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GB/T 42310-2023Nanotechnology—Measurement for specific surface area of graphene powder—Static volumetric method by argon gas adsorption (English PDF)

纳米技术 石墨烯粉体比表面积的测定 氩气吸附静态容量法

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Issued by

SAMR; SAC

Level / Type

National · Recommended

Issue date

March 17, 2023

Implementation date

October 1, 2023

Scope

GB/T 42310-2023 is the English-translated version of 纳米技术 石墨烯粉体比表面积的测定 氩气吸附静态容量法.

GB/T 42310-2023 is the Chinese national method for measuring the specific surface area of graphene powder by argon adsorption with the static volumetric technique.

It covers the principle, the reagents and materials, the instruments, the test procedure, the processing of the experimental data, the measurement uncertainty and the test report, with informative appendices on the adsorption behaviour of different adsorbates, their heat of adsorption, the effect of sample volume, degassing temperature by thermogravimetric analysis and the choice of BET calculation points for powders containing micropores.

Clause 1 applies it to powders whose adsorption isotherms are of type II or type IV, the latter with pores of 2 nm to 50 nm. Its introduction states that argon is preferred because nitrogen, having a quadrupole moment, adsorbs specifically on polar graphene surfaces. Issued on 17 March 2023, applicable since 1 October 2023.

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Document preview — GB/T 42310-2023

National Standard of the People's Republic of China

ICS
71.040.50
Classification
G 04

Issued by: State Administration for Market Regulation; Standardization Administration of the PRC

Contents

  • Preface
  • Introduction
  • 1 Scope
  • 2 Normative references
  • 3 Terms and Definitions
  • 4 Principle
  • 5 Reagent or material
  • 6 Instruments and equipment
  • 7 Test process
  • 8 Experimental data processing
  • 9 Measurement uncertainty
  • 10 Test report
  • Appendix A (informative) Adsorption behavior of different adsorbates on the surface of graphene powder samples
  • Appendix B (informative) Research on heat of adsorption of different types of graphene powder samples
  • Appendix C (informative) Test example of relationship between specific surface area and sample volume
  • Appendix D (informative) Thermogravimetric analysis to determine the degassing temperature test example of the test sample
  • Appendix E (informative) BET specific surface area calculation point selection process of graphene powder containing micropores
  • Reference

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.

Introduction

The specific surface area of graphene powder is one of the key characteristic parameters affecting its application performance. Nitrogen adsorption (Brunauer-Emmett- Teler) method is a common method for testing the specific surface area of solid substances, but its applicable premise is that nitrogen is used as the adsorbate on the surface of solid adsorbent.

The adsorption behavior fits the ideal classical physical adsorption model. There are various types of industrialized graphene powder in my country, and different types of samples contain different Intra-sheet defects, sheet edge dislocations, grain boundaries, etc., make the chemical activity and number of carbon atoms in the above places also exist. difference. In addition, due to different production processes, the functional groups (such as -OH) introduced on the surface of different types of powder samples are also different. nitrogen Gas molecules have a quadrupole moment, and as an adsorbate, they will interact with polar adsorbents to form specific adsorption, which is different from ideal classical physical adsorption.

The molecular arrangement and orientation of the model may cause poor linear correlation of the multi-point BET diagram, so the accuracy and reliability of the specific surface area test results Sex is also poor. The adsorption behavior of different adsorbates on the surface of graphene powder is shown in Appendix A.

Argon molecules are monatomic gas molecules, electrons have been completely paired and there is no bonding orbital, and it is generally considered to have no chemical activity. sex. There is no quadrupole moment for argon molecules, and when adsorbed on the surface of graphene powder materials as an adsorbate, it is sensitive to the surface structure or functional groups of the sample.

The sensitivity is low, and its adsorption behavior conforms to the ideal classical physical adsorption model, so when the specific surface area is measured at the temperature of liquid argon, the classical physical adsorption model can be used.

BET theory for calculations. Since the polarizability and molecular size of argon and nitrogen are very similar, their non-specific adsorption properties are also very similar.

Similarly, on nonpolar adsorbents, the heat of adsorption of nitrogen is almost equal to that of argon. For polar graphene powder materials, argon and nitrogen There is a significant difference in the heat of adsorption of argon and gas (see Appendix B for relevant examples), which further confirms that the use of argon as the adsorbate to determine the graphene powder ratio The science and plausibility of surface area.

1 Scope

This document describes a method for the determination of the specific surface area of graphene powders by the argon adsorption static volumetric method.

This document is applicable to the determination of adsorption isotherms with type II (dispersed, non-porous or macroporous) and type IV (mesoporous, pore size 2nm~50nm)

Specific surface area of graphene powder. Contains a small amount of micropores, and the adsorption isotherm shows a combination of type II and type I or a combination of type IV and type I It is also applicable to the determination of specific surface area of graphene powder. Other types of carbon-based nanomaterials, such as carbon nanotubes, carbon fibers, porous carbon, etc. The determination of the volume refers to the use.

2 Normative references

This document has no normative references.

3 Terms and Definitions

The following terms and definitions apply to this document.

3.1 Graphene

graphene layer graphenelayer single-layer graphene single-layergraphene; monolayergraphene A monolayer of carbon atoms that combines one carbon atom with three surrounding carbon atoms to form a honeycomb structure.

NOTE 1. It is an important building block of many carbon nanoobjects.

Note 2. Since graphene has only one layer, it is often called monolayer graphene. Graphene is abbreviated as 1LG to distinguish it from bilayer graphite abbreviated as 2LG ene and few-layer graphene abbreviated as FLG.

NOTE 3. Graphene has boundaries and has defects and grain boundaries where carbon-carbon bonds have been disrupted. [Source: GB/T 30544.13-2018, 3.1.2.1]

3.2 Graphene powder

It is a black or brownish-yellow powder mainly composed of graphene and related two-dimensional materials.

Note: Graphene powder includes single-layer graphene (1LG), double-layer graphene (2LG), few-layer graphene (FLG), graphene nanosheet (GNP), mechanical exfoliation stone Graphene, chemically dissociated graphene, small molecule synthesis (CVD, PVD) graphene, reduced graphene oxide (rGO), graphene oxide (GO), etc.

3.3 Nanosheets made of graphene layers

NOTE: The common thickness of GNPs is 1 nm to 3 nm, and the lateral dimensions range from approximately 100 nm to 100 µm. [Source: GB/T 30544.13-2018, 3.1.2.11]

3.4 graphene oxide graphene oxide; GO

The chemically modified graphene obtained after oxidation and exfoliation of graphite has its basal plane modified by strong oxidation.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 22 pages — is available in the English PDF.

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