ISO 19749:2021
Nanotechnologies — Measurements of particle size and shape distributions by scanning electron microscopy
This document specifies methods of determining nanoparticle size and shape distributions by acquiring and evaluating scanning electron microscope images and by obtaining and reporting accurate results.
NOTE 1 This document applies to particles with a lower size limit that depends on the required uncertainty and on the suitable performance of the SEM, which is to be proven first -according to the requirements described in this document.
NOTE 2 This document applies also to SEM-based size and shape measurements of larger than nanoscale particles.
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
3.1 General terms
3.2 Core terms: image analysis
3.3 Core terms: statistical symbols and definitions
3.4 Core terms: measurands and descriptors
3.5 Core terms: metrology
3.6 Core terms: scanning electron microscopy
4 General principles
4.1 SEM imaging
4.2 SEM image-based particle size measurements
4.3 SEM image-based particle shape measurements
5 Sample preparation
5.1 Sample preparation fundamental information
5.2 General recommendations
5.3 Ensuring good sampling of powder or dispersion-in-liquid raw materials
5.3.1 Powders
5.3.2 Nanoparticle dispersions in liquids
5.4 Ensuring representative dispersion
5.5 Nanoparticle deposition on a substrate
5.5.1 General
5.5.2 Nanoparticle deposition on wafers and chips of silicon or other materials
5.5.3 Nanoparticle deposition on TEM grids
5.6 Number of samples to be prepared
5.7 Number of particles to be measured for particle size determination
5.8 Number of particles to be measured for particle shape determination
6 Qualification of the SEM for nanoparticle measurements
7 Image acquisition
7.1 General
7.2 Setting suitable image magnification and pixel resolution
8 Particle analysis
8.1 Particle analysis fundamental information
8.2 Individual particle analysis
8.3 Automated particle analysis
8.4 Automated particle analysis procedure example
9 Data analysis
9.1 General
9.2 Raw data screening: detecting touching particles, artefacts and contaminants
9.3 Fitting models to data
9.4 Assessment of measurement uncertainty
9.4.1 General
9.4.2 Example: Measurement uncertainty for particle size measurements
9.4.3 Bivariate analysis
10 Reporting the results
Annex A (normative) Qualification of the SEM for nanoparticle measurements
Annex B (informative) Cross-sectional titanium dioxide samples preparation
Annex C (informative) Case study on well-dispersed 60 nm size silicon dioxide nanoparticles
Annex D (informative) Case study on 40 nm size titanium dioxide nanoparticles
Annex E (informative) Example for extracting particle size results of SEM-based nanoparticle measurements using ImageJ
Annex F (informative) Effects of some image acquisition parameters and thresholding methods on SEM particle size measurements
Annex G (informative) Example for reporting results of SEM-based nanoparticle measurements
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
3.1 General terms
3.2 Core terms: image analysis
3.3 Core terms: statistical symbols and definitions
3.4 Core terms: measurands and descriptors
3.5 Core terms: metrology
3.6 Core terms: scanning electron microscopy
4 General principles
4.1 SEM imaging
4.2 SEM image-based particle size measurements
4.3 SEM image-based particle shape measurements
5 Sample preparation
5.1 Sample preparation fundamental information
5.2 General recommendations
5.3 Ensuring good sampling of powder or dispersion-in-liquid raw materials
5.3.1 Powders
5.3.2 Nanoparticle dispersions in liquids
5.4 Ensuring representative dispersion
5.5 Nanoparticle deposition on a substrate
5.5.1 General
5.5.2 Nanoparticle deposition on wafers and chips of silicon or other materials
5.5.3 Nanoparticle deposition on TEM grids
5.6 Number of samples to be prepared
5.7 Number of particles to be measured for particle size determination
5.8 Number of particles to be measured for particle shape determination
6 Qualification of the SEM for nanoparticle measurements
7 Image acquisition
7.1 General
7.2 Setting suitable image magnification and pixel resolution
8 Particle analysis
8.1 Particle analysis fundamental information
8.2 Individual particle analysis
8.3 Automated particle analysis
8.4 Automated particle analysis procedure example
9 Data analysis
9.1 General
9.2 Raw data screening: detecting touching particles, artefacts and contaminants
9.3 Fitting models to data
9.4 Assessment of measurement uncertainty
9.4.1 General
9.4.2 Example: Measurement uncertainty for particle size measurements
9.4.3 Bivariate analysis
10 Reporting the results
Annex A (normative) Qualification of the SEM for nanoparticle measurements
Annex B (informative) Cross-sectional titanium dioxide samples preparation
Annex C (informative) Case study on well-dispersed 60 nm size silicon dioxide nanoparticles
Annex D (informative) Case study on 40 nm size titanium dioxide nanoparticles
Annex E (informative) Example for extracting particle size results of SEM-based nanoparticle measurements using ImageJ
Annex F (informative) Effects of some image acquisition parameters and thresholding methods on SEM particle size measurements
Annex G (informative) Example for reporting results of SEM-based nanoparticle measurements
Bibliography