session 15: measuring substrate-independent · 2016. 9. 4. · the solution: accounting for...

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Page 1 Session 15: Measuring Substrate-Independent Young’s Modulus of Thin Films Jennifer Hay Factory Application Engineer Nano-Scale Sciences Division Agilent Technologies [email protected] To view previous sessions: https://agilenteseminar.webex.com/agilenteseminar/onstage/g.php?p=117&t=m

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Page 1: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 1

Session 15: Measuring Substrate-Independent

Young’s Modulus of Thin Films

Jennifer Hay

Factory Application Engineer

Nano-Scale Sciences Division

Agilent Technologies

[email protected]

To view previous sessions: https://agilenteseminar.webex.com/agilenteseminar/onstage/g.php?p=117&t=m

Page 2: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

What’s the problem?

Page 2

• Low-k film (440

nm) on silicon

• Berkovich indenter

• CSM (1nm, 75 Hz)

• Oliver-Pharr

analysis

?

Page 3: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

The solution: accounting for substrate influence

Page 3

• Low-k film (440

nm) on silicon

• Berkovich indenter

• CSM (1nm, 75 Hz)

• Oliver-Pharr

analysis PLUS

thin-film analysis

Hay, J.L. and Crawford, B., "Measuring Substrate-Independent Modulus

of Thin Films," Journal of Materials Research 26(6), 2011.

“It was fun to read.” – Prof. Gang Feng, Villanova University

Page 4: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 4

Both film and substrate influence measured

response

Development of strain field during nano-indentation of a film-substrate system, from Modelling

Simul. Mater. Sci. Eng. 12 (2004) 69–78. (Authors: Yo-Han Yoo, Woong Lee and Hyunho Shin)

Page 5: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 5

Review of efforts to solve this problem

• (1986) Doerner and Nix: Analytic model assuming linear

transition from to substrate and including an empirically

determined constant.

• (1989) King: Form of Doerner-Nix model with no adjustable

parameters.

• (1989) Shield and Bogy: Analytic model, but with physical

problems.

• (1992) Gao, Chiu, and Lee: Simple approximate model.

• (1997) Mencik: Practical refinements to the Gao model.

• (1999-2006) Song, Pharr, and colleagues: Alternate version

of Gao’s approximate model.

Page 6: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 6

The Song-Pharr model with Gao’s weight function

a

t film, mf

substrate, ms

mmm fsa

II11

)1(1

00

m ≡ shear modulus; E = 2m(1+n)

Page 7: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Modeling the relationship between two springs

Springs (of differing stiffness) in series,

subject to a force:

• The deformation in each spring is

DIFFERENT. The more compliant spring

deforms more.

• The MORE COMPLIANT spring dominates

the response.

Page 7

Springs (of differing stiffness) in parallel,

subject to a force:

• The springs undergo the SAME

deformation.

• The STIFFER spring dominates the

response

Page 8: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

How to account for lateral support of the film?

Page 8

When film is stiff:

• Deformation in the top

layer of the substrate

approaches that of the film.

• Film dominates the

response.

clearly

series

Parallel

?

Page 9: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Allow film to act both in series and parallel (Hay & Crawford, 2011)

Page 9

film

Indentation force

substrate

film

substrate film

Indentation force

previous form new form

Page 10: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

But previous advancements are retained

• Gao’s weight functions, I0 & I1 for gradually shifting influence

of each spring with indentation depth.

• Mencik’s suggestion that t = t0 – hc.

• Definition of effective Poisson’s ratio suggested by Song and

Pharr.

Page 10

Page 11: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

A new model for elastic film-substrate response

Page 11

film

substrate film

Applied indentation force

Page 12: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

A new model for elastic film-substrate response

Page 12

mf : shear modulus, film

ms : shear modulus, substrate

F : empirical constant;

F = 0.0626

a : contact radius

t : film thickness

D : relates stiffness to

modulus; D=4a/(1-na)

I0 : Gao’s weighting function;

as a/t → 0, I0 → 1;

as a/t → ∞, I0 → 0

force

Page 13: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 13

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Page 14: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 14

Hay & Crawford, 2011

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Page 15: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 15

Hay & Crawford, 2011

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Page 16: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 16

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Page 17: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 17

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Page 18: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 18

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Page 19: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 19

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Page 20: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 20

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Page 21: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 21

Hay & Crawford, 2011

Gao, et al., 1992

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Gao, et al., 1992

Page 22: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 22

Hay & Crawford, 2011

Gao, et al., 1992

Menčίk et al., 1997

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Gao, et al., 1992

Page 23: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 23

Hay & Crawford, 2011

Gao, et al., 1992

Menčίk et al., 1997

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Gao, et al., 1992

Page 24: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

The value of finite-element simulations

Page 24

t Ef-in

70.3o

0

0.05

0.1

0.15

0.2

0 50 100 150 Lo

ad

on

Sam

ple

/mN

Displacement/nm

Eout Analytic

model

Page 25: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

The value of finite-element simulations

Page 25

t Ef-in

70.3o

0

0.05

0.1

0.15

0.2

0 50 100 150 Lo

ad

on

Sam

ple

/mN

Displacement/nm

Eout

≡Eapparent

Sneddon

Page 26: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

The value of finite-element simulations

Page 26

t Ef-in

70.3o

0

0.05

0.1

0.15

0.2

0 50 100 150 Lo

ad

on

Sam

ple

/mN

Displacement/nm

Eout

≡Efilm

Sneddon &

Hay-Crawford

Page 27: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 27

Summary of 70 finite-element simulations (2D)

.

Simulation Es, GPa Maximum indenter displacement (h), nm

1-10 100 20 40 60 80 100 120 140 160 166 174

11-20 50 20 40 60 80 100 120 140 160 166 184

21-30 20 20 40 60 80 100 120 140 160 180 200

31-40 10 20 40 60 80 100 120 140 160 180 200

41-50 5 20 40 60 80 100 120 140 160 180 200

51-60 2 20 40 60 80 100 120 140 160 180 200

61-70 1 20 40 60 80 100 120 140 160 180 200

500 nm Ef = 10GPa

70.3o

Page 28: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 28

Summary of 70 finite-element simulations (2D)

.

Simulation Es, GPa Maximum indenter displacement (h), nm

1-10 100 20 40 60 80 100 120 140 160 166 174

11-20 50 20 40 60 80 100 120 140 160 166 184

21-30 20 20 40 60 80 100 120 140 160 180 200

31-40 10 20 40 60 80 100 120 140 160 180 200

41-50 5 20 40 60 80 100 120 140 160 180 200

51-60 2 20 40 60 80 100 120 140 160 180 200

61-70 1 20 40 60 80 100 120 140 160 180 200

500 nm Ef = 10GPa

70.3o

Page 29: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Is everything OK with simulations?

Page 29

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef=Es, apparent

input film modulus for all simulations

Page 30: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Is everything OK with simulations?

Page 30

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef=Es, apparent

Ef=Es, film alone

input film modulus for all simulations

Page 31: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 31

Summary of 70 finite-element simulations (2D)

.

Simulation Es, GPa Maximum indenter displacement (h), nm

1-10 100 20 40 60 80 100 120 140 160 166 174

11-20 50 20 40 60 80 100 120 140 160 166 184

21-30 20 20 40 60 80 100 120 140 160 180 200

31-40 10 20 40 60 80 100 120 140 160 180 200

41-50 5 20 40 60 80 100 120 140 160 180 200

51-60 2 20 40 60 80 100 120 140 160 180 200

61-70 1 20 40 60 80 100 120 140 160 180 200

500 nm Ef = 10GPa

70.3o

Page 32: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 32

Simulations: Compliant film on stiff substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 0.1, apparent

input film modulus for all simulations

Page 33: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 33

Simulations: Compliant film on stiff substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 0.1, apparent

Ef/Es = 0.1, film alone

input film modulus for all simulations

Page 34: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 34

Simulations: Compliant film on stiff substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 0.1, apparent

Ef/Es = 0.1, Film (Hay)

Ef/Es = 0.1, Film (Song-Pharr)

input film modulus for all simulations

Page 35: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 35

Summary of 70 finite-element simulations (2D)

.

Simulation Es, GPa Maximum indenter displacement (h), nm

1-10 100 20 40 60 80 100 120 140 160 166 174

11-20 50 20 40 60 80 100 120 140 160 166 184

21-30 20 20 40 60 80 100 120 140 160 180 200

31-40 10 20 40 60 80 100 120 140 160 180 200

41-50 5 20 40 60 80 100 120 140 160 180 200

51-60 2 20 40 60 80 100 120 140 160 180 200

61-70 1 20 40 60 80 100 120 140 160 180 200

500 nm Ef = 10GPa

70.3o

Page 36: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 36

Simulations: Stiff film on compliant substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 10, apparent

input film modulus for all simulations

Page 37: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 37

Simulations: Stiff film on compliant substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 10, apparent

Ef/Es = 10, Film (Hay)

input film modulus for all simulations

Page 38: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 38

Simulations: Stiff film on compliant substrate

.

0

2

4

6

8

10

12

14

16

18

20

0 10 20 30 40

Yo

un

g's

Mo

du

lus

[G

Pa

]

Indenter Penetration / Film Thickness [%]

Ef/Es = 10, apparent

Ef/Es = 10, Film (Hay)

Ef/Es = 10, Film (Song-Pharr)

input film modulus for all simulations

Page 39: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 39

Determining the value of F (fudge factor)

. Ef-out (P, h)

Ef = 2mf(1-nf)

Ef-in

0

/

:

70

1

2

dF

EEEd

Fi

infinfoutf i

F was determined as that value which minimized the sum of

the squared relative differences (between output and input

film moduli) over all 70 simulations.

F = 0.0626

sim

Page 40: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hay & Crawford, 2011

Solving for film modulus: mf = f(ma, mf, t0, a, hc, F)

Page 40

Hay & Crawford, 2011

Gao, et al., 1992

Menčίk et al., 1997

Sneddon, 1965, as implemented by

Oliver and Pharr, 1992

Song & Pharr, 1999

Gao, et al., 1992

Page 41: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

NanoSuite integration in CSM “thin film” methods

Page 41

Page 42: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

NanoSuite integration in ET “thin film” methods

Page 42

Page 43: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 43

Application: SiC on Si wafers

Sample ID Description t

nm

16 Silicon carbide (SiC) on Si 150

17 Silicon carbide (SiC) on Si 300

Page 44: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Experimental method

Page 44

• Materials:

o A set of 2 SiC films on Si

• Platform: Agilent G200 NanoIndenter with

o DCM head

o CSM option

o Berkovich indenter

o New test method: “G-Series DCM CSM Hardness,

Modulus for Thin Films.msm”

Page 45: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Stiff films on compliant substrates: SiC on Si

Page 45

0

50

100

150

200

250

300

350

400

0 10 20 30 40 50

Yo

un

g's

Mo

du

lus

[G

Pa]

Indenter Penetration / Film Thickness [%]

t=150nm, apparent

citation of results

Page 46: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Stiff films on compliant substrates: SiC on Si

Page 46

0

50

100

150

200

250

300

350

400

0 10 20 30 40 50

Yo

un

g's

Mo

du

lus

[G

Pa]

Indenter Penetration / Film Thickness [%]

t=150nm, apparent

t=150nm, film

citation of results

Page 47: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Stiff films on compliant substrates: SiC on Si

Page 47

0

50

100

150

200

250

300

350

400

0 10 20 30 40 50

Yo

un

g's

Mo

du

lus

[G

Pa]

Indenter Penetration / Film Thickness [%]

t=150nm, apparent

t=150nm, film

t=300nm, apparent

citation of results

Page 48: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Stiff films on compliant substrates: SiC on Si

Page 48

0

50

100

150

200

250

300

350

400

0 10 20 30 40 50

Yo

un

g's

Mo

du

lus

[G

Pa]

Indenter Penetration / Film Thickness [%]

t=150nm, apparent

t=150nm, film

t=300nm, apparent

t=300nm, film

citation of results

Page 49: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

SiC on Si: Modulus at h/t = 20%

Page 49

0

50

100

150

200

250

300

350

400

SiC on Si (t=150nm) SiC on Si (t=300nm)

Yo

un

g's

mo

du

lus

, h

/t=

20

%

[GP

a]

Sample

Film

Apparent

Film modulus is about 25% higher than apparent modulus!

Page 50: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Page 50

t0 = 445 nm t0 = 1007 nm

“Rapid Mechanical Characterization of low-k Films,”

http://cp.literature.agilent.com/litweb/pdf/5991-0694EN.pdf

Application: low-k materials (on silicon)

Page 51: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Experimental method

Page 51

• Materials:

o Two low-k films on Si

• Platform: Agilent G200 NanoIndenter with

o DCM head

o CSM option

o Express Test option

o Berkovich indenter

• Test Methods:

o G-Series DCM CSM Hardness, Modulus for Thin

Films

o Express Test for Thin Films

Page 52: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Modulus of low-k film (t = 1mm) is 4.44±0.08GPa

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Page 53: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Hardness of low-k film (t = 1mm) is 0.70±0.02GPa

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Page 54: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Application: Ultra-thin films

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Page 55: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Four samples

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Substrate: sintered Al2O3 and TiC

Basecoat: sputter-deposited Al2O3

(2600nm)

Page 56: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Four samples

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Substrate: sintered Al2O3 and TiC

Basecoat: sputter-deposited Al2O3

(2600nm)

PECVD SiO2 (50nm) OR ALD Al2O3 (50nm)

Page 57: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

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• Agilent G200 with DCM II head and NanoVision

• Express Test

• Berkovich indenter

• Thin-film model applied to both basecoat and top layers.

Experimental method

Page 58: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Substrate – independent

modulus of 50nm films

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E = 146 GPa

Application note: http://cp.literature.agilent.com/litweb/pdf/5991-4077EN.pdf

Page 59: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

In summary, the proposed model…

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• Has been verified by simulation and experiment.

• Is an improvement over prior models, because it works

well whether the film is more compliant or more stiff

than the substrate.

• Decreases experimental uncertainty by allowing

measurements to be made at larger depths which would

otherwise be unduly affected by substrate influence.

Page 60: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Application: Mechanical characterization of SAC

305 Solder by Instrumented Indentation Wednesday, May 14, 2014, 11:00 (New York)

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Abstract The reliability of soldered connections in electronic packaging depends on

mechanical integrity; mechanical failure can cause electrical failure. Mechanical

integrity, in turn, depends on mechanical properties. In this presentation, we focus

on the SAC 305 solder alloy (96.5% tin, 3% silver, and 0.5% copper) due to its

prevalent utilization in electronic packaging. First, we demonstrate the use of

nanoindentation to measure the elastic and creep properties of SAC 305. Next, we

utilize an advanced form of nanoindentation to quantitatively map mechanical

properties of all the components of a realistic SAC 305 solder joint.

To register:

https://agilenteseminar.webex.com/agilenteseminar/onstage/g.php?p=117&t=m

Page 61: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Session 16: Best Practice for Instrumented

Indentation Wednesday, June 11, 2014, 11:00 (New York)

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Abstract The purpose of this presentation is to provide a practical reference guide for

instrumented indentation testing. Emphasis is placed on the better-developed

measurement techniques and the procedures and calibrations required to obtain

accurate and meaningful measurements.

Recommended Reading Hay J.L. and Pharr G.M., “Instrumented Indentation Testing,” ASM Handbook:

Mechanical Testing and Evaluation, Volume 8, pp. 232-243 (2000).

To register: https://agilenteseminar.webex.com/agilenteseminar/onstage/g.php?p=117&t=m

Page 62: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Thank you!

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Page 63: Session 15: Measuring Substrate-Independent · 2016. 9. 4. · The solution: accounting for substrate influence Page 3 •Low-k film (440 nm) on silicon •Berkovich indenter •CSM

Two (sort of) independent problems

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• Composite compliance: Substrate influences the

stiffness that is measured.

• Errant contact area: Common model for

determining contact area is strained in its

application to thin films.

These two problems are easily convoluted,

because they both tend to push the calculated

Young’s modulus in the same direction.