Skip to main content Accessibility help
Hostname: page-component-99c86f546-4k54s Total loading time: 0.23 Render date: 2021-12-06T04:10:28.224Z Has data issue: true Feature Flags: { "shouldUseShareProductTool": true, "shouldUseHypothesis": true, "isUnsiloEnabled": true, "metricsAbstractViews": false, "figures": true, "newCiteModal": false, "newCitedByModal": true, "newEcommerce": true, "newUsageEvents": true }

A simple low-cost synthesis of brookite TiO2 nanoparticles

Published online by Cambridge University Press:  22 November 2012

Todd C. Monson*
Sandia National Laboratories, Albuquerque, New Mexico 87185
Mark A. Rodriguez
Sandia National Laboratories, Albuquerque, New Mexico 87185
Jean L. Leger
Sandia National Laboratories, Albuquerque, New Mexico 87185
Tyler E. Stevens
Sandia National Laboratories, Albuquerque, New Mexico 87185
Dale L. Huber
Sandia National Laboratories, Albuquerque, New Mexico 87185
a)Address all correspondence to this author. e-mail:
Get access


A new low-cost synthesis of brookite TiO2nanoparticles using isopropanol as both the solvent and ligand is described here. Other ligands can be bound to the titania surface during or postsynthesis to tailor the particles’ functionality. The often extremely rapid hydrolysis of titanium isopropoxide has been successfully controlled so that nanoparticle growth is achieved. The resulting 4-nm particles are nonagglomerated, stable in solution, and have a low polydispersity. The synthesis is scalable and enables the simple fabrication of large amounts of titania nanoparticles that do not scatter visible light and are highly suited for incorporation into optical composites.

Copyright © Materials Research Society 2012

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)


Arango, A.C., Carter, S.A., and Brock, P.J.: Charge transfer in photovoltaics consisting of interpenetrating networks of conjugated polymer and TiO2 nanoparticles. Appl. Phys. Lett. 74, 1698 (1999).CrossRefGoogle Scholar
Gratzel, M.: Photoelectrochemical cells. Nature 414, 338 (2001).CrossRefGoogle ScholarPubMed
Stark, W.J., Wegner, K., Pratsinis, S.E., and Baiker, A.: Flame aerosol synthesis of vanadia-titania nanoparticles: Structural and catalytic properties in the selective catalytic reduction of NO by NH3. J. Catal. 197, 182 (2001).CrossRefGoogle Scholar
Yu, J.C., Yu, J.G., Ho, W.K., and Zhang, L.Z.: Preparation of highly photocatalytic active nano-sized TiO2 particles via ultrasonic irradiation. Chem. Commun. 19, 1942 (2001).CrossRefGoogle Scholar
Martin, S.T., Herrmann, H., Choi, W.Y., and Hoffmann, M.R.: Time-resolved microwave conductivity. 1. TiO2 photoreactivity and size quantization. J. Chem. Soc., Faraday Trans. 90, 3315 (1994).CrossRefGoogle Scholar
Choi, W.Y., Termin, A., and Hoffmann, M.R.: The role of metal-ion dopants in quantum-sized TiO2 - correlation between photoreactivity and charge-carrier recombination dynamics. J. Phys. Chem. 98, 13669 (1994).CrossRefGoogle Scholar
Anpo, M., Shima, T., Kodama, S., and Kubokawa, Y.: Photocatalytic hydrogenation of CH3CCH with H2O on small-particle TiO2: Size quantization effects and reaction intermediates. J. Phys. Chem. 91, 4305 (1987).CrossRefGoogle Scholar
Feldmann, C. and Jungk, H.O.: Polyol-vermittelte präparation nanoskaliger oxidpartikel. Angew. Chem. 113, 372 (2001).3.0.CO;2-J>CrossRefGoogle Scholar
Yu, K.F., Zhao, J.Z., Guo, Y.P., Ding, X.F., Bala, H., Liu, Y.H., and Wang, Z.C.: Sol-gel synthesis and hydrothermal processing of anatase nanocrystals from titanium n-butoxide. Mater. Lett. 59, 2515 (2005).CrossRefGoogle Scholar
Huang, S.Y., Kavan, L., Exnar, I., and Gratzel, M.: Rocking chair lithium battery based on nanocrystalline TiO2 (anatase). J. Electrochem. Soc. 142, L142 (1995).CrossRefGoogle Scholar
Will, G., Rao, J.S.S.N., and Fitzmaurice, D.: Heterosupramolecular optical write-read-erase device. J. Mater. Chem. 9, 2297 (1999).CrossRefGoogle Scholar
Sotomayor, J., Will, G., and Fitzmaurice, D.: Photoelectrochromic heterosupramolecular assemblies. J. Mater. Chem. 10, 685 (2000).CrossRefGoogle Scholar
Frindell, K.L., Bartl, M.H., Popitsch, A., and Stucky, G.D.: Sensitized luminescence of trivalent europium by three-dimensionally arranged anatase nanocrystals in mesostructured titania thin films. Angew. Chem. 114, 1001 (2002).3.0.CO;2-8>CrossRefGoogle Scholar
Morrison, P.W., Raghavan, R., Timpone, A.J., Artelt, C.P., and Pratsinis, S.E.: In situ Fourier transform infrared characterization of the effect of electrical fields on the flame synthesis of TiO2 particles. Chem. Mater. 9, 2702 (1997).CrossRefGoogle Scholar
Yang, G.X., Zhuang, H.R., and Biswas, P.: Characterization and sinterability of nanophase titania particles processed in flame reactors. Nanostruct. Mater. 7, 675 (1996).CrossRefGoogle Scholar
Seifried, S., Winterer, M., and Hahn, H.: Nanocrystalline titania films and particles by chemical vapor synthesis. Chem. Vap. Deposition 6, 239 (2000).3.0.CO;2-Q>CrossRefGoogle Scholar
Aruna, S.T., Tirosh, S., and Zaban, A.: Nanosize rutile titania particle synthesis via a hydrothermal method without mineralizers. J. Mater. Chem. 10, 2388 (2000).CrossRefGoogle Scholar
Cheng, H.M., Ma, J.M., Zhao, Z.G., and Qi, L.M.: Hydrothermal preparation of uniform nanosize rutile and anatase particles. Chem. Mater. 7, 663 (1995).CrossRefGoogle Scholar
Reddy, K.M., Guin, D., Manorama, S.V., and Reddy, A.R.: Selective synthesis of nanosized TiO2 by hydrothermal route: Characterization, structure property relation, and photochemical application. J. Mater. Res. 19, 2567 (2004).CrossRefGoogle Scholar
Reddy, K.M., Manorama, S.V., and Reddy, A.R.: Band gap studies on anatase titanium dioxide nanoparticles. Mater. Chem. Phys. 78, 239 (2003).CrossRefGoogle Scholar
Wang, C.C. and Ying, J.Y.: Sol-gel synthesis and hydrothermal processing of anatase and rutile titania nanocrystals. Chem. Mater. 11, 3113 (1999).CrossRefGoogle Scholar
Lim, K.T., Hwang, H.S., Ryoo, W., and Johnston, K.P.: Synthesis of TiO2 nanoparticles utilizing hydrated reverse micelles in CO2. Langmuir 20, 2466 (2004).CrossRefGoogle Scholar
Spatz, J., Mossmer, S., Moller, M., Kocher, M., Neher, D., and Wegner, G.: Controlled mineralization and assembly of hydrolysis-based nanoparticles in organic solvents combining polymer micelles and microwave techniques. Adv. Mater. 10, 473 (1998).3.0.CO;2-Q>CrossRefGoogle ScholarPubMed
Niederberger, M., Bartl, M.H., and Stucky, G.D.: Benzyl alcohol and titanium tetrachloride - a versatile reaction system for the nonaqueous and low-temperature preparation of crystalline and luminescent titania nanoparticles. Chem. Mater. 14, 4364 (2002).CrossRefGoogle Scholar
Trentler, T.J., Denler, T.E., Bertone, J.F., Agrawal, A., and Colvin, V.L.: Synthesis of TiO2 nanocrystals by nonhydrolytic solution-based reactions. J. Am. Chem. Soc. 121, 1613 (1999).CrossRefGoogle Scholar
Vioux, A.: Nonhydrolytic sol-gel routes to oxides. Chem. Mater. 9, 2292 (1997).CrossRefGoogle Scholar
Cassaignon, S., Koelsch, M., and Jolivet, J-P.: Selective synthesis of brookite, anatase and rutile nanoparticles: Thermolysis of TiCl4 in aqueous nitric acid. J. Mater. Sci. 42, 6689 (2007).CrossRefGoogle Scholar
Kandiel, T.A., Feldhoff, A., Robben, L., Dillert, R., and Bahnemann, D.W.: Tailored titanium dioxide nanomaterials: Anatase nanoparticles and brookite nanorods as highly active photocatalysts. Chem. Mater. 22, 2050 (2010).CrossRefGoogle Scholar
Kobayashi, M., Tomita, K., Petrykin, V., Yoshimura, M., and Kakihana, M.: Direct synthesis of brookite-type titanium oxide by hydrothermal method using water-soluble titanium complexes. J. Mater. Sci. 43, 2158 (2008).CrossRefGoogle Scholar
Lin, H., Li, L., Zhao, M., Huang, X., Chen, X., Li, G., and Yu, R.: Synthesis of high-quality brookite TiO2 single-crystalline nanosheets with specific facets exposed: Tuning catalysts from inert to highly reactive. J. Am. Chem. Soc. 134, 8328 (2012).CrossRefGoogle ScholarPubMed
Morishinia, Y., Kobayashi, M., Petrykin, V., Kakihana, M., and Tomita, K.: Microwave-assisted hydrothermal synthesis of brookite nanoparticles from a water-soluble titanium complex and their photocatalytic activity. J. Ceram. Soc. Jpn. 115, 826 (2007).CrossRefGoogle Scholar
Murakami, N., Kamai, T.-a., Tsubota, T., and Ohno, T.: Novel hydrothermal preparation of pure brookite-type titanium(IV) oxide nanocrystal under strong acidic conditions. Catal. Commun. 10, 963 (2009).CrossRefGoogle Scholar
Ohno, Y., Tomita, K., Komatsubara, Y., Taniguchi, T., Katsumata, K-I., Matsushita, N., Kogure, T., and Okada, K.: Pseudo-cube shaped brookite (TiO2) nanocrystals synthesized by an oleate-modified hydrothermal growth method. Cryst. Growth Des. 11, 4831 (2011).CrossRefGoogle Scholar
Tang, J., Redl, F., Zhu, Y.M., Siegrist, T., Brus, L.E., and Steigerwald, M.L.: An organometallic synthesis of TiO2 nanoparticles. Nano Lett. 5, 543 (2005).CrossRefGoogle Scholar
Qiu, X., Thompson, J.W., and Billinge, S.J.L.: PDFgetX2: A GUI-driven program to obtain the pair distribution function from x-ray powder diffraction data. J. Appl. Crystallogr. 37, 678 (2004).CrossRefGoogle Scholar
Farrow, C.L., Juhas, P., Liu, J.W., Bryndin, D., Božin, E.S., Bloch, J., Proffen, T., and Billinge, S.J.L.: PDFfit2 and PDFgui: Computer programs for studying nanostructure in crystals. J. Phys. Condens. Matter 19, 335219 (2007).CrossRefGoogle ScholarPubMed
Turova, N.Y., Turevskaya, E.P., Kessler, V.G., and Yanovskaya, M.I.: The Chemistry of Metal Alkoxides (Kluwer Academic Publishers, New York, NY, 2002); pp. 107125.Google Scholar
Kotov, N.A., Meldrum, F.C., and Fendler, J.H.: Monoparticulate layers of titanium dioxide nanocrystallites with controllable interparticle distances. J. Phys. Chem. 98, 8827 (1994).CrossRefGoogle Scholar
Hague, D.C. and Mayo, M.J.: Controlling crystallinity during processing of nanocrystalline titania. J. Am. Ceram. Soc. 77, 1957 (1994).CrossRefGoogle Scholar
Stallings, W.E. and Lamb, H.H.: Synthesis of nanostructured titania powders via hydrolysis of titanium isopropoxide in supercritical carbon dioxide. Langmuir 19, 2989 (2003).CrossRefGoogle Scholar
Koelsch, M., Cassaignon, S., Guillemoles, J.F., and Jolivet, J.R.: Comparison of optical and electrochemical properties of anatase and brookite TiO2 synthesized by the sol-gel method. Thin Solid Films 403, 312 (2002).CrossRefGoogle Scholar
Henderson, M.A.: A surface science perspective on photocatalysis. Surf. Sci. Rep. 66, 185 (2011).CrossRefGoogle Scholar

Send article to Kindle

To send this article to your Kindle, first ensure is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about sending to your Kindle. Find out more about sending to your Kindle.

Note you can select to send to either the or variations. ‘’ emails are free but can only be sent to your device when it is connected to wi-fi. ‘’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

A simple low-cost synthesis of brookite TiO2 nanoparticles
Available formats

Send article to Dropbox

To send this article to your Dropbox account, please select one or more formats and confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your <service> account. Find out more about sending content to Dropbox.

A simple low-cost synthesis of brookite TiO2 nanoparticles
Available formats

Send article to Google Drive

To send this article to your Google Drive account, please select one or more formats and confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your <service> account. Find out more about sending content to Google Drive.

A simple low-cost synthesis of brookite TiO2 nanoparticles
Available formats

Reply to: Submit a response

Please enter your response.

Your details

Please enter a valid email address.

Conflicting interests

Do you have any conflicting interests? *