Phase ID with 1D & 2D Detectors

Phase ID with Linear/Area Detectors

Comparison of geometry and data from 0D/1D/2D

Bob B. He Topics discussed in the ICDD 1D and 2D Detector Task Group Meeting Optics and Geometry Defocusing and resolution Preferred orientation and relative intensity

Page .1 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

Comparison of 0D, 1D and 2D Detectors

PSD GADDS

scintillation detector

small spot measured scan necessary long measuring time

large 2 range measured simultaneously medium measuring time

large 2 and chi range measured simultaneously measurement of oriented samples very short measuring times intensity versus 2 by integration of the data

Page .2 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

1D2D: Soller slits can be used for 0D and 1D

In cases of 0D and 1D, the intensity is a superposition of slices from diffraction ring, all same geometry condition. All within diffractometer plane and same Lorentz polarization and absorption correction.
Page .3 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

No soller slits can be used for 2D - point beam is required

XRD2:

Smearing effect from line focus beam

Diffraction rings from point focus beam

Page .4 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

Phase ID: -integration with merged frames

Out of diffractometer plane and different Lorentz polarization and absorption correction at different angle.
Page .5 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors Bragg-Brentano Geometry Conventional X-ray Diffraction

Page .6 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

2D detector for phase ID at various 2 angles

Diffraction pattern is measured at different detector swing angle to cover different 2 range.
Page .7 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D XRD2: Data Collection: Detectors Acetaminophen powder

5 second data collection 30 second data collection

Lin (Cps)

10

20

30

40

2-Theta - Scale
Page .8 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

Defocusing with 1D or 2D detectors Capillary smaller than beam size

Reflection mode

Transmission mode
Page .9 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2: No slits or monochromator in front of the

detector to stop air scatter or fluorescence
Air scatter from the incident beam

Open incident beam path

Air scatter from the diffracted beam

Page .10 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2 :
Defocusing at low incident angle in reflection

Lower resolution when 2 or (2-) 90

B sin 2 sin(2 ) = = b sin 1 sin

Page .11 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

Defocusing effect with reflection sample depends on detector and data collection strategy

XRD2:

Cylinder detector with 5 incident angle for 5~80 2

Flat detector with several (5,15,25,35) incident angles for 5~80 2

Page .12 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

Defocusing effect with reflection sample depends on detector and data collection strategy
12 10 Defocusing Factor 8 6 4 2 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 T wo T heta
Page .13 Bob He, 2004 Bruker AXS All Rights Reserved

XRD2:

Defocusing vs. Detectors

Cylinder detector may collect large 2 range, but with large defocusing effect at high 2 angle
Flat Cylinder BB

Defocus effect can be minimized with data collection strategy

Phase ID with 1D & 2D Detectors XRD2: reflection vs. transmission

Reflection mode frame from corundum at 5 incident angle.

Transmission mode frame with perpendicular incident beam.

Page .14 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with Reflection and Transmission Data Collection: 1D & 2D Detectors

Ibuprofen powder
10 second overall data collection
1.5

1.4

1.3

1.2

1.1

1.0

Lin (Cps)

0.9

0.8

0.7

0.6

0.5

0.4

0.3

R T T
3
10
20
30

0.2

0.1

2-Theta - Scale
Page .15 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

0D/1D/2D: Samples with preferred orientation

Bragg-Brentano Configuration. Diffraction vector parallel to sample normal

Same 2 with unsymmetrical incident and diffracted angles

1D detector with one incident angle but a range of diffracted angles

Page .16 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

0D1D2D: Samples with preferred orientation

Random powder sample with same relative intensity at all angles

Sample with preferred orientation (fiber texture), relative intensity varies with angles
Page .17 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

1D: Relative intensity with preferred orientation

15% 10% 5% 0% -5% -10% -15% -20% 25.576 35.149 88.993 95.249 127.68 136.08

Relative Intensity from Linear Detectors)

The relative intensities from NIST 1976 are measured with 6 line detectors. The vertical scale is the deviation from the relative intensities measured with Bragg-Brentano system The 6 detectors show consistent deviations due to preferred orientation in NIST 1976.
Page .18 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

0D/1D/2D:

2 resolution between 0D/1D/2D XRD

In BB system, the resolution can be changed with incident and receiving slits. No slits can be used in front of 1D/2D to improve the resolution. In addition to the condition of the incident X-ray beam, the resolution is determined by the detector spatial resolution and distance. The spatial resolution depends on the point spread function and the pixel size.

Page .19 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

1D/2D: Point Spread Function and Resolution

Consider a very small diffraction spot (blue linedelta function) An adjacent spot red line

A perfect detector - dashed blue line. A real detector - intensity in a spread distribution. Can be measured if the separation is larger than FWHM.
Page .20 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 2D detector resolution: K1-K2 split 1D & 2D Detectors

at 35 2 with NIST1976 (measured with VNTEC-2000)

(K2-K1) 2=0.06 210 m on the detector (20 cm)

Page .21 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

Summary

Many advantages of 1D and 2D detectors, such as high speed, high sensitivity and angular coverage in direction, have been recognized by XRD users. The discrepancy between diffraction patterns from conventional Bragg-Brentano system and diffractometers with 1D and 2D detectors can be analyzed and corrected. The instrument parameters for systems with 1D and 2D detectors should be investigated and considered in qualitative and quantitative phase analysis.

Page .22 Bob He, 2004 Bruker AXS All Rights Reserved

Phase ID with 1D & 2D Detectors

XRD2:

References

Philip R. Rudolf and Brian G. Landes, Two-dimensional X-ray diffraction and scattering of microcrystalline and polymeric Materials, Spectroscopy, 9(6), pp 22-33, Jul/Aug, 1994 B. B. He and U. Preckwinkel, X-ray optics for two-dimensional diffraction, Advances in X-ray Analysis, Vol. 45, 2001. B. He, Satish Rao, and C.R. Houska, A simplified procedures for obtaining relative x-ray intensities when a texture and atomic displacements are present, J. Appl. Phys. Vol. 75, No 9, May 1994. B. B. He, Introduction to two-dimensional X-ray diffraction, Powder Diffraction, Vol. 18, No 2, June 2003.

Page .23 Bob He, 2004 Bruker AXS All Rights Reserved