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P A P E R

3 E 1

The Use of Non-Destructive


Tools for Characterization of
Hydrogen in Advanced Alloys

ANGELIQUE LASSEIGNE

BIOGRAPHY

CEO, METALLURGICAL AND


MATERIALS ENGINEER
Generation 2 Materials Technology, LLC
10281 Foxfire Street
Firestone, Colorado 80504
USA
T: 303-304-9785
F: 720-836-4194
E: angelique@g2mt.com

Dr. Lasseigne is a metallurgical and


materials engineer at Generation 2
Materials Technology, LLC focusing
on the development of real-time insitu non-destructive systems to give
complete characterization of
materials before significant damage
occurs. Angelique received her
undergraduate degrees in Physics
and Metallurgical and Materials
Engineering from Centenary College
of Louisiana and Colorado School
of Mines in Golden, Colorado. She
continued on at the Colorado
School of Mines for Masters and
Ph.D. degrees in Metallurgical and
Materials
Engineering.
Dr.
Lasseigne completed a National
Research Council Post-Doctoral
Fellowship in the Materials
Reliability Division at the National
Institute of Standards and
Technology in Boulder, Colorado
where she worked on development
of
advanced
sensors
to
characterize the state of materials
before the occurrence of defects or
failure. Angelique has also been
Research Faculty and is currently

Co-authors

J.E. JACKSON
PRESIDENT
Generation 2 Materials Technology, LLC

K.E. KOENIG
GRADUATE STUDENT
Colorado School of Mines

D.L. OLSON
PROFESSOR OF METALLURGICAL AND
MATERIALS ENGINEERING
Colorado School of Mines

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an Adjunct Faculty to the Colorado


School of Mines.

ABSTRACT
Many advanced materials that are
considered to have superior
corrosion resistance experience
severe problems in hydrogencontaining
environments.
Susceptible alloys can absorb large
amounts of hydrogen, especially at
higher temperatures, resulting in
hydrogen saturation and the
formation of hydride phases. The
alloy composition and microstructure
is directly related to the solubility of
hydrogen,
and
therefore,
susceptibility to hydrogen damage.
Non-destructive electronic and
magnetic tools can be used to
assess the electronic structure of an
alloy and are sensitive to any
perturbations in the structure.
Thermoelectric power and low
frequency impedance sensors have
successfully been utilized to quickly
achieve
the
non-destructive
equivalent of the pressurecomposition-temperature (activity)

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diagram. Linking non-destructive


sensors with the activity diagram for
the specific material allows for rapid
direct assessment of hydrogen
solubility and phase. The use of
thermoelectric power and low
frequency impedance to characterize
hydrogen content in advanced alloys
is presented.

KEYWORDS
hydrogen content
determination
non-destructive electronic tools
materials characterization
thermoelectric power
low frequency impedance

INTRODUCTION
Hydrogen can be both beneficial
and detrimental to material
properties
and
capabilities
dependent upon the material.
Hydrogen has many desirable
properties for use as an energy
source, which requires materials that
can safely and efficiently absorb and
desorb hydrogen. In other cases,
hydrogen can potentially begin as a
beneficial alloying element (interstitial
hydrogen acts as interstitial
strengthener) until a specific
hydrogen concentration is achieved.
A critical hydrogen concentration
would need to be determined at the
point where degradation of material
properties begin to prevent
significant damage or catastrophic

and hydride concentrations and


limits to achieve the desired material
properties.
A
pressure-compositiontemperature diagram can be used to
characterize the phase of hydrogen
present at specific temperatures,
pressures,
and
hydrogen
concentrations. Figure 2 is a
schematic PCT diagram showing
three distinct regions. In the first
region, hydrogen is in solid solution
and is known as the alpha phase ().
The reaction of hydrogen absorbed
in this region is 1/2 H 2(g) H(M).
The second region is a two-phase
region (+), which is the so-called
plateau region. In this second region,
there is the coexistence of solid
solution and hydride phase. In the
third region, hydrogen is in the form
of a metal hydride and is called beta
phase (). The PCT diagram can be
used to determine the phase of
hydrogen present in a material and
therefore the materials susceptibility
to hydrogen damage.
A new generation of materials
characterization is emerging through
the
use
of
electronic,
electromagnetic, and elastic nondestructive tools. Electronic and
electromagnetic non-destructive
tools can detect very small changes
in the electronic structure of a
material due to perturbations in the
electronic structure from alloying
additions, interstitials (such as
hydrogen), phase changes, residual
stress,
aging,
service
and

failure. As material capabilities are


being pushed to extreme limits, the
critical hydrogen concentration is
even more important because even
very small amounts of hydrogen can
change the properties of many
advanced materials.
The ability of a metal alloy to
absorb and desorb hydrogen
depends on the interaction with the
metals electronic bands. When
hydrogen enters the crystal lattice it
acts as either an electron acceptor
or an electron donor as seen in
Figure 1. The elements to the left of
manganese on the periodic table are
electron acceptors; having a negative
heat of mixing with hydrogen, which
results in the formation of hydrides.
The elements to the right of
manganese on the periodic table are
electron donors; having a positive
heat of mixing so that hydrogen
stays in solution. There are materials
consisting of elements that
transcend these extremities of the
periodic table, producing alloys that
can have large ( (interstitial
hydrogen) + (formed hydride))region and offer large hydrogen
storage and rapid charging and
discharging characteristics. For the
safe and reliable use of advanced
materials in hydrogen environments,
it is essential to have a means of
monitoring hydrogen concentrations
to determine whether the material of
interest
accepts
hydrogen
interstitially or as a formed hydride,
and then to determine the hydrogen

Figure 1. Electronic behavior of hydrogen in transition metal alloys.

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processing, etc. Non-destructive


tools have been used to rapidly
generate equivalent PCT diagrams
for materials to determine the
hydrogen solubility and phase, and
therefore the materials susceptibility
to hydrogen damage. Thermoelectric
power and low frequency impedance
sensors have successfully been
designed to quickly generate and
achieve equivalent PCT diagrams in
various materials. A brief background
is described for the use of
thermoelectric power and low
frequency impedance to characterize
hydrogen in materials.
Thermoelectric Power
The thermoelectric power coefficient
(also referred to as the Seebeck
coefficient) is a temperaturedependent electronic material
property that can be described as
the entropy of the free electrons in
the alloy. In metallic alloys, the value
and the sign of the thermoelectric
power coefficient are dependent
upon factors including the electronic
features in the vicinity of the Fermi
energy level, the effective mass
tensor, the density of electronic
states and the dominating scattering
mechanism [1]. In turn, the value of
the Fermi energy (the Fermi energy
surface in the k-space) changes with
electronic filling in the conduction
band due to electron donation by
hydrogen atoms. For example, with
the high degeneracy of free electron
gas, the resulting thermoelectric
power coefficient, is related to
electronic theory through the
following expression:

related to the Fermi energy. The


electronic effective mass defines the
rate of Fermi energy change with
increasing electron concentration[1].
The effective mass can be
described as:

thermoelectric power coefficient of


the a, is then calculated as:

where Cu is the thermoelectric power


coefficient of the reference copper
probe. A schematic thermoelectric
power sensor used for powder
materials is shown in Figure 3, where
heating cartridges are inside each
probe to maintain the temperature
difference necessary to develop a
measurable potential difference.
Figure 4 shows thermoelectric power
probes designed for determination of
nitrogen and hydrogen in stainless
steel weldments.

where k is the wave number. The


effective mass, m e, describes the
shape of the s, p, and d bands that
are in contact with the Fermi energy
level. The shape of the bands at the
contact
position
offers
a
characteristic indication that can be
measured with changes in the Fermi
energy level due to electron
donation from the hydrogen
addition. To gauge the magnitude
of the thermoelectric power effect,
the thermoelectric power coefficient,
, is defined as the potential
difference developed, dV, per unit
temperature difference, dT:

Figure 2. Schematic pressurecomposition-temperature (activity)


diagram.

Two copper probes maintained at a


constant temperature difference are
placed on the material, which then
gives rise to a developed potential,
V, between the copper probe and
the material being investigated. The

Figure 3. Schematic thermoelectric power probes for powder materials [2].

where r is the scattering parameter


determined by the dominating
scattering mechanism, and h is

Plancks constant, k is Boltzmanns


constant, n* is the electron
concentration, and me is the effective
mass. From the free electron model,
the electron concentration is directly
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Low Frequency Impedance


Low
frequency
impedance
measurements offer an alternative
and complimentary technique to
thermoelectric power because they
provide a means to perform nondestructive, non-contact hydrogen
content measurements as a
function of depth in materials.
Previous research has found that
low
frequency
impedance
measurements are extremely
sensitive to variations in hydrogen
content in high-strength steel
specimens [4].
In eddy current testing for
hydrogen
determination
in
materials, a low frequency
electromagnetic coil is used to

be expressed:

induce an electromagnetic field (by


an alternating current) into a
material. In response, the induced
electromagnetic field produces
eddy currents in the sample
opposing
the
generated
electromagnetic field. The induced
electromagnetic field is compared
to the opposing electromagnetic
field produced (due to Lenzs law)
within the inspected material.
When an alternating current is
applied to the material being
inspected, the electromagnetic coil
possesses both resistance and
reactance. Along with resistance,
there is a changing flux in the coil,
which exhibits inductance [5] . The
impedance, , of the system can

where is angular frequency, L is


inductance, C is capacitance, and R
is resistance. Impedance is a
measurement of resistance, but with
depth capabilities provided by the
angular frequency. At very low
frequencies, impedance becomes a
resistance measurement making it
easier to see the changes in
resistivity with the addition of each
hydrogen
atom.
Resistance
measurements bring into play new
factors that are not included in
thermoelectric power measurements

Figure 4. Photograph of thermoelectric power surface probes designed for weldments [3].

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because impedance is pushing


current, which means that any
scattering sites within the material
lattice will change the value of
resistance. This means that low
frequency impedance will require
more variable separation and
calibrations necessary for use, but
it may be worth it to have a means
of monitoring hydrogen in materials
without having to touch the surface
of the specimen. But for a resistance
type of measurement, it is essential
to have a mean of separating out the
effects of all scattering sites to
achieve an accurate hydrogen
content measurement [4] . Further
theoretical
development
of

thermoelectric power and low


frequency impedance are discussed
in multiples sources [4].
A
photograph
of
an
electromagnetic coil designed for
low frequency impedance hydrogen
content measurements on pipeline
steel weldments is shown in Figure
5 [6] . The electromagnetic coil has
been designed in this manner to
create a powerful magnetic field
strength to overcome any magnetic
remanence present in the pipeline
from smart pigging and the welding
process. The electromagnetic coils
are designed for each application
and material and can have a size
range spanning from less than a

couple of centimeters to arrays of


coils for inspecting very large
sections of materials. Low
frequency impedance hydrogen
content measurements have been
successfully performed in the
laboratory and in the field [6].

EXAMPLES OF NONDESTRUCTIVE CHARACTERIZATION OF HYDROGEN IN


ADVANCED ALLOYS
Thermoelectric power and low
frequency impedance have both
been developed to monitor
hydrogen contents in many different
advanced alloys such as MONEL

Figure 5. Photograph of electromagnetic coil designed for low frequency impedance hydrogen content measurements in pipeline
steel weldments [6].

MONEL is a registered trademark of Special Metals Corp.

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K-500, hydrogen storage materials,


pipeline steels, zirconium, etc.
Examples
of
the
use
of
thermoelectric power and low
frequency impedance are described
in the following section.

hardness. Thermoelectric power


coefficient measurements were
performed on MONEL K-500 to
assess the effect of cathodic
charging from cathodic protection[1].
The
correlation
between
thermoelectric power coefficient and
the hydrogen content of hydrogen
charged MONEL K-500 specimens
is shown in Figure 6, which
illustrates the hydrogen content at
the advent of metal hydride
formation. Figure 6 is the nondestructive corollary to the
pressure-composition-temperature
diagram shown in Figure 2 because
it can be divided into distinct
regions, the -region (diffusible
hydrogen) and the ( + )-region
(diffusible hydrogen and formed
hydrides). Determination and
monitoring of the onset and
progression of hydride phase
formation can prevent material
degradation and failure.

Characterization of Hydrogen
in MONEL K-500
MONEL K-500 (UNS N05500) is
an age-hardenable copper-nickel
alloy with excellent corrosion
resistance and high-strength and

Figure 6. TEP coefficient a function of charged hydrogen content in MONEL K-500 [1].

Characterization of Hydrogen
in LaNi 5 Hydrogen Battery
Materials
LaNi 5 is a reversible metal-hydride
battery material, which operates in
the two-phase, ( + )-region, as
seen on the pressure-compositiontemperature diagram (activity
diagram) for LaNi 5 shown in Figure
7. For reversible metal-hydride
batteries, the two-phase region,
consisting of both soluble (diffusible)
hydrogen and formed hydrides, is
the most important region because
as a battery is charged, the H/LaNi 5
ratio is on the far right side of the
activity diagram where it is pure
hydride phase, then as the diffusible
hydrogen is released for energy
usage, the hydrogen concentration
in the material goes back to the very
beginning of the ( + )-phase
formation. Theoretically, the rule-ofmixtures can be utilized in the twophase region to determine the
percentage of hydride and diffusible
hydrogen at a given H/LaNi 5 value.
Sieverts law holds true for hydrogen
in the alpha-phase region because

Figure 7. Isotherms of hydrogen gas (pressure p atm) in equilibrium with absorbed


hydrogen in LaNi5 (concentration: H atoms/LaNi5).7 Notice the alpha-region is where
hydrogen is in solid solution, the (alpha+beta)-region is made-up of both solid solution
hydrogen and hydrides, and the beta-region is primarily formed hydride.

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hydrogen gas molecules become


dissociated into atoms while being
dissolved into metals in the region
where hydrogen can be regarded as
an ideal gas. At higher pressures
and temperatures, the chemical
potential and solubility of hydrogen
deviates from the ideal gas behavior,
thus Sieverts law no longer applies.
The ability to quantify and
characterize both the diffusible
hydrogen and hydride contents in
the two-phase region is critical to
the performance of the reversible
hydrogen
storage
materials.
Thermoelectric
power
measurements can successfully
generate an equivalent activity
diagram for LaNi 5 at room
temperature and 190C (374F) as
shown in Figure 8. Notice how each
region in Figure 8 corresponds to the
activity diagram in Figure 7.
Thermoelectric power can therefore
be utilized as a hydrogen fuel gauge.

Figure 8. Thermoelectric power coefficient as a function of H atoms/LaNi 5 for hydrogen


charged LaNi 5 at room temperature (green) and 190C (374F) (blue) [8].

Figure 9. Pressure-composition-temperature isotherms for NaAlH 4 and Na 4AlH 6-[2,9].

Characterization of Hydrogen
in NaAlH 4
NaAlH4 is another hydrogen storage
material similar to LaNi 5 discussed
in Figures 7 and 8, however NaAlH 4
has a dual two-phase region shown
in Figure 9 indicating formation of
different hydride phases at specific
hydrogen concentrations. The
activity (PCT) diagram for NaAlH 4
(Figure 9) shows that primary
reaction occurs from approximately
0 to 1.0 H/Al and a secondary
reaction occurs from approximately
1.0 to 2.5 H/Al. Thermoelectric
power
measurements
were
performed as a non-destructive
means of generating an activity
diagram shown in Figure 10.
Thermoelectric power as a function
of H/Al (Figure 10) exhibits the same
two-reaction behavior as indicated
in Figure 9.
Characterization of Hydrogen
in Pipeline Steel
Pipeline operators are moving to
higher strength steels for the
development of future pipelines.
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Most steels have problems in


hydrogen environments, but as the
strength of the steel increases the
threshold content leading to failure

due to hydrogen is lowered.


Thermoelectric
power
measurements were performed in
the three examples discussed, but

for hydrogen content determination


in operating pipeline steels, low
frequency impedance is essential
because surface contact is not
always possible. Induced current low
frequency impedance analysis has
been developed to make noncontact determination of hydrogen
content in linepipe steel specimens
in the laboratory and in the field.
Laboratory low frequency impedance
experiments show that impedance
is very sensitive to small changes in
hydrogen content as seen in Figure
11. The figure shows impedance as
a function of hydrogen for hydrogen
charged X80 linepipe steel
specimens at a frequency of 100 Hz
(bulk of the specimen). Impedance
measurements appear to be more
sensitive than other analytical
techniques
to
hydrogen
concentrations below less than one
part per million. For measurements
performed in the field, separation of

Figure 10. Thermoelectric power coefficient as a function of H/Al for hydrogen


charged NaAlH 4 [4].

Figure 11. Frequency sweep of impedance with change in hydrogen content in tin coated hydrogen charged X80 steel specimens [4].

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the variables associated with an


operating pipeline is necessary.
Further description of field low
frequency impedance hydrogen
content measurements can be found
in References 4 and 6.
Characterization of Hydrogen
in Zirconium Alloys
Along with many other special
metals, zirconium also faces
detrimental effects when in
hydrogen environments. Low
frequency
impedance
and
thermoelectric power measurements
have
been
performed
to
characterize hydrogen in zirconium
alloys in water (for specific
application). The activity diagram for
hydrogen in zirconium is shown in
Figure 12, which also exhibits a dual
two-phase region. Using both
thermoelectric power and low
frequency
impedance
measurements can very insightful,
especially when there is no available
pressure-composition-temperature
diagrams available. The data
between both thermoelectric power
and low frequency impedance
measurements should indicate
phase changes at the same
hydrogen content if there is not too
much interference from other
variables. Figure 13 shows
thermoelectric power measurements
of a zirconium alloy in water
compared to the low frequency
impedance measurements of a
zirconium alloy in water at 200 Hz
(determined optimum frequency).
The yellow lines indicate the onset
of different phases. Notice how all
of the yellow lines between the
thermoelectric power and low
frequency
data
align.
The
thermoelectric power data appears
to have one more yellow line in a
region of uncertainty. The accuracy
of the lines are being verified and
determined with x-ray diffraction and
electron microscopy. The yellow
lines in Figure 13 would correspond
to the phase changes in Figure 12,
but at this point it is very difficult to
C O R R O S I O N

Figure 12. Pressure-composition-temperature diagram for the atomic ratio of


hydrogen to zirconium [10].

distinguish the direction of these


lines below 500C (932F) and
above a hydrogen content of
approximately 200 ppm. Further

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analysis is being performed to


determine what happens when the
data from both tools are combined
in order to separate out variables.

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CONCLUSIONS
Knowledge of the amount and type
of hydrogen present in a material is
crucial to the performance of critical
materials. Non-destructive electronic
and electromagnetic tools can be
successfully developed to monitor
hydrogen contents in advanced
materials through the use of
equivalent activity diagrams to
monitor the hydrogen content and
extend materials lifeteime while
preventing failures.

Figure 13a &13b. Impedance as a function of hydrogen content for hydrogen charged
Zircaloy-4 at 200 Hertz in water [4].

ACKNOWLEDGEMENTS
Generation 2 Materials Technology
appreciates the guidance and
advice of Steve Sparkowich of ATI
Wah Chang. a

REFERENCES
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2.

3.

4.

5.

Y.D. Park, A.N. Lasseigne, V.I.


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A.N.Lasseigne, "NonDestructive Determination of
Interstitial Nitrogen Content in
Austenitic Stainless Steel Weld
Metal Utilizing Thermoelectric
Power," Masters Thesis, T5899, May 2004.
A.N. Lasseigne, Development
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Electromagnetic Techniques for
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Advanced Materials, Ph.D.
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Mines, 2006.
D. E. Bray and R.K. Stanley,
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