Issue 35, 2013

Focused radiation heating for controlled high temperature chemistry, exemplified with the preparation of vanadium nitride nanoparticles

Abstract

A compact apparatus employing heating with concentrated light was designed for desktop laboratory application to run syntheses in the range 200–850 °C in short times under a satisfying control of the temperature, heating ramps, and adjustable chemical environments. The device is composed of 4 halogen lamps oriented to a centre point and allows fast heating rates up to 100 K min−1 of medium size scale samples (volume < 7 mL). This method can be proven to be more energetically efficient and allows for better temperature control over standard furnace methods. Herein we exemplify with a typical high temperature synthesis of non-oxide ceramic (vanadium nitride) nanoparticles. These nanoparticles can be obtained in different sizes and crystallinity ranges by varying the reaction conditions, following the urea glass route and applying the non-classical rapid heating method. Nanoparticles containing both carbon and nitrogen and showing the typical crystal structure of VN were obtained with sizes below 10 nm within a short reaction time (5 min at 750 °C) and in a fast heating procedure (50 K min−1). Moreover, quasi-quenching of samples through a fast cooling procedure allows the detection of various intermediate oxide species that otherwise were not observed.

Graphical abstract: Focused radiation heating for controlled high temperature chemistry, exemplified with the preparation of vanadium nitride nanoparticles

Supplementary files

Article information

Article type
Paper
Submitted
01 Mar 2013
Accepted
12 Jun 2013
First published
13 Jun 2013

RSC Adv., 2013,3, 15337-15343

Focused radiation heating for controlled high temperature chemistry, exemplified with the preparation of vanadium nitride nanoparticles

T. C. M. Corbiere, D. Ressnig, C. Giordano and M. Antonietti, RSC Adv., 2013, 3, 15337 DOI: 10.1039/C3RA41040D

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