Thermogravimetric analysis (TGA) has been recognized as a simple and reliable analytical tool for characterization of industrially manufactured graphene powders. Thermal properties of graphene are dependent on many parameters such as particle size, number of layers, defects and presence of oxygen groups to improve the reliability of this method for quality control of graphene materials, therefore it is important to explore the influence of these parameters. This paper presents a comprehensive TGA study to determine the influence of different particle size of the three key materials including graphene, graphene oxide and graphite on their thermal parameters such as carbon decomposition range and its temperature of maximum mass change rate (Tmax). Results showed that Tmax values derived from the TGA-DTG carbon combustion peaks of these materials increasing from GO (558–616 °C), to graphene (659–713 °C) and followed by graphite (841–949 °C) The Tmax values derived from their respective DTG carbon combustion peaks increased as their particle size increased (28.6–120.2 µm for GO, 7.6–73.4 for graphene and 24.2–148.8 µm for graphite). The linear relationship between the Tmax values and the particle size of graphene and their key impurities (graphite and GO) confirmed in this study endows the use of TGA technique with more confidence to evaluate bulk graphene-related materials (GRMs) at low-cost, rapid, reliable and simple diagnostic tool for improved quality control of industrially manufactured GRMs including detection of “fake” graphene.

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Printed electronic sensors offer a breakthrough in the availability of low-cost devices for improving quality of human life. Conductive ink is the core of printing technology and one of the...

Counterfeits in the supply chain of high-value advanced materials such as graphene and their derivatives have become a concerning problem with a potential negative impact on this growing and emerging industry. Recent studies have revealed alarming facts that a large percentage of manufactured graphene materials on market are not graphene, raising considerable concerns for the end users. The common and recommended methods for the characterization of graphene materials, such as transmission electron microscopy (TEM), atomic force microscopy (AFM), and Raman spectroscopy based on spot analysis and probing properties of individual graphene particles, are limited to provide the determination of the properties of "bulk" graphene powders at a large scale and the identification of non-graphene components or purposely included additives. These limitations are creating counterfeit opportunities by adding low-cost black carbonaceous materials into manufactured graphene powders. To address this problem, it is critical to have reliable characterization methods, which can probe the specific properties of graphene powders at bulk scale, confirm their typical graphene signature, and detect the presence of unwanted additional compounds, where the thermogravimetric analysis (TGA) method is one of the most promising methods to perform this challenging task. This paper presents the evaluation of the TGA method and its ability to detect low-cost carbon additives such as graphite, carbon black, biochar, and activated carbon as potential counterfeiting materials to graphene materials and their derivatives such as graphene oxide (GO) and reduced GO. The superior performance of the TGA method is demonstrated here, showing its excellent capability to successfully detect these additives when mixed with graphene materials, which is not possible by two other comparative methods (Raman spectroscopy and powder X-ray diffraction (XRD)), which are used as the common characterization methods for graphene materials.

Research on graphene-related two-dimensional (2D) materials (GR2Ms) in recent years is strongly moving from academia to industrial sectors with many new developed products and devices on the market. Characterization and quality control of the GR2Ms and their properties are critical for growing industrial translation, which requires the development of appropriate and reliable analytical methods. These challenges are recognized by International Organization for Standardization (ISO 229) and International Electrotechnical Commission (IEC 113) committees to facilitate the development of these methods and standards which are currently in progress. Toward these efforts, the aim of this study was to perform an international interlaboratory comparison (ILC), conducted under Versailles Project on Advanced Materials and Standards (VAMAS) Technical Working Area (TWA) 41 “Graphene and Related 2D Materials” to evaluate the performance (reproducibility and confidence) of the thermogravimetric analysis (TGA) method as a potential new method for chemical characterization of GR2Ms. Three different types of representative and industrially manufactured GR2Ms samples, namely, pristine few-layer graphene (FLG), graphene oxide (GO), and reduced graphene oxide (rGO), were used and supplied to ILC participants to complete the study. The TGA method performance was evaluated by a series of measurements of selected parameters of the chemical and physical properties of these GR2Ms including the number of mass loss steps, thermal stability, temperature of maximum mass change rate (T p) for each decomposition step, and the mass contents (%) of moisture, oxygen groups, carbon, and impurities (organic and non-combustible residue). TGA measurements determining these parameters were performed using the provided optimized TGA protocol on the same GR2Ms by 12 participants across academia, industry stakeholders, and national metrology institutes. This paper presents these results with corresponding statistical analysis showing low standard deviation and statistical conformity across all participants that confirm that the TGA method can be satisfactorily used for characterization of these parameters and the chemical characterization and quality control of GR2Ms. The common measurement uncertainty for each parameter, key contribution factors were identified with explanations and recommendations for their elimination and improvements toward their implementation for the development of the ISO/IEC standard for chemical characterization of GR2Ms.

Polluted waters are complex systems with many different co‐existing contaminants that make their simultaneous removal a very challenging task. To address this problem, all‐in‐one ad/ab‐sorbent with unique combination of interfacial properties and multiple surface chemistry is developed to simultaneously and efficiently remove several pollutants including heavy metals, dyes, oils, and organic solvents. By mimicking the wetting micro‐topology of a darkling beetle with a combined hydrophilic‐hydrophobic surface, a new bioinspired adsorbent, graphene biopolymer foam (Alg‐Fe3O4‐rGO‐4S) for removal of multiple water pollutants is engineered by combining alginate (Alg) and reduced graphene oxide (rGO) functionalized with tetrathiol that is also decorated with iron oxide nanoparticles (Fe3O4). This concept is first proved by single pollutant removal, showing adsorption capacity of 789.7 ± 36 mg/g for methylene blue (MB), 107.0 ± 2.1 mg/g for Hg (II), 73.5 ± 0.7 mg/g for Cu (II), and rapid oil‐water separation with high sorption capacity (11–18 g/g). A remarkable performance for simultaneous removal of their mixtures in milli‐Q, river, and sea water is demonstrated with efficiency for MB (≈90%), Cu (II) (>99.99%) and Hg (II) (100%) and rapid (≈30 s) uptake of organic solvents and oils. The obtained results indicate a valuable potential of proposed concept for simultaneous removal of co‐existing water pollutants.

There is a pressing need for reliable, reproducible and accurate measurements of graphene’s properties, through international standards, to facilitate industrial growth. However, trustworthy and verified standards require rigorous metrological studies, determining, quantifying and reducing the sources of measurement uncertainty. Towards this effort, we report the procedure and the results of an international interlaboratory comparison (ILC) study, conducted under Versailles Project on Advanced Materials and Standards (VAMAS). This ILC focusses on the comparability of Raman spectroscopy measurements of chemical vapour deposition (CVD) grown graphene using the same measurement protocol across different institutes and laboratories. With data gathered from 17 participants across academia, industry (including instrument manufacturers) and national metrology institutes, this study investigates the measurement uncertainty contributions from both Raman spectroscopy measurements and data analysis procedures, as well as provides solutions for improved accuracy and precision. While many of the reported Raman metrics were relatively consistent, significant and meaningful outliers occurred due to differences in the instruments and data analysis. These variations resulted in inconsistent reports of peak intensity ratios, peak widths and the coverage of graphene. Due to a lack of relative intensity calibration, the relative difference reported in the 2D- and G peak intensity ratios (Ι_2D/Ι_G) was up to 200%. It was also shown that the standard deviation for Γ_2D values reported by different software packages, was 15× larger for Lorentzian fit functions than for pseudo-Voigt functions. This study has shown that by adopting a relative intensity calibration and consistent peak fitting and data analysis methodologies, these large, and previously unquantified, variations can be significantly reduced, allowing more reproducible and comparable measurements for the graphene community, supporting fundamental research through to the growing graphene industry worldwide. This project and its findings directly underpin the development of the ISO/IEC standard “DTS 21356-2 - Nanotechnologies - Structural Characterisation of CVD-grown Graphene”.