Nanoindentation

Lecture 1 Basic Principle

Do Kyung Kim Department of Materials Science and Engineering KAIST

Indentation 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 Microhardness Vickers microindentation : size of pyramid comparable to microstructural features. You can use to assess relative hardness of various phases or microconstituents. Nanoindentation

Microhardness - Vickers and Knoop

Microindentation
Mechanical property measurement in micro-scale (Micro-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.

Optical micrograph of a Vickers indentation (9.8 N) in soda-lime glass including impression, radial cracking, and medial cracking fringes.

Nanoindentation
Nanoindentation is called as, The depth sensing indentation The instrumented indentation Nanoindentation method gained popularity with the development of, Machines 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.

Micro vs Nano Indentation

Microindentation
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, Principles of nanoindentation, training lecture

Basic Hertz s elastic solution (1890s)

Schematics of indenter tips

Vickers

Berkovich

Knoop

Conical

Rockwell

Spherical

4-sided indenters

3-sided indenters

Cone indenters

Indenter geometry
Indenter type Projected area Semi angle ( U) N/A 65.3 r 68 r
U1=86.25 r U2=65 r

Effective cone angle (E ) N/A 70.2996 r 70.32 r 77.64 r

Intercept factor 0.75 0.75 0.75 0.75

Geometry correction factor (F) 1 1.034 1.012 1.012

Sphere Berkovich Vickers Knoop

A } T2Rhp A = 3hp2tan2U A = 4hp2tan2U A = 2hp2tanU1tanU2 A = 3hp2tan2U A = Thp2tan2E

Cube Corner

35.26 r

42.28 r

0.75

1.034

Cone

0.72

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

Stress field under indenter - contact field

Boussinesq fields (point load)

Hertzian fields (spherical indenter)

Brian Lawn, Fracture of Brittle Solids, 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 Good 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 hr : plastic deformation after load removal he : surface displacement at the contact perimeter

Analytical Model

Basic Concept

Nearly all of the elements of this analysis were first developed by workers at the Baikov Institute of Metallurgy in Moscow during the 1970's (for a review see Bulychev and Alekhin). The basic assumptions of this approach are

Deformation upon unloading is purely elastic The compliance of the sample and of the indenter tip can be combined as springs in series

The contact can be modeled using an analytical model for contact between a rigid indenter of defined shape with a homogeneous isotropic elastic half space using

where S is the contact stiffness 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 of shapes.

Analytical Model

Doerner-Nix Model

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

Analytical Model

Field and Swain

They treated the indentation as a reloading of a preformed impression with depth hf into reconformation with the indenter.
Field, Swain, J Mater Res, 1993

Analytical Model

Oliver and Pharr

Oliver & Pharr, J Mater Res, 1992

Continuous Stiffness Measurement (CSM)

The nanoindentation system applies a load to the indenter tip to force the tip into the surface while simultaneously superimposing an oscillating force with a force amplitude generally several orders of magnitude smaller than the nominal load. It provides accurate measurements of contact stiffness at all depth. The stiffness values enable us to calculate the contact radius at any depth more precisely.
Oliver, Pharr, Nix, J Mater Res, 2004

Analysis result
Reduced modulus

1 1  Y 2 1  Y '2 !  * E E E'
dP !2 dh
*

E: modulus of specimen E : modulus of indenter

Stiffness

A p
2 2

Contact area

! 3 3h p tan 2 65.3 ! 24.5h p

for Berkovich indenter

Hardness

P H! 2 24.5h p
*

Elastic modulus

dP 1 1 dh 2h p F

T 24.5

F ! 1.034 for Berkovich indenter

One of the most cited paper in Materials Science

Nov 28, 2006

No of citation Nov 2003 - 1520, Nov 2005 - 2436

Material response

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

Nanoindenter tips

Berkovich indenter
tan 60 o ! l! l a/2

3 a 2 3 2 al ! ! a proj 2 4 h cos 65.27 o ! b a cos 65.3o a ! h! 2 3 sin 65.3o 2 3 tan 65.3o a ! 2 3h tan 65.3o
! 3 3h 2 tan 2 65.3o ! 24.56h 2

Projected area

proj

Berkovich vs Vickers indenter

Berkovich projected area Vickers projected area

Aproj ! 3 3h 2 tan 2 65.3o ! 24.56h 2

Face angle of Berkovich indenter: 65. 3 r

proj

! 4h 2 tan 2 68o ! 24.504h 2

Same projected area-to-depth ratio as Vickers indenter Equivalent semi-angle for conical indenter: 70.3 r

! h p tan 2

Commercial machines
MTS_Nano-Indenter XP CSIRO_UMIS
(Ultra-Micro-Indentation System)

Hysitron_Triboscope

CSM_NHT
(Nano-Hardness Tester)

Commercial machine implementation

MTS_Nano-Indenter CSIRO_UMIS

Inductive force generation system Displacement measured by capacitance gage

Load via leaf springs by expansion of load actuator Deflection measured using a force LVDT

Hysitron_TriboScope

CSM_NHT

Two perpendicular transducer systems Displacement of center plate capacitively measured

Force applied by an electromagnetic actuator Displacement measured via a capacitive system

Force actuation
Electromagnetic actuation Electrostatic actuation

most common means long displacement range & wide load range Large and heavy due to permanent magnet

Electrostatic force btwn 3-plate transducer applied Small size (tenths of mm) & good temperature stability Limited load(tenths of mN) & displacement(tenths of QN)

Spring-based force actuation

Piezo/spring actuation

Tip attached to end of cantilever & Sample attached to piezoelectric actuator Displacement of laser determine displacement

Tip on leaf springs are displaced by piezoelectric actuator Force resolution is very high ( pN range), As resolution goes up, range goes down & Tip rotation

Displacement measurement
Differential capacitor Optical lever method

C!

I I0 A d

Measure the difference btwn C1 and C2 due to ( High precision(resolution < 1 ) & small size Relatively small displacement range

Photodiode measures lateral displacement Popular method in cantilever based system Detection of deflection < 1

Linear Variable Differential Transducer (LVDT)

Laser interferometer

AC voltage proportional to relative displacement High signal to noise ratio and low output impedance lower resolution compared to capacitor gage

Beam intensity depends on path difference Sensitivity < 1 & used in hostile environment Fabry-Perot system used for displacement detection

Factor affecting nanoindentation

Thermal Drift Initial penetration depth Instrument compliance Indenter geometry Piling-up and sinking-in Indentation 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

Indenter 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 loaddisplacement data

Machine 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 It 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

Machine compliance calibration

Usually done by manufacturer using materials with known properties (aluminum for large penetration depths, fused silica for smaller depth).

Using an accurate value of machine stiffness is very important for large contacts, where it can significantly affect the measured loaddisplacement data.

Real tip shape

Deviation from perfect shape

Sphero-Conical tips

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

Area function calibration

Ideal tip geometry yields the following area-todepth ratio: A = 24.5 hc2 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 = C1hc2 + C2hc + C3hc1/2 + C4hc1/4 + C5hc1/8 +

Surface roughness

As sample roughness does have a significant effect on the measured mechanical properties, one could either try to incorporate a model to account for the roughness or try to use large indentation depths at which the influence of the surface roughness is negligible. A model to account for roughness effects on the measured hardness is proposed by Bobji and Biswas. Nevertheless it should be noticed that any model will only be able to account for surface roughnesses which are on lateral dimensions significantly smaller compared to the geometry of 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 Important parameter to determine is the strain rate sensitivity The average strain rate can be given by

I ind

1 dhc ! hc dt

It can be done by experiments at different loading rate or by studying the holding segment of a nanoindentation.

Fracture toughness measurement

Combining of Laugier proposed toughness model and Ouchterlonys radial cracking modification factors, fracture toughness can be determined. Fracture toughness expression Kc = 1.073 xv (a/l)1/2 (E/H)2/3 P / c3/2

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 Measurements 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 Metal-Matrix Composites Diamond Like Carbon Coatings Semiconductors Polymers Thin Films Testing and Development Property/Processing Relationships