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Characterization of Thermal Spray Coatings

Characterization of Thermal Spray Coatings

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Description of methods for characterization of HVOF coatings
Description of methods for characterization of HVOF coatings

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Published by: rkkumarcpri on Oct 14, 2010
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MATERIALS CHARACTERIZATION 42:93–100 (1999)© Elsevier Science Inc., 1999. All rights reserved.1044-5803/99/$see front matter655 Avenue of the Americas, New York, NY 10010PII S1044-5803(98)00048-5
haracterization of Thermal Spray Coatings
Brian S. Schorr, Kevin J. Stein, and Arnold R. Marder
Department of Materials Science and Engineering, Lehigh University, Bethlehem, PA 18015-3195
The ability to characterize fully the microstructure of a coating is paramount for under-standing the in-service properties and eventual optimization of the coating. This article dis-cusses sample preparation and subsequent analytical techniques (LOM, SEM, XRD, WDS,and QIA) for several cermet thermal spray coatings and provides a detailed analysis of as-sprayed microstructures in addition to processing trends for several FeCrAIY-carbide coat-ings. It was found that the splats produced in these high velocity oxy-fuel (HVOF) coatingstended to exhibit a predominantly dendritic structure most likely retained from the gas at-omization process that produced the original powder. Chemical analysis showed that thecarbides tend to breakdown during spraying producing a complex mixture of oxides andvarious carbides. Finally, image analysis revealed that as the carbides in the pre-sprayedpowder were increased, more carbides and oxides with less FeCrAIY and thinner coatingswere found. These techniques allow the thorough characterization of thermal spray cermetcoatings, which in turn should further the understanding of the thermal spray processes and help provide superior coatings in the future. © Elsevier Science Inc., 1999. All rightsreserved.
Thermal spray coatings have become animportant part of modern industry, offer-ing customized surface properties for a va-riety of industrial applications ranging fromthermal barrier coatings for high tech tur- bine blades to erosion resistant coatings for boiler tubes. Although the usage of thermalspray coatings has increased dramatically,the characterization and analysis of thesecoatings has lagged behind. Characteriza-tion is critical for understanding why ther-mal spray coatings behave the way they do,and offering guidelines for improved coat-ing performance in the future.Thermal spray coatings are formed bymelting materials in particulate form orwire feed stock and accelerating the moltenor partially molten droplets toward a sub-strate. Once these molten droplets strikethe substrate they expand out in a radialfashion and form a splat. As additional par-ticles impact the specimen splats will even-tually interact with one another and form acontinuous coating. Splat-to-substrate, aswell as splat-to-splat, bonding tends to beweak, providing little resistance to pulloutduring the mechanical processing (cutting,grinding, and polishing) of the coating formetallographic preparation. In addition,multi-phase coatings, such as cermets, canhave enhanced pullout due to the differentsizes and densities of the as-sprayed pow-ders. Consequently, if care is not takenwhen preparing a thermal spray coating foranalysis, pullout can cause erroneous po-rosity, volume %, and even chemistry mea-surements.Several papers have dealt with metallo-graphic preparation and routine analysis ofthermal spray coatings, Blann [1, 2] con-ducted a thorough study of cutting, grind-ing, and polishing procedures on the poros-ity levels of various thermal spray coatings.Blann discovered that by using a low speedcut off saw, diamond lapping discs, lownap polishing clothes, and a vibratory pol-isher the erroneous porosity levels in ther-mal spray coatings, especially cermets,
B. S. Schorr et al.
could be drastically reduced [1,2]. Addi-tionally, by adding a fluorescent dye to theepoxy mounting material porosity andpullout can be further separated. Throughcapillary action the fluorescent dye ispulled into the porosity of the coating andwhen viewed under fluorescent light, theporosity would appear bright while the restof the coating, including the pullout, ap-peared dark.Although there has been some work onmetallographic preparation and routine ex-amination of thermal spray materials, fewstudies have done thorough examinationsof both the chemistry and physical struc-ture of the as sprayed coating. This paper briefly explores some basic sample prepa-ration methodologies and provides in depthtechniques for analysis of complex as sprayedcoatings. The analysis of the coatings centerson quantifying the structure of the coatingand determining the chemical makeup ofthe various phases in the coating.
cermet coatings were ap-plied to low carbon steel substrates using ahigh velocity oxy-fuel (HVOF) spray sys-tem. The carbide ranges sprayed and chem-ical composition of the pre-sprayed pow-ders can be found in Tables 1 and 2respectively.
 Once the samples were sprayed, the coat-ings were then sectioned on a BuhlerIsomet low speed abrasive cut off saw andvacuum mounted in epoxy mixed with afluorescent dye, the configuration of themounted samples can be seen in Fig. 1. Thesamples were mounted coating-to-coatingto help maintain the coating’s edge and avoidrounding. The samples were then groundthrough 600 grit using SiC papers, polishedto 1
 m diamond with a low nap cloth on aBuhler auto polisher, and finally polishedwith colloidal silica for 15 minutes on a vi- bratory polisher. Finally, the coatings wereetched with various chemicals, Table 3, toprovide different contrast mechanisms.
Table 1
Reported Chemistry and Compositions of Pre-Sprayed Powders (all values are wt%)
Powder TypeAluminumCarbonChromiumIronNickelYttriumOther
Table 2
Starting Powder Compositions
Weight % FeCrAlYWeight % Cr
. 1.
Schematic of mounted sample. (A) Epoxymount with dye. (B) Low carbon steel substrate. (C)Thermal spray coating.
Characterization of Thermal Spray Coatings
The coatings were first photographed using both a Zeis and Reikert-Jung light opticalmicroscope (LOM) in addition to a JEOLscanning electron microscope (SEM) to pro-vide preliminary phase identification. TheReikert LOM was used in Nomarski modeto enhance the contrast of the HVOF coat-ings and allow detailed analysis of the coat-ing inter-splat structure. SEM images tendto be sensitive to differences in atomicnumber even in secondary electron imag-ing, where higher atomic number regionswill be darker.The chemistry of the individual phases thatcomprised each coating were determinedusing several complementary methods. X-ray diffraction patterns of all of the coat-ings were obtained using a Siemens diffrac-tometer. In this case, the coatings were re-moved from their substrates and broken upusing liquid nitrogen prior to testing. WDSdot maps were also used to help with phasedetermination and confirm the x-ray datausing a JEOL Superprobe. Finally, micro-hardness measurements of each phase werealso conducted to complete the qualitativechemical analysis of the various coatings.Once the chemical nature of each phasehad been determined the coatings werethen quantified using a LECO 2001 imageanalysis system. The volume percent ofeach phase, in addition to the thickness ofeach coating, was determined. Since thecarbide and FeCrAIY matrix had similargray levels the matrix had to be etchedaway using a HC1-HNO
etch (see Table 3for the composition of this etch). With theFECrAIY matrix gone all of the phasescould be easily distinguished by threshold-ing; the missing FeCrAIY appeared black,the carbides white and the various oxidephases were gray. Figure 2 shows an exam-ple of the thresholding process for a ther-mal spray coating.The volume percent of the FeCrAIY andCr
in the various powder blends werealso verified using a similar etching tech-nique to the final as sprayed coatings men-tioned above. The powders were vacuummounted and a region of the mount wasscribed with a 50
m circle. The volumepercent of the powder within the circle wasthen measured, the FeCrAIY was etchedaway, and the volume percent of the re-maining powder was measured again. Theunetched portion corresponded to the vol-ume percent of carbide present and whensubtracted from 100 produced the volumepercent of FeCrAIY.
 Figure 3a shows the etched microstructureof a 60% FeCrAIY-40% carbide coating.From Fig. 3a it is clear that the heat input(time and temperature) involved in theHVOF process was not high enough to meltthe FeCrAIY or carbide powder. Due to thelack of melting the FeCrAIY structure pro-duced during powder fabrication, dendrites,remained in the final coating. To verify thepresence of the dendrites during powderfabrication, the mounted powder was etchedas shown in Fig. 3b. Figure 3b clearlyshows the same dendritic structure foundin the final coating (Fig. 3a), consequently,it is safe to assume that little, if any, meltinghas occurred and the dendritic structure isretained from gas atomization processingof the powder. It would also be expectedthat any melting would tend to produce a
Table 3
Composition and Use of Etchants
Boiling Picric (electrolytic)5g picric, 2ml HCl, & 100ml H
Oetch FeCrAlY alloy30 secHCl-HNO
mixture12ml HNO
, 20ml HCl,20ml H
O, & 40ml H
etch FeCrAlY and Fe/Al alloy10 sec

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