Research Collection. Doctoral Thesis. ETH Library. Author(s): Piippo, Juha. Publication Date: 1993
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1 Research Collection Doctoral Thesis Electrochemical characterization of inorganic coatings titanium nitride and aluminium oxide coatings characterized using electrochemical impedance spectroscopy Author(s): Piippo, Juha Publication Date: 1993 Permanent Link: Rights / License: In Copyright - Non-Commercial Use Permitted This page was generated automatically upon download from the ETH Zurich Research Collection. For more information please consult the Terms of use. ETH Library
2 ETHICS ETH-BIB warn Diss: ETH x-j > Diss. ETH No Electrochemical Characterization of Inorganic Coatings Titanium Nitride and Aluminium Oxide Coatings Characterized Using Electrochemical Impedance Spectroscopy A Dissertation submitted to the SWISS FEDERAL INSTITUTE OF TECHNOLOGY for the Degree of Doctor of Technical Sciences presented by Juha Piippo Dipl. Ing. born June 12, 1964 citizen of Finland accepted on the recommendation of Prof. Dr. H. Bohni, examiner Prof. Dr. L. Gauckler, co-examiner Dr. B. Elsener, co-examiner 1993
3 4 A ABSTRACT The electrochemical characterization and the characterization methods of inorganic coating systems are studied in this work. Special attention is paid to the application of the electrochemical impedance spectroscopy (EIS) to the characterization of the coatings and the interpretation of the results. In the literature various models describe the impedance response of coated systems. None of them is a physical model and thus they can not describe the effect of coating thickness on the impedance and the current distribution. In this work three-dimensional models based on the electrochemical behavior of porous electrodes are developed. They describe the electrochemical interaction of substrate and coating in situ and in the case, when the coated system is studied in the three electrode cell. The validity of the model system is tested with chemical vapor-deposited titanium nitride (TiN) on stainless steel AISI 316L and on inert silicon nitride (Si3N4), and plasma-sprayed aluminium oxide (AI2O3) coatings on stainless steel AISI 304. In addition to the EIS measurements, potential measurements, potentiodynamic polarization measurements and the water impregnation for porosity determination were carried out. The electrochemical behavior of the titanium nitride coatings is found to depend on the coating thickness and the aggressivity of the electrolyte. The performance of the 2.2 jxm thick coating on AISI 316L was clearly weaker than that of the 7 im thick coating. In dilute electrolytes the substrate is passive and the EIS response describes the behavior of the coating. The coatings on the AISI 316L and on the Si3N4 both behave similarly. A change in the electrochemical behavior is obtained when the substrate becomes active due to more aggressive electrolytes and increased porosity. Because the impedance of the substrate is essentially lower than that of the coating, the EIS response describes the electrochemical behavior of the substrate and the mass transport through the pores. In the strong electrolyte, the coating is found to be activated due to the dissolution of the oxide film on TiN. A model that describes the spontaneous passivation of titanium nitride is proposed. The dissolved titanium atoms form an oxide film on the coating / electrolyte interface and the nitrogen from the nitride lattice is reduced to the ammonium ions.
4 5 Plasma-sprayed aluminium oxide coatings with three different thicknesses were studied in order to apply the model to the case of greater coating thickness and higher ohmic resistance. The performance of the coatings was found to depend essentially on the porosity and the coating thickness. Generally, the corrosion resistance of the AI2O3 coatings improves with the increasing coating thickness due to the high resistances of the coating materials and the long pores. However, the advantage of the increased thickness could be neutralized by the high porosity. The coating thickness was found to have no effect on the coating porosity. The application of the fitting model to aluminium oxide coatings was difficult. A capacitor concept based on the dielectricity of alumina was not suitable, because the plasma-sprayed coating is heterogeneous, and there are corrosion product formations on the coating material particles. The interpretation of the EIS spectra of the coated materials is possible if there is enough supportive data available from the measurements performed with other methods. The credibility of the simulations is increased by keeping the system as stable and as simple as possible by choosing such an electrolyte that keeps the system stationary and that activates only the wanted component of the coated system.
5 6 B ZUSAMMENFASSUNG Ziel dieser Arbeit war die Charakterisierung von anorganischen Beschichtungen mit elektrochemischen Methoden, speziell mit der elektrochemischen Impedanzspektroskopie, und eine kritische Auseinandersetzung mit dieser Methode sowie der Interpretation der gemessenen Resultate. In der Literatur gibt es verschiedene Modelle, die das Impedanzverhalten beschreiben. Keines ist ein physikalisches Modell und daher sind sie nicht fahig, den Effekt der Schichtdicke auf die Impedanz und auf die Stromverteilung zu beschreiben. Dreidimensionale Modelle, die sich auf das elektrochemische Verhalten poroser Elektroden griinden, sind in dieser Arbeit entwickelt worden. Sie beschreiben die Wechselwirkung zwischen dem Substrat und der Schicht in situ und fur den Fall, untersucht wird. dass das beschichtete System in einer Dreielektrodenzelle Die Giiltigkeit des 3D-Modells ist mit CVD beschichtetem Titannitrid (TiN) auf rostfreiem Stahl AISI 316L und auf inertem Siliziumnitrid (Si3N4) sowie mit plasmagespritztem Aluminiumoxyd auf rostfreiem Stahl AISI 304 iiberpriift worden. Zusatzlich wurden Korrosionpotentialmessungen, Strom-Spannungsmessungen und Wasserimpregnationmessungendurchgefuhrt. Die Experimente zeigen, dass das elektrochemische Verhalten der Systeme Titannitrid / hochlegierter Stahl von der Schichtdicke und von der Aggressivitat des Elektrolyts abhangig ist. Die Korrosionsschutzeigenschaften der 2.2 urn dicken Schicht sind eindeutig schlechter als diejenigen der 7 im dicken Schicht. In den verdiinnten Losungen ist das Substrat passiv und die EIS Messungen beschreiben die Eigenschaften der Beschichtung. Die elektrochemischen Eigenschaften der Beschichtungen auf AISI 316 und Si3N4 sind ahnlich. Das elektrochemische Verhalten verandert sich, wenn das Substrat wegen des aggressiven Elektrolyts oder der zugenommenen Porositat aktiv wird. Weil dann die Impedanz des Substrats wesentlich kleiner als diejenige der Beschichtung wird, beschreiben die Impedanzmessungen in diesem Fall das elektro chemische Verhalten des Substrats und den Stofftransport konzentrierten Elektrolyt wird wegen der Auflosung Beschichtung selbst aktiviert. durch Poren. In einem der Oxidschicht auf Titannitrid die Diese dunne Oxidschicht auf Titannitrid ist anscheinend verantwortlich fur die guten Korrosionseigenschaften von Titannitrid. Ein Ansatz, welcher die spontane Passivierung von Titannitrid beschreibt, wird vorgeschlagen. Danach bilden die
6 Grenzflache 7 gelosten Titanionen eine Oxidschicht auf der Schicht / Elektrolyt - Stickstoff aus dem Nitridgitter wird zu Ammoniumionen reduziert. und der Die Anwendbarkeit des in dieser Arbeit entwickelten 3D-Modells im Falle von dicken Beschichtungen und hohen ohm'schen Widerstanden wurde mit plasmagespritzten Aluminiumoxydbeschichtungen Verhalten der Beschichtungen war hauptsachlich mit drei verschiedenen Schichtdicken untersucht. Das von der Porositat und der Schicht dicke abhangig. Der Korrosionsschutz durch Aluminiumoxydbeschichtungen verbessert sich mit zunehmender Schichtdicke wegen der hohen Widerstande des Schichtmaterials und wegen der langen Poren. Der Vorteil einer dicken Schicht kann jedoch durch die hohe Porositat zunichte gemacht werden. Die Schichtdicke hat keinen Effekt auf die Porositat. Die Anwendung des 3D-Modells fiir Aluminiumoxydbeschichtungen war schwierig. Ein Kondensatormodell, das auf dem dielektrischen Verhalten des Schicht materials aufgebaut ist, ist nicht zweckmsssig, weil die plasmagespritzte Schicht heterogen ist und die Korrosions-produkte an den Porenwanden gebildet werden. Die Interpretation experimentell gemessener Impedanzspektren an beschichteten Materialien ist moglich, wenn geniigend zusatzliche Resultate von anderen elektro chemischen Methoden vorliegen. Die Qualitat der Simulationen ist besser, wenn das untersuchte System moglichst einfach gehalten wird. Der Elektrolyt soil das System stationar halten und nur den gewiinschten Teil (Substrat oder Schicht) vom beschichteten System aktivieren.
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