XRD

What is XRD?
8 Reasons to use XRD
Theory of Diffraction
Periodic Table
X-ray Diffractometer
What is a Powder
Diffractogram?
Factors influencing the quality
of a powder diffractogram
Analysis of Data
Safety
Applications of XRD
Sample Preparation
 • Powder: loose agglomerate of
Sample Preparation small particles, typically less
than 0.5 μm in diameter
• Solid (bulk): Compact piece of
material (stone, coin or pellet)
• Thin Film: Very smooth (shiny
polished surface) coating of less
than 100 nm (inorganic
materials) or less than 300 nm
(organic materials). Otherwise,
they are to be treated as
smooth bulk materials. Sample
coating thickness must be
below 100 nm.
Small Sample (usually less than 0.5 g)
• Use flat surface of glass sample holder
• Place 1 drop of nail polish onto sample holder
• Add half-filled micro spatula with sample to nail polish.
Sample amount should not be larger than the amount of
nail paint
• Use spatula to mix and spread sample to a thin layer over
the sample holder
• Sample and nail paint should be thoroughly mixed and
spread over a larger area
• The dispersion of the sample particles in a highly viscous
liquid like nail paint prevents preferred orientation.
• Let it dry
• Use acetone to remove sample
Large Sample (usually more than 0.5 g)
• Scrap some powder
• Deposit into the depression of the sample holder
• Collect powder in the depression
• Spread powder sample evenly with glass slide

*Notes: (1) surface should be even and smooth, (2)

sample height should match sample holder height,
(3) excessive polishing is not good
Large Sample (usually more than 0.5 g)
For air-sensitive samples (preparation speed
matters)
• Use cello-tape to protect sample from moisture
and air. This method is only suitable for mildly air
sensitive sample
• Cello-tape is used as it does not affect diffraction
peaks of its own other tapes, other tapes should
be tested prior to the experiment
Large Sample (usually more than 0.5 g)
For air-sensitive samples (preparation speed
matters)
• Use cello-tape to protect sample from
moisture and air. This method is only
suitable for mildly air sensitive sample
• Cello-tape is used as it does not affect
diffraction peaks of its own other tapes,
other tapes should be tested prior to the
experiment
Large Sample (usually more than 0.5 g)
Grind: For soft brittle and relatively homogenous sample
• Scoop some powder, use agate mortar if available (ceramic
mortars tend to contaminate sample by abrasion)
• Deposit sample in mortar
• Crush sample with circular rolling motion when grinding the
specimen. The sample should be crushed rather than
smeared (Smearing breaks down the crystal structure
particularly in soft organic samples).
• Place metallic balls into the vial
• Tighten the vial
• Loosen the clamp
• Place the vial in ball mill
• Tighten the clamp
• Close the cover of the mill
 • Bulk sample holder is required since both
upper and lower side of the sample mould
Crystallite Shape need to be open (bottom up)
• Place bulk sample holder onto glass slide with
engraved dot facing down
• Deposit powder into hold, fill sample mould
completely
• Seal the sample hole with cello tape to
prevent the sample from falling out of the
sample mould
• Flip both glass slide and sample holder
• Slide off the glass slide. Slide off carefully to
prevent polishing effect
Solid (Bulk) – Rough Sample: Course,
uneven surface
• Polish with sandpaper and followed by fine polishing using 3 micron
diamond paste.
• It is not necessary to fine polished until mirror like surface.
• Use bulk sample holder to secure sample.

Solid (Bulk) – Smooth sample

• Smooth (at best polished), even surface
Thin Film
Test 1
• 60% (Wrong 8 questions)