Inorganics 2014, 2(3), 410-423; doi:10.3390/inorganics2030410
Article

Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling

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Received: 8 May 2014; in revised form: 2 July 2014 / Accepted: 14 July 2014 / Published: 4 August 2014
(This article belongs to the Special Issue Innovative Inorganic Synthesis)
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Abstract: Innovative synthetic approaches should be simple and environmentally friendly. Here, we present the surface modification of inorganic submicrometer particles with long alkyl chain organophosphorus coupling agents without the need of a solvent, which makes the technique environmentally friendly. In addition, it is of great benefit to realize two goals in one step: size reduction and, simultaneously, surface functionalization. A top-down approach for the synthesis of metal oxide particles with in situ surface functionalization is used to modify titania with long alkyl chain organophosphorus coupling agents. A high energy planetary ball mill was used to perform reactive milling using titania as inorganic pigment and long alkyl chain organophosphorus coupling agents like dodecyl and octadecyl phosphonic acid. The final products were characterized by IR, NMR and X-ray fluorescence spectroscopy, thermal and elemental analysis as well as by X-ray powder diffraction and scanning electron microscopy. The process entailed a tribochemical phase transformation from the starting material anatase to a high-pressure modification of titania and the thermodynamically more stable rutile depending on the process parameters. Furthermore, the particles show sizes between 100 nm and 300 nm and a degree of surface coverage up to 0.8 mmol phosphonate per gram.
Keywords: reactive milling; titania particles; long alkyl chain organophosphorus coupling agents; tribochemical phase transition
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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MDPI and ACS Style

Betke, A.; Kickelbick, G. Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling. Inorganics 2014, 2, 410-423.

AMA Style

Betke A, Kickelbick G. Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling. Inorganics. 2014; 2(3):410-423.

Chicago/Turabian Style

Betke, Annika; Kickelbick, Guido. 2014. "Long Alkyl Chain Organophosphorus Coupling Agents for in Situ Surface Functionalization by Reactive Milling." Inorganics 2, no. 3: 410-423.

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