Specialized XRD application courses on Empyrean and X’Pert3 Powder (X’Pert Pro MPD)

Specialized courses covering a number of XRD applications from phase analysis to reflectometry and epitaxy; from basic principles to data collection and analysis.

The courses are intended for both new and existing users of Empyrean, X’Pert3 Powder and MRD diffractometers, who want to get in-depth training in special applications and the corresponding Software packages. It is strongly recommended for the new users to follow beforehand the X-Ray Powder Diffraction course, or to have a solid background and hands-on experience in XRD before registering for the Specialized XRD application courses. 

Several different courses are offered in the same week (of which a maximum of 3 can be followed in one week):

• HighScore / HighScore Plus (3 days)
• Texture analysis using Texture software (2 days)
• Residual stress analysis using Stress software (2 days)
• Reflectometry course (3 days)
• Non-ambient XRD with Anton Paar non-ambient chambers (1 day)
• Small-Angle X-ray Scattering (SAXS) (2 days)
• Pair Distribution Function (PDF) (2 days) • Grazing Incidence Small Angle X-ray Scattering (GISAXS) on Empyrean (2 days)
• Computed Tomography (CT) (2 days)

Each course starts with the introduction to the basic principles behind the corresponding technique, followed by extensive hands-on training on the instrument (Empyrean, X’Pert3 Powder or X’Pert3 MRD) and/or corresponding software module to help you to optimize data collection and analysis procedure specific for your application(s). 

HighScore / HighScore Plus

From basics of crystallography via measurement strategies to qualitative/quantitative phase analysis using HighScore Plus.  

This advanced course is intended for both new and existing users of Empyrean and X’Pert3 Powder (X’Pert PRO MPD) diffractometers with a good working knowledge of XRD and preferable experienced with HighScore (Plus). For the new users of Malvern Panalytical XRD systems we strongly recommend first to follow the X-Ray Powder Diffraction course. The main purpose of the HighScore Plus course is to provide you with the roots of crystallography, which gives a solid base for understanding the Rietveld method. Particular emphasis is put on the hands-on training, starting from the sample preparation and data collection strategies on Empyrean or X’Pert3 Powder to the Rietveld refinement of an XRD pattern using the HighScore Plus software package. The ultimate goal of this course is to help you to establish the most optimal strategy for the analysis of your sample(s). Participants can bring their own ‘problem’ files for the hands-on sessions and further discussions.  

Course content

During the course the following topics will be discussed:  
• Measurement strategies and set-up of data collection for crystallography  
• Data treatment:  
    o Preparation of data o Profile fitting  
• Crystallographic symmetry elements, point groups and space groups  
• Crystallographic analysis:  
    o Indexing and unit cell refinement  
    o Theoretical basis of the Rietveld method  
• Rietveld analysis:  
    o Simulations of powder diffractograms  
    o Entering crystallographic data  
    o Refinement of crystal structure data from powder measurements  
    o Quantitative phase analysis  
    o Refinement strategies  
• Optional (on demand, to be agreed in advance)  
    o Quantification of amorphous content  
    o Cluster analysis o Line profile analysis  
    o Structure determination  

Texture analysis using Texture software

The course is intended for both new and existing users of Empyrean and X’Pert3 MRD diffractometers. For the new users the maximum outcome will be gained if the Texture course is taken after the X-Ray Powder Diffraction course. Starting with the basics of texture analysis and overview of the possible instrumental setups for texture measurements, course participants will go through extensive hands-on training covering data collection strategies and data analysis from single pole figure to the calculation of an orientation distribution function (ODF), providing you the most complete information about texturing of your sample(s).  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

Course content

In the duration of the course the emphasis will be placed on the following subjects:  
• Measurement strategies and set-up of data collection for pole figure(s) and background corrections  
• Data treatment: visualization and correction of pole figures  
• Construction of the Orientation Distribution Function  
• Recalculation of pole figures  
• Normalization factors  

Residual stress analysis using Stress software

The course is intended for both new and existing users of Empyrean, X’Pert3 Powder or X’Pert3 MRD (X’Pert PRO MPD) systems. For the new users the full advantage of the course will be gained if the Stress course is taken after the X-Ray Powder Diffraction course. Theoretical aspects of Residual Stress analysis using XRD and discussion of possible measurement geometries and instrument setup will be followed by extended practical sessions. The main purpose of the course is to teach you how to choose and execute the most appropriate measurement type and analysis strategy suitable for your sample, starting from sample alignment, choice of the wavelength and of the peak position to be analysed, optimization of data collection, all the way to the analysis of the results using the Stress software.  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

During the course the following aspects will be covered:
• Fundamentals of Residual Stress evaluation using XRD  
• Measurement strategies and set-up of data collection for residual stress  
• Verification and calibration of the set-up with a stress-free sample  
• Chi-tilt and omega-offset stress methods  

Reflectometry course

This course is intended for users seeking to expand their knowledge on thin film analysis. The course covers basic principles and practical aspects of X-ray reflectometry as well as higher skills to analyze details. To help you to get the best possible result out of your analysis, emphasis is placed on selecting the most appropriate hardware and data collection strategies to match your sample. Epitaxy and Reflectivity software will be used to analyze the reflectivity curves and diffraction space maps collected. Simulation of various example structures will be explained and their nature attuned to the interest of the course participants.  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

The main aspects covered during the course are the following:
• Basic principles of X-ray Reflectometry  
• Hardware components and their impact on data quality  
• Practical aspects of sample alignment procedure and data collection  
• Extracting information from reflectivity curves:  
    o Layer thicknesses  
    o Density  
    o RMS surface and interface roughness  
• Interface morphology from diffuse scattering  
• Extracting information from reciprocal space maps:  
    o Lateral coherence information  
    o Vertical coherence information  
    o Bragg peaks  

Non-ambient XRD with Anton Paar non-ambient chambers

Investigation of pressure/temperature/humidity effect on structural properties of a material using Empyrean, X’Pert3 Powder or MRD combined with Anton Paar non-ambient chambers.  

The course is intended for both new and existing users of Empyrean, X’Pert3 Powder (X’Pert Pro MPD) or MRD diffractometers. However, for the new users we strongly recommend first to follow the X-Ray Powder Diffraction course to get hands-on experience and a solid knowledge of your XRD system.  

Basic principles of XRD measurements at non-ambient conditions and overview of all Anton Paar chambers, will be followed by practical sessions covering sample preparation, instrument setup, data collection and analysis strategies with the focus on your analytical problem(s). Hands-on experience of work with HTK1200N, CHCPlus+, TTK 600, MHCtrans and/or DHS900 (or DHS1100) will be provided.  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

Course content

In the duration of the course the following aspects will be covered:  
• Basic principles of XRD at non-ambient conditions  
• Sample preparation for non-ambient experiment  
• Measurement strategies and set-up of data collection  
• Effective use of line and area detectors (PIXcel3D and GaliPIX3D)  
• Data analysis strategies  

Small-Angle X-ray Scattering (SAXS)

Basics and practical applications of SAXS on Empyrean or X’Pert3 Powder and X'Pert PRO MPD. Covers sample preparation, instrument setup, data collection and data analysis.  

The course is intended for both new and existing users of the Empyrean and X’Pert3 Powder (X’Pert Pro MPD) diffractometers. For the new users the full advantage of this course will be gathered if the SAXS course is followed after the X-Ray Powder Diffraction course. The topics ranges from an introduction to the SAXS technique, to the instrument configuration, as well as practical sessions covering sample preparation, data collection and data analysis using the EasySAXS software. The main purpose of this course is to help you to solve your analytical problem in the most effective way.  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

Course content

During the course the following aspects will be covered, both in interactive lectures and in practical sessions:  
• Introduction to the SAXS technique  
• Instrument setup  
• Sample preparation  
• Data collection strategies  
• Data analysis with EasySAXS software 


Pair Distribution Function (PDF)

The course is intended for both new and existing users of Empyrean and X’Pert3 Powder (X’Pert Pro MPD) diffractometers. For the new users of Malvern Panalytical XRD systems, the full advantage of this course will be gained if the PDF course is taken after the X-Ray Powder Diffraction course.  

The main purpose of the course is to provide you with the basic knowledge of the theoretical aspects of PDF analysis and their practical realization on Empyrean or X’Pert3 Powder (Pro MPD) system.  

Measurement strategies and possible instrument geometries will be discussed. The hands-on part will be focused on the sample preparation and on the data collection with the fast GaliPIX3D detector, as well as on the data treatment using HighScore software.  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

Course content

In the duration of the course the following aspects will be discussed:  
• Fundamental aspect of PDF technique  
• Measurement strategies, possible instrument setups  
• Optimal choice of optical components  
• Sample preparation  
• Data collection with the fast GaliPIX3D detector  
• Data treatment and calculation of the PDF  
• Analysis of the PDF  

Grazing Incidence Small Angle X-ray Scattering (GISAXS) on Empyrean

This course is intended for Empyrean users with some knowledge of X-ray diffraction and X-ray scattering, especially X-ray reflectivity. The course covers technique used to study nanostructured layers and thin films by means of grazing incidence small angle X-ray scattering (GISAXS) techniques.  

Greatest benefit can be derived from the course after the instrument has been installed at the user site and the participant has had an opportunity to become acquainted with the equipment.  

The course will provide both the basic theoretical concepts of grazing incidence small angle X-ray scattering technique, as well as experimental practices using Empyrean system. Special emphasis will be placed on instrument handling and sample alignment optimization. The capabilities and limitations of the technique for thin film materials analysis will be described. Further the basic analysis on the generated 2D data will be discussed.  
As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

The main aspects covered during the course are the following:
• Basic principles of GISAXS  
• System preparation and setting up GISAXS application  
• Hardware components and their impact on data quality  
• Practical aspects of alignment procedures  
• Basics of data treatment and analysis using XRD2DScan software 

Computed Tomography (CT)

The course is intended for both new and existing users of Empyrean diffractometer. For the new users of Malvern Panalytical XRD systems, it is advised to follow the CT course after attending the Basic XRD course.  

The main purpose of the course is to provide the participants with the basics of CT, 3D reconstruction and their practical realization on an Empyrean system. Measurement strategies and possible instrument geometries will be discussed. The hands-on part will be equally focused on performing the experiment and the data analysis. Special attention will be paid to the sample preparation steps and performing the measurements (optimization of sample dimensions, generator and detector settings …).  

As a participant you are encouraged to bring with you one or two of your characteristic samples (together with the corresponding safety data sheet).  

The main aspects covered during the course are the following:
• Basics of the CT technique  
• Possible instrument configurations  
• Performing the CT experiment  
• 3D reconstruction  
• Basics of visualization and analysis of the reconstructed object