Steps to be followed for x-ray diffraction measurements.

Find the launch icon for starting the “ xpert data collector” from the desktop.
The user name is : xrd
Password is : xpert

After logging into the data collector you see a blank window as shown above.
In order to start any measurements you have to choose the optics( what type of
monochromator , and the type of detector)
We have
3 different monochromators.
(1) 4 crystal – used for high precision measurements. You will recognize it from the
picture of 4 crystals on top of the monochromator. From this you get a highly
monochromatic Cu Kα1 radiation. But it is at a cost of intensity.
(2) hybrid mirror: it is used for analyzing samples which are thin and have poor
crystalline quality. It is also important for measuring the nitride thin films in the
asymmetric mode.
Please note: handle this optics carefully. It is both extremely costly and sensitive.
Also be careful with the wire attached to the beam attenuator placed in front of this
monochromator.
(3) This is more of a slit rather than a monochromator. It should be used for reflectivity
measurements. The x-ray beam out of this monochromator is not pure (Kα1, Kα2 and kβ
components are still present. Secondly the intensity is also very large. you should be very
careful when using this with the normal detectors, as the intensity of the beam is high and
might damage the detectors. Use Al foils to reduce the intensity which can be removed
during measurement.

Detectors
(1) optics 1--- this is to be used with any of the monochromators.
This arrangement is also called triple crystal arrangement. This uses an analyzer
crystal to reduce the diffuse scattering. This is the perfect or theoretical method to
evaluate the crystalline properties. However there is a huge loss in intensity when
using this optics. Hence use it only when the films are thick more than 1 micron and
of good quality.

(2) optics 2 this is typically used for routine measurements. The diffracted beam is
collimated using a slit- usually we use 1/8 slit.

(3)------ this detector is used for reflectivity measurements.

Loading the sample

Load the sample and align it to the center on the x-ray beam ( changing x, y) using the ( ).
change psi from 90 to 0 ( so that the sample is in the vertical plane)

using hybrid and optics 1.

-> TO MAKE THE SAMPLE PARALLEL TO THE X-RAY BEAM

make the detector to see the max intensity:
measure -> manual scan-> 2theta scan
Make a 2theta scan in the range .4 to 1 degree.
Move the goinometer to the max position. Note the intensity at this position

Increase the Z position so that the sample blocks half the intensity
Slowly increase the value of z so that the intensity is reduced to slightly less than ½ I
Now do an omega scan ( range = 1 degree) and move the goniometer to the max intensity
positon
Then finally adjust the value of Z to half intensity value.

Now the sample is aligned for diffraction.

Depending on the sample you need to measure get the corresponding 2theta , omega
values from the instrument settings window.
Make sure that the value of psi =0 and phi ~30. ( for symmetric reflections)
Move to the new position
Make the scans in the following order
Omega scan ( range 1 degree)
Psi scan ( range 8 degrees)
Repeat the above 2 scans until u are satisfied with the shape of the omega scan
( note omega scan will be pretty in linear scale and
2theta- omega scan will be good in a log scale.)

2theta scan ( range 1 degree)

2theta omega scans ( 1 degree or more depending on the sample)

Note: all are the above scans are rough scans and can be done with a time step of 0.5 sec
or .25 sec
For the final scan choose the desired range, and with a step of 4 – 5 sec.
Make a new 2-theta omega scan
And a omega scan.