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

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.