This is powder diffraction!
Calcite, Aragonite, Brucite
12000
11000
10000
Lin (Counts)
9000
8000
7000
6000
5000
4000
3000
2000
1000
0
10
20
30
40
50
60
70
2-Theta - Scale
Calcite, A ragonite, B rucite - File: m1.R A W - Type: 2Th/Th locked - S tep: 0.020 ° - S tep time: 10.0 s - Theta: 1.000 °
Operations: Import
Peter J. LaPuma1
© 1998 BRUKER AXS, Inc. All Rights Reserved
This is powder diffraction!!!!
Calcite, Aragonite, Brucite
12000
11000
10000
Lin (Counts)
9000
8000
7000
6000
5000
4000
3000
2000
1000
0
10
20
30
40
50
60
70
2-Theta - Scale
Calcite, A ragonite, B rucite - File: m1.R A W - Type: 2Th/Th locked - S tep: 0.020 ° - S tep time: 10.0 s - Theta: 1.000 °
Operations: Import
Peter J. LaPuma2
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 DISCOVER WITH GADDS
Powders
Speed
Texture
Versatility
Micro-diffraction
Power
Stress
Precision
SAXS
Accuracy
Peter J. LaPuma3
© 1998 BRUKER AXS, Inc. All Rights Reserved
Single Crystal Diffraction
Peter J. LaPuma4
© 1998 BRUKER AXS, Inc. All Rights Reserved
2-D Single crystal data
Peter J. LaPuma5
© 1998 BRUKER AXS, Inc. All Rights Reserved
Micro-Diffraction
Peter J. LaPuma6
© 1998 BRUKER AXS, Inc. All Rights Reserved
2-D Micro-diffraction data
Peter J. LaPuma7
© 1998 BRUKER AXS, Inc. All Rights Reserved
Diffraction of textured materials
Peter J. LaPuma8
© 1998 BRUKER AXS, Inc. All Rights Reserved
2-D Texture data
Peter J. LaPuma9
© 1998 BRUKER AXS, Inc. All Rights Reserved
Powder Diffraction
Peter J. LaPuma10
© 1998 BRUKER AXS, Inc. All Rights Reserved
Powder diffraction data
Peter J. LaPuma11
© 1998 BRUKER AXS, Inc. All Rights Reserved
General Area Detector Diffraction
Solution
2-D position sensitive
detector
Collects data from the entire
Debye ring without moving
True Photon counter
200 micron spatial
resolution
Variable detector distances
50 - 300 mm for resolution
or intensity
Peter J. LaPuma12
© 1998 BRUKER AXS, Inc. All Rights Reserved
Point detector vs. area detector
Peter J. LaPuma13
© 1998 BRUKER AXS, Inc. All Rights Reserved
Point detector vs. area detector
Peter J. LaPuma14
© 1998 BRUKER AXS, Inc. All Rights Reserved
Point detector vs. area detector
Peter J. LaPuma15
© 1998 BRUKER AXS, Inc. All Rights Reserved
Point detector vs. area detector
Peter J. LaPuma16
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 DISCOVER with GADDS
Real and useable intensity data from preferentially
oriented samples
Single crystal, textured, and non-textured materials can be
collected simultaneously in minutes
Small sample amounts can be measured quickly with real
intensities
Large quantities of data and information with little or no
sample movement
Peter J. LaPuma17
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 Discover with GADDS - Applications
Powder diffraction
Texture
Stress
Micro-diffraction
SAXS
Peter J. LaPuma18
© 1998 BRUKER AXS, Inc. All Rights Reserved
Basic Configuration - Beam Path
Peter J. LaPuma19
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 DISCOVER with GADDS
Basic Configuration
Peter J. LaPuma20
© 1998 BRUKER AXS, Inc. All Rights Reserved
Powder Diffraction
Analyze 70 deg. of 2 theta
without moving the
detector
Collect full patterns in
seconds
Intensity integration
removes preferred
orientation effects
Integration converts data
into 2theta vs. intensity
Phase ID from small
sample amounts
Peter J. LaPuma21
© 1998 BRUKER AXS, Inc. All Rights Reserved
Powder diffraction - Analysis
Advanced phase
identification with to PDF
database
Quantitative analysis
Percent crystallinity
Crystallite size and strain
Profile fitting
Lattice parameter
indexing and refinement
Direct cut and paste into
reports
Peter J. LaPuma22
© 1998 BRUKER AXS, Inc. All Rights Reserved
Texture analysis
a)
b)
c)
Peter J. LaPuma23
© 1998 BRUKER AXS, Inc. All Rights Reserved
Texture analysis - Speed
Simultaneous measurement of single crystal, textured
and untextured materials
Data for multiple pole figures are collected
simultaneously in minutes
Chi motion not needed due to 2-D detector
Peak height and background are collected
simultaneously in one frame
Scintillation detector
– 1296 separate sample positions
– One pole figure
D8 DISCOVER with GADDS
– 72 separate sample positions
– Multiple pole figures
Peter J. LaPuma24
© 1998 BRUKER AXS, Inc. All Rights Reserved
Texture data analysis
User friendly analysis
software for pole figure
representation
3-D and contour plot
representation of pole
figures
Calculation of ODF
Peter J. LaPuma25
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 DISCOVER with GADDS
all purpose configuration
Peter J. LaPuma26
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis does not
occur in 1-D
Peter J. LaPuma27
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis - Full Debye
ring fitting
Peter J. LaPuma28
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis - Full Debye
ring fitting
Peter J. LaPuma29
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis - Textured
materials
Peter J. LaPuma30
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis
Most accurate stress measurements ever due to full
Debye ring fitting
Stress in different directions measured with one set
of frames simultaneously
Peak position height and background from 1 set of
frames
Stress values with standard deviations as low as 3%
Stress values from textured materials
Peter J. LaPuma31
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis - Goebel
Mirrors and pinhole collimators
Cross coupled Goebel
mirrors provide a highly
parallel highly intense Xray beam perfect for
stress analysis
Pinhole collimators
reduce spot size down to
50 microns
Coupled with laser /video
alignment system, stress
in sample can be mapped
a function of position
Peter J. LaPuma32
© 1998 BRUKER AXS, Inc. All Rights Reserved
Residual stress analysis - software
Powerful - user friendly
software
Easy display of all psi
angles
Calculations of Sin
squared psi data
Easy cut and paste into
reports
Peter J. LaPuma33
© 1998 BRUKER AXS, Inc. All Rights Reserved
Micro-diffraction - Beam Path
Peter J. LaPuma34
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 DISCOVER with GADDS
Micro-diffraction Configuration
Peter J. LaPuma35
© 1998 BRUKER AXS, Inc. All Rights Reserved
Micro-diffraction - Laser video
alignment
Peter J. LaPuma36
© 1998 BRUKER AXS, Inc. All Rights Reserved
Laser - Video Alignment
Peter J. LaPuma37
© 1998 BRUKER AXS, Inc. All Rights Reserved
Micro-diffraction
Diffraction from points as small as 50 microns
Easy sample alignment and positioning with X,Y,Z
stage and Laser-video microscope
Laser-video image on the computer screen with cross
hairs
Patterns with accurate relative intensities due to data
integration
Highly parallel, highly intense X-ray beam due to
Goebel Mirrors
Highly intense X-ray beam due to MonoCapTM
Collimator
Diffraction data can be analyzed by phase
identification, profile fitting, quantitative analysis, etc.
Peter J. LaPuma38
© 1998 BRUKER AXS, Inc. All Rights Reserved
Small Angle X-ray Scattering
Peter J. LaPuma39
© 1998 BRUKER AXS, Inc. All Rights Reserved
Small Angle X-ray Scattering
Peter J. LaPuma40
© 1998 BRUKER AXS, Inc. All Rights Reserved
Small Angle X-ray Scattering
Cross-coupled Goebel mirrors for highly intense
parallel beam
Evacuated or He beam path for reduction of air scatter
D8 DISCOVER with GADDS system measures isotropic
and anisotropic scattering
SAXS has very low signals due to transmission
measurements - perfect for D8 DISCOVER with GADDS
Peter J. LaPuma41
© 1998 BRUKER AXS, Inc. All Rights Reserved
D8 Discover with GADDS
More information faster
than ever before
Pinhole collimators and
laser/video microscope
provide micro-diffraction,
micro-stress, microtexture, etc.
Highly intense and highly
parallel X-rays with
MonoCapTM collimators
and Goebel mirrors
Most powerful and user-
friendly software available
Peter J. LaPuma42
© 1998 BRUKER AXS, Inc. All Rights Reserved
