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WHAT IS NANOINDENTATION

‘TO UNDERSTAND THE VERY LARGE, WE MUST UNDERSTAND THE VERY SMALL’
DEMOCRITUS (470-380 BC)

• Such an indentation testing in which both load and the depth of


penetration are in the micro scale or lower.
• Gives real time measurement of Load and Depth

WHY NANOINDENTATION
• To engineer better materials, mechanical properties play a very critical role.
• Nanoscale engineering makes materials lighter, stronger, cheaper, more
recyclable.
Conventional Hardness testing Vs Nanoindentation

CONVENTIONAL NANOINDENTATION
1 HARDNESS TESTING 2 TESTING

• Large and varied tip shapes • Precise tip shape and


indenter geometry
• Not very good spatial
resolution of the indenter • High spatial resolution to
rigs. place indents

• Micro indentation gives the • Provides real time load


average hardness over the displacement data while
large area. indentation is in progress.
REQUIREMENTS OF NANOINDENTATION

• Unlike Conventional hardness testing


Nanoindentation requires some conditions to
be fulfilled:

BERKOVICH TIP
Total included angle: 142.3˚
with an half angle of 65.35˚
Average radius of curvature
between 100 and 200 nm
REQUIREMENTS OF NANOINDENTATION

• Unlike Conventional hardness testing


Nanoindentation requires some conditions to
be fulfilled:
• High accuracy, precision equipment's for
recording the small load and displacement
Total included angle: 142.3˚
with an half angle of 65.35˚
Average radius of curvature
between 100 and 200 nm
REQUIREMENTS OF NANOINDENTATION

• Unlike Conventional hardness testing


Nanoindentation requires some conditions to
be fulfilled:
• High accuracy, precision equipment's for
recording the small load and displacement
• Analytical modeling for utilizing the load Total included angle: 142.3˚
displacement curve data for determining the with an half angle of 65.35˚
Average radius of curvature
various mechanical properties. between 100 and 200 nm
PROCESS
Loading and then Unloading is done on
the material surface

outer electrode
springs

center electrode

outer electrode

indenter
The maximum value of mean contact
pressure obtained during loading is
called HARDNESS

Pmax
Ac

hc hmax

𝑃max
𝐻=
𝐴𝐶
The data obtained during unloading forms the
basis for contact area during Maximum load

Load, P
hf
0
0

Depth, h

A load/displacement curve is generated


from each test, yielding insights into the
nanomechanical behavior of the material
Stiffness obtained from the unloading curve

Load, P
hf
0
0

Depth, h

S 
Er =
2 Ac
LOAD DISPLACEMENT CURVE - ANALYSIS
OLIVER-PHARR METHOD- MORE
COMPLICATED, NON-LINEAR CURVE FIT,
MORE ACCURATE RESULTS

MODULUS OF THE MATERIAL IS INVERSLY


PROPORTIONAL TO STIFFNESS VALUE
Load, P

SLOPE OF UNLOADING CURVE GIVES US


STIFFNESS OF THE MATERIAL BEING TESTED

ANALYSIS OF CURVE CAN GIVE US


0 hf
0 HARDNESS, ELASTIC MODULUS

Depth, h
LOAD DISPLACEMENT CURVE HAS TWO
PARTS
LOADING
UNLOADING
NANOSCALE APPLICATIONS AND MATERIALS
• Semiconductor Materials
• Through-silicon via, wafer on wafer
• Quality control & failure analysis ✓ Thin Films
• Energy ✓ Nanowires
• Battery components ✓ Bulk Metallic Glass
• Irradiated materials ✓ Polymer/CNT Composites
• Oil shale
✓ Piezo Materials
• Thin films for solar
✓ Low k dielectrics
• Protective coatings for oil & gas

• Automotive ✓ Graphene

• Lightweight metals / alloys ✓ DLC


✓ CNT
• Aerospace & Defense
✓ Metals
• Superalloys, Bond Coatings
✓ Silicon
• Biological / Biomedical
✓ Ceramics
• Mineralized tissues (bones, teeth)
• Collagen fibers

• MEMS / NEMS
• Composites
• Particle / matrix
• Carbon Nanotubes
NG50 – Nanoindenter with in-situ SPM Imaging
Scanner

Transducer

Specimen Translator

Motorized Stage

Stage plates

Granite

Vibration Isolation
in-situ SPM Imaging

Utilizes same probe used for nanomechanical testing

612 x 498 µm 218 x 176 µm 3-Axis Piezo Positioner


Optical

3-Plate Capacitive Transducer

20 x 20 µm
In-Situ SPM

5 x 5 µm
Quantitativ
e Data
NG50 – Performs below mentioned tests

• NanoIndentation
• To characterize Nanoscratch
• Hardness, elastic modulus, stiffness
• Creep, stress relaxation
• Fracture toughness
• Nanoscartach
• To characterize
• Coefficient of friction Nanoindentation Nanowear
• Scratch resistance, critical load
• Thin film adhesion, delamination
• Nanowear 5 µm
• To characterize area
• ScanningWear
• Wear depth, wear resistance Indenter-
• Nanomachining, nanolithography based SPM
in-situ SPM Images
Friction Welded Sample – Nanoindentation Test

Figure 1: 778 x 564 µm optical micrographs of (a) Bare


Region and (b) Welded Region of FSW steel sample as
seen from the instrument’s optics.
Figure 2: Load Displacement Curve for bare region,
advancing region and the nugget region

Figure 4: Hardness and Reduced Modulus as a


Figure 3: (a) Modulus and (b) Hardness as a function of function of contact depth corresponding to the
contact depth for the three different regions of the sample. region demonstrated by the schematic of the
sample.
Friction Welded Sample – Nanowear Test

Figure 1: 778 x 564 µm optical


micrographs of (a) Bare Region 1 PASS 5 PASS 1 PASS 5 PASS
and (b) Welded Region of FSW
Figure 2: Topographical in-situ SPM images of Figure 3: Topographical in-situ SPM images of
steel sample as seen from the
wear tests performed at 50 µN ((a) 1 pass and wear tests performed at 50 µN ((a) 1 pass and
instrument’s optics.
(b) 5 passes) and 100 µN (c) 1 pass and (d) (b) 5 passes) and 100 µN (c) 1 pass and (d)
5 passes on the nugget region. 5 passes on the bare region.
3D PRINTED GLASS SAMPLE – RESPECTIVE
NANOINDENTATION TESTS

Figure 2. Topographical in-situ SPM image of the all four samples

Figure 1 Sample mounting scheme to study


the properties Glass samples

Figure 4 Comparative Hardness and reduced modulus of the glass samples


Reduced
Hardness
Sample Modulus
(GPa)
(GPa)
1 6.57 73.65
2 8.87 96.81
3 5.35 67.3
Figure 3 comparative load displacement data 4 and Reduced
Table: 2 Hardness 5.81modulus data of
72.85
glass samples
3D PRINTED GLASS SAMPLE – RESPECTIVE
NANOINDENTATION TESTS – Contd…

Figure 2. Topographical in-situ SPM image of the all four samples after tests

Figure 1 Sample mounting scheme to study


the properties Glass samples

Figure 4 Comparative Hardness and reduced modulus of the glass samples


Reduced
Hardness
Sample Modulus
(GPa)
(GPa)
1 6.57 73.65
2 8.87 96.81
3 5.35 67.3
Figure 3 comparative load displacement data 4 and Reduced
Table: 2 Hardness 5.81modulus data of
72.85
glass samples
NANOINDENTATION TESTS & IMAGING
50X50 um
50x50µm

Automation feature
helps user to select
specific location as
circled in the Fig. 3 to
perform tests at
those specified
Fig. 1 SEM Image of HIF Fig. 2 SPM Image of HIF locations

Fig. 3 SPM Image after Indentation

Hardness = 3.3 Gpa


SD = 0.19 GPa

Fig. 4 HIF sample SPM images with different scan size Fig. 5 Load –Displacement curves at different location
NANOINDENTATION TESTS & IMAGING

Figure 1 Sample mounting


scheme allowing to study the
nanomechanical properties
(a) at the core and (b) at the
cylindrical surface of the Figure 2 Load displacement curves for LGS and LS2 Figure 3 LGS sample: Hardness and Reduced Modulus
sample as a function of contact depth measured at core and
cylindrical surface

Figure 4 (a) Topographic (b) gradient in-situ SPM images of the Figure 5 (a) Topographic (b) gradient in-situ SPM images of the LS2
LGS
For further details reach sujit@industronnano.com , +91-7902516561

THANK YOU

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