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# Nanoindentation

Lecture 1

Basic Principle

Do Kyung Kim

Department of Naterials Science and

Engineering

KA!ST

!ndentation test (Hardness test)

Hardness - resistance to penetration of a hard indenter

Hardness

Hardness is a measure of a material's resistance to surface

penetration by an indenter with a force applied to it.

Hardness

Brinell, 10 mm indenter, 3000 kg Load F /surface area of

indentation A

vickers, diamond pyramid indentation

Nicrohardness

vickers microindentation : size of pyramid comparable to

microstructural features. You can use to assess relative

hardness of various phases or microconstituents.

Nanoindentation

Nicrohardness · vickers and Knoop

Nicroindentation

Optical micrograph of a Vickers

indentation (9.8 N) in soda-lime glass

including impression, radial cracking,

and medial cracking fringes.

Nechanical property

measurement in micro·scale

(Nicro·indentation)

To study the mechanical

behavior of different

orientations, we need

single crystals.

For a bulk sample, it is

hard to get a nano·scale

response from different

grains.

very little information on

the elastic·plastic

transition.

Nanoindentation

Nanoindentation is called as,

The depth sensing indentation

The instrumented indentation

Nanoindentation method gained popularity with the

development of,

Nachines that can record small load and displacement

with high accuracy and precision

Analytical models by which the load·displacement data

can be used to determine modulus, hardness and other

mechanical properties.

Nicro vs Nano !ndentation

Nicroindentation

A prescribed load appled to an indenter in

contact with a specimen and the load is

then removed and the area of the residual

impression is measured. The load divided

by the by the area is called the hardness.

Nanoindentation

A prescribed load is appled to an indenter

in contact with a specimen. As the load is

applied, the depth of penetration is

measured. The area of contact at full load

is determined by the depth of the

impression and the known angle or radius

of the indenter. The hardness is found by

dividing the load by the area of contact.

Shape of the unloading curve provides a

measure of elastic modulus.

Anthony C. Fischer-Cripps, PrincipIes of nanoindentation, training Iecture

Basic Hertz's elastic solution (1830s)

Schematics of indenter tips

Vickers Berkovich Knoop Conical Rockwell Spherical

·sided indenters

3·sided indenters

one indenters

!ndenter geometry

!ndenter type Projected area

Semi angle

(7

ective

cone angle

(-

!ntercept

actor

Ceometry

correction

actor (.

Sphere A 62Rh

p

N/A N/A 0.7S 1

Berkovich A = 3h

p

2

tan

2

7 6S.3 H 70.2336 H 0.7S 1.034

vickers A = 4h

p

2

tan

2

7 68 H 70.32 H 0.7S 1.012

Knoop A = 2h

p

2

tan7

1

tan7

2

7

1

=86.2S H

7

2

=6S H

77.64 H 0.7S 1.012

Cube Corner A = 3h

p

2

tan

2

7 3S.26 H 42.28 H 0.7S 1.034

Cone A = 6h

p

2

tan

2

- - - 0.72 1

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer

Stress field under indenter · contact field

Boussinesq fields (point load) Hertzian fields (spherical indenter)

rian Lawn, Fracture of rittIe SoIids, 1993, Cambridge Press

Anthony Fischer-Cripp, Intro Contact Mechanics, 2000, Springer

Sharp indenter (Berkovich)

Advantage

Sharp and well·defined

tip geometry

Well·defined plastic

deformation into the

surface

Cood for measuring

modulus and hardness

values

Disadvantage

Elastic·plastic transition

is not clear.

Blunt indenter · spherical tip

Advantage

Extended elastic·plastic

deformation

Load displacement results

can be converted to

indentation stress·strain

curve.

Useful in determination of

yield point

Disadvantage

Tip geometry is not very

sharp and the spherical

surface is not always

perfect.

Data Ananlysis

P : applied load

h : indenter displacement

h

r

: plastic deformation after load removal

h

e

: surface displacement at the contact perimeter

Analytical Nodel - Basic Concept

Nearly all o the elements o this analysis were irst developed by workers at the

Baikov !nstitute o Netallurgy in Noscow during the 1370's (or a review see Bulychev

and Alekhin. The basic assumptions o this approach are

eormation upon unloading is purely elastic

The compliance o the sample and o the indenter tip can be

combined as springs in series

The contact can be modeled using an analytical model or

contact between a rigid indenter o deined shape with a

homogeneous isotropic elastic hal space using

where S is the contact stiness and A the contact area. This relation was presented

by Sneddon. Later, Pharr, Oliver and Brotzen where able to show that the equation is

a robust equation which applies to tips with a wide range o shapes.

Analytical Nodel - Doerner·Nix Nodel

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer

Analytical Nodel - Field and Swain

They treated the indentation as a reloading of a preformed

impression with depth h

f

into reconformation with the

indenter.

FieId, Swain, J Mater Res, 1993

Analytical Nodel - Oliver and Pharr

Iiver & Pharr, J Mater Res, 1992

Continuous Stiffness Neasurement (CSN)

The nanoindentation system

applies a load to the indenter

tip to orce the tip into the

surace while simultaneously

superimposing an oscillating

orce with a orce amplitude

generally several orders o

magnitude smaller than the

nominal load.

!t provides accurate

measurements o contact

stiness at all depth.

The stiness values enable us

to calculate the contact radius

at any depth more precisely.

Iiver, Pharr, Nix, J Mater Res, 2004

Analysis result

ardness

'

' 1 1 1

2 2

*

E E E

; ;

p

A

E

dh

dP

*

2

2

2

2

5 . 24 3 . 65 tan 3 3

p p

h h A

5 . 24

1

2

1

*

6

.

p

h dh

dP

E

2

5 . 24

p

h

P

H

lastic modulus

Contact area

Stiness

Reduced modulus

34 . 1 . or Berkovich indenter

modulus o specimen

modulus o indenter

or Berkovich indenter

Nov 28, 2006

No of citation

Nov 2003 - 1520, Nov 2005 - 2436

One of the most cited paper in Naterials Science

Naterial response

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer

Nanoindenter tips

Berkovich indenter

Projected area

2 2 2

2

56 . 24 3 . 65 tan 3 3

3 . 65 tan 3 2

3 . 65 tan 3 2 3 . 65 sin 3 2

3 . 65 cos

27 . 65 cos

4

3

2

2

3

2 /

6 tan

h h A

h a

a a

h

b

h

a

al

A

a l

a

l

o

proi

o

o o

o

o

proi

o

b

Berkovich vs vickers indenter

ace angle o Berkovich indenter 6S. 3 H

Same projected area·to·depth ratio as vickers indenter

quivalent semi·angle or conical indenter 70.3 H

- 6

2

2

tan

p

h A

2 2 2

56 . 24 3 . 65 tan 3 3 h h A

o

proi

2 2 2

54 . 24 68 tan 4 h h A

o

proi

Berkovich projected area vickers projected area

Commercial machines

NTS_Nano·!ndenter XP

CSN_NT

(Nano·ardness Tester

ysitron_Triboscope

CS!RO_UN!S

(Ultra·Nicro·!ndentation System

Commercial machine implementation

NTS_Nano·!ndenter

CS!RO_UN!S

Hysitron_TriboScope CSN_NHT

!nductive orce generation system

isplacement measured by capacitance gage

Two perpendicular transducer systems

isplacement o center plate capacitively measured

Load via lea springs by expansion o load actuator

election measured using a orce LvT

orce applied by an electromagnetic actuator

isplacement measured via a capacitive system

Force actuation

Electromagnetic actuation Electrostatic actuation

Spring·based force actuation Piezo/spring actuation

most common means

long displacement range S wide load range

Large and heavy due to permanent magnet

lectrostatic orce btwn 3·plate transducer applied

Small size (tenths o mm S good temperature stability

Limited load(tenths o mN S displacement(tenths o 3N

Tip attached to end o cantilever S

Sample attached to piezoelectric actuator

isplacement o laser determine displacement

Tip on lea springs are displaced by piezoelectric actuator

orce resolution is very high ( pN range,

As resolution goes up, range goes down S Tip rotation

Displacement measurement

Differential capacitor Optical lever method

Linear variable Differential

Transducer (LvDT)

Laser interferometer

Neasure the dierence btwn C

1

and C

2

due to

igh precision(resolution < 1 Ä S small size

Relatively small displacement range

d

A

C

c c

1 1

Photodiode measures lateral displacement

Popular method in cantilever based system

etection o delection < 1 ?

AC voltage proportional to relative displacement

igh signal to noise ratio and low output impedance

lower resolution compared to capacitor gage

Beam intensity depends on path dierence

Sensitivity < 1 Ä S used in hostile environment

abry·Perot system used or displacement detection

Factor affecting nanoindentation

Thermal Drift

!nitial penetration depth

!nstrument compliance

!ndenter geometry

Piling·up and sinking·in

!ndentation size effect

Surface roughness

Tip rounding

Residual stress

Specimen preparation

Thermal drift

Drift can be due to vibration or a thermal drift

Thermal drift can be due to

Different thermal expansion in the machine

Heat generation in the electronic devices

Drift might have parallel and/or a perpendicular component

to the indenter axis

Thermal drift is especially important when studying time

varying phenomena like creep.

Thermal drift calibration

ndenter displacement vs time

during a period of constant

load. The measured drift rate

is used to correct the load

displacement data.

Application of thermal

drift correction to the

indentation load-

displacement data

Nachine compliance

Displacement arising from the compliance of the testing

machine must be subtracted from the load·displacement

data

The machine compliance includes compliances in the

sample and tip mounting and may vary from test to test

!t is feasible to identify the machine compliance by the

direct measurement of contact area of various indents in a

known material

Anther way is to derive the machine compliance as the

intercept of 1/total contact stiffness vs 1/ sqrt(maximum

load) plot, if the Young's modulus and hardness are

assumed to be depth·independent

Nachine compliance calibration

&sually done by manufacturer

using materials with known

properties (aluminum for large

penetration depths, fused

silica for smaller depth).

&sing an accurate value

of machine stiffness is

very important for large

contacts, where it can

significantly affect the

measured load-

displacement data.

Real tip shape

Deviation from perfect shape

Sphero-Conical tips

Anthony C. Fischer-Cripps, Nanoindentation, 2002, Springer

Area function calibration

!deal tip geometry yields

the following area·to·

depth ratio:

A = 2.S h

c

2

Real tips are not perfect!

Calibration

Use material with known elastic

properties (typically fused silica)

and determine its area as a

function of contact

New area function

A = C

1

h

c

2

+ C

2

h

c

+ C

3

h

c

1/2

+ C

h

c

1/

+ C

S

h

c

1/8

+ .

Surface roughness

As sample roughness does have a signiicant eect on the measured

mechanical properties, one could either try to incorporate a model to

account or the roughness or try to use large indentation depths at which

the inluence o the surace roughness is negligible.

A model to account or roughness eects on the measured hardness is

proposed by Bobji and Biswas.

Nevertheless it should be noticed that any model will only be able to

account or surace roughnesses which are on lateral dimensions

signiicantly smaller compared to the geometry o the indent

Pile·up and Sinking·in

Phase transition measurement

Nanoindentation on silicon and Raman analysis

Creep measurement

Plastic deformation in all

materials is time and

temperature dependent

!mportant parameter to

determine is the strain rate

sensitivity

The average strain rate can

be given by

!t can be done by experiments at different loading rate

or by studying the holding segment of a

nanoindentation.

dt

dh

h

c

c

ind

1

1

Fracture toughness measurement

Combining of Laugier proposed toughness

model and Ouchterlony's radial cracking

modification factors, fracture toughness

can be determined.

Fracture toughness expression

K

c

= 1.073 x

v

(a/l)

1/2

(E/H)

2/3

P / c

3/2

High temperature measurement

Nanindentation with or

without calibration

Temperature match btw. indenter and sample is

important for precision test.

Prior depth calibration and post thermal drift correct are

necessary.

Nanomechanical testing

Tests

Nanohardness/Elastic

modulus

Continuous Stiffness

Neasurements

Acoustic Emmisions

Properties at various

Temperature

Friction Coefficient

Wear Tests

Adhesion

NanoScratch Resistance

Fracture Toughness

Delamination

Common Applications

Fracture Analysis

Anti·Wear Films

Lubricant Effect

Paints and Coatings

Nanomachining

Bio·materials

Netal·Natrix Composites

Diamond Like Carbon

Coatings

Semiconductors

Polymers

Thin Films Testing and

Development

Property/Processing

Relationships