Effects of Heat Treatment on Microstructure and Wear Resistance of Superalloys

Kuan Jiang

M. A. Sci. Candidate

Ottawa- Carleton Institute for Mechanical Engineering Ottawa, Canada Fall 2012

Outline
Introduction

Experimental procedures
Results and discussion
Microstructure development

Hardness, wear volume loss

Worn surface analysis

Conclusion and future work Acknowledgement

Introduction
Wear Failure of Materials
Wear failure occurred frequently on mechanical components operating in high temperature, wear, corrosion, oxidation environment.
The total economical loss caused by wear failure is as much as 7% of Gross National Product in many industrialized nations every year. Wear failures of some mechanical components served in severe environment can be catastrophic.

Introduction
Materials for High Temperature Environment
Superalloys: Primary design for high temperature(540C) applications. Typically examples: Stellite alloys, Tribaloy alloys. Stainless steels: Strong resistance for corrosion and high temperature attack.

Research Background
Coating Techniques
Chemical vapor deposition (CVD), Physical vapor deposition (PVD), Slurry coating, etc.

Slurry Coating Process

Mixing

Spraying

Drying

Sintering

Research Objectives
Investigate the influence of sintering heat treatment on the microstructure and wear resistance of superalloys. Explore wear mechanism of superalloys at room temperature and elevated temperatures (250C, 450C).

Alloy Selection And Chemical Compositions

Two cobalt-based superalloys (T-400C, Stellite 22) at cast state were selected.

Alloy Type

Chemical composition (wt%, Co in balance) of the selected superalloys.

Process Co Cr Mo C Fe Ni Si

Mn

T-400C

Sand Cast

Bal

14

26

2.6

Stellite22

Sand Cast

Bal

27

11

0.25

2.75

Heat treatment Cycle

Micro Hardness Test

Specimen with 6.5mm in diameter and 1.5-2mm in thickness Well polished; methanol cleaned; air dried Exposure temperatures: 25C, 250C, 450C, 600C Indentation area: each individual phases and overall microstructure. Hot-Stage Assembly

Pin-on-disc Wear Test

Pin: ball (94% WC+6% Co) Disc: sample disk Exposure temperatures: 25C, 250C, 450C

Wear tracks on a worn specimen surface.

Pin Disk Sample

Disc

Microstructure Development
T-400C
Intermetallic Laves phase (Co3Mo2Si or CoMoSi) boundary became finer Precipitation of some white phases As-cast T-400C (1.00kx)
Co solid solution Newly precipitated Laves phase

Heat-treated T-400C (1.00kx)

Primary intermetallic Laves phase

EDS results of T-400C

Primary Laves phase
Si, Mo decreased
Si K

As-cast T-400C Laves phase

Element Weight% 3.56 12.14 1.05 46.24 37.02 100.00 Atomic% 8.21 15.07 1.21 50.61 24.90 100.00

Heat-treated T-400C Laves phase

Element Si K Cr K Fe K Co K Mo L Total Weight% 3.43 12.66 1.03 47.30 35.59 100.00 Atomic% 7.86 15.64 1.18 51.50 23.82 100.00

Solid solution
Si, Mo decreased

Cr K Fe K Co K

Laves phase

Solid solution

Mo L Total

As-cast T-400C Solid solution Element Si K Cr K Fe K Weight% 2.21 16.16 1.42 Atomic% 4.86 19.16 1.56

Heat-treated T-400C Solid solution Element Si K Cr K Fe K Weight% 1.88 17.10 1.53 Atomic% 4.10 20.10 1.67

Co K
Mo L Total

56.86
23.35 100.00

59.42
15.00 100.00

Co K
Mo L Total

58.84
20.65 100.00

60.97
13.15 100.00

Microstructure Development
Stellite 22
A finer eutectic boundary was found in heat-treated alloy White area and black area became more distinct in multi-phase eutectic
As-cast Stellite 22 (2.00kx)
Primary dendritic Co solid solution

Heat-treated Stellite 22 (2.00kx)

Cr7C3 carbide

Co3Mo and Co7Mo6

Secondary multiphase eutectic

Primary sold solution

Results of Hardness Test

Results of Wear Test

Variation of wear volume with temperature in T-400C and Stellite 22 has a similar trend. Each alloy exhibited different wear behavior at room temperature and at elevated temperature Wear volume loss of materials at different temperatures

Worn Surface Analysis

T-400C
Plowing of the solid solution accompanied with fracture of the Laves phase Oxidation had occurred in the specimen surfaces Worn surface of T-400C tested at room temperature As-cast Heat-treated
Cavities

Oxide residuals

Worn Surface Analysis

T-400C
Worn surface is very smooth, and also do not show any oxides. Loose/brittle silicates and small amount of hard/strong Cr-oxides were vulnerable under mechanical attack. Worn surface of T-400C tested at 250C As-cast Heat-treated

Worn Surface Analysis

T-400C
Severe oxidation had occurred Glaze effects Worn surface of T-400C tested at 450C As-cast Heat-treated
Oxide residuals

Worn Surface Analysis

Stellite 22
Some areas are smooth where the material was scraped away by the pin under normal loading and some area were deformed with large plastic flow. Worn surface of heat-treated Stellite 22 is more smooth than that of as-cast one. Worn surface of Stellite 22 tested at room temperature As-cast Heat-treated

Plastic flow

Worn Surface Analysis

Stellite 22
Less plastic deformation is found in specimen tested at 250C Particle spallation had occurred on specimen surface. Worn surface of Stellite 22 tested at 250C As-cast Heat-treated

Particle spallation

Worn Surface Analysis

Stellite 22
Surface oxidation is observed obviously in the as-cast specimen surface Oxide films decreased the frictional coefficient in as-cast specimen.

Worn surface of Stellite 22 tested at 450C As-cast Heat-treated

Oxide films

Conclusions
Annealing heat treatment promoted diffusion of alloying elements such as Si and Mo, thus contributed to the secondary precipitation of hard phases in T-400C and Stellite 22. The heat treatment increased the hardness and wear resistance of T400C . As for Stellite 22, the hardness is increased while the tribological properties is degraded. T-400C and Stellite exhibited least wear resistance at elevated temperature at 250C which may be attributed to the softening of material and formation of easily removed oxides.

Future work
More superalloys will also be studied for the influence of heat treatment. Superalloys will be applied in a series of other heat treatment cycles to determine the effects of various heat treatment parameters such as heating temperature, holding time, cooling speed and cooling medium on these high temperature alloys. The heat treatment effects on superalloys with various other fabrication state (e.g. HIP) will be investigated.

The effects of heat treatment on the corrosion behavior of superalloys will be studied.

Acknowledgement
I would like to thank people who made this work possible:
Prof. Ming Liang, Dept. of Mechanical and Aerospace Engineering, University of Ottawa Prof. Rong Liu, Dept. of Mechanical and Aerospace Engineering, Carleton University Dr. Kuiying Chen, Institute for Aerospace Research, NRC Kennametal Stellite Inc.

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Vickers Hardness Results

As-cast T-400C
Average hardness values (HV) for as-cast T-400C
Temperature Primary Laves phase 25C 250C 450C 600C 1068 (2.31%) 1034 (3.46%) 909 (2.29%) 878 (2.41%) 380 (3.51%) 342 (2.53%) 329 (2.36%) 324 (2.54%) Solid solution Overall microstructure 574 (4.51%) 529 (3.04%) 494 (3.87%) 477 (4.68%)

Vickers Hardness Results

Heat-treated T-400C
Average hardness values (HV) for heat-treated T-400C
Temperature Primary Laves phase 25C 250C 450C 600C 1048 (2.49%) 980 (3.69%) 908 (2.46%) 889 (3.39%) 485 (1.37%) 445 (3.47%) 441 (2.38%) 429 (2.43%) Solid solution Overall microstructure 587 (2.58%) 546 (4.38%) 505 (3.48%) 495 (3.59%)

Vickers Hardness Results

As-cast Stellite 22
Average hardness values (HV) for as-cast Stellite 22.
Temperature Solid solution Eutectic mixture Overall microstructure 25C 250C 450C 600C 314 (2.56%) 255 (3.57%) 242 (3.63%) 246 (2.95%) 501 (1.65%) 393 (2.54%) 328 (2.18%) 310 (2.38%) 420 (3.59%) 342 (2.71%) 326 (3.06%) 305 (2.38%)

Vickers Hardness Results

Heat-treated Stellite 22
Average hardness values (HV) for heat-treated Stellite 22.
Temperature Solid solution Eutectic mixture Overall microstructure 25C 250C 450C 600C 307 (2.47%) 271 (3.42%) 241 (3.69%) 211 (2.34%) 646 (3.54%) 542 (3.38%) 418 (2.44%) 360 (3.36%) 433 (2.75%) 375 (3.49%) 338 (2.53%) 311 (3.45%)