Direct galvanic metallization of insulating substrates [Elektronische Ressource] : mechanism and applications for microstructuring / Thanh Tung Mai

Direct galvanic metallization of insulating substrates [Elektronische Ressource] : mechanism and applications for microstructuring / Thanh Tung Mai

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Direct Galvanic Metallization of insulating Substrates: Mechanism and Applications for Microstructuring Inaugural - Dissertation zur Erlangung des Doktorgrades der Mathematischen-Naturwissenschaftlichen Fakultät der Heinrich-Heine-Universität Düsseldorf Thanh Tung Mai aus Hanoi Düsseldorf 2003 Gedruckt mit Genehmigung der Mathematisch-Naturwissenschaflichen Fakultät der Heinrich- Heine-Universität Düsseldorf Erster Gutachter: Prof. Dr. J. W. Schultze Zweiter Gutachter: PD. Dr. G. Staikov Dritter Gutachter: Prof. Dr. K. Schierbaum Tag der mündlichen Prüfung: 18.06.2003 This work was performed at the Institute für Physikalische Chemie und Elektrochemie at the Heinrich-Heine-Universität Düsseldorf under the supervision of Prof. Dr. J.W. Schultze. Research of the PLATO technique is carried out in the frame of the project “Elektroschemische Mikro- und Nanosysteme”(ElMiNoS) of the state Nordrhein Westfallen (Germany), in cooperation with the company ENTHONE GmbH (Langenfeld). Research of the composite material phosphate/PEDT was supported by the Gottlieb-Daimler und Karl Benz Stiftung.

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Direct Galvanic Metallization of insulating Substrates:
Mechanism and Applications for Microstructuring











Inaugural - Dissertation
zur
Erlangung des Doktorgrades der
Mathematischen-Naturwissenschaftlichen Fakultät
der Heinrich-Heine-Universität Düsseldorf













Thanh Tung Mai

aus Hanoi




Düsseldorf 2003







































Gedruckt mit Genehmigung der Mathematisch-Naturwissenschaflichen Fakultät der Heinrich-
Heine-Universität Düsseldorf

Erster Gutachter: Prof. Dr. J. W. Schultze
Zweiter Gutachter: PD. Dr. G. Staikov
Dritter Gutachter: Prof. Dr. K. Schierbaum
Tag der mündlichen Prüfung: 18.06.2003















































































This work was performed at the Institute für Physikalische Chemie und Elektrochemie at the
Heinrich-Heine-Universität Düsseldorf under the supervision of Prof. Dr. J.W. Schultze.
Research of the PLATO technique is carried out in the frame of the project
“Elektroschemische Mikro- und Nanosysteme”(ElMiNoS) of the state Nordrhein Westfallen
(Germany), in cooperation with the company ENTHONE GmbH (Langenfeld). Research of
the composite material phosphate/PEDT was supported by the Gottlieb-Daimler und Karl
Benz Stiftung. Financial and technological supports of those organizations are acknowledged.




During the years that I have worked with this thesis, I have had the opportunity to work with a
quite large number of people to whom I would like to express my deepest gratitude. I would
also like to thank them not just for their work, but also for their support and company during
my stay in Germany.

I am specially thankful to my supervisor Prof. Dr. J.W. Schultze for his guidance throughout
my PhD study, his precious supports in difficult phases, for the freedom in working with
many topics and methods as well as chances to publicize and present my works in scientific
conferences.

I am also grateful to PD. Dr. G. Staikov for a lot of exciting discussions and motivations, and
his acceptance to reference my work.

I appreciate my colleges C. Stromberg and A. Kurowski, not only for our together working
and interesting scientific discussions, but also for their helpful supports at any time I need
them, for the wonderful atmosphere, table tennis and café.

I would like to give my special thanks to Frau Hofmann, who always helped me kindly and
remembered my birthdays, which I always forgot.

I would like to thank all institute members for the warm atmosphere, and for their helpful and
joyful activities.

I want to thank my parents, my brothers and sisters for the remote support during my stay in
Germany.

Last, but not least, I am grateful to my beloved wife, Ky, for all the love I have been
privileged from you, your patience and understanding. You have been wonderful and I would
not change you for anything.

















































LIST OF PUBLICATIONS

?? T.T. Mai, J.W. Schultze, G. Staikov
“ Relation between Surface Preconditioning and Metal Deposition in Direct Galvanic
Metallization of Insulating Surfaces“
Solid State Electrochemistry, printed

??
“Microstructured Metallization of insulating polymers “
Electrochimica Acta, printed

?? T.T. Mai, J.W. Schultze, G. Staikov
”Deposition Mechanism of Metals in Direct Galvanic Metallization of Insulating
Substrates using metal sulphide”
in preparation

and further publications

ORAL PRESENTATIONS

?? T.T. Mai, N. Müller und J.W. Schultze
„ Influence of Electrolyte on the Formation of Phosphate Layer and Formation of
Composite Phosphate-Conducting Polymers“
INTERFINISH 2000, 13.-15. September 2000, Garmisch-Partenkirchen

?? T.T. Mai, G. Staikov, J.W. Schultze
“Microstructuring and Metallization of insulating Polymers by PLATO-Technique”
Joint Meeting of International Society of Electrochemistry (ISE) and The
Electrochemical Society (ESC), 1.-9. September 2001, San Francisco (USA)

?? T.T. Mai, G. Staikov, J.W. Schultze
“Application of PLATO-Technique for Microstructured Mettalization of Polymers in
Electronics”
European Academy of Surface Technology Forum (EAST), 10.-13. October 2001,
Chalkidiki (Greece)



Further presentations

?? T.T. Mai, J.W. Schultze, G. Staikov
“Mechanismus der Metallisierung von Kunststoffen nach dem PLATO-Verfahren”
75. AGEF-Seminar Elektochemische Oberflächen-, Mikro- und Nanotechnology,
6.Juni 2003, Fa. Enthone-OMI, Langenfeld
??
“Direct metallization of insulating polymers using metal sulphide and applications for
microstructuring”
Oberflächentage 2003, 17. - 19. September 2003, Bremen
?? T.T. Mai, J.W. Schultze, G. Staikov
“Direkt Metallisierung isolierender Kunststoffe mittels PLATO-Verfahren und
Anwendung zur Mikrostrukturierung“
Jahrestagung der Gesellschaft Deutscher Chemiker (GDCh), 6.-11. October 2003,
München

POSTER PRESENTATIONS

?? T.T.Mai, J.W.Schultze
„ Composite Phosphate-Conducting Polymers for Corrosion Protection“
EMT( Electrochemical Microsystem Technologies) 2000, 11.-13. September 2000,
Garmisch-Partenkirchen

?? T.T.Mai, G. Staikov, J.W. Schultze
„Metallisierung und Mikrostrukturierung insolierender Kunststoffe mittels PLATO-
Verfahren“
Jahrestagung der Gesellschaft Deutscher Chemiker (GDCh), 27.-29. September 2001,
Würzburg
(Prize for second best Poster)

?? T.T. Mai, G. Staikov, J.W. Schultze
“ Direct Metallization of Insulating Polymers by PLATO technique”
rd53 Annual Meeting of the International Society of Electrochemistry (ISE), 15.-20.
September 2002, Düsseldorf

?? T.T. Mai, A. Kurowski, J.W. Schultze, M.J. Schönning, H. Lüth
“Negative Mikrostrukturierung”
th70 AGEF Seminar, Düsseldorf, 26 April 2002

CONTENTS



PREFACE

1. INTRODUCTION ………………………………………………………….……… 1

2. BACKGROUND …………………………………………………………………… 3
2.1. PLATO technique ……………………………………………………….…….. 3
2.2. Microstructured metallization of insulating substrates ………………………... 13

3. EXPERIMENTAL …………………………………………………………………. 15
3.1. Materials and Chemicals ………………………………………………………. 15
3.2. Methods ……………………………………………………………………….. 19

4. MECHANISMS OF PRETREATMENT (ETCHING AND ACTIVATION) 28
4.1. Etching ………………………………………………………………………… 30
4.1.1. Roughness (AFM) ………………………………………………………. 30
4.1.2. Surface groups (XPS) …………………………………………………… 35
4.1.3. Surface energy …………………………………………………………... 41
4.2. Activation ……………………………………………………………………... 43
4.2.1. Surface characterization ………………………………………………… 43
4.2.2. Influence of activation cycle on the coverage ………………………….. 46

5. MECHANISMS OF METAL DEPOSITION …………………………….……… 49
5.1. Electrochemistry of cobalt sulphide ………………..…………………………. 50
5.1.1. Electrochemistry of cobalt sulphide in Ni free solution …….…………. 50
5.1.2. Electrochemistry of cobalt sulphide in Ni containing solution ………... 57
5.2. Kinetics of metal deposition ..…………………………………………………. 58
5.2.1. Formation of Ni layer ………………………………………………….. 58
5.2.2. Influence of potential, coverage and Ni concentration …………….…... 72
5.3. Deposition mechanis …………………………………………………………... 77
5.3.1. Formation of primary layer ……………………………………………... 77
5.3.2. Formation of secondary layer …………………………………………... 79

6. APPLICATIONS …………………………………………………………………... 81
6.1. PLATO technique with different substrates and metals ………………………. 81
6.2. Microstructured metallization ……………………………………………….… 85

7. CONCLUSIONS …………………………………………………………………… 90
8. APPENDICES ……………………………………………………………………… 93
REFERENCES……………………….. 100