JP2005148003A - Cross section working apparatus and cross section evaluating method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a work section evaluating apparatus and a cross section evaluating method, capable of working a cross section and accurately acquiring information on a work section in a state where the temperature of a specimen is regulated. <P>SOLUTION: A cross section working apparatus used for working the cross section of the specimen, is provided with a stage for placing the specimen; a temperature regulation means for regulating the temperature of the specimen; a beam generating means for irradiating the specimen with a beam to work the specimen; and a sealing means for containing/sealing the specimen and the stage before conveying the specimen and the stage in a step prior to working. Furthermore, the cross section evaluating method is provided with a first step in which the temperature of the specimen is regulated; a second step in which the specimen is irradiated with the beam, and the cross section is cut and separated; a third step in which the specimen whose temperature is regulated is sealed; a fourth step in which the sealed specimen is conveyed to other apparatus; and a fifth step in which the conveyed specimen is evaluated by using the other apparatus. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a sample processing apparatus, and more particularly to a cross-section processing apparatus and a cross-section evaluation method for processing a cross-section of a sample whose state and form change due to temperature changes.

  The demand for cross-sectional evaluation of organic materials such as ecosystems and plastics and the processing of fine structures are increasing as functional devices increase.

  As main cross-section preparation methods used to obtain information on the structure of organic matter, cutting methods using blades, resin embedding methods, freeze embedding methods, freeze cleaving methods, ion etching methods, etc. are known, When observing the internal structure of an organic substance with an optical microscope, a method is generally employed in which the organic substance is embedded with a resin and then cut with a microtome.

  However, the optical microscope is limited to the macroscopic observation of the cross section, and the cutting position cannot be specified. Therefore, in order to observe and analyze the structure at the specified position, it is very often necessary to repeat the cross section preparation work. It took a lot of effort.

Therefore, recently, as disclosed in Patent Document 1, a focused ion beam (FIB) apparatus capable of processing a predetermined place has been developed. The FIB apparatus is an apparatus that performs processing by etching or the like by finely focusing an ion beam from an ion source and irradiating a processing sample. This FIB etching technique is becoming quite popular, and is widely used particularly for structural analysis of semiconductors, failure analysis, transmission electron microscope sample preparation, and the like.
JP-A-5-8247

  However, when observing and analyzing the cross-sectional structure of a sample whose state or form changes depending on the temperature, such as organic matter, using the above-described conventional FIB apparatus, the temperature of the sample changes due to heat generated during FIB processing. As a result, the state and form of the sample change, and the cross-sectional structure of the sample cannot be analyzed accurately.

  An object of the present invention is to solve the above-described problems and provide a cross-section processing apparatus including information acquisition that can acquire information on a surface for which information is desired to be acquired with the temperature of a sample adjusted.

  Furthermore, the present invention provides a cross-section processing apparatus and a cross-section evaluation method that can solve the above-described problems and can process a cross-section while adjusting the temperature of a sample.

  In addition, the present invention provides a processing unit evaluation apparatus and a cross-sectional evaluation method capable of solving the above-mentioned problems and processing a sample in a state in which the temperature of the sample is adjusted and accurately acquiring information on the processing unit. There is to do.

In accordance with the present invention,
An apparatus for processing a cross section of a sample,
A mounting table for mounting the sample;
Temperature adjusting means for adjusting the temperature of the sample;
Beam generating means for irradiating the sample with a beam to process the sample;
Sealing means for storing and sealing the sample and the mounting table before transporting the mounting table and the sample before processing;
It is provided with the cross-section processing apparatus characterized by comprising.

Also according to the present invention,
A first step of adjusting the temperature of the sample;
A second step of irradiating the sample with a beam to cut out a cross section;
A third step of sealing the temperature controlled sample;
A fourth step of transporting the sealed sample to another device;
A fifth step of evaluating the conveyed sample using the other device;
A method for evaluating a cross section is provided.

  In the present invention as described above, since the temperature of the sample is always adjusted, for example, the temperature of the sample is maintained at a desired temperature even during FIB processing. Therefore, there is no change in the state or form of the sample as in the prior art.

  In the present invention, the cross section does not only indicate a surface viewed from one surface inside the sample, but also when the sample is processed (including deposition and etching), when viewed from a certain viewpoint after the processing. Includes observable surfaces.

  As described above, according to the present invention, exposure of a surface to obtain information and acquisition of information are performed in a state in which a sample that changes in state and form due to temperature change is adjusted to a desired temperature. It is possible to obtain accurate information on the desired surface.

  Further, when the present invention is used as a cross-section evaluation apparatus, it is possible to perform cross-section processing and evaluation while maintaining a sample whose state or form changes due to a temperature change at a desired temperature. Evaluation can be made.

  Next, embodiments of the present invention will be described with reference to the drawings.

(Embodiment 1)
FIG. 1 is a schematic configuration diagram of a focused ion beam apparatus for cross-section processing that is a first embodiment of the cross-section processing apparatus of the present invention. The focused ion beam apparatus includes a heat retaining unit 2a for fixing the sample 1 and maintaining the temperature of the fixed sample 1 at a set temperature, and a holding base 2 for supporting the heat retaining unit 2a. The heat retaining unit 2 a can be accommodated in the sample chamber 3.

The sample chamber 3 is provided with an ion beam generating unit 4 for irradiating the sample 1 fixed to the heat retaining unit 2a with an ion beam and a detecting unit 5 for detecting a signal generated from the sample 1 by irradiation of the ion beam. Furthermore, a gas introduction part 6 and a cover 7 are provided. The inside of the sample chamber 3 is evacuated by a pump (not shown) so that a predetermined low pressure can be maintained, so that ion beam irradiation is possible. In the present invention, the pressure in the sample chamber is preferably 1 × 10 ² Pa or less.

  The ion beam generator 4 is used not only for irradiating the sample 1 with an ion beam and cutting out a cross section, but also for SIM observation. In the case of SIM observation, secondary electrons or secondary ions generated when the sample 1 is irradiated with an ion beam are detected by the detector 5 and imaged based on a detection signal from the detector 5. .

  The gas introduction unit 6 is used to control the atmosphere around the sample 1. It can also be used to increase the pressure in the sample chamber 3. After separating the sample chamber side and the vacuum line while keeping the ion beam generating unit 4 and the detector 5 in a high vacuum with a shutter (not shown), the sample 1 can be covered with the cover 7 in the sample chamber 3 together with the heat retaining unit 2a. The sample chamber 3 leaks. Since the sample 1 is in the cover 7 and the atmosphere around the sample is controlled from the gas introduction unit 6, a sample having a necessary condition can be selected depending on the material and temperature of the sample 1. Further, the leakage of the sample chamber 3 can be performed from a leak valve (not shown).

  A detection signal from the detector 5 is supplied to the control unit 9, and the imaging during the SIM observation and the imaging during the SEM observation are performed by the control unit 9. For example, the control unit 9 acquires video information (mapping information) from the detection signal from the detector 5 and visualizes the acquired video information on a display device (not shown). In addition, the control unit 9 controls the generation of the ion beam in the ion beam generation unit 4 and controls the irradiation and scanning of the sample 1 with the ion beam. The beam scanning can be controlled on the beam side and / or on the stage side where the sample is fixed. However, in consideration of the scanning speed and the like, it is desirable to control on the beam side.

  Note that the configuration of the ion beam generation unit and the like may be a configuration as described in JP-A-6-342638.

(Configuration of temperature adjustment means)
The temperature adjusting means in the present embodiment includes a heat retaining unit capable of adjusting the temperature of the sample. The heat retaining unit 2a is a sample stage with a temperature controller, for example. FIG. 2 shows a schematic configuration of the sample stage with a temperature controller.

  Referring to FIG. 2, a sample stage with a temperature controller includes a sample stage 8 having a temperature variable mechanism 12 at a portion where the sample 1 is fixed, a thermometer 11 a that directly detects the temperature of the sample 1, and a temperature variable mechanism 12. A thermometer 11b that detects the temperature in the vicinity of the sample 1 fixed to the temperature variable mechanism 12 and adjusts the temperature in the temperature variable mechanism 12 based on the temperature detected by the thermometer 11b. And a temperature control unit 9a for keeping the sample 1 at a preset temperature.

  In addition, although not shown in FIG. 2, the display part which displays the temperature detected with the thermometer 11a is provided, and the operator can confirm the temperature of the sample 1 from the temperature displayed on this display part. it can. Moreover, the temperature control part 9a can also be comprised so that the temperature in the temperature variable mechanism 12 may be adjusted based on the temperature detected by both the thermometers 11a and 11b, and it is more accurate by comprising in this way. In addition, the temperature of the sample 1 can be controlled. In some cases, control may be performed using only the thermometer 11b.

  The temperature variable mechanism 12 is unitized with the thermometer 11b, and a unit capable of controlling a necessary temperature range can be incorporated in the sample stage 8 according to the set temperature. Examples of such a unit include a high temperature unit having a heating mechanism such as a heater and a low temperature unit having a cooling mechanism. Moreover, it is also possible to use a unit having a temperature variable function on both the low temperature side and the high temperature side near room temperature as required.

  The sample stage 8 is connected to a holding table 2 (not shown), and the fixed sample 1 can be mechanically moved up and down, left and right, or inclined, thereby moving the sample 1 to a desired evaluation position. be able to. The movement control of the sample 1 in the sample stage 8 is performed by the control unit 9 described above.

  The cooling mechanism may be a cooling mechanism such as a Peltier element or a helium refrigerator. Alternatively, a method may be used in which a refrigerant pipe for flowing a refrigerant is provided on the side of the heat retaining unit facing the portion where the sample is fixed, and a liquid or vaporized refrigerant such as nitrogen or water is in thermal contact with the heat retaining unit.

  Further, in order to increase the efficiency of absorbing heat generated during processing, it is preferable to devise to increase the contact efficiency between the sample and the cooling unit (heat retaining unit).

  Such a device can be configured to wrap a sample, for example, and a sample holder having a shape that does not obstruct the optical system of the device used during processing and observation, or the shape of the sample is mounted It is possible to keep the maximum contact area while processing it into a shape matched to the above.

  Or you may make it further coat | cover only the part which a beam system does not obstruct | occlude the cooling member which coat | covers the non-processed area | region of a sample.

(Section evaluation method of sample)
Below, the cross-sectional evaluation method according to the present invention will be described. In addition, the cross section of a sample here shows the cross section of the element and material to evaluate. In addition, if a sample cross section is set in advance on the upper surface of the sample, it is possible to evaluate information on the surface direction of a certain depth of elements and materials.

  FIG. 3 is a flowchart showing a procedure for evaluating a cross section of a sample using the cross section processing apparatus shown in FIGS. 1 and 2. Hereinafter, the procedure for cross-sectional evaluation will be described with reference to FIG. 3, and the control for SIM observation by the control unit 9 and the temperature control of the sample by the temperature control unit 9a in accordance with the procedure will be specifically described.

  First, the sample 1 is fixed to a predetermined position (temperature variable mechanism 12) of the sample stage 8 (step S10), and after introducing it into the sample chamber 3, the evaluation temperature is set (step S11). When the evaluation temperature is set, the temperature in the temperature variable mechanism 12 is controlled by the temperature controller 9a, and the temperature of the sample 1 is maintained at the set evaluation temperature.

  The temperature of the sample 1 at this time is detected by the thermometer 11a, and the handler can check whether the sample 1 is maintained at the evaluation temperature from the detected temperature displayed on the display unit (not shown). it can.

  In the present embodiment, it is preferable to perform processing while the sample is cooled from room temperature. Moreover, when it cools to the temperature below 0 degree | times, when there exists the water | moisture content in a sample, it can solidify and it is more preferable.

  In such a cooling process, the sample is first cooled to a predetermined temperature below room temperature, the cooled sample is held in a reduced-pressure atmosphere, and the focused beam is irradiated while absorbing heat generated from the vicinity of the irradiation surface of the sample. Thus, it may be processed while maintaining the shape of the portion that is not irradiated.

  Moreover, when cooling a sample, you may cool rapidly from a room temperature state. In this case, it is preferable to cool at a cooling rate of 40 ° C./min or more. Thereby, for example, when it is desired to measure the cross-sectional shape of the mixture whose dispersibility changes depending on the temperature, the cross-section in a rapidly cooled state can be observed.

  The cooling step is preferably performed before the decompression step. This makes it possible to suppress evaporation of the sample due to reduced pressure. However, when the sample is made of a substance with a small amount of evaporation, the sample may be cooled simultaneously with decompression.

  The cooling process varies depending on the target sample, but in the case of a general organic substance such as PET, it is preferable to cool in a temperature range of 0 ° C. to −200 ° C., preferably −50 ° C. to −100 ° C.

  Further, if the processing time and the cooling time become too long during low-temperature cooling, residual gas in the sample chamber and substances generated during processing may be adsorbed on the low-temperature sample, making desired processing and observation difficult. For this reason, it is preferable to provide trap means for adsorbing residual gas and substances generated during processing, and to process and acquire information while cooling the trap means.

  In the present invention, the target sample can be suitably applied to organic substances, in particular, substances that are sensitive to heat, such as proteins and other biological substances, and compositions containing moisture. In particular, a composition containing moisture can be processed while keeping moisture in the sample, which is preferable.

  In particular, when the focused ion beam is irradiated, it is performed in a reduced pressure atmosphere. Therefore, when processing a composition containing water or highly volatile organic molecules, the water may evaporate due to heat generated during processing, and the effect of providing the temperature adjusting means of the present invention is great. .

  In order to perform more accurate processing and structural evaluation, it is also preferable to include a step of extracting a suitable holding temperature during processing in advance. In this case, it is preferable to use a sample equivalent to the sample to be processed as a reference, perform processing at a plurality of set temperatures, and determine a preferable holding temperature after examining the relationship between the damage of the processed portion and the cooling temperature.

  In addition, in the case of a general FIB processing apparatus, after processing, it is often moved to another apparatus such as an SEM apparatus to perform other operations such as observation. After returning the temperature to room temperature, it had to move to the observation means. In the present embodiment, the sample can be observed after being processed in a cooled state, and suitable sample processing can be provided without worrying about the influence of the processed surface due to adhesion of water droplets or the like on the sample surface during cooling. .

  After confirming that the sample 1 is maintained at the evaluation temperature, SIM observation of the surface of the sample 1 is performed while constantly confirming the temperature of the sample 1 (step S12). In this SIM observation, the control unit 9 controls the irradiation of the ion beam by the ion beam generation unit 4 and the movement of the sample stage 8, thereby scanning the sample 1 with the ion beam from the ion beam generation unit 4. Further, in synchronization with this scanning, secondary electrons (or secondary ions: the same applies hereinafter) are detected by the detector 5, and the control unit 9 displays a SIM image (not shown) based on the detection signals of the secondary electrons. Display on the display. Thereby, the handler can perform SIM observation of the surface of the sample 1. This SIM observation uses a weak ion beam for observation.

  Next, a cross-sectional evaluation position is accurately determined from an image obtained by SIM observation of the surface of the sample 1 (a SIM image displayed on the display unit) (step S13), and the determined cross-sectional evaluation position is further processed by a processing beam. The SIM is observed (step S14).

  Next, FIB processing conditions are set (step S15). In this FIB processing condition setting, a cutting region and a cutting position are determined on the SIM image obtained by the surface SIM observation in step S14, and further, cross-section processing conditions for acceleration voltage, beam current, and beam diameter are set. The cross-section processing conditions include rough processing conditions and finishing processing conditions, which are set at this point. The rough machining conditions are such that the beam diameter and the amount of energy are larger than those of the finishing machining conditions. The cutout region and cutout position can be determined on the SIM image of the observation beam obtained in step S12. However, in consideration of the problem of accuracy, the SIM of the ion beam that is actually processed is taken into consideration. More preferably, it is performed on the image.

  When the FIB machining conditions are set, first, FIB machining (rough machining) is performed (step S16). In this rough machining, the control unit 9 controls the ion beam generator 4 under the rough machining conditions set above, and further controls the movement of the sample stage 8, so that the cutout region and cutout position determined in step S15 are controlled. Then, an ion beam of an amount necessary for cutting is irradiated.

  After rough processing, the surface of the sample 1 is observed by SIM, and it is confirmed whether or not the surface of the sample 1 is processed to a desired position on the image (SIM image) obtained by the SIM observation (step S17). If it has not been machined to the desired position, the above steps S16 and S17 are repeated. Even when the processed surface SIM image of the cross section is extremely rough, the above steps S16 and S17 are repeated. In this case, an operation such as gradually decreasing the amount of the ion beam is added. The control of the surface SIM observation in step S17 is the same as that in step S12.

  If it is confirmed that the rough machining has been performed to the vicinity of the desired position, then FIB machining (finishing) is performed (step S18). In this finishing process, the ion beam generator 4 is controlled by the control unit 9 under the finishing process conditions set above, and the movement of the sample stage 8 is further controlled, so that the part processed roughly in step S16 is finished. A necessary amount of ion beam is irradiated. By this finishing process, for example, a smooth cross section that can be observed at a high magnification using a scanning electron microscope can be produced.

  Next, the sample chamber 3 and the vacuum line are separated from each other while the ion beam generator 4 and the detector 5 are kept at a high vacuum by a shutter (not shown), and then the sample chamber 3 is leaked (step S19). At this time, the gas used for the leak can be appropriately selected depending on the evaluation sample material and the evaluation temperature, but in order to prevent moisture and the like from adhering to the sample, it is preferable to use a dry gas from which moisture has been removed. For example, nitrogen or an inert gas is used. If necessary, the temperature change of the sample can be minimized by using a gas having a preset temperature.

  Further, the cover 7 in the sample chamber 3 is put on the sample 1 together with the heat retaining portion 2a (step S20), and the sample stage with the sample 1 is put on the sample while the cover 7 is attached while the atmosphere inside the cover is controlled by the gas introducing portion 6. Remove from the chamber (step S21).

  Finally, the sample 1 produced and taken out as described above is transferred to another evaluation apparatus (for example, SEM), and the cross section of the sample is evaluated (step S22).

  As described above, in the cross-section evaluation method of the present embodiment, the temperature of the sample 1 to be evaluated can always be kept at a set value, so that the state and form of the sample 1 do not change during FIB processing. Therefore, accurate microstructure evaluation can be performed.

  In the embodiment described above, the processing of the sample by the ion beam does not generate shear stress, compressive stress and tensile stress as seen in machining such as cutting and polishing, and therefore, materials having different hardness and brittleness are mixed. It is possible to produce a sharp cross section for a composite sample, a sample having voids, a fine structure of an organic substance formed on a substrate, a sample that is easily dissolved in a solvent, and the like.

  In addition, because the sample temperature can be kept at the set value, even if the sample contains materials whose state and form change depending on the temperature, the specified position can be obtained at the desired set temperature without causing structural destruction of the layer. Can be observed directly.

  The cross-sectional evaluation method in each embodiment described above is used to analyze a desired temperature of a sample including a polymer structure on various substrates such as glass, a polymer structure including microparticles and liquid crystals, a particle dispersion structure in a fibrous material, and a temperature transition material. It is effective against this. Needless to say, it is also effective for a sample that is easily damaged by an ion beam or an electron beam.

(Embodiment 2)
In the present embodiment, as shown in FIG. 4, in addition to the configuration of the first embodiment, a trap means 16 is provided for preventing reattachment of residual gas in the sample chamber and substances generated during processing to the sample.

  The trap means is made of a metal having a good thermal conductivity and is held at a temperature equal to or lower than the temperature of the sample during cooling of the sample.

  This embodiment is effective in preventing the adhesion of impurities to the sample when processing and observation are performed with the sample held at room temperature or lower.

  Such a trap means is placed at a position that does not hang on the beam system during detection and processing in a state in which the mounting table on which the sample is placed, the ion beam generating means, the electron beam generating means, and the detecting means are arranged. Be placed. In order to improve trapping efficiency, it is preferable that the trap means be positioned as close to the sample as possible as long as it does not interfere with detection and processing. Furthermore, it is possible to arrange one or more places in the sample chamber kept at a low pressure.

(Embodiment 3)
In the present embodiment, as shown in FIG. 5, an apparatus having a configuration in which a sample chamber is separated from a main body that performs sample processing is shown. After the sample is processed in the main body 8, the sample is transferred to the sample chamber 3 while maintaining the vacuum, and after separating the main body 8 and the vacuum line, the dry gas is introduced from the gas introduction unit 6 as in the first embodiment. Can do. As a result, gas introduction does not reach the main body 8 at all, and the sample chamber 3 can be minimized. Therefore, it is possible to reduce the amount of gas from the gas introduction part, and the temperature of the sample 1 can be easily controlled.

(Embodiment 4)
The example which used the apparatus in this invention as a cross-sectional evaluation apparatus in the manufacturing process of a liquid crystal display device or an organic semiconductor is shown.

  In the present embodiment, a case where temperature adjustment is performed on a sample having a relatively large area will be described.

  If you want to accurately evaluate the state of the cross section of a part of a large sample such as a glass substrate coated with liquid crystal used in a large-screen liquid crystal display device, adjust the temperature locally only in the area near the processed part. However, it is also preferable to adjust the temperature of the entire substrate. In this case, it is preferable to cool the entire holder by providing a refrigerant flow tube for flowing a refrigerant at a position facing the sample installation surface of the heat retaining unit.

  Here, an example in which the cross-sectional evaluation of the sample is actually performed using the cross-sectional evaluation apparatus of each of the above-described embodiments will be described.

(Example 1)
In this embodiment, the focused ion beam apparatus for cross-section processing shown in FIG. 1 was used. As the heat retaining unit 2, a liquid crystal (two-frequency drive liquid crystal: DF01XX manufactured by Chisso Corporation) is used on a glass substrate using a sample stage with a temperature controller shown in FIG. A cross-sectional evaluation of a sample in which a polymer structure (polymerized monomer: HEMA, R167, HDDA mixed with liquid crystal and polymerized) was prepared was performed according to the following procedure.

  First, the sample was fixed with a carbon paste on a unit having a low temperature variable mechanism, and this unit was set on the sample stage 8. After the sample stage 8 on which this sample was set was introduced into the sample chamber 3, the sample chamber 3 was evacuated to a predetermined low pressure.

  Next, the set temperature was set to −100 ° C., and it was confirmed that the sample was maintained at the evaluation temperature. Surface SIM observation was performed on the region including the cross-sectional observation position of the sample while constantly checking the sample temperature. From the image obtained by surface SIM observation, the substantially central part of the sample was determined as the cross-sectional observation position. The ion beam at this time was performed under extremely weak conditions in the observation mode. Specifically, a gallium ion source was used, the acceleration voltage was 30 kV, the beam current was 20 pA, and the beam diameter was about 30 nm. And the cross-section processing position was designated with respect to the taken-in SIM image.

  Next, FIB processing (rough processing) was performed on the designated cross-section processing position. Specifically, a rectangular recess having a 40 μm square and a depth of 30 μm was formed at the cross-section processing position with an acceleration voltage of 30 kV, a beam current of 50 nA, and a beam diameter of about 300 nm. In this rough processing, the processing was performed step by step under weak conditions, and during processing, the surface of the sample being processed was sometimes observed by SIM to confirm whether it was processed close to the desired position. When the processing was almost completed, the beam was switched to a weak beam for observation, and the processing cross section was adjusted so that it could be scanned at an angle of about 60 °, and cross section SIM observation was performed.

  After confirming that the workpiece has been processed to the desired position, as a finishing process to improve the cross-section processing accuracy, rough processing was performed with a narrower beam than in rough processing under the same weak conditions as in SIM observation. The cross-section processing position was further processed. FIG. 6A is a schematic view of a cross section produced by this FIB processing. A rectangular recess is formed in the approximate center of the sample 30 by irradiation with the ion beam 20. In cross-section SIM observation, the stage was tilted and confirmed by irradiating a weak beam for observation at an angle as shown in FIG.

  Next, after slightly raising the pressure in the sample chamber 3 with dry nitrogen from which water has been sufficiently removed, the sample is covered with the cover 7 while introducing the same dry nitrogen from the cover 7 slightly from the gas introduction part 6. Sample 1 was removed from the FIB apparatus.

  Finally, the sample prepared as described above was introduced into the SEM while maintaining the sample temperature, and SEM observation of the cross section was performed.

  The conditions for SEM observation at this time were an acceleration voltage of 800 V and an imaging magnification of up to 50,000 times. By this SEM observation, it was possible to observe how the liquid crystal was wrapped in the polymer layer.

  As described above, in this example, FIB processing was performed while maintaining the temperature of the sample at −100 ° C., so that the cross-section processing could be performed without the liquid crystal layer being darrel during processing. Moreover, since it introduce | transduced into SEM and SEM observation was able to be performed, maintaining the temperature as it was, it was able to observe cross-section that a liquid crystal exists in a polymer.

(Example 2)
In this example, cross-sectional evaluation of polymer particles (polystyrene) produced on a pet substrate was performed according to the following procedure. The processed part was the end of the sample, and the evaluation was SEM observation and elemental analysis.

  The set temperature was set to about 10 ° C., and processing was performed to a depth of about 60 μm by cutting about 10 μm with a length of about 20 μm on one side of the sample. In order to prevent charge-up before FIB processing, platinum having a thickness of about 100 nm was deposited on the surface of the sample by ion beam sputtering. Other than the above, finishing was performed under the same conditions as in Example 1 above. FIG. 7A is a schematic view of a cross section produced by this FIB processing. A rectangular recess is formed on one side surface of the sample 31 by irradiation with the ion beam 20.

  Next, a cover was attached in the same manner as in Example 1 and introduced into an SEM with an EDS detector. When the sample 31 was tilted and observed by SEM, it was found that the polymer particles were in close contact with the substrate. The conditions at this time were an acceleration voltage of 15 kV and a magnification of about 30,000 times.

  Next, when characteristic X-rays emitted from the cross section of the sample 31 during the SEM observation were taken to obtain a mapping image (elemental analysis), it was found that aluminum was dispersed in the polymer. FIG. 7B is a schematic diagram showing electron beam irradiation and characteristic X-ray emission during the elemental analysis. The electron beam 21 is irradiated perpendicularly to the cross section of the sample 31 shown in FIG. 7A, and characteristic X-rays are emitted from the cross section of the sample 31 in response to this irradiation. Elemental analysis was performed by detecting the emitted characteristic X-rays.

  In the present embodiment, the method for evaluating the cross section of the sample has been described, but the present invention is not limited to this. For example, the present invention also includes a configuration in which the surface adhering substance is removed, the surface to be observed is exposed, and the surface is observed.

It is a schematic block diagram of the focused ion beam processing apparatus for cross-section processing which is 1st Embodiment of the cross-section evaluation apparatus of this invention. It is a block diagram which shows schematic structure of the sample stage with a temperature controller which is an example of the heat retention part shown in FIG. It is a flowchart figure which shows one procedure of the cross-section evaluation of the sample using the focused ion beam processing apparatus for cross-section processing shown in FIG. It is a schematic block diagram of the focused ion beam processing apparatus for cross-section processing which is 2nd Embodiment of the cross-section evaluation apparatus of this invention. It is a schematic block diagram of the scanning electron microscope for process surface observation which is 3rd Embodiment of the cross-sectional evaluation apparatus of this invention. (A) is a schematic diagram which shows an example of the cross section produced by FIB process, (b) is a schematic diagram which shows the state at the time of SIM observation of the cross section shown to (a). (A) is a schematic diagram which shows an example of the cross section produced by FIB process, (b) is a schematic diagram which shows the state at the time of elemental analysis of the cross section shown to (a).

Explanation of symbols

DESCRIPTION OF SYMBOLS 1, 30, 31 Sample 2 Holding stand 2a Heat retention part 3 Sample room 4 Ion beam generation part 5 Detector 6 Gas introduction part 7 Cover 8 Sample stage 9 Control part 9a Temperature control part 11a, 11b Thermometer 12 Temperature variable mechanism 16 Trap Means 20, 21 Ion beam 22 Electron beam 23 Characteristic X-ray

Claims (8)

An apparatus for processing a cross section of a sample,
A mounting table for mounting the sample;
Temperature adjusting means for adjusting the temperature of the sample;
Beam generating means for irradiating the sample with a beam to process the sample;
Sealing means for storing and sealing the sample and the mounting table before transporting the mounting table and the sample before processing;
A cross-section processing apparatus comprising:   In the state where the sample is adjusted to a preset temperature by the temperature adjusting means, sample processing by the beam generating means, acquisition of information by the detecting means, and attachment of a cover with atmospheric protection means, a gas introducing means is attached. The cross-section processing apparatus according to claim 1, wherein gas is introduced into the cover.   The cross-section processing apparatus according to claim 1, wherein the temperature adjusting unit includes a cooling unit that cools the sample to a temperature equal to or lower than room temperature.   4. The apparatus according to claim 1, wherein the mounting table, the beam generation unit, and the detection unit further include a trap unit that is disposed in a chamber capable of controlling an atmosphere and traps a gas remaining in the chamber. The section processing apparatus as described.   The cross-section processing apparatus according to claim 1, wherein the beam is an ion beam. A first step of adjusting the temperature of the sample;
A second step of irradiating the sample with a beam to cut out a cross section;
A third step of sealing the temperature controlled sample;
A fourth step of transporting the sealed sample to another device;
A fifth step of evaluating the conveyed sample using the other device;
A cross-sectional evaluation method comprising:   The cross-sectional evaluation method according to claim 6, further comprising a step of introducing a gas around the sample to be sealed.   The cross-sectional evaluation method according to claim 7, wherein the introduced gas is an inert gas or a gas that does not damage the sample of dry nitrogen.

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