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TASK 70-48-04-220-011

METALLOGRAPHIC EXAMINATION
1. General.
A. The metallographic examination of plasma coatings is used
to detect oxide inclusions, voids, unmelted particles and
other metallurgical defects by comparison with standard
photomicrographs.
B. Produce a test specimen prior to each repair so as to
check the coating to be sprayed over the part for good
quality. Also coat one or several test specimens at the
same time as the part.
C. A new test specimen must be coated each time one of the
R following parameters is changed for initial coating
R qualification (100% frequency):
(1) Material of the repaired part.
(2) Nature of the coating.
(3) Particle size of the powders.
(4) Spraying equipment.
(5) Setting of the spraying equipment.
(6) Surface preparation of the parts.
(7) Personnel carrying out the spraying operations.
R NOTE: Depending upon experience and practice, the
R frequency of producing test specimens required
R for metallographic examination, may be lowered
R as follows :
R As spraying continues, passing data should be
R gathered and analized by an acceptable statistical
R process control (SPC) system. The frequency of
R testing may then be reduced (or the time intervals
R between quality control testing increased)based on
R the statistical analysis if consistent results are
R obtained. The frequency intervals should all be
R based on requirements documented in the repair shop’s
R internal Quality Assurance System.
D. In case of a coating applied over a base coat, a
metallographic inspection is made on a test specimen
sprayed both with the base coating and the finishing top
coat in the same thickness as required for the part.

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2. Test Equipment.
A. Equipment.
(1) Tooling to prepare micrographic sections (slicing
machine, polishing turret, etc.).
(2) Metallographic microscope, magnification power x 100
and 500.
B. Test Specimens.
(1) Dimensions
The test specimens are made of rectangular metal panels.
There is no required size but a recommended size :
approximately 3.0 x 1.75 x 0.05 inches (75 x 45 x 1,2
mm) large enough to be held during the spray and
mounting process.
(2) Material.
Part Material Test Specimen Material
Commercial Designation Specification Ref.
R Austenitic steel
R Martensitic steel AISI 321 or AMS 5510 (Z10CNT18)
R Nickel alloy HASTELLOY X AMS 5536, (NC22FeD)
R Cobalt alloy
Titanium alloy A 40 or T40, AMS 4902
A 110 AT or TA5E, AMS 4910
Ti 6-4 TA6V, AMS 4911
Aluminum alloy 5052 or AG3, AMS 4015
6061 AG1, AMS 4025
3. Suitability Test Specimens
A. Surface Preparation of Test Specimens.
The surface preparation of the test specimens must be
identical to that indicated for the part to be sprayed.
B. Spraying the Coating.
The coating must be sprayed onto the test specimen in
exactly the same way as onto the part.
The thickness of the coating must be:
(1) Suitability test specimens.

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(a) Coatings with no base coat:
0.008 to 0.010 inch (0,20 to 0,25 mm).
(b) Coatings applied over a base coat.
The thicknesses of the base coat and of the
final top coat must be identical to those called
for on the parts.
(2) In-process test specimens.
The thickness of the coating (s) must be identical to
that planned on the parts.
C. Preparing Samples.
(1) The metallographic inspection is done on a 0.8 inch
(20 mm) micrographic section taken from the center of
the test specimen, perpendicular to the spray
direction of the coating.
(2) Obtain the sample by cutting with an abrasive cutoff
wheel, continually watered.
NOTE: Direction of the cut should advisably be
through the coating and moving toward the
substrate to avoid damaging the coating.
(3) Coat the specimen with a film of epoxy resin or
bakelite so that the face under examination is normal
to the spray direction of coating.
(4) Using silicon carbide abrasive paper 120-mesh
particle size or appropriate grinding compound,
prepolish the specimen, with supply of coolant
water. Remove a thickness between 0.06 and 0.10 inch
(1,5 and 2,5 mm) from the initial surface of the
specimen.
(5) Use silicon carbide abrasive paper having finer
particle size - 220, 400, 800 or appropriate polishing
compound to carry out successive polishings, with
supply of coolant water.
(6) Use a 3-micrometer diamond paste to carry out final
polishing.
NOTE: To avoid damaging the coating, apply low
pressure when polishing.
(7) Clean, then dry the surface to be examined.

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D. Mark the test specimen so that the test specimens can be
cross-referenced to the required part.
4. Method of Test.
A. Micrographic examinations are carried out with 100-power
magnification. The regions considered as representing the
average of the specimen are examined under 500 x power
magnification.
B. Typical micrographic appearance of coatings at 500 x
magnification, as shown in figures 1 thru 5 may assist the
metallographer in interpreting the micrographic specimens,
but the decision to accept or reject shall be taken in
accordance with the acceptable limits specified in Table 1.
___________________________________________________________________
Coating Acceptable limits Acceptable limits
for Voids for unmelted
CP No. particles
and Max. Micro- Micro- Max. Micro- Micro-
Description Rate meters inches Rate meters inches
___________________________________________________________________
CP6001 5% 10 400 5% 25 1000
Tungsten Carbide,
Cobalt Powder
CP6002 5% 10 400 10% 25 1000
Cobalt, Chromium,
Nickel,
Tungsten Powder
CP6003 15% 30 1200 15% 60 2400
Copper, Nickel, (NOTE)
Indium Powder
CP6004 5% 10 400 5% 25 1000
Tungsten
Carbide,
Cobalt Powder
CP6005 15% 30 1200 15% 60 2400
Nickel,
Aluminum
Powder

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___________________________________________________________________
Coating Acceptable limits Acceptable limits
for Voids for unmelted
CP No. particles
and Max. Micro- Micro- Max. Micro- Micro-
Description Rate meters inches Rate meters inches
___________________________________________________________________
CP6006 15% 30 1200 15% 60 2400
Nickel,
Chrome,
Aluminum Powder
CP6007 15% 30 1200 15% 60 2400
Nickel, (NOTE)
Aluminum
Powder
CP6008 5% 10 400 5% 25 1000
Tungsten
Carbide
Cobalt Powder
CP6009 15% 25 1000 15% 30 1200
Aluminum
Oxide Powder
CP6010 5% 10 400 5% 25 1000
Aluminum
Silicon
Polyester Powder
CP6011 5% 10 400 5% 25 1000
Aluminum
Bronze
CP6017 5% 20 800 5% 25 1000
Chrome
Carbide
Nickel
Chromium Powder
CP6019 15% 30 1200 15% 60 2400
Molybdenum
Powder
CP6020 10% 20 800 5% 25 1000
Cobalt
Molybdenum
Chromium
Silicon Powder

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___________________________________________________________________
Coating Acceptable limits Acceptable limits
for Voids for unmelted
CP No. particles
and Max. Micro- Micro- Max. Micro- Micro-
Description Rate meters inches Rate meters inches
___________________________________________________________________
CP6021 8% 10 400 5% 25 1000
Triballoy
T800
CP6023 15% 30 1200 15% 90 3600
Nickel
Chromium
Aluminum
Yttrium Powder
CP6024 15% 30 1200 5% 25 1000
Zirconium
Oxide
Yttrium Powder
CP6025 10% 20 800 5% 25 1000
Nickel
Chromium
Iron
Molybdenum Powder
CP6026 5% 10 400 5% 25 1000
Tungsten
Carbide Powder
CP6027 15% 30 1200 15% 60 2400
Copper
Nickel
Indium Powder
CP6028
Aluminum Powder 15% 30 1200 15% 60 2400
CP6029 15% 30 1200 15% 90 3600
Cobalt, Chromium
Nickel, Tunsgten
Powder

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___________________________________________________________________
Coating Acceptable limits Acceptable limits
for Voids for unmelted
CP No. particles
and Max. Micro- Micro- Max. Micro- Micro-
Description Rate meters inches Rate meters inches
___________________________________________________________________
CP6030 10 % 20 800 10 % 85 3400
Aluminum Oxide
Titanium Dioxide
Powder
CP6031 5% 10 400 5% 25 1000
Tungsten Carbide
Cobalt Powder
CP6032 1% 5 200 15% 30 1200
Nickel Chromium Iron
Molybdenum powder
INCO 718-HVOF
CP6033 5% 20 800 5% 25 1000
Chrome Carbide Nickel
Chromium HVOF Powder
CP6041 15% 30 1000 10% 50 2000
Cobalt Chromium Aluminum Ytrium
R Silicium Boron Nitride
R NOTE: For this coating, figures 10 and 11 illustrate the maximum
R and minimum permitted proportions of boron nitride.

___________________________________________________________________
Table 1
C. Voids.
The voids must be evenly distributed, and must meet the
required values indicated in Table 1 for each type of
deposit, both as regards content and size. Figures 1 and
2 show the acceptability limit applicable to void content

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and average diameter (rate and dimension) of the
representative porosity of the coating.
D. Unmelted or Slightly Unmelted Particles.
Unmelted particles or slightly unmelted particles (see
figure 4) must be evenly distributed, and must meet the
required values indicated in Table 1 for each type of
deposit, both as regards content and size (rate and average
diameter).
E. Appearance of the Interface.
Oxides, voids or abrasive grains, located at the metal-to-
coating interface, must not cover more than 25 % of the
length of the micrographic specimen in case of fine,
widely dispersed discontinuities, and 30 % in case of
coarse, isolated discontinuities. See figure 3.
F. Oxides in the Deposit.
Figures 1 and 2 show the acceptability limits for certain
type of coating as regards the oxide content.
G. Cracks.
In case of cracks, the coating is unacceptable. Spraying
conditions shall be reconsidered. See figure 5.

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Typical Micrographic Appearance for 10-45 Micrometer Particle
Size powder
Figure 1

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Typical Micrographic Appearance for 45-90 Micrometer Particle
Size powder
Figure 2

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Typical Appearance of Interface
Figure 3 (Sheet 1 of 2)

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Typical Appearance of Interface
Figure 3 (Sheet 2 of 2)

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Typical Appearance of Unmelted Particles
Figure 4

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Cracks
Figure 5

Typical appearance of oxides inclusions and porosity contents


Projection applied using JET KOTE 2A and jet propulsive propane
Figure 6

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R Voids, porosity and oxides in As-Sprayed Coating
Figure 7

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Interface contamination in the As-Sprayed Coating viewed
200X. Magnification in the As-Polished and Unetched condition
(Note : Arrows show the location of grit, oxide and voids at the
R interface)
Figure 8

Unmelter particles plasma sprayed coating – T800


Note : example of unmelted particle is circled for
identification. Unmelted particles are spherical non flattened,
or partially flattened particles with an aspect ratio of width to
height less than 3:2, viewed at 200X magnification
Figure 9

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R Maximum permitted proportion of boron nitride
R in CP6041 coating
R Figure 10

R Minimum permitted proportion of boron nitride


R in CP6041 coating
R Figure 11

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R Voids and Porosity in as sprayed coating.
Note: Porosity and voids are shown as dark areas.
Figure 12

R
Voids and Porosity in as sprayed coating.
Note: Porosity and voids are shown as dark areas.
Figure 13

R
Oxides in the As-Sprayed Coating viewed at 200X
Magnification in the As-Polished and Unetched
Condition. (Note : Example of concentration of oxides
in clusters are circled.)
Figure 14

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