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113/581/NP Nanomanufatcuring – Key Control Characteristics – Part 6-18: Graphene powder – Functional groups: TGA-FTIR

Scope

This part of IEC/TS 62607 establishes a standardized method to determine the chemical key control characteristics functional groups in graphene powder by Thermal Gravimetric Analysis (TGA) coupled with Fourier Transform Infrared Spectroscopy (FTIR), referred to as TGA-FTIR.

A sample heated in a TGA furnace using a predetermined temperature profile typically undergoes one or more weight losses. The content of functional groups in graphene powder is derived by changes in mass of the sample as a function of temperature using TGA. Materials evolved during these weight losses are then analyzed using coupled FTIR to identify functional groups.

– The functional groups determined according to this standard is listed as a key control characteristic in the blank detail specification for graphene IEC/TS 62565-3-1 for graphene powder.

– The method is applicable for graphene powder with functional groups that can be pyrolyzed and gasified with elevated temperature during TGA.

– Typical application areas are quality control for graphene manufacturers, and product selection for downstream users.

Purpose

One of the most well-studied routes for the preparation of graphene is the oxidation and reduction process. The most cost-effective process to obtain graphene is the exfoliation of natural graphite layers after oxidation to get individual oxidized layers and then de-oxygenation (reduction) of these individual layers. During the oxidation process, various functionalized groups (-OH, -O-, -COOH, C=O, etc.) go into the graphene skeleton, breaking the π bond of graphene structure. Oxygen attachment to graphene in any chemical form (epoxide, hydroxyl, carboxyl and ketonic-type functional groups) both on the basal plane and at the edges reduces electronic states at the Fermi level. The type and content of functional groups affect the physiochemical properties of graphene. Therefore, the identification and quantification of functional groups on graphene powder is believed to be a key control characteristic for its production and application.

Coupling thermal gravimetric analysis (TGA) and Fourier Transform infrared spectroscopy (FTIR) is an excellent solution to identify and quantify functional groups on graphene powder. In TGA-FTIR, while mass changes such as sample pyrolysis and vaporization that accompany changes in temperature are measured quantitatively by the TGA, qualitative analysis of the gaseous components can be conducted simultaneously by FTIR measurement of the obtained spectra. This standard focuses on determining the type and content of functional groups (e.g. hydroxyl, amino, carboxyl, alkyl, carbonyl, sulfonic acid group, etc) on graphene powder by coupling TGA and FTIR.

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