X-ray Diffraction

Labs are due Monday at 5pm in 410 Rhodes.

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Evaluations from Fall 04 (Currently missing)
Evaluations from Fall 06
Evaluations from Winter 02
Evaluations from Spring 01
Evaluations from Winter 01
Evaluations from Spring 00
Evaluations from Spring 99

Quarter: Spring, 2009
Prof. G. Beaucage
Office 492 Rhodes Hall, 556-3063
beaucag@uc.edu

Teaching Assistant:   Sachit Chopra email: choprast@email.uc.edu

Textbooks:
"Web Notes XRD" (below), G. Beaucage, updated when needed (last 2006)
"Elements of X-ray Diffraction", B. D. Cullity and S. R. Stock, 3’nd Edition (2001)
        (You will probably need a copy of this text which is fairly comprehensive and useful to own,
        but it is possible to share a copy with other students or to use the web notes if you can't spare
        the funds.) 
       1956 Out of Copyright Edition From Internet Archives
Other sources:
"X-ray Diffraction Methods in Polymer Science", L. E. Alexander (1969)
"Methods of X-Ray and Neutron Scattering in Polymer Science", R. J. Roe (2000)

Quizzes S2001 PDF:    Quiz 1; Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8; Quiz 9
Quizzes W2002 PDF:  Quiz 1; Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8
Quizzes F2004 PDF:    Quiz 1; Quiz 2;Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8; Quiz 9; Final
Quizzes F2006 PDF:    Quiz 1;Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8; Quiz 9; Final (3 Quiz) (All Quizzes but final.pdf)
Quizzes S2009 PDF:    Quiz 1; Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Final (3 Quizzes)

Web Text XRD

TOPIC: 1. What are x-rays, How are they Made & Detected	Chapter1.html         -Overview of EM Based Techniques         -Background on EM Radiation         -EM waves and Imaginary Numbers            EM Spectrum, Tape Generator,            Cow Alignment, Hungary Polarization,            Collimated, Black Holes            Stanford X-ray Laser, Hamburg            Posphor Screen, Scintillation, Proportional
2. Review of Crystalline Structure	Chapter2.html          -Crystal Lattices Web Link          -3D Crystal Planes, Paper Models                  and more          -Crystal Structures          -More crystal Lattice things          -Yet more crystal Lattice things          -And so on crystal Lattice things          -Link to Metal Crystal Structures                 Link to Rasmol to view 3D                    from above site (small pgm)          -Debye Scherrer from Cubic Stru.          -d-spacing equations          -Crystallographic angle equations          -Table of Interplanar Angles          -Wiki Crystal Structures          -Twinning in Geology
3. Basic Idea of Diffraction, X-ray Cameras	Chapter3.html          -Sathish Sukumaran's           Scherrer Derivation
4. Reciprocal Space	Appendix1.html-Reciprocal Road Map.html -Cambridge XRD -Local Link to Cambridge Page -Inverse Sp. -Electron Diffraction
5. Models For Diffracted Intensity	Chapter4.html           -Calculation of Intensity.html-Complex Exponential.html -Why Use Complex Numbers
6. XRD of Semi-Crystalline Polymers	XRD of Semi-Crystalline Polymers.html           -Paul Phillips Review 1990           -Paul Phillips Review 1994           -Bassett Pictures of Crystals           -Polymer Crystal Structure Slides*           -Chapter 4 Polymer Crystalline Structure           -Paul Ehrlich           -Chain Folding AFM           -Lamellar Growth Movie           -A Swedish course on Polymer crystals:             (Local Copy Part 1; Local Copy Part 2; Local Copy Part 3)           -Spherulitic Growth Eric Baer Science Paper 2009
7. Small-Angle Scattering of X-rays	SAXS/SANS           -Old Small-Angle Scattering of X-rays.html           -Glatter on SAXS           -Rod scattering           -SAXS Page Drexel           -SANS ISIS           -SAXS Okla. U.           -UNICAT Chicago           -SSRL SAXS Pople
8. Other Analytic Techniques Using EM Waves	Spectroscopy, Dynamic Light Scattering           -IR Spectroscopy, Wikipedia IR           -NMR Spectroscopy, Wikipedia NMR
9. Electron Diffraction	TEM ppt presentation Vidhya Sagar Jayaseelan
Other things	Appendix           -History of XRD from PSU           -Neutron Diffraction at LANL

The course will follow Cullity's text with some additions mostly pertaining to polymer crystallography. A good source for polymer crystallography is the book by R. J. Roe (of our department) or the book by Alexander mentioned in the syllabus. Students will learn the basics of production and use of x-rays, and their application to the characterization of crystalline and semi-crystalline structure in metals, polymers and ceramics.

You will need to be fully acquainted with the lab write-up prior to the lab. A short (10 minute) quiz will be given prior to the lab which will reflect 15% of the lab grade.  Labs will generally require 2 hours and will in some cases require sample preparation prior to the lab on the part of the students. This will be a rotating assignment and the student responsible for preparing samples will be graded on his work (30% of that labs grade. The student is responsible to meet with the TA to prepare the samples for that weeks lab.)
Lab reports are due Monday at 5:00 pm in 410 Rhodes.  Late reports will not be accepted.

You should work in a group to analyze data and develop your tables and plots to some extent but the words you write (the text) need to be your own.  Each student needs to prepare a separate lab report that is distinguishable from your group members.  You should look at the lab reports as a learning opportunity for technical writing. 

Labs:

Lab Report Format.html   Lab Notebook Format.html (grading is at the discretion of TA)		Error Analysis.html P. R. Bevington's paperback "Data Reduction and Error Analysis for the Physical Sciences", McGraw Hill, NY (1969) Any Physical Chemistry Laboratory Text UMich Error Site UC Physics Error Site Lab Report Format.pdf  More details on Reports Lab Notebook Format.pdf (grading is at the discretion of TA)
WEEK OF:	Lab:	Background:	Data:
April 7	Lab 1 Laser Diffraction.html	Draw what you see in microscope and see Fourier Transform (diffraction pattern).java Polymer Crystallites Background Some Optical Micrographs of Polymer Spherulites Simple Image Manipulation Shareware for Micrographs and LS Images jFourier1 Program to calculate FT of your drawings. Hair Scattering Help.pdf Similar Lab from Cornell www.ccmr.cornell.edu/education/modules/documents/Diffraction_000.pdf	2009 LS and Micrographs.zip 2006 LS and Micrographs 2004 LS and Micrographs 2002 SALS Patterns and Micrographs for Lab 2001 SALS Patterns and Micrographs for Lab 2000 SALS Patterns and Micrographs for Lab
April 14	PLEASE BRING ANY SAMPLES YOU WANT TO THIS LAB (See old lab data for interesting samples) Lab 2 Pinhole Camera.html	Orientation Function Notes.html;pdf of same ".gif" Table of Polymer XRD Peaks XLS of 2 Theta positions for Common Polymers Link to Metal Crystal Structures Excel Macro to Convert UDF (diffractometer text) to excel format. Instructions for Excel Macro	2009 Data.zip 2006 Pinhole Data.zip 2004 Fall Pinhole and Diff. Data W02 Pinhole Data F01 Polaroids PP Stretched shows Silica band (grainy) Oriented PHB Film from 2D image plate detector Pinhole Photos from Spring 2001 Data for Orientation Calculation.xls Pinhole Photos from Winter 2001 Pinhole Photos from 2000 Pinhole Photos from 1999 UHMWPE.gif ".zip" file of Azimuthal and Radial Averages for Lab (same as next two) + Polymer Spread Sheet (Need pkunzip, or winzip) Download Azimuthal Averaged Data.MSExcel Download Radial Averaged Data.MSExcel Spun High Density Polyethylene Fibers Blown Films of Linear Low Density Polyethylene
April 21	Lab 3 Stereographic Projections, A.html Details of Lab & Graph Paper	Java programs that work Java Applet to make stereographic projections (Wulff Nets) (Doesn't draw great circles though.) Wulff Net ps files About Stereographic Projections IUCrSimple Wulff Net ppt Wulff point and plane movies Fairly detailed Wulff Net Black Wulff Net Boule Wikipedia Text For Lab Pole Figure Wikipedia Pole Figure uk	Copy the link: http://www.eng.uc.edu/~gbeaucag/Classes/XRD/c2.pdf to your browser Copy the link: http://www.eng.uc.edu/~gbeaucag/Classes/XRD/c14.pdf to your browser
April 28	Lab 4 Laue Method.html	Laue Method Schematic Greninger Chart Slides on Diffraction Measurements Java programs that work Java Applet to Calculate Laue patterns for SimpleC, FCC and BCC DOS Program for calculating Laue Patterns Text Another program for Laue Debye-Scherrer and Powder calculations Laue Movie; Link to Laue Digital Camera Company	2009 Data 2006 Data Crystal Quality KBr Laue Photos from 2000 Laue Photos from 1999 http://www.eng.uc.edu/~gbeaucag/Classes/XRD/c16.pdf
May 5	Lab 5 Debye Scherrer Camera Hull-Davey Charts.html X-Pert High Score Plus (ITC Database)	Indium A6 Structure Excel Macro to Convert UDF (diffractometer text) to excel format. Instructions for Excel Macro	2009 Data Zip 2006 Data Zip 2004 Fall Data, Zip of all 2001 Spring Diffractometer Runs for Indexing Link to Indium Structure (A6 by Strukturbericht ...) 2000 Indium 1999 Data (.hqx files of excel spreadsheets): Copper (FCC) Germanium Single Crystal (Diamond Cubic) Molybdenum (BCC) Indium(BC Tetragonal) Brass Key (FCC Compare to Copper) Germanium Ground to Powder(Compare with Germanium Single Crystal above, Diamond Cubic) Second Run of Moly(BCC) Zinc (HCP in Table 10.2)
May 12	Lab 6 Diffractometer, Metal Phase Analysis.html	Instructions for Excel Macro	2009 Data.zip Groups 1 Gand 2, Groups 3 and 4 2006 Data 2004, zip of folder Metal Phase Spring 2001.xls Data.xls for 2000 1999 Data (.hqx of excel spreadsheets): Copper Wire (oriented), Copper Plate (unoriented), Zinc Powder, Brass Key, Moly Powder, Moly/Copper Powder
May 19	Lab 7 SAXS	Semi-crystalline Polymer Morphology XRD of Semi-Crystalline Polymers SAXS Notes	SAXS Data 2009.rar SAXS Data 2006 2004 Data 2001 Data q* vs Temp data for Hoffman Analysis Aerogel 2D PE isotropic 2D HDPE Aerogel 2D All 1-d files are columns of q (1/Angstrom), I (counts), Standard Deviation (counts) Aerogel 1D PET (Bad) 1D PE 1D LDPE Processing Data LDPE 2d SAXS and XRD of Blown LDPE Films
May 26	Lab 8 Diffractometer, Polymer Degree of Crystallinity.html	Instructions for Excel Macro Polymer Crystalline Morphology Polymer Handbook (e-ref at UC only)	2009 DOC.zip 2006 Data Gps 1 and 2; Gps 3 and 4 2004 DOC Data, SAXS and XRD PET PET Data 020228 CONTAINS NEW GOOD AMORPHOUS PET (Polyethylene Pterapthalate(sp)) for a series of crystallization temperatures and an amorphous run. DCS Trace for PET, Tg~85C 2001 Spring PE different DOC 2000 Data (.xls file of Durm and PETE Bottle) Drum Heads and PET Bottle Data 1999 Data (.hqx files of excel spreadsheets): Polyethylene Trace Close to Amorphous PE Trace Metallocene Low Crystallinity
June 2 307? ERC	Lab 9 TEM.html Keith's Writeup.html C20	Hyojin Song's Standard Spot Patterns Program for calculating Kossel patterns, Laue and Kikuchi Lines Lab 9.pdf Keith's.pdf German TEM Web page	Data 2009 (From Hyojin Song) Data 2006 Lab on June 2 will be taught by Hyojin Song songhn@email.uc.edu He is an expert in electron diffraction and TEM.

Lab Groups:

Course Requirements

Quizzes: Each Wednesday. Quizzes will be held at the end of class for 1/2 hour.

Occasional Homework: Due 1 week from assignment (very rare).

Labs: Don't copy old labs.

All labs are due Monday at 5 pm for all lab sections.

Work together on labs and share data but your write-up should be done independently.

A short quiz (10 minutes) will be given at the start of each lab period covering the lab.  This will reflect 15% of your lab grade.

Grading

All assignments (quizzes, labs and occasional homework) will receive equal weight. The following letter grades will be based on the average of these assignments,

• A = 90.0-100
• B = 80.0 - 89.9
• C = 70.0 - 79.9

Only Whole Grades Are Used Unless the Class Petitions for Half Grades at the Start of the Quarter (first week).

A comprehensive final based on all quizzes, homework and labs will be worth 3 assignment grades.

                                           Schedule for the End of the Quarter

Monday, June 8, 9:45 - 11:45 a.m.
    

A = 100-90.0; B = 89.9-80.0; C = 79.9-70.0
Code = last three digits of M number.

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