QPA Training
QPA Training
QPA Training
Here are the instructions to perform a Rietveld quantitative analysis on a ZrO2/Al2O3 powder
sample using Maud.
Version 2.03 (released September 12, 2005) or higher is needed for this tutorial.
The spectrum for the analysis has been collected using a standard Bragg-Brentano diffractometer
and the data file is located in the datasets and examples directory of Maud (the one created by you
at the first run of the program). The procedure will start creating a basic analysis file setting up the
datafile and the two phases to analyse. We will build this analysis file in two steps:
• Step 1: load the datafile
• Step 2: load and modify the phases
Once defined the analysis file, we will start the analysis following two steps:
• Step 3: set up some "visible" parameters (specifically, the T-PSZ cell parameters)
• Step 4: refine the spectrum by the wizard
The final step (Step 5) will show the analysis output to the user. The tutorial will also guide the user
to a more accurate and precise analysis if some parameters were not as expected.
The tutorial has been added by several figures to help the novice in figuring out easily the basic
procedure to perform this kind of analysis.
Well, try this tutorial and e-mail us for any problem or question (luca.lutterotti_at_unitn.it).
You may zoom in the spectrum plot in some details by click, old and drag the mouse over the
window part you want to zoom in. Double clicking the plot reset the zoom to the normal. By right
clicking on the plot (CTRL+click, if you have a one-button mouse) you have a small context menu
for manual zooming or get a coordinate window. Pressing the Plot options button you gain control
over some plot characteristics.
We do not need to modify the Instrument (inside the dataset) as the one loaded by default is a
Bragg-Brentano with the correct instrumental aberrations for this data file.
Before to proceed with Step 2 (load and modify the phases) we save this analysis at the present state
giving it a new name so we can load it again if needed. To complete this choose Save analysis as...
and choose a location (better not inside the databases and examples directory) and a name for the
file. It is advised to use a name with extension .par so in certain system (OS X for example) can be
recognised as a Maud analysis file and double clicking the file, it will be loaded automatically in
Maud.
Building the analysis file (step 2: load and modify the phases)
Select the Phases tabPanel in the main Maud window.
There should be no phases in the list. If any, select it and press the remove button in the toolbar (the
one with a red cross).
Press the Load an object from a (CIF) database or file... button to add a new phase (each button on
the toolbar acts on the selected list and or object/s). Select the database file structures.mdb from the
databases and examples folder. A window will appear where you can choose the corundum (Al2O3)
phase first from the visible listbox (Figure 3).
Figure 5: Pattern computed for the first time based on initial input.
2. The intensity is quite low and the computed spectrum in the high 2θ part does not correspond
correctly to the experimental part (see between 140˚ and 150˚).
3. Zoom in the plot panel in the 70˚-77˚ 2θ region by clicking and dragging a rectangle around the
plot part you want to zoom in. You should see the two peaks of the tetragonal as in the next
figure. The first peak (do not consider the small first one) correspond to the 004 reflection of the
tetragonal PSZ, the second one to the 220. The calculated peaks are instead shifted towards high
angle. This because the cell parameters depend strongly on the Ce content and the phase in the
database has a different Ce content respect to the one in the experimental pattern. We will
change the cell parameters to provide a better starting point (the calculated peaks actually are
too far from the experimental ones; the least square will diverge).
4. Go to the lower panel containing a list (tree) of objects and parameters. Look for the cell
parameters of the PSZ and click on the parameter value of cell parameter a. Like in Figure 6.
Figure 6: Enlarging the pattern in the 70-77˚ region and changing the cell parameter.
Near the value (inside the two arrow buttons) there is a step value. Change the value to 0.01 like in
the picture. Clicking on the left or right arrow buttons you can decrease or increase the value of the
parameter by the step value. The change in the value will be followed by a quick computation and
update of the plot to reflect the change. Try to increase the value of cell parameter a until the
calculated second peak will be under the experimental one. Do the same for the cell parameter c that
will only change the position of the first peak. The final result will be like in Figure 7.
Double click on the plot window to reset the zoom and see the result on the entire spectrum. Now
you can see there is a better correspondence between computed and experimental peaks. The phases
are the correct ones.
The intensity is quite low, so we try to increase it to have a better view. Go again in the lower
parameter panel and look for the Intensity (scale factor) parameter under the Instrument inside the
dataset. Select the value, change the step value to 10 and press the right button few times until you
get an intensity comparable with the experimental one.
Figure 7: Cell optimised manually using the arrow buttons and checking the plot.
5. Look inside the panel. It is useful to have an idea on how the analysis worked out. The most
important parameters are the final Rw and sigma values (Figure 11).
Figure 11: R values at the end of the automatic quantitative analysis.
For this analysis, you should have something like: Rw<15.0 and sig<2.0.
If the values are higher, press again the refinement button (the hammer button on the toolbar) or
choose 'Refinement' from the 'Analysis' menu bar to let the program do some additional refinement
iterations with the last parameters refinable.
Figure 12: Separated plot window, useful for customising and copying the plot to another program.
Figure 15: sample panel showing the volume and weight fractions.
In the main Maud window, select the 'sample' tab panel in the upper-left part of the window. Select
the only sample present there and press the 'edit' toolbar button ('eye' toolbar button). A new
window will appear like in Figure 15. Looking at the picture where the red circle is, you can select
the phase you want and see the volume and phase fractions. Errors are reported only for the refined
phase fraction in the result (Figure 14) or parameter list (Figure 16) windows.
You may check the entire parameter list to see which parameters the program has been set refinable
automatically. TIP: actually the parameter list panel below the plot does not have a button/options to
expand the entire tree of objects/parameters. But if you choose 'Parameters list' from the 'Analysis'
menu bar, the a new window will appear (Figure 16). Enlarge the window by dragging down its
lower/right corner until you will see all the buttons in the lower panel of the window and press the
'Expand all' button near the 'Close' button in the lower-right corner.
Figure 16: parameter list window, you need to press the “Expand all” button to see all parameters in
the tree or expand one by one.