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Early stage development of precipitation strengthened CCAs in the AlCrFeNiTi

system for high temperature structural applications

Silas Wolff-Goodrich and Christian Liebscher

In Collaboration With: Dr. Konda G. Pradeepand Marshal Amalraj

15.02.2018

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Outline

2

Motivation and application of interest

CCA development methodology

Material system of interest

Preliminary work

Summary

Work plan

Next steps …

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Motivation – High Temperature Structural Materials

Steam turbines are used to generate ~80% world’s energy

3

http://www.mechscience.com/steam-turbine-introduction-and-principle-operations/

Novel high temperature materials needed!

https://commons.wikimedia.org/wiki/File:ASHBY_D.png

Need for more affordable materials in this range

Where do we begin the search for new materials that fill the gaps between conventional alloy classes??

Alloys need:

• Low-cost & low-density: 6-7 g/cm3

• Creep resistance up to 900ºC• Maximized solid solution

strengthening & precipitation hardening

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Compositionally Complex Alloy Development Methodology

4

• Method most efficient for application specific search.

• “Spider plot” used for screening.

• Failure in one property = failure of alloy overall.

Miracle, Daniel, et al. "New strategies and tests to accelerate discovery and development of multi-principal element structural alloys." Scripta Materialia 127 (2017): 195-200.

“No longer safe along corners and edges of ternary phase diagrams, the materials community is now thrust into an uncharted, hyper-dimensional territory that is difficult to conceive, difficult to visualize, and difficult to explore systematically.” [2]

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Miracle, D. B., and O. N. Senkov. "A critical review of high entropy alloys and related concepts." Acta Materialia 122 (2017): 448-511.

Stage 0 Stage 1 Stage 2

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Alloy System of Interest - AlCrFeNiTi

5

Song, Gian, et al. "Ferritic alloys with extreme creep resistance via coherent hierarchical precipitates." Scientific reports 5 (2015).

0 at.% Ti

2 at.% Ti

4 at.% Ti

• Coherent B2-NiAl precipitates in BCC matrix for AlCrFeNi

• Addition of Ti changes precipitate morphology and structure to combined L21-Ni2TiAl and B2-NiAl

• Creep resistance of hierarchical B2/L21 structure greatly improved

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Arc Melting

Vacuum Induction Casting

Directional Solidification

In collaboration with Pradeep& Marshal at RWTH Aachen

• XRD• SEM• (S)TEM• 3D APT

Work Flow

6

Bulk Synthesis

Bulk Mechanical Testing

Microstructural Characterization

Rapid Screening

High-throughput characterization:• SEM/EDS/XRD• Nano-hardness

Magnetron Sputtering

DSC and Heat Treatment

• Compression• Tension• Nano- and micro-

hardness• Creep

Objectives• BCC-CCAs with tailored B2/L21-precipitates

• Low-cost, low-density alloys: 6-7 g/cm3

• Creep resistance up to 900ºC• Maximized solid solution strengthening &

precipitation hardening

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Arc Melted Compositions

7

Planned Rating Categories:• Solid solution structure• Precipitation phases• Density• Castability• Cost• Hardness• Ductility

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B1 (Al20Cr20Fe20Ni20Ti20)

• DSC results indicate that the first major thermal effect occurs around 1150 °C. Homogenization will be conducted at 1200 °C and annealing at 900 °C.

• As-cast material:

8

L21 α-FeC14

10 μm

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B1 (Al20Cr20Fe20Ni20Ti20)

• DSC results indicate that the first major thermal effect occurs around 1150 °C. Homogenization will be conducted at 1200 °C and annealing at 900 °C.

• As-cast material:

9

α-FeC14 L21

1 μm

C14

L21

α-Fe

Ti-rich ppt

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B2 (Al25Cr10Fe35Ni25Ti5)

• DSC results indicate that the first major thermal effect occurs around 1150 °C. Homogenization will be conducted at 1200 °C and annealing at 900 °C.

• As-cast material:

10

L21 α-Fe

10 μm

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B2 (Al25Cr10Fe35Ni25Ti5)

• DSC results indicate that the first major thermal effect occurs around 1150 °C. Homogenization will be conducted at 1200 °C and annealing at 900 °C.

• As-cast material:

11

α-FeL21

1 μm

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B3 (Al35Cr10Fe10Ni10Ti35)

• As-cast material:

12

Single Hexagonal

Phase detected

10 μm

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Results Summary

13

10 μm

1 μm

1 μm

B1

B2

B3

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Next Steps …

• Priorities for the next steps in the project include:

– Obtain thin film samples from collaborators in Aachen

– Standardize SEM and XRD measurement and analysis procedures

– Refine alloy rating scheme

– Characterize heat treated samples and refine heat treatment

– Begin mechanical property screening

14

Thanks for your

attention!

Questions??

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Sources

[1] Miracle, Daniel, et al. "New strategies and tests to accelerate discovery and development of multi-principal element structural alloys." Scripta Materialia127 (2017): 195-200.

[2] Miracle, D. B., and O. N. Senkov. "A critical review of high entropy alloys and related concepts." Acta Materialia 122 (2017): 448-511.

[3] Vo, Nhon Q., et al. "Creep properties and microstructure of a precipitation-strengthened ferritic Fe–Al–Ni–Cr alloy." Acta Materialia 71 (2014): 89-99.

[4] C.H. Liebscher, V.R. Radmilović, U. Dahmen, N.Q. Vo, D.C. Dunand, M. Asta, G. Ghosh, Acta Materialia, 92 (2015) 220-232.

[5] Song, Gian, et al. "Ferritic alloys with extreme creep resistance via coherent hierarchical precipitates." Scientific reports 5 (2015).

16

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B1 (Al20Cr20Fe20Ni20Ti20)

• DSC results indicate that the first major thermal effect occurs around 1150 °C. Homogenization will be conducted at 1200 °C and annealing at 900 °C.

17

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Early Results – B2 (Al25Cr10Fe35Ni25Ti5)

• For Comparison with Equimolar alloy, homogenization will be conducted at 1200 °C and annealing at 900 °C.

18

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

HEA and CCA Definitions and Differences

19

EquiatomicHEA/CCA

Non-equiatomicHEA/CCA

B

A

C

Conventional Alloys

HEA

5 or more elements5 at.% ≤ Χi ≤ 35 at.%

Single Solid Solution Phase

CCA

2+ Phases which may includeHE solid solution

HEA Branch

Aims at understanding structure and properties resulting from

high entropy effect

CCA Branch

Aims to identify and tailor chemistry and microstructural features for optimized mechanical properties in promising alloy systems

“High entropy alloys (HEAs) and … [compositionally complex] alloys (CCAs) open alloy development to a vast richness of complexity.” [1]

Miracle, Daniel, et al. "New strategies and tests to accelerate discovery and development of multi-principal element structural alloys." Scripta Materialia 127 (2017): 195-200.

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

20

Bulk Synthesis

Microstructural Characterization

Bulk Mechanical testing

Rapid Screening

High-throughput characterization:• SEM/EDS,EBSD• XRD• Nano-hardness

Thin Film Magnetron Sputtering

In collaboration with Pradeep& Marshal at RWTH Aachen

Composition selection

Marshal, A., et al. "Combinatorial synthesis of high entropy alloys: Introduction of a novel, single phase, body-centered-cubic FeMnCoCrAl solid solution." Journal of Alloys and Compounds 691 (2017): 683-689.

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

21

Rapid Screening

High-throughput characterization:• SEM/EDS,EBSD• XRD• Nano-hardness

In collaboration with Pradeep& Marshal at RWTH Aachen

Thin Film Magnetron Sputtering

Composition selection

Marshal, A., et al. "Combinatorial synthesis of high entropy alloys: Introduction of a novel, single phase, body-centered-cubic FeMnCoCrAl solid solution." Journal of Alloys and Compounds 691 (2017): 683-689.

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

22

Bulk SynthesisRapid Screening

Combinatorial Vacuum Induction Casting

Arc Melting• Use high throughput characterization to compare with thin films• Far from equilibrium solidification

Vacuum Induction Casting• Produces enough material for bulk mechanical testing• Can produce several compositions in single cast

Directional Solidification• For testing single crystal properties of most promising alloys

Ma, Duancheng, et al. "Phase stability of non-equiatomic CoCrFeMnNihigh entropy alloys." Acta Materialia 98 (2015): 288-296.

Bulk material to be combined with DSC results to select heat treatment schedules

Microstructural characterization will be used to direct alloy selection

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

23

Bulk Synthesis

Microstructural Characterization

Rapid Screening

• XRD• SEM/EDS• (S)TEM• 3D APT

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

24

Bulk Synthesis

Microstructural Characterization

Bulk Mechanical testing

Rapid Screening

Silas Wolff-Goodrich s.wolffgoodrich@mpie.de

Work Flow

25

Bulk Synthesis

Bulk Mechanical Testing

Microstructural Characterization

Rapid Screening

High-throughput characterization:• SEM/EDS/XRD• Nano-hardness

Magnetron Sputtering

Arc Melting

Vacuum Induction Casting

Directional Solidification

In collaboration with Aachen

Pradeep & Marshal

DSC and Heat Treatment

• Compression• Tension• Nano- and micro-

hardness• Creep

Objectives• BCC-CCAs with tailored B2/L21-precipitates

• Low-cost, low-density alloys: 6-7 g/cm3

• Creep resistance up to 900ºC• Maximized solid solution strengthening &

precipitation hardening

• XRD• SEM• (S)TEM• 3D APT

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