Ultrasonic Synthesis of Carbon Nanotube-Titanium Dioxide Composites: Process Optimization via Response Surface Methodology
Open accessAbstract
In this study, the central composite design of response surface methodology was applied to optimize the ultrasonic synthesis of multiwalled carbon nanotube-titanium dioxide (MWNT-TiO2) composites. Twenty composites were prepared by adjusting three parameters (MWNT concentration in water, sonication to disperse/exfoliate MWNTs in water, and sonication to attach TiO2 onto MWNTs) at five levels. On the basis of the experimental design, semiempirical expressions were developed, analyzed, statistically assessed, and subsequently applied to predict the impact of the studied parameters on composite synthesis. The composite synthesis process was optimized to capture the experimental conditions favoring the highest productivity (i.e., MWNT-TiO2 formation or percent TiO2 attachment) utilizing minimal resources. The synthesis process optimization results showed that, to make a MWNT-TiO2 composite in 10 mL of water, 23.2 mg (∼99% of 23.4 mg) of TiO2 can be attached to 2.6 mg of MWNTs. This process requires only 727 J sonication energy, of which 592 J is invested to exfoliate MWNTs (Sonication 1) and 135 J to attach TiO2 (Sonication 2) to MWNTs. Finally, the optimally synthesized composite was extensively characterized using SEM, surface area and porosity analysis, TGA, and ζ-potential analysis/DLS. Also, this composite was tested for stability under variable pH and solvent polarity. The approach developed in this study could be used to optimize the synthesis process of other similar composites.
The claims and statistics of this paper haven’t been checked yet.
Run the check — free, no account needed. It reads the open-access text and checks the sources it cites.
Integrity signals
Registry
Cites
Statistics
Claims the paper makes
The claims and statistics of this paper haven’t been checked yet.
Run the check — free, no account needed. It reads the open-access text and checks the sources it cites.
Claims other papers make about this one
Each is checked against this paper’s own text: does it say what the citing paper says it does?
The RSM model exhibited satisfactory approximation of actual Cr(VI) adsorption removal, with a high correlation coefficient R2 of 0.99, implying that 99% of variations in results can be attributed to studied factors.
“The RSM model exhibited satisfactory approximation of the actual Cr(VI) adsorption removal (%), as demonstrated by the high correlation coefficient (R2) of 0.99 (Fig. 3), implying that 99% of the variations in the results can be attributed to the studied factors34,35.”
From Optimized removal of hexavalent chromium from water using spent tea leaves treated with ascorbic acid (2022) · cites this paper as [35]
The Results and Discussion, under “Model Development and Fitting” (page not provided), report a good fit between predicted and experimental values for two RSM responses. But those responses are MWNT expansion and TiO₂ attachment, not Cr(VI) adsorption removal, and the reported regression coefficient is approximately 0.9, not 0.99. The source therefore does not support the claim that 99% of variation in Cr(VI) removal was attributable to the studied factors. (LLM, conf=0.85)
Experimental — accuracy not yet measured
Self-check
Percentages, sums and reported differences re-computed from the paper’s own numbers.
The self-check needs the paper’s full text.
Cites
Processable aqueous dispersions of graphene nanosheets
Li, D., Müller, M. B., Gilje, S., Kaner, R. B., & Wallace, G. G. (2008) · Nature Nanotechnology · doi:10.1038/nnano.2007.451 · Cited by 9,122 · see citing works
Response surface methodology (RSM) as a tool for optimization in analytical chemistry
Bezerra, M. A., Santelli, R. E., Oliveira, E. P., Villar, L. S., & Escaleira, L. A. (2008) · Talanta · doi:10.1016/j.talanta.2008.05.019 · Cited by 6,075 · see citing works
Advances in the science and technology of carbon nanotubes and their composites: a review
Thostenson, E. T., Ren, Z., & Chou, T. (2001) · Composites Science and Technology · doi:10.1016/s0266-3538(01)00094-x · Cited by 5,017 · see citing works
Hurum, D. C., Agrios, A. G., Gray, K. A., Rajh, T., & Thurnauer, M. C. (2003) · The Journal of Physical Chemistry B · doi:10.1021/jp0273934 · Cited by 2,015 · see citing works
Bansal, R. C., & Goyal, M. (2005) · CRC Press eBooks · doi:10.1201/9781420028812 · Cited by 1,872 · see citing works
Why is anatase a better photocatalyst than rutile? - Model studies on epitaxial TiO2 films
Luttrell, T., Halpegamage, S., Tao, J., Kramer, A. R., Sutter, E., & Batzill, M. (2014) · Scientific Reports · doi:10.1038/srep04043 · Cited by 1,548 · see citing works
Dong, H., Zeng, G., Tang, L., Fan, C., Zhang, C., He, X., & He, Y. (2015) · Water Research · doi:10.1016/j.watres.2015.04.038 · Cited by 1,490 · see citing works
Multi-Factor Experimental Designs for Exploring Response Surfaces
Box, G. E. P., & Hunter, J. S. (1957) · The Annals of Mathematical Statistics · doi:10.1214/aoms/1177707047 · Cited by 1,440 · see citing works
Photocatalytic degradation of azo dye acid red 14 in water on ZnO as an alternative catalyst to TiO2
Daneshvar, N., Salari, D., & Khataee, A. (2003) · Journal of Photochemistry and Photobiology A Chemistry · doi:10.1016/s1010-6030(03)00378-2 · Cited by 1,401 · see citing works
Photocatalytic Carbon‐Nanotube–TiO2 Composites
Woan, K. V., Pyrgiotakis, G., & Sigmund, W. M. (2009) · Advanced Materials · doi:10.1002/adma.200802738 · Cited by 1,393 · see citing works
Principles of Instrumental Analysis
Townshen, A. (1983) · Analytica Chimica Acta · doi:10.1016/s0003-2670(00)84936-3 · Cited by 1,084 · see citing works
A structural investigation of titanium dioxide photocatalysts
Bickley, R. I., González-Carreño, T., Lees, J. S., Palmisano, L., & Tilley, R. J. D. (1991) · Journal of Solid State Chemistry · doi:10.1016/0022-4596(91)90255-g · Cited by 1,055 · see citing works
Crystal faces of rutile and anatase TiO2 particles and their roles in photocatalytic reactions
Ohno, T., Sarukawa, K., & Matsumura, M. (2002) · New Journal of Chemistry · doi:10.1039/b202140d · Cited by 784 · see citing works
Herrmann, J. M. (2005) · Topics in Catalysis · doi:10.1007/s11244-005-3788-2 · Cited by 764 · see citing works
RSM simplified : optimizing processes using response surface methods for design of experiments
Anderson, M. J., & Whitcomb, P. J. (2005) · Cited by 591 · see citing works
Photoreactive TiO2/Carbon Nanotube Composites: Synthesis and Reactivity
Yao, Y., Li, G., Ciston, S., et al. (2008) · Environmental Science & Technology · doi:10.1021/es800191n · Cited by 573 · see citing works
Xu, Y., Zhuang, Y., & Fu, X. (2010) · The Journal of Physical Chemistry C · doi:10.1021/jp909855p · Cited by 542 · see citing works
Gunaraj, V., & Murugan, N. (1999) · Journal of Materials Processing Technology · doi:10.1016/s0924-0136(98)00405-1 · Cited by 531 · see citing works
Semiconductor-Based Composite Materials: Preparation, Properties, and Performance
Rajeshwar, K., de Tacconi, N. R., & Chenthamarakshan, C. R. N. (2001) · Chemistry of Materials · doi:10.1021/cm010254z · Cited by 510 · see citing works
Puma, G. L., Bono, A., Krishnaiah, D., & Joseph, C. G. (2008) · Journal of Hazardous Materials · doi:10.1016/j.jhazmat.2008.01.040 · Cited by 443 · see citing works
The 2 k-p Fractional Factorial Designs Part I
Box, G. E. P., & Hunter, J. S. (2000) · Technometrics · doi:10.2307/1271430 · Cited by 416 · see citing works
Yu, Y., Yu, J. C., Chan, C.-Y., Che, Y., Zhao, J., Ding, L., Ge, W., & Wong, P. K. (2005) · Applied Catalysis B: Environmental · doi:10.1016/j.apcatb.2005.03.008 · Cited by 413 · see citing works
Recombination Pathways in the Degussa P25 Formulation of TiO2: Surface versus Lattice Mechanisms
Hurum, D. C., Gray, K. A., Rajh, T., et al. (2004) · The Journal of Physical Chemistry B · doi:10.1021/jp045395d · Cited by 395 · see citing works
Sakkas, V. A., Islam, M. A., Stalikas, C. D., & Albanis, T. A. (2009) · Journal of Hazardous Materials · doi:10.1016/j.jhazmat.2009.10.050 · Cited by 381 · see citing works
Kwak, J.-S. (2004) · International Journal of Machine Tools and Manufacture · doi:10.1016/j.ijmachtools.2004.08.007 · Cited by 376 · see citing works
Synthesis and characterization of carbon nanotubes–TiO2 nanocomposites
Jitianu, A., Cacciaguerra, T., Benoit, R., Delpeux, S., Béguin, F., & Bonnamy, S. (2004) · Carbon · doi:10.1016/j.carbon.2003.12.041 · Cited by 341 · see citing works
Recombination Pathways in the Degussa P25 Formulation of TiO2: Surface versus Lattice Mechanisms
Hurum, D. C., Gray, K. A., Rajh, T., et al. (2005) · The Journal of Physical Chemistry B · doi:10.1021/jp050520m · Cited by 335 · see citing works
Li, G., & Gray, K. A. (2007) · Chemical Physics · doi:10.1016/j.chemphys.2007.05.023 · Cited by 309 · see citing works
Khataee, A., Fathinia, M., Aber, S., et al. (2010) · Journal of Hazardous Materials · doi:10.1016/j.jhazmat.2010.05.096 · Cited by 302 · see citing works
Preparation of a Novel TiO2-Based p−n Junction Nanotube Photocatalyst
Chen, Y., Crittenden, J. C., Hackney, S., et al. (2005) · Environmental Science & Technology · doi:10.1021/es049252g · Cited by 288 · see citing works
Photocatalytic degradation of the alimentary azo dye amaranth
Karkmaz, M., Puzenat, E., Guillard, C., & Herrmann, J. M. (2004) · Applied Catalysis B: Environmental · doi:10.1016/j.apcatb.2004.02.009 · Cited by 270 · see citing works
Probing reaction mechanisms in mixed phase TiO2 by EPR
Hurum, D. C., Agrios, A. G., Crist, S. E., et al. (2005) · Journal of Electron Spectroscopy and Related Phenomena · doi:10.1016/j.elspec.2005.01.294 · Cited by 261 · see citing works
Genotoxic effects of nanosized and fine TiO2
Falck, G. C. ‐., Lindberg, H., Suhonen, S., Vippola, M., Vanhala, E., Catalán, J., Savolainen, K., & Norppa, H. (2009) · Human & Experimental Toxicology · doi:10.1177/0960327109105163 · Cited by 202 · see citing works
Preparation of photocatalytic TiO2 coatings of nanosized particles on activated carbon by AP-MOCVD
Zhang, X., Zhou, M., & Lei, L. (2005) · Carbon · doi:10.1016/j.carbon.2005.02.013 · Cited by 179 · see citing works
Wang, W., da Silva, C. G., & Faria, J. L. (2006) · Applied Catalysis B: Environmental · doi:10.1016/j.apcatb.2005.11.034 · Cited by 162 · see citing works
Photoinduced transformations in semiconductormetal nanocomposite assemblies
Kamat, P. V. (2002) · Pure and Applied Chemistry · doi:10.1351/pac200274091693 · Cited by 147 · see citing works
Obeng, D. P., Morrell, S., & Napier-Munn, T. J. (2005) · International Journal of Mineral Processing · doi:10.1016/j.minpro.2005.01.002 · Cited by 145 · see citing works
Photocatalytic degradation of phenol using TiO2 nanocrystals supported on activated carbon
Carpio, E., Zúñiga, P., Ponce, S., et al. (2004) · Journal of Molecular Catalysis A Chemical · doi:10.1016/j.molcata.2004.09.066 · Cited by 141 · see citing works
TiO2 activation by using activated carbon as a support
Araña, J., Doña-Rodrı́guez, J. M., Rendón, E. T., Cabo, C. G. I., Dı́az, O. G., Melián, J. A. H., Pérez‐Peña, J., Colón, G., & Navío, J. A. (2003) · Applied Catalysis B: Environmental · doi:10.1016/s0926-3373(03)00075-4 · Cited by 132 · see citing works
Chen, Y., & Dionysiou, D. D. (2006) · Applied Catalysis A General · doi:10.1016/j.apcata.2006.10.025 · Cited by 126 · see citing works
Zaib, Q., Khan, I. A., Saleh, N. B., Flora, J. R. V., Park, Y.-G., & Yoon, Y. (2012) · Water Air & Soil Pollution · doi:10.1007/s11270-012-1109-5 · Cited by 92 · see citing works
Self-citationHwang, K., Lee, J., Shim, W., et al. (2011) · Advanced Powder Technology · doi:10.1016/j.apt.2011.05.010 · Cited by 75 · see citing works
Surface characteristics and photocatalytic activity of TiO2 loaded on activated carbon fibers
Yuan, R., Zheng, J., Guan, R., et al. (2005) · Colloids and Surfaces A Physicochemical and Engineering Aspects · doi:10.1016/j.colsurfa.2004.11.027 · Cited by 66 · see citing works
Staniszewska, M., Graca, B., & Nehring, I. (2015) · Chemosphere · doi:10.1016/j.chemosphere.2015.11.081 · Cited by 57 · see citing works
Anatase TiO 2 ‐Coated Multi‐Wall Carbon Nanotubes with the Vapor Phase Method
Fan, W., Gao, L., & Sun, J. (2005) · Journal of the American Ceramic Society · doi:10.1111/j.1551-2916.2005.00755.x · Cited by 55 · see citing works
Yoo, K. S., Choi, H., & Dionysiou, D. D. (2005) · Catalysis Communications · doi:10.1016/j.catcom.2005.01.010 · Cited by 54 · see citing works
Feng, W., Feng, Y., Wu, Z., et al. (2005) · Journal of Physics Condensed Matter · doi:10.1088/0953-8984/17/27/011 · Cited by 47 · see citing works
Khataee, A. (2009) · Green Sciences · doi:10.2478/v10026-009-0041-y · Cited by 35 · see citing works
Zaib, Q., Mansoor, B., & Ahmad, F. (2013) · Environmental Science Processes & Impacts · doi:10.1039/c3em00150d · Cited by 31 · see citing works
Self-citationKang, S., Cui, Z., & Mu, J. (2007) · Fullerenes Nanotubes and Carbon Nanostructures · doi:10.1080/15363830601177719 · Cited by 30 · see citing works
Ultrasonication Study for Suspending Single-Walled Carbon Nanotubes in Water
Zaib, Q., Khan, I. A., Yoon, Y., Flora, J. R. V., Park, Y.-G., & Saleh, N. B. (2012) · Journal of Nanoscience and Nanotechnology · doi:10.1166/jnn.2012.6212 · Cited by 21 · see citing works
Self-citationExperimental study of TiO2 nanoparticle adhesion to silica and Fe(III) oxide-coated silica surfaces
Dietrich, L. A. S., Sahu, M., Biswas, P., et al. (2012) · Chemical Geology · doi:10.1016/j.chemgeo.2012.09.043 · Cited by 12 · see citing works
Flagged first, then by citations
Research works printed but not linked: 2
- Raj K. J. A.; Viswanathan B. Effect of surface area, pore volume and particle size of P25 titania on the phase transformation of anatase to rutile. Indian J. Chem., Sect. A: Inorg., Bio-inorg., Phys., Theor. Anal. Chem. 2009, 48, 1378– 1382.
- Santos H. M.; Lodeiro C.; Capelo-Martínez J.-L. The Power of Ultrasound. In Ultrasound in Chemistry: Analytical Applications; Wiley-VCH Verlag GmbH & Co. KGaA: Berlin, 2009; pp 1– 16.
Cited by
Sorted by citations
Zaib, Q., & Kyung, D. (2022) · Scientific Reports · doi:10.1038/s41598-022-12787-0 · Cited by 28 · see citing works
Self-citation
- Authors
- Zaib, Q., Jouiad, M., & Ahmad, F.
- Affiliations
- Khalifa University of Science and Technology (AE)
- Corresponding author
- Ahmad, Farrukh
- Venue
- ACS Omega
- Publisher
- American Chemical Society (ACS)
- Published
- 2019-01-08
- Volume
- 4
- Issue
- 1
- Pages
- 535-545
- ISSN
- 2470-1343 (ISSN-L)
- PMC
- PMC6648941
- OpenAlex
- W2910069005
- Cited by
- 22
- References
- 52
- Citations by year
- 2026: 5 · 2025: 3 · 2024: 2 · 2022: 5 · 2021: 4 · 2020: 2 · 2019: 1
- FWCI
- 1.08
- Type
- journal article
- Language
- en
- Open access
- gold
- doi.org
- Licence
- Locations
- ACS Omega (publishedVersion, other-oa)
- PubMed Central (publishedVersion)
- PubMed (publishedVersion)
- HAL (submittedVersion)
- DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion, cc-by-sa)
- Funders
- Masdar Institute of Science and Technology
- Topics
- Physical Sciences › Materials Science › Materials Chemistry › Carbon Nanotubes in Composites
- Physical Sciences › Materials Science › Materials Chemistry › Ultrasound and Cavitation Phenomena
- Physical Sciences › Materials Science › Materials Chemistry › Mesoporous Materials and Catalysis
- Keywords
- multi-walled carbon nanotubes, titanium dioxide, sonochemical synthesis, sonochemical exfoliation, process optimization, composite stability
About these checks
Registry, retraction, Cites and statistics results are computed, not judged, with one exception: a printed reference that no index lists is read once by a model before it counts as a citation error. Claims are extracted by a model and kept only when their quote appears verbatim in the text; each cited source is then checked, with a model’s help, for whether it says what the claim relies on. Those verdicts can be wrong — read the claim’s quote and the cited source before relying on one.
Statistics and arithmetic are recomputed, not judged.
Confidence bands are shown only for fields calibrated on our annotated test set. None is calibrated yet, so no band is shown.
What counts as a claim ›How we measure confidence ›How we check this ›
Are you an author, or do you see a problem with this page? Request a review