X-ray Diffraction

Course Number: 20 261 424
MWF 12:00-12:50 Baldwin 643
Labs Monday (1) 1:00 to 2:30, (2) 2:30 to 4:00, Wednesday (3) 1:00 to 2:30, (4) 2:30 to 4:00  513 Rhodes

Labs are due Monday at 5 and Wednesday at 5
Please leave reports in the mailbox of Sandip Argekar near 401 Rhodes.

                =>To Class Notes Below
                =>To Lab Table Below
             =>To Course Requirements Below
                =>To Current Grade Sheet by Student Number Below
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                Comments/Corrections (beaucag@uc.edu)

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: Fall, 2006
Prof. G. Beaucage
Office 492 Rhodes Hall, 556-3063
beaucag@uc.edu

Teaching Assistant:   Sandip Argekar email:Sandip.Argekar@gmail.com or argekasu@email.uc.edu
                                    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.) 
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 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 F2004 PDF:    Quiz 1; Quiz 2;Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8; Quiz 9; Final
Quizzes W2002 PDF:  Quiz 1; Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8
Quizzes S2001 PDF:    Quiz 1; Quiz 2; Quiz 3; Quiz 4; Quiz 5; Quiz 6; Quiz 7; Quiz 8; Quiz 9

Web Text XRD

TOPIC:

  1. What are x-rays, How are they Made & Detected
  2. Review of Crystalline Structure
  3. Basic Idea of Diffraction, X-ray Cameras
  4. Reciprocal Space
  5. Models For Diffracted Intensity
  6. XRD of Semi-Crystalline Polymers
  7. Small-Angle Scattering of X-rays
  8. Electron Diffraction

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.

The class will be split into four groups as noted in grade sheet below. (Code is last 2 digits of student number)

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 1.5 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 Tuesday at 5:00 pm in 410 Rhodes for all lab sections.  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)
 
Lab Report Format.pdf
 
Lab Notebook Format.pdf
(grading is at the discretion of TA)
WEEK OF:
Lab:
Background:
Data:
September 25
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

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

October 2
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

2006 Pinhole Data
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
October 9
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
 
October 16
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
2006 Data

Crystal Quality KBr

Laue Photos from 2000

Laue Photos from 1999

October 23
Lab 5 Debye Scherrer Camera
Hull-Davey Charts.html
Indium A6 Structure

Excel Macro to Convert UDF (diffractometer text) to excel format.

Instructions for Excel Macro
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)
October 30
Lab 6 Diffractometer,
Metal Phase Analysis.html
Instructions for Excel Macro
Groups 1 and 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

November 6
Lab 7 SAXS
Semi-crystalline Polymer Morphology

XRD of Semi-Crystalline Polymers

SAXS Notes
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
November 13
Lab 8 Diffractometer,
Polymer Degree of Crystallinity.html
Instructions for Excel Macro

Polymer Crystalline Morphology
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

November 27

Demo Lab
(Write-up is a Summary Report)

(Keith Leonard) Lab 9 TEM.html

Keith's Writeup (nice).html

C20

Program for calculating Kossel patterns, Laue and Kikuchi Lines

Lab 9.pdf

Keith's.pdf
Data 2006

Class on Monday Nov. 20 and Lab will be taught by Vidhya Sagar Jayaseelaw
Jayasevs@email.uc.edu
562 ERC
He is an expert in electron diffraction and TEM especially from diamond films. 

Course Requirements

Quizzes: Each Wednesday including 9/27. 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 Tuesday 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,

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

Dec  5 Tuesday Final Baldwin 643 Time 4 pm
     Final will be 3 of the previous quizzes but not the previous Friday's quiz.

Current Grade Sheet (RED = Imminent Danger of a 0; LIGHT BLUE = Redo old quiz 2's for an 85; Bold italic means grade so far not used)
Bold Final Grade is Final Grade, others are subject to further grade logging by TA etc.

A = 100-90.0; B = 89.9-80.0; C = 79.9-70.0
Code = last four digits of student number.  Lab groups meet 1: M 1pm; 2: M 2:30pm; 3: W 1pm; 4: W 2:30
(RED = Imminent Danger of a 0; LIGHT BLUE = Redo old quiz 2's for an 85; Bold italic means grade so far not used)
Bold Final Grade is Final Grade, others are subject to further grade logging by TA etc.

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Copyright (c) 1999, 2004, 2006

XRD page, designed by / G. Beaucage / beaucag@uc.edu


 

 
 
 
 
 
 
 
 
 
 
 
 

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