IP Library › Granted Patent US 12,399,141
Granted Patent B2
US 12,399,141 · App. 18/124,585 · Granted Aug 26, 2025

Damage measurement method, apparatus and program, and x-ray diffraction apparatus

Inventors: Ryouichi Yokoyama (Tokyo, JP); Kazuhiko Omote (Tokyo, JP); Daisuke Kobayashi (Aichi, JP)
Assignees: RIGAKU CORPORATION; CHUBU ELECTRIC POWER COMPANY, INCORPORATED
G01N23/2055
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,399,141
App. No.
18/124,585
Granted
Aug 26, 2025
Kind
B2
Abstract

A damage measurement technique capable of measuring damage of a sample in a single crystal state, regardless of the surrounding condition, includes irradiating microbeam white X-rays to a sample in a single crystal state, diffraction of a spot generated by the irradiation is detected, a coefficient on variance of an intensity distribution in a specific direction in the detected diffraction spot is calculated, and a damaged state of the sample is specified based on the calculated coefficient.

Claims (82)

1. A damage measurement method, comprising:

irradiating microbeam white X-rays with 70 keV or higher to a sample in a single crystal state,

detecting a diffraction spot generated by the irradiation,

calculating a coefficient on variance of an intensity distribution in a specific direction in the detected diffraction spot, and

specifying a damage state of the sample based on the calculated coefficient,

wherein the sample is a metal material having a dendritic structure, and

the detected diffraction spot occurs at 100 μm or more below the surface over the sample.

2. The damage measurement method according to claim 1 ,

wherein the damage state is defined by a degree of damage and a direction of damage.

3. The damage measurement method according to claim 1 ,

wherein the sample is a single crystal material, a directionally solidified material or a polycrystalline material.

4. The damage measurement method according to claim 1 ,

wherein the irradiated white X-ray is incident at 90° with respect to a surface of the sample, and

the diffraction spot is detected by a transmission method, the transmission method has a predetermined relationship between an incident X-ray and a diffracted X-ray.

5. The damage measurement method according to claim 1 ,

wherein the sample is coated with a polycrystalline coating.

6. The damage measurement method according to claim 1 ,

wherein the white X-ray to be irradiated is formed into a focal size at a sample position equivalent to a grain size of a subcrystalline grain in the sample.

7. An X-ray diffraction apparatus used for the damage measurement method according to claim 1 , comprising:

an X-ray irradiator configured to irradiate microbeam white X-rays to a sample,

a sample stage for mounting the sample, and

an X-ray detector configured to detect X-rays diffracted by the sample, wherein the sample is in a single crystal state.

8. A damage measurement method 3 , comprising:

irradiating microbeam white X-rays to a sample in a single crystal state;

detecting a diffraction spot generated by the irradiation, calculating a coefficient on variance of an intensity distribution in a specific direction in the detected diffraction spot; and

specifying a damage state of the sample based on the calculated coefficient:

wherein an energy of the irradiated white X-ray is set such that a transmittance at a position in a depth of 7 mm in the sample from an incident position on the sample is 1/e or higher.

9. A damage measurement method, comprising:

irradiating microbeam white X-rays to a sample in a single crystal state;

detecting a diffraction spot generated by the irradiation, calculating a coefficient on variance of an intensity distribution in a specific direction in the detected diffraction spot; and

specifying a damage state of the sample based on the calculated coefficient;

wherein the irradiated white X-rays have a focal spot size of 150 μm or more and 500 μm or less at a sample position.

10. A damage measurement method, comprising:

irradiating microbeam white X-rays to a sample in a single crystal state;

detecting a diffraction spot generated by the irradiation, calculating a coefficient on variance of an intensity distribution in a specific direction in the detected diffraction spot; and

specifying a damage state of the sample based on the calculated coefficient;

wherein a collimator forms a divergence angle of the white X-rays and wherein the divergence angle of the white X-ray is 0.2° or less.

11. An X-ray diffraction apparatus, comprising:

an X-ray irradiator configured to irradiate microbeam white X-rays to a sample,

a sample stage for mounting the sample, and

an X-ray detector configured to detect X-rays diffracted by the sample,

wherein the sample is in a single crystal state, and

wherein the X-ray irradiator includes a collimator for forming a divergence angle of the irradiated white X-rays to 0.2° or less.

12. A damage measurement apparatus comprising:

processing circuitry configured to

calculate a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays with 70 keV or higher to a sample in a single crystal state, and

specify a damage state of the sample based on the calculated coefficient,

wherein the sample is a metal material having a dendritic structure, and

the detected diffraction spot occurs at 100 μm or more below the surface over the sample.

13. A non-transitory computer readable recording medium having recorded thereon a damage measurement program causing a computer to execute a method, the method comprising:

calculating a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays with 70 keV or higher to a sample in a single crystal state, and

specifying a damage state of the sample based on the calculated coefficient,

wherein the sample is a metal material having a dendritic structure, and

the detected diffraction spot occurs at 100 μm or more below the surface over the sample.

14. A damage measurement apparatus comprising:

processing circuitry configured to

calculate a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state, and

specify a damage state of the sample based on the calculated coefficient,

wherein an energy of the irradiated white X-ray is set such that a transmittance at a position in a depth of 7 mm in the sample from an incident position on the sample is 1/e or higher.

15. A damage measurement apparatus comprising:

processing circuitry configured to

calculate a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state, and

specify a damage state of the sample based on the calculated coefficient,

wherein the irradiated white X-rays have a focal spot size of 150 μm or more and 500 μm or less at a sample position.

16. A damage measurement apparatus comprising:

processing circuitry configured to

calculate a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state, and

specify a damage state of the sample based on the calculated coefficient,

wherein a collimator forms a divergence angle of the white X-rays, and

wherein the divergence angle of the white X-ray is 0.2° or less.

17. A non-transitory computer readable recording medium having recorded thereon a damage measurement program causing a computer to execute a method, the method comprising:

calculating a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state; and

specifying a damage state of the sample based on the calculated coefficient,

wherein an energy of the irradiated white X-ray is set such that a transmittance at a position in a depth of 7 mm in the sample from an incident position on the sample is 1/e or higher.

18. A non-transitory computer readable recording medium having recorded thereon a damage measurement program causing a computer to execute a method, the method comprising:

calculating a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state; and

specifying a damage state of the sample based on the calculated coefficient,

wherein the irradiated white X-rays have a focal spot size of 150 μm or more and 500 μm or less at a sample position.

19. A non-transitory computer readable recording medium having recorded thereon a damage measurement program causing a computer to execute a method, the method comprising:

calculating a coefficient on variance of an intensity distribution in a specific direction in a diffraction spot based on intensity data acquired by irradiating microbeam white X-rays to a sample in a single crystal state, and

specifying a damage state of the sample based on the calculated coefficient,

wherein a collimator forms a divergence angle of the white X-rays, and wherein the divergence angle of the white X-ray is 0.2° or less.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 22, 2023
From: YOKOYAMA, RYOUICHI; OMOTE, KAZUHIKO; KOBAYASHI, DAISUKE
To: RIGAKU CORPORATION; CHUBU ELECTRIC POWER COMPANY, INCORPORATED
Reel/Frame 063055/0660 →
Priority Claims (1)
JP 2022-046746 · Mar 23, 2022 · national
Continuity (1)
Related Publication 20230304948A1 · Sep 28, 2023
References Cited (22)
US 5235523A · Karen · 1993 [cited by examiner]
US 6005913A · Zombo · 1999 [cited by examiner]
US 7212607B1 · Rao · 2007 [cited by examiner]
US 7796726B1 · Gendreau · 2010 [cited by examiner]
US 9129715B2 · Adler · 2015 [cited by examiner]
US 11448603B1 · Norman · 2022 [cited by examiner]
US 20050074092A1 · Borgstahl · 2005 [cited by examiner]
US 20050139772A1 · Hasegawa · 2005 [cited by examiner]
US 20090103680A1 · Park · 2009 [cited by examiner]
US 20100239068A1 · Belassel · 2010 [cited by examiner]
US 20110164729A1 · Kikuchi · 2011 [cited by examiner]
US 20150362500A1 · Anker · 2015 [cited by examiner]
US 20190003988A1 · Solarz · 2019 [cited by examiner]
US 20190120753A1 · Prater · 2019 [cited by examiner]
US 20200225171A1 · Griffiths · 2020 [cited by examiner]
US 20210025835A1 · Griffiths · 2021 [cited by examiner]
US 20220026377A1 · Yamamoto · 2022 [cited by examiner]
JP 4719836B2 · 2011 [cited by applicant]
JP 5324735B2 · 2013 [cited by applicant]
JP 2020159850A · 2020 [cited by examiner]
Translation of JP-2020159850 (Year: 2020). [cited by examiner]
Japanese Office Action issued Apr. 22, 2025 in corresponding Japanese Patent Application No. 2022-046746, 6 pages. [cited by applicant]