05 Leoni M

Line Profile Analysis in the 3rd millennium: what can we learn from peak profile shape?
Enemies in structure solution

7000
Nanocrystalline ceria
Defects in Structural Materials - Diamond Light Source 29-09-2009
6000
Intensity (counts)
Broad peaks Angle-dependent broadening
5000 4000 3000 2000 1000 0 20 40 60 80 100 120 140

5000 4500 4000
Pattern features determined by the microstructure (i.e. presence of defects)
2 (degrees)
Poorly ordered Kaolinite KGA-2
Intensity (counts)
3500 3000 2500 2000 1500 1000 500 0 10 20 30 40 50 60 70 80
diffraction band
Those features are considered as a nuisance by most scientists!
2 (degrees)
How to analyse analyse? ? Peak fitting

What most scientists know about XRD data processing in the XRD community
Parameters
ARBITRARY bell-shaped functions
Nonlinear least squares routine
exptl data
Processing of fit parameters
BINGO! Major problems: profile functions are arbitrary, physical meaning of profile data
In the Rietveld method an alternative?

Most widely used tool for the analysis of diffraction patterns.
yic ( 2 ) = yib + s mk LPk Fk G ( ik )

2 k
Some Rietveld codes modified through the years to introduce microstructure and stacking effects (BGMN, MAUD, Fullprof,Topas, partly GSAS). Models are usually simple and effective.We have two worlds: Microstructure (domains, microstrain,) Structure/microstructure interplay (layered systems..)
All software can deal with the first; TOPAS can effectively reproduce diffraction bands, BGMN can go little further. There is usually a big limit: Rietveld method considers Bragg scattering on 3D periodic lattice (does not consider whats in between lattice points.. diffuse scattering)
Scherrer formula, Williamson Williamson-Hall plot

What most Rietveld codes and most scientists use for microstructure analysis is Williamson-Hall plot i.e. Scherrer formula (1918) for average size determination and differential of Bragg law for microstrain determination
(d
)=
K L
+ 2
2 1/ 2
d*
(d ) (10 )
-1
-2
2
2 1/2
intercept related to average domain size
slope = 2< > intercept = 1/KL
slope related to microstrain Integral Breadth or Full Width At Half Maximum of the peak
0 0.0
0.2
0.4
d ( )
-1
0.6
0.8
1.0
average domain size is NOT the average size of the (nano) particles microstrain is a quite general term and does not identify the defect types
What most people do (unconsciously)

In traditional methods of analysis we loose the direct contact with the experimental data
EXTRACTION
ANALYSIS
Diffraction Pattern Profile parameters: FWHM, b, Fourier Coeff. ...
Microstructure Parameters
arbitrary bell-shaped function
some models
It is a two-step forward procedure. We analyse some profile parameters and not the data! The backward traceability (self consistence) is seldom (almost never) checked!
A FIRST KNOWN SOLUTION IN THE XRD COMMUNITY
Whole Powder Pattern Modelling

Some arbitrary hypotheses removed by directly modelling the whole pattern in terms of physical models of the microstructure
MODELLING
Physical models
Diffraction Pattern
Nonlinear least squares
Microstructure Parameters
WPPM
It is a self-consistent one-step procedure: fine details in the pattern can be unveiled. We do not care about structure, i.e. there are no structural constraints (peak intensity is a fitting parameter)
WPPM basics
Pattern as sum of broadened peaks + background +
20
30
2 (d e g re e s )
40
50
60
a kind of Pawley or Rietveld-like approach BUT.
WPPM basics
Each profile synthesised (in reciprocal space) from its Fourier transform calculated by physical modelling of all broadening sources
Fourier space (complex Fourier profile)
reciprocal space (diffraction peak)
2 space (diffraction peak)
Fourier transform
Space remapping
WPPM basics
Broadening sources we frequently meet
instrument
dislocations
Emission Profile
W
0.18 domain-size distribution 0.16 0.14 0.12
stacking faults
domain shape
frequency
0.10 0.08 0.06 0.04 0.02 0.00 0 10 20 30 40
D (nm)
WPPM basics
Broadening effects are convoluted. In Fourier space convolution is transformed into product. The intensity can be written as:
I{hkl} d * , d{*hkl} = k d * whkl

hkl
( )
hkl ( L) exp ( 2 iL shkl ) dL

Therefore, Fourier Transforms of the various effects are multiplied:
Diffraction profiles result from a convolution of effects.
IP F F APB GSR GSR CF CF TpV A{Shkl} A{D ( A + iB ) A ( A + iB ) ( A + iB hkl hkl hkl hkl hkl hkl ) ... hkl} {hkl}
Instrumental Profile Domain size
Faulting
APB
Stoichiometry fluctuations
Dislocations
Grain surface relaxation
Additional line broadening sources can be included through the corresponding FTs
WPPM fingerprint of effects

I{hkl} d * , d{*hkl} = k d * whkl
( )
hkl
hkl ( L) exp ( 2 iL shkl ) dL
IP F F APB GSR GSR CF CF TpV A{Shkl} A{D ( A + iB ) A ( A + iB ) ( A + iB hkl hkl hkl hkl hkl hkl ) ... hkl} {hkl}
IP pV
Sample independent (fixed parameters from a profile standard powder) Depends on grain shape and size distribution (may depend on {hkl}) Only superstructure {hkl} profiles are affected (with a specific law) on the diffraction profile sub-components
A{Shkl}
A{APB hkl}
F F Complex hkl dependence Ahkl , Bhkl
A{D hkl}
Depends on {hkl} through Chkl according to the Laue group invariant.
WPPM EXAMPLES
Nano CeO2 - TEM

CeO2 xerogel calcinated at 400C for 1h Grains are almost spherical and well separated
40 35 30 25 20 15 10 5 0 0 2 4 6 8 10 12
TEM (average over 800 grains)
Frequency
Grain diameter (nm)
Nano CeO2 WPPM (lab data)

7000
Intensity (counts)
6000 5000 4000 3000 2000 1000
Peaks are NOT fitted with Voigtians
<D> =4.4(6) nm
0 20 40 60 80 100 120 140
1.4(9)1016 m-2
2 (degrees)
40 35 30
TEM WPPM
Frequency
25 20 15 10 5 0 0 2
Grain diameter (nm)
10
12
ca. 1 dislocation every 3-4 grains
Annealing kinetics
Advantage of using defect density: not affected by the recrystallization / grain coarsening transition. Milled Fe1.5Mo at different heating rates (2.5, 7.5, 15 K/min)
3.60
Heating rate
Dislocation density (10 m )
16
3.00 2.40 1.80 1.20 0.60 0.00 0
recovery
2.5 C/min 7.5 C/min 15 C/min
-2
recrystallization?
100 200 300 400 500 600 700 800 900 1000
ESRF ID31
T (C)
Annealing kinetics
Activation energy via Kissinger method
XRD
(=> GB diffusion)
-12
DTA
(=> self diffusion)
15
-10.5 -11.0
7.5
ln(/T2flex)
-13
ln(/Tpk)
-11.5 -12.0
2.5
-12.5
-14 0.90 0.92 0.94 0.96 0.98 1.00 1.02
1.16
1.17
1.18
1.19
-1
1.20
1.21
1000/Tflex (K-1)
1000/T (K )
QXRD = 116 +/- 12 kJ/mol
QDTA = 338 +/- 73 kJ/mol
Microstructure stabilisation (SR data)

Improvement of Fe1.5Mo resistance via grain boundary pinning (1.5%SiO2)
ESRF ID31
110 3.5 3.0 2.5 2.0 1.5 1.0
90 80 70 60 50 40 30 20 10 0 0 100 200 300 400 500 600 700 800 900 1000
Dislocation density [x 10 m ]
(J/m )
2
Mean domain size <D> [nm]
16
-2
100
+1.5%SiO2
4.0
1.4
+1.5%SiO2
Temperature [C]
1.2
0.5
1.0
0.8
0.6
0.4
Grain boundary energy calculated assuming Geometrically Necessary dislocations (grain boundary dislocations)
0.2
0.0 0 100 200 300 400 500 600 700 800 900 1000
T (C)
SiSi -nc in oxycarbide glass - luminescence

ESRF ID31
1.0
1h @ 1100C 0.8 0.6 0.4 0.2 0.0 0 5 10 2h @ 1100C 1h @ 1200C
WPPM
1.1 1.0
1h @ 1100C
p(D)
0.9 0.8 0.7
PL
0.6 0.5 0.4
2h @ 1100C 1h @ 1200C
15
20
0.3 0.2 0.1
D (nm)
Literature
0.0 200
400
600
800
1000
wavelength (nm)
SiOC glass
Si
HOWEVER, WPPM CANNOT SOLVE ALL PROBLEMS!
I have a dream...
We would like to have a tool:
To model odd data (structures with extended defects) [considering the physics of microstructure, like WPPM] Able to deal with local and long range effects [like the Pair Distribution Function (PDF)] Flexible as the Rietveld method Being able to work directly on the measured data (and not on whatsoever extracted information) [not the traditional LPA, no PDF] Making use of a priori information I may have Being freely available
First step step: : getting rid of 3D periodicity

We should change the point of view! Structure and microstructure can be very close relatives!
Traditional approach (e.g. Rietveld)
Alternative approach
3D periodic lattice 3D periodic case only periodic defects!
2D periodic lattice Layer disorder
Interlayered systems Modular sets Ion substitution/ordering ... Modulated structures?
M. Leoni, A.F. Gualtieri, N. Roveri Simultaneous refinement of structure and microstructure of layered materials. J. Appl. Cryst. 37 (2004), 166-173
Second step: getting back to childhood
Combine the two and obtain DIFFaX+

DIFFaX+ is a structure/microstructure refinement code based on the same recursive algorithm of DIFFaX (corrected and extended)
Layer remapping Soft constraints Emission profile
Spurious reflections
starting parameters
RAW data
Pauling rules
Aberrations Texture Bond valence data Crystallographic handling
Full pattern synthesis for <3D periodic lattices
Nonlinear least squares engine Markov chain layers information refined parameters WinplotR out CIF structure
Polyhedra constraints
size/strain contribution
DIFFaX+
Pattern synthesis for <3D periodic lattices
Generation of equivalent positions for atoms in the cells
Starting definition of layers (asymmetric unit , group, transitions, sacking vectors) X-rays (lab and synchro) Neutrons (CW) Electrons Evaluation of the profile shape considering instrument, finite domain size and stacking defects
Calculation of layer structure factors
Treacy et al. recursion formula and Fast integration in reciprocal space
Diffraction pattern
M. Leoni, A.F. Gualtieri, N. Roveri Simultaneous refinement of structure and microstructure of layered materials. J. Appl. Cryst. 37 (2004), 166-173 M.M.J. Treacy, J.M. Newsam, M.W. Deem, A general recursion method for calculating diffracted intensities from crystals containing planar faults. PRS. Lond. A (1991) 433, 499-520 .
DIFFaX+ as LEGO: modular materials

The overall structure can be defined in a modular way, specifying any detail of the objects to be stacked,This is a possible example of a complex supercell
...
B
layer
Stacking direction <001>
Stacking vector 2/3 1/3 1
LAYER 5 = 2 MIRROR Y
LAYER 4 = CELL 3
<001>
0 0 1
LAYER 3 = VOID z
B A
<001> <001> <111>
0 0 0.85 0 0 1 0 0 1
LAYER 2 = CELL 2 LAYER 1 = CELL 1 x
Stacking modes and probabilities

Objects
Transition vectors
B A B
(0,0,1)
(0,0,1)
(0,0,1)
(0,0,1)
Probability matrix
P= AA BA AB BB AA AB ... probability that the block A is followed by A probability that the block A is followed by B
Perron-Frobenius theorem for Markov chains: Pn probability after n steps
When Mother Nature plays

Nano chrysotile
G. Falini, E. Foresti, M. Gazzano, A.F. Gualtieri, M. Leoni, I. G. Lesci, N. Roveri, "Tubular-shaped stoichiometric chrysotile nanocrystals", Chem. Eur. J. 10 (2004), 3043-3049.
Diffraction pattern of nano nano-chrysotile

Modelling done by assuming the cylindrical lattice planes as quasi-randomly stacked.
7000
6000
5000
Intensity (counts)
no b shift b shift 1/4 b shift 1/3 b shift 1/2 b shift 2/3 b shift 3/4
4000
3000
2000
1000
20
40
60
80
2 (degrees)
AVAILABILITY
Acknowledgements
The WPPM method has been developed by P. Scardi and M.Leoni. The PM2K software has been developed by M.Leoni with the help of T. Confente and M. Ortolani.The software testers and co-developers are greatly acknowledged: Mirco DIncau Matteo Ortolani Emmanuel Garnier DIFFaX+ is mainly a hobby project. The contribution from volunteers is therefore essential. Several people need to be deeply acknowledged for their encouragement and invaluable help. Among them, a special thank to: Alessandro Gualtieri Norberto Roveri Rune Johnsen Kristin Schoenau Gerhard Miehe Andreas Leineweber Marie-Pierre Crosnier-Lopez Franoise Le Berre Simone Ferrari Carlos de la Calle Arancha Argelles Velez Juan Carlos Corona
REFERENCES
References (WPPM)
[1] P. Scardi, plenary talk at EPDIC-7, Barcelona, 20-23.05.2000. In P. Scardi, Y.H.Dong, M.Leoni, Line profile analysis in Rietveld method and Whole Powder Pattern Fitting, Mat. Sci. Forum 378-381 (2001) 132-139. [2] P. Scardi, M. Leoni, Y.H. Dong, Whole diffraction pattern-fitting of polycrystalline fcc materials based on microstructure, Eur. Phys. J. B 18 (2000) 23-30.
[3] P. Scardi, M. Leoni, Y.H. Dong, Whole Powder Pattern Modelling, CPD Newsletter 24 (2000) 23-24. ISSN 1591-9552. [4] P. Scardi and M. Leoni, Whole Powder Pattern Modelling: theory and application, in: Diffraction Analysis of the Microstructure of Materials, edited by E. J. Mittemeijer & P. Scardi, Springer Series in Materials Science, Vol. 68. (SpringerVerlag, Berlin, 2004). ISBN 3-540-40519-4. p. 51-91. [5] P. Scardi, M. Leoni, Diffraction line profiles from polydisperse crystalline systems. Acta Crystallographica A57 (2001) 604-613. [6] P. Scardi & M. Leoni, Whole powder pattern modelling . Acta Crystallographica A58 (2002) 190-200. [7] M. Leoni and P. Scardi, Surface Relaxation Effects in Nanocrystalline Powders, in: Diffraction Analysis of the Microstructure of Materials, edited by E.J. Mittemeijer and P. Scardi, Springer Series in Materials Science, Vol. 68. (SpringerVerlag, Berlin, 2004). ISBN 3-540-40519-4. p. 413-454. [8] M. Leoni & P. Scardi, Surface relaxation in nano-sized powders, CPD Newsletter 28 (2002) 21-22. ISSN 1591-9552. [9] M. Leoni, Grain surface relaxation and grain interaction in powder diffraction, Mat. Sci. Forum 443-444 (2004) 1-10. (EPDIC Award 2002 lecture) [10] P. Scardi & M. Leoni, Whole Powder Pattern Modelling for the study of Anti-Phase Domains, CPD Newsletter 28 (2002) 810. ISSN 1591-9552. [11] P. Scardi, Profile Modelling versus Profile Fitting in Powder Diffraction, Z. Kristallogr. 217 (2002) 420-421. [13] E. Estevez-Rams, M. Leoni, P. Scardi, B. Aragon-Fernadez & H. Fuess, On the powder diffraction pattern of crystals with stacking faults, Philosophical Magazine 83 [36] (2003) 4045-4057. [14] M. Leoni & P. Scardi, Nanocrystalline domain size distributions from powder diffraction data, J. Appl. Cryst. 37 (2004) 629-634.
References (WPPM)
[15] M. Leoni, R. Di Maggio, S. Polizzi & P. Scardi, An X-ray diffraction methodology for the microstructural analysis of nanocrystalline powders: application to cerium oxide. J. Am. Ceram. Soc. 87 (2004) 1133-1140. [16] P. Scardi, M. Leoni & R. Delhez, Line-broadening analysis using integral breadth methods: a critical review, J. Appl. Cryst. 37 (2004) 381-390.
[17] P. Scardi & M. Leoni, Diffraction whole-pattern modelling for the study of anti-phase domains in Cu3Au, Acta Mater. 53 (2005) 5229-5239. [18] P. Scardi, Microstructure and lattice defects in highly deformed metals by X-ray Diffraction Whole Powder Pattern Modelling, Z. Metall. 96 (2005) 698-702. [19] G. De Giudici, R. Biddau, M. DIncau, M. Leoni, P. Scardi, Reactivity of nanocristalline fluorite powders: defect density threshold, Geochimica et Cosmochimica Acta 69 [16] (2005) 4073-4083. [20] P. Scardi, M. Leoni, D. G. Lamas, E. D. Cabanillas Grain size distribution of nanocrystalline systems, Powder Diffraction 20 [4] (2005) 353-358. [21] P. Scardi & M. Leoni, Line profile analysis: pattern modelling versus profile fitting, J. Appl. Cryst. 39 (2006) 24-31. [Cited in IUCr Newsletter 14 (2006) 5] [22] N. Armstrong, M. Leoni & P. Scardi Some considerations concerning Wilkens theory of dislocation line-broadening, Z. Kristallogr. Suppl. 23 (2006) 81-86. [23] M. Leoni, T. Confente & P. Scardi, PM2K: a flexible program implementing Whole Powder Pattern Modelling, Z. Kristallogr. Suppl. 23 (2006) 249-254. [24] P. Scardi, M. Leoni, J. Faber, Diffraction line profile from a disperse system: a simple alternative to Voigtian profiles, Powder Diffraction 21 (2006). 270-277. [25] M. Leoni, G. De Giudici, R. Biddau, M. DIncau & P. Scardi Analysis of polydisperse ball-milled fluorite powders using a full pattern technique, Z. Kristallogr. Suppl. 23 (2006) 111-116. [26] P. Scardi, M. Leoni, Advances in line profile analysis for the study of nanocrystalline systems. ECS Transactions, Vol. 3 [9] (2006) 125-132. In: Nanostructured Metal Oxides: Processing and Applications, Editor(s): E. Traversa, G. Hunter, G. Oskam, R. Penn.
References (WPPM)
[27] P. Scardi, M. Leoni, M. DIncau, Whole Powder Pattern Modelling of cubic metal powders deformed by high energy milling, Z. Kristallogr. 222 (2007) 129-135. [28] P. Scardi, M. Leoni, G. Straffelini, G. De Giudici, Microstructure of Cu-Be alloy triboxidative wear debris, Acta Mater. 55 (2007) 2531-2538.
[29] P. Scardi, M. DIncau, M. Leoni, Full pattern methods for the analysis of plastically deformed materials, Solid State Phenomena 130 (2007) 27-32. [30] M. D'Incau, M. Leoni, P. Scardi, High energy grinding of FeMo powders, J. Mat. Research 22 (2007) 1744-1753. [31] S. Brimaud, C. Coutanceau, E. Garnier, J.-M. Lger, F. Grard, S. Pronier, M. Leoni, "Influence of surfactant removal by chemical or thermal methods on structure and electroactivity of Pt/C catalysts prepared by water-in-oil microemulsion", J. Electroanal. Chem. 602 [2] (2007) 226-236. [32] P. Scardi, Microstructural properties: lattice defects and domain size effects, Cap. 13 in: Powder Diffraction: Theory and Practice, edited by R.E. Dinnebier and S.J.L. Billinge. (The Royal Society of Chemistry, Cambridge, 2008). ISBN 978-0-85404231-9. p. 376-413. [33] M. Leoni, J. Martinez-Garcia & P. Scardi, Dislocation effects in powder diffraction, J. Appl. Cryst. 40 (2007) 719-724. [34] J. Martinez-Garcia, M. Leoni & P. Scardi, Analytical expression for the dislocation contrast factor of the <001>{100} cubic slip-system: application to Cu2O, Phys. Rev. B 76 (2007). 174117. [35] J. Martinez-Garcia, M. Leoni & P. Scardi, Analytical contrast factor of dislocations along orthogonal diad axes, Phil. Mag. Letters 88 [6] (2008) 443-451. [36] J. Martinez-Garcia, M. Leoni, P. Scardi, A general approach for determining the diffraction contrast factor of straightline dislocations, Acta Cristallogr. A, 65 (2009) 109-119. [37] H. Pesenti, M. Leoni, P. Scardi, XRD Line Profile Analysis of calcite powders produced by high energy milling, Z. Kristallogr. Suppl. 27 (2008) 143-150. [38] K. R. Beyerlein, A. Cervellino, M. Leoni, P. Scardi, Debye equation versus Whole Powder Pattern Modelling: Real versus reciprocal space modelling of nanomaterials, Z. Kristallogr. Suppl. (2009). In press
References (DIFFaX (DIFFaX+) +)

[1] M. Leoni, A. Gualtieri, N. Roveri Simultaneous refinement of structure and microstructure of layered materials. J. Appl. Cryst. 37 (2004), 166-173. [2] S. Ferrari, A.F. Gualtieri, G.H. Grathoff, M. Leoni, Model of disorder and structure refinement of illite, Z. Kristallogr. Suppl. 23 (2006) 493-498. [3] A. F. Gualtieri, S. Ferrari, M. Leoni, G. Grathoff, R. Hugo, M. Shatnawi, G. Paglia, S. Billinge, Structural characterization of the clay mineral illite-1M, J. Appl. Cryst. 41 (2008) 402-415. [4] M. Leoni, Diffraction analysis of layer disorder, Z. Kristallogr. 223 223 (2008) 561568. [5] A. Leineweber, M. Leoni, Refinement of layer-faulting in Nb2Co7 intermetallic compound using DIFFaX+, Z. Kristallogr. Suppl. (2009). In press. [6] A. Argelles, M. Leoni, C. H. Pons, C. De la Calle J. A. Blanco, C. Marcos, Structure and microstructure of Mgvermiculite, Z. Kristallogr. Suppl. (2009). In press. [7] M. Leoni, M.-P. Crosnier-Lopez, F.Le Berre, The chameleonic perovskite, 2009). Submitted.

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Line Profile Analysis in the 3rd millennium: what can we learn from peak profile shape?

Enemies in structure solution

Defects in Structural Materials - Diamond Light Source 29-09-2009

Broad peaks Angle-dependent broadening

5000 4000 3000 2000 1000 0 20 40 60 80 100 120 140

Pattern features determined by the microstructure (i.e. presence of defects)

Poorly ordered Kaolinite KGA-2

3500 3000 2500 2000 1500 1000 500 0 10 20 30 40 50 60 70 80

Those features are considered as a nuisance by most scientists!

How to analyse analyse? ? Peak fitting

ARBITRARY bell-shaped functions

Nonlinear least squares routine

Processing of fit parameters

In the Rietveld method an alternative?

yic ( 2 ) = yib + s mk LPk Fk G ( ik )

Scherrer formula, Williamson Williamson-Hall plot

intercept related to average domain size

slope = 2< > intercept = 1/KL

What most people do (unconsciously)

Diffraction Pattern Profile parameters: FWHM, b, Fourier Coeff. ...

arbitrary bell-shaped function

A FIRST KNOWN SOLUTION IN THE XRD COMMUNITY

Whole Powder Pattern Modelling

Nonlinear least squares

a kind of Pawley or Rietveld-like approach BUT.

Fourier space (complex Fourier profile)

reciprocal space (diffraction peak)

2 space (diffraction peak)

0.10 0.08 0.06 0.04 0.02 0.00 0 10 20 30 40

I{hkl} d * , d{*hkl} = k d * whkl

hkl ( L) exp ( 2 iL shkl ) dL

Diffraction profiles result from a convolution of effects.

Instrumental Profile Domain size

Grain surface relaxation

WPPM fingerprint of effects

hkl ( L) exp ( 2 iL shkl ) dL

F F Complex hkl dependence Ahkl , Bhkl

Depends on {hkl} through Chkl according to the Laue group invariant.

Nano CeO2 - TEM

Grain diameter (nm)

Nano CeO2 WPPM (lab data)

6000 5000 4000 3000 2000 1000

Peaks are NOT fitted with Voigtians

Defects in Structural Materials - Diamond Light Source 29-09-2009

0 20 40 60 80 100 120 140

Grain diameter (nm)

ca. 1 dislocation every 3-4 grains

Dislocation density (10 m )

3.00 2.40 1.80 1.20 0.60 0.00 0

2.5 C/min 7.5 C/min 15 C/min

QXRD = 116 +/- 12 kJ/mol

QDTA = 338 +/- 73 kJ/mol

Microstructure stabilisation (SR data)

Mean domain size <D> [nm]

SiSi -nc in oxycarbide glass - luminescence

Defects in Structural Materials - Diamond Light Source 29-09-2009

1h @ 1100C 0.8 0.6 0.4 0.2 0.0 0 5 10 2h @ 1100C 1h @ 1200C

0.9 0.8 0.7

0.6 0.5 0.4

0.3 0.2 0.1

HOWEVER, WPPM CANNOT SOLVE ALL PROBLEMS!

First step step: : getting rid of 3D periodicity

I{hkl} d * , d{hkl} = k d whkl