Automated device for the purification of graphene oxide dispersions: integration of cross-flow filtration and dialysis
Source abstract
Abstract
Graphene oxide (GO) dispersions require extensive purification to remove contaminants from synthesis. Conventional methods, such as dialysis, filtration and centrifugation are effective, but also labor-intensive, time-consuming, and challenging to automate. These approaches consume large volumes of water and energy, and limited efficiency in removing residues can compromise the properties of GO. We present a fully automated device integrating cross-flow filtration and dialysis using polyethersulfone (PES) membrane. Real-time conductivity monitoring enables optimal water exchange and resource use. The optimized system reduced conductivity from ~70 to < 0.5 mS cm −1 in under 16 h for 1.0 L dispersion at 1 mg mL −1 . Chemical analysis showed effective removal of ions (93% Cl − , 97% Mn 2+ , 92% SO 4 2− ), outperforming commercial samples. GO morphology and lateral dimensions were preserved, as verified by comprehensive characterization. This scalable platform enables high-throughput, application-ready GO purification, providing a practical solution for laboratories and industry seeking consistent, high-purity nanomaterials.
Source: openalex_inverted_index · Quality: baseline
Research context
OpenAlex topics: Graphene and Nanomaterials Applications · Graphene research and applications · Electrohydrodynamics and Fluid Dynamics
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
References (58)
Show source-provided references
1. Novoselov, K. S. et al. Electric field effect in atomically thin carbon films. Science 306, 666–669 (2004).10.1126/science.1102896 ↗
2. Zhao, Y. & Lin, L. Graphene, beyond lab benches. Science 386, 144–146 (2024).10.1126/science.ads4149 ↗
3. Peplow, M. Coming of age. Science 386, 138–143 (2024).10.1126/science.adt6839 ↗
4. Balandin, A. A. et al. Superior thermal conductivity of single-layer graphene. Nano Lett. 8, 902–907 (2008).10.1021/nl0731872 ↗
5. Bolotin, K. I. et al. Ultrahigh electron mobility in suspended graphene. Solid State Commun. 146, 351–355 (2008).10.1016/j.ssc.2008.02.024 ↗
6. Frank, I. W., Tanenbaum, D. M., Van Der Zande, A. M. & McEuen, P. L. Mechanical properties of suspended graphene sheets. J. Vac. Sci. Technol. B Microelectron. Nanometer Struct. Process. Meas. Phenom. 25, 2558–2561 (2007).
7. Ghosh, S. et al. Extremely high thermal conductivity of graphene: Prospects for thermal management applications in nanoelectronic circuits. Appl. Phys. Lett. 92, 151911 (2008).10.1063/1.2907977 ↗
8. Lee, C., Wei, X., Kysar, J. W. & Hone, J. Measurement of the elastic properties and intrinsic strength of monolayer graphene. Science 321, 385–388 (2008).10.1126/science.1157996 ↗
9. Hirata, M., Gotou, T., Horiuchi, S., Fujiwara, M. & Ohba, M. Thin-film particles of graphite oxide 1. Carbon 42, 2929–2937 (2004).
10. Stankovich, S. et al. Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide. Carbon 45, 1558–1565 (2007).10.1016/j.carbon.2007.02.034 ↗
11. Eda, G. & Chhowalla, M. Chemically derived graphene oxide: towards large-area thin-film electronics and optoelectronics. Adv. Mater. 22, 2392–2415 (2010).10.1002/adma.200903689 ↗
12. Aramayo, M. A. F. et al. Eco-friendly waterborne polyurethane coating modified with ethylenediamine-functionalized graphene oxide for enhanced anticorrosion performance. Molecules 29, 4163 (2024).10.3390/molecules29174163 ↗
13. Cui, G. et al. A comprehensive review on graphene-based anti-corrosive coatings. Chem. Eng. J. 373, 104–121 (2019).10.1016/j.cej.2019.05.034 ↗
14. Stankovich, S. et al. Graphene-based composite materials. Nature 442, 282–286 (2006).10.1038/nature04969 ↗
15. Huang, X., Qi, X., Boey, F. & Zhang, H. Graphene-based composites. Chem. Soc. Rev. 41, 666–686 (2012).10.1039/C1CS15078B ↗
16. Krishnan, D. et al. Energetic graphene oxide: Challenges and opportunities. Nano Today 7, 137–152 (2012).10.1016/j.nantod.2012.02.003 ↗
17. Rocha, J. F. et al. Graphene oxide fibers by microfluidics assembly: a strategy for structural and dimensional control. Nanoscale 13, 6752–6758 (2021).10.1039/D0NR08380A ↗
18. Georgakilas, V. et al. Noncovalent functionalization of graphene and graphene oxide for energy materials, biosensing, catalytic, and biomedical applications. Chem. Rev. 116, 5464–5519 (2016).10.1021/acs.chemrev.5b00620 ↗
19. Nishina, Y. Mass production of graphene oxide beyond the laboratory: bridging the gap between academic research and industry. ACS Nano 18, 33264–33275 (2024).10.1021/acsnano.4c13297 ↗
20. Donato, K. Z. et al. Graphene oxide classification and standardization. Sci. Rep. 13, 6064 (2023).10.1038/s41598-023-33350-5 ↗
21. Abdel-Motagaly, A. T., El Rouby, W. M. A., El-Dek, S. I., El-Sherbiny, I. M. & Farghali, A. A. Fast technique for the purification of as-prepared graphene oxide suspension. Diam. Relat. Mater. 86, 20–28 (2018).10.1016/j.diamond.2018.04.006 ↗
22. Tölle, F. J., Gamp, K. & Mülhaupt, R. Scale-up and purification of graphite oxide as intermediate for functionalized graphene. Carbon 75, 432–442 (2014).10.1016/j.carbon.2014.04.022 ↗
23. Santos, M. A., Marques, L. & Silva, C. D. C. C. Purification of graphene oxide dispersions by using a fluidic cell. Anal. Methods 12, 3575–3581 (2020).10.1039/D0AY00600A ↗
24. Barbolina, I. et al. Purity of graphene oxide determines its antibacterial activity. 2D Mater. 3, 025025 (2016).10.1088/2053-1583/3/2/025025 ↗
25. Faria, A. F., Perreault, F. & Elimelech, M. Elucidating the role of oxidative debris in the antimicrobial properties of graphene oxide. ACS Appl. Nano Mater. 1, 1164–1174 (2018).10.1021/acsanm.7b00332 ↗
26. Ali-Boucetta, H. et al. Purified graphene oxide dispersions lack in vitro cytotoxicity and in vivo pathogenicity. Adv. Healthc. Mater. 2, 433–441 (2013).10.1002/adhm.201200248 ↗
27. Mrózek, O. et al. Salt-washed graphene oxide and its cytotoxicity. J. Hazard. Mater. 398, 123114 (2020).10.1016/j.jhazmat.2020.123114 ↗
28. Tene, T. et al. Toward large-scale production of oxidized graphene. Nanomaterials 10, 279 (2020).10.3390/nano10020279 ↗
29. Ceriotti, G., Romanchuk, A. Y., Slesarev, A. S. & Kalmykov, S. N. Rapid method for the purification of graphene oxide. RSC Adv. 5, 50365–50371 (2015).10.1039/C5RA07604H ↗
30. Chen, J., Li, Y., Huang, L., Li, C. & Shi, G. High-yield preparation of graphene oxide from small graphite flakes via an improved Hummers method with a simple purification process. Carbon 81, 826–834 (2015).10.1016/j.carbon.2014.10.033 ↗
31. Mikheev, I. V. et al. High-throughput preparation of uncontaminated graphene-oxide aqueous dispersions with antioxidant properties by semi-automated diffusion dialysis. Nanomaterials 12, 4159 (2022).10.3390/nano12234159 ↗
32. Alhourani, A. H., Cashman, J. & Schöne, K. An Improved Method to Wash Graphene Prior to Use as a Drug Delivery Vehicle. Application Note, Sartorius Lab Instruments GmbH & Co. Available at: https://www.sartorius.com/download/947254/vivaflow-graphene-application-note-en-l-sartorius-pdf-data.pdf (2021).
33. Li, C., Guo, Y., Shen, L., Ji, C. & Bao, N. Scalable concentration process of graphene oxide dispersions via cross-flow membrane filtration. Chem. Eng. Sci. 200, 127–137 (2019).10.1016/j.ces.2019.01.045 ↗
34. Bhunia, P., Kumar, M. & De, S. Rapid and efficient removal of ionic impurities from graphene oxide through hollow fiber diafiltration. Sep. Purif. Technol. 209, 103–111 (2019).10.1016/j.seppur.2018.07.025 ↗
35. Bhunia, P., Kumar, M. & De, S. Fast purification of graphene oxide solution by continuous counter current hollow fibre dialysis: A step towards large scale production. Can. J. Chem. Eng. 97, 1596–1604 (2019).10.1002/cjce.23380 ↗
36. Hummers, W. S. & Offeman, R. E. Preparation of graphitic oxide. J. Am. Chem. Soc. 80, 1339–1339 (1958).10.1021/ja01539a017 ↗
37. Bird, R. B., Stewart, W. E. & Lightfoot, E. N. Transport Phenomena. (J. Wiley and sons, New York Chichester Brisbane [etc.], 1960).
38. Ye, R. et al. Manganese deception on graphene and implications in catalysis. Carbon 132, 623–631 (2018).10.1016/j.carbon.2018.02.082 ↗
39. Farivar, F., Lay Yap, P., Karunagaran, R. U. & Losic, D. Thermogravimetric analysis (TGA) of graphene materials: effect of particle size of graphene, graphene oxide and graphite on thermal parameters. C J Carbon Res 7, 41 (2021).10.3390/c7020041 ↗
40. Jiříčková, A., Jankovský, O., Sofer, Z. & Sedmidubský, D. Synthesis and applications of graphene oxide. Materials 15, 920 (2022).10.3390/ma15030920 ↗
41. Al-Gaashani, R., Najjar, A., Zakaria, Y., Mansour, S. & Atieh, M. A. XPS and structural studies of high quality graphene oxide and reduced graphene oxide prepared by different chemical oxidation methods. Ceram. Int. 45, 14439–14448 (2019).10.1016/j.ceramint.2019.04.165 ↗
42. Yu, H., Zhang, B., Bulin, C., Li, R. & Xing, R. High-efficient synthesis of graphene oxide based on improved hummers method. Sci. Rep. 6, 36143 (2016).10.1038/srep36143 ↗
43. Dimiev, A. M. & Tour, J. M. Mechanism of graphene oxide formation. ACS Nano 8, 3060–3068 (2014).10.1021/nn500606a ↗
44. Pattisson, S. et al. Tuning graphitic oxide for initiator- and metal-free aerobic epoxidation of linear alkenes. Nat. Commun. 7, 12855 (2016).10.1038/ncomms12855 ↗
45. Aixart, J., Díaz, F., Llorca, J. & Rosell-Llompart, J. Increasing reaction time in Hummers’ method towards well exfoliated graphene oxide of low oxidation degree. Ceram. Int. 47, 22130–22137 (2021).10.1016/j.ceramint.2021.04.235 ↗
46. Al-Gaashani, R. et al. Effects of preparation temperature on production of graphene oxide by novel chemical processing. Ceram. Int. 47, 10113–10122 (2021).10.1016/j.ceramint.2020.12.159 ↗
47. Guo, S., Garaj, S., Bianco, A. & Ménard-Moyon, C. Controlling covalent chemistry on graphene oxide. Nat. Rev. Phys. 4, 247–262 (2022).10.1038/s42254-022-00422-w ↗
48. Ikram, R., Jan, B. M. & Ahmad, W. An overview of industrial scalable production of graphene oxide and analytical approaches for synthesis and characterization. J. Mater. Res. Technol. 9, 11587–11610 (2020).10.1016/j.jmrt.2020.08.050 ↗
49. Kovtun, A. et al. Accurate chemical analysis of oxygenated graphene-based materials using X-ray photoelectron spectroscopy. Carbon 143, 268–275 (2019).10.1016/j.carbon.2018.11.012 ↗
50. Marcano, D. C. et al. Improved synthesis of graphene oxide. ACS Nano 4, 4806–4814 (2010).10.1021/nn1006368 ↗
51. Perrozzi, F., Prezioso, S. & Ottaviano, L. Graphene oxide: from fundamentals to applications. J. Phys. Condens. Matter 27, 013002 (2015).10.1088/0953-8984/27/1/013002 ↗
52. Loh, K. P., Bao, Q., Eda, G. & Chhowalla, M. Graphene oxide as a chemically tunable platform for optical applications. Nat. Chem. 2, 1015–1024 (2010).10.1038/nchem.907 ↗
53. Dreyer, D. R., Park, S., Bielawski, C. W. & Ruoff, R. S. The chemistry of graphene oxide. Chem. Soc. Rev. 39, 228–240 (2010).10.1039/B917103G ↗
54. Palermo, V., Kinloch, I. A., Ligi, S. & Pugno, N. M. Nanoscale mechanics of graphene and graphene oxide in composites: a scientific and technological perspective. Adv. Mater. 28, 6232–6238 (2016).10.1002/adma.201505469 ↗
55. Smith, A. T., LaChance, A. M., Zeng, S., Liu, B. & Sun, L. Synthesis, properties, and applications of graphene oxide/reduced graphene oxide and their nanocomposites. Nano Mater. Sci. 1, 31–47 (2019).10.1016/j.nanoms.2019.02.004 ↗
56. Yoo, B. M., Shin, H. J., Yoon, H. W. & Park, H. B. Graphene and graphene oxide and their uses in barrier polymers. J. Appl. Polym. Sci. 131, app39628 (2014).10.1002/app.39628 ↗
57. Dong, L., Yang, J., Chhowalla, M. & Loh, K. P. Synthesis and reduction of large sized graphene oxide sheets. Chem. Soc. Rev. 46, 7306–7316 (2017).10.1039/C7CS00485K ↗
58. Dideikin, A. T. & Vul’, A. Y. Graphene oxide and derivatives: the place in graphene family. Front. Phys. 6, 149 (2019).10.3389/fphy.2018.00149 ↗