XRD data analysis in SmartLab Studio II

SmartLab Studio II is an integrated software package, combining all the functionality previously available in SmartLab Guidiance, GlobalFit, PDXL, 3D explorer, and DataMapper. When SmartLab Studio II is installed on your personal computer, you will have access to all the data analysis tools, but not the machine control.

The licenses for the software are floating network licenses, and hence you shall close the software when you are not using it. User management and data transfer can be done by connecting to the SQL server ,as described in [XRD/software]. If connected Data will be stored on the SQL server and be available on any computer.

The different packages available for data treatment is listed below. Compared to the old software it is more intuitive, as the package is in general named by the measurement type. The help functions included in the program in general gives a good overview of the options available when setting up fitting, please use them by clicking on the small question mark in the pane you want to know more about. XRR

Gaining information about thin films with X-Ray Reflectivity, does like ellipsometry require some prior knowledge of the sample. In SLSII you create a layer structure with initial parameters. Then the software will fit the generated model to obtain the thickness, roughness, and density of your layers.

Load data:
Configure sample model:
- Set substrate material and initial values.
- Add layers. Consider adding interface layers like native oxides.
- Set layer materials and initial values.
- Define Graded Layers if any.
- Define Super Lattices if any.
- Link layers, formula is of the type th[1], for linking thickness to layer L1.
Oscillation analysis (optional):
- Run Analysis.
- Look over the list of Residual oscillation components.
- Check if the number of layers and the thickness are as expected.
- If acceptable, Optimize and Apply Sample.
Set simulation parameters
- Check the Horizontal axis angles, to exclude the noise tail from the fit.
- Consider to auto transform the Horizontal and Vertical axes.
Set fit algorithm and Run Fit
- Select the Fit method, Generic Algorithm is for global optimization, while the two others are local optimizations.
- Change fit method parameters and settings as needed.
- If wanted set an instrumental function in the tab below the fit parameters window.

For more information on how to use the XRR plugin, read the manual by clicking on the ? in the software or from labmanager.

HRXRD

The HRXRD package is used for analysis of crystalline materials. It can be used to derive information about crystallinity, strain, composition, and thickness. Meaning that HRXRD are used with rockingcurve and reciprocal space mapping data. Like the XRR plugin, the flow is to load data, generate a model of the layers, simulate initial parameters, and finally fit the to the data.

Three modes are available for Rocking Curve analysis: Evaluation and Fit, Evaluation, or Fit. The procedure differs only slightly from one to the other

Load data:
Configure sample model:
- Set substrate material and initial values.
- Add layers. Consider adding interface layers like native oxides.
- Set layer materials and initial values.
- Define Graded Layers if any.
- Define Super Lattices if any.
- Link layers, formula is of the type th[1], for linking thickness to layer L1.
Set peak parameters and Evaluate:
- Associate peaks with layers or substrate.
- Select if the peak is a Bragg Peak or a Harmonic peak.
- For Harmonic peaks chose the harmonic order.
- When done press Evaluate to update fitting parameters.
Set X-ray parameters:
- Check values for wavelength and reflection.
Set simulation parameters:
- Select the scan type and the range for simulation.
- Click Auto in Horizontal transform to align the offset in 2θ.
- In Vertical transform, chose the background type and click auto to add a background function to the simulation.
- Optional add the some of the values as fitting parameters.
Set fit algorithm and Run Fit
- Select the Fit method, Generic Algorithm is for global optimization, while the two others are local optimizations.
- Change fit method parameters and settings as needed.
- If wanted set an instrumental function in the tab below the fit parameters window.

For RSM data analysis use the RSM flow in the HRXDR plugin.

Load data:
- On the chart toolbar, plot options can be change, of note it is possible to change between angular and reciprocal space coordinates.
Smoothing and background subtraction:
- The data can be smoothed, by weighted average of nearby neighbors.
- Background subtraction either in the form of a fitted background or a constant value is possible.
Search peaks
- Chose the settings for peak search.
- Verify the Peaks for Evaluation list.
Configure sample model:
- Set substrate material and initial values.
- Add layers. Consider adding interface layers like native oxides.
- Set layer materials and initial values.
- Define Graded Layers if any.
- Define Super Lattices if any.
- Link layers, formula is of the type th[1], for linking thickness to layer L1.
Generate hkl:
- Set the rotation angle, ϕ, of the substrate.
- Set the tilt of the substrate, χ, for an in-plane measurement, it is called 2θχ.
- Adjust the other parameters as wanted.
- Press generate hkl.

For more information on how to use the HRXRD plugin, read the manual by clicking on the ? in the software or from labmanager.

Texture

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 random distributed crystals, and substract this from the oriented texture data.

A texture calculation processed as follows:

Load data:
- Chose 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 labmanager.

Powder XRD

For powder analysis licenses for Search/Match and Comprehensive analysis are available for SmartLab Studio II, if something more advanced, like Rietveld (WPPF), is needed please use the software from HighScore from Malvern Panalytical, which is available in the equipment room 346-904, or as a remote session for one user at a time.

If only a simple analysis of the data is needed, please follow this guide to use SmartLab Studio II on you own PC. To convert data from XRD Powder to enable loading in SmartLab Studio II please look here.

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:
- Chose 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.
- 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 comprehensive analysis, in the task drop down menu in the flow bar select Comprehensive analysis. Three flows are available here, Crystallite size and strain, Lattice parameter refinement, and Crystallinity.

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

Data Visualization Data Manager Logging User Manager DB Manager Materials Manager