JP2022143774A - Sample analyzer and method for analyzing sample - Google Patents

Abstract

To provide a sample analyzer and a method for analyzing a sample that can accurately detect depth-directional features of a sample.SOLUTION: A laser contactless three-dimensional shape measuring device 10 measures the shape of a sample. A low load polishing device 19 performs polish processing on the surface of the sample. A Fourier transformation infrared spectroscopic analyzer 20 executes spectroscopic analysis on the processing surface of the sample. A numerical value operation device 17 analyzes features of the sample in the depth direction of the polishing processing on the sample on the basis of the result of measuring the shape of the sample and the result of the spectroscopic analysis.SELECTED DRAWING: Figure 4

Description

The present disclosure relates to a sample analysis device and a sample analysis method.

A surface analysis apparatus described in Patent Document 1 includes an ion gun for polishing a sample surface by ion etching. This surface analysis device includes a detection device that detects the emission from the sample surface due to probe irradiation and analyzes the components of the sample surface to detect depth data, and a detection device that measures data in the height direction of the sample surface to determine the actual depth. and a scanning probe microscope for detecting the data. The actual depth data measured by the scanning probe microscope is used as the depth direction data of the depth data measured by the detection device.

JP-A-7-159302

In the apparatus described in Patent Document 1, since an ion gun is used as a processing mechanism, the characteristics of the sample in the depth direction cannot be detected accurately. This is because a polymer sample cannot be processed while maintaining the bonding state.

SUMMARY OF THE INVENTION Therefore, an object of the present disclosure is to provide a sample analysis device and a sample analysis method that can accurately detect the characteristics of a sample in the depth direction.

The sample analysis apparatus of the present disclosure includes a shape measuring device for measuring the shape of a sample, a low-load polishing device for polishing the surface of the sample, a spectroscopic analysis device for performing spectroscopic analysis on the processed surface of the sample, and a shape of the sample. and an arithmetic device for analyzing the characteristics of the sample at the depth of polishing of the sample based on the measurement result of and the result of the spectroscopic analysis.

The sample analysis method of the present disclosure includes the steps of measuring the shape of the sample before polishing, polishing the sample with a low load, measuring the shape of the sample after polishing, and measuring the shape of the sample before polishing. and the shape of the sample after polishing, calculating the polishing depth of the sample, performing spectroscopic analysis of the processed surface of the sample, and based on the results of the spectroscopic analysis, and analyzing the properties of the specimen at the depth of polishing of the specimen.

According to the present disclosure, since the sample is polished with a low load, it is possible to accurately detect the characteristics of the sample in the depth direction.

It is a figure for demonstrating diagonal cutting. It is a figure for demonstrating the relationship between a sample shape and a depth direction. 4 is a flow chart showing the procedure of depth direction analysis of a curved structure sample. 1 is a diagram illustrating a configuration example of a sample analyzer according to Embodiment 1; FIG. FIG. 2 is a diagram showing the procedure of sample analysis by the sample analyzer of Embodiment 1; 3 is a diagram showing an initial shape (x, y, z0) acquired from the laser non-contact three-dimensional shape measuring device 10; FIG. FIG. 3 is a diagram representing the three-dimensional shape (x, y, z1) of a polypropylene strip sample after polishing; It is a figure showing depth information (x, y, d). It is a graph representing (y, d). FIG. 3 represents the FT-IR spectra obtained at the indicated points; 4 is a graph showing the relationship between depth d and degree of deterioration E; 4 is a diagram showing in-plane distribution data (x, y, E) of the degree of deterioration E; FIG. 4 is a diagram showing correlation data (d, E) between depth d and degree of deterioration E; FIG. FIG. 10 is a diagram showing the procedure of sample analysis by the sample analyzer of Embodiment 2; FIG. 13 is a diagram showing an example of a display screen according to Embodiment 3; FIG. FIG. 11 is a diagram showing a configuration example of a sample analyzer of Embodiment 4; FIG. 12 is a diagram showing the procedure of sample analysis by the sample analyzer of Embodiment 4; FIG. 10 is a diagram showing the procedure of sample analysis by the sample analyzer of Embodiment 5;

Reference example.
As a reference example, a general technique described in "Journal of Adhesion Society of Japan Vol.44, No.4 (2008), p.124" will be described.

FIG. 1 is a diagram for explaining oblique cutting. FIG. 1(a) is a cross-sectional view of a sample. FIG. 1(b) is a top view of the sample after cutting. A membrane 2 is arranged on a substrate 3 and a membrane 1 is arranged on the membrane 2 .

As shown in FIG. 1, by cutting the sample from the surface at an angle θ, it is possible to expose a width (1/sin θ) times the target layer with thickness t. For cutting the sample, a microtome, a special oblique cutting device SAICAS (manufactured by Daipla Wintes), or the like is widely used. For example, if θ is set to 0.05°, a film with a thickness of 100 nm is expanded 1000 times to a width of 100 μm and exposed on the surface. Even such an extremely thin film can be easily analyzed by an analytical method with relatively low spatial resolution by the oblique cutting method. In the known examples such as the reference examples, flat plate-shaped samples are all analyzed. However, a target sample for which information is actually desired is not limited to a flat plate.

FIG. 2 is a diagram for explaining the relationship between the sample shape and the depth direction. FIG. 2 depicts the difference in lateral (X) distribution versus depth exposed by oblique cutting for flat and curved samples.

FIG. 2(a) represents a flat structure sample. As shown in FIG. 2(b), in the case of a flat sample, the relationship between the horizontal direction and the processing depth is linear. can get.

FIG. 2(c) represents a sample with a curved structure. As shown in FIG. 2(d), in the case of a sample with a curved structure, the relationship between the horizontal direction and the processing depth is not a linear relationship. , it becomes necessary to select points to be analyzed.

FIG. 3 is a flow chart showing the procedure of depth direction analysis of a curved structure sample.

In step S101, the three-dimensional shape measuring device measures the three-dimensional shape of the sample before processing.

In step S102, the processing device cuts the sample. Since it is not a necessary condition that the bending structure sample be processed obliquely, it is described as (oblique) cutting.

In step S103, the three-dimensional shape measuring device measures the three-dimensional shape of the processed sample.

In step S104, the analysis device can obtain the correspondence information between the horizontal coordinate and the processing depth obtained by obtaining the difference in shape of the sample before and after processing. An analysis device selects a predetermined abscissa and analyzes the surface of the sample, such as by Fourier transform infrared spectroscopy (FT-IR), thereby analyzing the sample information according to the processing depth.

Between each step of these four steps, sample attachment/detachment processing and transport processing are required. Since the (x, y) coordinates of each device slightly shift each time the sample is attached or detached, as long as it is done manually, it is necessary to correct the (x, y) coordinates of each data. For example, if the (x, y) coordinates of the three-dimensional shape measurement (before processing) and the (x, y) coordinates of the three-dimensional shape measurement (after processing) do not exactly match, the (x, y) coordinates The processing depth z becomes an erroneous value. Also, even if the (x, y) coordinates of the three-dimensional shape measurement (before processing) and the (x, y) coordinates of the three-dimensional shape measurement (after processing) are matched, the coordinates are shifted in the analysis in step S104. , the depth corresponding to the analyzed sample information will be incorrect. In addition, it is necessary to replace the sample in each device. In many cases, these instruments are used for different purposes and are rarely located close to each other, often involving long distance travel, making it extremely difficult to obtain analytical results. time consuming. As described above, the known technique has the problem that an accurate depth direction cannot be obtained and the problem that the measurement takes too much time. The sample analyzer of the embodiment solves the problems of conventional sample analysis methods, and can accurately obtain analysis data in the depth direction in a short period of time.

Embodiment 1.
FIG. 4 is a diagram showing a configuration example of the sample analyzer of Embodiment 1. FIG.

The sample analyzer includes a sample stage 13, a sample stage drive rail 12, a non-contact laser three-dimensional shape measuring device 10, a low load polishing device 19, a Fourier transform infrared spectroscopic analyzer 20, and a numerical calculation device 17. , a keyboard 15 , a mouse 16 and a monitor 18 .

FIG. 4 shows an example using Fourier transform infrared spectroscopy (FT-IR) as a measuring device for surface analysis, but the present invention is not limited to this. It is also possible to apply measuring devices for surface analysis by other methods. FIG. 4 shows an example in which a non-contact laser three-dimensional shape measuring device is used as a shape measuring device for obtaining data in the depth direction before and after processing, but the present invention is not limited to this. A shape measuring device using other measuring methods can also be applied.

The positional relationship between the Fourier transform infrared spectroscopic analysis device 20, the non-contact laser three-dimensional shape measuring device 10, and the low-load polishing device 19 can be other than the positional relationship shown in FIG.

The keyboard 15 and mouse 16 function as input devices for receiving user input. The monitor 18 functions as a display device.

The sample stage 13 can be moved forward in the plane of the paper for exchanging the sample 11 . All of the mechanisms are connected to the numerical arithmetic unit 17, and all mechanisms are automatically driven by signals from the numerical arithmetic unit 17. FIG.

The sample stage 13 on which the sample 11 is mounted is transported by the sample stage drive rail 12 and is sequentially introduced into the laser non-contact three-dimensional shape measuring device 10, the low load polishing device 19, and the Fourier transform infrared spectroscopic analysis device 20. and carried out.

A non-contact laser three-dimensional shape measuring device 10 measures the shape of a sample. The laser non-contact three-dimensional shape measuring device 10 is capable of measuring a larger size sample than the scanning probe microscope used by the surface analysis device described in Patent Document 1, and is capable of measuring a wide height range. is possible.

A low-load polishing device 19 polishes the surface of the sample. Unlike the ion gun described in Patent Document 1, the low-load polishing apparatus 19 can process a polymer sample while maintaining the bonded state.

The Fourier transform infrared spectroscopic analysis device 20 performs spectroscopic analysis of the polished surface of the sample.

The numerical calculation unit 17 analyzes the characteristics of the sample at the polished depth of the sample based on the measurement result of the shape of the sample and the result of the spectroscopic analysis.

FIG. 5 is a diagram showing the procedure of sample analysis by the sample analyzer of Embodiment 1. FIG.

In step S<b>201 , the user sets the sample 11 on the sample stage 13 .

In step S202, the sample stage 13 is transported on the sample stage drive rail 12 and introduced into the laser non-contact three-dimensional shape measuring device 10 (shape measuring device).

In step S203, the laser non-contact three-dimensional shape measuring device 10 measures the initial shape, which is the initial height of the sample 11 before processing. The (x, y) coordinates and the data of the unprocessed height z0 corresponding to these coordinates are stored in the numerical calculation device 17. FIG.

In step S204, the user inputs the post-processing shape of the sample 11, the coordinate information (x, y) of the measurement position to be analyzed or the depth (post-processing displacement amount) d information, and the desired output format. Enter analysis conditions and send instructions. This instruction can also be input before setting the sample.

In step S205, the sample stage 13 on which the sample 11 is set is conveyed on the sample stage driving rail 12, carried out from the laser non-contact three-dimensional shape measuring device 10, and transferred to the low-load polishing device 19 (polishing device). be introduced.

In step S206, the low-weight polishing apparatus 19 performs low-weight polishing processing on the sample 11 in which the processing position and tilt axis are adjusted according to the instructed sample processing conditions. Polishing is done dry without using water.

In step S207, the sample stage 13 on which the polished sample 11 is set is conveyed on the sample stage driving rail 12, carried out from the low-load polishing device 19, and is again transferred to the laser non-contact three-dimensional shape measuring device 10. introduced into

In step S208, the laser non-contact three-dimensional shape measuring device 10 measures the shape (height) of the polished sample. The (x, y) coordinates and data of the processed height z1 corresponding to these coordinates are stored in the numerical calculation device 17 .

In step S209, the numerical calculation device 17 calculates the difference between the pre-machining height z0 and the post-machining height z1, and determines the polishing depth d (=z0-z1) corresponding to the (x, y) coordinates. calculate.

In step S210, the sample stage 13 on which the sample 11 whose shape measurement after polishing is completed is transported on the sample stage drive rail 12, carried out from the laser type non-contact three-dimensional shape measuring apparatus 10, and subjected to Fourier transform infrared measurement. It is introduced into the spectroscopic analysis device 20 (spectroscopic analysis device).

In step S211, the Fourier transform infrared spectroscopic analysis device 20 performs Fourier transform infrared spectroscopic analysis at the (x, y) coordinates designated by the user within the processing plane.

In step S212, the numerical calculation device 17 analyzes the data of the peak intensity E of the specific bonding state in the Fourier transform infrared spectroscopic analysis spectrum for each (x, y) coordinate within the processing plane. By setting the peak of the specific binding state to a peak whose intensity increases or decreases as the polymer deteriorates, the peak intensity E becomes a numerical value that directly indicates the degree of deterioration. The numerical arithmetic unit 17 outputs distribution data (x, y, E) of the degree of deterioration E corresponding to the (x, y) coordinates as a three-dimensional image, or correlation data (d , E).

Next, an example of the analysis procedure by the sample analyzer of Embodiment 1 will be described.

The sample was not a flat plate, but a piece of polypropylene with a unique structure curved in three dimensions.

FIG. 6 is a diagram showing the initial shape (x, y, z0) acquired from the laser non-contact three-dimensional shape measuring device 10. As shown in FIG. Processing conditions and measurement points were specified for the initial shape shown in FIG. The processing conditions were set such that the starting point was 4 mm from the end and the cutting angle was 3.4° so that the vicinity of the top of the polypropylene piece was cut with an inclination. With a load of 50 g, 90% was polished with #400 abrasive paper, and 10% was polished with #2500 abrasive paper. Buffing was performed with a diamond of 0.5 μm. Although not shown, the low-load polishing device 19 has a mechanism for automatically exchanging polishing paper.

FIG. 7 is a diagram showing the three-dimensional shape (x, y, z1) of the polypropylene strip sample after polishing. A three-dimensional shape (x, y, z1) is measured by a laser non-contact three-dimensional shape measuring device 10 .

FIG. 8 is a diagram representing depth information (x, y, d). d=z0−z1 is calculated by the numerical arithmetic unit 17. FIG.

FIG. 9 is a graph representing (y, d). In the graph of FIG. 9, the y-axis is a straight line of x=7.6 drawn in the direction of inclination from the coordinates of the starting point of machining.

An FT-IR spectrum is then acquired at the (x, y) coordinates corresponding to a given depth d. Points (arrows in FIG. 9) at processing depths d=0, 200, 400, 600, and 800 μm on the finger straight line x=7.6 were designated.

FIG. 10 represents the FT-IR spectra obtained at the designated points. In polypropylene, a peak derived from the basic skeleton at 1376 cm ⁻¹ and a C=O double bond peak generated by oxidation degradation at 1735 cm ⁻¹ are detected.

FIG. 11 is a graph showing the relationship between depth d and degree of deterioration E. In FIG.

Here, the parameter E indicating the degree of deterioration is a value normalized by the C=O double bond peak intensity and the basic skeleton peak intensity.

From this result, the degree of deterioration E becomes 0 at a depth of approximately 500 μm. That is, it can be seen that the depth of deterioration of this polypropylene sample is about 500 μm.

By exhaustively selecting the (x, y) coordinates at intervals of 0.5 mm and performing Fourier transform infrared spectroscopic analysis, the deterioration distribution for each coordinate can also be obtained.
FIG. 12 is a diagram showing in-plane distribution data (x, y, E) of the degree of deterioration E. FIG.

FIG. 13 is a diagram showing correlation data (d, E) between depth d and degree of deterioration E. In FIG.

In Embodiment 1, three-dimensional shape measurement (before processing) A, processing B, three-dimensional shape measurement (after processing) C, and analysis D in FIG. Therefore, it is possible to obtain a true analysis result with higher accuracy than the conventional technique. In addition, since the attachment and detachment of the sample is unnecessary and automated, the analysis can be performed in a short time. Although it is an independent trial calculation, according to the first embodiment, the processing and analysis that takes two days at the earliest even when the devices are arranged side by side in a state where each device is separated from each other, is approximately It can be done in half a day. Further, depth direction distribution analysis using oblique processing can generally be performed only for a plate-shaped sample, but according to Embodiment 1, it can be performed for samples of any shape.

In Embodiment 1, the sample of resin was taken as an example, but the same effect can be obtained with a metal or other compound.

Although the three-dimensional shape of the sample was measured using a laser type non-contact three-dimensional shape measuring device, it is not limited to this. A similar effect can be obtained by using another three-dimensional shape measuring device such as an optical microscope or a stylus type. An example of using a Fourier transform infrared spectroscopic analyzer as a spectroscopic analyzer for obtaining peak intensity data of a specific binding state has been shown, but the present invention is not limited to this. A device that performs Raman spectroscopy may be used.

A substance having a C=O double bond can be detected by detecting the specific binding state of the C=O double bond, but the specific binding state of other substances may also be detected. This also makes it possible to analyze the composition ratio of the sample.

Furthermore, the surface elemental composition (ratio of constituent atoms) can be analyzed by using SEM (scanning electron microscope), AES (Auger electron spectroscopy), or XPS (X-ray photoelectron spectroscopy). Alternatively, trace impurities and the like can be analyzed by using TOF-SIMS (secondary ion mass spectrometry in flight).

Embodiment 2.
The configuration of the sample analyzer of the second embodiment is similar to that of the sample analyzer of the first embodiment shown in FIG.

FIG. 14 is a diagram showing the procedure of sample analysis by the sample analyzer of the second embodiment.

Steps S201 to S205 are executed in the same manner as in the first embodiment.

In step S400, the numerical calculation device 17 extracts the machining time included in the input machining conditions. Alternatively, the numerical calculation device 17 may calculate the machining time based on the initial shape data and machining conditions. The numerical calculation device 17 predicts the shape of the sample when the polishing process is stopped when a predetermined time in the middle of the polishing process of the sample 11 elapses. For example, the numerical calculation device 17 predicts the intermediate shape of the sample when polishing is stopped at half the processing time. The numerical calculation device 17 stores the generated intermediate predicted shape data.

In step S401, the low-load polishing apparatus 19 performs the first half low-load polishing process on the sample 11 in which the processing position and tilt axis are adjusted according to the instructed processing conditions. The low-load polishing device 19 stops polishing the sample when half the processing time has elapsed.

In step S402, the sample stage 13 on which the sample 11 is set is conveyed on the sample stage drive rail 12, carried out from the low-load polishing apparatus 19, and introduced again into the laser type non-contact three-dimensional shape measuring apparatus 10. .

In step S403, the laser non-contact three-dimensional shape measuring device 10 measures the intermediate shape of the sample when the polishing process is stopped. The (x, y) coordinates and the data of the height z1A after 1/2 of the machining time corresponding to the coordinates are stored in the numerical calculation unit 17 as intermediate shape data.

In step S404, the numerical calculation device 17 corrects the machining conditions based on the intermediate predicted shape data and the intermediate shape data so that the initially input post-machining shape is obtained. For example, the numerical calculation device 17 compares the processing rate at which the intermediate predicted shape is formed and the processing rate at which the intermediate shape is formed, and corrects the parameter error related to the processing rate. The processing rate is obtained by dividing the volume of the sample polished by the polishing time. Alternatively, the numerical calculation device 17 may calculate the machining time until the initially input post-machining shape is obtained when machining is performed at a machining rate at which an intermediate shape is formed, and correct the machining time.

In step S405, the sample stage 13 on which the sample 11 is set is transported on the sample stage driving rail 12, carried out from the laser non-contact three-dimensional shape measuring apparatus 10, and transferred to the low load polishing apparatus 19 (polishing apparatus). be introduced.

In step S406, the low-load polishing device 19 performs the latter half of the low-load polishing process on the sample 11 according to the modified processing conditions.

In step S407, the sample stage 13 on which the sample 11 that has been polished (second half) is set is transported on the sample stage drive rail 12, carried out from the low-load polishing device 19, and again laser-type non-contact three-dimensional shape. It is introduced into the measuring device 10 .

Subsequent steps S208 to S212 are the same as in the first embodiment.

As described above, according to Embodiment 2, the shape of the sample after polishing can be brought closer to the shape predicted in advance, and the desired shape of the sample can be accurately obtained. In addition, although the method in which the processing is divided into two steps is described above, a more accurate analysis can be performed by dividing the processing into three or more steps. The difference between the intermediate shape data and the intermediate prediction data, the correction of the processing rate, and the like are automatically performed by the numerical arithmetic unit 17, so confirmation by the user is unnecessary.

Embodiment 3.
The configuration of the sample analyzer of Embodiment 3 is the same as that of the sample analyzer of Embodiment 1 shown in FIG. The sample analysis procedure of the third embodiment is the same as the sample analysis procedure of the first embodiment shown in FIG. Embodiment 3 differs from Embodiments 1 and 2 in the method of inputting the processing conditions for the sample 11 .

The numerical calculation device 17 displays the shape of the sample before processing and the processed surface on the monitor 18 .

The numerical calculation device 17 changes the position and orientation of the processed surface of the sample 11 according to the user's input from the keyboard 15 or the mouse 16, and displays the predicted shape of the processed sample 11 according to the processed surface on the monitor 18. indicate.

FIG. 15 is a diagram showing an example of a display screen according to the third embodiment. Within the monitor display frame 22 are a machining condition instruction display frame 23, a post-machining predicted shape display frame 24, a post-machining predicted shape plan view display frame 25, a post-machining predicted shape front view display frame 26, and a post-machining predicted shape side view display. A frame 27 and a post-processing depth distribution display frame 35 are arranged.

In the processing condition instruction display frame 23, a three-dimensional view 28 of sample shape before processing and a processed surface 29 representing the initial shape of the sample 11 obtained by the laser type non-contact three-dimensional shape measuring device 10 are displayed.

A user can operate the processing surface 29 with the mouse 16 . The user can rotate or move the processing surface 29 in any direction.

Numerical values representing the machining surface are displayed in the machining parameter display frame 34 . The numerical values representing the machining surface include, for example, the origin coordinates of the machining surface representing the position of the machining surface, and the inclination and orientation of the machining surface representing the direction of the machining surface. The user can change the machining surface by inputting numerical values from the keyboard 15 .

A three-dimensional drawing 30 of the sample shape after processing is displayed in the predicted shape display frame 24 after processing. A post-machining predicted shape plan view 31 is displayed in the post-machining predicted shape plan view display frame 25 . A post-machining predicted shape front view 32 is displayed in the post-machining predicted shape front view display frame 26 . A post-machining predicted shape side view 33 is displayed in the post-machining predicted shape side view display frame 27 . A processing depth distribution graph 36 is displayed in the processing depth distribution display frame 35 . When the user changes the position and orientation of the processing surface 29, the three-dimensional view 30 of the sample after processing, the plan view 31 of the predicted shape after processing, the front view 32 of the predicted shape after processing, and the side view 33 of the predicted shape after processing change. do. The user can designate machining conditions while viewing the predicted shape in this way.

According to Embodiment 3, it is possible to acquire information on an interesting site inside the sample without error.

Embodiment 4.
FIG. 16 is a diagram illustrating a configuration example of a sample analyzer according to Embodiment 4. FIG. In the sample analyzer of Embodiment 4, the low load polishing device 19 has an air blow mechanism 37 .

FIG. 17 is a diagram showing the procedure of sample analysis by the sample analyzer of the fourth embodiment.

The sample analysis procedure of Embodiment 4 differs from the sample analysis procedure of Embodiment 1 shown in FIG. 5 in the following points.

Steps S201 to S206 are executed in the same manner as in the first embodiment.

After step S206, in step S301, the sample stage 13 on which the polished sample 11 is set is blown by an air gun (not shown) in the air blow mechanism 37 and cleaned.

After that, as in the first embodiment, in step S207, the sample 11 is conveyed on the sample stage drive rail 12, carried out from the low-load polishing device 19, and introduced again into the laser non-contact three-dimensional shape measuring device 10. be done.

According to the fourth embodiment, it is possible to prevent errors in post-processing shape measurement data, errors in Fourier transform infrared spectroscopic analysis data, and contamination of the sample stage drive rail due to processing scraps. As a result, it is possible to improve the accuracy of the data and to maintain the equipment.

Embodiment 5.
The configuration of the sample analyzer of Embodiment 5 is the same as that of the sample analyzer of Embodiment 1 shown in FIG.

FIG. 18 is a diagram showing the procedure of sample analysis by the sample analyzer of the fifth embodiment.

A series of flow from shape measurement, polishing, shape measurement, and analysis in the fifth embodiment is the same as in the first embodiment. That is, steps S201 to S212 are executed as in the first embodiment. The sample analysis procedure of the fifth embodiment differs from the sample analysis procedure of the first embodiment shown in FIG. 5 in the following points.

When step S212 ends, the analysis of the single surface is completed. In step S501, the numerical calculation device 17 outputs the result of the depth-degradation degree correlation data of the single surface to the monitor 18, and at the same time, the numerical calculation device 17 In the storage area included in , the deterioration degree distribution data of a single plane with a depth d(1) is stored.

The sample is carried to the low-load polishing device 19 by the sample stage 13 again. The numerical calculation device 17 stores a set value n of the number of repetitions and a set value Δd of the thickness of the sample to be polished each time.

Thereafter, step S206 of polishing by the set thickness Δd each time, step S208 of measuring the shape of the sample after polishing, step S209 of calculating the polishing depth of the sample, and spectroscopic analysis. Step S211 to be executed and step S212 to analyze the characteristics of the sample are repeated a set number of times n. As a result, the characteristics of the sample 11 at a plurality of depths d(1) to d(n) of the polishing process of the sample 11, that is, deterioration degree distribution data are obtained.

At the stage when the set number of analyzes is completed, the numerical calculation device 17 performs reconstruction as four-dimensional data based on the stored distribution data (x, y, E) of the degree of deterioration E of each z-plane. . The analysis results are displayed by displaying E in a color scale, plotting three-dimensional coordinates, or making slice images.

In the first embodiment, the correlation data (d, E) of the degree of deterioration E with respect to the depth d is acquired based on the data at each point in the plane at different depths, but according to the fifth embodiment, , it becomes possible to more precisely acquire correlation data of the degree of deterioration in the depth direction at each point on the surface of a curved surface-shaped sample. Distinguishing whether deterioration occurs at a single point due to the influence of foreign matter, or only at a certain depth of the sample, when specific deterioration is observed at a certain point as a result of analysis. becomes possible. In particular, it is possible to accurately acquire deterioration information of a sample in which deterioration distribution occurs not only in the depth direction but also in the surface direction.

It should be considered that the embodiments disclosed this time are illustrative in all respects and not restrictive. The scope of the present disclosure is indicated by the scope of claims rather than the above description, and is intended to include all modifications within the scope and meaning of equivalents of the scope of claims.

Reference Signs List 1,2 film, 3 base material, 10 non-contact three-dimensional shape measuring device, 11 sample, 12 sample stage drive rail, 13 sample stage, 15 keyboard, 16 mouse, 17 numerical operation device, 18 monitor, 19 low weight polishing device , 20 Fourier transform infrared spectroscopic analyzer, 23 processing condition instruction display frame, 24 predicted shape display frame after processing, 25 predicted shape plan view display frame after processing, 26 predicted shape front view display frame after processing, 27 predicted shape after processing Side view display frame 28 Three-dimensional view of sample shape before processing 30 Three-dimensional view of sample shape after processing 31 Predicted shape plan view after processing 32 Predicted shape after processing Front view 33 Predicted shape side view after processing 34 Processing Parameter display frame 35 Post-machining depth distribution display frame 36 Post-machining depth distribution display frame 37 Air blow mechanism.

Claims (12)

a shape measuring device for measuring the shape of a sample;
a low-load polishing device for polishing the surface of the sample;
a spectroscopic analysis device that performs spectroscopic analysis of the processed surface of the sample;
and a computing device for analyzing the characteristics of the sample at the depth of polishing of the sample based on the measurement result of the shape of the sample and the result of the spectroscopic analysis. 2. The sample analyzer according to claim 1, wherein said spectroscopic analyzer performs Fourier transform infrared spectroscopic analysis of the processed surface of said sample. 3. The sample analyzer of claim 2, wherein said arithmetic unit identifies peak intensities of specific binding states within a Fourier transform infrared spectroscopy spectrum. a sample stage on which the sample is placed;
A sample stage drive rail for transporting the sample stage,
4. The sample analyzer according to any one of claims 1 to 3, wherein said sample stage is introduced into and carried out of said shape measuring device, said low-load polishing device, and said spectroscopic analysis device by said sample stage drive rail. . The sample analyzer according to any one of claims 1 to 4, wherein said low-load polishing device includes an air blow mechanism for cleaning the processed surface of said sample after polishing the surface of said sample. a display device;
an input device for accepting user input,
The computing device displays the shape of the sample before processing and the processed surface on the display device,
According to the user's input from the input device, the position and orientation of the processing surface are changed, and the predicted shape of the sample after processing according to the processing surface is displayed on the display device. A sample analyzer according to any one of claims 1 to 3. measuring the shape of the sample before polishing;
polishing the sample with a low load;
measuring the shape of the sample after polishing;
calculating the polishing depth of the sample based on the shape of the sample before polishing and the shape of the sample after polishing;
performing a spectroscopic analysis of the working surface of the sample;
and analyzing the characteristics of the sample at the depth of polishing of the sample based on the result of the spectroscopic analysis. 8. The method of analyzing a sample according to claim 7, wherein performing spectroscopic analysis comprises performing Fourier transform infrared spectroscopic analysis of a working surface of said sample. 9. The method of analyzing a sample according to claim 8, wherein analyzing the properties of the sample comprises identifying peak intensities of particular binding states in a Fourier transform infrared spectroscopy spectrum. The polishing step includes:
Predicting the shape of the sample when the polishing process is stopped when a predetermined time has elapsed during the time of polishing the sample;
polishing the sample according to processing conditions input by a user, and stopping the polishing when the predetermined time has elapsed;
measuring the shape of the sample when it stops;
a step of correcting the processing conditions so as to obtain the post-processing shape input by the user based on the predicted shape of the sample and the measured shape of the sample;
The sample analysis method according to any one of claims 7 to 9, comprising the step of performing polishing processing of said sample according to said modified processing conditions. The sample analysis method according to any one of claims 7 to 10, further comprising the step of cleaning the processed surface of the sample with an air blow mechanism after polishing the sample. the step of polishing, the step of measuring the shape of the sample after the polishing, the step of calculating the polishing depth of the sample, the step of performing the spectroscopic analysis, and the analysis of the characteristics of the sample. 12. The sample analysis method according to any one of claims 7 to 11, wherein the characteristics of the sample at multiple depths of polishing of the sample are obtained by repeating the steps of and a plurality of times.

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