Powder X-ray Diffractometry:

Errors and Effects of Sample Texture

MATSC 430
Pennsylvania State University
Fall 2009
Recall this type of experiment in reciprocal space

=constant Sample= usually polycrystalline

Intersection of two spheres is a circle

So, there is a cone of solutions
“Debye Cone”


o

Typical diffractometer has the Bragg-Brentano geometry
Low 2 High 2
X-ray source

X-ray detector Diffractometer Circle

Focusing Circle

Sample sits in center of diffractometer circle

 Systematic Errors in Powder Diffraction
Most common: Sample displacement error

Proper position
Displace position

2=-sin()/R 

R= diffractometer radius
Sample Texture e.g. Ni film grown on ZrO2 single crystal
substrate

Powder Diffraction Data 1 m

Intensity (counts)

ZrO2 (200)
ZrO2 (400)
Ni (111)

Ni (200) Ni (222)
40 50 60 70 80 90 100
2 theta (˚)
 Pole Figure Analysis

Ni Ni

2=2Ni200 2=2Ni111

Scattering Angle held constant and sample rotated along

2 independent axis ().

Plot scattered intensity as a function of sample orientation

Al2O3-ZrO2 Directionally Solidified
Eutectic

220 Z(c) 5 m
220 Z(t)

004 Z(t)
400 Z(c)
212 Z(t)
002 Z(t)
110 Z(t) 004 Z(t)
200 Z(c) 220 Z(t)
400 Z(c)

00.6 A 114 Z(t)

00.12 A
222 Z(t)
111 Z(c) 420 Z(c)
 b)
{11.3} Al2O3 a)
{220} ZrO2 (c)
{112} ZrO2 (t)

X-ray diffraction pole figures of a) Alumina {11.3} reflections and b) cubic Zirconia {220} and tetragonal
Zirconia {112} reflections