# US 7,609,812 B2 · Pore- or particle-size distribution measurement apparatus

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- Number: US 7,609,812 B2
- Document ID: US7609812B2
- Status: Granted
- Kind: B2
- Application number: 10/540,980
- Filed: 2003-12-26
- Published: 2007-01-11
- Granted: 2009-10-27
- Earliest claimed: 2002-12-27
- Assignees: Technos Co., Ltd.
- Inventors: Shinichi Terada
- Web page: https://patentgrep.com/patent/US7609812B2

## CPC

- G01N 23/203: Measuring back scattering
- G01N 15/0205: by optical means
- G01N 2015/0846: {by use of radiation, e.g. transmitted or reflected light}
- G01N 2015/086: {of films, membranes or pellicules}
- 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

A pore- or particle-size distribution measurement apparatus is provided. When the size of a pore existing in a porous insulator film or the size of a particle in a thin film is measured, a specimen having the insulator film on the surface of a substrate is irradiated, from the surface side thereof, with X-rays at a specified incident angle larger than the total reflection critical angle of the insulator film but less than 1.3 times the total reflection critical angle of the substrate. In the irradiated X-rays, among components exiting from the insulator film without entering the pore and scattering of reflection component of the X-rays reflected on the surface of the substrate after having entered the insulator film, the scattered component whose exit angle is larger than that of a component of the reflection component which exits from the insulator film without entering the pore is detected.

## Claims

### Claim 1

A pore or particle-size distribution measurement method for measuring size distribution of pores or particles existing within a porous insulator film formed on a surface of a substrate, comprising:
only irradiating the insulator film with X-rays from the insulator film's surface side at a single incident angle which is set to be larger than a total-reflection critical angle of the insulator film and larger than 1.0 times a total-reflection critical angle of the substrate but less than 1.3 times a total-reflection critical angle of the substrate; and
detecting among reflection components reflected on the surface of the substrate of the X-rays which have entered the insulator film, reflection components exiting from the insulator film after entering the pore or particle and scattering, having an exit angle larger than that of reflection components which exit from the insulator film without entering the pore or particle.

### Claim 2 (depends on 1)

The pore or particle-size distribution measurement method of claim 1, wherein the X-rays are generated by a line focus X-ray tube, and a parallel light flux, of the generated X-rays, composed of mutually-parallel components of a specific direction lying in a specific wavelength band is selected to enter the measurement target object at the incident angle,
and wherein only a specific-direction component of the X-rays coming from the measurement target object is allowed to pass through a slit, and the X-rays having passed through the slit is detected by a position-sensitive X-ray detector.

### Claim 3 (depends on 2)

The pore or particle-size distribution measurement method of claim 2, wherein a specific specular reflection component is prevented from entering a detection surface of the position-sensitive X-ray detector by an X-ray blocking plate, the specular reflection component being derived from the X-rays which are reflected from the surface of the substrate after having entered the insulator film and exited from the insulator film without entering the pore or particle.

### Claim 4 (depends on 1)

The pore or particle-size distribution measurement method of claim 1, wherein the X-rays are generated by a point focus X-ray tube, and an X-ray beam, of the generated X-rays, composed of specific-direction components which are mutually parallel and exist in a specific wavelength band is selected to enter the measurement target object at the incident angle,
and wherein the X-rays coming from the measurement target object are detected by a position-sensitive X-ray detector.

### Claim 5 (depends on 4)

The pore or particle-size distribution measurement method of claim 4, wherein a specific specular reflection component is prevented from entering a detection surface of the position-sensitive X-ray detector by an X-ray blocking plate, the specular reflection component being derived from the X-rays which are reflected from the surface of the substrate after having entered the insulator film and exited from the insulator film without entering the pore or particle.

### Claim 6 (depends on 1)

The pore or particle-size distribution measurement method of claim 1, wherein the X-rays are generated by an X-ray generating source and the generated X-rays are converged and made incident onto the measurement target object at the incident angle,
and wherein the X-rays coming from the measurement target object are detected by a position-sensitive X-ray detector.

### Claim 7 (depends on 6)

The pore or particle-size distribution measurement method of claim 6, wherein an area of incident of the X-rays on the measurement target object is regulated by an X-ray irradiation range regulatory plate that is arranged immediately above a position of incidence at a predetermined spacing.