Determination of quantitative structure-property and structure-process relationships for graphene production in water

• Published in: Nano research Vol. 8; no. 6; pp. 1865 - 1881
• Main Authors: Nacken, Thomas J., Damm, Cornelia, Xing, Haichen, Rüger, Andreas, Peukert, Wolfgang
• Format: Journal Article
• Language: English
• Published: Beijing Tsinghua University Press 01.06.2015; Springer Nature B.V
• Subjects: Aqueous solutions; Atomic/Molecular Structure and Spectra; Biomedicine; Biotechnology; Carbon; Chemical vapor deposition; Chemistry and Materials Science; Composite materials; Condensed Matter Physics; Defects; Delaminating; Delamination; Graphene; Graphite; Materials Science; Nanotechnology; Product quality; Research Article; Solvents; Spectrum analysis; Stress concentration; Stress intensity; Surfactants; Transistors; Viscosity; 产品分析; 定量结构; 性质; 水溶液; 生产; 石墨; 能量输入; 非离子表面活性剂; stirred-media mill; process parameters; statistical Raman spectroscopy; few-layer graphene; graphite delamination; graphene
• ISSN: 1998-0124; 1998-0000
• DOI: 10.1007/s12274-014-0694-6

A scalable method for graphene and few-layer graphene （FLG） production by graphite delamination in aqueous solutions of the nonionic surfactant TWEEN 80 （TW80） using stirred-media mills is presented. Delaminated product analysis using statistical Raman spectroscopy yielded extensive processing-structure-property relationships that revealed how stress intensity and specific energy input, i.e., the process parameters, govern the yield of graphene production and defect formation. The dispersed carbon concentration increased but the content and the quality of the FLG product decreased sharply with higher specific energy input. The FLG content of the product was up to 90%, especially for low specific energy input. Moreover, Raman analyses revealed that stress intensities greater than about I nJ were related to significant defect formation in the product particles. Another key parameter for graphene production is solvent viscosity. The FLG concentration in the product increased by a factor of 10 when the solvent＇s viscosity was increased from 1 to 6 mPa-s because shear- and friction-induced delamination was enhanced and in-plane fracture was reduced due to dampening of bead motion. Based on the processing-structure-property relationships found, we propose that the delamination process can be designed in such way that the product consists, almost totally, of FLG and that single-layer graphene is produced. The scalability of graphene production by stirred-media delamination was demonstrated when an increase in the batch size from 0.2 to 2 L had no significant effect on product quality.