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Publié par | rheinisch-westfalischen_technischen_hochschule_-rwth-_aachen |
Publié le | 01 janvier 2011 |
Nombre de lectures | 25 |
Langue | English |
Poids de l'ouvrage | 32 Mo |
Extrait
Fabrication of nanostructured materials and
their applications
Von der Fakulta¨t fu¨r Mathematik, Informatik und
Naturwissenschaften der RWTH Aachen University
zur Erlangung des akademischen Grades einer
Doktorin der Naturwissenschaften genehmigte Dissertation
vorgelegt von
Master of Science
Lindarti Purwaningsih
aus Sragen, Indonesia
Berichter: Prof. Dr. Martin Mo¨ller
Prof. Dr. Joachim P. Spatz
Tag der mu¨ndlichen Pru¨fung: 12. Januar 2011
Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek
online verfu¨gbar.Fabrication of nanostructured materials and
their applications
Dissertation
accepted by the
Faculty of Mathematics, Computer Science, and the Natural Sciences
of the Rheinisch-Westf¨alische Technische Hochschule Aachen
University, Germany for the degree of
Doctor of Natural Sciences
by
Master of Science
Lindarti Purwaningsih
born in Sragen, Indonesia
Referees: Prof. Dr. Martin Mo¨ller
Prof. Dr. Joachim P. Spatz
Oral examination: January 12, 2011
This dissertation is available online in the university library.Lindarti Purwaningsih
Fabrication of nanostructured
materials and their applications
D 82 (Diss. RWTH Aachen University, 2011)
Max Planck Institute for Metals Research
Department of New Materials and Biosystems, Stuttgart
2011This dissertation is dedicated to my parents:
Purwoatmojo & Sunarti
People who believe in education as a way on making
a better life and a better World.iv
The journey of life is to learn...
until we are wise enough to remember...
home.
-Aryani Willems-Contents
Summary 1
General introduction 3
General methods 5
2.1 Lithographies for nanostructure fabrication . . . . . . . . . . . . . . . . . . 5
2.2 Etching process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.2.1 Wet etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.2.2 Dry etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.3 Scanning Electron Microscopy (SEM) . . . . . . . . . . . . . . . . . . . . . 9
2.4 Image analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.4.1 Voronoi diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
2.4.2 Radial Distribution Function (RDF) . . . . . . . . . . . . . . . . . . 14
I Fabrication of nanopillar arrays and their applications 17
3 Introduction 19
3.1 The basic principle of antireflective surfaces . . . . . . . . . . . . . . . . . . 19
3.2 Cellular response to nanoscale topography . . . . . . . . . . . . . . . . . . . 22
3.3 Block copolymer micelle nanolithography (BCML) . . . . . . . . . . . . . . 23
4 Materials & methods 27
4.1 Fabrication of nanopillar arrays for antireflective surface applications . . . . 27
4.1.1 Synthesis of particle seeds inside the micellar cores . . . . . . . . . . 27
4.1.2 Nanoparticle enlargement by electroless deposition using hydroxy-
lamine . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.1.3 Reactive Ion Etching (RIE) for the fabrication of high aspect ratio
nanopillars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
4.2 Synthesis of nanopillar arrays with gold on top for biological applications . 29
4.2.1 Synthesis of gold nanoparticle arrays . . . . . . . . . . . . . . . . . . 29
4.2.2 Light-assisted nanoparticles enlargement . . . . . . . . . . . . . . . . 29
4.2.3 RIE for fabrication of cone-shaped nanopillars . . . . . . . . . . . . 29
vvi Contents
5 Nanopillar arrays 31
5.1 Fabrication of gold nanoparticle etching masks by BCML . . . . . . . . . . 31
5.2 Quartz vs. glass nanopillars . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
5.3 Influence of the etching parameters on nanopillar profiles . . . . . . . . . . 38
5.4 Silica nanopillar with gold on top . . . . . . . . . . . . . . . . . . . . . . . . 41
6 Applications 47
6.1 Antireflective surfaces . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
6.2 Biological application . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
7 Conclusions & Outlook 53
II Fabrication of particle and nanopore arrays and their applications 57
8 Introduction 59
8.1 Electrochemical biosensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
8.2 Colloidal lithography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
9 Materials & methods 65
9.1 Sensor chip fabrication . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
9.2 Colloidal lithography . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
9.3 Particle size reduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
9.4 Particle removal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
9.5 Reactive Ion Etching . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68
10 Fabrication of particle and nanopore arrays 69
10.1 Particle arrays by colloidal lithography . . . . . . . . . . . . . . . . . . . . . 69
10.2 Tunable size of particle mask arrays . . . . . . . . . . . . . . . . . . . . . . 72
10.3 Nanoporous thin gold layers . . . . . . . . . . . . . . . . . . . . . . . . . . . 74
10.4 Deep nanopore arrays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
11 Application 81
11.1 Electrochemical biosensor . . . . . . . . . . . . . . . . . . . . . . . . . . . . 81
11.2 Functionalization of nanopores . . . . . . . . . . . . . . . . . . . . . . . . . 84
12 Conclusions & outlook 87
III Porous silicon photonic crystal display 89
13 Introduction 91
13.1 Porous silicon . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91
13.1.1 Fabrication of porous silicon. . . . . . . . . . . . . . . . . . . . . . . 91
13.1.2 Reflectivity of porous silicon . . . . . . . . . . . . . . . . . . . . . . 93
13.2 Porous silicon photonic crystals . . . . . . . . . . . . . . . . . . . . . . . . . 94
13.2.1 Porous silicons display . . . . . . . . . . . . . . . . . . . . . . . . . . 95Contents vii
14 Materials & methods 97
14.1 Electrochemical etching (first layer - photonic crystal) . . . . . . . . . . . . 97
14.2 Surface modification . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
14.3 Electrochemical etching (second layer) . . . . . . . . . . . . . . . . . . . . . 98
14.4 Silver impregnation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
14.5 Electrochemical cell experiment . . . . . . . . . . . . . . . . . . . . . . . . . 99
14.6 Reflectivity measurement . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
14.7 Fourier-Transform Infrared spectroscopy . . . . . . . . . . . . . . . . . . . . 100
15 Porous silicon photonic crystal displays 101
15.1 Preparation of porous silicon photonic crystal displays . . . . . . . . . . . . 101
15.2 Performance of photonic crystal display . . . . . . . . . . . . . . . . . . . . 108
16 Conclusions & outlook 111
List of figures 113
Bibliography 123
Acknowledgements 141
IV Appendix 143
Appendix 145
1 Abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145
2 Symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146
3 Computing the total surface area of cone-shaped nanostructures . . . . . . 147Summary
Advances in fabrication of nanostructured materials offer the promise of new multifunc-
tional systems. This is owing to the abundance of novel physical, chemical, and biological
properties that can be exhibited, making nanostructured materials a fundamentally excit-
ing and technologically relevant area of research. By manipulating structure and proper-
ties on the nanometer scale, an extensive range of structural and functional applications
become available. Nanostructured materials can achieve alternate functions (i.e., antire-
flection), in addition to nanoscale manipulations of other entities (e.g., cell attachment
platforms, or biosensors). In this work, the fabrication of nanostructured arrays has been
studied and their utility in a number of applications has been demonstrated. This thesis
is divided into three Parts; each Part details the fabrication and applications of one of the
nanostructure types: nanopillars, ordered nanopores and unordered nanopores.
In Part I, the fabrication and applications of nanopillar arrays are discussed. The fabri-
cation of the nanopillar arrays was investigated on diverse substrates using a combination
ofmethods: blockcopolymermicellelithography(BCML),reactiveionetching(RIE),and
particle enlargement techniques. BCML resulted in ordered gold nanoparticle arrays with
inter-particle spacing which was modified from 50 to 120 nm. The gold nanoparticles sub-
sequently acted as an etching mask during RIE, which removed the surrounding material
resultinginthe’nanopillar’structures. Anintermediatesteptoenlargethegoldnanoparti-
cleswasnecessaryforproducinghigheraspectrationanopillarsandproducinggold-topped
nanopillars (where the initial gold particle was not completely etched away during RIE).
The employment of this combination of techniques, in addition to the different substrate
materials, resulted in a vast variety of nanostructure profiles, e.g., conical structures on
glass and cylindrical structures on quartz. It was deter