Training

This lecture is intended for people who want to become independent self-user of the small or wide angle X-ray scattering (SAXS) instrument in the MRL X-Ray Lab. SAXS describes the analysis of any sample that has nanostructured (1-100nm) electron density fluctuations -- i.e., nanoparticles in solution, block co-polymers, ionic liquids, soft matter, etc. Typically nanoscale electron density variations arise as structured (nanoscale object in a lattice), unstructured (in solution), or oriented (fiber or affixed to substrate) therefore treatment of each type of sample is on a case by case basis. Students must also attend SAXSLAB instrument specific training course to learn how to put the knowledge obtained in the lecture to practice. This lecture will survey the fundamentals of small angle X-ray scattering (SAXS), focusing on the bare essentials required to productively collect and analyze SAXS data. In addition to theory, this lecture will cover practical considerations such as common sources of error and a guide to structural interpretation and justification using SAXS patterns.
This course will teach you how to profile fit data in the program HighScore Plus. Profile fitting is the first step to quantification of XRPD data. Profile fitting allows a user to extract precise information about peak position, intensity, and width. Once XRPD data have been profile fit, a variety of calculations are possible. This session will focus on refining unit cell lattice parameters, indexing diffraction data, % crystallinity, and calculating the relative weight fractions of phases in a mixture (quantitative phase analysis). Additional workshops will focus on calculating nanocrystallite size and microstrain from peak broadening.
This workshop will introduce you to the X-ray powder diffraction data analysis software "HighScore Plus". This course will focus on phase analysis (phase ID) using HighScore Plus. Students will be practice using the interface to accomplish basic tasks such as visualizing data, fitting background, peak search; and phase analysis by comparing experimental data to reference patterns and automated search/match. This course is a pre-requisite for all advanced analysis workshops using HighScore Plus.
This class will teach students the basic operation of the Bruker D8 HRXRD instrument. The emphasis of this class will be on using triple-axis diffraction to collect data from epitaxial thin films. This session will cover collecting coupled-scans of Bragg peaks and rocking curves. This class will establish the foundation for collecting reciprocal space maps of epitaxial thin films, but the actual collection of RSMs will be covered in the separate class. This class will also cover the basis of collecting X-ray reflectivity (XRR) data from thin films.
The PANalytical X'Pert Pro diffractometer is an excellent choice for X-ray powder diffraction (XRPD). The default mode of this instrument is in Bragg-Brentano parafocusing geometry, which is used for polycrystalline materials. We usually keep a linear position sensitive detector on the instrument, which permits rapid data collection for angles higher than 4 degrees 2Theta. The basic instrument training session will focus on the collection of powder diffraction data using the high-speed optics, which consist of programmable divergence slits and X'Celerator high-speed detector, and the Open Eularian Cradle (OEC) sample stage. This configuration is best suited for high-speed high-resolution data collection from powders and polycrystalline thin films. Accessories include several different sample stages and optics. After you have completed this training, you can request individaul training on the other configurations available with this instrument. There are three other sample stages that are available: (1) the 15 position automatic sample changer, (2) the furnace that can heat samples up to 1200 C, and (3) the cyrostat that can cool samples down to 11 K. The PANalytical also can be configured parallel-beam optics for grazing incidence X-ray diffraction (GIXD). After you have completed the basic training, you can request individual training on using the other configurations. Users of this instrument should also strongly consider taking a data analysis course to suit their needs, such as the line profile fitting course for crystallite size and microstrain analysis, the Rietveld refinement series for quantitative phase analysis and unit cell analysis, or the Introduction to High Score Plus for qualitative phase identification and database search techniques.
The PANalytical Empyrean diffractometer is an excellent choice for X-ray powder/polycrystalline diffraction measurements with low background. The default mode of this instrument is in Bragg-Brentano parafocusing geometry with CuKa1,Ka2 doublet radiation. Samples can be loaded into a 45-position sample changer to input into the reflection-transmission spinner stage. The instrument has linear position sensitive detector (Pixcel 1D, max count rate: 6.5 x 10^9 cps) which permits rapid data collection up to 255 times faster than with a traditional point detector. The basic instrument training session will focus on the collection of powder diffraction data using the Bragg Brentano High Definition (BBHD) flat mirror optic, 45-position sample changer, reflection transmission spinner (in reflection geometry) and the Pixcel 1D detector. This configuration is best suited for high-speed high-resolution data collection from powders and polycrystalline thin films. Accessories include a Anton Paar CHC+ Cryo-Humidity stage. After you have completed this training, you can request individual training on the humidity stage available with this instrument. The sample temperature range is from –180 °C to +400 °C with liquid nitrogen cooling, and from –5 °C to +400 °C with compressed air cooling. The sample relative humidity range is 5 to 95 % RH at 10 °C to 60 °C and 5 to 70% RH at 80 °.  Users of this instrument should also strongly consider taking a data analysis course to suit their needs, such as the line profile fitting course for crystallite size and microstrain analysis, the Rietveld refinement series for quantitative phase analysis and unit cell analysis, or the Introduction to High Score Plus for qualitative phase identification and database search techniques. The basic instrument training session will focus on the collection of powder diffraction data using the Bragg Brentano High Definition (BBHD) flat mirror optic, 45-position sample changer, reflection transmission spinner (in reflection geometry) and the Pixcel 1D detector. This configuration is best suited for high-speed high-resolution data collection from powders and polycrystalline thin films. Accessories include a Anton Paar CHC+ Cryo-Humidity stage. After you have completed this training, you can request individual training on the humidity stage available with this instrument. The sample temperature range is from –180 °C to +400 °C with liquid nitrogen cooling, and from –5 °C to +400 °C with compressed air cooling. The sample relative humidity range is 5 to 95 % RH at 10 °C to 60 °C and 5 to 70% RH at 80 °.  Users of this instrument should also strongly consider taking a data analysis course to suit their needs, such as the line profile fitting course for crystallite size and microstrain analysis, the Rietveld refinement series for quantitative phase analysis and unit cell analysis, or the Introduction to High Score Plus for qualitative phase identification and database search techniques. SAXS - small angle X-ray scattering WAXS - wide angle X-ray scattering GISAXS - grazing incidence small angle X-ray scattering
This course will teach users the basics of data collection using the SAXSLAB instrument. The SAXSLAB system has automated detector positioning for SAXS/WAXS analyses of samples in capillaries or freestanding films in a transmission geometry and GISAXS/GIWAXS of samples supported on a monolithic substrate in grazing incidence reflection gemoetry. Calibration of the q-range using silver behenate, acquisition of empty, buffer (if sample is immersed in solvent) and dark current exposures for similar timescales and data reduction procedures will be covered. The SAXSLAB instrument is very well suited for analyzing polymers, soft materials, nanoparticles in solution or dried on substrates, porous samples, and nanostructured surfaces. The emphasis in this training session will be design of experiment, routine collection and data reduction. SAXS - small angle X-ray scattering WAXS - wide angle X-ray scattering GISAXS - grazing incidence small angle X-ray scattering
This class will teach the basics of collecting data using the Rigaku SmartLab with divergent beam and parallel-beam optics. The focus will be data collection from polycrystalline thin films using X-Ray Powder Diffraction (XRPD) techniques and Grazing Incidence X-Ray Diffraction (GIXD). The techniques will be applicable to other types of samples, such as powders and pellets. In addition, the basics of collecting X-ray reflectivity (XRR) data will be covered.