Syllabus    MSCI 537    Spring 2009                        PJL 1/3/09


CRYSTALLOGRAPHY AND DIFFRACTION LAB - Selected lab experiments in materials science.  This course is designed to complement the lectures in MSCI 535, which must be taken concurrently or previously.  The lab experiments concern the structure and constitution of materials as revealed by x-ray diffraction and refraction.


Instructors: Peter Loos   office: ME 215,  ext. 3698,  ploos@YouKnowWhere  mobile: 281-250-4998

                    Richard Crouse, SEA X-ray Lab Manager,  office: SS B08, ext. 3279, rcrouse@YouKnowWhere

                    and perhaps one graduate student teaching assistant


Schedule & Location:  Tentatively Tue. or Thu. 2:30-5:00pm.  Most of the equipment is in SS B06 (basement) and one machine is in GL 330.


Text:  Elements of X-ray Diffraction, either 3rd ed. or 2nd edition


Grading:  Based on attendance, participation, safety, ability to operate the equipment and neatness in lab as well as completeness, correctness, organization and clarity of expression in the lab reports.  Students whose efforts during the semester are unsatisfactory will have the opportunity to take a final exam for extra credit.


Safety:  There will be a quiz about x-ray safety.  Each student will take it as many times as required to get all the answers correct.


Experiments:  There will be seven lab experiments, accompanied by reading in the text and in other references.


#1 Instrument calibration, the emission spectrum of the Cu x-ray tube, filtering the spectrum.

#2 Measurement of Pt and Ti film thickness and stress using (a) Scherrer's formula and a

      Williamson-Hall plot and (b) x-ray reflectometry (XRR) methods.

#3 Identification of unknown powder samples using Jade and the PDF.  Determine Bravais

      lattice and lattice parameter by the spreadsheet method.

#4 Lattice parameter measurement and stoichiometry in alloys using Vegard's Law.

#5 Determination of volume fractions of multiple phases in a mixture using reference intensity ratios.

#6 Measurement of residual elastic stresses in a simple structure using the sine squared psi method.

#7 To be determined, probably use of pole figures or in-plane (grazing incidence) diffraction for evaluating preferred orientation.


Depending on student interest, availability of suitable sample materials, etc. there is a possibility of doing a small angle x-ray scattering (SAXS) measurement in experiment #7.


X-ray Instrumentation:  An old Siemens diffractometer will be used in experiment #1.  Two modern Rigaku Dmax machines will be used in experiments #2 - #5.  A state-of-the-art Rigaku SmartLab machine (first of its kind in the US) will be used in experiments #6 & #7.  The Rigaku machines are in SS B06 and the Siemens machine is in GL 330.  For info on the Rigaku machines, see and and concerning the Siemens machine see Cullity 2nd edition Figure 7-2(b) or


Lab Reports:  Students will work together in small groups when operating the equipment and collecting & analyzing data; however, students must work independently to write up the lab reports.  Lab reports are due three weeks after the data are collected.  Points will be deducted for late reports.


Computation:  Students will use Jade software and the ICDD Powder Diffraction File (PDF) database.  Four copies of this software are running on WinXP machines in SS B06.  Also, CaRIne software for calculating diffraction patterns and visualizing crystal structure is available in SS B06.  Spreadsheet software will also be used.


NOTICE:  Any student with a disability requiring accommodations in this class is encouraged to contact Instructor after class or during office hours.  Additionally, students should contact the Disabled Student Services office in the Ley Student Center.