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.

Rocking Curve

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.

Reciprocal Space Mapping

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.

RS viewer

RS viewer is an utility for simulating and viewing the reciprocal space for one or more materials at a time. In the old software this was called 'Diffraction Space Simulation'. The utility is handy for finding 2θ angles, and how to position the goniometer for measuring in screwed geometry. The RS viewer can be opened from either the measurement tan or the HRXRD tab, by clicking the button in at the ribbon.

In the RS viewer it is possible to make a sample model consisting of substrates and a number og layers on to. Unfortunately it is not possible to change the concentrations of different atoms in a composition as it is in the HRXRD sample building. But for each layer it is possible to change sample axis, eg. changing the substrate normal from (0 0 1) to (1 1 1). Using the RS viewer for setting up a Reciprocal space mapping (RSM) are done this way:

Sample:
- Change the substrate to right material.
- Check that 'Normal Sz' under 'Sample Axes' is correct.
- Add layers by right clicking on an existing layer and click Insert New Layer.
- Configure added layer with material and expected orientation.
Measurement:
- Chose the goniometer geometry wanted used in the measurement, often Inplane is wanted to avoid tilting the sample.
- Chose if the reflection is symmetric or asymmetric for Out of plane (ω step).
- Chose X-ray target as Cu-Kα₁.
Reflection information:
- Select the layer for measurement.
- Select the reflection for measurement, either by clicking on the simulation map or by typing in the number. Only allowed reflections in the chosen geometry are shown.
- In the reflection box, infomation about the reflection, like 2θ |F|, |F|² and the incident and reflected angles are listed.
- The five relevant axes for RSM configuration are listed below.
- Numbers at the left side of the slider are offsets needed for the measurement.
- To the right it is possible to chose if the measurement should be done relative to the offset or in absolute values.
- For the relevant axes, the measurement range can be set.
- At the bottom, show area will highlight the measurement area defined, and offsets can be send to the goniometer, while areas can be send to measurement configuration.

For more information please click on ? in the RS viewer window or see 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.

Basic/Evaluation

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.

Basic/RIR Quantification

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.

Comprehensive Analysis/Crystallite size and strain

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 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 LabManager

Comprehensive Analysis/Lattice parameter refinement

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 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 LabManager

Comprehensive Analysis/Crystallinity

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 LabManager

Data Visualization

The data visualization plugin is mainly used to show data mapping, this could be data acquired by the xy-stage. 1D and 2D data is supported, and 1D graphs can be extracted from 2D plots. It further support, smoothing, background subtraction, and peak search for all loaded data sets in one go.

For more information click on ? in the software to right corner or see LabManager.

Data Manager

The data manager can be used for visualizing several datasets at once. As for the data visualization plugin, it support batch processing of data sets. Data comparison can easily be done with data manager, and generate a great overview of differences and similarities between samples. It can also be used to concatenate data from several measurements into one data set, this is useful for data from the XRD Powder.

For more information click on ? in the software top rigth corner of see LabManager.

Materials Manager

The materials manager is used for adding crystal structures and amorphous material parameters for use in data simulation. For most users the compounds are proberly 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 have found the homepage Materials Project helpful. We recommend to download the symmetrized cif file for import. When adding materials please consider if the space group is the correct one. We would also prefer if the elastic stiffness tensor is entered into the software for all materials if available, which they often are on the Materials Project site.

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 LabManager.