JP2012013619A - Minute part analyzer using focused ion beam and minute part analysis method using focused ion beam - Google Patents

Abstract

PROBLEM TO BE SOLVED: To simply, quickly, and precisely measure a temperature of an analyzed part on a sample surface in analyzing behaviors of elements in the analyzed part on the sample surface.SOLUTION: In the minute part analyzer using the focused ion beam, Ga whose ion kind is Ga is poured on a surface of a sample 4 by pre-radiating Ga focused ion beam 3 to make it a reference element for measuring a surface temperature of the sample 4, and the temperature of the minute part on the surface of the sample 4 during analysis is determined. Yield of a secondary Ga ion emitted from the sample 4 is measured by pre-radiating the fixed amount of Ga focused ion beam 3 to the sample 4 at every appropriate surface temperature of the sample 4 in advance to obtain a relation of the yield of the secondary Ga ion with the surface temperature of the sample 4. Once this relation is examined, the temperature at the minute part on the surface of the sample 4 can be determined by measuring the yield of the secondary Ga ion when analyzing the plurality of samples 4.

Description

  The present invention relates to a micro site analysis apparatus using a focused ion beam and a micro site analysis method using a focused ion beam, and is particularly suitable for analyzing a micro site of a sample while changing the surface temperature of the sample. is there.

  It is important to measure the elemental composition and amount at the minute part of the material in order to evaluate the characteristics of the material, especially in the material manufacturing process, it is important to know the behavior of the element in various temperature ranges. . In order to analyze the fine part of the material, for example, secondary ion mass spectrometry (FIB-SIMS) using a focused ion beam, transmission electron microscope, electron beam microanalyzer, Auger electron spectroscopy (AES), photoelectron Spectroscopy or the like can be used. In order to know the behavior of an element in a material at a high temperature using such an analysis technique, conventionally, for example, an analysis sample is heated to a desired temperature and then rapidly cooled. Alternatively, the sample was heated while referring to the temperature of the sample stage in the vacuum vessel, and after sufficient temperature equilibration was obtained, the elemental composition of the sample was examined by performing AES analysis in situ ( (See Patent Document 1).

  However, in the preparation of a sample by rapid cooling, the state at a desired temperature may not necessarily be reflected depending on the change rate of the crystal structure of the fine part and the diffusion coefficient of the additive element in the base material. Further, only by measuring the temperature of the sample stage, it takes a long time until the surface of the sample reaches temperature equilibrium, and it is difficult to accurately measure the surface temperature of the sample until it reaches temperature equilibrium.

JP-A-6-308112

  The present invention has been made in view of the above circumstances, and allows the temperature of an analysis site on a sample surface to be easily and quickly measured with high accuracy when analyzing the behavior of an element at the analysis site on the sample surface. For the purpose.

  In order to achieve the above-described object, a micro site analysis apparatus using a focused ion beam according to the present invention includes a sample stage on which a sample is placed, and a focused ion that irradiates the sample placed on the sample stage with the focused ion beam. A beam irradiation device, an analysis device for mass spectrometry of secondary ions emitted from the surface of the sample by irradiating the sample with the focused ion beam from the focused ion beam irradiation device, and a plane formed by the surface of the sample A secondary electron detector arranged so that a detection surface is horizontal with respect to the sample table, the sample stage, the focused ion beam irradiation device, the analysis device, and a vacuum vessel in which the secondary electron detector is installed A sample heater for heating the sample, storage means for storing in advance temperature conversion information indicating the relationship between the surface temperature of the sample and the yield of the secondary ions, and the mass spectrometry Therefore, based on the measurement value of the yield of secondary ions emitted from the surface of the sample by irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus and the temperature conversion information, Determining means for determining the temperature of the analysis site on the surface, and the analyzer is adapted to release secondary ions released from the surface of the sample when the sample is heated to a room temperature or higher by the sample heater. Is characterized by mass spectrometry.

In another embodiment of the microscopic region analysis apparatus using the focused ion beam of the present invention, the temperature conversion information is obtained from the surface of the sample by pre-irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus. This is information obtained based on the yield of the released secondary ions and the temperature of the sample at that time, and the focused ion beam irradiation apparatus applies the focused ion beam to the sample under the same conditions as the pre-irradiation. The determination means determines the analysis site of the surface of the sample based on the measurement value of the yield of secondary ions released from the surface of the sample by the total irradiation and the temperature conversion information. It is characterized by determining the temperature.
In another embodiment of the microscopic region analysis apparatus using the focused ion beam of the present invention, the pre-irradiation is performed by continuously irradiating the focused ion beam under the condition that the irradiation fluence is 5.0 × 10 ¹⁵ ions / cm ² or less. It is characterized by being performed.

In another embodiment of the microscopic site analysis apparatus using the focused ion beam of the present invention, the yield of secondary ions emitted from the surface of the sample by irradiation with the focused ion beam is It has a proportional relationship with the temperature of the analysis site.
In another embodiment of the microscopic region analysis apparatus using the focused ion beam of the present invention, the ion species of the focused ion beam is Ga ion, and the focused ion beam has a beam diameter of 50 nm or less on the surface of the sample. It is characterized by being focused so that
In another embodiment of the microscopic region analysis apparatus using a focused ion beam according to the present invention, the inside of the vacuum vessel is maintained at a vacuum degree of 10 ⁻⁶ Pa or less.
In another embodiment of the fine region analyzing apparatus using the focused ion beam of the present invention, the maximum temperature of the sample heated by the sample heater is 1000 ° C.

According to another aspect of the fine region analyzing apparatus using a focused ion beam of the present invention, the sample heater includes a resistance heater.
According to another aspect of the fine region analyzing apparatus using a focused ion beam of the present invention, the resistance heater is installed on the sample stage.
In another embodiment of the microscopic region analysis apparatus using a focused ion beam according to the present invention, the jig for fixing the sample on the sample stage is made of boron nitride.

  The fine region analysis method using a focused ion beam according to the present invention includes a focused ion beam irradiation step of irradiating a sample placed on a sample stage with a focused ion beam irradiation device by a focused ion beam irradiation device, and the focused ion beam irradiation. An analysis process in which a secondary ion emitted from the surface of the sample is irradiated by a focused ion beam to the sample from the apparatus is analyzed by the analyzer, and a detection surface is horizontal with respect to a plane formed by the surface of the sample A secondary electron detection step of detecting secondary electrons emitted when the focused ion beam irradiated by the focused ion beam irradiation device bombards the surface of the sample by a secondary electron detector arranged to be The sample stage, the focused ion beam irradiation device, the analysis device, and the secondary electron detector are installed inside a vacuum vessel, and the true A vacuum process for maintaining the inside of the container at a predetermined degree of vacuum, a sample heating process for heating the sample with a sample heater, a yield of the secondary ions, a surface temperature of the sample, and a yield of the secondary ions A storage step for preliminarily storing temperature conversion information indicating the relationship between the secondary ions emitted from the surface of the sample by irradiating the sample with the focused ion beam from the focused ion beam irradiation device for the mass analysis. And determining the temperature of the analysis site on the surface of the sample based on the measured value of the yield of the sample and the temperature conversion information. The secondary ion released from the surface of the sample is subjected to mass spectrometry while being heated.

In another embodiment of the fine region analysis method using a focused ion beam of the present invention, the temperature conversion information is obtained from the surface of the sample by pre-irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus. This is information obtained based on the yield of the released secondary ions and the temperature of the sample at that time. In the focused ion beam irradiation step, the focused ion beam is sampled under the same conditions as in the pre-irradiation. The determination step is performed based on the measurement value of the yield of secondary ions released from the surface of the sample by the total irradiation and the temperature conversion information on the analysis site on the surface of the sample. It is characterized by determining the temperature.
In another embodiment of the fine region analysis method using a focused ion beam according to the present invention, the pre-irradiation is performed by continuously irradiating a focused ion beam under the condition that the irradiation fluence is 5.0 × 10 ¹⁵ ions / cm ² or less. It is characterized by being performed.

In another embodiment of the fine region analysis method using a focused ion beam of the present invention, the yield of secondary ions released from the surface of the sample by irradiation with the focused ion beam is It has a proportional relationship with the temperature of the analysis site.
In another embodiment of the fine region analysis method using the focused ion beam of the present invention, the ion species of the focused ion beam is Ga ion, and the focused ion beam has a beam diameter of 50 nm or less on the surface of the sample. It is characterized by being focused so that
In another embodiment of the fine region analysis method using a focused ion beam according to the present invention, the vacuum step maintains the inside of the vacuum vessel at a degree of vacuum of 10 ⁻⁶ Pa or less.
In another embodiment of the fine region analysis method using a focused ion beam according to the present invention, the maximum temperature of the sample heated by the sample heater is 1000 ° C.

  According to the present invention, temperature conversion information indicating the relationship between the surface temperature of a sample and the yield of secondary ions is stored in advance, the yield of secondary ions is measured during mass analysis, and the measured secondary ions are measured. Based on the yield and temperature conversion information, the temperature of the analysis site on the surface of the sample was determined. Therefore, once the temperature conversion information is created, the surface temperature of the sample at the time of mass spectrometry can be measured inexpensively, simply, quickly, and accurately without an expensive and highly accurate temperature measuring device. Thereby, the uncertainty of the element behavior until reaching the rapid cooling or temperature equilibrium state is eliminated, and the more accurate behavior of the element with respect to the temperature of the base material can be known.

It is a figure which shows an example of the whole structure of a micro site | part analyzer. It is a figure which shows an example of the relationship between the surface temperature of the sample (Binary alloy polycrystal sample which added Al to 6.1 atomic% to Fe), and the yield of secondary Ga ion. It is a figure which shows an example of the relationship between the calculated surface temperature of a sample, and the sample 4 surface temperature by a thermocouple. It is a figure which shows an example of the relationship between the surface temperature of a sample (fine-grained steel sample), secondary Fe ion, and secondary Al ion.

  DESCRIPTION OF EMBODIMENTS Hereinafter, embodiments for carrying out the present invention will be described together with illustrated examples. In the present specification and drawings, elements having substantially the same functional configuration are denoted by the same reference numerals, and redundant description is omitted.

FIG. 1 is a diagram conceptually illustrating an outline of an example of the entire configuration of the microscopic region analysis apparatus of the present embodiment. As shown in FIG. 1, the fine region analyzer mainly includes a focused ion beam irradiation device 2, a sample stage 5, an XYZ stage 6, a sample heater 7, an analyzer 8, and a secondary electron detector 9. And a vacuum vessel (not shown) that covers these components. Since the sample 4 is placed on the sample table 5, the sample table 5 is preferably kept horizontal. The inside of the vacuum vessel is preferably kept at a vacuum degree of 10 ⁻⁶ Pa or less.

  The focused ion beam irradiated from the focused ion beam irradiation apparatus 2 is preferably a Ga ion beam whose ion species is Ga, and is preferably focused so that the beam diameter is 50 nm or less on the surface of the sample 4. That is, Ga is the ion source with the highest convergence at present, and is most suitable for the analysis of fine parts. Moreover, since Ga is a liquid metal and has a low solid solubility in Fe and a high diffusion rate, surface segregation at the sample temperature immediately reaches equilibrium. Therefore, it is optimal for the standard of sample temperature.

  The XYZ stage 6 is composed of a motor or the like that translates the sample stage 5 in the three axis directions of XYZ, and corrects the position of the sample 4. These total three axis adjustments are preferably computer controlled. Further, the XYZ stage 6 is actively cooled with cooling water or the like so that the XYZ stage 6 is kept at a low temperature even during heating.

  The analyzer 8 is a general mass spectrometer used for analyzing secondary ions 10 emitted when the focused ion beam 3 irradiated by the focused ion beam irradiation device 2 bombards the surface of the sample 4. is there. Specific examples of the analyzer 8 include various devices such as a quadrupole secondary ion mass spectrometer and a time-of-flight secondary ion mass spectrometer.

  The secondary electron detector 9 detects the secondary electrons 11 emitted when the focused ion beam 3 irradiated by the focused ion beam irradiation device 2 bombards the surface of the sample 4 and detects the sample 4 as a secondary electron image. This is a general secondary electron detector used for observing the surface. Specific examples of the secondary electron detector 9 include a detector in which a scintillator and a photomultiplier tube are combined. Here, the shortest distance from the sample 4 to the detection surface of the secondary electron detector 9 is 175 mm or more so that radiant light from the surface of the sample 4 that has become hot does not enter the field of view of the secondary electron detector 9 as much as possible. In addition, the detection surface of the secondary electron detector 9 is made to be horizontal with respect to the plane formed by the surface of the sample 4.

  As the sample heater 7, a generally available one can be used, for example, a resistance heater coated with boron nitride. Using this sample heater 7, the sample 4 is heated to a desired temperature in the range of room temperature to 1000 ° C. And in the micro site | part analyzer of this embodiment, the sample heater 7 is plate-shaped, and installs the sample 4 on it. The temperature of the sample heater 7 is measured by a thermocouple 12 installed on the lower surface of the sample heater 7, and temperature control is performed.

In the measurement of the temperature of the analysis site (fine site) on the surface of the sample 4, focused ions injected onto the surface of the sample 4 by pre-irradiation with the focused ion beam 3 are used as reference ions for temperature measurement. First, a predetermined amount of the focused ion beam 3 is continuously irradiated for each appropriate “surface temperature of the sample 4” under a condition that the incident energy is 30 keV and the irradiation fluence is 5.0 × 10 ¹⁵ ions / cm ² or less. Pre-irradiation is performed, and immediately after that, the yield of the secondary ions 10 is measured by the analyzer 8 to obtain the relationship (conversion function) of the yield of the secondary ions with respect to the surface temperature of the sample 4. This conversion function is stored, for example, in a computer system included in the analysis device 8.

The reason why the irradiation fluence is 5.0 × 10 ¹⁵ pieces / cm ² or less is as follows. Although measured in high vacuum, the heated iron surface is oxidized by the influence of adsorbed water, residual oxygen, and the like. Therefore, 5 × 10 ¹⁵ atoms / cm ² or less of Ga is irradiated to remove the oxide film on the surface and to sufficiently inject Ga into the sample 4. The irradiation fluence of the focused ion beam 3 is appropriately selected within a range satisfying such conditions.
On the other hand, when the focused ion beam 3 having an irradiation fluence exceeding 5.0 × 10 ¹⁵ ions / cm ² is irradiated, the effect of increasing the roughness of the sample surface by Ga appears, so that it becomes difficult to obtain reproducibility of mass spectrometry. . At the time of mass analysis, the focused ion beam 3 is completely irradiated under the same conditions as when the conversion function is obtained, and immediately after that, simultaneously with mass analysis, the yield of the secondary ion 10 as a reference element is also measured. Determine the temperature. The surface temperature of the sample 4 can be determined by the analyzer 8, for example.

Example 1
In this example, a binary alloy polycrystal sample obtained by adding 6.1 atomic% of Al to Fe is used as sample 4, and the yield of secondary Ga ions as secondary ions 10 is converted to the surface temperature of sample 4. A conversion function was created. And the validity was shown.

  First, the sample 4 is placed on the sample table 5 on which a resistance heater is installed as the sample heater 7, and the sample 4 is fixed to the sample table 5 with a sample fixing jig made of boron nitride. In the state of room temperature, the analysis conditions such as the height of the sample 4 and the voltage applied to each part of the analyzer 8 were optimized. The focused ion beam 3 used for optimizing the analysis conditions is a pulsed Ga ion beam having an incident energy of 30 keV and a current value of 1 nA (pulse mode). The pulse frequency was set to 10 kHz and the pulse width was set to 200 ns. The analyzer 8 that performs mass analysis of the secondary ions 10 emitted by irradiation of the focused ion beam 3 is a reflectron type time-of-flight mass spectrometer having a total length of 1.3 m. In this example, when the voltage drawn into the analyzer 8 is −3 kV, the flight time of Ga is approximately 36 μs.

Next, similarly to the conventional method, the temperature of the surface of the sample 4 is changed to 590 with reference to the relationship between the surface temperature of the sample 4 and the lower surface temperature of the resistance heater, which are obtained by measuring with the thermocouple 12 in advance. Set to ° C. and hold for about 2 hours until sufficient temperature equilibrium is reached. When the temperature equilibrium was reached, pre-irradiation was performed using the focused ion beam 3 under the conditions described above. The field of view of the focused ion beam 3 was set to 100 μm square, and pre-irradiation was performed for 1 minute (min) until the irradiation fluence reached 3.6 × 10 ¹⁵ pieces / cm ² by continuous irradiation. Thereafter, irradiation was performed in a pulse mode, and the yield of secondary Ga ions was measured. The same operation was performed for the cases where the surface temperature of the sample 4 was 660 ° C. and 735 ° C., and the relationship between the surface temperature of the sample 4 and the yield of secondary Ga ions was plotted on the coordinates. FIG. 2 is a diagram showing the results. In FIG. 2, a straight line was drawn by the least square method based on the plotted points 21 to 23 to obtain the correspondence relationship (conversion function 24) of the yield of secondary Ga ions to each sample surface temperature. From this result, the relationship (conversion function 24) between the surface temperature T of the sample 4 and the yield X of secondary Ga ions at 590 ° C. or more can be expressed by a linear function as shown in the following equation (1).
T = aX + b (1)
In the example shown in FIG. 2, the slope a of the straight line can be determined to be −6.17 × 10 ⁻² ° C./count, and the intercept b (the surface temperature of the sample 4 where the yield X of secondary Ga ions is 0) can be determined to be 800 ° C. It was. The “count” represents the number of secondary ions generated per primary ion.

  Thereafter, in order to show that the obtained conversion function 24 does not depend on the surface condition (difference in crystal orientation distribution or crystal grain size) in the analytical field of view, a new unheated Fe—Al binary alloy polycrystalline sample (Al in Fe The amount of secondary Ga ions after pre-irradiation with a Ga ion beam at each temperature of 590 ° C. or higher is measured while the sample 4 is replaced by a conventional method using a thermocouple 12. Was measured. Using the conversion function 24 obtained in FIG. 2, the surface temperature of the sample 4 is calculated from the yield of secondary Ga ions, and the relationship between the calculated surface temperature of the sample 4 and the surface temperature of the sample 4 by the thermocouple 12 is coordinated. Plot to FIG. 3 is a diagram showing the results. In FIG. 3, these plotted points 31 to 38 are located in the vicinity of the line 39 of Y = X, where X is the horizontal axis and Y is the vertical axis, and the temperature calculated from the yield of secondary Ga ions is Sample 4 It was confirmed that the temperature was consistent with the temperature obtained by actual measurement with the thermocouple 12 within ± 3 ° C., regardless of the surface state of the film. That is, Ga implanted into the surface of the sample 4 by the pre-irradiation has a small surface binding energy because it is not captured between the lattices of the base material, and does not depend on the surface state of the sample 4. Therefore, since the yield of secondary Ga ions depends on the difference in “Ga diffusion rate from the analysis site” determined only by temperature, the surface temperature of the sample 4 can be measured.

(Example 2)
In this example, FIB-SIMS measurement was performed at a high temperature using a fine-grain steel sample as Sample 4, and the temperature dependency of the yield of secondary ions of Fe and Al was examined.
First, using a fine-grain steel sample for calibration, the slope a obtained by the same procedure as in Example 1 was −8.06 × 10 ⁻² ° C./count, and the intercept b was 710 ° C.

  Next, FIB-SIMS measurement was performed at a high temperature using a fine-grain steel sample for analysis. As shown in FIG. 4, when the surface temperature of the sample 4 is increased, the state of changes in the surface concentration of Fe and Al accompanying the steel transformation is observed between 700 ° C. and 750 ° C. before and after the steel transformation temperature. did it. That is, in the process of increasing the temperature of D4, the state of the surface of the steel changes due to the change of the steel from the bcc structure to the fcc structure in the phase transformation temperature range 41 (region shown in gray). The yield of secondary Fe ions increases (see graph 42). Thereafter, when the temperature of the sample 4 was lowered, the yield of secondary Fe ions decreased and returned to the value obtained in the case of the bcc structure (see graph 42). On the other hand, Al in the steel gradually increases due to diffusion to the surface in the process of raising the temperature of the sample 4, but suddenly decreases due to the decrease of the solid solution limit concentration of Al due to the structural change of the steel after the phase transformation. And then increased when the temperature of sample 4 was lowered (see graph 43). Here, the surface temperature of the sample 4 on the horizontal axis is the temperature determined by the method of this embodiment, and the time required from the temperature rise to the end of measurement at each temperature is 15 minutes (min).

  As described above, in the present embodiment, since the secondary Ga ions released from the analysis site are used for measuring the surface temperature of the sample 4, the surface temperature of the sample 4 at the time of analysis can be measured quickly and easily with high accuracy. Is possible. That is, since the reference element Ga (yield of secondary Ga ions) for measuring the surface temperature of the sample 4 is measured when analyzing the behavior of the elements on the surface of the sample 4, the yield of secondary Ga ions Once the correlation between the surface temperature of the sample 4 and the surface temperature of the sample 4 is examined, the surface temperature of the sample 4 at that time can be measured inexpensively, simply, quickly, and accurately, without an expensive and highly accurate temperature measuring device. Thereby, the uncertainty of the behavior of the element until the rapid cooling or the temperature equilibrium state is reached is eliminated, and the more accurate element behavior with respect to the temperature of the base material can be known.

  It should be noted that the embodiments of the present invention described above are merely examples of implementation in carrying out the present invention, and the technical scope of the present invention should not be construed as being limited thereto. Is. That is, the present invention can be implemented in various forms without departing from the technical idea or the main features thereof.

2 Focused ion beam irradiation device
3 Focused ion beam
4 samples
5 Sample stage
6 XYZ stage
7 Sample heater
8 Analyzer
9 Secondary electron detector
10 Secondary ion 11 Secondary electron 12 Thermocouple

Claims (17)

A sample stage on which the sample is placed;
A focused ion beam irradiation apparatus for irradiating the sample placed on the sample stage with a focused ion beam;
An analyzer for mass-analyzing secondary ions emitted from the surface of the sample when the sample is irradiated with the focused ion beam from the focused ion beam irradiation device;
A secondary electron detector arranged such that a detection surface is horizontal with respect to a plane formed by the surface of the sample;
A vacuum vessel in which the sample stage, the focused ion beam irradiation device, the analysis device, and the secondary electron detector are installed;
A sample heater for heating the sample;
Storage means for preliminarily storing temperature conversion information indicating the relationship between the surface temperature of the sample and the yield of the secondary ions;
Based on the measurement value of the yield of secondary ions emitted from the surface of the sample by irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus for the mass analysis and the temperature conversion information. Determining means for determining the temperature of the analysis site on the surface of the sample;
Comprising
The analysis device performs mass analysis of secondary ions emitted from the surface of the sample when the sample is heated to a room temperature or higher by the sample heater, and performs a fine site analysis using a focused ion beam apparatus. The temperature conversion information is based on the yield of secondary ions emitted from the surface of the sample by pre-irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus, and the temperature of the sample at that time. Information obtained,
The focused ion beam irradiation apparatus irradiates the sample with a focused ion beam under the same conditions as when the previous irradiation was performed,
The determining means determines the temperature of the analysis site on the surface of the sample based on the measurement value of the yield of secondary ions released from the surface of the sample by the total irradiation and the temperature conversion information. A fine region analyzing apparatus using the focused ion beam according to claim 1. The fineness using a focused ion beam according to claim 2, wherein the pre-irradiation is performed by continuously irradiating a focused ion beam under a condition that an irradiation fluence is 5.0 × 10 ¹⁵ ions / cm ² or less. Site analysis device.   4. The yield of secondary ions emitted from the surface of the sample by irradiation with the focused ion beam has a proportional relationship with the temperature of the analysis site on the surface of the sample. A fine region analysis apparatus using the focused ion beam according to claim 1.   The ion species of the focused ion beam is Ga ion, and the focused ion beam is focused so that the beam diameter is 50 nm or less on the surface of the sample. The micro site | part analyzer using the focused ion beam of description. The micro site analysis apparatus using a focused ion beam according to any one of claims 1 to 5, wherein the inside of the vacuum vessel is maintained at a degree of vacuum of 10 ^-6 Pa or less.   The fine region analysis apparatus using a focused ion beam according to any one of claims 1 to 6, wherein the maximum temperature of the sample heated by the sample heater is 1000 ° C.   The microscopic site analysis apparatus using a focused ion beam according to any one of claims 1 to 7, wherein the sample heater includes a resistance heater.   The fine region analysis apparatus using a focused ion beam according to claim 8, wherein the resistance heater is installed on the sample stage.   The fine site analysis apparatus using a focused ion beam according to any one of claims 1 to 9, wherein the jig for fixing the sample on the sample stage is made of boron nitride. A focused ion beam irradiation step of irradiating the sample placed on the sample stage with a focused ion beam irradiation device with a focused ion beam irradiation device;
An analysis step of performing mass analysis on the secondary ion emitted from the surface of the sample by irradiating the sample with the focused ion beam irradiation device from the focused ion beam irradiation device;
When the focused ion beam irradiated by the focused ion beam irradiation device bombards the surface of the sample by a secondary electron detector arranged so that the detection surface is horizontal with respect to a plane formed by the surface of the sample A secondary electron detection step of detecting the emitted secondary electrons;
A vacuum process in which the sample stage, the focused ion beam irradiation device, the analysis device, and the secondary electron detector are installed inside a vacuum vessel, and the inside of the vacuum vessel is maintained at a predetermined degree of vacuum;
A sample heating step of heating the sample with a sample heater;
A storage step for preliminarily storing temperature conversion information indicating the relationship between the surface temperature of the sample and the yield of the secondary ions;
Based on the measurement value of the yield of secondary ions emitted from the surface of the sample by irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus for the mass analysis and the temperature conversion information. A determination step for determining the temperature of the analysis site on the surface of the sample;
Comprising
The analysis step includes mass analysis of secondary ions emitted from the surface of the sample when the sample is heated to a room temperature or higher by the sample heater, and a fine region analysis using a focused ion beam Method. The temperature conversion information is based on the yield of secondary ions emitted from the surface of the sample by pre-irradiating the sample with the focused ion beam from the focused ion beam irradiation apparatus, and the temperature of the sample at that time. Information obtained,
The focused ion beam irradiation step irradiates the sample with the focused ion beam under the same conditions as the pre-irradiation,
The determining step determines the temperature of the analysis site on the surface of the sample based on the measurement value of the yield of secondary ions released from the surface of the sample by the total irradiation and the temperature conversion information. The fine site | part analysis method using the focused ion beam of Claim 11. 13. The fine irradiation using a focused ion beam according to claim 12, wherein the pre-irradiation is performed by continuously irradiating a focused ion beam under a condition that an irradiation fluence is 5.0 × 10 ¹⁵ ions / cm ² or less. Site analysis method.   14. The yield of secondary ions released from the surface of the sample by irradiation with the focused ion beam has a proportional relationship with the temperature of the analysis site on the surface of the sample. A method for analyzing a fine region using the focused ion beam according to claim 1.   The ion species of the focused ion beam is Ga ions, and the focused ion beam is focused so that the beam diameter is 50 nm or less on the surface of the sample. 4. A method for analyzing a fine region using the focused ion beam according to the item. 16. The method for analyzing a microscopic part using a focused ion beam according to claim 11, wherein the vacuum step maintains the inside of the vacuum vessel at a vacuum degree of 10 ⁻⁶ Pa or less. .   The fine region analysis method using a focused ion beam according to any one of claims 11 to 16, wherein the maximum temperature of the sample heated by the sample heater is 1000 ° C.

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