SLIDE 1 FATIGUE MECHANISMS IN P/M COMPONENTS
Worcester Polytechnic Institute April 28-29, 2004
Diana Lados & Diran Apelian
Morris Boorky Powder Metallurgy Research Center
SLIDE 2 OUTLINE
I. Impact of Porosity on Fatigue and Fatigue Crack Growth Behavior of P/M Components (examples from the literature)
- Relevance of open/closed porosity
- Open/closed porosity measurement techniques
II. WPI project … Objectives and Experimental Plan
SLIDE 3 BACKGROUND
Factors controlling fatigue behavior …
1. Porosity/density:
- Amount (% Porosity)
- Type (Open/Closed)
- Morphology (size/shape - due to initial powder
morphology and sintering conditions)
- Distribution (initial powder size)
2. Microstructural phases:
- Amount (% Phase)
- Type (Martensite, Bainite, Pearlite, Ferrite,
+ Cementite, Ni-rich areas, etc.)
SLIDE 4 BACKGROUND
Fatigue life vs. density/porosity …
Fatigue limit Porosity %
for both:
P/M iron P/M steels
in:
as-sintered heat treated (quench and tempered)
SLIDE 5 BACKGROUND
Fatigue life vs. density/porosity … sintered P/M iron
Water atomized Reduced sponge 4 hrs @ 2050°F 30 min @ 2280°F Sintering treatment affects fatigue life at intermediate porosity ranges (water atomized iron powder, single or double pressed, and sintered @ 2050°F (30 min) and 2280°F (4 hrs)) Life (samples from reduced sponge powder) > Life (samples from water atomized powder) (single, double, triple sequence sintering @ 2050°F or 2200°F)
SLIDE 6 BACKGROUND
Fatigue life vs. density/porosity … sintered P/M steels
Large Small Base Bimodal 20 min @ 2050°F 30 min @ 2340°F
ABC (atomized) MH (sponge) Fe-1.5Cu-1.75Ni-0.5Mo-0.5C (SE) Fe-1.5Cu-4Ni-0.5Mo-0.5C (AE)
and
Fe-2Cu-0.8C (30 min @ 2050°F)
SLIDE 7 BACKGROUND
Fatigue life vs. density/porosity … sintered P/M steels
Fe-2Cu-2.5Ni (60 min @ 2280°F) Fe-1.5Cu-0.6C (30 min @ 2050°F)
SLIDE 8 BACKGROUND
Fatigue life vs. density/porosity … Q&T - P/M steels
S Q&T Fe-1.5Cu-1.75Ni-0.5Mo-0.6C Fe-1.5Cu-1.75Ni-0.5Mo-0.5C (sponge) Fe-1.5Cu-1.75Ni-0.5Mo-0.5C (atomized) Fe-1.5Cu-4Ni-0.5Mo-0.5C (atomized)
SLIDE 9 BACKGROUND
∆Kth vs. density/porosity … sintered P/M iron and steels
Fe (atomized) S Q&T Fe-1.5Cu-1.75Ni-0.5Mo-0.5C (sponge) Fe-1.5Cu-1.75Ni-0.5Mo-0.5C (atomized) Fe-1.5Cu-4Ni-0.5Mo-0.5C (atomized) Fe-1.5Cu-1.75Ni-0.5Mo-0.6C Fe-1.75Ni-0.5Mo-0.5C (atomized)
SLIDE 10 BACKGROUND
FCGR and ∆KFT vs. density/porosity …
Fe-2Cu-2.5Ni (60 min @ 2280°F) Fe-1.5Cu-0.6C (30 min @ 2050°F)
SLIDE 11 BACKGROUND
∆KFT vs. density/porosity …
Fe-Cu-Ni-Mo-C alloys as-sintered Fe-0.8Cu-1.8Ni-0.5Mo-0.2Mn-0.4C
SLIDE 12 BACKGROUND
∆KFT vs. density/porosity …
FL 4605 FL 4605
heat treated as-sintered
FL = pre-alloyed FLN = pre-alloyed + elemental Ni blend FN = elemental blended
SLIDE 13
BACKGROUND
∆KFT vs. density/porosity …
Homogeneous Inhomogeneous
Fe-1.75Ni-0.5Mo-0.5C as-sintered
SLIDE 14 BACKGROUND
Total porosity vs. Open/Closed porosity …
Open porosity Isolated porosity Closed porosity
Total Porosity: Open + Closed + Isolated
Open porosity: continuous pore channels intersecting the surface of the specimen (and each other) Closed porosity: closed gaps between powder particles resulting from compaction and/or sintering (not accessible to the surface BUT can be connected to each other !!) Isolated porosity: pores present in the initial powder particles (not affected by compaction and sintering)
SLIDE 15 BACKGROUND
Open porosity … the controlling parameter ? P/M iron
Tension- Plane bending
- Axial testing – volume properties
- Bending – surface properties
compression
SLIDE 16
BACKGROUND
Open porosity … the controlling parameter ? P/M iron
Region I: closed porosity (∆Kth ≈ ct.) Region II: ∆Kth porosity Region III: open porosity (∆Kth ≈ ct. and low)
Fe-1.75Ni-0.5Mo-0.5C (no increase in threshold above ~7.5 g/cm3)
SLIDE 17
BACKGROUND
Open porosity level … function of density only ? Literature: Open porosity is assumed to gradually increase with density
Is this correct ? Or the “path to density” prevails over the “density” itself …
SLIDE 18 BACKGROUND
Open porosity measurement techniques …
Open porosity penetrated by He Isolated porosity Closed porosity Open porosity penetrated by oil Open porosity unresolved by penetrating oil
Oil-impregnation
(ASTM B328)
Gas-impregnation
More accurate measurements of
- pen porosity due to increased
pore penetration ability of gases compared to oils - RECOMMENDED Calculate the interconnected porosity from the volume of
- il that has impregnated the
specimen
SLIDE 19
BACKGROUND
Gas-impregnation measurement techniques … pycnometry Gas displacement pycnometer: a sample of known weight (a solid, a powder, or a porous material) is placed in one of the chambers and the change in pressure needed to balance the two chambers is used to calculate the volume of the sample (P1V1=P2V2) pore free density pycnometric density bulk density
SLIDE 20 BACKGROUND
Calculation of open/closed porosity using He pycnometry …
free pore bulk total
1 V
−
ρ ρ − = % Total porosity = 100 x Vtotal
c pycnometri bulk
1 V ρ ρ − =
% Open porosity = 100 x Vopen Vclosed = Vtotal – Vopen % Closed porosity = 100 x Vclosed
* The amount of isolated porosity was assumed insignificantly small
SLIDE 21 BACKGROUND
Open/closed porosity results … P/M iron
5 10 15 20 25 5.50 6.00 6.50 7.00 7.50 8.00 Density (g/cm3) Porosity (%)
Danninger et al. [18] Ledoux and Prioul [1] Lados and Apelian (pycnometry) Lados and Apelian (oil)
Total porosity Open porosity Closed porosity
SLIDE 22 BACKGROUND
Open/closed porosity results using He pycnometry … … P/M steels in sintered conditions
Sintered conditions 0.25 0.5 0.75 1 1.25 6.8 6.9 7 7.1 7.2 7.3 7.4 Density (g/cm3) Closed porosity (%)
A4601 A4001
A4601 A4001
SLIDE 23 BACKGROUND
Quenched and tempered conditions 0.25 0.5 0.75 1 1.25 6.8 6.9 7 7.1 7.2 7.3 7.4 Density (g/cm3) Closed porosity (%)
A4601 A4001
Open/closed porosity results using He pycnometry … … P/M steels in quenched and tempered conditions A4601 after oil quench A4001 after gas quench
SLIDE 24 BACKGROUND
Open/closed porosity results using He pycnometry … … P/M steels in high temperature/long time sintering
Sintered conditions 1 2 3 4 5 6 7 6.8 6.9 7 7.1 7.2 7.3 7.4 Density (g/cm3) Closed porosity (%)
A4601 @ 2350°F for 6 hrs A4601 @ 2050°F for 30 min
(pycnometry)
pycnometry
SLIDE 25 BACKGROUND
Sources of errors in evaluating open porosity …
1. Open porosity measurement technique:
- Higher closed porosity level is measured using oil-
impregnation (the segments of open porosity channels that are not reached by oil are incorrectly assumed to be closed porosity);
- It is more accurate at high level of closed porosity;
- Pycnometric measurements are more accurate;
2. Correlating open/closed porosity to density alone:
- Simple correlations open porosity level – density are
incorrect;
- The path followed to reach the density is critical for
correct interpretations of open/closed porosity;
- No closed porosity is achieved through compaction and
regular sintering T and t.
SLIDE 26 OBJECTIVES
- Study the effects of density/porosity on the fatigue
initiation and propagation in P/M components;
- Investigate the porosity/microstructure interactions;
- Understand the effects of different microstructural
phases on dynamic properties – mechanisms;
- Create guidelines for fatigue design corroborated with
the fundamental understanding of the alloys behavior;
- Optimize the material characteristics and processing
parameters for enhanced fatigue response.
SLIDE 27 EXPERIMENTAL APPROACH
Materials selection … Pre-alloyed (QMP ATOMET 4601 Ni-Mo pre-alloyed powder) Admixed (QMP ATOMET 4001 Mo pre-alloyed powder admixed with Ni) 0.6 0.15-0.18 0.50-0.55 1.75-1.8
[%] Sintered C Mn Mo Ni Chemical composition
Graphite Ni Graphite
Molding grades particles (70-85 µm)
SLIDE 28
EXPERIMENTAL APPROACH
Phases … Phase I (a): Phase I (a): Mechanistic understanding of the effects of pore amount on fatigue behavior;
Pore/Microstructure (matrix) interactions;
Phase I (b): Phase I (b): Microstructure effects on fatigue response;
Microstructure 1 vs. Microstructure 2;
Phase II: Phase II: Is fatigue resistance a state function ???
Effects of pore size/shape/type on fatigue.
SLIDE 29
EXPERIMENTAL APPROACH
Phase I … Two microstructural considerations Low High density density Pore Pore/Matrix Matrix control control control
A. ? ? B.
Cooling Fatigue rate 2 behavior 2 Cooling Fatigue rate 1 behavior 1 Microstructure 1 Microstructure 2
SLIDE 30 EXPERIMENTAL APPROACH
Phase I … Density levels selection Micro- structure Set 3 7.8+ Set 2 7.2-7.3 Set 1 ~6.8 Density [g/cm3]
- Produce samples of our composition in both pre-alloyed
and admixed conditions;
- Adjust compaction (conventional press, warm compaction,
powder forging, etc.) to get the full range of densities:
SLIDE 31 EXPERIMENTAL APPROACH
- Compaction:
- low densities (Set 1): normal compaction;
↔ intermediate densities (Set 2): controlled temperature compaction (warm compaction 145°F );
- high densities (Set 3): powder forging.
- Sintering:
temperature:T=2050°F ;
T and t invariant for phase I. Phase I … Compaction +Sintering
SLIDE 32 EXPERIMENTAL APPROACH
Phase I … Heat treatment
- Post sintering heat treatment:
austenitize @ 1700°F for 30 min (similar austenitic grains) quench to 2 microstructures (for both pre-alloyed and admixed): temper @ 400°F for 1 hr (similar matrix micro-hardness) Martensite + R.A. + (5%Ni reach areas) 35%Martensite + 60%Pearlite + R.A. + (~5%Ni reach areas)
SLIDE 33
EXPERIMENTAL APPROACH
Phase I … Heat treatment … Microstructures A4001 Martensite + R.A. + (5%Ni reach areas) 35%Martensite + 60%Pearlite + R.A. + (~5%Ni reach areas)
SLIDE 34
EXPERIMENTAL APPROACH
Phase I … Heat treatment … Microstructures A4601 Martensite + R.A. 35%Martensite + 60%Pearlite + R.A.
SLIDE 35 EXPERIMENTAL APPROACH
Fatigue testing … Specimens and equipment Dog-bone specimens for pull-pull/push-pull CT specimens for FCGR
[Courtesy of Westmoreland]
σmin σmax σmean σa
SLIDE 36 EXPERIMENTAL APPROACH
Fatigue testing …
conducted by the WPI team in collaboration with FTA;
- 1 sample for each of the 12
conditions (prealloyed+admixed, 3 density levels, 2 microstructures)
- The tests will be done at an
- utside testing facility in parallel
with the fatigue crack growth work;
- 3 failed samples at 4 life levels
for each of the 12 conditions):
* 103-104 * 104-105 * 105-106 * 106-107
tests (E647)
- 1. Pull-pull / Pull-push tests
(E466)
SLIDE 37 EXPERIMENTAL APPROACH
Phase II … Is Fatigue Limit a State Function ?
One density level is selected (~7.25 g/cm3, same as Set 2 in Phase I) and 4 ways of achieving are investigated in parallel (we choose the most attractive alloy from fatigue point of view [of the 12 combinations] and concentrate our attention on how pore size/shape will influence its behavior):
1. Compaction - coarser powder, 100-105 µm; 2. Normal compaction to *.* g/cm3, followed by a different temperature/time sinter (same closed porosity as Route 3); 3. Double press/Double sinter (same closed porosity as 2); 4. Surface densification (7.0 g/cm3 - core and 7.25 g/cm3 -
Pore size/shape/type effects on the fatigue behavior
SLIDE 38 EXPERIMENTAL APPROACH
Phase II … Various pore sizes/shapes
Pore morphology (size/shape)
densified (core 7.0 g/cm3 and
7.25 g/cm3)
3.
DP/DS
2.
Press to *.* g/cm3 and different sinter to 7.25 g/cm3
particles
100-105 µm
Molding grades particles
70-85 µm
Case study
7.0 / 7.25
- Fatigue crack growth work will be conducted for one
selected microstructure and one density level
SLIDE 39 EXPERIMENTAL APPROACH
Other experimental considerations …
- Inclusion level is low shed light on pore and
microstructure effects;
- Low residual stress levels are critical to understand the
true behavior of the materials and have a fair comparison basis:
- stress relief is done during tempering
- additional stress relieving may be needed after machining.
SLIDE 40 FUTURE WORK …
- Finish the open/closed porosity study;
- Do a parallel study high temperature/long time sintering vs.
DP/DS to determine the processing parameters allowing the same amount of closed porosity;
- Analyze microstructural results and microhardness for the two heat
treatments on both the homogeneous and non-homogeneous materials for each of the microstructures;
- Perform static tensile tests to get YS, Young’s modulus, UTS for all
cases;
- Check the residual stress level and decide if an additional stress
relieving is needed after the post-sintering heat treatment;
- Prepare samples for the life study (200 dog-bone samples) and the
fatigue crack growth work (16 compact tension specimens);
- Machine all the samples;
- Start fatigue work.