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[1] Zhang, J., & Singer, R.F. R.F. (2004). Effect of Zr and B on Castability of Ni-Based Superalloy IN792. Metallurgical and Materials Transactions,1337-342. [2] Radavich, J.F. (1979). A decade of study of Hf modified alloys. High Temperatures Seminar Report, Purdue University, 152-153 Susceptibility of Ni-Based Superalloys to Hot Tears with Minor Element Additions Student names: Faseel Ahmed, Theodore Curtiss, Varsha Ganapathy, Jason Kint Faculty Advisors: Dr. David Johnson Industrial Sponsors: Brian Griffin and Andrew Hinshaw Project Background Hot tearing susceptibility was investigated through minor element additions. After casting four molds each separately doped with B, P, Si, and Hf, the microstructural changes were observed to determine correlations to hot tearing. The P and Hf- doped molds exhibited the worst hot tearing properties due to an increased difference in the equilibrium and non-equilibrium solidus during solidification, segregation, and eutectic pool clustering. According to the microstructures, the B-doped mold should have developed a hot tear because it behaved similarly to the P and Hf-doped molds. When casting Ni-based superalloys, elements that contribute to these properties should be avoided to decrease the likelihood of hot tearing. Experimental Procedure Results & Discussion Recommendations Future work can include looking at solidification rates in the alloys. By decreasing solidification rates, the ΔT actual would become less than the ΔT E-S . From the results seen in the Si- doped mold, this would decrease the susceptibility to hot tear. Other future work can include using an alloy that has hot tearing problems to observe if additions can decrease hot tearing susceptibility. The B-doped mold’s microstructure was similar to that of P and Hf-doped molds, yet exhibited no noticeable hot tears. More research into B should be made. X-ray Photoelectron Spectroscopy can provide quantitative chemistry distribution and segregation data. MSE 430- 440: Materials Processing and Design This work is sponsored by Arconic Power and Propulsion, Whitehall, MI Arconic Power and Propulsion is a leader in investment casting superalloys for use in aero engines and industrial gas turbines. A casting defect called hot tearing occurs upon the last stages of the solidification process. Eutectic pools solidify last; thus, grain coalescence makes it difficult to feed the interdendritic regions. This coupled with solidification shrinkage induced tensile stresses can initiate a hot tear along grain boundaries. The need of this project is to understand compositional effects on the tendency to hot tear and the interactions at and away from the grain boundaries of Inconel 738 (IN738) with minor element additions. The goal is to understand compositional effects on microstructure and the tendency to hot tear in IN738. The interpretation of these results can then be carried over to other families of superalloys to alleviate hot tearing during investment casting. Figure 1:Schematic of (a) hot tearing insensitive and (b) hot tearing sensitive . Direction of the applied tensile stresses are indicated [1]. Arconic investment cast four molds, each containing eight hot tear specimens, eight tensile specimens, and two chemistry slugs. Each mold had a minor element addition. Mold 1 contained 0.034 wt.% B. Mold 2 contained 0.009 wt.% P. Mold 3 contained 0.1 wt.% Si. Mold 4 contained 0.39 wt.% Hf. Boron was added because research suggests it segregates at the grain boundaries and weakens grain boundary coalescence. Phosphorus lowers final solidification temperature and has been linked to hot tearing in industry. Silicon was chosen because it is a tramp element and has been linked to increasing the area of the mushy zone. Hafnium segregates heavily but is the industry standard to prevent hot tears. [2] High temperature tensile testing at 2000 °F was utilized to replicate intergranular fracture during solidification. Thermo-Calc software was utilized to investigate solidification behavior with element additions. The samples were sectioned, mounted, etched, and analyzed via optical and SEM microscopy. Figure 4: SEM image showing γ/γ’ eutectic and MC carbide along a hot tear crack in IN100 Post Investment Casting Investigation Mold Tensile Bar Specimen Hot Tear Count Hot Tear Specimen Hot Tear Count B-doped 0 0 P-doped 4 2 Si-doped 0 0 Hf-doped 3 0 Table 1 contains a list of what molds had observable hot tears in the tensile bars and hot tear specimen bars. Of the 16 specimens cast, 6 had hot tears in the P-dope mold and 3 from the Hf-doped mold. In the P-doped mold, hot tear specimens 1 and 2 exhibited a hot tear. This suggests that there is a correlation between constraint in the mold geometry and hot tearing susceptibility. Equilibrium and Non-Equilibrium Solidification Figure 2: The geometry of the hot tear specimens investment cast by Arconic. Note the change in the notch for the hot tear specimens. The specimens with larger notches are expected to hot tear due to the geometric constraint Figure 3: Image of Mold 1 before sectioning Table 1: A table containing observable hot tears after investment casting occurred. Figure 5: Hot tear specimens (left) and tensile bar specimens (right) after being broken out from the mold and sectioned. Figure 6: Scheil and Equilibrium solidification curves for the four altered chemistries. Baseline B-doped P -doped Si-doped Hf -doped Solidification Simulation Equilibrium Solidification Temperature (°C) Scheil Solidification Temperature (°C) ΔT E-S Composition of Last Liquid to Freeze (wt.%) Percent Increase in Concentration Baseline 1314 1177 137 - - B-doped 1253 1028 225 1.02 2900 P-doped 1117 908 209 0.73 8011 Si-doped 1312 1170 142 0.63 530 Hf-doped 1251 949 302 44.4 11,285 The Thermo-Calc analysis shows that all the doped chemistries, with the exception of Si, increase the equilibrium and non- equilibrium final temperature difference (ΔT E-S ) to above 200°C. Hafnium segregates the heaviest, followed by P and B. Silicon segregates the least and suggests it mixes better in Ni. It is hypothesized that the reason Hf and P experienced hot tears during solidification is due to the high levels of segregation these elements exhibit. Lower solidification temperatures coupled with segregation can promote eutectic pool formation and increase the amount of the last liquid to solidify. Increasing the amount of last liquid to freeze that is difficult to freeze in the interdendritic regions will increase hot tearing susceptibility. Table 2: Scheil and Equilibrium solidification data for the four altered chemistries. Carbide Distributions & Volume Fractions Figure 7: Unetched optical micrographs of undoped IN738 gating, B addition, P addition, Si addition, and Hf addition showing the carbides obtained from the chemistry slugs Carbide morphology and volume percent were found to be similar across all samples. The volume percent of the IN738 gating, B- doped, P-doped, Si-doped, and Hf-doped were 1.35%, 1.91%, 2.44%, 2.31%, and 1.81% respectively. Due to similarities in carbide morphology and volume percent, carbides are not believed to be related with the observed hot tearing behavior. IN738 Gating B-doped P -doped Si-doped Hf -doped Correlation of Tensile Fracture Surfaces with Eutectic Pool Morphology Figure 8: Optical micrographs of eutectic pools obtained from the chemistry slug specimens. B-doped P -doped Si-doped Hf -doped Figure 9: Optical micrographs of the high temperature tensile test fracture surfaces taken longitudinally. B-doped P -doped Si-doped Hf -doped Mold Eutectic Pool Volume Fraction Average and Standard Deviation Average Max Eutectic Pool Clustering Length and Std. Dev (μm) Volume Percent of Voids Near Fracture Surface and 95% C. I. B-doped 0.14 ± 0.05 342.5 ± 86.7 8.3 ± 2.5 P-doped 0.14 ± 0.09 395.6 ± 17.3 16.1 ± 6.7 Si-doped 0.04 ± 0.02 89.8 ± 17.3 0.5 ± 1.6 Hf-doped 0.14 ± 0.06 242.5 ± 47.6 8.8 ± 2.1 Table 3: Data of eutectic pool volume fractions away from fracture, volume percent of voids near the fracture, and the average maximum eutectic pool clustering length of the tensile bar specimens. . Boron pools tended to be thick in both directions and cluster often. Phosphorus pools are longer and thin and experience the heaviest clustering. Silicon pools are large but isolated. Hafnium had pools were largest but were very spread out throughout the microstructure with the least amount of coarse gamma prime. Large and long eutectic pools creates a torturous feeding path. The voids in the high temperature tensile specimens, caused by tensile stresses during tensile testing, take on the shape of the eutectic pools and occur between dendrite arms. This is where eutectic pools form as solute is partitioned to the interdendritic regions during solidification. The Si-doped sample has the fewest voids as well as the lowest volume fraction of eutectic pools. Under solidification stresses these areas are the first to separate and provide paths for hot tears to form. References Observed Correlations • Boron, P, and Hf-doped molds had a ΔT E-S above 200°C creating microstructures with large eutectic pool volumes and heavy clustering. By lowering the composition of elements that lower solidification temperatures, promote segregation, and increase the eutectic pool clustering, hot tearing susceptibility can be decreased. • The baseline and Si addition showed a ΔT E-S below 200°C. The solidification behavior of the Si addition was similar to the baseline. The Si-doped molds exhibited microstructures with isolated eutectic pools and little clustering leading to low hot tearing susceptibility. • Clustering of eutectic pools along grain boundaries could be pulled apart more easily during solidification to form a hot tear. Phosphorus and Hf-doped molds developed hot tears during casting and showed significant eutectic pool volume fraction and clustering. • Molds with high eutectic pool clustering formed more voids during high temperature tensile testing showing the ability to pull apart eutectic pools. Phosphorous-doped molds had the most voids from the tensile test showing the weakest intergranular constituents which led to the most hot tears during casting.

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[1] Zhang, J., & Singer, R.F. R.F. (2004). Effect of Zr and B on Castability of Ni-Based Superalloy IN792. Metallurgical and Materials Transactions,1337-342.[2] Radavich, J.F. (1979). A decade of study of Hf modified alloys. High Temperatures Seminar Report, Purdue University, 152-153

Susceptibility of Ni-Based Superalloys to Hot Tears with Minor Element AdditionsStudent names: Faseel Ahmed, Theodore Curtiss, Varsha Ganapathy, Jason KintFaculty Advisors: Dr. David JohnsonIndustrial Sponsors: Brian Griffin and Andrew Hinshaw

Project Background

Hot tearing susceptibility was investigated through minor element additions. After casting four molds each separately dopedwith B, P, Si, and Hf, the microstructural changes were observed to determine correlations to hot tearing. The P and Hf-doped molds exhibited the worst hot tearing properties due to an increased difference in the equilibrium and non-equilibriumsolidus during solidification, segregation, and eutectic pool clustering. According to the microstructures, the B-doped moldshould have developed a hot tear because it behaved similarly to the P and Hf-doped molds. When casting Ni-basedsuperalloys, elements that contribute to these properties should be avoided to decrease the likelihood of hot tearing.

Experimental Procedure

Results & Discussion

RecommendationsFuture work can include looking at solidification rates in thealloys. By decreasing solidification rates, the ΔTactual wouldbecome less than the ΔTE-S . From the results seen in the Si-doped mold, this would decrease the susceptibility to hottear. Other future work can include using an alloy that hashot tearing problems to observe if additions can decreasehot tearing susceptibility. The B-doped mold’s microstructurewas similar to that of P and Hf-doped molds, yet exhibited nonoticeable hot tears. More research into B should be made.X-ray Photoelectron Spectroscopy can provide quantitativechemistry distribution and segregation data.

MSE 430-440: Mater ials Processing and Design

This work is sponsored by Arconic Powerand Propulsion, Whitehall, MI

Arconic Power and Propulsion is a leader in investmentcasting superalloys for use in aero engines and industrial gasturbines. A casting defect called hot tearing occurs upon thelast stages of the solidification process. Eutectic poolssolidify last; thus, grain coalescence makes it difficult to feedthe interdendritic regions. This coupled with solidificationshrinkage induced tensile stresses can initiate a hot tearalong grain boundaries. The need of this project is tounderstand compositional effects on the tendency to hot tearand the interactions at and away from the grain boundariesof Inconel 738 (IN738) with minor element additions. Thegoal is to understand compositional effects on microstructureand the tendency to hot tear in IN738. The interpretation ofthese results can then be carried over to other families ofsuperalloys to alleviate hot tearing during investment casting.

Figure 1:Schematic of (a) hot tearing insensitive and (b) hot tearing sensitive . Direction of the applied tensile stresses are indicated [1].

Arconic investment cast four molds, each containing eighthot tear specimens, eight tensile specimens, and twochemistry slugs. Each mold had a minor element addition.Mold 1 contained 0.034 wt.% B. Mold 2 contained 0.009wt.% P. Mold 3 contained 0.1 wt.% Si. Mold 4 contained0.39 wt.% Hf. Boron was added because research suggestsit segregates at the grain boundaries and weakens grainboundary coalescence. Phosphorus lowers finalsolidification temperature and has been linked to hot tearingin industry. Silicon was chosen because it is a trampelement and has been linked to increasing the area of themushy zone. Hafnium segregates heavily but is the industrystandard to prevent hot tears. [2]

High temperature tensile testing at 2000 °F was utilized toreplicate intergranular fracture during solidification.Thermo-Calc software was utilized to investigatesolidification behavior with element additions. The sampleswere sectioned, mounted, etched, and analyzed via opticaland SEM microscopy.

Figure 4: SEM image showing γ/γ’ eutectic and MC carbide along a hot tear crack in IN100

Post Investment Casting Investigation

Mold Tensile Bar Specimen Hot Tear Count

Hot Tear Specimen Hot Tear Count

B-doped 0 0P-doped 4 2Si-doped 0 0Hf-doped 3 0

Table 1 contains a list of whatmolds had observable hot tearsin the tensile bars and hot tearspecimen bars. Of the 16specimens cast, 6 had hot tearsin the P-dope mold and 3 fromthe Hf-doped mold.

In the P-doped mold, hot tear specimens 1 and 2 exhibited a hottear. This suggests that there is a correlation between constraintin the mold geometry and hot tearing susceptibility.

Equilibrium and Non-Equilibrium Solidification

Figure 2: The geometry of the hot tear specimens investment cast by Arconic. Note the change in the notch for the hot tear specimens. The specimens with larger notches are expected to hot tear due to the

geometric constraint

Figure 3: Image of Mold 1 before sectioning

Table 1: A table containing observable hot tears after investment casting occurred.

Figure 5: Hot tear specimens (left) and tensile bar specimens (right) after being broken out from the

mold and sectioned.

Figure 6: Scheil and Equilibrium solidification curves for the four altered chemistries.

Baseline B-doped P-doped

Si-doped Hf-doped

Solidification Simulation

Equilibrium SolidificationTemperature

(°C)

Scheil SolidificationTemperature

(°C)

ΔTE-S

Composition of Last Liquid to Freeze (wt.%)

Percent Increase in

Concentration

Baseline 1314 1177 137 - -

B-doped 1253 1028 225 1.02 2900

P-doped 1117 908 209 0.73 8011

Si-doped 1312 1170 142 0.63 530

Hf-doped 1251 949 302 44.4 11,285

The Thermo-Calc analysis shows that all the doped chemistries,with the exception of Si, increase the equilibrium and non-equilibrium final temperature difference (ΔTE-S) to above 200°C.Hafnium segregates the heaviest, followed by P and B. Siliconsegregates the least and suggests it mixes better in Ni. It ishypothesized that the reason Hf and P experienced hot tearsduring solidification is due to the high levels of segregation theseelements exhibit. Lower solidification temperatures coupled withsegregation can promote eutectic pool formation and increase theamount of the last liquid to solidify. Increasing the amount of lastliquid to freeze that is difficult to freeze in the interdendriticregions will increase hot tearing susceptibility.

Table 2: Scheil and Equilibrium solidification data for the four altered chemistries.

Carbide Distributions & Volume Fractions

Figure 7: Unetched optical micrographs of undoped IN738 gating, B addition, P addition, Si addition, and Hf addition showing the carbides obtained from the chemistry slugs

Carbide morphology and volume percent were found to be similaracross all samples. The volume percent of the IN738 gating, B-doped, P-doped, Si-doped, and Hf-doped were 1.35%, 1.91%,2.44%, 2.31%, and 1.81% respectively. Due to similarities incarbide morphology and volume percent, carbides are notbelieved to be related with the observed hot tearing behavior.

IN738 Gating B-doped P-doped

Si-doped Hf-doped

Correlation of Tensile Fracture Surfaces with Eutectic Pool Morphology

Figure 8: Optical micrographs of eutectic pools obtained from the chemistry slug specimens.

B-doped P-doped Si-doped Hf-doped

Figure 9: Optical micrographs of the high temperature tensile test fracture surfaces taken longitudinally.

B-doped P-doped Si-doped Hf-doped

MoldEutectic Pool Volume Fraction Average and

Standard Deviation

Average Max Eutectic Pool Clustering Length

and Std. Dev (μm)

Volume Percent of Voids Near Fracture

Surface and 95% C. I.

B-doped 0.14 ± 0.05 342.5 ± 86.7 8.3 ± 2.5

P-doped 0.14 ± 0.09 395.6 ± 17.3 16.1 ± 6.7

Si-doped 0.04 ± 0.02 89.8 ± 17.3 0.5 ± 1.6

Hf-doped 0.14 ± 0.06 242.5 ± 47.6 8.8 ± 2.1

Table 3: Data of eutectic pool volume fractions away from fracture, volume percent of voids near the fracture, and the average maximum eutectic pool clustering length of the tensile bar specimens. .

Boron pools tended to be thick in both directions and clusteroften. Phosphorus pools are longer and thin and experiencethe heaviest clustering. Silicon pools are large but isolated.Hafnium had pools were largest but were very spread outthroughout the microstructure with the least amount ofcoarse gamma prime. Large and long eutectic pools createsa torturous feeding path. The voids in the high temperaturetensile specimens, caused by tensile stresses during tensiletesting, take on the shape of the eutectic pools and occurbetween dendrite arms. This is where eutectic pools form assolute is partitioned to the interdendritic regions duringsolidification. The Si-doped sample has the fewest voids aswell as the lowest volume fraction of eutectic pools. Undersolidification stresses these areas are the first to separateand provide paths for hot tears to form.

References

Observed Correlations• Boron, P, and Hf-doped molds had a ΔTE-S above 200°C

creating microstructures with large eutectic pool volumesand heavy clustering. By lowering the composition ofelements that lower solidification temperatures, promotesegregation, and increase the eutectic pool clustering, hottearing susceptibility can be decreased.

• The baseline and Si addition showed a ΔTE-S below 200°C.The solidification behavior of the Si addition was similar tothe baseline. The Si-doped molds exhibited microstructureswith isolated eutectic pools and little clustering leading tolow hot tearing susceptibility.

• Clustering of eutectic pools along grain boundaries couldbe pulled apart more easily during solidification to form ahot tear. Phosphorus and Hf-doped molds developed hottears during casting and showed significant eutectic poolvolume fraction and clustering.

• Molds with high eutectic pool clustering formed more voidsduring high temperature tensile testing showing the abilityto pull apart eutectic pools. Phosphorous-doped molds hadthe most voids from the tensile test showing the weakestintergranular constituents which led to the most hot tearsduring casting.