INDIAN INSTITUTE OF TECHNOLOGY KHARAGPUR

DEPARTMENT OF METALLURGICAL & MATERIALS ENGINEERING

Subject: Materials Characterization (MT 31 012)

Spring Semester End Term Exam, 2012-13 3rd Yr. B. Tech. (H)/Dual Degree Date: 15/04/2013 2-5 pm
Time: 3 hrs. Full Marks: 100 No. of Students: 125
Instructions:
• Answer ALL THE QUESTIONS.
• Show your working and reasoning carefully for credit. Draw schematic diagrams wherever necessary.
• Points for each question are written below.
• Use of books, notes, laptops and cell phones are prohibited. Onlycalculators are allowed.
Part -I
1. Fill in the blanks with appropriate word/s.
i. The 2"d phase distribution in a two-phase material with absolutely zero surface asperity where the
average size of the second phase in 50 nm can be imaged in AFM using mode.
ii. The average of the work functions of the tip & sample material in STM is called _ __
iii. The work function is the minimum energy needed to move an electron from the into
vacuum.
iv. Topographical imaging of a multiphase sample surface is possible by STM using mode.
v. One of the methods of fabricating the atomically sharp tip for STM study is _ __
vi. crystals are used for generating monochromatic X-Ray in XPS.
vii. analyzer detector is suitable for AES.
viii. is the distance where about 63% of the particles have been stopped.
ix. A dwell time is allowed at peak load during nanoindentation to remove the influence of _ __
x. The unloading portion of the load-displacement curve in nanoindentation is used as this portion
represents the of the material being tested.
xi. The thermal drift is ___ in electrostatic force actuation than electromagnetic force actuation in
nanoindentation.
xii. The continuous stiffness measurement during nanoindentation is accomplished by imposing a
small, varying signal on top of the DC signal that drives the motion of the indenter.
xiii. The anode materials for X-ray generation in XPS are generally _ __
xiv. The binding energy of an element in oxide form is than that of elemental state.
xv. In type DSC the temperatures of the sample and reference are controlled independently
using separate furnaces.
xvi. The crystallization behavior during thermal transition of a crystalline polymer is reaction in
nature.
xvii. The of a DSC curve decreases with increasing sample size.
xviii. Holding the indenter after 90% unloading during nanoindentation is done to rectify the _ __
xix. The applied load in a nanoindenter via electrostatic force actuation is proportional to ___.
xx. Using He is better than using N2 as the quenching gas during cooling the sample being tested in
dilatometer as He's is better than that of N2 .
20*1

1
2. Answer all the following questions in not more than one or two sentences.
i. The mass of the cantilever probe in an AFM should be of minimum value. Explain in terms of
spring constant (k) and resonant frequency (11).
ii. In STM, the lateral resolution is about 1A whereas a vertical resolution up to 0.01A can be
achieved. Why?
iii. The plastic deformation of the indenter is immaterial in nanoindentation result. True or false?
Explain.
2
iv. The projected area of an undamaged standard Berkovich tip is 24.56 h . Show your calculation.
v. Investigation of fatigue behavior is possible by quasi-static nanoindentatkm. Provide schematic in
support of your answer.
vi. Why does ultra high vacuum atmosphere required for operation of XPS and AES?
vii. Which characterization technique of the following two is suitqble for studying the oxidation kinetics
of a Cu thin film of 115 nm thickness and why? (I) EPMA, (II) XPS.
viii. Cylindrical mirror analyzer detector is suitable for XPS. True or false? Explain.
ix. Resolution of DSC curves improves with increasing heating rate. True or false? Explain.
X. Draw the top view (only) of a piezo-electric scanner with the capability of X-Y-Z direction
movement in an AFM.
10*2

3. Neatly draw and label the schematics of the following phenomena I set-up I mechanisms. No
explanation is needed.
i. The three different modes of operation in the force-displacement curve in AFM (Atomic Force
Microscopy)
ii. Quantum tunneling effect in between the probe and sample in STM (Scanning Tunneling
Microscopy)
iii. Jump-to-contact method for manipulating individual atoms or molecules on a substrate surface and
directing them continuously to predetermined positions by STM.
iv. The operation of three-plate capacitive transducer at rest and with load applied in a nanoindenter
v. Force vs. displacement curves during nanoindentation for (a) a low carbon steel, (b) Teflon and (b)
crystalline silicon
vi. The ejection of photoelectron and Auger electron from an atom structure in X-Ray Photoelectron
Spectroscopy (XPS) and Auger Electron Spectroscopy (AES)
vii. Difference between XPS spectra using monochromatic and non-monochromatic X-ray.
viii. Differential Scanning Calorimetry (DSC) curves for 5 grams and 10 grams lead from room
temperature to 500°C at constant heating rate of 10°C per minute.

8*5
Part -II
1. Give a schematic diagram of the instrumental set up of an atomic absorption spectroscopy.
Mention the various parts present there in the whole set up of the instrument (spectroscopy).
2. Draw the interaction volume and show the various signals coming out from the interaction volume
during electron-specimen interaction in a scanning electron microscope.
10*2