Metallographic

preparation of thermal
spray coatings Application
Notes
Thermal spraying was invented in the
early 1900s using zinc for „metallizing”
substrates for corrosion protection. The
development of the plasma spray gun in
the late 50s and 60s made it commercially
viable to use high temperature materials
such as ceramics and refractory metals
for coating materials. In addition to flame
and plasma spraying, today thermal spray
methods include high velocity and detona-
tion spraying using a multitude of different
spray materials for the most diverse and
demanding applications.

Thermal spray coatings are applied to a

substrate to give a specific surface quali-
ty, which it originally does not have. Thus Metallography of thermal spray coatings
the bulk strength of a part is given by the can have several purposes:
substrate, and the coating adds superior - To define, monitor and control spraying
surface qualities such as corrosion, wear conditions for quality control
or heat resistance. - For failure analysis
Therefore thermal spray coatings are wide- - For developing new products.
ly used in the aerospace and power gene-
ration industry for new and refurbished The procedure normally involves coating a
sections and parts for jet engines and test coupon to define and optimize the pro-
gas turbines, compressors and pumps. cess for the part to be sprayed. Sections
The properties of some coatings can only of this test coupon are then metallographi-
be fabricated by thermal spraying, using cally prepared and examined to assess
mainly metals, ceramics, carbides and coating thickness, size and distribution of
composites as well as mixtures of various porosity, oxides and cracks, adhesion to
materials. base material, interface contamination and Electric arc metal spray coating, showing grey oxides
and round, unmelted particles
presence of unmelted particles.

Difficulties during metallographic preparation Solution:

Cutting: Cracks in the coating due to Grinding and polishing: Because of smear- - Precision cutting
clamping the sample and using coarse ing of soft materials and pull-outs in brittle - Vacuum impregnation with epoxy resin
cut-off wheels; materials, it is difficult to establish and - Standardized, reproducible preparation
Delamination from substrate evaluate true porosity methods for thermal spray coatings
Mounting: Insufficient penetration of
mounting resin

Crack between a plasma spray coating 500x Fig.1: Ceramic spray coating, 200x Fig. 2: Same coating as Fig.1, 200x
and the substrate. The crack originates insufficiently polished polished correctly
from cutting

Abb. 1: Keramische Spritzschicht, 200x

unzureichend poliert
Riss zwischen Plasmaspritzschicht und 500x Abb. 2: Selbe Beschichtung wie Abb. 1, 200x
Spray methods
and applications
of thermal spray
coatings
Fig. 3:
Flame sprayed
coating; Ni5Al

and therefore the oxide content in these

coatings is relatively high (Fig. 3); adhesion
and density are moderate (subsequent fus-
ing to increase the density is possible).
Flame sprayed coatings are used for corro-
sion protection and/or wear protection of
structures and components, surface build-
up and repair of worn shafts, for coating
small parts and spots.
Brass synchronising rings flame-sprayed with
Unmelted molybdenum for wear resistance
particles Electric Arc spraying uses the heat of
Voids
an electric arc between two continu-
Oxides
Substrate
ous consumable wire electrodes made
of coating material to melt the wires. The
In the spraying process the coating mate- wires intersect in front of a jet of com-
rial, wire or powder, melts in a high tem- pressed air. As the heat from the arc melts
perature heat source in a spray gun and is the wires, the compressed air blows the
accelerated by the flame or plasma jet and molten droplets of the coating material
projected towards the substrate. A stream onto the substrate. The high arc tempera-
of molten and semi-molten particles im- ture and particle velocity gives this coating
pinges onto the substrate and forms a a bond strength and density superior to
coating. When the particles hit the work- flame sprayed coatings. However, because Fig. 4: Electric arc wire-sprayed metal coating

piece they mechanically lock onto the sur- of the use of compressed air the arc FeCrSiNi and Mn

face, deform and cool rapidly. The bonding sprayed coatings have a higher percentage
of single particles is through mechanical of oxides (Fig. 4). the workpiece with extremely high kinetic
interlocking, or in some cases metallurgical The advantage of arc wire spraying is its energy. These coatings have an excel-
bonding or diffusion. High velocity of the high deposition rate which makes it suit- lent density, integrity and adhesion to the
particles leads to better bonding and higher able for large areas or high volume produc- substrate. Due to the process conditions
density of the coating. For good adhesion tion applications: spraying of large struc- this method is limited to the application of
to the substrate it is essential that the tures like bridges and off-shore structures carbide coatings, mainly in the aerospace
surface is roughened by sandblasting and with corrosion resistant zinc or aluminium and aviation industry for wear-resistant
thoroughly degreased and cleaned before coatings, reclamation of engineering com- coatings.
spraying. ponents and spraying of electronic compo-
The various spraying techniques display nent housing with conductive coatings of In High Velocity Oxy-Fuel Combustion
different temperatures at the heat source copper or aluminium. spraying (HVOF) fuel gas and oxygen are
and different particle velocities, which, fed into a chamber in which combustion
together with the economical aspect, need For Detonation spraying small amounts of produces a supersonic flame, which is
to be taken into consideration for specific carbide powder, fuel gas and oxygen are forced down a nozzle increasing its veloc-
applications. In the following the main introduced in a closed tube and exploded. ity. Powder of coating material is fed into
spraying techniques are briefly described The detonation ejects the powder with this stream and the extreme velocity of the
and some of the most well-known applica- multiple sonic speed and shoots it onto particles when hitting the substrate creates
tions of the resulting coatings mentioned:
Principle of layer formation
Flame spraying is the oldest method of ap-
plying thermal spray coatings. The coating
material is either wire or powder, which
is fed into an oxygen-fuel gas flame. The
molten and atomized particles are ejected
in a directed stream through the spraying
gun nozzle. Due to the relatively low particle
velocity the oxygen exposure is increased
Flying drops of molten Impact on substrate Heat dissipation to Solidification and shrinking
coating material substrate of coating material
 Difficulties in
the preparation
of thermal spray
coatings
Fig. 5:
HVOF coating of
WC/12Co

a very dense, strong coating (Fig. 5). The Cutting: Clamping of spray coated work-
very high kinetic energy of the particles pieces for sectioning can introduce cracks
when striking the substrate ensures an in brittle coatings or compress very soft
adequate mechanical bond even without coatings.
the particles being fully molten. This makes
this spraying method particularly well-sui-
ted for spraying of coatings with carbides.
Typical applications are tungsten carbide
coatings on air engine turbine components
Combustion chamber with APS thermal barrier coating,
and valves, and nickel-chromium coatings bond coat NiCrAlY, topcoat ZrO² + Y² O³
for oxidation resistance.

Plasma spraying is the most common

method for thermal spray coatings, and is
applied as Air Plasma Spraying (APS) or Cracks introduced through sectioning
spraying under controlled atmosphere. An
electric arc is formed between a cathode Mounting: Cold mounting resins with high
and the concentric nozzle of the spray gun. shrinkage can cause damage to coatings
A mixture of gases with a high flow rate with weak adhesion to the substrate; due
along the electrode is ionised by the arc, to the shrinkage gap the coating is not
and forms plasma. This plasma stream is supported by resin, which can lead to de-
pushed out of the nozzle, where the pow- Fig. 6: APS coating with NiCr bond coat and titanium lamination of the coating during grinding
der of the coating material is injected into oxide top coating and polishing.
the plasma jet. The heat and velocity of the
plasma jet rapidly melts and accelerates high quality coatings and used for a wide Grinding and polishing: Edge-rounding can
the particles so that they are propelled onto range of applications, including coatings on lead to uneven polishing and subsequent
the substrate and form a coating. Plasma traction surfaces, thermal barrier coatings misinterpretation of the coating density
sprayed coatings have a denser structure on turbine combustion chambers, vanes (Fig. 7). Relief between coating and sub-
than flame sprayed coatings (compare and blades, biocompatible hydroxylapatite strate creates a shadow that can be misin-
Figs. 3 and 6). coatings for implants and ceramic coatings terpreted (Fig. 8).
Plasma spraying has the advantage that on print rolls.
it can spray materials with high melting How to estimate the true porosity in a me-
points such as ceramics or refractory met- tallographically prepared spray coating is
als. It is a versatile spraying method for still a reason for debate, as metallographic
grinding and polishing, if not carried out

Water cooled electrode, Powder injector (external)

cathode
Insulator
Plasmajet

Coating material

Fig. 7: Incorrect polish suggests less porosity

in the middle of the coating
Cooling
water Water cooled nozzle, anode

Plasma Plasma gases,

gases primary gases: Ar1, N2
secondary gases: H2, He
– +

Current
250 - 1000 A

Fig. 8: WC/Co spray coating with relief polish

Schematic drawing shows dark line at resin/coating interface.
of plasma spray gun Can lead to misinterpretation.
 Nickel flame spray coating
with 15% graphite

a) Metal spray coating after fine grinding

correctly, can introduce artefacts which are When cutting pieces other than test cou-
not part of the coating structure. For exam- pons, for instance samples for failure
ple, in metal or metal/ceramic coatings, the analysis, it is important to ensure that the
softer metal is smeared into pores during workpiece is clamped into the cut-off ma-
grinding and if not polished properly can chine in such a way that the cut-off wheel
cover up the true porosity (see Figs. a-c). is cutting into the coating towards the
In comparison, ceramic coatings are brit- substrate, and not from the substrate into
tle and particles break out of the surface the coating. As the bond of the coating is
during grinding. If not polished thoroughly, mainly mechanical, it can delaminate from
b) Same coating as in a) polished with 3 µm these break-outs leave an incorrect impres- the substrate due to the drag of the cut-off
sion of a high porosity (see Figs. d-f). wheel.

Particularly fragile or thin coatings can

Recommendations for first be vacuum impregnated with cold
the preparation of thermal mounting epoxy resin, and then the micro
spray coatings sections are cut and remounted for grind-
As there are many different spraying ing and polishing. This ensures maximum
materials with sometimes unusual com- support to the coating during sectioning.
binations, it is important to know the
correct spraying and substrate material. It The appearance of cracks in a coating
c) Same coating as in b) after final polish facilitates to estimate how the materials will after final polishing may or may not be
behave under mechanical abrasion. As dif- the result of cutting. It is recommended to
ferent spraying processes result in different regrind and polish the sample. If the crack
coating densities and structures it also is from cutting it will usually disappear, if
helps to know the spraying method used it is inherent in the coating it will reappear,
on a particular sample in order to estimate or cracks will surface in other areas of the
the expected porosity and oxide content. coating.

Cutting: Selection of the cut-off wheel is Mounting: Cold mounting with epoxy resin
based on the substrate material, which (ProntoFix , EpoFix, CaldoFix-2) is recom-
is usually metallic. A wheel with a looser mended as spray coatings are very easily
d) Ceramic spray coating after fine grinding bond (soft) is preferable to a denser bond damaged during hot compression mount-
(hard) as brittle particles of the coating ing (Figs. 9 and 10).
are dragged out by a hard cut-off wheel. In general, vacuum impregnation is rec-
This is particularly ommended for all
important when coatings. The depth
cutting parts with of impregnation var-
ceramic coatings. ies with the degree
Even if the coat- of open porosity and
ing is ceramic, it interconnections be-
constitutes only a tween the pores. Very
small percentage of the total cross section- porous coatings can be easier impregnated
e) Same coating as in d) polished with 3 µm al area and does not need to be cut with a than denser ones, and coatings with less
diamond cut-off wheel. Usually sectioning than 10% porosity can not be impreg-
is possible with a soft aluminium oxide nated successfully. As it can be difficult to
wheel. If the ceramic coating is very thick distinguish voids filled with transparent
and dense a resin-bonded diamond cut-off or translucent mounting resins from the
wheel can be used as an alternative. structural elements of the coating, it helps
to mix a fluorescent dye (Epodye) into the
A thin piece of styrofoam between clamps cold mounting resin. Viewed with a long
and sample can help to protect brittle and pass blue filter and a short pass orange
very soft coatings from being damaged. filter in the microscope, the fluorescent dye

f) Same coating as in e) after final polish

 Standard preparation method for
thermal spray coatings
Grinding

Step PG FG

Surface Foil/Paper MD-Largo

Fig.9: Damage to ceramic spray coating 200x Type SiC Diamond

due to hot compression mounting
Abrasive
Size #220 9 μm

examined as a whole, plane grinding with a Suspension/ Water DiaPro

stone may be preferred as it is faster. Lubricant Allegro/Largo 9*
Abb. 9: Beschädigung einer keramischen 200x
Spritzschicht durch Heißeinbetten Whichever method is use, one must always
be aware that the first preparation step rpm 300 150
should aim to re-
move any cracks that Force [N]/ 30 30
specimen
Fig. 9 : endommagement d'un revêtement 200x arise from cutting
par projection de céramique dû à
un enrobage à chaud avec compression without introducing
Time (min) Until plane 5
new damage from
coarse grinding.
Fig.10: Same coating as in Fig. 9, cold mounted 200x
Polishing
To retain flatness and assure a good mate-
Fig. 9: Daño en recubrimiento con spray cerámico 200x rial removal rate, fine grinding is preferably Step DP 1 DP 2 **
debido a embutición en caliente
done with diamond on a composite fine
Abb. 10: Dieselbe Beschichtung 200x grinding disc. For ceramic coatings the fine
Surface MD-Dac MD-Nap
wie in Abb. 9, in Kalteinbettung grinding disc MD-Allegro is recommended,
and for metal coatings MD-Largo. A tho- Type Diamond Diamond
rough polishing on a silk cloth (MD-Dur or Abrasive
图 9：
由于热压缩镶样对陶瓷喷涂层造成的损坏 200x Size 3 μm 1 μm
MD-Dac) will retain the flatness of the sam-
ple and guarantee the removal of smeared Suspension/ DiaPro DiaPro
Lubricant Dac 3* Nap B 1*
metal.
Fig. 10 : même revêtement que fig. 9, 200x
enrobé àWC/Co
Fig.11: froid plasma spray coating in bright field rpm 150 150
Metal coatings can be fine polished either
with 1 µm diamond or a colloidal silica
Force [N]/ 30 20
(OP-U NonDry) on a soft cloth. It is not specimen
recommended to use the colloidal silica
suspension OP-S NonDry for polishing Time (min) 5 1
Fig. 10: Mismo recubrimiento que en la Fig. 9; 200x metal spray coatings as it creates too much
embutición en frío relief. However, OP-S NonDry is suitable Valid for 6 mounted samples, 30 mm diam. clamped
for the final polishing of ceramic coatings in a holder.

as it gives a good contrast to the structure. Remarks:

*Alternatively DiaPro diamond suspension can be replaced
by DP-Suspension, P, 9 µm, 3 µm and 1 µm respectively,
In the trial stage for establishing prepara- applied with blue lubricant.
Fig.12: Same coating as in Fig.11 in fluorescent light tion methods both silicon carbide and **Alternatively, this diamond polishing step can be
diamond grinding can be tried to find out replaced by a polishing step with colloidal silica (OP-U NonDry
图 10：
will 与图 9 those
colour 相同的涂层，voids冷镶嵌 200x
yellow which have for metal, OP-S NonDry for ceramic coatings) for 30-60 sec.
which is the more suitable plane grinding
been filled with resin by the impregnation
method. The same applies to the final pol-
(Fig.11 and 12). The preparation method in the table
ishing step, for which 1µm diamond might
Unfortunately this method is not always above has successfully been used for the
in some cases be preferable to colloidal
applicable for ceramic coatings, because most common coatings. The data are for
silica.
ceramics are translucent and the whole 6 mounted samples, 30 mm diameter,
coating appears fluorescent. In general it is recommended that, if pos- clamped into a holder. DiaPro diamond
sible, a standard procedure is always used suspension can be replaced by DP-Sus-
Grinding and polishing: As a general rule for all coatings. With automatic preparation pension 9 µm, 3 µm and 1 µm respectively,
plane grinding should start with the finest equipment it is possible to control prepara- applied with blue lubricant.
possible silicon carbide foil/paper to avoid tion parameters, which guarantees consist-
creating artificial porosity by fracturing brit- ent results and excellent reproducibility. By Etching: In general, etchants that are rec-
tle particles. Exceptions can be very dense keeping the preparation conditions con- ommended for a specific material can also
or thick ceramic coatings, which are plane stant, it can then be assumed that sudden be used for spray coatings of this material.
ground more efficiently with diamond differences in the microstructure in most It can be expected that the more similar
(with e.g. MD-Piano 220). For high sample cases reflect differences in the spraying the substrate and coating materials are, the
volumes or large parts, which need to be process and not in the preparation process. more even the etching attack will be.
 Struers ApS
Pederstrupvej 84
DK-2750 Ballerup, Denmark
Phone +45 44 600 800
Fax +45 44 600 801
[email protected]
www.struers.com
Thermally sprayed
acetabular cup shell AUSTRALIAN & NEW ZEALAND NETHERLANDS
Struers Australia Struers GmbH Nederland
27 Mayneview Street Zomerdijk 34 A
Coatings sprayed in a controlled atmos- Milton QLD 4064 3143 CT Maassluis
Australia Telefoon +31 (10) 599 7209
phere have few or no oxides and it is dif- Phone +61 7 3512 9600 Fax +31 (10) 5997201
Fax +61 7 3369 8200 [email protected]
ficult to recognize the coating structure. [email protected]
NORWAY
Therefore these types of coatings need to BELGIUM (Wallonie) Struers ApS, Norge
Struers S.A.S. Sjøskogenveien 44C
be contrasted with chemical etching. 370, rue du Marché Rollay 1407 Vinterbro
F- 94507 Champigny Telefon +47 970 94 285
sur Marne Cedex [email protected]
Téléphone +33 1 5509 1430
Vacuum sprayed coatings on nickel and Télécopie +33 1 5509 1449 AUSTRIA
[email protected] Struers GmbH
cobalt based superalloys can be etched Zweigniederlassung Österreich
with the same solutions used for the sub- BELGIUM (Flanders)
Struers GmbH Nederland
Betriebsgebiet Puch Nord 8
5412 Puch
strate, or electrolytically with 10% aqueous SEM photomicrograph of thermally sprayed surface
Zomerdijk 34 A
3143 CT Maassluis
Telefon +43 6245 70567
Fax +43 6245 70567-78
oxalic acid. of acetabular cup shell Telefoon +31 (10) 599 7209 [email protected]
Fax +31 (10) 5997201
The structure of coatings containing mo- [email protected] POLAND
Struers Sp. z o.o.
lybdenum can be revealed by using the and that the diamond polish needs to be CANADA
Struers Ltd.
Oddział w Polsce
ul. Jasnogórska 44
following etchant: long enough to reveal the true porosity. 7275 West Credit Avenue 31-358 Kraków
Mississauga, Ontario L5N 5M9 Phone +48 12 661 20 60
Phone +1 905-814-8855 Fax +48 12 626 01 46
50 ml water Fax +1 905-814-1440 [email protected]
50 ml hydrogen peroxide (3%) The recommended preparation procedure [email protected]
ROMANIA
50 ml ammonia is based on experience and gives excel- CHINA Struers GmbH, Sucursala Bucuresti
Struers Ltd. Str. Preciziei nr. 6R
lent results for the majority of common No. 1696 Zhang Heng Road 062203 sector 6, Bucuresti
Caution: Always follow the recommended thermal spray coatings. However, it should
Zhang Jiang Hi-Tech Park
Shanghai 201203, P.R. China
Phone +40 (31) 101 9548
Fax +40 (31) 101 9549
safety precautions when working with be noted that for some specific proprietary
Phone +86 (21) 6035 3900
Fax +86 (21) 6035 3999
[email protected]

chemical reagents. coatings the polishing times may need to [email protected] SWITZERLAND
Struers GmbH
CZECH REPUBLIC & SLOVAKIA Zweigniederlassung Schweiz
be adjusted. Struers GmbH Organizační složka Weissenbrunnenstraße 41
Summary vědeckotechnický park
Přílepská 1920,
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Telefon +41 44 777 63 07
Thermal spray coatings are widely used to CZ-252 63 Roztoky u Prahy Fax +41 44 777 63 09
Application Notes Phone +420 233 312 625 [email protected]
give or improve a specific surface quality Metallographic preparation of thermal spray coatings Fax +420 233 312 640
[email protected] SINGAPORE
or function to a workpiece. Different spray- Elisabeth Weidmann, Anne Guesnier, Struers A/S, [email protected] Struers Singapore
627A Aljunied Road,
ing methods result in different character- Copenhagen, Denmark GERMANY #07-08 BizTech Centre
Brigitte Duclos, Struers S.A.S., Champigny, France Struers GmbH Singapore 389842
istics of the coatings, and they are mainly Carl-Friedrich-Benz-Straße 5 Phone +65 6299 2268
Acknowledgement D- 47877 Willich Fax +65 6299 2661
applied for corrosion, heat and wear resist- We wish to thank Sulzer Metco AG, Wohlen, Switzerland, Telefon +49 (0) 2154 486-0 [email protected]
Fax +49 (0) 2154 486-222
ance. Metallographic examination of spray for its cooperation and supplying information material. [email protected] SPAIN
Special thanks go to J. Hochstrasser and P. Ambühl for Struers España
coatings includes estimation of porosity, FRANCE Camino Cerro de los Gamos 1
sharing their extensive knowledge with us and supplying Struers S.A.S. Building 1 - Pozuelo de Alarcón
oxides and unmelted particles as well as the following images for reproduction: photo of spraying 370, rue du Marché Rollay CP 28224 Madrid
F-94507 Champigny Teléfono +34 917 901 204
adhesion to the substrate. Because incor- process and large micrograph on page 1; drawing:
sur Marne Cedex Fax +34 917 901 112
Principle of particle movement, photo synchronising Téléphone +33 1 5509 1430 [email protected]
rect grinding and polishing procedures can rings and micrographs on page 2; drawing, photo Télécopie +33 1 5509 1449
influence the evaluation of the true porosity combustion chamber and all micrographs on page 3 and [email protected] FINLAND
Struers ApS, Suomi
micrograph of nickel flame sprayed coating on page 4.
it is very important that metallographic HUNGARY
Struers GmbH
Hietalahdenranta 13
00180 Helsinki
We thank Richard Compton, Zimmer, Inc. USA, for
preparation is carried out systemati- the photo of the acetabular cup shell and the SEM
Magyarországi Fióktelep
Tatai ut 53
Puhelin +358 (0)207 919 430
Faksi +358 (0)207 919 431
cally and that the results are reproducible. photomicrograph on page 6. 2821 Gyermely
Phone +36 (34) 880546
[email protected]

Precision cutting with the correct cut-off Bibliography Fax +36 (34) 880547
[email protected]
SWEDEN
Struers Sverige
Metallographic preparation of thermally sprayed
wheel is recommended to avoid cracks in orthopaedic devices, Richard C. Compton, Zimmer, Inc.,
Box 20038
IRELAND 161 02 Bromma
the coating. Mounting should follow with USA, Structure 28, 1995 Struers Ltd. Telefon +46 (0)8 447 53 90
Unit 11 Evolution@ AMP Telefax +46 (0)8 447 53 99
Summary Report of the Plasma Spray Coatings
epoxy. Coarse grinding introduces the Whittle Way, Catcliffe [email protected]
Symposium at Struers, Copenhagen, May 25th to 27th, Rotherham S60 5BL
most damage to the coating and should 1988 Tel. +44 0845 604 6664 UNITED KINGDOM
Fax +44 0845 604 6651 Struers Ltd.
therefore be carried out with the finest grit Universal metallographic procedure for thermal spray [email protected] Unit 11 Evolution @ AMP
coatings, S. D. Glancy, Structure 29, 1996 Whittle Way, Catcliffe
possible. To avoid relief fine grinding with Materialographic characterization of modern multilayer ITALY Rotherham S60 5BL
Struers Italia Tel. +44 0845 604 6664
diamond on a rigid disc is recommended, coating systems used for hot-gas components in large Via Monte Grappa 80/4 Fax +44 0845 604 6651
gas turbines for static power generation, A. Neidel, 20020 Arese (MI) [email protected]
followed by a thorough diamond polish on S. Riesenbeck, T. Ulrich, J. Völker, Chunming Yao, Tel. +39-02/38236281
Fax +39-02/38236274 USA
a silk cloth. Siemens Power Generation, Berlin, Structure 2/2004 [email protected] Struers Inc.
24766 Detroit Road
JAPAN
It is particularly important to be aware that Marumoto Struers K.K.
Westlake, OH 44145-1598
Phone +1 440 871 0071
metal coatings behave differently to cera- Takanawa Muse Bldg. 1F
3-14-13 Higashi-Gotanda,
Fax +1 440 871 8188
[email protected]
mic coatings under mechanical abrasion Shinagawa
Tokyo
141-0022 Japan
Phone +81 3 5488 6207
Fax +81 3 5488 6237
[email protected]