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GB/T 45114-2024: Nanotechnologies - Measurements of particle size and shape distributions by transmission electron microscopy
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Nanotechnologies - Measurements of particle size and shape distributions by transmission electron microscopy
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GB/T 45114-2024
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Basic data | Standard ID | GB/T 45114-2024 (GB/T45114-2024) | | Description (Translated English) | Nanotechnologies - Measurements of particle size and shape distributions by transmission electron microscopy | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G30 | | Classification of International Standard | 07.180 | | Word Count Estimation | 74,787 | | Date of Issue | 2024-12-31 | | Date of Implementation | 2025-07-01 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration | GB/T 45114-2024: Nanotechnologies - Measurements of particle size and shape distributions by transmission electron microscopy
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ICS 07.180
CCSG30
National Standard of the People's Republic of China
Nanotechnology Transmission electron microscopy measures nanometers
Particle size and shape distribution
(ISO 21363.2020,IDT)
Released on 2024-12-31
2025-07-01 Implementation
State Administration for Market Regulation
The National Standardization Administration issued
Table of Contents
Preface III
Introduction IV
1 Scope 1
2 Normative references 1
3 Terms, definitions and symbols 1
3.1 Particle core terminology 1
3.2 Image acquisition and analysis core terms 4
3.3 Statistical symbols and core terms 5
3.4 Core terms for measured quantities 6
3.5 Core terminology for measurement 9
3.6 Transmission Electron Microscopy Key Terms 10
3.7 Statistical symbols, measurands and parameters 11
4 User requirements for TEM measurement programs12
5 Sample preparation 13
5.1 Overview 13
5.2 Sample Source 13
5.3 Use of representative samples14
5.4 Reducing particle agglomeration during sample dispersion 14
5.5 Support membrane selection 14
6 Instrumental factors 15
6.1 Instrument Setup 15
6.2 Calibration 15
6.3 Setting up TEM operating conditions for calibration 17
7 Image acquisition 18
7.1 Overview 18
7.2 Setting the appropriate image magnification and pixel resolution 18
7.3 Minimum particle area 18
7.4 Counting the number of particles in size and shape distribution 19
7.5 Uniform background 19
7.6 Measurement steps 19
7.7 Adjusting the image acquisition scheme 20
8 Particle Analysis20
8.1 Overview 20
8.2 Single Particle Analysis 20
8.3 Automatic particle analysis 20
8.4 Example of an automated particle analysis program 21
9 Data Analysis 21
9.1 Overview 21
9.2 Raw Data Classification - Identification of Contact Particles, Unselected Particles, Artifacts and Contaminants 22
9.3 Data Quality Assessment - Repeatability, Inter-period Precision and Reproducibility 23
9.4 Fitting distribution to data 24
9.5 Measurement uncertainty of samples evaluated under repeatability, interim precision or reproducibility conditions 25
9.6 Bivariate Analysis 26
10 Report 26
Appendix A (Informative) Case Study Overview 30
Appendix B (Informative) Discrete Spherical Nanoparticles 32
Appendix C (Informative) Particle Size Mixture 34
Appendix D (Informative) Shape Mixture 43
Appendix E (Informative) Amorphous Aggregates 46
Appendix F (Informative) Nanocrystalline Aggregates 49
Appendix G (Informative) Nanofibers with Irregular Cross-Sections 52
Appendix H (Informative) Nanoparticles with Specific Crystal Habits 58
References 64
Foreword
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for standardization work Part 1.Structure and drafting rules for standardization documents"
Drafting.
This document is equivalent to ISO 21363.2020 "Nanotechnology - Measurement of nanoparticle size and shape distribution by transmission electron microscopy".
The following minimal editorial changes were made to this document.
---Added a note after Table 1;
---5.5 added notes;
--- The informative reference GB/T 21636-2021 replaces ISO 22309.2011;
--- Change "Classification (see 9.1)" in 7.7 to "Classification (see 9.2)" to make the clause number and content correspond;
--- Change "method (see 9.2)" in 9.2 to "method (see 9.4)" to make the clause number and content correspond;
--- When there is no parallel item in the note, change Note 1 to Note.
Please note that some of the contents of this document may involve patents. The issuing organization of this document does not assume the responsibility for identifying patents.
This document was proposed by the Chinese Academy of Sciences.
This document is under the jurisdiction of the National Nanotechnology Standardization Technical Committee (SAC/TC279).
This document was drafted by. China Institute of Metrology, Test Dog (Chengdu) Laboratory Testing Co., Ltd., Henan University of Science and Technology, Chalco
Technology Research Institute Co., Ltd., Beijing Academy of Science and Technology Analysis and Testing Institute (Beijing Physical and Chemical Analysis and Testing Center), Beijing Zhixin Micro
Electronic Technology Co., Ltd., Shandong Institute of Metrology, Tsinghua University Shenzhen International Graduate School, Shanghai Jiaotong University, Central South University,
Southwest University of Science and Technology, Nanjing Metrology Supervision and Inspection Institute.
The main drafters of this document are. Li Xu, Ren Lingling, Zhang Yi, Wang Yuting, Huang Lu, Lou Huafen, Mo Yongda, Cao Cong, Liu Weili, Li Shi, Ma Yongjun,
Wang Liying, Guo Xinqiu, Liu Junjie, Zhao Dongyan, Liang Xiaopeng, Lei Qian, Gao Sitian, Shi Yushu, Cui Lei, and Wang Yalei.
Introduction
Typically, nanoparticle measurements include, but are not limited to, particle size, shape, surface structure (or texture), and surface chemistry.
This paper focuses on discrete, agglomerated and aggregated nano-objects (objects that have at least one dimension).
Transmission electron microscopy is a technique used to measure the morphological properties of particles. particle size and shape distribution.
A standard measurement tool at the nanoscale that provides a two-dimensional projection image of particles. Measure and evaluate particle size and shape distribution at the nanoscale
General examples of sample preparation, instrument commissioning, image acquisition, particle analysis, data analysis, and reporting are presented in this document.
This paper reports on three discrete particle test samples.
The products are. spheres (gold nanospheres), bimodal mixtures of particle sizes (silica sol), and mixtures of particle shapes (gold nanorods and gold nanocubes).
The document reports two types of aggregates tested. amorphous alveolar aggregates (carbon black) and primary microcrystalline aggregates (titanium dioxide).
Methods for measuring low aspect ratio samples and nanoparticles with specific crystal orientations are given. Some of the case studies in this document are presented by New Materials and
Interlaboratory Comparisons (ILCs) are provided under the guidance of the Versailles Association for Standardization (VAMAS) [47].
This document considers three types of particle size and shape parameters. Particle size parameters include those determined by linear or area measurements. Shape
Parameters include extension parameters, such as the ratio of two length parameters, and roughness parameters, which represent surface irregularities.
The measurement approach in this document emphasizes that users should conduct both qualitative and quantitative analysis of data quality. Qualitative comparison of data sets involves determining the quality of individual parameters.
Quantitative comparison of data sets is based on the similarity or difference between the reference model parameters of the fitted parametric distribution.
The definition of a parametric distribution requires at least two parameters (mean and spread) and their uncertainties.
In some cases, two quantitative parameters and their uncertainties may not be sufficient to characterize the size and shape distribution. Data visualization techniques such as residuals and quantile plots can be used to
Data correlation techniques such as paired size and shape parameters or fractal analysis can provide additional methods to evaluate and differentiate test samples.
In short, qualitative and quantitative quality measures coupled with visualization and correlation tools allow users to develop
plan.
Nanotechnology Transmission electron microscopy measures nanometers
Particle size and shape distribution
1 Scope
This document specifies the acquisition, measurement and analysis of transmission electron microscope (TEM) images to obtain nanoparticle size and shape.
Distribution method.
This document is applicable to nano-objects and particles larger than 100 nm. The specific scope of application depends on the required uncertainty and transmission.
Electron microscope performance.
2 Normative references
The contents of the following documents constitute the essential clauses of this document through normative references in this document.
For referenced documents without a date, only the version corresponding to that date applies to this document; for referenced documents without a date, the latest version (including all amendments) applies to
This document.
ISO 9276-3 Representation of particle size analysis results Part 3.Adjustment of experimental curves to a reference model
ISO 9276-6 Expression of results of particle size analysis Part 6.Qualitative and quantitative expression of particle shape and morphology
Note. GB/T 15445.6-2014 Expression of particle size analysis results Part 6.Qualitative and quantitative expression of particle shape and morphology (ISO /T S9276-6.
2008, IDT)
ISO 29301 Method for calibration of image magnification using periodic structure reference materials in microbeam analysis transmission electron microscopy (Mi-
Note. GB/T 34002-2017 Method for calibrating image magnification using periodic structure reference materials in microbeam analysis transmission electron microscopy
(ISO 29301.2010, IDT)
3 Terms, definitions and symbols
The following terms and definitions apply to this document.
ISO and IEC provide terminology databases for standardization at the following URLs.
3.1 Particle Core Terminology
3.1.1
Nano-object
An object with one, two or three dimensions on the nanometer scale (3.1.2).
[Source. GB/T 32269-2015, 2.2, modified]
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