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The evolution of powder particle size, crystal structure, and surface chemistry was evaluated for micron scale NiO powders subjected to impact milling with commonly employed milling additives: methanol, Vertrel XF, and amorphous carbon. The effect of the different comminution protocols on sintered body microstructure was evaluated for high temperature sintering in inert atmosphere (N2). X-ray photoelectron spectroscopy showed that NiO powder surface chemistry is surprisingly sensitive to milling additive choice. In particular, the proportion of powder surface defect sites varied with additive, and methanol left an alcohol or alkoxy residue even after drying. Upon sintering to intermediate temperatures (1100 ℃), scanning electron microscopy (SEM) showed that slurry milled NiO powders exhibit hindered sintering behaviors. This effect was amplified for NiO milled with methanol, in which sub-500 nm grain sizes dominated even after sintering to 1100 ℃. Upon heating to high temperatures (1500 ℃), simultaneous differential scanning calorimetry/thermogravimetric analysis (DSC/TGA) showed that the powders containing carbon residues undergo carbothermal reduction, resulting in a melting transition between 1425 and 1454 ℃. Taken together, the results demonstrated that when processing metal oxide powders for advanced ceramics, the choice of milling additive is crucial as it exerts significant control over sintered body microstructure.


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The effect of milling additives on powder properties and sintered body microstructure of NiO

Show Author's information L. Jay DEINERa( )Michael A. ROTTMAYERbBryan C. EIGENBRODTc
Department of Chemistry, New York City College of Technology, City University of New York,300 Jay St., Brooklyn, NY 11201, USA
The Air Force Research Labs, Wright-Patterson Air Force Base, OH 45433, USA
Department of Chemistry, Villanova University, 800 E. Lancaster Ave., Villanova, PA 19085, USA

Abstract

The evolution of powder particle size, crystal structure, and surface chemistry was evaluated for micron scale NiO powders subjected to impact milling with commonly employed milling additives: methanol, Vertrel XF, and amorphous carbon. The effect of the different comminution protocols on sintered body microstructure was evaluated for high temperature sintering in inert atmosphere (N2). X-ray photoelectron spectroscopy showed that NiO powder surface chemistry is surprisingly sensitive to milling additive choice. In particular, the proportion of powder surface defect sites varied with additive, and methanol left an alcohol or alkoxy residue even after drying. Upon sintering to intermediate temperatures (1100 ℃), scanning electron microscopy (SEM) showed that slurry milled NiO powders exhibit hindered sintering behaviors. This effect was amplified for NiO milled with methanol, in which sub-500 nm grain sizes dominated even after sintering to 1100 ℃. Upon heating to high temperatures (1500 ℃), simultaneous differential scanning calorimetry/thermogravimetric analysis (DSC/TGA) showed that the powders containing carbon residues undergo carbothermal reduction, resulting in a melting transition between 1425 and 1454 ℃. Taken together, the results demonstrated that when processing metal oxide powders for advanced ceramics, the choice of milling additive is crucial as it exerts significant control over sintered body microstructure.

Keywords:

nickel oxide, impact milling, sintering, densification, grain growth
Received: 15 December 2014 Revised: 26 February 2015 Accepted: 27 February 2015 Published: 30 May 2015 Issue date: June 2015
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Publication history
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Publication history

Received: 15 December 2014
Revised: 26 February 2015
Accepted: 27 February 2015
Published: 30 May 2015
Issue date: June 2015

Copyright

© The author(s) 2015

Acknowledgements

The authors thank the N.Y.S. Graduate Research and Teaching Initiative (GRTI) for financial support. L. J. D. thanks the Air Force Summer Faculty Fellowship program for fellowship support. The authors thank the Advanced Imaging Facility of the College of Staten Island for SEM images, and Prof. William L’Amoreaux and Dr. Mike Bucaro for their help with SEM images.

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