X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph...

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X-ray Diffraction - Solving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist

Transcript of X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph...

Page 1: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

X-ray Diffraction -Solving Problems with Phase Analysis

Joseph R. Swider, Ph.D.Senior Research Scientist

Page 2: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Uses of X-ray Diffraction

• phase identification of materials- different phases of materials with the same elemental composition can have extremely different properties

• commonly used for inorganics but many organics can be identified

• degree of crystallinity

Page 3: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Elemental and Phase

Identification

Phase: how are the atoms in a sample arranged?

TiO2

brookite

anataserutile

Elemental: What is the amount of each element in a sample?

TiO2

Mass Percent:60% Ti40% O

Page 4: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Phase IdentificationCalcium carbonate

CaCO3

calcitearagonite

Page 5: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

XRD Theory

• X-rays acting as waves interfere with each other, constructively or destructively

• A bright reflection occurs when the path length difference is an integral number, or

nl = 2d sin q

q q

d

Page 6: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Powder XRD

single crystal

powder sample

Page 7: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

XRD Instrumentation

X-ray source

sample

detection

CCD

film

Page 8: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

XRD Data

Page 9: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

International Centre for Diffraction

Data (ICDD)

Page 10: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Rigaku Micro-XRD

• Rotating anode

• Image plate detection

• Particles in the 100 -10µm size range

• 100µm beam size

Page 11: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Extraction and Mounting Particles

for micro-XRD

Page 12: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase
Page 13: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase
Page 14: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Other XRD Sample Mounting

Page 15: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Sample Submission

• What form is the sample?

– Bulk

– Powder

– Particle(s) to be extracted

• Will elemental analysis (EDS) be required?

• What data analysis will be needed?

– Comparison to ICDD

– Relative crystallinity

– Comparison to standards

Page 16: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Common Requests

Pharmaceutical verification

USP method <941>

Contamination identification

Corrosion products

Paint and pigments

Organics

Crystallinity

Page 17: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Limitations

**Quantitative XRD

**Percent crystallinity

Indexing

Single crystal analysis

Cryo or low temperature

In situ samples larger than ~1cm

Page 18: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Pigments and Paint

Phthalocyanine Blue

Synthetic Ultramarine Blue

Prussian Blue

Page 19: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Crystallinity

crystalline

semi-crystalline

amorphous

Page 20: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

20 µm particle

Page 21: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

10 µm mineral

Page 22: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Corrosion

Identification

Page 23: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Fresco Deterioration

• Several frescoes in a university hall were cracking with numerous accretions or spall

• Architectural conservators wanted to identify the spall-this would indicate what materials were underneath the painted layer and source the problem

• Samples of spall and from an intact fresco tested for the presence of gypsum

Page 24: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Sample 1 with spall

Sample 2 intact

Page 25: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase
Page 26: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Surface Contamination

Page 27: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase
Page 28: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Particles Removed from

Cross-Section Layers

High-Resolution Imaging and ElementalScanning Electron Microscopy with

Energy Dispersive X-ray Spectrometry (SEM/EDS)

Optical Properties and ImagingLight Microscopy (LM)

Organic ClassificationFourier-Transform Infrared Spectroscopy (FTIR)

Phase IdentificationX-ray Diffraction (XRD)

Organic QuantificationGas, Liquid Chromatography

Raman Microscopy

Raman Microscopy

Polarized Light Microscopy (PLM)

Page 29: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Cross-Section Evaluation

1

3

2

Page 30: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Test Painting

• Simple primed canvas with three layers of known pigment and media or commercial paint

• Sections taken and the layers analyzed for pigment and media by particle

• Not embedded in epoxy

Page 31: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Test Painting Area 1

Titanium white

Zincite

Barite

Rutile

Prussian Blue

1 23

Cadmium Yellow Light

Page 32: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Test Painting Area 3

3

2

1

Burnt Sienna in oilHematite, quartz, barite

Prussian Blue Hue watercolor

copper and iron phthalocyanines

indigo in linseed oil

barite

Page 33: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Architectural Lead Paint Identification

• Elemental (EDS or XRF) will identify Pb in paint structures or layers from samples but will not determine if it is white lead carbonate, the white pigment discontinued from industrial paints and known to be a health hazard

• Received samples as polished mounts with EDS map and Pb-rich layers to sample for identification of white lead carbonate

• Particles removed from chips or dust wipes can confirm the presence of white lead carbonate

Page 34: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Polished Mounts

8

10

1816

Page 35: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

15th

century Spanish panel

painting

Page 36: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Painting

Sample

4

5

3

2

1

Page 37: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Sample 1, Layer 2

Layer 2 , blue

Page 38: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Particle from Layer 4

Page 39: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Joseph R. Swider, Ph.D.Senior Research Scientist

[email protected]• (630) 887-7100

Thank you for joining us.

Page 40: X-ray Diffraction - Solving Problems with Phase AnalysisSolving Problems with Phase Analysis Joseph R. Swider, Ph.D. Senior Research Scientist. Uses of X-ray Diffraction • phase

Layer 2, red

Sample 2, Layer 2


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