1. Examples of our own Tricks

2. Tools Microscope Razor blade Spatula Mortar & Pestle
Zero background holder
Microscope slide
2 sided tape
Camel hair brushes
Hydrochloric Acid
Nitric Acid
Sodium Hydroxide
Metal File
Dental Pick
Dissection Kit
Vaseline
Apiezon Grease
Mylar (polyester)Film
Kapton (polyimide) Film
Hammer
Rubber Mallet
Tim

3. Sample Holder for Foils
Denver X-Ray Conference, 2002
Sample Holder for Foils
To reduce the background scattering from the glass wall, powdered samples are also dusted on thin foils and fixed by a light touch of hair spray.
We use 15 μm sheets of Hostaphan or 6 μm sheets of Polypropylen or 3 μm sheets of Mylar.
The foil is held by Vaseline on the sample holder, and is also suitable for fixation to goniometer heads as well as to metal pegs. In this picture the sample holder is fastened on a goniometer head.
This image represents the diffractogram of a suspected white specimen, which was sent by mail after the attack on the World Trace Center.
We could identify Sucrose and Gypsum.
Preparation of Small Amounts of Powder on a Sample Holder with a 3 μm Sheet of Mylar
Tim

4. Pt/Rd Mesh, High Temperature Mount
Use Mesh
Room Temp
450 C
AXA, Vol. 25, pp
Mount on Goniometer

5. An example of preferred orientation: Palmierite, K2Pb(SO4)2As
prepared
Annealed
Oriented
Random
1mm
1mm
K2Pb(SO4)2 unit cell:
Hexagonal
a = 5.5 Å
c = 20.8 Å
c-axis
Typical as-prepared grain
shows plate-like morphology
Tissot et. al. (2001) Powder Diffr
Mark

6. The ‘As-prepared’ sample showed c-axis preferred orientation
while the ‘Annealed’ sample was much more random.
(003)
(101)
(012)
(104)
(006)
(015)
Two-Theta (degrees)
Calculated
From
Annealed
As-prepared
Intensity (arb. units)
Too high!
Good!
Tissot et. al. (2001) Powder Diffr
Mark

7. Reactive samples: “baggie technique” for Li-ion battery anode
Prepare reactive samples using inert atmosphere (e.g. glove box)
Place prepared specimen in polypropylene (or polyurethane) baggie ~25 mm thick
Evacuate baggie of Ar gas with hand-pump and seal baggie using “seal-a-meal”
 inexpensive, no modification of XRD instrumentation
 tends to leak so run soon after prep, will get plastic peaks in pattern
Prepared specimen in
Baggie awaiting XRD
Plastic bag peaks
LiC6
(001)
LiC12
(002)
Graphite
Mark