamber for installing a sample to be subjected to microfabrication and tissue observation while irradiating the ion beam, and a gas nozzle for ejecting a deposition gas that reacts with the ion beam into the sample chamber And an introduction mechanism. Both are vacuum systems, and as the ion beam source, Ga ions are generally used, but sometimes a helium ion source is also used. As the deposition gas, various gas types for depositing tungsten (W), carbon, platinum and the like are used.

  By the way, if there is a secondary electron detection device that detects secondary electrons generated when the target beam is irradiated with the ion beam, and the secondary electron intensity is reflected on the cathode ray tube in synchronization with the scanning ion beam, A scanning ion microscope image can be obtained. For example, since the Ga ion beam to be scanned can be narrowed down to a diameter of several tens of nm, it is possible to simultaneously observe a scanning ion microscope structure at a high magnification of several tens of thousands of times. As a result, for the purpose of measuring the temperature by specifying a micro structure on the order of μm, it is necessary to move the thermocouple tip with a precision of the order of μm or higher accuracy even for a local region temperature measurement device. become.

  As described above, the focused ion beam apparatus emits a gas for adhering the tip of the thermocouple to the observation region or processing region of the target sample in the vicinity of the μm order by the beam assist deposition function. It is essential that the nozzle introduction mechanism is installed. When measuring the temperature in a very small region, if the tip of the thermocouple and the sample are in point contact, the thermal resistance is a major obstacle, so the sample can be deposited by vapor deposition using conductive tungsten, carbon, or platinum. And the thermocouple tip must be integrated.

  For example, in the case of depositing tungsten, a crystal powder of hexacarboxyl tungsten is used as a gas source, which is gasified by heating to about 70 ° C. and sprayed near the sample portion in the sample chamber. By scanning the Ga ion beam there, a chemical reaction occurs only in the portion irradiated with Ga ions, and an amorphous tungsten film is formed. With this mechanism, it is possible to freely form an amorphous tungsten vapor deposition film in a μm size region where the Ga ion beam is scanned.

  FIG. 1 illustrates an example of the configuration of the present apparatus by showing a sectional view of the temperature measuring apparatus attached to the focused ion beam apparatus. The ion beam assist gas discharge nozzle is not shown in this figure because it is installed at a position to avoid collision. The holder 3 of the local region temperature measuring device is inserted into the vacuum casing through the chamber 2 attached to the focused ion beam casing wall 1. A preliminary exhaust mechanism 4 is attached to the chamber 2 before the temperature measuring device holder is inserted into the vacuum system. If it is used in a state where it is always inserted into the housing due to device restrictions, it is more convenient to insert the temperature measuring device only during use.

  The contact-type temperature measuring unit 5 at the tip of the holder of the local region temperature measuring device observes the target material structure in the focused ion beam device and is in the order of μm, and three of x, y, z with respect to the housing axis. The temperature measuring device holder 3 includes a fine driving device 6 and a portion (fine driving control unit) 7 for controlling the driving thereof so as to freely move in the axial direction. As an example of driving, for example, a mechanism that can be moved by a piezoelectric element from three axial directions can be applied to the holder 3, and these are remotely controlled.

  Next, the holder 3 of the local region temperature measurement apparatus has an inner flange structure 11 that can move back and forth, and an insulated conductor 8 is passed through it, but in order to improve temperature measurement accuracy A temperature compensating lead wire is used as this lead wire. The external terminal 9 is also connected to the temperature measurement unit 10 with a conductive wire. When a thermocouple is attached to the contact-type temperature measuring unit, the electromotive force is measured here. In either case, it is preferable to use a temperature compensation lead wire.

  The structure of the holder 3 of the local region temperature measuring apparatus is as follows. The holder shaft part itself moves into the housing through the chamber 2, and the inner structure 11 is movable back and forth as its internal structure. I explained earlier that I have. A contact-type temperature measurement unit is attached to the sample-side tip. As an example, in FIG. 1, the connection terminal 12 from a very small thermocouple is attached. The tip structure of the extremely small thermocouple includes a connection port 14 on the tip side of the thermocouple, a thermocouple element 15, and a thermal contact 16 that joins them together. 8 is connected to the outside. The inner rod 11 moves back and forth in the holder 3 of the local region temperature measuring device. That is, a portion 13 having a bellows mechanism capable of a sliding operation while securing a vacuum with the drive operation unit (fine drive device) 6 is held. In FIG. 1, a portion including the connection terminal 12, the thermocouple connection port 14, the thermocouple wire 15, and the thermal contact 16 corresponds to the contact-type temperature measurement unit at the tip. This local region temperature measuring device has a contact-type temperature measuring unit at the tip of the holder and an insulating guide 17 that protects the contact-type temperature measuring unit when it is taken in and out of the focused ion beam device.

  Next, the contact-type temperature measuring unit at the tip which is important in the invention of the temperature measuring device will be described in more detail with reference to FIG. When attaching ultrafine thermocouple strands and extremely small thermocouple tips, insert / remove the holder of the local region temperature measurement device, and x, y, and z directions of the minimal thermocouple tips near the observation field When moving to a position, a location collision in a narrow sample chamber with a beam-assisted deposition nozzle or the like often occurs. Therefore, an insulator guide 17 is attached to the tip of the temperature measuring holder, and when the temperature measuring holder is inserted into and removed from the housing, the tip of the extremely small thermocouple is used as a retractable type as shown in FIG. In order to protect the sample and bring it closer to the temperature measurement target portion of the sample while observing it, as shown in FIG. Move to. At this time, if the guide is parallel to the sample holder, there will be more cases where it will collide with the gas deposit during insertion, so the minimum thermocouple will move downwards by about 45 ° from the sample holder axis, preferably 45 ° or more if possible. It is preferable to have such a guide angle as possible. In general, since the angle of the ion beam deposition gun is fixed at about 80 °, Table 1 shows the degree of impact of the tip of the thermocouple in the sample chamber during operation when the inclination angle of the insulating guide is changed. Summarized in The larger the guide angle, the more advantageous is the case where it is desired to measure the temperature of the concave portion of the sample.

  Fig. 3 shows a schematic diagram of the geometric arrangement of the contact-type temperature measuring unit of the local region temperature measuring device and the observation sample at the nozzle tip from the position gun with an ion beam.

  Next, in the case where the contact-type temperature measuring unit is composed of a thermocouple, a detailed description will be given of the thermal contact portion of the thermocouple.

  In temperature measurement, accurate temperature measurement cannot be performed unless the thermal contact of the contact-type temperature measurement unit, that is, the temperature detector portion is sufficiently smaller than the measurement target. The size of the main measurement object in the present invention may be as fine as several tens of μm. That is, the case where the temperature rise becomes a problem in the focused ion beam processing apparatus is when a minute section of several tens of μm is cut out from a very small part of a large sample size of several millimeters. In a thermocouple having a hot junction size of 100 μm, the temperature is not sufficiently transmitted to the tip of the thermocouple via the hot junction. Therefore, it is necessary to process the hot contact portion into a rod shape having a diameter of about 20 μm or less and to adhere to the target sample measurement temperature portion. At this size, the thermal resistance becomes too large for simple contact, and temperature measurement is not possible, so the rod-shaped thermocouple tip can be obtained using the gas deposition function possessed by many general-purpose focused ion beam devices. There is a need for a method of adhering to the sample. Since the tip of the thermocouple can be processed by the focused ion beam processing technique, when the sample size to be measured is 10 μm, the tip diameter portion of the thermocouple is preferably processed to 10 μm or less. However, it is more important to integrate the thermocouple contact and measurement object than beam size by beam-assisted deposition. Temperature measurement becomes possible. Another reason for making the rod shape is that when the temperature measurement is completed and it is desired to remove the thermocouple from the sample, the rod-shaped portion can be easily cut and separated by the focused ion beam machining method.

  Although it is actually a very small thermocouple, the above-mentioned problem when measuring a smaller temperature measurement object is apparent from the actual photograph shown in FIG. Fig. 4 (a) shows a state in which the thermocouple contact point and the measurement object are in point contact. The thermal resistance in such point contact is large, and the adhesion area is increased by the beam assist deposition function. Was necessary. FIG. 4 (b) shows a case where the temperature measurement object is as small as 20 μm or less compared to a thermocouple contact portion having a diameter of 70 μm. In such a case, it is considered that the temperature flow is reversed. In reality, stable temperature measurement was not possible.

  In addition, it is preferable that the position which adhere | attaches a contact-type temperature measurement part is the range of 0.01-50 micrometers from an observation part temperature measurement position, for example. When the distance is smaller than 0.01 μm, the temperature measurement unit may cover the observation area, and when the distance is more than 50 μm, there may be a problem in the followability of the temperature measurement section with respect to the temperature change in the observation area. In addition, when measuring the temperature of the local region at room temperature, the accuracy is preferably within 10 μm from the temperature measurement position of the observation unit.

  Next, the material of the thermocouple will be described. As described above, the sheath-type thermocouple is difficult to use considering that the thermocouple tip is fixed a plurality of times by the adhesion method. In addition, a commercially available minimum diameter sheathed thermocouple has a diameter of about 100 μm, and is too large to be used for temperature measurement in a region of a few tens of μm, which is a subject of the present invention. Therefore, it is preferable to use a bare ultrafine wire thermocouple that can be easily reworked. At this time, the wire diameter of the ultrathin wire thermocouple is also important, and usually, for example, an ultrafine wire of 30 μm or less is used. However, when the tip portion is extremely thinned into a rod shape, for example, an ultrafine wire of 20 μm or less is preferable. As the type of the ultrafine wire thermocouple, for example, an alumel-chromel type can be stably used in a temperature range from room temperature to several hundred degrees Celsius. Further, at a low temperature, for example, a Cu-constantan type, and at a high temperature, for example, a platinum-platinum / rhodium type, etc. are selected. . Note that the tip of a commercially available thermocouple is generally a spherical contact. If the object to be measured is small, the thermal resistance at the point contact becomes large, making it difficult to use. Therefore, it is preferable to process the spherical contact with a focused ion beam so that the tip of the spherical contact has a rod shape. However, even if it is spherical, there is no problem if sufficient thermal contact with the target object can be obtained by ion beam assisted deposition.

  In addition, as described above, in order to accurately measure the temperature of the minute part, it is necessary to adhere the tip rod-shaped part of the extremely small thermocouple to the target object at the time of measurement, and after the measurement, it is cut and gradually shortened. It will become. For this reason, it is necessary to frequently replace the tip portion of the minimum thermocouple. As shown in FIG. 2, the tip portion of the tip which is the tip from the electric terminal pin which is an example of the thermocouple connection port 14 is the sample holder. It is devised so that it can be easily removed and replaced by an insertion method or the like via the thermocouple connection port 18 on the side.

  Next, the actual temperature measuring method will be described again with reference to FIG.

The object of temperature measurement which is the object of the present invention is used in a focused ion beam processing apparatus when performing high-temperature observation using a small area of several tens of μm that is finely processed or extracted, or a heating stage. In many cases, the region is observed with a scanning ion microscope image of the focused ion beam apparatus, that is, a region of several tens of μm to several hundreds of μm. With respect to such a small object, as shown in FIG. 3, the rod-like portion 16 (corresponding to the thermal contact 16) at the tip of the extremely small thermocouple is discharged from the beam assist deposition nozzle 19, for example, , W (CO) ₆ gas is ejected to the sample observation site (in the figure, the gas ejection region is indicated by 20), and this gas ejection region 20 is irradiated with a Ga ion beam to perform a kind of chemical vapor reaction. The amorphous W film is formed and bonded between the sample and the tip of the rod-shaped thermocouple. In FIG. 3, this adhesion region is indicated by 21. In this state, since the temperature measurement object 23 and the extremely small thermocouple are bonded, the temperature sensed by the rod-like contact portion 16 is the voltage difference between the two thermocouple wires 15 as the thermocouple connection port 14 and the electric terminal. The pin 12 is connected to an external voltage measuring instrument for measuring electromotive force.

  At this time, a significant difference from the temperature measurement method using a normal thermocouple is that Ga ion is irradiated to the temperature measurement target part at the time of temperature measurement. Since the electromotive force value generated by the measurement conditions fluctuates, as a result of investigation from various viewpoints, the ion current resulting from Ga ion irradiation and the current due to secondary electrons generated at that time are detected through the thermocouple compensation line. It turns out that there is a case. In order to drastically prevent this, it has been found that it is necessary to electrically ground the temperature measurement object as indicated by reference numeral 22 in FIG. For this reason, the object which can measure temperature correctly with the method of this invention is restrict | limited to a conductor. In addition, it is necessary that the extremely small thermocouple tip and the temperature measurement object are electrically at zero potential.

  Examples of the present invention will be described below.

Example 1
As an embodiment of the present invention, it is possible to measure the amount of temperature rise in the vicinity of a processed portion when a minute region is processed with an ion beam. Under the measurement conditions as shown in FIG. 5, the temperature was measured at a point 0.01 μm away from the processing region when the irradiation power of the irradiated Ga ion beam was gradually increased. The sample was grounded on a conductive sample stage. As a result, the temperature change when the ion beam current amount is sequentially changed is shown in FIG. It was found that the temperature rise amount was at most 60 ° C. even at the maximum value of the irradiation power during general beam processing. It was also found that the ion beam used for general processing did not rise above 40 ° C. This is a case of a conductive metal, and the presence or absence of temperature rise during ion beam processing has been a big problem in the past, but this experiment has led to the conclusion that the amount is almost negligible. Of course, the results with insulating materials are different. At this time, the angle of the insulating guide is 45 ° so that the extremely small thermocouple contact portion does not collide with the beam assist deposition device. The thermocouple contact portion has a rod shape with a diameter of 30 μm. Furthermore, in this example, when the contact portion of the thermocouple is a point contact, or when the sample is not grounded, a certain extra electromotive force is generated and the temperature rises. A misleading result was obtained. Only when all the conditions of the temperature measurement method of the present invention are satisfied, such a temperature measurement in the local region becomes possible.

(Example 2)
One of the advantages of the focused ion beam processing apparatus as a tissue observation apparatus is that a fine unevenness contrast of the sample and a contrast depending on the azimuth change can be easily obtained. Further, the internal structure can be observed by ion beam processing from the sample surface at a high temperature. For this reason, when observing the sintering process, the apparatus of the present invention was used to measure the actual sample temperature. The state of the experiment is schematically shown in FIG. 7 (a). As shown in the figure, a small heating stage was mounted in the focused ion beam apparatus, and the sample stage was filled with a powder sample. At this time, since the unevenness was severe, an insulating guide having an angle of close to 80 ° was used even in an extremely small temperature measuring device so that the thermocouple contact portion could be pushed into the powder.

Next, using an alumel-chromel type miniature thermocouple, the heating current value was kept at 250 mA and held for 10 minutes until the temperature of the thermocouple became constant. This is because it has been confirmed by repeated experiments in advance that the temperature rise of the heating stage and the entire sample becomes uniform by using this extremely small thermocouple and maintaining the heating current value of the heater at 250 mA. . In this experiment, in this state, a rod-shaped thermocouple contact portion having a diameter of 20 μm was pushed into the powder, and was bonded and integrated with the sample using a beam-assisted deposition apparatus. It is a position 50 μm away from the center of the observation field. Then, the heating current value was gradually increased, and the temperature of the sample portion was measured from the generated electromotive force at that time. The result is shown in FIG. 7 (b). In FIG. 7B, the rhombus plot indicates the temperature at each heating current value, and the square plot indicates the generated electromotive force at each heating current value. From this, it was found that the temperature was raised to about 1150 ° C. with a temperature rise change as shown in FIG. 7 (b). As is apparent from this graph, it was possible to accurately investigate the temperature rise change of the observed tissue which is not a simple proportion, using the focused ion beam apparatus equipped with the local region temperature measuring apparatus of the present invention. This result was applied to the observation of structural changes such as the initial sintering process. As a result, it has been clarified that the high-temperature in-situ observation experimental technique has been dramatically improved.

  As mentioned above, although preferred embodiment of this invention was described referring an accompanying drawing, it cannot be overemphasized that this invention is not limited to this example. It will be apparent to those skilled in the art that various changes and modifications can be made within the scope of the claims, and these are naturally within the technical scope of the present invention. Understood.

It is a cross-sectional schematic diagram of the state in which the temperature measuring device which concerns on one Embodiment of this invention was attached to the focused ion beam apparatus. It is a schematic diagram for demonstrating the detail of the holder front-end | tip part of the local region temperature measuring device which concerns on the embodiment. It is explanatory drawing which shows the positional relationship of the measuring object in a focused ion beam apparatus, a gas deposition nozzle, and a contact-type temperature measurement part. It is a photograph which shows the positional relationship of a measuring object and a thermocouple. 6 is a schematic diagram for explaining a state of adhesion of a contact-type temperature measurement unit to a measurement object in Example 1. FIG. It is a graph which shows the relationship between the amount of ion beam electric currents in Example 1, and measurement temperature. It is a figure which shows the (a) measurement condition and (b) measurement result in Example 2. FIG.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Focused ion beam housing | casing wall 2 Chamber 3 Holder 4 Pre-exhaust mechanism 5 Contact type | mold temperature measurement part 6 Fine movement drive device 7 Fine drive control part 8 Conductor 9 External terminal 10 Temperature measurement part 11 Inner tube structure 12 Connection terminal 13 Bellows mechanism 14 Thermocouple connection port 15 Thermocouple wire 16 Thermal contact 17 Insulation guide 18 Thermocouple connection port 19 Beam assist deposition nozzle 20 Gas ejection region 21 Adhesion region 22 Ground 23 Temperature measurement object

Claims (6)

A focused ion beam device having a local region temperature measurement function and a beam assist deposition function,
A local area temperature measuring device;
An ion gun that emits an ion beam;
A sample chamber for installing a sample to be subjected to fine processing or tissue observation while irradiating the ion beam;
A gas discharge nozzle for beam assist deposition for ejecting a deposition gas to be reacted with an ion beam into the sample chamber;
Comprising at least
The local region temperature measuring device and the beam assisted deposition gas discharge nozzle are arranged at positions opposed to the irradiation axis of the ion beam irradiated from the ion gun toward the sample ,
The local area temperature measuring device is:
A contact-type temperature measuring unit provided at the tip of the holder of the local region temperature measuring device;
An insulating guide for protecting the contact-type temperature measuring unit;
A fine movement drive control unit for exposing the contact-type temperature measurement unit from the insulating guide;
At least Bei to give a,
The insulating guide has a slope of 45 ° or more with respect to the holder axis ;
The focused ion beam device having a local region temperature measuring device, wherein the contact-type temperature measuring unit is moved along the insulating guide and exposed . The contact temperature measuring unit, Ri Do from the thermocouple,
2. The focused ion beam device having a local region temperature measuring device according to claim 1 , wherein a hot contact portion of the thermocouple is processed by a focused ion beam and has a rod shape having a diameter of 50 μm or less. . The contact temperature measuring unit, characterized in that said a structure detachable in the holder tip and insertion system, focused ion beam apparatus having a local region temperature measuring device according to claim 1 or 2. A method of measuring a temperature of a local region in a focused ion beam device, which measures the temperature of a temperature measurement object during processing, in the focused ion beam device including the local region temperature measuring device according to any one of claims 1 to 3. Because
The contact-type temperature measurement unit is moved and exposed from the insulating guide by the fine movement drive control unit, and the temperature-measurement object and the contact-type temperature measurement unit are moved by the beam-assisted deposition function in the vicinity of the observation region of the temperature measurement object. Then, the ground is taken through the temperature measurement object, and the observation region of the temperature measurement object is processed into a predetermined shape by a focused ion beam processing method while measuring the temperature of the temperature measurement object. A method for measuring a temperature in a local region in a focused ion beam apparatus, wherein after the processing is finished, an adhesive portion between the temperature measuring object and the contact-type temperature measuring unit is separated by a focused ion beam processing method. A temperature measurement method for a local region in a focused ion beam device, which measures the temperature of a temperature measurement object during heating in the focused ion beam device including the local region temperature measurement device according to any one of claims 1 to 3. Because
After grounding through the temperature measurement object, observe the state change of the observation region while heating / cooling the temperature measurement object to a predetermined temperature, and at any temperature, the contact-type temperature measurement unit is a fine movement drive control unit The temperature measurement object is moved and exposed from the insulation guide, and the temperature measurement object is bonded to the contact-type temperature measurement unit by a beam assist deposition function in the vicinity of the observation area of the temperature measurement object. A sample in a focused ion beam apparatus characterized by measuring the temperature of an object and, after completion of the temperature measurement, separating a bonded portion between the temperature measurement object and the contact-type temperature measuring unit by a focused ion beam processing method. A method for measuring the temperature of the local area during heating. The local region temperature measurement method according to claim 4 or 5 , wherein a position where the contact-type temperature measurement unit is bonded is in a range of 0.01 to 50 µm from the observation region.