Method of measuring crosslink densities in sulfur-containing polymer composite material

Patent metadata

Field	Value
Publication number	US-9874530-B2
Application number	US-201514825642-A
Country	US
Kind code	B2
Filing date	Aug 13, 2015
Priority date	Sep 11, 2014
Publication date	Jan 23, 2018
Grant date	Jan 23, 2018

Abstract

Provided is an evaluation method that provides detailed information on the crosslink densities in sulfur-containing polymer composite materials. The present invention relates to a method of measuring crosslink densities in a sulfur-containing polymer composite material, the method including: a measurement step of irradiating the sulfur-containing polymer composite material with high intensity X-rays and measuring an X-ray absorption spectrum of the composite material while varying the energy of the X-rays; a visualization step of determining the three-dimensional structure of sulfur atoms in the sulfur-containing polymer composite material by the reverse Monte Carlo method from the X-ray absorption spectrum; and a calculation step of calculating, from the three-dimensional structure of sulfur atoms, a crosslink density for each number of sulfur atoms bonded.

First claim

The invention claimed is:

1. A method of measuring crosslink densities in a sulfur-containing polymer composite material, the method comprising:
a measurement step of irradiating the sulfur-containing polymer composite material with high intensity X-rays and measuring an X-ray absorption spectrum of the composite material while varying the energy of the X-rays;
a visualization step of determining a three-dimensional structure of sulfur atoms in the sulfur-containing polymer composite material by a reverse Monte Carlo method from the X-ray absorption spectrum;
a calculation step of calculating, from the three-dimensional structure of sulfur atoms, a crosslink density for each number of sulfur atoms bonded; and
a determination step of determining the sulfur crosslinked structure of the sulfur-containing polymer composite material based on the calculated crosslink density for each number of sulfur atoms bonded.

2. The method according to claim 1 ,
wherein, in the measurement step, the composite material is scanned with the X-rays in an energy range of 2300 to 4000 eV to measure an X-ray absorption spectrum near the K-shell absorption edge of sulfur.

3. The method according to claim 1 ,
wherein, in the measurement step, the X-rays have a number of photons of 10 7 photons/s or more, and a brilliance of 10 10 photons/s/mrad 2 /mm 2 /0.1% bw or higher.

Assignees

• Sumitomo Rubber Ind

Inventors

• Kaneko Fusae
• Kishimoto Hiroyuki

Classifications

• G01N23/085

  X-ray absorption fine structure [XAFS], e.g. extended XAFS [EXAFS] · CPC title

• G01N2223/203

  synchrotron · CPC title

• G01N23/087 Primary

  using polyenergetic X-rays · CPC title

• G01N33/445 Primary

  Rubber · CPC title

• G01N23/063

  Physics · mapped topic