NANO INDENTATION

TECHNIQUE
Presented by – Manvir (16108029)
Major (16108032)
Rima (16108085)
Vageesha (16108086)
What is Nano Indentation?

 Nanoindentation is a variety of indentation hardness tests applied to small

volumes(Nano scale). Indentation is perhaps the most commonly applied
means of testing the mechanical properties of materials
 The nanoindentation technique was developed in the mid-1970s to measure
the hardness of small volumes of material.
 Indents are extremely small.
 Loads applied and the tip geometry are much smaller.
Macro/Micro Indentation vs Nano Indentation

 In a traditional indentation test (macro or micro indentation), a hard tip

whose mechanical properties are known (frequently made of a very hard
material like diamond) is pressed into a sample whose properties are
unknown.
 Nanoindentation improves on these macro- and micro-indentation tests by
indenting on the nanoscale with a very precise tip shape, high spatial
resolutions to place the indents, and by providing real-time load-
displacement (into the surface) data while the indentation is in progress.
Why Nano-Indentation?

 Macro indentation test only gives us a property of the bulk.

 But, with Nano-indentation properties of individual phases can be extracted.

 Features less than 100 nm across, as well as thin films less than 5 nm thick,
can be evaluated.

 Mechanical properties of thin films, coatings and small volumes can be

learned without any substrate effect.
NANO-INDENTATION TECHNIQUE
 Nano-Indenting is performed in conjunction with atomic force microscopy
(AFM). The area for testing is located by AFM imaging, and indentations and
scratching marks are imaged by AFM after testing. A three-sided, pyramid-
shaped diamond probe tip is typically used to indent, scratch and image the
sample.

 For indentation, the probe is forced into the surface at a selected rate and to
a selected maximum force. In scratching, the probe is dragged across the
sample surface. The force, rate, length and angle of the scratch is controlled.

 A force-displacement curve obtained during indentation also provides

indications of the sample material’s mechanical and physical properties.
INSTRUMENTATION

 The nanoindentation instrument should be insulated against temperature

variation, vibration and noise in normal laboratory conditions. A specially
designed enclosure designed to reduce thermal and electrical interference to
a minimum is usually supplied by the manufacturer as part of the installation.

 The loading column and base of a nanoindentation instrument should be

heavy.

 Specimens are typically mounted on a metal base with wax or mounting

adhesive.
Experimental Setup
BERKOVICH INDENTER

A=24.56h2
BERKOVICH INDENTER
 Three-sided pyramid which is geometrically self-similar.
 The popular Berkovich now has a very flat profile, with a half angle of 65.27
degrees, measured from the axis to one of the pyramid flats.
 Deeper penetration > 50nm
 Tip radius : 40-100nm
ENGINEERING SAMPLE PREPARATION
1. TEST AREA
 When performing nano indentation, it is critical to note which area was
tested, as chemical composition and thus material properties may vary
between regions within the same sample.

2. SAMPLE PREPARATION
 Larger specimens may be tested if they are properly mounted. The surface of
the specimen must be free from grease, finger prints, dust, and preferably
free of oxide layers.
 Any polishing compound residue will have to be completely removed. Even
washing with acetone can sometimes leave an oily film on the surface which
will affect the results.
2. SPECIMEN MOUNTING
 A specimen is mounted onto a hardened base or specimen mount using a very
thin layer of glue.
 Holding devices such as magnets, vacuum chucks or spring clamps may be
used.
 If a polishing technique is employed to prepare a surface, the properties of
the surface material may be altered . Indentations placed on scratches,
inclusions, or voids will give unpredictable results.
 A heat softening glue such as “Crystal-bond” is suitable for specimen
mounting but it is important to ensure that the specimen makes good
mechanical contact with the mount, and that the glue only fills in the
asperities in the contact surface. If too much glue is used, the glued joint will
affect the results.
PROCEDURE

 Berkovich indenter is forced into the specimen at the selected location.

 The load and displacement of the indenter are recorded during loading and
unloading.
 Loads used in this technique is 1nN to several Newton.
 The depth varies between several tens of nanometer and several micrometer.
 The principal mechanical property determined in indentation test is hardness
H.
 Obtained P-h curves are used to calculate the nano-mechanical properties of
the thin film or coating.
 Repeat the experiment at least 25 times on each phase to obtain the reliable
data.
Load- Displacement Curve
Mechanical Properties measured using Nano-Indentation

 Hardness (H)
 Stiffness (S)
 Young’s Modulus (E)
 Strain Rate sensitivity index (m)
 Elastic and Plastic work/ energy of the deformed material
Mechanical Properties measured using Nano-Indentation

 Stiffness (S): Stiffness of the contact is given by the slope of the unloading
curve, dP/dh

 Young’s Modulus:

 Strain Rate Sensitivity: It can be found by determining the flow stress and
strain rate produced during indentation

 Elastic/Plastic Work: By calculating area under the Load-Displacement curve.

APPLICATIONS
 Nano indentation has been utilized in many, many different research areas
for evaluating mechanical properties of bulk nanostructured components. In
specifically for microelectronic mechanical systems or nano electronic
mechanical systems, biosensors even tissue engineering.
 Also, to utilize mechanical properties of finding mechanical properties of
carbon Nano tube based composites.
 We can also see what is the role of particular phase or particular grain or
particular precipitate in dictating the overall mechanical property.
 Nanoindentation can be used for determination of local properties of
homogeneous as well as heterogeneous materials.
Applications
Metallurgical Study of Multiphase Material Using Nano-Indentation

 Advanced materials often contain multiple phases in special

microstructure and texture to achieve desired mechanical properties
for target application in industrial practice. Nano-indentation is
widely applied to measure the mechanical behaviors of materials at
small scales.
 However, it is challenging and time-consuming to precisely select
specific locations for indentation in a very small area. A reliable and
user-friendly procedure of Nano-indentation testing is in need to
determine the mechanical properties of different phases of a material
with high precision and timely measurement.
Applications (contd.)
 In this application, Nano-indentation equipment is used to measure the
mechanical properties of multiphase metallurgical sample.
Applications(contd.)
 Load-Displacement curves of Nano-indentation
Other Applications

 Shape Memory Alloy

 Carbon Nanotube based composites
 Thin Film Testing
 Scratch Testing
 Soft Films (paints)
Advantages

 High accuracy
 A number of mechanical properties can be studied
 Properties of coatings can be learned without substrate affect
 Real-time data can be generated
 Easy to use equipment
LIMITATIONS

 Conventional nanoindentation methods for calculation of Modulus of elasticity

(based on the unloading curve) are limited to linear, isotropic materials.
 While nanoindentation testing can be relatively simple, the interpretation of
results is challenging. One of the main challenges is the use of proper tip
depending on the application and proper interpretation of the results . For
examples - Berkovich tip is very good for metal and ceramics.
 Nanoindentation of soft material has intrinsic challenges due to adhesion,
surface detection and tip dependency of results. There is an ongoing research
to overcome such problems.
 The stiffness( in case of soft materials ) should be accurate of the machine if
the stiffness is too high it will run through the sample and if its too low then
it will not make the proper indentation.
References

 Principle of Nano-Indentation by Prof. Do Kyung Kim

 Nanomaterials Characterization by Prof. Kantesh Balani (IIT-K)
 https://hal.archives-ouvertes.fr/hal-00826308/document
 https://www.azom.com/article.aspx?ArticleID=5426
THANK YOU