Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

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Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

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Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2). Powder Diffraction Methods • Qualitative Analysis – Phase Identification • Quantitative Analysis – Lattice Parameter Determination – Phase Fraction Analysis • Structure Refinement – Rietveld Methods - PowerPoint PPT Presentation

Transcript of Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Page 1: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Phase Identification by X-ray Diffraction(From Chapter 9 of Textbook 2)

Page 2: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Powder Diffraction Methods• Qualitative Analysis– Phase Identification• Quantitative Analysis– Lattice Parameter Determination– Phase Fraction Analysis• Structure Refinement– Rietveld Methods• Structure Solution– Reciprocal Space Methods– Real Space Methods• Peak Shape Analysis– Crystallite Size Distribution– Microstrain Analysis– Extended Defect Concentration

Page 3: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

1930’sHanawalt, Rinn and Frevel (Dow Chemical): diffraction data on about 1000 compounds

JCPDS, ICDD: Joint Committee on Powder DiffractionStandards; 1978 was renamed International Center forDiffraction Data.

Hanawalt Method: (Grouping scheme) values of the three strongest lines (d1, d2, d3) and intensities (I/I1)

Page 4: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

lowest-angle linethree strongest lines

Filenumber

data ondiffraction

method used

optical andother data

data onspecimen

diffraction pattern

crystallographicdata

Chemical formula andname of substance

Specialsymbol

Page 5: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Special symbols give extra information:

*: well-characterized chemistry, quantitative measure of intensity, high-quality d-spacing data (3 to 4 significant digits, no serious systematic errors) i: reasonable range and even spread of intensity, “sensible” completeness of the pattern, good d-spacing data (3 significant digits) o: low precision data, possible multi-phase mixture, possible poor chemical characterization c: powder pattern calculated from structural parameters

Page 6: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Procedure

(1) Locate proper d1 group(2) Find the closest match to d2 (±0.01 Å)(3) Follow by matching d3

(4) Compare relative intensity(5) Good agreement in search manual locate the proper PDF card compare the d and I/I1values of all the peaks

Page 7: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Examples: unknown pattern from measurement:

strongest lines in the powder pattern:d1 = 2.82; d2 = 1.99; d3 = 1.63

Page 8: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Portion of the ICDD Hanawalt search manual:

d1 = 2.82; d2 = 1.99; d3 = 1.63

Matched, turn to card number 5-628

Page 9: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

higherIntensity?

AbsorptioneffectNot

listed

Very weak K

(220) plane

Discrepancies!!

2×2.18×sin = 1.54 = 20.68o

2×d×sin 20.68o = 1.392 d = 1.97

Page 10: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Identification of Phases in Mixtures

d: 3.01 2.47 2.13 2.09 1.80 1.50 1.29 1.28I/I1: 5 72 28 100 52 20 9 18

d: 1.22 1.08 1.04 0.98 0.91 0.83 0.81I/I1: 4 20 3 5 4 8 10

No substance matching (d1:2.09; d2:2.47; d3: 1.80) all together probably a mixture Assume: d1 and d2 not the same phase. d1 and d3 the same phase find Cu Check the Pattern of Cu:

d: 2.088 1.808 1.278 1.090 1.044 0.904 0.830 0.808I/I1: 100 46 20 17 5 3 9 8

Examples: pattern of unknown

Page 11: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Remainder of pattern of unknown:

d: 3.01 2.47 2.13 1.50 1.29 1.28 0.98I/I1: 5 72 28 20 9 4 5I/I1: 7 100 39 28 13 6 7 Normalized

Following the steps of searching again Cu2O

Page 12: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Overlapped diffraction lines carefully subtract theintensity from the already identified phases to helpfurther identification of other phases.

Example

Page 13: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)
Page 14: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Computer searching of the PDF: Computerization has dramatically improved the efficiency of searching the JCPDS database Cards are no longer printed –data are on CD-ROM Numerous third-party vendors have software for searching the PDF database Computerized “cards” can contain much more crystallographic information Database is still expanding … New approach – whole pattern fitting

Page 15: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Specialsymbol

Page 16: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

Searching of the PDF requires high-quality data

Accurate line positions are a must!Calibration of camera and diffractometer with standardsCareful measurement of line intensitiesElimination of artifacts (e.g. preferred orientation)Solid solutions and strains shift peak positions“Garbage in, garbage out” Errors in database

Page 17: Phase Identification by X-ray Diffraction (From Chapter 9 of Textbook 2)

EVA software

TOPAS software


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