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This page intentionally left blank
 I N T RO DUCT ION TO THE HI GH- TEMP ERATURE
OXIDATION OF METALS

A straightfoward treatment describing the oxidation processes of metals and alloys

at elevated temperatures. This new edition retains the fundamental theory but incor-
porates advances made in understanding degradation phenomena. Oxidation pro-
cesses in complex systems are dicussed, from reactions in mixed environments
to protective techniques, including coatings and atmosphere control. The authors
provide a logical and expert treatment of the subject, producing a revised book
that will be of use to students studying degradation of high-temperature materials
and an essential guide to researchers requiring an understanding of this elementary
process.

neil birks was Professor Emeritus in the Department of Materials Science and
Engineering at the University of Pittsburgh.
gerald h. meier is William Kepler Whiteford Professor in the Department of
Materials Science and Engineering at the University of Pittsburgh.
fred s. pettit is Harry S. Tack Professor in the Department of Materials Science
and Engineering at the University of Pittsburgh.
 IN T RODUC TI O N TO T HE
HIGH- TE M P ER ATUR E OXIDAT ION
OF M E TAL S

2nd Edition

NEIL BIRKS
Formerly of University of Pittsburgh

GERALD H. MEIER
University of Pittsburgh

FRED S. PETTIT
University of Pittsburgh
cambridge university press
Cambridge, New York, Melbourne, Madrid, Cape Town, Singapore, São Paulo

Cambridge University Press

The Edinburgh Building, Cambridge cb2 2ru, UK
Published in the United States of America by Cambridge University Press, New York
www.cambridge.org
Information on this title: www.cambridge.org/9780521480420

© N. Birks, G. H. Meier and F. S. Pettit 2006

This publication is in copyright. Subject to statutory exception and to the provision of

relevant collective licensing agreements, no reproduction of any part may take place
without the written permission of Cambridge University Press.

First published in print format 2006

isbn-13 978-0-511-16089-9 eBook (EBL)

isbn-10 0-511-16089-5 eBook (EBL)

isbn-13 978-0-521-48042-0 hardback

isbn-10 0-521-48042-6 hardback

isbn-13 978-0-521-48517-3
isbn-10 0-521-48517-7

Cambridge University Press has no responsibility for the persistence or accuracy of urls
for external or third-party internet websites referred to in this publication, and does not
guarantee that any content on such websites is, or will remain, accurate or appropriate.
Professor Neil Birks
This book is dedicated to one of its coauthors, Professor Neil Birks, who passed
away during the preparation of the second edition. Neil was an accomplished
researcher and educator in a number of fields including high-temperature oxidation,
corrosion, erosion, and process metallurgy. He was also a good friend.
Neil’s legacy to science and engineering is well established in his scholarly
publications and the numerous students he mentored. It is our hope that this book
will complete that legacy.
GHM
FSP
 Contents

Acknowledgements page viii

Preface ix
Introduction xi
1 Methods of investigation 1
2 Thermodynamic fundamentals 16
3 Mechanisms of oxidation 39
4 Oxidation of pure metals 75
5 Oxidation of alloys 101
6 Oxidation in oxidants other than oxygen 163
7 Reactions of metals in mixed environments 176
8 Hot corrosion 205
9 Erosion–corrosion of metals in oxidizing atmospheres 253
10 Protective coatings 271
11 Atmosphere control for the protection of metals during production
processes 306
Appendix A. Solution to Fick’s second law for a semi-infinite solid 323
Appendix B. Rigorous derivation of the kinetics of internal oxidation 327
Appendix C. Effects of impurities on oxide defect structures 332
Index 336

vii
 Acknowledgements

The authors gratefully acknowledge the scientific contributions of former and cur-
rent students. Drs. J. M. Rakowski, M. J. Stiger, N. M. Yanar, and M. C. Maris-Sida
are thanked for their assistance in preparing figures for this book.
The authors also greatly appreciate the helpful comments made by Professor J. L.
Beuth (Carnegie Mellon University), Professor H. J. Grabke (Max-Planck Institüt
für Eisenforschung), and Professor R. A. Rapp (Ohio State University) on parts of
the manuscript.

viii
 Preface

Few metals, particularly those in common technological applications, are stable

when exposed to the atmosphere at both high and low temperatures. Consequently,
most metals in service today are subject to deterioration either by corrosion at room
temperature or by oxidation at high temperature. The degree of corrosion varies
widely. Some metals, such as iron, will rust and oxidize very rapidly whereas other
metals, such as nickel and chromium, are attacked relatively slowly. It will be seen
that the nature of the surface layers produced on the metal plays a major role in the
behaviour of these materials in aggressive atmospheres.
The subject of high-temperature oxidation of metals is capable of extensive
investigation and theoretical treatment. It is normally found to be a very satisfying
subject to study. The theoretical treatment covers a wide range of metallurgical,
chemical, and physical principles and can be approached by people of a wide range
of disciplines who, therefore, complement each other’s efforts.
Initially, the subject was studied with the broad aim of preventing the deterio-
ration of metals in service, i.e., as a result of exposing the metal to high tempera-
tures and oxidizing atmospheres. In recent years, a wealth of mechanistic data has
become available. These data cover a broad range of phenomena, e.g., mass transport
through oxide scales, evaporation of oxide or metallic species, the role of mechan-
ical stress in oxidation, growth of scales in complex environments containing more
than one oxidant, and the important relationships between alloy composition and
microstructure and oxidation. Such information is obtained by applying virtually
every physical and chemical investigative technique to the subject.
In this book the intention is to introduce the subject of high-temperature oxi-
dation of metals to students and to professional engineers whose work demands
familiarity with the subject. The emphasis of the book is placed firmly on supplying
an understanding of the basic, or fundamental, processes involved in oxidation.
In order to keep to this objective, there has been no attempt to provide an exhaus-
tive, or even extensive, review of the literature. In our opinion this would increase

ix
 Preface

the factual content without necessarily improving the understanding of the subject
and would, therefore, increase both the size and price of the book without enhanc-
ing its objective as an introduction to the subject. Extensive literature quotation is
already available in books previously published on the subject and in review arti-
cles. Similarly the treatment of techniques of investigation has been restricted to a
level that is sufficient for the reader to understand how the subject is studied with-
out involving an overabundance of experimental details. Such details are available
elsewhere as indicated.
After dealing with the classical situations involving the straightforward oxida-
tion of metals and alloys in the first five chapters, the final chapters extend the
discussion to reactions in mixed environments, i.e., containing more than one oxi-
dant, to reactions involving a condensed phase as in hot corrosion, and the added
complications caused by erosive particles. Finally, some typical coatings for high-
temperature applications and the use of protective atmospheres during processing
are described.

Pittsburgh GHM
2005 FSP

x
 Introduction

The primary purpose of this book is to present an introduction to the fundamental

principles that govern the interaction of reactive gaseous environments (usually
containing oxygen as a component) and solid materials, usually metals, at high
temperatures. These principles are applicable to a variety of applications, which
can include those where oxidation is desirable, such as forming a resistive silica
layer on silicon-based semiconductors or removing surface defects from steel slabs
during processing by rapid surface oxidation. However, most applications deal
with situations where reaction of the component with the gaseous atmosphere is
undesirable and one tries to minimize the rate at which such reactions occur.
The term ‘high-temperature’ requires definition. In contrast to aqueous corrosion,
the temperatures considered in this book will always be high enough that water,
when present in the systems, will be present as the vapour rather than the liquid.
Moreover, when exposed to oxidizing conditions at temperatures between 100
and 500 ◦ C, most metals and alloys form thin corrosion products that grow very
slowly and require transmission electron microscopy for detailed characterization.
While some principles discussed in this book may be applicable to thin films, ‘high
temperature’ is considered to be 500 ◦ C and above.
In designing alloys for use at elevated temperatures, the alloys must not only be as
resistant as possible to the effects produced by reaction with oxygen, but resistance
to attack by other oxidants in the environment is also necessary. In addition, the
environment is not always only a gas since, in practice, the deposition of ash on the
alloys is not uncommon. It is, therefore, more realistic in these cases to speak of
the high-temperature corrosion resistance of materials rather than their oxidation
resistance.
The rate at which the reactions occur is governed by the nature of the reac-
tion product which forms. In the case of materials such as carbon the reaction
product is gaseous (CO and CO2 ), and does not provide a barrier to continued
reaction. The materials that are designed for high-temperature use are protected by

xi
 Introduction

the formation of a solid reaction product (usually an oxide) which separates the
component and atmosphere. The rate of further reaction is controlled by transport
of reactants through this solid layer. The materials designed for use at the high-
est temperatures are ones which form the oxides with the slowest transport rates
for reactants (usually α-Al2 O3 or SiO2 ), i.e., those with the slowest growth rates.
However, other materials are often used at lower temperatures if their oxides have
growth rates which are ‘slow enough’ because they may have better mechanical
properties (strength, creep resistance), may be easier to fabricate into components
(good formability/weldability), or are less expensive.
In some cases, the barriers necessary to develop the desired resistance to corro-
sion can be formed on structural alloys by appropriate composition modification.
In many practical applications for structural alloys, however, the required compo-
sitional changes are not compatible with the required physical properties of the
alloys. In such cases, the necessary compositional modifications are developed
through the use of coatings on the surfaces of the structural alloys and the desired
reaction-product barriers are developed on the surfaces of the coatings.
A rough hierarchy of common engineering alloys with respect to use temperature
would include the following.
r Low-alloy steels, which form M3 O4 (M = Fe, Cr) surface layers, are used to temperatures
of about 500 ◦ C.
r Titanium-base alloys, which form TiO2 , are used to about 600 ◦ C.
r Ferritic stainless steels, which form Cr2 O3 surface layers, are used to about 650 ◦ C. This
temperature limit is based on creep properties rather than oxidation rate.
r Austenitic Fe–Ni–Cr alloys, which form Cr2 O3 surface layers and have higher creep
strength than ferritic alloys, are used to about 850 ◦ C.
r Austenitic Ni–Cr alloys, which form Cr2 O3 surface layers, are used to about 950 ◦ C,
which is the upper limit for oxidation protection by chromia formation.
r Austenitic Ni–Cr–Al alloys, and aluminide and MCrAlY (M = Ni, Co, or Fe) coatings,
which form Al2 O3 surface layers, are used to about 1100 ◦ C.
r Applications above 1100 ◦ C require the use of ceramics or refractory metals. The lat-
ter alloys oxidize catastrophically and must be coated with a more oxidation-resistant
material, which usually forms SiO2 .

The exercise of ‘alloy selection’ for a given application takes all of the above factors
into account. While other properties are mentioned from time to time, the emphasis
of this book is on oxidation and corrosion behaviour.

xii
 1
Methods of investigation

The investigation of high-temperature oxidation takes many forms. Usually one

is interested in the oxidation kinetics. Additionally, one is also interested in the
nature of the oxidation process, i.e., the oxidation mechanism. Figure 1.1 is a
simple schematic of the cross-section of an oxide formed on the surface of a metal
or alloy. Mechanistic studies generally require careful examination of the reaction
products formed with regard to their composition and morphology and often require
examination of the metal or alloy substrate as well. Subsequent sections of this
chapter will deal with the common techniques for measuring oxidation kinetics
and examining reaction-product morphologies.
In measuring the kinetics of degradation and characterizing the correspond-
ing microstructures questions arise as to the conditions to be used. Test condi-
tions should be the same as the application under consideration. Unfortunately, the
application conditions are often not precisely known and, even when known, can
be extremely difficult to establish as a controlled test. Moreover, true simulation
testing is usually impractical because the desired performance period is generally
much longer than the length of time for which laboratory testing is feasible. The
answer to this is accelerated, simulation testing.
Accelerated, simulation testing requires knowledge of microstructure and mor-
phological changes. All materials used in engineering applications exhibit a
microstructural evolution, beginning during fabrication and ending upon termi-
nation of their useful lives. In an accelerated test one must select test conditions
that cause the microstructures to develop that are representative of the application,
but in a much shorter time period. In order to use this approach some knowledge
of the degradation process is necessary.

Measurements of reaction kinetics

In the cases of laboratory studies, the experimental technique is basically simple.
The specimen is placed in a furnace, controlled at the required temperature, and

1
2 Methods of investigation

Oxidizing gas

Oxide

Alloy

Figure 1.1 Schematic diagram of the cross-section of an oxide layer formed on

the surface of a metal or alloy.

allowed to react for the appropriate time. The specimen is then removed, allowed
to cool, and examined.
Although this procedure is simple, one drawback is that the start time for the reac-
tion cannot be accurately established. Several starting procedures are commonly
used.

(1) The specimen may simply be placed in the heated chamber containing the reactive
atmosphere.
(2) The specimen may be placed in the cold chamber containing the atmosphere and then
heated.
(3) The specimen may be placed in the cold chamber, which is then evacuated or flushed
with inert gas, heated and then, at temperature, the reactive gas is admitted.

In all cases the start of the reaction is in doubt either because of the time required
to heat the specimen or the inevitable formation of thin oxide layers, even in inert
gases or under vacuum. This is true especially in the case of more reactive metals,
so that when the reaction is started by admitting the reactive gas an oxide layer
already exists.
Attempts have been made to overcome this by heating initially in hydrogen
which is then flushed out by the reactive gas. This also takes a finite time and thus
introduces uncertainty concerning the start of the reaction.
Thin specimens may be used to minimize the time required to heat the specimen.
In this case care should be taken that they are not so thin and, therefore, of such low
thermal mass that the heat of reaction, released rapidly during the initial oxidation
period, causes severe specimen overheating.
The uncertainty concerning the start of the reactions usually only affects results
for short exposure times up to about ten minutes and becomes less noticeable at
longer times. However, in some cases such as selective oxidation of one element
 Measurements of reaction kinetics 3

from an alloy, these effects can be quite long-lasting. In practice specimens and
procedures must be designed with these factors in mind.
Many early investigations were simply concerned with oxidation rates and not
with oxidation mechanisms. The rate of formation of an oxide in a metal according
to the reaction (1.1),

2M + O2 = 2MO, (1.1)

can be investigated by several methods. The extent of the reaction may be measured
by the following.

(1) The amount of metal consumed.

(2) The amount of oxygen consumed.
(3) The amount of oxide produced.

Of these only (2) can be assessed continuously and directly.

(1) The amount of metal consumed

In practice this may be assessed by observing (a) the weight loss of the specimen or
(b) the residual metal thickness. In both cases the specimen must be removed from the
furnace, thus interrupting the process.
(2) The amount of oxygen consumed
This may be assessed by observing either the weight gain or the amount of oxygen used.
Both of these methods may be used on a continuous and automatic recording basis.
(3) The amount of oxide produced
This may be assessed by observing the weight of oxide formed or by measuring the
oxide thickness. Of course, in the latter case it is necessary to destroy the specimen, as
it is with method (1).

Of the above methods, only those involving measurement of weight gain and
oxygen consumption give the possibility of obtaining continuous results. The
other methods require destruction of the specimen before the measurement can
be achieved and this has the drawback that, in order to obtain a set of kinetic data,
it is necessary to use several specimens. Where the specimen and the methods of
investigation are such that continuous results can be obtained, one specimen will
give the complete kinetic record of the reaction.
When representing oxidation kinetics, any of the variables mentioned above can
be used, and can be measured as a function of time because, of course, they all
result in an assessment of the extent of reaction. Nowadays it is most general to
measure the change in mass of a specimen exposed to oxidizing conditions.
It is found experimentally that several rate laws can be identified. The principal
laws are (1) linear law, (2) parabolic law, and (3) logarithmic law.
4 Methods of investigation

(1) The linear law, for which the rate of reaction is independent of time, is found to refer
predominantly to reactions whose rate is controlled by a surface-reaction step or by
diffusion through the gas phase.
(2) The parabolic law, for which the rate is inversely proportional to the square root of
time, is found to be obeyed when diffusion through the scale is the rate-determining
process.
(3) The logarithmic law is only observed for the formation of very thin films of oxide,
i.e., between 2 and 4 nm, and is generally associated with low temperatures.

Under certain conditions some systems might even show composite kinetics,
for instance niobium oxidizing in air at about 1000 ◦ C initially conforms to the
parabolic law but later becomes linear, i.e., the rate becomes constant at long times.

Discontinuous methods of assessment of reaction kinetics

In this case the specimen is weighed and measured and is then exposed to the con-
ditions of high-temperature oxidation for a given time, removed, and reweighed.
The oxide scale may also be stripped from the surface of the specimen, which is
then weighed. Assessment of the extent of reaction may be carried out quite sim-
ply either by noting the mass gain of the oxidized specimen, which is the mass
of oxygen taken into the scale, or the mass loss of the stripped specimen, which
is equivalent to the amount of metal taken up in scale formation. Alternatively,
the changes in specimen dimensions may be measured. As mentioned before these
techniques yield only one point per specimen with the disadvantages that (a) many
specimens are needed to plot fully the kinetics of the reaction, (b) the results
from each specimen may not be equivalent because of experimental variations, and
(c) the progress of the reaction between the points is not observed. On the other hand
they have the obvious advantage that the techniques, and the apparatus required,
are extremely simple. In addition, metallographic information is obtained for each
data point.

Continuous methods of assessment

These methods fall into two types, those which monitor mass gain and those which
monitor gas consumption.

Mass-gain methods
The simplest method of continuous monitoring is to use a spring balance. In this case
the specimen is suspended from a sensitive spring whose extension is measured,
using a cathetometer, as the specimen mass changes as a result of oxidation, thus
 Measurements of reaction kinetics 5
Gas exit tube
(may be turned, raised, or lowered)

Rigid epoxy resin joint

Serrated edge
(allows point of suspension to be changed)

Pyrex tube

Pyrex or silica
spiral Cathetometer target

Silica or refractory tube with ground joint

Tube furnace
Silica rod suspension

Specimen

Thermocouple

Gas inlet

Figure 1.2 Features of a simple spring balance (for advanced design see ref. 1).

giving a semi-continuous monitoring of the reaction. Apparatus suitable for this

is shown diagrammatically in Figure 1.2 which is self-explanatory.1 An important
feature is the design of the upper suspension point. In Figure 1.2 this is shown
as a hollow glass tube which also acts as a gas outlet. The tube can be twisted,
raised, or lowered to facilitate accurate placing of the specimen and alignment of
the spring. A suspension piece is rigidly fastened to the glass tube and provides
a serrated horizontal support for the spring whose suspension point may thus be
adjusted in the horizontal plane. These refinements are required since alignment
between the glass tube containing the spring and the furnace tube is never perfect
and it is prudent to provide some means of adjustment of the spring position in order
to ensure accurate placing of the specimen. It would be possible of course to equip
a spring balance with a moving transformer, which would enable the mass gain to
6 Methods of investigation

be measured electrically, and automatically recorded. Although the simple spring

balance should be regarded as a semi-continuous method of assessment, it has the
advantage that a complete reaction curve can be obtained from a single specimen.
The disadvantage of the spring balance is that one is faced with a compromise
between accuracy and sensitivity. For accuracy a large specimen is required whereas
for sensitivity one needs to use a relatively fragile spring. It is obviously not possible
to use a fragile spring to carry a large specimen and so the accuracy that is obtained
by this method is a matter of compromise between these two factors.
By far the most popular, most convenient, and, unfortunately, most expensive
method of assessing oxidation reactions is to use the continuous automatic record-
ing balance. Obviously the operator must decide precisely what is needed in terms
of accuracy and sensitivity from the balance. For straightforward oxidation experi-
ments it is generally adequate to choose a balance with a load-carrying ability of up
to about 25 g and an ultimate sensitivity of about 100 µg. This is not a particularly
sensitive balance and it is rather surprising that many investigators use far more
sophisticated, and expensive, semi-micro balances for this sort of work. In fact
many problems arise from the use of very sensitive balances together with small
specimens, to achieve high accuracy. This technique is subject to errors caused
by changes in Archimedean buoyancy when the gas composition is changed or
the temperature is altered. An error is also introduced as a result of a change in
dynamic buoyancy when the gas flow rate over the specimen is altered. For the
most trouble-free operation it is advisable to use a large specimen with a large flat
surface area in conjunction with a balance of moderate accuracy. Figure 1.3 shows
a schematic diagram of a continuously reading thermobalance used in the authors’
laboratory.
Using the automatic recording balance it is possible to get a continuous record
of the reaction kinetics and, in this way, many details come to light that are hidden
by other methods. For instance spalling of small amounts of the oxide layer is
immediately detected as the balance registers the mass loss; separation of the scale
from the metal surface is recorded when the balance shows a slow reduction in rate
well below rates that would be expected from the normal reaction laws; cracking of
the scale is indicated by immediate small increases in the rate of mass gain. These
features are shown in Figure 1.4. The correct interpretation of data yielded by the
automatic recording balance requires skill and patience but, in almost every case,
is well worthwhile.

Gas consumption
Continuous assessment based on measurement of the consumption of gas may be
done in two ways. If the system is held at constant volume then the fall in pressure
may be monitored, continuously or discontinuously. Unfortunately, allowing the
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