Gas-Phase Deposition of Thin Aluminium Oxide Films at Ambient Conditions David Valdesueiro

153 Pages·2016·10.07 MB·English

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Gas-phase Deposition
of Thin Aluminium Oxide Films
at Ambient Conditions

Proefschrift

ter verkrijging van de graad van doctor
aan de Technische Universiteit Delft,
op gezag van Rector Magnificus prof. ir. K.C.A.M. Luyben,
voorzitter van het College van Promoties,
in het openbaar te verdedigen op

woensdag 4 november 2015
om 12:30 uur

door

David VALDESUEIRO

Ingeniero Químico
Universidad de Valladolid, Spanje
geboren te León, Spanje
This dissertation has been approved by the
promotor: Prof. dr. ir. M. T. Kreutzer
copromotor: Dr. ir. J. Ruud van Ommen
copromotor: Dr. ir. Gabrie M. H. Meesters

Composition of the doctoral committee:

Rector Magnificus chairman
Prof. dr. ir. Michiel T. Kreutzer Technische Universiteit Delft, promotor
Dr. ir. J. Ruud van Ommen Technische Universiteit Delft, copromotor
Dr. ir. Gabrie M.H. Meesters Technische Universiteit Delft, copromotor

Independent members:
Prof. dr. Andreas Schmidt-Ott, Technische Universiteit Delft
Prof. dr. Christophe Detarvernier Universiteit Gent
Prof. dr. Mato Knez CIC nanoGUNE
Dr. Rob Geertman DSM Fibre Intermediates
Prof. dr. Stephen J. Picken Technische Universiteit Delft, reserve

The research reported in this thesis was conducted in the Product and Process
Engineering section of the Chemical Engineering department, Faculty of Applied
Sciences (TNW) of the Delft University of Technology and received funding from the
European Union Seventh Framework Program FP7/2007-2013 under grant agreement
no. 26722, and from Royal DSM.

ISBN: 978-94-6186-564-9
Copyright © 2015 by David Valdesueiro
Printed in The Netherlands by CPI Wöhrmann Print Service

All rights reserved. Parts of this thesis are published in scientific journals and
copyright is subjected to different terms and conditions.
To my parents

Contents

Summary xi

Samenvatting xv

1. Introduction 1
1.1 Research Field . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.1.1 Particle technology . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.1.2 Coating techniques for particles . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.1.3 Atomic Layer Deposition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.1.4 Fluidization of particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
1.2 Objectives of this study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
1.3 Outline . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

2. Gas-phase deposition of ultrathin Al O films on nanoparticles at ambient 13
2 3
conditions
2.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.2 Experimental section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.2.1 Experimental setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.2.2 Design of experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.2.3 Characterization of the coating . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
2.3.1 Base case coating experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
2.3.2 Coating with excess of precursors at ambient conditions . . . . . . . . 19
2.3.3 Coating with excess of precursors at 1 bar and 170 °C . . . . . . . . . 21
2.3.4 Alumina film density . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
2.4 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Supplementary information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
v
Contents

3. Tuning roughness and gloss of powder coating paint by encapsulating the 35
particles with Al O films
2 3
3.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
3.2 Experimental section . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
3.2.1 Experimental setup and compounds . . . . . . . . . . . . . . . . . . . . . . . . 37
3.2.2 Coating experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
3.2.3 Characterization of the coated particles and panels . . . . . . . . . . . . 38
3.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
3.3.1 Characterization of the coated particles . . . . . . . . . . . . . . . . . . . . . 38
3.3.2 Characterization of the sprayed panels . . . . . . . . . . . . . . . . . . . . . . 45
3.4 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Supplementary information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

4. The deposition mechanism of Al O on QD films at atmospheric pressure and 69
2 3
room temperature
4.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70
4.2 Experimental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
4.2.1 PbSe QD solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71
4.2.2 EDA in ethanol solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
4.2.3 Quartz substrate . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
4.2.4 Fabrication of QD films . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
4.2.5 Alumina coating reactor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 72
4.2.6 Alumina coating precursors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
4.2.7 Alumina coating experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
4.2.8 Characterization of the deposition of Al O . . . . . . . . . . . . . . . . . . 73
2 3
4.2.9 Characterization of the air stability of the coated QD films . . . . . . 74
4.2.10 Preparation of the dodecanethiol self-assembled monolayer . . . . . 74
4.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
4.3.1 Deposition of Al O using water as precursor . . . . . . . . . . . . . . . . 75
2 3
4.3.2 Estimation of the growth per cycle of Al O . . . . . . . . . . . . . . . . . . 77
2 3
4.3.3 Study of the deposition mechanism of Al O . . . . . . . . . . . . . . . . . 77
2 3
4.3.4 Study of the reaction of TMA on a dodecanethiol SAM . . . . . . . . . 77
vi
Contents

4.3.5 XPS depth profile of an uncoated QD film . . . . . . . . . . . . . . . . . . . 78
4.3.6 Reaction between TMA and amine groups . . . . . . . . . . . . . . . . . . . 80
4.3.7 Study of the air stability of Al O -coated QD films . . . . . . . . . . . . 80
2 3
4.3.8 Study of the deposition of Al O using synthetic air as oxidiser . . 81
2 3
4.4 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82
Supplementary information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87

5. Producing SiC tracer particles using gas-phase deposition of Al O at ambient 91
2 3
conditions
5.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
5.2 Experimental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
5.3 Results and discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
5.4 Conclusions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
Supplementary information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 104

6. Outlook 111
6.1 Open questions and complementary studies . . . . . . . . . . . . . . . . . . . . . . . . 112
6.1.1 Optimization of the results obtained in the previous chapters . . . . 112
6.1.2 Characterization of the strength of the alumina coating . . . . . . . . . 114
6.1.3 Necessity for accurate characterization techniques . . . . . . . . . . . . . 115
6.1.4 Industrial implementation of ALD on powders . . . . . . . . . . . . . . . . 116
6.1.5 Investigation of the interparticle forces . . . . . . . . . . . . . . . . . . . . . . 117
6.1.6 Study of different fluidization assistance methods . . . . . . . . . . . . . 117
6.2 Broadening the applicability of this work . . . . . . . . . . . . . . . . . . . . . . . . . . 118
6.2.1 Deposition of other compounds at ambient conditions . . . . . . . . . 118
6.2.2 Biocompatibility study of ultrathin films . . . . . . . . . . . . . . . . . . . . 118
6.3 Analysis of ALD for product development . . . . . . . . . . . . . . . . . . . . . . . . . 119

List of publications 125

Acknowledgements 127

Curriculum vitae 131

vii