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Politecnico di Torino Porto Institutional Repository [Other] Microstructural, mechanical and fatigue properties of Cobalt alloys Original Citation: Scavino G., Matteis P., Mortarino G.M.M., Firrao D. (2010). Microstructural, mechanical and fatigue properties of Cobalt alloys.. Availability: This version is available at : http://porto.polito.it/2458377/ since: October 2011 Terms of use: This article is made available under terms and conditions applicable to Open Access Policy Article ("Public - All rights reserved"), as described at http://porto.polito.it/terms_and_conditions. html Porto, the institutional repository of the Politecnico di Torino, is provided by the University Library and the IT-Services. The aim is to enable open access to all the world. Please share with us how this access benefits you. Your story matters. (Article begins on next page)

Microstructural, Mechanical and Fatigue Properties of Cobalt Alloys G. Scavino, P. Matteis, G.M.M. Mortarino, D. Firrao Dip. Scienza dei Materiali ed Ingegneria Chimica Politecnico di Torino

Introduction - General goals reduction of fuel consumption and pollutant emission higher efficiency motor development increase of fuel injection pressure in cylinders higher stresses in injection system components inadequacy of steels use of cobalt based alloys (Stellites) for components mechanically stressed at high temperature literature about Co alloys mainly concerned on wear and corrosion resistance at high temperature few data about high temperature fatigue available

Materials & specimens Tensile and fatigue cylindrical (not notched) specimens, 8 mm diameter stellite 6 type alloy produced by casting stellite 6 type alloy produced by powder metallurgy + hipping Mechanical tests hardness and micro-hardness test at R.T. tensile tests at R.T., 250 or 500 C pulsed traction fatigue tests (R 0) up to 2 10 6 cycles at 250 or 500 C Crystallographic and micro-structural tests both on as received material, and after 250 or 500 C treatments X ray diffraction (Co anode) optical and electronic metallography and EDS micro-analysis Fractography Experimental methods

Chemical composition of cast or HIP stellite grade 6. (% wt.) CAST Co C Cr W Ni Si Mn Fe V Nb bal. 1.19 25.54 5.21 1.99 1.56 0.69 0.85 0.028 0.034 HIP Co C Cr W Ni Si Mn Fe V Nb bal. 1.48 27.21 4.78 0.30 1.21 0.21 0.44 0.021 0.002

Cast sample XRD Analyses (Brag-Brentano geometry, Co anode) - Shallow and partially overlapped peaks (e.g.40-65 range) - Possible phases: Co CFC, Co HCP, Co 25 Cr 25 W 8 C 2, Cr 7 C 3, Cr 23 C 6, Cr 3 C 2, Co 3 W 3 C, Co 4 W 2 C, Co 6 W 6 C, W 2 C, Co 3 W, Co 7 W 6 - Probable prevalence of Co CFC in respect to Co HCP - Possible phase evolution on heating at 250 or 500 C

Hipped sample XRD Analyses (Brag-Brentano geometry, Co anode) - Shallow and partially overlapped peaks (e.g.40-65 range) - Possible phases: Co CFC, Co HCP, Co 25 Cr 25 W 8 C 2, Cr 7 C 3, Cr 23 C 6, Cr 3 C 2, Co 3 W 3 C, Co 4 W 2 C, Co 6 W 6 C, W 2 C, Co 3 W, Co 7 W 6 - Probable prevalence of Co CFC in respect to Co HCP - No phase evolution on heating at 250 or 500 C

Cast samples micro-structure Main primary dendrites Inter-dendritic carbides (mainly lamellar form) As received, 456 x 362 μm No microstructural differences due to treatment at 250 and 500 C are noticeable After treatment at 500 C, 456 x 362 μm

Hipped sample microstructure Co rich matrix, dispersed carbides, about 2 µm diameter. Grain size in the range of 5-40 µm with the most part in the range 5-10 µm. Larger grains are richer in Co (EDS analysis).

Cast sample micro-analysis (EDS) Metallic matrix Cr Co W Mo Si 24 71 3.5 0.24 0.65 Cr rich carbides Cr Co W Mo 78 15 6.3 0.43 Co, W rich carbides Cr Co W Mo 21 47 29 2.7 Back-scattered electrons image

Hardness and micro-hardness HV 0.05 HV 0.05 Samples HV 50 Dendritic zones Carbides rich zones Room temperature 370 400-430 530-1100 Heating at 395 390-410 550-1000 Heating at 385 380-400 800-1100 low heat treatment effect on hardness of matrix Cast sample: scattered results on precipitated carbide zone (hardness indent large in respect to dimension of carbides) The hardness tests effected on the transverse section of the HIP samples reveal 660 HV for the 50 g tests and 460 HV for the 50 kg tests. As received cast sample, 92 x 69 μm

Mechanical tests

Mechanical tests Fatigue Fatigue tests: - pulsed traction fatigue R 0 - staircase method up to 2 10 6 cycles, 30 Hz, temperature 250 or 500 C Results: the highest fatigue resistance was observed for HIP samples there is a great difference in the behaviour of cast and hipped samples results obtained through 250 or 500 C tests are similar but the best behaviour has been observed at the lower temperature under the maximum stress the fracture occurred after a greater cycle number for the samples tested at the lower temperature

Mechanical tests Cast tensile test sample (no necking). Hipped tensile test sample (shear lips presence)

Fractography cast sample tensile test fracture at 500 C Mainly inter-dendritic fracture and trans-dendritic quasi-cleavage fracture

Fractography cast sample fatigue test at 250 C Fracture nucleation from a shrinkage defect

Fractography cast sample fatigue test at 500 C Nucleation and propagation fatigue fracture zones detail of stair-step fatigue propagation

Fractography HIP sample tensile test fracture at 500 C The fracture is ductile, nucleated by the presence of an inclusion

Fractography hipped sample fatigue test at 500 C Fracture surface observed by means of Stereo Macro-scope. The fatigue fracture is nucleated by the presence of a defect constituted by an Al- Mg oxide. Nucleation zone (detail) Defect EDS

Fractography hipped sample fatigue test at 500 C Fatigue propagation zone Final fracture zone characterized by ductile morphology

Discussion and conclusions (I/II) Cast samples are constituted by cobalt rich primary dendrites and lamellar inter-dendritic zones (eutectic mixtures) with high carbides content. Dendritic matrix is constituted by a solution of the alloying elements in CFC Co. EDS micro-analyses have evidenced two carbide types: one with high Cr content, the other with high W content. Hipped samples present a Co rich matrix and dispersed carbides, about 2 µm diameter. Grain size is in the range of 5-40 µm with the most part in the range 5-10 µm. XRD analyses have shown shallow and partially overlapped peaks (e.g.40-65 range) with the probable prevalence of Co CFC in respect to Co HCP and the presence of mixed carbides. The cast sample show a phase evolution changing the test temperature, not observed for hipped samples.

Discussion and conclusions (II/II) The best performance both in tensile tests and in fatigue tests was observed for the hipped samples The effect of temperature on tensile and fatigue properties is limited; particularly, the observed fracture mechanisms do not change varying the temperature between 250 and 500 C. In tensile test samples the fracture of cast samples is mainly inter-dendritic and only in some zones the fracture are completed by a quasi cleavage interdendritic fracture. In hipped samples the ductile mode fracture is nucleated by an inclusional defect. In fatigue tests, the crack of cast samples is nucleated by casting defects and propagates on crystallographic planes, in a trans-dendritic way, with a stairstep morphology. The crack of hipped samples is nucleated by an inclusion and the fracture is mainly ductile.

Fractography tensile test fracture at 500 C (II/II) quasi-cleavage

Mechanical tests Tensile tests cast sample: No necking Fatigue tests: - pulsed traction fatigue R 0 - staircase method up to 2 10 6 cycles, 30 Hz, temperature 250 or 500 C - results obtained through 250 or 500 C tests are similar

CAST Co-Alloy pulsed traction fatigue tests (R 0), up to 2 10 6 cycles, at 500 C Strenght Specimens results Results Mpa 1 2 3 4 5 6 7 8 9 10 11 X O 450 X 1 440 430 420 410 X X 2 400 X 1 390 O X O X X 3 2 380 O 1 370 O 1 X: specimen broken before 2 10 6 cycles O: specimen completes 2 10 6 cycles

CAST Co-Alloy pulsed traction fatigue tests (R 0), up to 2 10 6 cycles, at 250 C Strenght Specimens results Results Mpa 1 2 3 4 5 6 7 8 9 10 11 X O 450 X 1 440 430 X X 2 420 410 X O X 2 1 400 X 1 390 O X O 1 2 380 O 1 X: specimen broken before 2 10 6 cycles O: specimen completes 2 10 6 cycles

HIP Co-alloy pulsed traction fatigue tests (R 0), up to 2 10 6 cycles, at 500 C Strenght Specimens results Results Mpa 1 2 3 4 5 6 7 8 9 10 11 X O 740 X 1 720 700 X 1 680 X O 1 1 660 O O 2 X: specimen broken before 2 10 6 cycles O: specimen completes 2 10 6 cycles