# US 10,410,825 B2 · Electron probe microanalyzer and storage medium

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- Number: US 10,410,825 B2
- Document ID: US10410825B2
- Status: Granted
- Kind: B2
- Application number: 15/991,034
- Filed: 2018-05-29
- Published: 2019-01-03
- Granted: 2019-09-10
- Earliest claimed: 2017-06-30
- Assignees: Shimadzu Corporation
- Applicants: Shimadzu Corporation
- Inventors: Hiroshi Sakamae
- Web page: https://patentgrep.com/patent/US10410825B2

## CPC

- H01J 37/256: using scanning beams
- G01N 23/2252: Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
- G01N 2223/402: mapping distribution of elements
- G01N 2223/418: electron microscope
- G01N 2223/605: phases
- H01J 2237/2442: Energy-dispersive (Si-Li type) spectrometer
- H01J 2237/24425: Wavelength-dispersive spectrometer
- H01J 2237/24571: Measurements of non-electric or non-magnetic variables
- H01J 2237/2485: Electric or electronic means
- H01J 2237/2561: electron
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

An EDS 5 acquires first spectrum data by detecting an X-ray generated from a sample. A WDS 6 acquires second spectrum data by detecting the X-ray generated from the sample. A phase distribution map generation processing unit 11 generates a phase distribution map of a substance of the sample in a measurement region, on the basis of the first spectrum data acquired with respect to each pixel in the measurement region on a sample surface. A composition information acquisition processing unit 13 acquires element composition information of each phase, on the basis of the second spectrum data acquired with respect to a position on the sample corresponding to a representative pixel in the measurement region corresponding to each of the phases of the phase distribution map.

## Claims

### Claim 1

An electron probe microanalyzer, comprising:
an electron probe irradiation unit generating an X-ray by irradiating a sample with an electron probe;
an energy dispersive X-ray spectrometer acquiring first spectrum data by detecting the X-ray generated from the sample;
a wavelength dispersive X-ray spectrometer acquiring second spectrum data by detecting the X-ray generated from the sample;
a phase distribution map generation processing unit generating a phase distribution map of a substance of the sample in a measurement region, on the basis of the first spectrum data acquired with respect to each pixel in the measurement region on a sample surface; and
a composition information acquisition processing unit acquiring element composition information of each phase, on the basis of the second spectrum data acquired with respect to a position on the sample corresponding to a representative pixel in the measurement region corresponding to each of the phases of the phase distribution map.

### Claim 2 (depends on 1)

The electron probe microanalyzer according to claim 1, further comprising:
a display image generation processing unit generating a display image by reflecting the element composition information of each of the phases acquired by the composition information acquisition processing unit on each of the phases of the phase distribution map.

### Claim 3 (depends on 1)

The electron probe microanalyzer according to claim 1, further comprising:
an X-ray intensity map generation processing unit generating an X-ray intensity map by adjusting a peak wavelength condition of the wavelength dispersive X-ray spectrometer with respect to each of the detected elements, on the basis of the element composition information of each of the phases acquired by the composition information acquisition processing unit, and by measuring an X-ray intensity of each of the pixels in the measurement region.

### Claim 4 (depends on 3)

The electron probe microanalyzer according to claim 3, further comprising:
an average value calculation processing unit calculating an average value of X-ray intensities of a peak wavelength with respect to a pixel in a range of each of the phases, on the basis of the X-ray intensity map; and
an average element concentration calculation processing unit calculating an average element concentration of each of the phases by comparing the average value of the X-ray intensities of the peak wavelength calculated by the average value calculation processing unit with an X-ray intensity of a peak wavelength in a case where a concentration is known.

### Claim 5 (depends on 4)

The electron probe microanalyzer according to claim 4,
wherein the X-ray intensity map generation processing unit generates an X-ray intensity map of a peak wavelength and an X-ray intensity map of a background wavelength by adjusting a peak wavelength condition and a background wavelength condition of the wavelength dispersive X-ray spectrometer with respect to each of the detected elements, on the basis of the element composition information of each of the phases acquired by the composition information acquisition processing unit, and by measuring an X-ray intensity of each of the peak wavelength and the background wavelength of each of the pixels in the measurement region,
the average value calculation processing unit calculates an average value of the X-ray intensities of each of the peak wavelength and the background wavelength with respect to the pixel in the range of each of the phases, on the basis of the X-ray intensity map of the peak wavelength and the X-ray intensity map of the background wavelength, and
the average element concentration calculation processing unit calculates the average element concentration of each of the phases by comparing a result obtained by subtracting the average value of the X-ray intensities of the background wavelength from the average value of the X-ray intensities of the peak wavelength calculated by the average value calculation processing unit with a height of a peak in a case where a concentration is known.

### Claim 6

A storage medium storing a data processing program used for an electron probe microanalyzer, which includes an electron probe irradiation unit generating an X-ray by irradiating a sample with an electron probe, an energy dispersive X-ray spectrometer acquiring first spectrum data by detecting the X-ray generated from the sample, and a wavelength dispersive X-ray spectrometer acquiring second spectrum data by detecting the X-ray generated from the sample, the medium allowing a computer to function as:
a phase distribution map generation processing unit generating a phase distribution map of a substance of the sample in a measurement region, on the basis of the first spectrum data acquired with respect to each pixel in the measurement region on a sample surface; and
a composition information acquisition processing unit acquiring element composition information of each phase, on the basis of the second spectrum data acquired with respect to a position on the sample corresponding to a representative pixel in the measurement region corresponding to each of the phases of the phase distribution map.

### Claim 7 (depends on 6)

The storage medium according to claim 6, further allowing the computer to function as:
a display image generation processing unit generating a display image by reflecting the element composition information of each of the phases acquired by the composition information acquisition processing unit on each of the phases of the phase distribution map.

### Claim 8 (depends on 6)

The storage medium according to claim 6, further allowing the computer to function as:
an X-ray intensity map generation processing unit generating an X-ray intensity map by adjusting a peak wavelength condition of the wavelength dispersive X-ray spectrometer with respect to each of the detected elements, on the basis of the element composition information of each of the phases acquired by the composition information acquisition processing unit, and by measuring an X-ray intensity of each of the pixels in the measurement region.

### Claim 9 (depends on 8)

The storage medium according to claim 8, further allowing the computer to function as:
an average value calculation processing unit calculating an average value of X-ray intensities of a peak wavelength with respect to a pixel in a range of each of the phases, on the basis of the X-ray intensity map; and
an average element concentration calculation processing unit calculating an average element concentration of each of the phases by comparing the average value of the X-ray intensities of the peak wavelength calculated by the average value calculation processing unit with an X-ray intensity of a peak wavelength in a case where a concentration is known.

### Claim 10 (depends on 9)

The storage medium according to claim 9,
wherein the X-ray intensity map generation processing unit generates an X-ray intensity map of a peak wavelength and an X-ray intensity map of a background wavelength by adjusting a peak wavelength condition and a background wavelength condition of the wavelength dispersive X-ray spectrometer with respect to each of the detected elements, on the basis of the element composition information of each of the phases acquired by the composition information acquisition processing unit, and by measuring an X-ray intensity of each of the peak wavelength and the background wavelength of each of the pixels in the measurement region,
the average value calculation processing unit calculates an average value of the X-ray intensities of each of the peak wavelength and the background wavelength with respect to the pixel in the range of each of the phases, on the basis of the X-ray intensity map of the peak wavelength and the X-ray intensity map of the background wavelength, and
the average element concentration calculation processing unit calculates the average element concentration of each of the phases by comparing a result obtained by subtracting the average value of the X-ray intensities of the background wavelength from the average value of the X-ray intensities of the peak wavelength calculated by the average value calculation processing unit with a height of a peak in a case where a concentration is known.