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9
Non-destructive Evaluation of Porosity in
Thermally Sprayed Coatings Using
Permeability Measurement

By Aadil1,2, Praveen R2, Matt Siopsis3, Dheepa Srinivasan2,4

1
Indian Institute of Science, Bangalore -560012 (India).
2
Pratt and Whitney, Research and Development Center, Bangalore – 560012 (India).
3
Pratt & Whitney, East Hartford, United States.
4
MS Ramaiah University of Applied Sciences, Bangalore, India.
Email : [email protected]

The assessment of porosity in thermally sprayed coatings, cause rejections in the coating during quality control (Ref
particularly ceramic coatings, is a challenging and error- 5, 6). It therefore becomes imperative to develop other
prone task due to artifacts associated with metallographic methods of assessing the coating quality, especially via
specimen preparation. Existing methods for porosity non-destructive techniques. Non-destructive techniques
evaluation in thermal spray coatings are predominantly such as pycnometry (Ref 7), gamma-ray transmission (GRT)
qualitative in nature. This article is an attempt to enable a (Ref 8), X-ray computer tomography (CT) (Ref 9), Ultrasonic
more quantitative measurement of the porosity using a testing (Ref 10), Infrared thermography (Ref 11), and
permeability tester based on the principles of pressure Terahertz time-domain spectroscopy (Ref 12) have been
drop across a porous framework, using a Kermetico attempted, and have their respective merits and de-merits.
permeability rig on an air plasma sprayed MCrAlW coating There is a need for a simpler and agile technique to assess
with an unknown porosity. Porosity and volume fraction of thermally sprayed coatings porosity during production.
the coating were evaluated and validated using microscopy
and a transfer function was established, correlating In this study, a Kermetico permeability rig (Fig. 1a) was
permeability with pore size. used to measure the volumetric fluid flow rate through
porous coatings by using the pressure drop across the
Thermally sprayed coatings, such as thermal barrier coating, placed along with sintered porous discs of known
coatings (TBCs), are engineered to be porous to maximize porosity. This technique, designed for calculating the
their thermal insulation performance (Ref. 1-2). The volume fraction of interconnected pores, requires a free-
porosity ranges from 5-25%, based on the actual standing coating for qualification, making it an effective
component and application, such as for oxidation and candidate for non-destructive evaluation in production
thermal protection or for use as an abradable coating (Ref. settings. The purpose of this effort is to establish a reliable
3). For many of the functional applications, it becomes very baseline for using this permeability rig to evaluate porosity
challenging to get reliable and repeatable data on the in abradable coatings by identifying the correct porous disc
coating porosity. Establishing the coating thickness, for spraying. Assuming negligible inertia for gas through
porosity, and interfacial characteristics (with the substrate) interconnected pores, the coefficient of viscous Gas
are part of the production quality control processes (Ref 4). Permeability (Yn) is calculated using Darcy’s equation Eq.
The current process for evaluating the coating quality is via (1), which considers the pressure gradient (∆P), thickness
metallographic analysis which involves subjecting the of the sample (d), cross-sectional area (A), dynamic
coating through a rigorous mechanically intense process viscosity (h), and volumetric flow rate (Q) of the test fluid.
such as sectioning, mounting, grinding, and polishing,
which can result in significant damage and cause pull outs 𝑌𝑌𝑛𝑛 =
𝑄𝑄∙ℎ∙𝑑𝑑
[1]
that may exaggerate the sample porosity and may tend to 𝐴𝐴∙∆𝑃𝑃
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10 The rig comprises of a pressure gauge, pressure minimal resistance to gas flow, owing to the open pore
regulator, two flowmeters, and a test cell with specific network within the sintered discs allow free flow of the
technical characteristics as shown in Fig. 1a. The working gas with little or no resistance. OD on the other hand
range of the permeability rig with compressed air / exhibited a permeability of 1.4 ∗ 10−22 𝑚𝑚2 . The
nitrogen as the fluid is (0.01-21) * 105 Pa. To start with, systematic variation of permeability with ODP with
the pressure regulator is connected to compressed air. A different sintered discs is shown in Fig. 4, indicating a
210 Soft Buna-N O-ring was placed in the chamber as linear relationship between flow rate (Q) and pressure
shown in Fig. 1b, to ensure an airtight stack for measuring differential (∆P), in accordance with Darcy’s equation.
accurate fluid flow across the sample of interest, with ODP with a 2 µm disc showed a lower slope (21.45)
grease applied to the O-ring to ensure a leak proof compared to the 20 µm (22.59) vs the 40 µm disc (22.54),
interface (Fig. 1c). The free-standing coating was placed as expected. Table 1 lists the measured slope, and the
on top of the O-ring, followed by the porous sintered disc, viscous permeability coefficient (Yn) calculated using the
as shown in the schematic Fig. 1(d). The cell lid was slope.
secured with four thumb screws, and compressed air was
passed through the combination of porous sintered disc
(P), free standing coating (referred to as ‘dummy coating
– ‘D’) and the O-ring ‘O’. The pressure was controlled by
the pressure regulator and recorded by an electronic
pressure gauge, as shown in Fig. 1a. The rig consisted of
two flow meters (I and II) with maximum flow rates (Q) of
5.6 ml/min and 51 ml/min.

A NiCrAlW air plasma sprayed free standing abradable

coating of unknown porosity was taken as the test
sample ‘D’, in the form of a disc having a diameter of 25.4
mm and 2.47 mm thickness. Porous stainless-steel
sintered discs, with a pore size of 2, 5, 10, 20 and 40 μm,
were procured from McMaster, USA, and verified for
porosity using scanning electron microscopy (Carl Zeiss,
Ultra55, FESEM). Fig. 2 shows representative SEM
micrographs of porous discs of 2 μm (Fig. 2a) and 40 μm
(Fig. 2b) to indicate the pore sizes (inserts). Fig 2c is a
representative SEM micrograph of the NiCrAlW coating
with unknown porosity. The nominal composition of the
coating was 71.92% Ni, 9.14% Cr, 7.47% Al, and 11.46% W as
measured using Energy dispersive X-ray spectroscopy
(EDS).

To characterize the pore size of the coating (D) with

unknown porosity, combinations of the porous discs (P)
and Dummy (D) were utilized in three different
configurations along with the O-ring (O), designated as
OD, OP, and ODP, as depicted in Fig. 3. For each
configuration, nine trials were conducted by three
separate operators to ensure the repeatability of the flow
data.

OP showed high permeability across all pore sizes from 2

μm, 5 μm, 10 μm, 20 μm, and 40 μm) and did not show any Figure 1: (a) Gas Permeability Tester (b) Experimental Cell,
sensitivity to the pressure. In fact, at very low pressures, (c) O-ring with grease, (d) schematic of the coating gas-
the flow maxed out indicating that each disc offered permeability rig
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Figure 2: Representative SEM taken from (a-b) sintered porous discs with average pore sizes of
2 µm and 40 µm, (c) NiCrAlW coating along with its (d) EDS elemental spectrum

Figure 3: Configuration of, O-ring (O), ’D’ and porous sintered discs (P) used for measurements

Figure 4: Flowrate Q (ml/min) vs Differential pressure

 SPRAYTODAY™ | iTSA FEATURE
12 Table 1: Permeability of sample OD and ODP measurement of porosity, based on volumetric flow is
Sample Measured Calculated Permeability valid for pressure drop across interconnected porosity in
µm Slope (𝒎𝒎𝟐𝟐 ) ∗ 𝟏𝟏𝟏𝟏−𝟐𝟐𝟐𝟐 thermal sprayed coatings.
“D” 24.82 1.40
+ 2 µm 21.45 1.21
+ 5 µm 22.69 1.28
+ 10 µm 23.90 1.34
+ 20 µm 25.59 1.44
+ 40 µm 22.54 1.27

It is interesting to note the linear increase in permeability

from 1.21* 10-22 m2 (for 2 µm) with the pore size up to 20
µm (1.44 * 10-22 m2) and the dip to 1.27 * 10-22 m2 for the
40 μm sintered disc. This clearly brings in the choice of
sintered disc for carrying out the measurements on the
coating with unknown porosity and brings in the interplay Figure 5: Permeability of the combination (ODP) vs pore
between the restricted flow between the coating and the size of porous disc
pore size of the disc. For smaller pore sizes (2 μm and 5
μm), the disc introduces an additional bottleneck, limiting Acknowledgments
the flow more than discs with large pores. As pore size
Mr. Andrew A. Verstak from Kermetico Inc is
increases (10 μm and 20 μm), there is a larger volumetric
acknowledged for his valuable discussion. Pratt &
flow diminishes, and the permeability of ODP approaches
Whitney is acknowledged for enabling the internship for
that of the coating alone (1.4∗ 10−22 𝑚𝑚2). As the sintered
Mr. Aadil, at the Pratt & Whitney R&D Center, Bangalore.
discs pore size increases further, to 40 μm, the sheer
The usage of characterization facilities at the Center for
volume of flow ceases to have any significant effect on
Nanoscience and Engineering (CeNSE), IISc, is gratefully
the pressure drop and possibly the thicker framework of
acknowledged.
the disc serving to block accessibility of gas flow through
the coating and hence reduce the overall permeability. References
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 FEATURE SPRAYTODAY™ | iTSA
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