Sample holder for detection of hydrogen permeation and hydrogen permeation and diffusion path observation device

Patent metadata

Field	Value
Publication number	US-12535451-B2
Application number	US-202118028862-A
Country	US
Kind code	B2
Filing date	Aug 19, 2021
Priority date	Sep 29, 2020
Publication date	Jan 27, 2026
Grant date	Jan 27, 2026

Abstract

The sample holder 30 comprises: a holder body 31 for holding the sample 17 ; an electrolyte introduction chamber 31 b provided with an opening 31 c that opens to a measurement region 17 a of the sample; a retainer plate 33 , which is provided with a through-hole 33 a corresponding to the measurement region of the sample, for retaining the sample from the electron source side around the through-hole to sandwich the sample airtightly with the holder body; double sealing members 32 arranged between the surface of the holder body and the sample so as to surround the periphery of the measurement region of the sample; a differential exhaust pipe 35 , which opens to a space between the sealing members on the surface of the holder body, for exhaust the space through the opening; and electrodes 19 for electrolysis made up of a bias application electrode 19 a and an opposing electrode 36.

First claim

What is claimed is:

1 . A sample holder for detection of hydrogen permeation, comprising:
a holder body to be mounted to a scanning electron microscope for holding a sample to detect hydrogen ions generated by an electron beam irradiation; an electrolyte introduction chamber provided with an opening that opens to a measurement region of the sample; a retainer plate, which is provided with a through-hole corresponding to the measurement region of the sample, for retaining the sample from an electron source side of the scanning electron microscope around the through-hole to hold the sample airtightly against the holder body; double sealing members arranged between a surface of the holder body and the sample so as to surround the periphery of the measurement region of the sample; a differential exhaust pipe, which opens to a space between the double sealing members on the surface of the holder body, for exhaust from the opening; and electrodes made up of a bias application electrode and an opposing electrode for electrolysis, wherein the retainer plate is made of a conductive material as the bias application electrode, the opposing electrode is disposed within the electrolyte introduction chamber, or the holder body is made to serve as the opposing electrode, and a voltage is applied between the bias application electrode and the opposing electrode to introduce hydrogen from the electrolyte into the sample.

2 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein the electrolyte introduction chamber is comprised of an opening that opens to the surface of the holder body and a hollow part that extends from the opening toward inside of the holder body, and the opposing electrode is disposed inside the hollow part.

3 . The sample holder for detection of hydrogen permeation as set forth in claim 2 , wherein an internal surface of the hollow part is provided with an insulation and an anticorrosion coating.

4 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein the electrolyte introduction chamber is defined by a back surface of the sample, an inner sealing member of the double sealing members, and the surface of the holder body.

5 . The sample holder for detection of hydrogen permeation as set forth in claim 4 , wherein the opposing electrode is connected to the holder body.

6 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein a feed pipe for supplying electrolyte to the electrolyte introduction chamber and an exhaust pipe for discharging the electrolyte are provided.

7 . The sample holder for detection of hydrogen permeation as set forth in claim 6 , wherein the electrolyte is supplied through the feed pipe and at the same time used electrolyte is discharged through the exhaust pipe during electrolysis.

8 . The sample holder for detection of hydrogen permeation as set forth in claim 6 , wherein air bubbles generated during electrolysis are discharged through the exhaust pipe.

9 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein the holder body, the opposing electrode, the electrolyte introduction chamber, and sealing members are respectively made of a material that can endure a baking process.

10 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein the holder body is made of a conductive material, serves as the opposing electrode, and is electrically insulated from the retainer plate.

11 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein
the hollow part opens to a back surface side of the holder body, and an open end of the back surface side is sealed by a cover member via an ultrahigh-vacuum seal, a vessel that serves as the electrolyte introduction chamber is supported by an elastic member on a front side of the cover member, and an open top end of the vessel abuts against a back surface of the sample within the sealed hollow part by a biasing force of the elastic member.

12 . The sample holder for detection of hydrogen permeation as set forth in claim 1 , wherein an opening is absent from the space other than the opening of the differential exhaust pipe.

13 . A hydrogen permeation and diffusion path observation device, comprising:
a scanning electron microscope for detecting secondary electrons generated by irradiating a sample with an electron beam within an analysis chamber; a sample holder for detection of hydrogen permeation that is mounted to the scanning electron microscope to hold the sample, the sample having a measurement region for detecting hydrogen ions generated by the electron beam irradiation, and a hydrogen ion detector for detecting hydrogen ions generated by the electron beam shot on hydrogen that is discharged to a surface from a back face of the sample held by the sample holder, wherein the sample holder comprises a holder body, a retainer plate for holding the sample from a surface side of the holder body, a differential exhaust pipe that opens to a space between sealing members on the surface of the holder body and communicates with outside, and electrodes made up of a bias application electrode and an opposing electrode for electrolyzing the electrolyte, the holder body comprises:
an electrolyte introduction chamber having an opening that opens at least to the measurement region of the sample;
electrolyte that fills the electrolyte introduction chamber up to a back surface of the sample; and
double sealing members disposed on a surface of the sample holder body so as to surround the periphery of the measurement region of the sample,
the retainer plate is provided with a through-hole that corresponds to the measurement region of the sample, presses down the sample from an electron source side around the periphery of the through-hole, and thus sandwiches the sample air-tightly between the sample holder and the double sealing members,
the entire electrolyte introduction chamber is sealed in a state where the electrolyte has been introduced to the electrolyte introduction chamber and the sample is mounted to the sample holder,
the retainer plate is made to serve as a bias application electrode, and the opposing electrode is disposed in the electrolyte introduction chamber, or the holder body is made to serve as the opposing electrode,
a voltage is applied between the bias application electrode and the opposing electrode to cause electrolysis to occur, and
by irradiating the hydrogen discharged to a surface from the back surface of the sample held by the sample holder with the electron beam, hydrogen ions generated by the electron beam are measured by the hydrogen ion detector.

14 . The hydrogen permeation and diffusion path observation device as set forth in claim 13 , wherein an opening is absent from the space other than the opening of the differential exhaust pipe.

Assignees

• Nat Inst Materials Science

Inventors

• Nakamura Akiko
• Yakabe Taro
• Miyauchi Naoya

Classifications

• G01N27/404 Primary

  Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid {, e.g. Clark-type oxygen sensors} · CPC title

• H01J2237/24585

  Other variables, e.g. energy, mass, velocity, time, temperature · CPC title

• H01J2237/2803

  characterised by the imaging method · CPC title

• H01J2237/2813

  characterised by the application · CPC title

• H01J2237/182

  Obtaining or maintaining desired pressure · CPC title