Specific Process Knowledge/Characterization/XRD/SLSII analysis: Difference between revisions

'''Packages''' available for data treatment are listed below. Each package is named by the measurement type.  

'''Help functions''' included in the program usually give a good overview of the options available when setting up fitting. You can access the relevant help sections by clicking on the small question mark in the pane you want to know more about. The exception is that due to a bug the question-mark-click-for-help function does not work in the software in the cleanroom, but it should work on your computer. If it doesn't, you can find the full help documents on the Cleanroom-drive - ask staff for details.

# Load data:

# Load data:

The texture plugin is used for Pole Figure analysis and Orientation distribution functions (ODF). However we do not have a license for ODF. To enable Orientation functions to be calculated 2 or more pole figures are needed. The texture plugin has two types of calculations, a Defocusing project and texture calculation. The defocusing project will not be discussed here, as it is not strictly needed for the texture calculation, however the idea with this is to measure on substrate with randomly distributed crystals and subtract this from the oriented texture data.

A texture calculation processed as follows:

*Load data:

**Choose one or more pole figure data sets to load.

*Load defocusing project:

**This is only possible if a randomly oriented sample has been measured.

*Configure sample:

**Set the material and the reflections that have been measured.

**Extra reflections and materials can be added by the add reflection and add phase tools.

**Also connect the reflections to the correct pole figures.

**When all materials and reflection is set, press Estimate 2θB, to calculate the 2θ angles.

*Make pole figure corrections:

**Activate and change the settings of the preferred corrections in the right panel.

**Apply the corrections

**To read out the result, click on orientation function at the lower pane.

For more information on how to use the Texture plugin, read the manual by clicking on the ? in the software or from [http://labmanager.dtu.dk/view_binary.php?fileId=4244 LabManager] - requires login.

The use of the plugin for basic analysis is as following. The walk-through is written for the RIR Quantification flow; if only Search/Match is wanted the evaluation flow has the same steps except the RIR part:

*Load data:

** Data from XRD Powder has to be converted to .asc or .xy before load.

*Peak evaluation:

**Choose the settings for the peak search and profile fitting

**Press Run

*Phase identification:

**To search for the peaks, press Search/Match in the left window.  

**One of the best ways to limit the amount of data found is to use the element filter.

**Material can be set to unknown, not included, included, or include one at least by clicking on the materials several times.

**When the material filters are set correctly press run to search the database (''see link above on how to add reference spectra to the database from the ICSD)''.

**The found candidates are listed in Phase identification window. The candidate with the smallest FOM/F20 is the most likely candidate to be present in the sample.

**Always use the prior knowledge of the sample to evaluate the outcome of the search.

**The found results can be moved to the candidate phase list, for use in RIR quantification.

**Press set above the candidate phase list before moving on.

For Reference Intensity Ratio (RIR) chose the RIR Quantification flow, which add the following step to basic evaluation.

*Configure RIR quantification:

**Chose the Miller indices to user for RIR.

**You can then right click on the dataset below the RIR Quantification window and click chart to see the distribution of the phases.

For Crystallite size and strain the first steps are the same as for Search/Match evaluation and the following is added.

*Configure size & strain:

**Select the dataset to analyse.

**Select or deselect peaks that are to be used or not for the calculation.

**Select the analysis method.

**Select 'Use e.s.d. for weight factor' (estimated standard deviation).

**Chose if width corrections is to be used.

For Lattice parameter refinement, follow the steps for search and match. After phase identification do the following.

*Configure lattice parameter refinement:

**Select the dataset to analyse.

**Select or deselect peaks that are to be used or not for the calculation.

**Select the Angular correction to use.

For crystallinity calculation, follow the steps for search and match. After phase identification the following steps are needed.

*Confirm crystallinity:

**Decide whether to include background.

**Chose if a line should be subtracted from background.

**Select the target crystalline phase.

For more info on these see the manual by clicking ? in the right panel for the plugin (Crystallite Size and Strain, Lattice Parameter Refinement, or %Crystallinity) or in [http://labmanager.dtu.dk/view_binary.php?fileId=4247 LabManager] - requires login

The materials manager is used for adding crystal structures and amorphous material parameters for use in data simulation. For some users the compounds are of most interest, as it is in here that you can generate materials like In(x)Ga(1-x)As. Materials not listed can be added by either importing a cif file or defining it by hand. I (Kristian Hagsted) have found the homepage [http://materialsproject.org/#search/materials Materials Project] helpful; see also [http://labadviser.nanolab.dtu.dk/index.php/Specific_Process_Knowledge/Characterization/XRD/XRD_Reference_Data this page] also linked to above on how to look up or add reference spectra from the Inorganic Crystal Structure Database (ICSD) (for DTU users and others with access to the ICSD).

For information about how to use the plugin please look in section 3.2 in the manual opened by clicking on the ? in the software to right corner or from [http://labmanager.dtu.dk/view_binary.php?fileId=4246 LabManager] - requires login.