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Fundamentals of X-Ray Powder Diffraction

The "Introduction to X-Ray Powder Diffraction" course (EPS400 Topics) will not be offered in Spring, 2013 and it is unlikely to be offered again in the same format as offered previously (since 2002). There are a few reasons for this change. The acquisition of our new lab instruments (the Rigaku SmartLab general purpose diffractometer and the Rigaku Dmax Rapid II microdiffraction instrument) is expanding the capabilities of our laboratory significantly beyond straight powder diffraction; new capabilities include thin film work (both glancing angle and high-resolution rocking curves), small angle X-ray Scattering (SAXS) in transmission and reflection modes, pole figures for investigation of material textures, work with samples in micro-capillaries, and microdiffraction on intact samples utilizing a large 2-dimensional detector. This Spring three of us (Jim Connolly, Darren Dunphy and Eric Peterson) will be spending a lot of our time developing our capabilities with the new instrument, training new users in their operation and working to push the experimental envelope of diffraction and scattering research. In addition, the long-time lab manager, Jim Connolly, is retired as of September 1, 2013. The next time this course (or whatever substitutes for it) is offered it will include sections or modules on many of the new capabilities in addition to the fundamentals of powder diffraction.

While the course in its traditional form has gone away, this page remains, renamed "Fundamentals of X-Ray Powder Diffraction". It includes the same course materials prepared by James R. Connolly for the course (as offered last in Spring, 2012) presented in the same order taught in the class listed by week with subject headings. The subject headings include links to a variety of resources that visitors to this site may personally download to teach themselves something about X-rays, scattering, diffraction and how these phenomena are used it the study of crystalline materials. All of these materials have been prepared by James R. Connolly who is responsible for any errors and omissions (of which there are undoubtedly many).These materials may be read and freely copied for personal use, but may not be recopied or distributed without permission from the author. Permission requests should be directed to Jim Connolly via Email to connolly@unm.edu or jrc347@gmail.com.

The materials presented here form a decent introduction to X-Ray diffraction in general and analysis of powders specifically, however anyone who plans to seriously pursue the use of XRD as an analytical method would be well served to acquire an actual published text produced by folks who are experts in the field. Toward that end I have prepared an annotated list of recommended texts; the annotations should give the reader an idea of what texts might work best for their needs. Click here to read the list.

Prerequisites

Background that will be helpful to your understanding of the material presented here include geometry and trigonometry to include basic understanding of the trigonometric functions (sine, cosine, tangent, etc. and calculations involved in various permutations of right triangles), familiarity with basic crystallography such as what is taught in an upper-division undergraduate course in mineralogy or materials science. Understanding of the principles of the scientific method as used in experimental investigation is essential to treating work in X-ray diffraction and scattering experiments is essential. Those who expect to take data, plug it into a software black box and get answers will be sorely disappointed by the result. To successfully understand and interpret your diffraction data you must understand what is going on.

Radiation Safety

Most facilities (including UNM) that produce diffraction data require that operators must take and pass a Radiation Safety Exam for XRD users and be trained on the systems that they plan to use before being allowed to use them. The "Week 2" materials provide an introduction to Radiation Safety and additional materials will be found on the XRD Lab "Resources" page (http://epswww.unm.edu/xrd/resources.htm) in the "Radiation Safety Information and Tutorials" section. UNM faculty, staff and student who plan to use the lab should see our "Requirements for Users" page; this recently revised page includes everything you need to know to get qualified by the Radiation Safety office including study materials.

Instructor: Jim Connolly (connolly@unm.edu)

Office: Northrop, Rm 108 (across from the Main office, near the elevator)

Synopsis of Course

An introduction to the use of X- ray Powder Diffraction as an analytical method. The course will emphasize the practical use of X-ray diffraction as an analytical tool for the identification of crystalline materials in minerals, rocks, soils and engineered materials. Topics to be covered:

Resource Links for Class

Another source of online resources is our lab's XRD Resource page. Here you will find links to online tutorials on topics related to XRD, equipment manufacturer's web pages, and a variety of resources to supplement the course materials linked below.

Instructional Materials

These materials form the required text for this class. Students are responsible for the material contained in the Acrobat PDF files listed below regardless of whether that material is covered directly in class.


Acrobat PDF Note: Different web browsers can respond to Acrobat PDF files in a variety of manners. For most browsers, to view the Acrobat PDF files in your web browser, just click on them. To download the files so you can have a copy for reference, use your right-Mouse button (Mac users, just hold the mouse button down) and choose to "Save Target as .." or "Save Link As. ." to save a copy of the file. The files may be printed from your Web browser or from Acrobat Reader after downloading. Sometimes files will print more reliably if downloaded first and printed directly from Acrobat Reader (instead of printed from your web browser).


PowerPoint Note: I have discontinued attempts to make versions of the class PowerPoint presentations available that can be displayed in web browsers. I have found that these things in most cases cannot be printed, and do not display well. I have decided to make versions available in the native PowerPoint 2003 ("PPT") file type for those who want the full presentations.

I am also making Acrobat PDF versions of the same PowerPoint presentations that have all of the information in the slides without the display animations; these will have the same filename as the PowerPoint presentations with the addition of PPT at the end to differentiate them from the PDF text tutorials of the same name. To view the Acrobat versions, you just need a version of Acrobat Reader. To view the fully animated presentations, you will need:

Because these files are usually very large (since all graphics are included) and will take a some time to download, it is strongly suggested that you download the files to your local system (Right-click and "Save file as . . " or "Save Link") and open them after they have downloaded.


Week 1: Introduction to X-Ray Powder Diffraction (Acrobat PDF-561 KB, Rev. 1/1/07) (Powerpoint Presentation-3.9MB, Rev. 2/2/10; Acrobat PDF Version of Powerpoint Presentation-1.9MB, 2/2/10; ) (Nov 2011 E&PS Dept. Seminar Talk: Powerpoint Presentation-7.4MB; Acrobat PDF Version of Powerpoint-6.2MB)

Week 2: Radiation Safety for X-ray Diffraction Users (Acrobat PDF-296 KB, Minor Rev. 1/23/12) (Powerpoint Presentation-601KB, Rev. 1/23/12; Acrobat PDF version of Powerpoint Presentation-1.1MB, Rev 1/23/12)

Week 3: Generation of X-Rays (Acrobat PDF-699 KB, Rev. 2/1/12) (Powerpoint Presentation-4.2MB, Rev. 2/7/12; Acrobat PDF Version of Powerpoint Presentation-2.4MB, Rev 2/7/17)

Week 4: Crystallography Review (Acrobat PDF-1.5 MB, Rev. 2/22/12) (Powerpoint Presentation-9.0MB, Rev. 2/7/12; Acrobat PDF Version of Powerpoint Presentation-3.9MB; Rev. 2/2/10)

Week 5: Introduction to Diffraction and the Reciprocal Lattice (Acrobat PDF-1.5 MB, Rev. 2/15/12) (Powerpoint Presentation-6.9 MB, Rev. 2/15/12; Acrobat PDF Version of Powerpoint Presentation-6.9 MB; Rev. 2/15/12)

Week 6: Diffraction II: Intensities and Extinctions (Acrobat-PDF-691 KB, Rev 2/22/12) (PowerPoint Presentation-2.8MB, Rev. 2/22/12; Acrobat PDF Version of Powerpoint Presentation-2.5MB; Rev. 2/22/12).

Week 7: An Introduction the use of X-ray Diffraction in Clay Mineralogy (Dr. Dewey Moore) (PowerPoint Presentation-27MB, Rev. 2/28/12; Acrobat PDF Version of PowerPoint Presentation-5.9MB; Rev. 2/28/12)
Reading/Study Materials for Clay Mineralogy: For those who plan to use XRD for the study and analysis of clay minerals, I recommend that you acquire a copy of "X-Ray Diffraction and the Identification and Analysis of Clay Minerals, 2nd Edition" by Duane M. Moore and Robert C. Reynolds, Jr. (1997; Oxford University Press). It is a good introduction to a very complex subject.

Week 8 A Brief Introduction to our Scintag XRD and MDI Software (Powerpoint Presentation-2.5MB, Rev. 2/2/10; Acrobat PDF Version of Powerpoint Presentation-1.3MB 2/2/10). See Week 9 (March 21) listings for Printed Material Related to this topic.

Week 9: Introduction to Jade 9.x and DataScan software (Acrobat-PDF-675 KB, Rev. 2/15/09). Supplemental Document: Scintag "XRD Lab Cookbook" (Acrobat-PDF-592 KB, Rev. 4/3/09)

Week 10: Systematic Errors and Sample Preparation (Acrobat-PDF-600 KB, Rev. 3/2/09) (PowerPoint Presentation-7.9MB 2/2/10; Acrobat PDF Version of Powerpoint Presentation-4.2MB, 2/2/10)
Supplemental Documents: How to use the: Bico Jaw Crusher,(138 KB PDF); Spex Shatterbox,(150 KB PDF); Brinkmann Grinder (122 KB PDF)

Week 11: Introduction to practical Clay Mineral sample preparation and analysis -- Guest Presentation by Anthropologist Dr. Connie Constan (Acrobat PDF (Rev. 4/2/2012) of Connie's Powerpoint Presentation)

Week 12: Introduction to Quantitative Methods (Intro to Quant XRD-Acrobat PDF - 373 KB, Rev. 4/18/12; In-class Powerpoint Presentation - 1.1MB Rev. 4/18/12; Acrobat PDF Version of Powerpoint Presentation - 1.1MB Rev 4/18/12).
Some Quantitative Methods Resources: One of the best places to start for understanding the Reitveld method is Dr. Hugo Reitveld's classic 1969 paper -- well written and understandable -- available here in printable Acrobat PDF format. A source of Free structural information for Minerals (for use in Reitveld refinements) can be found here at the Mineralogical Society of America. A paper in printable Acrobat PDF format describing how to use the database is available here.

Week 13: Free or Inexpensive Software Alternatives for X-Ray Diffraction (Software for XRD-Acrobat PDF - 130 KB Rev. 4/27/10)
Round 2 Laboratory Exercise due before class.

 


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