JP6963076B2 - Analytical equipment and analytical method - Google Patents

Description

The present invention relates to an analyzer and an analytical method.

In an analyzer such as a scanning electron microscope (SEM) equipped with an energy dispersive X-ray spectroscope (EDS) or a scanning transmission electron microscope (STEM), a sample is scanned with an electron probe and X-rays are emitted from each point. A technique is known for obtaining an element distribution image by imaging the difference in the amount of emission. At this time, as a scanning method, a method of integrating signal data by repeatedly scanning at a high scanning speed and a method of acquiring data by slowing down the scanning speed in one scan are known. Has been done.

For example, Patent Document 1 discloses a technique of integrating a plurality of images obtained by repeatedly scanning a sample while correcting a positional deviation due to drift between the images to generate one image.

Japanese Unexamined Patent Publication No. 2007-299768

Here, some of the samples to be analyzed change their element distribution and shape when irradiated with an electron beam. In addition, some of the samples to be analyzed change their element distribution and shape when the sample environment (temperature, etc.) changes.

When an element distribution image is obtained from such a sample using the above analyzer, in the technique of Patent Document 1 described above, even if the element distribution changes during the measurement, the signal of the frame before the element distribution changes. It is possible to extract the data and draw the element distribution image, but it is not possible to extract the signal data of the frame after the element distribution has changed and draw the element distribution image.

The present invention has been made in view of the above problems, and one of the objects according to some aspects of the present invention is to measure a sample whose state changes during measurement. It is an object of the present invention to provide an analyzer and an analysis method capable of extracting data before and after a state change.

The analyzer according to the present invention is
An analyzer that repeatedly scans a sample with a charged particle beam, detects a signal from the sample, and analyzes the sample.
An environmental control device that controls the environment of the sample,
A data storage processing unit that stores the signal data obtained by detecting the signal together with position information data indicating the irradiation position of the charged particle beam on the sample, and a data storage processing unit.
A control unit that detects a change in the signal between frames based on the signal data stored in the storage unit and controls the environment control device based on the change in the signal between frames.
including.

In such an analyzer, the control unit controls the environmental control device based on the change in the signal between frames. Therefore, in the measurement of the sample in which the state of the sample changes during the measurement, the signal of the sample has a predetermined environmental condition. When the change is made in, the predetermined environmental conditions can be maintained. Therefore, the signal from the sample can be detected by repeatedly scanning the sample with a charged particle beam under the environmental conditions in which the signal of the sample changes. This makes it possible to obtain signal data after the state of the sample has changed.

The analyzer according to the present invention is
An analyzer that repeatedly scans a sample with a charged particle beam, detects a signal from the sample, and analyzes the sample.
A data storage processing unit that stores the signal data obtained by detecting the signal together with position information data indicating the irradiation position of the charged particle beam on the sample, and a data storage processing unit.
A signal change detection unit that detects a change in the signal between frames based on the signal data stored in the storage unit, and a signal change detection unit.
An image generation unit that generates an image based on the signal data stored in the storage unit and the detection result of a change in the signal between frames.
Including
The image generation unit generates the image by associating the intensity of the signal with the brightness of the image and the detection result of the change in the signal between frames with the saturation of the image.

In such an analyzer, since the image generator generates an image in which the detection result of the signal change between frames corresponds to the saturation, it is easy to determine whether or not the state of the sample has changed during the measurement. be able to.

The analysis method according to the present invention is
An analytical method in which a sample is repeatedly scanned with a charged particle beam to detect a signal from the sample, and the sample is analyzed.
The process of controlling the environment of the sample and
A step of storing the signal data obtained by detecting the signal in the storage unit together with the position information data indicating the irradiation position of the charged particle beam on the sample.
A step of detecting a change in the signal between frames based on the signal data stored in the storage unit and controlling the environment control device based on the change in the signal between frames.
including.

In such an analysis method, since the environmental control device is controlled based on the change in the signal between frames, the signal of the sample changes under a predetermined environmental condition in the measurement of the sample in which the state of the sample changes during the measurement. In some cases, the predetermined environmental conditions can be maintained. Therefore, the signal from the sample can be detected by repeatedly scanning the sample with a charged particle beam under the environmental conditions in which the signal of the sample changes. This makes it possible to obtain signal data after the state of the sample has changed.

The analysis method according to the present invention is
An analytical method in which a sample is repeatedly scanned with a charged particle beam to detect a signal from the sample, and the sample is analyzed.
A step of storing the signal data obtained by detecting the signal in the storage unit together with the position information data indicating the irradiation position of the charged particle beam on the sample.
A step of detecting a change in the signal between frames based on the signal data stored in the storage unit, and
A step of generating an image based on the signal data stored in the storage unit and the detection result of a change in the signal between frames.
Including
In the step of generating the image, the intensity of the signal is made to correspond to the brightness of the image, and the detection result of the change of the signal between frames is made to correspond to the saturation of the image to generate the image.

In such an analysis method, since the detection result of the signal change between frames is generated as an image corresponding to the saturation, it can be easily determined whether or not the state of the sample has changed during the measurement.

The figure which shows typically the analyzer which concerns on 1st Embodiment. The figure which shows typically the structure of the data stored in the storage part. The figure for demonstrating the position information data. The figure which shows an example of the X-ray spectrum generated by extracting the X-ray signal data. The flowchart which shows an example of the analysis method by the analyzer which concerns on 1st Embodiment. The figure which shows typically the main window displayed on the display part. A graph showing changes in the ROI count in a designated area. The graph which shows the change of the count of ROI_2. The graph which shows the difference value g _{n of each frame.} The graph which shows the change of the count of ROI_2. The figure which shows typically the comparison window displayed on the display part. The figure for demonstrating the processing when the element is added. The figure for demonstrating the processing when the element is added. The figure for demonstrating the process of changing the range of the frame which constitutes each frame group. The figure for demonstrating the process of changing the range of the frame which constitutes each frame group. The graph which shows the change of the count of ROI_1 and the count of ROI_2. The graph which shows the difference value g _{n of each frame.} A graph showing changes in the ROI count in a designated area. A graph showing the similarity of each frame. The figure which shows typically the comparison window displayed on the display part. The figure which shows typically the analyzer which concerns on 2nd Embodiment. The figure which shows typically the structure of the data stored in the storage part. The graph which shows the change of the temperature of a sample. The graph which shows the difference value Δt _{n of each frame.} The figure which shows typically the comparison window displayed on the display part. A graph showing changes in the specified ROI count and changes in sample temperature. The figure which shows typically the analyzer which concerns on 4th Embodiment. The figure which shows typically the main window displayed on the display part. The figure for demonstrating the process of desaturating according to the intensity of an X-ray signal. The figure which shows typically the analyzer which concerns on 5th Embodiment. The figure which shows an example of the GUI screen of the analyzer which concerns on 5th Embodiment.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings. The embodiments described below do not unreasonably limit the content of the present invention described in the claims. Moreover, not all of the configurations described below are essential constituent requirements of the present invention.

1. 1. First Embodiment 1.1. Analytical device First, the analytical device according to the first embodiment will be described with reference to the drawings. FIG. 1 is a diagram schematically showing an analyzer 100 according to the first embodiment. Here, an example will be described in which the analyzer 100 is a scanning electron microscope (SEM) including an energy dispersive X-ray detector (EDS detector) 40.

As shown in FIG. 1, the analyzer 100 includes an optical system 10, an optical system control unit 19, a sample stage 20, a sample stage control unit 22, a secondary electron detector 30, and an electronic signal processing unit 32. , EDS detector 40, X-ray signal processing unit 42, processing unit 50, operation unit 60, display unit 62, and storage unit 64.

In the analyzer 100, when the surface of the sample 1 is scanned with an electron probe (an example of a charged particle beam) formed by the optical system 10, a secondary electron signal (a signal from the sample) emitted from the irradiation point of the electron probe is used. An example) can be detected by the secondary electron detector 30 and imaged. Further, in the analyzer 100, the EDS detector 40 detects an X-ray (characteristic X-ray) signal (an example of a signal from the sample) generated when the sample 1 is irradiated with an electron probe, and the EDS spectrum and elements are detected. A distribution image can be obtained.

The optical system 10 includes an electron radiation source 12, a focusing lens 14, an objective lens 16, and a deflector 18. The electron radiation source 12 generates an electron beam EB. The electron source 12 is, for example, a known electron gun. The focusing lens 14 focuses the electron beam EB emitted from the electron beam source 12. The objective lens 16 is a final stage electron probe forming lens arranged immediately before the sample 1. The deflector 18 deflects the electron beam EB (electron probe) focused by the focusing lens 14 and the objective lens 16. The deflector 18 deflects the electron beam EB (electron probe) focused by the focusing lens 14 and the objective lens 16, so that the electron beam EB can be scanned on the sample 1. The position where the electron beam EB irradiates the sample 1 is determined by the applied voltage of the deflector 18. The optical system control unit 19 controls the acceleration voltage applied to the electron beam source 12, the exciting current of the focusing lens 14 and the objective lens 16, the applied voltage of the deflector 18, and the like.

The sample stage 20 can support the sample 1 and move the sample 1. The sample stage control unit 22 controls the operation of the sample stage 20.

The secondary electron detector 30 detects the secondary electrons emitted from the sample 1 by being irradiated with the electron beam EB. The secondary electron detector 30 includes, for example, a scintillator and a photomultiplier tube. The electronic signal processing unit 32 performs a process of sending the intensity of the secondary electrons detected by the secondary electron detector 30 to the processing unit 50 as a digital signal. The electronic signal data (an example of signal data) output from the electronic signal processing unit 32 is sent to the processing unit 50 in association with the position information data of the electron beam EB determined by the applied voltage of the deflector 18.

The EDS detector 40 detects the characteristic X-rays generated from the sample 1 by being irradiated with the electron beam EB. The EDS detector 40 includes, for example, a silicon drift detector (SDD). The X-ray signal processing unit 42 includes a multi-channel analyzer, analyzes the energy value by the multi-channel analyzer based on the pulse peak value of the X-ray signal detected by the EDS detector 40, and corresponds to the channel. Performs the process of allocating. The X-ray signal data (an example of signal data) output from the X-ray signal processing unit 42 is sent to the processing unit 50 in association with the position information data of the electron beam EB determined by the applied voltage of the deflector 18.

The operation unit 60 acquires an operation signal according to the operation by the user and sends the operation signal to the processing unit 50. The function of the operation unit 60 can be realized by, for example, buttons, keys, a touch panel display, a microphone, and the like.

The display unit 62 displays an image generated by the processing unit 50, and its function can be realized by an LCD, a CRT, or the like. For example, a secondary electron image (SEM image), an element distribution image, or the like is displayed on the display unit 62.

The storage unit 64 stores programs, data, and the like for the processing unit 50 to perform various calculation processes and control processes. The storage unit 64 is also used as a work area of the processing unit 50, and is also used to temporarily store the calculation results and the like executed by the processing unit 50 according to various programs. The function of the storage unit 64 can be realized by a hard disk, RAM, or the like. As will be described later, the storage unit 64 stores electronic signal data, X-ray signal data, position information data of the electron beam EB, and elapsed time information data.

The processing unit 50 is for generating an element distribution image, generating a secondary electron image, generating a control signal for controlling the optical system control unit 19, and controlling the sample stage control unit 22. Performs processing such as generating a control signal. The function of the processing unit 50 can be realized by hardware such as various processors (CPU, DSP, etc.) or a program. The processing unit 50 includes a data storage processing unit 52, a frame group extraction unit 54, an image generation unit 56, and a control unit 58.

The data storage processing unit 52 performs a process of storing (recording) the electronic signal data and the X-ray signal data in the storage unit 64 together with the position information data of the electron beam EB and the elapsed time information data of the measurement.

Here, the structure of the data stored in the storage unit 64 will be described.

In the analyzer 100, the applied voltage of the deflector 18 corresponding to the irradiation position of the electron beam EB is controlled by the optical system control unit 19, and the electron beam EB is irradiated to a predetermined coordinate position of the sample 1. Then, the X-ray signal generated by the irradiation of the electron beam EB is detected by the EDS detector 40 and converted into X-ray signal data by the X-ray signal processing unit 42. Further, the secondary electron signal generated by the irradiation of the electron beam EB is detected by the secondary electron detector 30 and converted into electronic signal data by the electron signal processing unit 32. The X-ray signal data and the electronic signal data are stored in the storage unit 64 as a data string (time-series data) combined in a time series together with the position information data and the elapsed time information data of the electron beam EB. The analyzer 100 repeatedly scans a predetermined region of the sample 1 with an electron beam EB to detect a characteristic X-ray signal and a secondary electron signal, and sequentially stores the above-mentioned various data in the storage unit 64.

FIG. 2 is a diagram schematically showing the structure of data stored in the storage unit 64. In FIG. 2, the position information data is represented by “P”, the X-ray signal data is represented by “D”, the electronic signal data is represented by “S”, and the elapsed time information data is represented by “T”. Further, in FIG. 2, data from the first frame to the mth frame (m is an integer of 3 or more) is shown.

As shown in FIG. 2, the data (data string) stored in the storage unit 64 measures the position information data P, the X-ray signal data D, the electronic signal data S, and the elapsed time information data T along the measured elapsed time axis. It is arranged time series data. The data storage processing unit 52 accumulates the position information data P, the X-ray signal data D, the electronic signal data S, and the elapsed time information data T to form a data string having the data structure shown in FIG.

The position information data P is data representing the irradiation position of the electron beam EB on the sample 1. The position information data P is, for example, a coordinate value representing an irradiation position on the sample 1, and includes data of coordinate values of the X-axis and the Y-axis representing the position in the horizontal direction. The position information data P may further include coordinate values such as a Z axis representing a position orthogonal to the X axis and the Y axis, a T axis representing the inclination of the sample 1, and an R axis representing the rotation of the sample 1. ..

FIG. 3 is a diagram for explaining the position information data P. Here, a case where the surface analysis is performed using the section set on the sample 1 as the unit of the position information data P will be described with reference to FIG.

As shown in FIG. 3, the start position of one scan (1 frame) of the electron beam EB is represented by the position information data “P1” (n = 1), and the end position of one scan is the position information data. It is represented by "Pe" (n = e (e is a positive integer)).

For example, one frame is obtained by extracting the X-ray signal data D sandwiched between the position information data P1 and the position information data P1 that appears next from the data string stored in the storage unit 64 shown in FIG. The X-ray signal data D of the minute can be extracted. Further, for example, in the data string stored in the storage unit 64, two position information data Ps are specified, and the X-ray signal data D sandwiched between the two position information data Ps is extracted to extract the two position information. The X-ray signal data D of the irradiation region represented by the data P can be obtained. For example, from the data string stored in the storage unit 64, the X-ray signal data D between the position information data Pn (n is an integer satisfying 1 ≦ n ≦ e) and the position information data Pn + m + 1 (m is a positive integer). By extracting the above, the X-ray signal data D in the range from the region indicated by the position information data Pn shown in FIG. 3 to the region indicated by the position information data Pn + m can be extracted. By designating the area (position information range) using the position information data P in this way, the X-ray signal data D of an arbitrary irradiation position and an arbitrary area is extracted from the data string stored in the storage unit 64. can do.

The X-ray signal data D is data representing an X-ray signal (characteristic X-ray signal) detected by the EDS detector 40. The X-ray signal data D is data representing an energy value (or a channel assigned by a multi-channel analyzer) obtained by analyzing an X-ray quantum incident on the EDS detector 40. It is desirable that the X-ray signal data D has a depth of about 13 bits.

The electronic signal data S is data obtained by detecting the secondary electronic signal with the secondary electron detector 30. The electronic signal data S includes information on the strength of the secondary electronic signal.

The electronic signal data S may be reflected electronic signal data. That is, although not shown, the analyzer 100 may include a reflected electron detector, and the electronic signal data S may be data obtained by detecting the reflected electron signal with the reflected electron detector. Further, the electronic signal data S may include both the data of the secondary electronic signal and the data of the backscattered electron signal.

The elapsed time information data T is data representing the elapsed time of measurement, and is the actual elapsed time (Real).
Data including at least one of Time) and Live Time. Here, the actual elapsed time is the time actually elapsed from the start of measurement, and the effective time is the measurement time excluding the dead time of EDS.

For example, from the data string stored in the storage unit 64, the elapsed time information data T having the data of the elapsed time a and the elapsed time information data T of the elapsed time a + b when the time b elapses from the elapsed time a. By extracting the X-ray signal data D included in the interval, the X-ray signal data D collected between the time a and the time a + b can be extracted.

As described above, the data storage processing unit 52 forms the data sequence shown in FIG. 2 by accumulating various data individually and storing them in order. Therefore, for example, the signal data of the sample absorption current and the cathode luminescence. Data other than the above, such as signal data, can also be added.

FIG. 4 is a diagram showing an example of an X-ray spectrum generated by extracting X-ray signal data D from the data stored in the storage unit 64. In the graph shown in FIG. 4, the horizontal axis represents the energy of X-rays, and corresponds to each channel divided into predetermined energy intervals of the multi-channel analyzer. The vertical axis is a value obtained by integrating the number of X-ray signal data D for each channel (that is, X-ray intensity).

ROI_1, ROI_2, and ROI_3 indicate an energy range (ROI, Region Of interest) for selecting only an X-ray signal having a desired energy. The energy range indicated by the ROI can be arbitrarily set by the user. The analyzer 100 has a function of automatically setting an ROI corresponding to an element when the user specifies an element. For example, ROI_1 corresponds to oxygen (O), ROI_2 corresponds to chromium (Cr), and ROI_3 corresponds to iron (Fe).

For example, by integrating all the X-ray signal data D of the data string shown in FIG. 2, it is possible to obtain information on the X-ray intensity in the entire energy range. Further, by integrating the number of X-ray signal data D (ROI count) included in the designated ROI, information on the X-ray intensity of the designated ROI can be obtained. For example, by integrating the number of X-ray signal data D included in the energy range indicated by ROI_1, information on the X-ray intensity of oxygen can be obtained. Similarly, by integrating the number of X-ray signal data D included in the energy range indicated by ROI_2, information on the X-ray intensity of chromium can be obtained, and the X-ray signal data D included in the energy range indicated by ROI_3 can be obtained. Information on the X-ray intensity of iron can be obtained by integrating the numbers of.

The frame group extraction unit 54 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and based on the change in the X-ray signal between frames, from a plurality of consecutive frames. The frame group is extracted.

The frame group extraction unit 54 extracts a frame group composed of a plurality of consecutive frames based on the intensity difference of the X-ray signals of two consecutive frames. For example, the frame group extraction unit 54 extracts a range in which frames having a threshold value or less in which the intensity difference of the X-ray signals of two consecutive frames is set are continuous as a frame group. As a result, it is possible to extract from the frames stored in the storage unit 64 a frame group composed of a plurality of consecutive frames in which the fluctuation of the intensity of the X-ray signal is small.

The intensity of the X-ray signal to be detected is, for example, the intensity of the X-ray signal in the specified energy range (ROI) in the specified region (irradiation region, position information range). The intensity of the X-ray signal to be detected may be the intensity of the X-ray signal of the specified ROI in the entire region (the entire irradiation region). When the intensities of the X-ray signals of two consecutive frames are _{expressed as f n} and f _n-1 , the intensity difference of the X-ray signals can be expressed _{by | f n} − f _{n-1 |.} Further, the threshold value can be set arbitrarily.

Here, an example in which the frame group extraction unit 54 detects the change in the intensity of the X-ray signal between frames and the difference in the intensity of the X-ray signals of two consecutive frames has been described. The method for determining the change in the intensity of is not limited to this. For example, a change in the intensity of the X-ray signal may be detected from the difference between the intensity of the X-ray signal of the first frame and the intensity of the X-ray signal of the nth frame.

The image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group extracted by the frame group extraction unit 54 from the X-ray signal data recorded in the storage unit 64, and extracts the element distribution. Generate an image. When a plurality of ROIs are specified, the image generation unit 56 selects the X-rays included in each of the designated ROIs from the X-ray signal data of the plurality of frames constituting the extracted frame group. The number of signal data is counted for each irradiation position, and an element distribution image corresponding to each ROI is generated.

When the frame group extraction unit 54 extracts a plurality of frame groups, the image generation unit 56 extracts the X-ray signal data for each frame group from the X-ray signal data recorded in the storage unit 64. An element distribution image is generated for each frame group.

The control unit 58 performs a process of generating a control signal for controlling the optical system control unit 19 and a control signal for controlling the sample stage control unit 22. For example, when the operation unit 60 receives an operation for changing the conditions of the user's optical system, the control unit 58 receives a control signal (control signal for controlling the optical system control unit 19) based on the operation signal from the operation unit 60. To generate. As a result, the optical system can be set to the conditions specified by the user. Further, for example, when the operation unit 60 receives an operation for moving the sample 1 to a desired position, the control unit 58 controls a control signal (control for controlling the sample stage control unit 22) based on the operation signal from the operation unit 60. Signal) is generated. As a result, the position of the sample 1 can be moved to the position specified by the user.

1.2. Analytical Method Next, the analytical method by the analyzer 100 will be described with reference to the drawings. FIG. 5 is a flowchart showing an example of an analysis method by the analyzer 100.

First, as shown in FIG. 2, the data storage processing unit 52 stores the X-ray signal data and the electronic signal data in the storage unit 64 together with the position information data and the elapsed time information data (step S100).

Next, the frame group extraction unit 54 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and sets the frame group based on the change in the X-ray signal between frames. Extract (step S102).

FIG. 6 is a diagram schematically showing the main window 2 displayed on the display unit 62 of the analyzer 100. As shown in FIG. 6, the main window 2 displays secondary electron images 4a and 4b and element distribution images 6a, 6b and 6c generated from the data (see FIG. 2) stored in the storage unit 64. ing. The secondary electron image 4a is, for example, the secondary electron image of the first frame, and the secondary electron image 4b is, for example, the secondary electron image of the frame currently being measured. The secondary electron image 4b may be a secondary electron image obtained by integrating all the frames stored in the storage unit 64. The element distribution images 6a, 6b, and 6c are element distribution images of the designated element (for example, an oxygen element distribution image, a chromium element distribution image, and an iron element distribution image). The element distribution images 6a, 6b, and 6c are obtained by integrating the number of X-ray signal data included in the ROI corresponding to the specified element from the X-ray signal data of all the frames stored in the storage unit 64. It is an image that was made.

For example, when the operation unit 60 receives an operation of specifying the region (position information range) on the element distribution images 6a, 6b, 6c of the user and the ROI to be detected, the frame group extraction unit 54 extracts the frame group. Start the process for.

Hereinafter, the process of extracting the frame group in the frame group extraction unit 54 will be described.

FIG. 7 is a graph showing changes in the ROI count in the designated area. The graph shown in FIG. 7 is a plot of the count (X-ray intensity) of ROI (ROI_1, ROI_2, ROI_3) in the designated region for each frame. In the graph shown in FIG. 7, the horizontal axis is a frame, and the frames are arranged in order from the frame 1 which is the first scan to the frame m which is the final scan from the left side of the paper surface to the right side of the paper surface. The vertical axis is the ROI count, which corresponds to the X-ray intensity of the element corresponding to each ROI.

In the graph shown in FIG. 7, the X-ray signal data of the area specified based on the position information data is extracted for each frame from the data string stored in the storage unit 64, and the graph is designated from the extracted X-ray signal data. It is created by counting the number of X-ray signal data included in the ROI.

Here, the case where ROI_2 is specified will be described.

FIG. 8 is a graph showing changes in the count of ROI_2. When ROI_2 is specified, the frame group extraction unit 54 extracts a frame group based on the count difference of ROI_2 between two consecutive frames.

The frame group extraction unit 54 detects a change in the ROI count by applying a one-dimensional difference filter represented by the following equation (1) to the ROI_2 counts of frames 1 to frame m.

g _n = f _n −f _n-1 (1)

However, g _n is the filtered value (difference value) of the _{nth frame, f n} is the ROI count of the nth frame, and f _n-1 is the ROI count of the n-1st frame. be.

Figure 9 is a graph showing the difference value g _n of each frame. As shown in FIG. 9, the threshold value + TS, -TS (except TS> 0) is set and the frame group and extracts the range frame are consecutive comprised between difference values _{g n} is the threshold + TS and the threshold -TS And. That is, a range in which frames having a threshold value TS or less in which the ROI count difference between two consecutive frames is set is continuous is extracted and used as a frame group. In the example shown in FIG. 9, three continuous ranges of frames in which the ROI count difference between two consecutive frames is equal to or less than the threshold TS are extracted.

FIG. 10 is a graph showing changes in the count of ROI_2. As shown in FIG. 10, as a result of the above processing, the frame groups A, B, and C are extracted. In this way, the frame group extraction unit 54 can extract the frame groups A, B, and C.

Next, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group from the X-ray signal data stored in the storage unit 64, and of the designated ROI (element). An element distribution image is generated (step S104).

For example, when it is specified to generate the element distribution images of ROI_1, ROI_2, and ROI_3, the image generation unit 56 comprises a plurality of frames A formed from the X-ray signal data stored in the storage unit 64. The X-ray signal data of the frame is extracted, and an element distribution image of ROI_1, an element distribution image of ROI_2, and an element distribution image of ROI_3 are generated. Similarly, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group B from the X-ray signal data stored in the storage unit 64, and extracts the element distribution image of ROI_1, ROI_2. An element distribution image and an element distribution image of ROI_3 are generated. Similarly, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group C from the X-ray signal data stored in the storage unit 64, and extracts the element distribution image of ROI_1, ROI_2. An element distribution image and an element distribution image of ROI_3 are generated.

The image generation unit 56 performs a process of applying a two-dimensional filter to the generated element distribution image, and a process.
It is possible to perform processing such as changing the color scale.

FIG. 11 is a diagram schematically showing a comparison window 8 displayed on the display unit 62. The image generation unit 56 includes element distribution images 6a-A, 6a-B, 6a-C of ROI_1 of frame groups A, B, and C, and element distribution images 6b-A, 6b- of ROI_2 of frame groups A, B, and C. The element distribution images 6c-A, 6c-B, 6c-C of ROI_3 of B, 6b-C and frame groups A, B, C are displayed in the comparison window 8.

Further, the image generation unit 56 extracts the electronic signal data of a plurality of frames constituting the frame group A and integrates the electronic signal data for each frame to generate the secondary electron image 4-A. Similarly, the image generation unit 56 extracts the electronic signal data of a plurality of frames constituting the frame group B and integrates the electronic signal data for each frame to generate the secondary electron image 4-B. Similarly, the image generation unit 56 extracts the electronic signal data of a plurality of frames constituting the frame group C and integrates the electronic signal data for each frame to generate the secondary electron image 4-C. Then, the image generation unit 56 displays these secondary electron images 4-A, 4-B, 4-C in the comparison window 8.

Further, the image generation unit 56 displays the frame bar 9 for displaying the range of the frames constituting the frame groups A, B, and C in the comparison window 8.

By the above steps, an element distribution image can be generated.

12 and 13 are diagrams for explaining the processing when the element is added. By operating the element addition button 7 of the main window 2 shown in FIG. 12, the element for displaying the element distribution image can be added. When the element (ROI_4) is added by operating the element addition button 7, the element distribution image 6d of the added ROI_4 is displayed in the main window 2. Then, the image generation unit 56 generates the element distribution images 6d-A, 6d-B, 6d-C of ROI_4 for each of the frame groups A, B, and C, and displays them in the comparison window 8 as shown in FIG. do.

14 and 15 are diagrams for explaining a process of changing the range of frames constituting each of the frame groups A, B, and C (that is, a process of changing the range of the signal data to be extracted).

For example, in the main window 2 and the comparison window 8, a frame bar 9 for displaying and changing the range of the frames constituting the frame groups A, B, and C is displayed, and the frame bar 9 is operated. Therefore, the range of the frames constituting each frame group A, B, and C can be changed. When the operation of changing the frame range is performed, the image generation unit 56 extracts the X-ray signal data for the changed frame groups A, B, and C, and generates an element distribution image. In the illustrated example, the range of the frames constituting the frame group B is changed, and the image generation unit 56 outputs the X-ray signal data of a plurality of frames included in the range of the frames constituting the changed frame group B. Extraction is performed to generate element distribution images 6a-B, 6b-B, 6c-B, 6d-B. At this time, the secondary electron image 4-B of the modified frame group B is also generated in the same manner.

In the above-described embodiment, the case where one ROI (ROI_2) is specified in the step of extracting the frame group (step S102) has been described, but a plurality of ROIs may be specified. Hereinafter, processing when a plurality of ROIs are specified in the step of extracting the frame group will be described.

FIG. 16 is a graph showing changes in the count of ROI_1 and the count of ROI_2.

When the specified ROIs are ROI_1 and ROI_2, the frame group extraction unit 54 extracts the frame group based on the count difference of ROI_1 between two consecutive frames and the count difference of ROI_2 between two consecutive frames. do. Specifically, the frame group extraction unit 54, by multiplying the count and ROI_2 counts of ROI_1, one-dimensional differential filter respectively above the _{(g n = f n -f n} -1), the count of ROI_1 And changes in the count of ROI_2 are detected.

17, each frame is a graph showing the difference value _{g n} of the difference values _{g n} and ROI_2 of ROI_1. As shown in FIG. 17, threshold values + TS _{1 and −TS 1} (where TS ₁ > 0) are set for ROI_1, and threshold values + TS ₂ and _{−TS 2} (where TS ₂ > 0) are set for ROI_1. .. Then, the difference value _{g n} is the threshold TS ₁ the following frame is consecutive ROI_1, and extracts a range difference values _{g n} of ROI_2 threshold TS ₂ the following frames are consecutive, a frame group. In the example shown in FIG. 17, the difference value _{g n} is the threshold TS ₁ the following frame is consecutive ROI_1, and range difference values _{g n} is the threshold TS ₂ the following frames are consecutive ROI_2 are four extraction ..

FIG. 18 is a graph showing changes in the ROI count in the designated area. As shown in FIG. 18, as a result of the above processing, the frame groups A, B, C, and D are extracted. In this way, the frame group extraction unit 54 can extract the frame groups A, B, C, and D even when a plurality of ROIs are specified.

The analyzer 100 has, for example, the following features.

In the analyzer 100, the frame group extraction unit 54 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and is continuous based on the change in the X-ray signal between frames. Extract a frame group consisting of multiple frames. Therefore, in the measurement of the sample 1 in which the state of the sample 1 changes during the measurement, the X-ray signal data before the X-ray signal changes and the X-ray from the X-ray signal data obtained by repeatedly scanning the sample 1. The X-ray signal data after the signal has changed can be extracted respectively. In this way, the analyzer 100 can extract the X-ray signal data before and after the change of the X-ray signal, so that the change in the state (element distribution) of the sample 1 can be easily confirmed. In addition, even when the number of frames becomes enormous due to long-term measurement, it is possible to easily extract X-ray signal data before and after the state (elemental distribution) of the sample changes, which enables analysis. Increased throughput.

In the analyzer 100, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group from the X-ray signal data stored in the storage unit 64 to generate an element distribution image. Therefore, in the measurement of the sample 1 in which the state of the sample 1 changes during the measurement, it is possible to obtain an element distribution image before the X-ray signal changes and an element distribution image after the X-ray signal changes.

In the analyzer 100, when the frame group extraction unit 54 extracts a plurality of frame groups, the image generation unit 56 extracts X-ray signal data for each frame group and generates an element distribution image for each frame group. Therefore, it is possible to obtain an element distribution image before and after the change of the X-ray signal.

In the analyzer 100, since the frame group extraction unit 54 extracts the frame group based on the intensity difference of the X-ray signals of two consecutive frames, in the measurement of the sample 1 in which the state of the sample 1 changes during the measurement, the sample is sampled. From the X-ray signal data obtained by repeatedly scanning step 1, the X-ray signal data before and after the change in the intensity of the X-ray signal can be extracted.

In the analysis method according to the present embodiment, in order to extract a frame group consisting of a plurality of consecutive frames based on the change of the X-ray signal between frames, the X-ray signal data before and after the change of the X-ray signal is extracted. be able to.

1.3. Modification Example Next, a modification of the analyzer according to the first embodiment will be described. The configuration of the analyzer according to this modification is the same as the configuration of the analyzer 100 shown in FIG. 1, and the illustration is omitted. Hereinafter, points different from the above-mentioned example of the analyzer 100 will be described, and description of the same points will be omitted.

In the above-mentioned example of the analyzer 100, the frame group extraction unit 54 extracts the frame group based on the change in the X-ray signal.

On the other hand, in the analyzer according to the present modification, the frame group extraction unit 54 extracts the frame group based on the change in the secondary electron signal.

The frame group extraction unit 54 detects a change in the electronic signal between frames based on the electronic signal data stored in the storage unit 64, and extracts a frame group based on the change in the electronic signal. For example, the frame group extraction unit 54 extracts a frame group based on the similarity between the two secondary electron images generated from the electronic signal data of two consecutive frames. The frame group extraction unit 54 extracts the electronic signal data of two consecutive frames from the data string stored in the storage unit 64, and generates a secondary electron image for each frame. Then, the similarity between the two generated secondary electron images is obtained. The frame group extraction unit 54 monitors the similarity and detects changes by sequentially performing this process for each frame.

The similarity of the secondary electron images is, for example, SAD (Sum of Absolute Difference), SSD (Sum of Squared Difference), NCC (Normalized Cross-Correlation), ZNCC (Zero-mens Is used.

_{Incidentally, SAD (S SAD), SSD} (S SSD), NCC (S NCC), ZNCC (S ZNCC) is expressed by the following equation.

However, X is the number of pixels in the horizontal direction, Y is the number of pixels in the vertical direction, x is the coordinates in the horizontal direction, y is the coordinates in the vertical direction, and F _n is the brightness of the nth frame. Yes, F _n-1 is the brightness of the n-1st frame. Further, μ _n is the average value of the brightness of the nth frame, and μ _n-1 is the average value of the brightness of the n-1st frame.

FIG. 19 is a graph showing the similarity of each frame. In FIG. 19, SAD is used as the similarity. It can be said that the smaller the SAD value, the more similar the two images are.

As shown in FIG. 19, a threshold value TS _SAD (however, TS _SAD is an arbitrary value) is set, and _{a range in which frames whose SAD is} equal to or lower than the threshold value TS SAD are continuous is extracted to form a frame group. In the example shown in FIG. 19, four continuous ranges of frames below the _{threshold TS SAD are extracted.} In this way, the frame group extraction unit 54 can extract the frame groups A, B, C, and D.

The image generation unit 56 generates an element distribution image by extracting the X-ray signal data “D” of a plurality of frames constituting the frame group from the X-ray signal data “D” stored in the storage unit 64. (Step S104).

The image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group A from the X-ray signal data stored in the storage unit 64, and generates an element distribution image. When a plurality of ROIs are specified (ROI_1, ROI_2, ROI_3, ROI_4 are specified), the image generation unit 56 uses the element distribution image of each designated ROI (element distribution image of ROI_1, element of ROI_2). A distribution image, an element distribution image of ROI_3, and an element distribution image of ROI_4) are generated.

The image generation unit 56 performs the same processing on the frame groups B, C, and D, and generates an element distribution image for each of the frame groups B, C, and D.

FIG. 20 is a diagram schematically showing a comparison window 8 displayed on the display unit 62. The image generation unit 56 includes element distribution images 6a-A, 6a-B, 6a-C, 6a-D, and ROI-2 element distribution images 6b-A, 6b- of the generated frame groups A, B, C, and D. Element distribution images of ROI_3 of B, 6b-C, 6b-D, frame groups A, B, C, D 6c-A, 6c-B, 6c-C, 6a-D, frame groups A, B, C, D The element distribution images 6d-A, 6d-B, 6d-C, and 6d-D of ROI_4 of the above are displayed in the comparison window 8. Further, the image generation unit 56 generates secondary electron images 4-A, 4-B, 4-C, 4-D of the frame groups A, B, C, and D and displays them in the comparison window 8.

In the analyzer according to this modification, the frame group extraction unit 54 detects a change in the electronic signal between frames based on the electronic signal data stored in the storage unit 64, and is based on the change in the secondary electronic signal between frames. To extract frames. As a result, in the measurement of the sample whose state (for example, shape) changes during the measurement, the X-ray signal data before and after the secondary electron signal changes from the X-ray signal data obtained by repeatedly scanning the sample 1. Can be extracted. Therefore, it is possible to obtain an element distribution image before and after the secondary electron signal of the sample 1 changes.

In the analyzer according to this modification, the frame group extraction unit 54 extracts a frame group based on the similarity of the two secondary electron images generated from the secondary electron signal data of two consecutive frames. As a result, in the measurement of the sample 1 in which the state (for example, the shape) of the sample 1 changes during the measurement, the similarity of the secondary electron image of the sample 1 is obtained from the X-ray signal data obtained by repeatedly scanning the sample 1. The X-ray signal data before and after the change can be extracted. Therefore, it is possible to obtain element distribution images before and after the degree of similarity of the secondary electron image of sample 1 changes.

In this modification, an example in which the frame group extraction unit 54 extracts the frame group based on the similarity of the two secondary electron images generated from the secondary electron signal data has been described, but the frame group extraction unit 54 has been described. May extract a group of frames based on the similarity of the two element distribution images generated from the X-ray signal data of two consecutive frames. As a result, in the measurement of the sample whose state changes during the measurement, the X-ray signal data before and after the change in the element distribution of the sample is extracted from the X-ray signal data obtained by repeatedly scanning the sample 1. be able to. Therefore, it is possible to obtain an element distribution image before and after the element distribution of the sample changes.

2. Second Embodiment 2.1. Analytical device Next, the analytical device according to the second embodiment will be described with reference to the drawings. FIG. 21 is a diagram schematically showing the analyzer 200 according to the second embodiment. Hereinafter, in the analyzer according to the second embodiment, the members having the same functions as the constituent members of the analyzer 100 according to the first embodiment are designated by the same reference numerals, and detailed description thereof will be omitted.

As shown in FIG. 21, the analyzer 200 is configured to include, in addition to the constituent members of the analyzer 100, a temperature variable holder 210 and a temperature control unit 212 for controlling the temperature of the temperature variable holder 210. ing.

The variable temperature holder 210 is a heating holder capable of holding the sample 1 on the sample stage 20 and heating the sample 1. The temperature variable holder 210 may be a cooling holder for cooling the sample 1. The temperature of the temperature variable holder 210 is controlled by the temperature control unit 212. The temperature control unit 212 sends the temperature information of the temperature variable holder 210 to the processing unit 50. Here, the temperature information of the temperature variable holder 210 output by the temperature control unit 212 may be temperature information based on the control information for the temperature control unit 212 to control the temperature of the temperature variable holder 210. It may be the information of the measurement result which actually measured the temperature of the temperature variable holder 210.

The data storage processing unit 52 stores (records) the electronic signal data and the X-ray signal data in the storage unit 64 together with the position information data of the electron beam EB, the elapsed time information data of the measurement, and the temperature information data (an example of the environmental information data). ) Perform the process.

FIG. 22 is a diagram schematically showing the structure of the data stored in the storage unit 64. In FIG. 22, the position information data is represented by “P”, the X-ray signal data is represented by “D”, the electronic signal data is represented by “S”, the elapsed time information data is represented by “T”, and the temperature information data is represented by “t”. Further, in FIG. 22, the data from the first frame to the mth frame are shown.

As shown in FIG. 22, the data storage processing unit 52 includes position information data “P”, X-ray signal data “D”, electronic signal data “S”, elapsed time information data “T”, and temperature information data “t”. Are piled up to form a data string having the data structure shown in FIG.

The temperature information data "t" is information on the temperature of the sample 1. The temperature information data "t" may be the temperature information obtained by directly measuring the sample 1, or the temperature of the temperature variable holder 210 for controlling the temperature of the sample 1 or the temperature control information of the temperature variable holder 210. May be good. The data storage processing unit 52 receives the temperature information of the temperature variable holder 210 output from the temperature control unit 212, and stores it in the storage unit 64 as the temperature information data “t”. Further, although not shown, the analyzer 200 includes a sample temperature measuring device for measuring the temperature of the sample 1, and the data storage processing unit 52 receives the information of the measurement result of the temperature measuring device, and the temperature information data "t". May be stored in the storage unit 64. The temperature information data "t" is stored in the storage unit 64 at predetermined time intervals (for example, a plurality of times for one frame).

The frame group extraction unit 54 detects a change in the temperature of the temperature variable holder 210 between frames based on the temperature information data stored in the storage unit 64, and based on the temperature change of the temperature variable holder 210, a plurality of continuous frames. Extract a frame group consisting of frames.

The frame group extraction unit 54 extracts a frame group composed of a plurality of consecutive frames based on the temperature difference of the sample 1 of two consecutive frames. As a result, it is possible to extract from the frames stored in the storage unit 64 a frame group composed of a plurality of continuous frames in which the temperature fluctuation of the sample 1 is small.

The image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group extracted by the frame group extraction unit 54 from the X-ray signal data recorded in the storage unit 64, and extracts the elements. Generate a distribution image.

The control unit 58 performs a process of generating a control signal for controlling the temperature control unit 212. For example, when the operation unit 60 receives an operation for setting the temperature of the user's sample 1 (temperature variable holder 210), the control unit 58 controls a control signal (temperature control unit 212) based on the operation signal from the operation unit 60. (Control signal for) is generated. As a result, the temperature of the sample 1 can be set to the temperature specified by the user.

2.2. Analytical Method Next, the analytical method by the analyzer 200 will be described with reference to the drawings. The flow of the analysis method by the analyzer 200 is the same as the flowchart shown in FIG. 5, and the illustration is omitted.

First, as shown in FIG. 22, the data storage processing unit 52 converts the X-ray signal data “D” and the electronic signal data “S” into the position information data “P”, the elapsed time information data “T”, and the temperature information data. Together with "t", it is stored in the storage unit 64 (step S100).

Next, the frame group extraction unit 54 detects a change in the temperature of the sample 1 between frames based on the temperature information data stored in the storage unit 64, and extracts the frame group based on the change in the temperature of the sample 1. (Step S102).

For example, when the operation unit 60 receives an operation to start the process of generating the element distribution image of the user, the frame group extraction unit 54 starts the process for extracting the frame group composed of a plurality of continuous frames.

Hereinafter, the process of extracting the frame group in the frame group extraction unit 54 will be described.

FIG. 23 is a graph showing changes in the temperature of sample 1. The graph shown in FIG. 23 is a plot of the temperature of sample 1 for each frame. In the graph shown in FIG. 23, the horizontal axis is a frame, and the frames are arranged in order from the frame 1 which is the first scan to the frame m which is the final scan from the left side of the paper surface to the right side of the paper surface. The vertical axis is the temperature of sample 1.

The temperature of the sample 1 in each frame is, for example, the temperature information “t” extracted between the position information data “P1” and the position information data “P1” that appears next in the data string shown in FIG. Was taken as the average value.

The frame group extraction unit 54 extracts a frame group based on the temperature difference of the sample 1 between two consecutive frames.

Specifically, the frame group extraction unit 54 detects a change in the temperature of the sample 1 by applying a one-dimensional difference filter shown in the following equation to the temperature of the sample 1 in the frames 1 to frame m.

Δt _n = t _n −t _n-1
However, Δt _n is the difference value of the temperature of the nth frame, t _n is the temperature of the sample 1 of the nth frame, and t _n-1 is the temperature of the sample 1 of the n-1st frame. ..

FIG. 24 is a graph showing _{the difference value Δt n of each frame.} As shown in FIG. 24, the threshold value + TS _t , −TS _t (where TS _t > 0) is set, and the range in which the frame _{in which the difference value Δt n} is included between the threshold value + TS _t and the threshold value −TS _{t is continuous.} Extract and use as a frame group. _{That is, a range in which frames having a threshold value TS t} or less in which the temperature difference of the sample 1 between two consecutive frames is set is continuously extracted is used as a frame group. In the example shown in FIG. 24, three continuous ranges of frames having _{a threshold value of TS t} or less in which the temperature difference of the sample 1 between two consecutive frames is set are extracted.

Next, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group from the X-ray signal data stored in the storage unit 64, and extracts the X-ray signal data of the specified element (ROI). An element distribution image is generated (step S104).

The image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group A from the X-ray signal data stored in the storage unit 64, and extracts the element distribution image of ROI_1 and the element distribution image of ROI_2. , Generates an elemental distribution image of ROI_3. Similarly, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group B from the X-ray signal data stored in the storage unit 64, and extracts the element distribution image of ROI_1, ROI_2. An element distribution image and an element distribution image of ROI_3 are generated. Similarly, the image generation unit 56 extracts the X-ray signal data “D” of a plurality of frames constituting the frame group C from the X-ray signal data stored in the storage unit 64, and extracts the element distribution image of ROI_1. , The element distribution image of ROI_2 and the element distribution image of ROI_3 are generated.

FIG. 25 is a diagram schematically showing a comparison window 8 displayed on the display unit 62. The image generation unit 56 includes element distribution images 6a-A, 6a-B, 6a-C of ROI_1 of frame groups A, B, and C, and element distribution images 6b-A, 6b- of ROI_2 of frame groups A, B, and C. The element distribution images 6c-A, 6c-B, 6c-C of ROI_3 of B, 6b-C and frame groups A, B, C are displayed in the comparison window 8. Further, the image generation unit 56 generates secondary electron images 4-A, 4-B, 4-C of the frame groups A, B, and C and displays them in the comparison window 8. At this time,
The image generation unit 56 displays information on the average temperature of the sample 1 for each frame group. The average temperature of the sample 1 in the frame group is an average value of temperature information data included in a plurality of frames constituting the frame group.

Further, as shown in FIG. 25, in the comparison window 8, when the cursor C is placed on the frame bar 9, the temperature information of the sample 1 of the frame selected by the cursor C is displayed in the window W.

The analyzer 200 has, for example, the following features.

In the analyzer 200, the frame group extraction unit 54 detects a change in the temperature of the sample 1 between frames based on the temperature information data stored in the storage unit 64, and continuously based on the change in the temperature of the sample 1 between the frames. Extract a frame group consisting of a plurality of frames. Therefore, in the measurement of a sample whose state changes during the measurement, it is possible to extract the X-ray signal data before and after the temperature of the sample changes from the X-ray signal data obtained by repeatedly scanning the sample 1. can. As a result, when measuring a sample whose element distribution changes according to the temperature of the sample during measurement, before and after the element distribution of sample 1 changes from the X-ray signal data obtained by repeatedly scanning the sample 1. X-ray signal data can be extracted.

In the analyzer 200, the frame group extraction unit 54 extracts the frame group based on the temperature difference of the sample 1 between the frames. Therefore, the temperature of the sample is obtained from the X-ray signal data obtained by repeatedly scanning the sample 1. The X-ray signal data before and after the change can be extracted.

In the above-described embodiment, the example in which the analyzer 200 includes the temperature variable holder 210 for controlling the temperature of the sample 1 has been described, but the analyzer 200 controls the environment of the sample 1 other than the temperature. It may be provided with an environmental control device for the purpose. Examples of such an environmental control device include a pressure control device for controlling the pressure in the space containing the sample 1, and a reaction gas control device for controlling the concentration of the reaction gas for reacting with the sample 1. And so on.

In this case, the data storage processing unit 52 performs a process of storing the environmental information data, which is information on the environment of the sample 1 other than the temperature, in the storage unit 64 instead of the temperature information data. Examples of such information on the environment of the sample 1 include information on the pressure in the space in which the sample 1 is housed, information on the concentration of the reaction gas, and the like. In such an analyzer, the data storage processing unit 52 stores the X-ray signal data and the like in the storage unit 64 together with the environmental information data of the sample 1, and the frame group extraction unit 54 stores the sample between frames based on the environmental information data. It is possible to detect a change in the environment of 1 and extract a frame group based on the change in the environment between frames. Therefore, in the measurement of a sample whose state changes during the measurement, the X-ray signal data before and after the change in the sample environment can be extracted from the X-ray signal data obtained by repeatedly scanning the sample.

3. 3. Third Embodiment Next, the analyzer according to the third embodiment will be described. The configuration of the analyzer according to the third embodiment is the same as the configuration of the analyzer 200 shown in FIG. 21, and the illustration is omitted. Hereinafter, points different from the example of the analyzer 200 according to the second embodiment described above will be described, and description of the same points will be omitted.

In the analyzer according to the third embodiment, the control unit 58 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and the temperature is based on the change in the X-ray signal. It controls the variable holder 210 (temperature control unit 212).

For example, when the control unit 58 controls to change the temperature of the sample 1 at a constant rate and the intensity of the X-ray signal becomes equal to or less than the threshold value, the temperature variable holder 210 keeps the temperature of the sample 1 constant. Switch to control. The intensity of the X-ray signal is, for example, the intensity of the X-ray signal in the specified energy range (ROI) in the specified region.

First, the control unit 58 controls to change the temperature of the sample 1 at a constant rate. Then, the control unit 58 determines whether or not the X-ray signal between frames has changed based on the X-ray signal data stored in the storage unit 64. For example, the control unit 58 monitors the specified ROI count of each frame, and when the ROI count of the subsequent frames becomes X% or less with respect to the ROI count of the first frame, the X-ray signal changes. It is determined that it has been done. The control unit 58 substitutes the designated ROI count of each frame into the following equation (2), and determines whether or not the ROI count has become X% or less, that is, whether or not the ROI count has changed.

ただし、Ｃｎはｎ番目のフレームのＲＯＩカウントであり、Ｃ１は１番目のフレームのＲＯＩカウントであり、Ｘは規定したパーセントである。

However, Cn is the ROI count of the nth frame, C1 is the ROI count of the first frame, and X is a specified percentage.

FIG. 26 is a graph showing changes in the specified ROI count and changes in the temperature of sample 1. In the graph shown in FIG. 26, the horizontal axis is a frame, and the frames are arranged in order from the frame 1 which is the first scan to the frame m which is the final scan from the left side of the paper surface to the right side of the paper surface. The vertical axis is the ROI count, which corresponds to the X-ray intensity of the element. The threshold value TS _{C in} FIG. 26 is TS _C = ((100-X) / 100) × C1 (the right side of the above equation (2)).

Control unit 58, as shown in FIG. 26, when the difference between the ROI counts of the first ROI count and n-th frame of the frame is equal to or less than a threshold value TS _C (see arrows in FIG. 26), X-ray Determine that the signal has changed. Then, when it is determined that the X-ray signal has changed, the control unit 58 controls the temperature variable holder 210 (temperature control unit 212) so that the temperature of the sample 1 becomes constant.

Here, the control unit 58 makes a determination based on the difference between the intensity of the X-ray signal of the first frame and the intensity of the X-ray signal of the nth frame. The determination may be made based on the intensity difference of the line signal (see the above equation (1)).

In the analyzer according to the present embodiment, the frame group extraction unit 54 and the image generation unit 56 perform the same operations as the above-described analyzer 100, for example. The frame group extraction unit 54 extracts the frame groups A and B shown in FIG. 26 based on the change in the X-ray signal between the frames. Then, the image generation unit 56 extracts the X-ray signal data of a plurality of frames constituting the frame group A from the X-ray signal data stored in the storage unit 64 to generate an element distribution image, and generates a frame. An element distribution image is generated by extracting the X-ray signal data of a plurality of frames constituting the group B.

Here, an example in which the control unit 58 controls the temperature variable holder 210 (temperature control unit 212) based on the change in the intensity of the X-ray signal has been described, but the control unit 58 is similar to the electron image and the element distribution image. The temperature variable holder 210 (temperature control unit 212) may be controlled based on the degree (see “1.3. Modification example” described above).

In the analyzer according to the third embodiment, the control unit 58 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and based on the change in the X-ray signal between frames. , Controls the temperature variable holder 210 (temperature control unit 212). Therefore, for example, as shown in FIG. 26, when the sample causes a change in the element distribution at a predetermined temperature, the temperature (predetermined temperature) can be maintained. Therefore, the X-ray signal from the sample 1 can be detected by repeatedly scanning the sample 1 with an electron beam at a temperature at which the signal of the sample changes. This makes it possible to obtain X-ray signal data after the state of sample 1 has changed.

In the analyzer according to the third embodiment, the control unit 58 controls the temperature variable holder 210 (temperature control unit 212) to change the temperature of the sample 1, and the X-ray signal data stored in the storage unit 64. Based on the above, a process of determining whether or not the X-ray signal between frames has changed, and a control of keeping the temperature of the sample 1 constant when it is determined that the X-ray signal has changed are performed. Thereby, for example, as shown in FIG. 26, when the sample causes a change in the element distribution at a predetermined temperature, the temperature (predetermined temperature) can be maintained. Therefore, it is possible to easily obtain X-ray signal data before and after the element distribution of the sample changes.

Also in this embodiment, as in the case of the analyzer 200, the environmental information of the sample 1 is not limited to the temperature. That is, in the present embodiment, the control unit 58 controls the environment control device based on the change of the X-ray signal between the frames. Thereby, in the measurement of the sample whose state changes during the measurement, when the X-ray signal of the sample 1 changes under a predetermined environmental condition, the predetermined environmental condition can be maintained. Therefore, the signal from the sample 1 can be detected by repeatedly scanning the sample 1 with an electron beam under the environmental conditions in which the X-ray signal of the sample 1 has changed. This makes it possible to obtain X-ray signal data after the state of sample 1 has changed.

The present embodiment can also be applied to a case where the control unit controls the processing device when analyzing the sample 1 while processing it using a processing device (FIB device or the like) in the analyzer.

4. Fourth Embodiment Next, the analyzer according to the fourth embodiment will be described with reference to the drawings. FIG. 27 is a diagram schematically showing the analyzer 300 according to the fourth embodiment. Hereinafter, in the analyzer according to the fourth embodiment, the members having the same functions as the constituent members of the analyzer according to the first to third embodiments are designated by the same reference numerals, and detailed description thereof will be omitted.

In the analyzer 300, as shown in FIG. 27, the processing unit 50 includes a signal change detection unit 55. The signal change detection unit 55 detects a change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64. The intensity of the X-ray signal to be detected is, for example, the intensity of the X-ray signal of the specified ROI for each irradiation position.

The signal change detection unit 55 detects, for example, a change in the intensity of the X-ray signal from the difference between the intensity of the X-ray signal (ROI count) of the first frame and the intensity of the X-ray signal of the nth frame ( Refer to the above equation (2), FIG. 26, etc.). The signal change detection unit 55 determines that the intensity of the X-ray signal has changed when, for example, the ROI count becomes 20% or less (X = 20 in the equation (2)).

The image generation unit 56 generates an element distribution image of a designated ROI (element) based on the X-ray signal data recorded in the storage unit 64. The image generation unit 56 integrates all the frames recorded in the storage unit 64 to generate an element distribution image of the designated ROI (element).

FIG. 28 is a diagram schematically showing the main window 2 displayed on the display unit 62. The image generation unit 56 includes the element distribution image 6a of ROI_1, the element distribution image 6b of ROI_2, and R.
The element distribution image 6c of OI_3 and the element distribution image 6c are generated and displayed in the main window 2. Here, the element distribution images 6a, 6b, and 6c count the number of X-ray signal data included in the ROI corresponding to the designated element from all the X-ray signal data stored in the storage unit 64 for each region. It is an image obtained by. That is, the element distribution images 6a, 6b, and 6c are images obtained by integrating all the frames.

In the element distribution images 6a, 6b, and 6c, the image generation unit 56 corresponds the element type (ROI) to the color, the intensity of the X-ray signal to the brightness, and colors the change of the X-ray signal. Corresponds to the degree. For example, the image generation unit 56 displays the element distribution image 6a of ROI_1 in red, the element distribution image 6a of ROI_1 in blue, and the element distribution image 6a of ROI_1 in green. Further, the image generation unit 56 increases the brightness of the element distribution image, for example, at a position where the intensity of the X-ray signal is stronger (the number of ROI counts is larger). When the signal change detection unit 55 determines that the intensity of the ROI_1 X-ray signal has changed at a certain irradiation position, the image generation unit 56 determines the saturation of the position on the element distribution image corresponding to the irradiation position. Reduce from the initial value of 100% to 80%. For example, in the element distribution image 6a of ROI_1, when the X-ray intensity of the element corresponding to ROI_1 of the region SA being measured decreases, the saturation of the region SA is displayed lower than that of the other regions.

In the above, the initial value of saturation is set to 100%, but the initial value of saturation may be set to 50%. Thereby, for example, when the X-ray intensity of the element increases, the saturation can be increased, and when the X-ray intensity of the element decreases, the saturation can be decreased.

Further, in the above, the image generation unit 56 has performed the process of reducing the saturation when the intensity of the X-ray signal changes, but may perform the process of reducing the saturation according to the intensity of the X-ray signal.

FIG. 29 is a diagram for explaining a process of reducing the saturation according to the intensity of the X-ray signal. As shown in FIG. 29, a plurality of thresholds TS _C- 1 (X = 20 in equation (2)), TS _C- 2 (X = 40 in equation (2)), TS _C -3 (X = 40 in equation (2)). X = 50) is set and the image generation unit _56, | if is below threshold _{TS C-1,} lowering the saturation to 80% to _{100%, | | C n -C} n-1 C n When −C _n-1 | is _{below the threshold TS C-2} , the saturation is reduced from 80% to 60%, and when | C _n −C _n-1 | is below the _{threshold TS C-3.} In addition, a process of reducing the saturation from 60% to 40% is performed.

Further, in the above, the signal change detection unit 55 has detected the intensity of the X-ray signal of the designated ROI for each irradiation position, but detects the intensity of the X-ray signal of the designated ROI in the designated area. You may.

The analyzer 300 has, for example, the following features.

In the analyzer 300, the signal change detection unit 55 detects the change in the X-ray signal between frames based on the X-ray signal data stored in the storage unit 64, and the image generation unit 56 detects the X-ray signal data and the X between frames. An element distribution image is generated based on the detection result of the change of the line signal. Then, the image generation unit 56 makes the intensity of the X-ray signal correspond to the brightness of the element distribution image, and the detection result of the change of the X-ray signal between frames corresponds to the saturation of the element distribution image to generate the element distribution image. Generate. Therefore, it can be easily determined whether or not the state of the sample 1 has changed during the measurement.

5. Fifth Embodiment Next, the analyzer according to the fifth embodiment will be described with reference to the drawings. FIG. 30 is a diagram schematically showing the analyzer 400 according to the fifth embodiment. Hereinafter, in the analyzer according to the fifth embodiment, the members having the same functions as the constituent members of the analyzer according to the first embodiment are designated by the same reference numerals, and detailed description thereof will be omitted.

In the analyzer 300, as shown in FIG. 1, the processing unit 50 includes a frame group extraction unit 54, and the frame group extraction unit 54 extracts a frame group based on a change in the X-ray signal. It was processing.

On the other hand, in the analyzer 400, as shown in FIG. 30, the processing unit 50 does not have the frame group extraction unit 54. In the analyzer 400, the operation unit 60 receives an operation for designating a frame group composed of a plurality of consecutive frames by the user, and the image generation unit 56 stores the operation information in the storage unit 64 based on the operation information from the operation unit 60. From the X-ray signal data, the X-ray signal data of a plurality of frames constituting the designated frame group is extracted to generate an element distribution image.

FIG. 31 is a diagram showing an example of a GUI (Graphical User Interface) screen 402 of the analyzer 300.

As shown in FIG. 31, the GUI screen 402 displays a frame bar 9 for displaying and changing the range of the frames constituting the frame groups A, B, and C, and the cursor is displayed on the frame bar 9. By specifying the frame range with 404, the range of the frames constituting each frame group A, B, and C can be specified. When the operation of designating the frame range is performed, the image generation unit 56 extracts the X-ray signal data in the frame range constituting the designated frame groups A, B, and C, and generates an element distribution image.

The analysis method by the analyzer 400 will be described. In the analyzer 400, in the analysis method by the analyzer 100 shown in FIG. 5 and the step of extracting the frame group (step S102), the user bases on the change of the X-ray signal (or secondary electron signal) between the frames. The difference is that a frame group consisting of a plurality of consecutive frames is extracted.

Specifically, the user confirms the change in the X-ray signal by looking at the element distribution image generated for each frame, and uses the frame bar 9 and the cursor 404 of the GUI screen shown in FIG. 31 to display the frame group. Extract. At this time, the user can extract a plurality of frame groups (frame groups A, B, C in the illustrated example) as shown in FIG. 31.

According to the analyzer 400, the data storage processing unit 52 stores the X-ray signal data together with the position information data in the storage unit 64, and the operation unit 60 performs an operation for designating a frame group composed of a plurality of consecutive frames. Upon reception, the image generation unit 56 extracts the signal data of a plurality of frames constituting the designated frame group from the X-ray signal data stored in the storage unit 64 based on the operation signal from the operation unit 60. And generate an image. Therefore, in the measurement of the sample whose state changes during the measurement, it is possible to extract the data before and after the change of the X-ray signal of the sample.

The user confirms the change in the secondary electron image between frames by looking at the secondary electron image generated for each frame, and sets the frame group based on the change (similarity) in the secondary electron image between frames. It may be extracted.

The present invention is not limited to the above-described embodiment, and various modifications can be made within the scope of the gist of the present invention.

In the above-described embodiment, an example in which the analyzers 100, 200, 300, and 400 are scanning electron microscopes (SEMs) equipped with the EDS detector 40 has been described, but the analyzer according to the present invention is a sample with a charged particle beam. Any device may be used as long as it is an apparatus for analyzing a sample by repeatedly scanning the above to detect a signal from the sample. Such an analyzer includes at least one of a scanning electron microscope equipped with a wavelength dispersion type X-ray detector (WDS detector), an EDS detector, a WDS detector, and an electron energy loss spectrometer (EELS). Examples thereof include a scanning electron microscope (STEM). Here, when a scanning transmission electron microscope is used as the analyzer according to the present invention, the signal from the sample includes a transmission electron signal transmitted through the sample 1, and the electronic signal data “S” (see FIG. 2) is a transmission electron signal. Is the data obtained by detecting with a transmission electron detector.

The above-described embodiments and modifications are merely examples, and the present invention is not limited thereto. For example, each embodiment and each modification can be combined as appropriate.

The present invention includes substantially the same configurations as those described in the embodiments (eg, configurations with the same function, method and result, or configurations with the same purpose and effect). The present invention also includes a configuration in which a non-essential part of the configuration described in the embodiment is replaced. The present invention also includes a configuration that exhibits the same effects as the configuration described in the embodiment or a configuration that can achieve the same object. Further, the present invention includes a configuration in which a known technique is added to the configuration described in the embodiment.

2 ... main window, 7 ... element addition button, 8 ... comparison window, 9 ... frame bar, 10 ... optical system, 12 ... electron source, 14 ... focusing lens, 16 ... objective lens, 18 ... deflector, 19 ... Optical system control unit, 20 ... sample stage, 22 ... sample stage control unit, 30 ... secondary electron detector, 32 ... electronic signal processing unit, 40 ... EDS detector, 42 ... X-ray signal processing unit, 50 ... processing unit , 52 ... Data storage processing unit, 54 ... Frame group extraction unit, 55 ... Signal change detection unit, 56 ... Image generation unit, 58 ... Control unit, 60 ... Operation unit, 62 ... Display unit, 64 ... Storage unit, 100 ... Analytical device, 200 ... Analytical device, 210 ... Variable temperature holder, 212 ... Temperature control unit, 300 ... Analytical device, 400 ... Analytical device, 402 ... GUI screen, 404 ... cursor

Claims (6)

An analyzer that repeatedly scans a sample with a charged particle beam, detects a signal from the sample, and analyzes the sample.
An environmental control device that controls the environment of the sample,
A data storage processing unit that stores the signal data obtained by detecting the signal together with position information data indicating the irradiation position of the charged particle beam on the sample, and a data storage processing unit.
A control unit that detects a change in the signal between frames based on the signal data stored in the storage unit and controls the environment control device based on the change in the signal between frames.
Including analyzer. In claim 1,
The environmental control device is an analyzer that controls the temperature of the sample. An analyzer that repeatedly scans a sample with a charged particle beam, detects a signal from the sample, and analyzes the sample.
A data storage processing unit that stores the signal data obtained by detecting the signal together with position information data indicating the irradiation position of the charged particle beam on the sample, and a data storage processing unit.
A signal change detection unit that detects a change in the signal between frames based on the signal data stored in the storage unit, and a signal change detection unit.
An image generation unit that generates an image based on the signal data stored in the storage unit and the detection result of a change in the signal between frames.
Including
The image generation unit is an analyzer that generates the image by associating the intensity of the signal with the brightness of the image and the detection result of a change in the signal between frames with the saturation of the image. An analytical method in which a sample is repeatedly scanned with a charged particle beam to detect a signal from the sample, and the sample is analyzed.
The process of controlling the environment of the sample and
A step of storing the signal data obtained by detecting the signal in the storage unit together with the position information data indicating the irradiation position of the charged particle beam on the sample.
A step of detecting a change in the signal between frames based on the signal data stored in the storage unit and controlling the environment control device based on the change in the signal between frames.
Analytical methods, including. In claim 4,
The environmental control device is an analytical method for controlling the temperature of the sample. An analytical method in which a sample is repeatedly scanned with a charged particle beam to detect a signal from the sample, and the sample is analyzed.
A step of storing the signal data obtained by detecting the signal in the storage unit together with the position information data indicating the irradiation position of the charged particle beam on the sample.
A step of detecting a change in the signal between frames based on the signal data stored in the storage unit, and
A step of generating an image based on the signal data stored in the storage unit and the detection result of a change in the signal between frames.
Including
In the step of generating the image, an analysis method in which the intensity of the signal is made to correspond to the brightness of the image, and the detection result of the change in the signal between frames is made to correspond to the saturation of the image to generate the image. ..

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