Principal Component Analysis of the Effect of Batch Variation, TiO2 Content and Reduction Temperature on the Surface Energy of TiO2/Graphene Oxide Membranes upon UV-C Activation


In this work principal component analysis (PCA) was used to study the effect of batch, reduction temperature, TiO2 content and UV-C irradiation on the surface energy, -polarity and interlayer spacing of photoactive TiO2/GO composite membranes. Two PCA models were successfully developed. The first PCA model shows a negative correlation between reduction temperature and d-spacing. Less hydrophilic TiO2/GO membranes were obtained at 160 °C compared to membranes reduced at 140 °C. Also, the surface polarity and surface energy were significantly enhanced by the addition of higher TiO2 content. The second model explain the effect of UV-C activation on the surface energy of the TiO2/GO composite membranes. For the GO membranes containing TiO2 a significant increase in surface energy and -polarity was observed after UV-C activation. Moreover, a positive correlation between the TiO2 content and surface energy after UV-C activation was observed. Higher TiO2 content results in higher surface energy. GO batches prepared by different groups was not found to significantly affect the properties of the TiO2/GO composite membranes suggesting that the preparation method is relative robust.

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  1. 1.

    Bui X-T, Chiemchaisri C, Fujioka T, Varjani S (2019) Introduction to recent advances in water and wastewater treatment technologies. In: Agarwal AK, Pandey A (eds) Water and wastewater treatment technologies, 1st edn. Springer, Singapore, pp 3–12

    Google Scholar 

  2. 2.

    Nam S-W, Jo B-I, Yoon Y, Zoh K-D (2013) Occurrence and removal of selected micropollutants in a water treatment plant. Chemosphere 95:156–165

    Article  Google Scholar 

  3. 3.

    Sikdar SK, Criscuoli A (2017) Sustainability and how membrane technologies in water treatment can be a contributor. In: Figoli A, Criscuoli A (eds) Sustainable membrane technology for water and wastewater treatment, 1st edn. Springer, Singapore, pp 1–21

    Google Scholar 

  4. 4.

    Van Der Bruggen B, Vandecasteele C (2003) Removal of pollutants from surface water and groundwater by nanofiltration: overview of possible applications in the drinking water industry. Environ Pollut 122:435–445

    Article  Google Scholar 

  5. 5.

    Mehta R, Brahmbhatt H, Saha NK, Bhattacharya A (2015) Removal of substituted phenyl urea pesticides by reverse osmosis membranes: laboratory scale study for field water application. Desalination 358:69–75

    CAS  Article  Google Scholar 

  6. 6.

    Jhaveri JH, Murthy Z (2016) A comprehensive review on anti-fouling nanocomposite membranes for pressure driven membrane separation processes. Desalination 379:137–154

    CAS  Article  Google Scholar 

  7. 7.

    Pedersen MLK, Jensen TR, Kucheryavskiy SV, Simonsen ME (2018) Investigation of surface energy, wettability and zeta potential of titanium dioxide/graphene oxide membranes. J Photochem Photobiol A Chem 366:162–170

    CAS  Article  Google Scholar 

  8. 8.

    Athanasekou CP, Morales-Torres S, Likodimos V, Romanos GE, Pastrarna-Martinez LM, Falaras P, Dionysiou DD, Faria JL, Figueiredo JL, Silva AMT (2014) Prototype composite membranes of partially reduced graphene oxide/TiO2 for photocatalytic ultrafiltration water treatment under visible light. Appl Catal B Environ 158–159:361–372

    Article  Google Scholar 

  9. 9.

    Chen L, Shi G, Shen J, Peng B, Zhang B, Wang Y, Bian F, Wang J, Li D, Qian Z, Xu G, Liu G, Zeng J, Zhang L, Yang Y, Zhou G, Wu M, Jin W, Li J, Fang H (2017) Ion sieving in graphene oxide membranes via cationic control of interlayer spacing. Nature 550:380–383

    CAS  Article  Google Scholar 

  10. 10.

    Werber JR, Osuji CO, Elimelech M (2016) Materials for next-generation desalination and water purification membranes. Nat Rev Mater 1:1–15

    Article  Google Scholar 

  11. 11.

    Kumar R, Singh RK, Kumar V, Moshkalev SA (2018) Functionalized nanosize graphene and its derivatives for removal of contaminations and water treatment. In: Naushad M (ed) A new generation material graphene: applications in water technology, 1st edn. Springer, Cham, pp 133–185

    Google Scholar 

  12. 12.

    Yu W, Yu T, Graham N (2017) Development of a stable cation modified graphene oxide membrane for water treatment. 2D Mater 4:1–14

    Article  Google Scholar 

  13. 13.

    Sengupta I, Chakraborty S, Talukdar M, Pal SK (2018) Thermal reduction of graphene oxide: how temperature influences purity. Mater Res Soc 33:4113–4122

    CAS  Article  Google Scholar 

  14. 14.

    Wei Y, Zhang Y, Gao X, Ma Z, Wang X, Gao C (2018) Multilayered graphene oxide membrane for water treatment: a review. Carbon 139:964–981

    CAS  Article  Google Scholar 

  15. 15.

    Alhadhrami A, Salgado S, Maheshwari V (2016) Thermal reduction to control the spacing in graphene oxide membranes: effect on ion diffusion and electrical conduction. R Soc Chem 6:70012–70017

    CAS  Google Scholar 

  16. 16.

    Yang E, Ham MH, Park HB, Kim CM, Song JH, Kim IS (2018) Tunable semi-permeability of graphene-based membranes by adjusting reduction degree of laminar graphene oxide layer. J Membr Sci 547:73–79

    CAS  Article  Google Scholar 

  17. 17.

    Homaeigohar S, Elbahri M (2017) Graphene membranes for water desalination. NPG Asia Mater 9:427–427

    Article  Google Scholar 

  18. 18.

    Safarpour M, Vatanpour V, Khataee A, Esmaeili M (2015) Development of a novel high flux and fouling-resistant thin film composite nanofiltration membrane by embedding reduced graphene oxide/TiO2. Sep Purif Technol 154:96–107

    CAS  Article  Google Scholar 

  19. 19.

    Zhu C, Liu G, Han K, Ye H, Wei S, Zhou Y (2017) One-step facile synthesis of graphene oxide/TiO2 composite as efficient photocatalytic membrane for water treatment: crossflow filtration operation and membrane fouling analysis. Chem Eng Process Process Intensif 120:20–26

    CAS  Article  Google Scholar 

  20. 20.

    Safarpour M, Khataee A, Vatanpour V (2015) Thin film nanocomposite reverse osmosis membrane modified by reduced graphene oxide/TiO2 with improved desalination performance. J Membr Sci 489:43–54

    CAS  Article  Google Scholar 

  21. 21.

    Khataee AR, Safarpour M, Zarei M, Aber S (2012) Combined heterogeneous and homogeneous photodegradation of a dye using immobilized TiO2 nanophotocatalyst and modified graphite electrode with carbon nanotubes. J Mol Catal A Chem 363–364:58–68

    Article  Google Scholar 

  22. 22.

    Štengl V, Bakardjieva S, Grygar TM, Bludská J, Kormunda M (2013) TiO2-graphene oxide nanocomposite as advanced photocatalytic materials. Chem Cent J 7:1–12

    Article  Google Scholar 

  23. 23.

    Tayel A, Ramadan AR, El Seoud OA (2018) Titanium dioxide/graphene and titanium dioxide/graphene oxide nanocomposites: synthesis, characterization and photocatalytic applications for water decontamination. Catalysts 8:491–535

    Article  Google Scholar 

  24. 24.

    Banerjee S, Dionysiou DD, Pillai SC (2015) Self-cleaning applications of TiO2 by photo-induced hydrophilicity and photocatalysis. Appl Catal B Environ 176–177:396–428

    Article  Google Scholar 

  25. 25.

    Simonsen ME, Li Z, Søgaard EG (2009) Influence of the OH groups on the photocatalytic activity and photoinduced hydrophilicity of microwave assisted sol-gel TiO2 film. Appl Surf Sci 255:8054–8062

    CAS  Article  Google Scholar 

  26. 26.

    Liu J, Bai H, Wang Y, Liu Z, Zhang X, Sun DD (2010) Self-assembling TiO2 nanorods on large graphene oxide sheets at a two-phase interface and their anti-recombination in photocatalytic applications. Adv Funct Mater 20:4175–4181

    CAS  Article  Google Scholar 

  27. 27.

    Naghdi S, Jaleh B, Shahbazi N (2016) Reversible wettability conversion of electrodeposited graphene oxide/titania nanocomposite coating: investigation of surface structures. Appl Surf Sci 368:409–416

    CAS  Article  Google Scholar 

  28. 28.

    Marcano DC, Kosynkin DV, Berlin JM, Sinitskii A, Sun Z, Slesarev A, Alemany LB, Lu W, Tour JM (2010) Improved synthesis of graphene oxide. ACS Nano 4:4806–4814

    CAS  Article  Google Scholar 

  29. 29.

    Simonsen ME, Jensen H, Li Z, Søgaard EG (2008) Surface properties and photocatalytic activity of nanocrystalline titania films. J Photochem Photobiol A Chem 200:192–200

    CAS  Article  Google Scholar 

  30. 30.

    Owens DK, Wendt RC (1969) Estimation of the surface free energy of polymers. J Appl Polym Sci 13:1741–1747

    CAS  Article  Google Scholar 

  31. 31.

    Fowkes FM (1964) Attractive forces at interfaces. Ind Eng Chem 56:12, 40–52

    CAS  Article  Google Scholar 

  32. 32.

    Esbensen KH, Geladi P (2009) Principal component analysis: concept, geometrical interpretation, mathematical background, algorithms, history, practice. In: Comprehensive chemometrics: chemical and biochemical data analysis. Elsevier, Amsterdam, pp 211–226

  33. 33.

    Guardia L, Villar-Rodil S, Paredes JI, Rozada R, Martín-Alonso A, Tasón JMD (2012) UV light exposure of aqueous graphene oxide suspensions to promote their direct reduction, formation of graphene-metal nanoparticle hybrids and dye degradation. Carbon 50:1014–1024

    CAS  Article  Google Scholar 

  34. 34.

    Williams G, Seger B, Kamat PV (2008) TiO2-graphene nanocomposites. UV-assisted photocatalytic reduction of graphene oxide. ACS Nano 2:1487–1491

    CAS  Article  Google Scholar 

  35. 35.

    Szabó T, Veres Á, Cho E, Khim J, Vargo N, Dékány I (2013) Photocatalyst separation from aqueous dispersion using graphene oxide/TiO2 nanocomposites. Colloids Surf A Physicochem Eng Asp 433:230–239

    Article  Google Scholar 

  36. 36.

    Singh R (2014) Membrane technology and engineering for water purification: application, systems design and operation, 2nd edn. Elsevier, Amsterdam

    Google Scholar 

  37. 37.

    Lundstrom I (1983) Surface physics and biological phenomena. Phys Scr 4:5–13

    Article  Google Scholar 

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Correspondence to Morten E. Simonsen.

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Simonsen, K.R., Sharker, T., Rask, M. et al. Principal Component Analysis of the Effect of Batch Variation, TiO2 Content and Reduction Temperature on the Surface Energy of TiO2/Graphene Oxide Membranes upon UV-C Activation. Top Catal (2020).

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  • Graphene oxide membrane
  • TiO2
  • Principal component analysis
  • Surface energy
  • d-spacing