NATIONAL INSTITUTE OF TECHNOLOGY ROURKELA

MID - TERM EXAMINATION, 2016

SESSION: 2015 2016 (Autumn)
B. Tech. 5th Semester

Subject code: CR-311 Subject Name: Instrumental Characterization Dept. Code: CR

No. of pages: 2 Full Marks: 60 Duration: 2h

Figures at the right hand margin indicate marks.

All parts of a question should be answered at one place.
Q.No. Particulars Marks

1. (i) What are the conditions for diffraction? What type of information do 2
you get from Moseleys law?
(ii) Which of these is not involved in the diffraction of X-ray through a 2
crystal? (a) Electron transition (b) Crystallographic Planes (c)
Nuclear interaction (d) Constructive interference.
What is the short-wavelength limit of the continuous spectrum
emitted for an X-ray tube operated at 50,000 volts?

(iii) What is the role of a filter in X-ray? Which filter material is used for 2
a Copper target and why?
(iv) Why the thermocouples are made up of two dissimilar metals? 2

(v) Why DTA, TGA and Dilatometer are useful for practical applications? 2
Explain each in brief.
(vi) Why intensity of (111) reflection will be 4/3 that of (100) reflection? 2

2. (i) Sketch the cooling curve of pure aluminium (Al) as it is cooled from 3
750 C. Given Melting point = 660 C. How would the DTA plot look
like?
(ii) A FCC crystal of iridium (Ir) is analyzed by x-ray diffraction through 3
exposure to molybdenum (atomic number 42) K radiation, for
which K = 0.721 . Calculate the angle of reflection, , of the
lowest-index plane. If you want to increase the angle, would you
replace the Mo target with a silver (Atomic number 47) target or a
copper (Atomic number 29) target? Explain the reasoning behind
your choice. The lattice constant of Ir, a, is 3.84 .
(iii) A glass-ceramic sample undergoes a heat-treatment from room 3
temperature to 1000 C. The following thermal event took place: (i)
glass-transition (at 250 C), (ii) crystallization (at 350 C), (iii)
polymorphic conversion (500 C) and melting (at 950 C). Draw
DSC curve of this glass-ceramics. [Al2O3 is used as a reference
material]
 (iv) Draw DTA curves for hydrated calcium oxalate (CaC2O4H2O) in the 3
presence of oxygen and nitrogen atmosphere. The following thermal
events are known to occur between 30C to 1000 C. (i) The
removal of adsorbed water took place at ~200C; (ii) calcium
oxalate converted to calcium carbonate at ~500 C and conversion
of calcium carbonate to calcium oxide took place at ~900 C.
(v) Justify that the second order diffraction from (110) plane [3]
superimpose on the first order diffraction from (220) plane.
(vi) Define sequential s value for FCC cubic cell using structural factor. [3]

3. Calculate the breadth B (in degrees of 2), due to small crystal [5]
effect alone, of the powder pattern lines of particles of diameter
1000 . Assume = 45 and = 1.5 ?

4. Fine Calcium carbonate powders are heated from room temperature [5]
to 1000 C at a heating rate of 10 C/min in a DTA instrument.
Show DTA curve in this range if the calcium carbonate powders are
tight packed in one case and loose packed in another case. [Assume
alumina is used as reference material].

5. The X-ray analysis of a crystal is made with monochromatic X-rays [5]

of wavelength 0.58 . Braggs reflections are obtained at angles of
6.45, 9.15 and 13. Which is the angle represents second order
reflection and calculate the interplanar spacing of the crystal.

6. How X-rays are produced? Briefly describe the continuous and [5]
characteristics lines spectrum?

7. How heating rate (2, 5 and 10 C/min) effects the shape of melting [5]
in a heat-flux DSC? Explain.

8. For an unknown cubic metal the diffracting angles (), obtained with [5]
Cu-K radiation ( = 1.541 ) are: 13.70, 15.89, 22.75, 26.91,
28.25, 33.15, 36.62, 37.60 and 41.95. Determine the
structure, lattice constant a and atomic radius for this metal.