Dynamic Beam Optimization

Perfect Powder Diffraction Data Automatically:
Dynamic Beam Optimization

Welcome to today’s webinar from our

Bruker AXS office in Karlsruhe, Germany!
Dr. Arnt Kern Dr. Christina Drathen

Product Line Manager XRD Product Manager XRD
May 5, 2020 2
Outline

• Origins of parasitic scattering in XRPD data
• Minimizing parasitic scattering: Dynamic Beam Optimization
Application examples
Instrument considerations
• Supported instrument configurations
• Instrument upgrades
Wrap-up
• 3 Things to remember
• Question & Answers
May 5, 2020 3
Outline

• Instrument upgrades
Wrap-up
May 5, 2020 4
The Source of Parasitic Scattering...
... and its Consequences
• Parasitic Scattering makes data

analysis harder and can lead to
incorrect results. Air scattering
• For good data, we want to minimize "Amorphous bump"
or completely avoid scattering that from sample support
does not come from the sample.
Main contributions Typical phenomena Analytical Consequences
(Broad) peaks from sample Incorrect relative intensities;

Beam overflow
holder Incorrect amorphous content
High background at low and Miss low angle peaks, wrong
Air-scattering
medium angles phase-ID; worse LOD* and LOQ**
Very high background at Difficult to differentiate between
Direct beam spill
very low angles SAXS and parasitic signal
Fluorescence Background is high Worse LOD and LOQ
* Limit of Detection ** Limit of Quantification
May 5, 2020 5
Parasitic Scattering
Traditional Beam Conditioning
• Beam spillover and air-scattering at

low angles can be avoided by
choosing appropriate diffractometer 2 3
settings
1
• But optimizing the set-up for low
angles can lead to detrimental
negative effects at higher angles
• In reality, we often live with a
compromise
Component Low angles Higher angles
1. Divergence slit size Avoid beam-spill Maximize intensity
 Small slit  Large slit
2. Knife edge position Shield air scattering Avoid cutting the beam
 Knife close to sample  Knife away from sample
3. Detector opening Shield air scattering Maximize intensity
 Small window  Maximum window
Fixed vs. Motorized Divergence Slits
• Fixed Divergence Slits (FDS):

• Beam spillover at low angles 2θ, therefore scattering from the sample support and
intensity losses at small angles 2θ
• Motorized Divergence Slits (MDS):
• Fixed illuminated specimen area, therefore NO beam spillover and NO scattering
from the sample support; higher intensity
Beam spillover No beam spillover,

at low angles 2θ no scatter from the sample support
Fixed vs. Motorized Anti-Scatter Screen
• Traditional fixed knife edge

• Placed as close to the beam as possible, risk of beam cropping
• Motorized Anti-Scatter Screen
• Fully software controlled retraction of the knife, thus air scattering is almost
entirely eliminated without ANY cropping of the beam
• The Motorized Anti-Scatter Screen is THE component providing the greatest
improvement on data quality
The beam is increasingly No beam cropping

cropped as 2θ increases
Variable Active Detector Window
• Fully software controlled switching-on of individual strips

to "open" the active detector window as a function of 2θ, to further
minimize air scattering
• Effective for data acquisition at angles <5° 2θ.
 Reliable data acquisition starting at angles as low as ~ 0.3° 2θ
Fully software controlled synchronization of

1. Motorized Divergence Slits,
2. a Motorized Anti-Scatter Screen,
3. and a Variable Active Detector Window
2
3
1
Outline

• Instrument Upgrades
Wrap-up
May 5, 2020 11
Background Optimization
High background – air scattering
A common source of elevated

background comes from air
scattering…
October 23 - 27, 2017 12

By placing a fixed knife 5mm above

the sample, the background level
improves dramatically
October 23 - 27, 2017 13

The usage of a motorized knife

improves the background even
more, especially at low angles
October 23 - 27, 2017 14

Quantitative Mineralogy
Shale Rock
• Comparison of fixed slit and motorized slit

• With MASS: improved low angle background, and no cropping of beam
at high angles
May 5, 2020 15
Quantification of amorphous content
5% and 1.5% Slag in Cement
170
• Quantification of amorphous 5.1%

165 C3S <M3> HKL 13.84 %
160 Bkg 0.00 %
155 Wax 0.00 %
150 Sucrose 0.00 %
145
components is challenging
Slag 5.18 %
140
135
C3S <M1> 39.24 %
130 C2S_beta 13.64 %
125 C3A_cubic 1.36 %
C3A_orthorhombic 0.25 %
DBO ensures that signal is coming only

120
•
115 C4AF 11.60 %
110
Lime 0.31 %
105
Portlandite 1.52 %
100
Periclase 0.01 %
from sample
95
90 Quartz 0.33 %
85 Arcanite 0.60 %
80 Langbeinite 0.06 %
75 Aphthitalite 0.45 %
Sqrt(I)
70
Gypsum 0.00 %
65
Bassanite 1.09 %
60
55 Anhydrite 2.13 %
50 Calcite 8.40 %
45
40
21,000
20,500
Slag 0.00 % 35
30
20,000 Wax 0.00 % 25
20
19,500 Sucrose 0.00 % 15
19,000 10
5
18,500 0
18,000 -5
-10
17,500
-15
17,000 -20
16,500 -25
-30
16,000 -35
15,500 -40
-45
15,000 -50
14,500 -55
14,000 5 10 15 20 25 30 35 40 45 50 55 60 65
13,500
13,000
12,500
C3S <M3> HKL 11.09 %
1,5%
165
12,000 160 Bkg 0.00 %
11,500 155 Wax 0.00 %
150
11,000 145
Sucrose 0.00 %
10,500 140
Slag 1.48 %
135 C3S <M1> 38.22 %
10,000
130 C2S_beta 12.93 %
9,500 125 C3A_cubic 1.41 %
9,000 120 C3A_orthorhombic 0.14 %
Slag
115
8,500 C4AF 10.89 %
110
Lime 0.29 %
8,000 105
100 Portlandite 1.30 %
7,500 95 Periclase 0.06 %
7,000 90 Quartz 0.47 %
85 Arcanite 0.53 %
6,500
80 Langbeinite 0.03 %
6,000 75
Aphthitalite 0.43 %
Sqrt(I)
70
5,500 Gypsum 0.01 %
65
Grinding aid
5,000 60 Bassanite 0.94 %
4,500 55 Anhydrite 2.04 %
50 Calcite 17.74 %
4,000 45
3,500 40
35
3,000 30
2,500 25
20
2,000
15
1,500 10
1,000 5
0
500 -5
0 -10
-15
-500 -20
-1,000 -25
-30
5 10 15 20 25 30 35 40 45 50 55 60
-35
Fit of slag sample in DIFFRAC.TOPAS

-40
-45
-50
-55
5 10 15 20 25 30 35 40 45 50 55 60 65
16
Very low angle measurement using VDO
SAXS signal in SBA-15
Measurement conditions
• VDS @ 20 mm
• Automatic MASK
• 0,4° initial detector opening
• 3,3° full detector opening @ 2𝜃𝜃=4°
0,4°
17
Very low angle measurement using VDO
SAXS signal in SBA-15
SBA-15
True SAXS signal
LaB6
LaB6
SBA-15 (same conditions)
18
Outline

Wrap-up
May 5, 2020 19
Supported Instrument Configurations
Supported instruments:
• D8 ENDEAVOR, D8 ADVANCE, D8 DISCOVER
Dynamic beam components:

• Motorized Divergence Slits
• Variable Active Detector Window
 Fully software controlled / synchronized, no user-intervention required

 Not all 3 components are required. All dynamic beam components may also
be operated independently (unsynchronized) or in any dual combination
(synchronized) - at the user's discretion
May 5, 2020 20
Upgrades
Dynamic beam components:

• Motorized Divergence Slits
• Most instruments are already equipped with motorized slits
• Upgrade recommended when beam spillover is an issue or to reduce measurement
time
• The core component of Dynamic Beam Optimization with the highest benefit in
terms of data quality
• "Must have" to effectively minimize air scattering, specifically when using
Motorized Divergence Slits
• Variable Active Detector Window
• Recommended for data acquisition at angles <5° 2θ only
• Always included with the SSD160-2, LYNXEYE-2, LYNXEYE XE, LYNXEYE XE-T and
EIGER2 R 500K detectors. No upgrade required.
• Not available for SSD-160 and LYNXEYE detectors
Please contact your local Bruker AXS office

or contact us via info.baxs@bruker.com
May 5, 2020 21
Outline

Wrap-up
May 5, 2020 22
3 Things to Remember
1. Dynamic beam optimization allows to acquire data virtually free of

air, instrument, and sample support scatter
2. Dynamic beam optimization significantly enhances lower limits of

detection and enables accurate quantification of minor crystalline
and amorphous phases
3. Dynamic beam optimization delivers unparalleled data quality for

materials with low angle peaks (large d-spacings) such as clays,
pharmaceuticals, zeolites, and porous framework materials
May 5, 2020 23
Any Questions?
info.baxs@bruker.com
Coming next:
"Sorry we won’t see you at EPDIC. Join our digital luncheon!"
May 25th, 1:30 to 3pm (CET)
May 5, 2020 24
Innovation with Integrity
© Copyright Bruker Corporation. All rights reserved.

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Perfect Powder Diffraction Data Automatically: