evirgen 1 , i. karaman 1 , r. santamarta 2 , j. pons 2

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TAMU-UIB collaboration: TAMU-UIB collaboration: characterization of Ni-Ti-Zr characterization of Ni-Ti-Zr and Ni-Ti-Hf high temperature and Ni-Ti-Hf high temperature shape memory alloys shape memory alloys A. Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2 1. Dept. of Mechanical Eng., Texas A&M University, TX, USA 2. Dept. of Physics, Univ. Balearic Islands, Palma de Mallorca, Spain

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TAMU-UIB collaboration: characterization of Ni-Ti-Zr and Ni-Ti-Hf high temperature shape memory alloys. Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2 1. Dept. of Mechanical Eng., Texas A&M University, TX, USA 2. Dept. of Physics, Univ. Balearic Islands, Palma de Mallorca, Spain. - PowerPoint PPT Presentation

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Page 1: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

TAMU-UIB collaboration: TAMU-UIB collaboration:

characterization of Ni-Ti-Zr and Ni-Ti-Hf characterization of Ni-Ti-Zr and Ni-Ti-Hf

high temperature shape memory alloyshigh temperature shape memory alloys

TAMU-UIB collaboration: TAMU-UIB collaboration:

characterization of Ni-Ti-Zr and Ni-Ti-Hf characterization of Ni-Ti-Zr and Ni-Ti-Hf

high temperature shape memory alloyshigh temperature shape memory alloys

A. Evirgen1, I. Karaman1, R. Santamarta2, J. Pons2

1. Dept. of Mechanical Eng., Texas A&M University, TX, USA

2. Dept. of Physics, Univ. Balearic Islands, Palma de Mallorca, Spain

Page 2: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011

PhD Student Exchange Activity: TAMU – UIB

Summer research stay of ALPER EVIRGEN (I. Karaman’s PhD

student) in UIB. July 2011 Financed by IIMEC

Research topic:

Study of (Ni-rich) Ni-Ti-Zr and Ni-Ti-Hf HTSMAs

Page 3: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011

PhD Student Exchange Activity: TAMU – UIB

Summer research stay of ALPER EVIRGEN (I. Karaman’s PhD

student) in UIB. July 2011 Financed by IIMEC

Research topic:

Study of (Ni-rich) Ni-Ti-Zr and Ni-Ti-Hf HTSMAs

NiTi: TM ~ 80ºC Increase of Ni content → TM drops

Substitution of Ti by Hf or Zr raises TM (Ti+Hf/Zr)-rich ternary alloys

Recently, study of Ni-rich ternary alloys

High industrial interest (automotive, aerospace, …)

Page 4: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011Activity in the framework of IIMEC in 2011

Page 5: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

MaterialsMaterialsMaterialsMaterials

Materials: Selected in TAMU

Ni50.3Ti34.7Zr15 15Zr (at%)

Ni50.3Ti29.7Zr20 20Zr

Ni50.3Ti34.7Hf15 15Hf

Hot extruded (900ºC)

Solution Heat Treatment: 900oC, 1h + WQ (SHT)

Page 6: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Collaboration planCollaboration planCollaboration planCollaboration plan

“Macroscopic” characterization of

functional properties

DSC

Thermal cycling under stress

Thermal treatments to

improve functional properties

Alper’s PhD

Microstructural characterization

TEM, HRTEM

EDX

Most of observations

performed during Alper’s stay

Afterwards: Analysis of results

Page 7: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

General ResultsGeneral ResultsGeneral ResultsGeneral Results

VERY FRUITFUL ACTIVITY:

Education:

Intense immersion in practical TEM/HRTEM work

(preparation of samples and observations)

Personal life:

Stay in a country with different culture

Collaboration:

Strong impulse to TAMU-UIB collaboration

Scientific:

Good results suitable for several publications

Page 8: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

As extruded and Solution Heat Treated state

Low TM temperatures and poor reproducibility

Thermal treatments to improve the alloy

performance

20Zr

15Hf

Page 9: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

20Zr DSC results

Page 10: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf DSC results

Page 11: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

20Zr Furnace cooling from 700ºC to 100ºC in 48h

Page 12: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf SHAPE MEMORY EFFECT

10h at 550ºC

~ 2.5%

Page 13: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

Microstructural observations in aged samples

Precipitation of a new phase

Ni-rich NiTi Ni4Ti3 or Ni3Ti Not in ternary alloys

Page 14: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

15Zr 200h at 500ºC Austenite at RT

Lenticular precipitates in austenitic matrix. ~ 20 nm

Scientific ResultsScientific ResultsScientific ResultsScientific Results

TEM HRTEM

Page 15: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

The precipitates show an enhanced contrast every three 011 planes and extra spots in the diffraction patterns. They are fully coherent with austenitic matrix.

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Zr 200h at 500ºC Austenite at RT

Page 16: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

15Hf 10h at 450ºC Austenite at RT

Nanometric precipitates (~5 nm)

Scientific ResultsScientific ResultsScientific ResultsScientific Results

Page 17: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

20Zr 48h at 500ºC

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf 3h at 500ºC

Precipitates in martensite

Page 18: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

20Zr 700ºC-100ºC FC

Long precipitates O(100 nm)

Scientific ResultsScientific ResultsScientific ResultsScientific Results

Page 19: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

EDX Microanalysis

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf 10h at 600ºC

20Zr 700ºC-100ºC FC

at% Ni Ti Hf Precipitates 52.5 21.2 26.3 Matrix 49.2 34.0 16.8

at% Ni Ti Zr Precipitates 52.6 18.8 28.6 Matrix 49.6 30.8 19.6

Precipitates are richer in Hf/Zr and poorer in Ti, and a bit richer in Ni.

Page 20: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Twinning modes of B19’ martensite in samples with precipitates

Scientific ResultsScientific ResultsScientific ResultsScientific Results

Page 21: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Twinning modes of B19’ martensite in samples with precipitates

Scientific ResultsScientific ResultsScientific ResultsScientific Results

(011)B19’ Type I twinning Twin plane || intervariant boundary

(001)B19’ compound twinning (internal twins - LIS)

Same twinning modes and boundaries as reported in literature for Ni-Ti-Hf alloys

{111} and {113}-type intervariant boundaries

Page 22: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Intervariant boundaries

Scientific ResultsScientific ResultsScientific ResultsScientific Results

{111} or {113}-type boundaries quite irregular

(011)

Perfect (011) boundaries

|| twin plane

Page 23: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Intervariant boundaries

Scientific ResultsScientific ResultsScientific ResultsScientific Results

{111} or {113}-type boundaries quite irregular

(011)

Perfect (011) boundaries

|| twin plane

Page 24: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Structural model of the precipitate new phase

Scientific ResultsScientific ResultsScientific ResultsScientific Results

Page 25: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Benefits received from IIMECBenefits received from IIMECBenefits received from IIMECBenefits received from IIMEC

Benefits in Alper’s education and personal life

The summer stay provided a strong impulse to TAMU-UIB

collaboration

Several good publications envisaged

Creation of a good scientific common background for possible

future applications of research projects in International

Programs (NSF, EU, …)

Page 26: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Thanks for your attention!!!Thanks for your attention!!!Thanks for your attention!!!Thanks for your attention!!!

Page 28: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf SHAPE MEMORY EFFECT

SHT

~ 3.5%

Page 29: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

20Zr Af temperature vs ageing time

Page 30: Evirgen 1 , I. Karaman 1 , R. Santamarta 2 , J. Pons 2

[email protected]

Scientific ResultsScientific ResultsScientific ResultsScientific Results

15Hf Af temperature vs ageing time