Structural aspects. Povo (Trento), Italy. 1 Institute of Physics, Academy of Sciences of the Czech Republic, Prague
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1 Structural aspects of B K edge XANES of minerals O. Šipr, 1 A. Šimůnek, 1 J. Vackář, 1 F. Rocca, G. Dalba 3 1 Institute of Physics, Academy of Sciences of the Czech Republic, Prague Istituto di Fotonica e Nanotecnologie del CNR, Sezione ITC-CeFSA, Povo (Trento), Italy 3 INFM and Dipartimento di Fisica, Università di Trento, Povo (Trento), Italy p.1/3
2 Outline Introducing XANES technique p./3
3 Outline Introducing XANES technique Spectra of minerals with pure BO 3 or BO coordinations p./3
4 Outline Introducing XANES technique Spectra of minerals with pure BO 3 or BO coordinations Minerals with boron in both BO 3 and BO units p./3
5 Outline Introducing XANES technique Spectra of minerals with pure BO 3 or BO coordinations Minerals with boron in both BO 3 and BO units Search for markers of BO 3 and BO coordinations in XANES spectra p./3
6 Outline Introducing XANES technique Spectra of minerals with pure BO 3 or BO coordinations Minerals with boron in both BO 3 and BO units Search for markers of BO 3 and BO coordinations in XANES spectra Explore influence of technical parameters (scattering potential, core hole, size of cluster) p./3
7 Outline Introducing XANES technique Spectra of minerals with pure BO 3 or BO coordinations Minerals with boron in both BO 3 and BO units Search for markers of BO 3 and BO coordinations in XANES spectra Explore influence of technical parameters (scattering potential, core hole, size of cluster) Inspect prospective use of B K edge XANES in quantitative studies of structure of glasses p./3
8 X-ray absorption spectroscopy in a nutshell p.3/3
9 X-ray absorption spectroscopy x-rays are absorbed in the sample via a photoelectron effect more detection techniques are possible p./3
10 Taxonomy Low photoelectron energies ( 50 ev) XANES (X-ray Absorption Near Edge Structure) High photoelectron energies ( ev) EXAFS (Extended X-ray Absorption Fine Structure) p.5/3
11 Local probe Offers a view from one particular site (chemically selective) Outgoing photoelectron is scattered by the neighbors Constructive/destructive interference depending on interatomic distance p./3
12 EXAFS Several approximations possible in the EXAFS region Structural information can be straightforwardly extracted EXAFS oscillations are sometimes too faint to measure p.7/3
13 XANES Physics more complicated Some structural information is there but difficult to extract Fingerprinting may be dangerous (no unique correspondence between structural elements and spectral features) p.8/3
14 Theoretical framework Spectra calculated in a real space (finite clusters of atoms) p.9/3
15 Theoretical framework Spectra calculated in a real space (finite clusters of atoms) Full multiple scattering included p.9/3
16 Theoretical framework Spectra calculated in a real space (finite clusters of atoms) Full multiple scattering included True crystal geometry taken from literature, all atoms at correct positions (no simplification of the structure) p.9/3
17 Theoretical framework Spectra calculated in a real space (finite clusters of atoms) Full multiple scattering included True crystal geometry taken from literature, all atoms at correct positions (no simplification of the structure) Scattering potentials mostly non-self-consistent (Mattheiss prescription) [checked that self-consistent potentials yield similar results] p.9/3
18 Theoretical framework Spectra calculated in a real space (finite clusters of atoms) Full multiple scattering included True crystal geometry taken from literature, all atoms at correct positions (no simplification of the structure) Scattering potentials mostly non-self-consistent (Mattheiss prescription) [checked that self-consistent potentials yield similar results] Core hole treated statically (final state rule, relaxed and screened model) p.9/3
19 Minerals with only one boron site p.10/3
20 Minerals with only BO 3 units BO 3 B K edge XANES [arb. units] calciborite ludwigite vonsenite p.11/3
21 Minerals with only BO 3 units A B K edge XANES [arb. units] BO 3 C experiment theory calciborite ludwigite vonsenite Pre-peak followed by a main peak, about 10 ev apart p.11/3
22 Minerals with only BO units BO B K edge XANES [arb. units] danburite datolite sinhalite p.1/3
23 Minerals with only BO units BO B B K edge XANES [arb. units] experiment theory danburite datolite sinhalite Experiment: Main peak with a shoulder Theory: Single peak p.1/3
24 Basic typology A B BO 3 C BO B K edge XANES [arb. units] experiment theory calciborite ludwigite B K edge XANES [arb. units] experiment theory danburite datolite vonsenite sinhalite Characteristic shapes of XANES spectra depend on the presence of either BO 3 or BO unit p.13/3
25 Using various scattering potentials B K edge XANES of ludwigite non-scf pot no hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite non-scf pot rel & scr core hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite non-scf pot core hole "(Z+1) " experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential no hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential rel & scr core hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential core hole "(Z+1) " experiment (EELS) experiment (FY-XAS) theory p.1/3
26 Core hole effect at the pre-edge B K edge XANES of ludwigite non-scf pot no hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite non-scf pot rel & scr core hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite non-scf pot core hole "(Z+1) " experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential no hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential rel & scr core hole experiment (EELS) experiment (FY-XAS) theory B K edge XANES of ludwigite SCF potential core hole "(Z+1) " experiment (EELS) experiment (FY-XAS) theory p.1/3
27 Sinhalite does not quite follow the herd BO B B K edge XANES [arb. units] experiment theory danburite datolite sinhalite p.15/3
28 Sinhalite does not quite follow the herd BO B B K edge XANES [arb. units] experiment theory danburite datolite sinhalite Three B-O bonds of 1. Å, one bond of 1.58 Å it is rather a 3+1 coordination p.15/3
29 Cluster size effect BO 3 units ludwigite vonsenite B K edge XANES of ludwigite 7 51 exper B K edge XANES of vonsenite exper Spectra for clusters of atoms and of 50 atoms are very similar p.1/3
30 Cluster size effect BO 3 units ludwigite vonsenite B K edge XANES of ludwigite 7 51 exper B K edge XANES of vonsenite exper Spectra for clusters of atoms and of 50 atoms are very similar Fine structure between the pre-peak and the main peak is due to medium- and long-range order p.1/3
31 Cluster size effect BO units danburite sinhalite B K edge XANES of danburite exper B K edge XANES of sinhalite exper Spectra for clusters of 5 atoms and of 50 atoms again very similar p.17/3
32 Cluster size effect BO units danburite sinhalite B K edge XANES of danburite exper B K edge XANES of sinhalite exper Spectra for clusters of 5 atoms and of 50 atoms again very similar Pre-peak and shoulder do not appear for any size of cluster p.17/3
33 Pre-peak and shoulder for BO units B K edge XANES [arb. units] B danburite datolite Systematic deviations between theory and experiment p.18/3
34 Pre-peak and shoulder for BO units B K edge XANES [arb. units] B danburite datolite Systematic deviations between theory and experiment Pre-edge region XANES is prone to radiation damage just consequence of BO 3 defects? p.18/3
35 Pre-peak and shoulder for BO units B K edge XANES [arb. units] B danburite datolite Systematic deviations between theory and experiment Pre-edge region XANES is prone to radiation damage just consequence of BO 3 defects? Shoulder region: Displayed by none of the theoretical spectra at the BO sites. Disorder, impurities, main peak of BO 3 units,...? p.18/3
36 BPO is peculiar XANES of BPO does not fit into the typology B K edge XANES of BPO theory exper p.19/3
37 BPO is peculiar XANES of BPO does not fit into the typology B K edge XANES of BPO exper Spectra for small and large clusters differ considerably p.19/3
38 BPO is peculiar (and not useful) XANES of BPO does not fit into the typology B K edge XANES of BPO exper Spectra for small and large clusters differ considerably XANES governed by medium- and long-range order Too symmetric to smooth out the contributions from distant atoms p.19/3
39 BPO is peculiar (and not useful) XANES of BPO does not fit into the typology B K edge XANES of BPO exper Spectra for small and large clusters differ considerably XANES governed by medium- and long-range order Too symmetric to smooth out the contributions from distant atoms Not useful for fingerprinting XANES of glasses p.19/3
40 Minerals with borons in both BO 3 and BO units p.0/3
41 Minerals with both BO 3 and BO name formula BO 3 BO boracite Mg 3 ClB 7 O 13 1 borax Na B O 5 (OH) 8 (H O) 1 1 colemanite CaB 3 O (OH) 3 H O 1 howlite Ca SiB 5 O 9 (OH) 5 1 kernite Na B O (OH) 3 (H O) kurnakovite MgB 3 O 3 (OH) 5 5 (H O) 1 meyerhofferite Ca B O (OH) 10 (H O) 1 probertite NaCaB 5 O 7 (OH) 3 (H O) 3 tincalconite Na B O 5 (OH) 3 (H O) 1 1 ulexite NaCaB 5 O (OH) 5 (H O) 3 Spectra generated at inequivalent sites of the same system are aligned one to another by the theory p.1/3
42 Spectra of borons in BO 3 units 8 Sites with BO 3 coordination B K edge XANES [Mb] 13 sites, 10 minerals p./3
43 Spectra of borons in BO 3 units 8 Sites with BO 3 coordination B K edge XANES [Mb] average 7% 100% 13 sites, 10 minerals Confidence intervals either 7% or 100% of all curves fall within these limits p./3
44 Spectra of borons in BO units 8 Sites with BO coordination B K edge XANES [Mb] sites, 10 minerals p.3/3
45 Spectra of borons in BO units 8 Sites with BO coordination B K edge XANES [Mb] average 7% 100% sites, 10 minerals Confidence intervals either 7% or 100% of all curves fall within these limits p.3/3
46 Markers of BO 3 and BO B K edge XANES [Mb] 8 A B C average 7% 100% Features characteristic for BO 3 or BO coordinations well separated p./3
47 Markers of BO 3 and BO B K edge XANES [Mb] 8 A B C average 7% 100% Features characteristic for BO 3 or BO coordinations well separated Similar picture obtained no matter what scattering potential is used p./3
48 Markers of BO 3 and BO B K edge XANES [Mb] 8 A B average 7% 100% C Features characteristic for BO 3 or BO coordinations well separated Similar picture obtained no matter what scattering potential is used B K edge is well-suited for structural studies p./3
49 Short-range order is dominant B K edge XANES [Mb] 8 Large clusters A B C average 7% 100% B K edge XANES [Mb] 8 Small clusters A B C Clusters of 10 atoms and of or 5 atoms yield similar picture p.5/3
50 Short-range order is dominant B K edge XANES [Mb] 8 Large clusters A B C average 7% 100% B K edge XANES [Mb] 8 Small clusters A B C Clusters of 10 atoms and of or 5 atoms yield similar picture XANES shape is governed by short-range order p.5/3
51 Short-range order is dominant B K edge XANES [Mb] 8 Large clusters A B C average 7% 100% B K edge XANES [Mb] 8 Small clusters A B C Clusters of 10 atoms and of or 5 atoms yield similar picture XANES shape is governed by short-range order Results may be transferred from crystal to glasses p.5/3
52 Trying to make quantitative estimates p./3
53 Variations in peak areas (BO 3 ) 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range B K edge XANES [Mb] p.7/3
54 Variations in peak areas (BO 3 ) B K edge XANES [Mb] 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range For each peak, find deviation of its area from the average p.7/3
55 Variations in peak areas (BO 3 ) B K edge XANES [Mb] 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range For each peak, find deviation of its area from the average p.7/3
56 Variations in peak areas (BO 3 ) B K edge XANES [Mb] 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range For each peak, find deviation of its area from the average For 7% percents of peaks, their areas deviate from the average by less than % p.7/3
57 Variations in peak areas (BO 3 ) B K edge XANES [Mb] 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range For each peak, find deviation of its area from the average For 7% percents of peaks, their areas deviate from the average by less than % Maximum deviation from the average is about 1% p.7/3
58 Variations in peak areas (BO 3 ) B K edge XANES [Mb] 8 Sites with BO 3 coordination Measuring peak area over a 10 ev range For each peak, find deviation of its area from the average For 7% percents of peaks, their areas deviate from the average by less than % Maximum deviation from the average is about 1% Choice of scattering potential and other technical parameters does not matter p.7/3
59 Variations in peak areas BO B K edge XANES [Mb] 8 Sites with BO coordination Measuring peak area Find deviations from the average p.8/3
60 Variations in peak areas BO B K edge XANES [Mb] 8 Sites with BO coordination Measuring peak area Find deviations from the average p.8/3
61 Variations in peak areas BO B K edge XANES [Mb] 8 Sites with BO coordination Measuring peak area Find deviations from the average p.8/3
62 Variations in peak areas BO B K edge XANES [Mb] 8 Sites with BO coordination Measuring peak area Find deviations from the average Statistics similar as in the case of BO 3 sites Standard deviation of the area is %, maximum deviation from the average is 1% p.8/3
63 Quantifying ratio of BO 3 and BO 8 Sites with BO 3 coordination 8 Sites with BO coordination B K edge XANES [Mb] B K edge XANES [Mb] Area of the main peak depends only on the number of nearest oxygens p.9/3
64 Quantifying ratio of BO 3 and BO 8 Sites with BO 3 coordination 8 Sites with BO coordination B K edge XANES [Mb] B K edge XANES [Mb] Area of the main peak depends only on the number of nearest oxygens (it does not depend on compound, distances, middle-range order etc.) p.9/3
65 Quantifying ratio of BO 3 and BO 8 Sites with BO 3 coordination 8 Sites with BO coordination B K edge XANES [Mb] B K edge XANES [Mb] Area of the main peak depends only on the number of nearest oxygens (it does not depend on compound, distances, middle-range order etc.) Ratio of areas of main peaks is a measure of the ratio of three-fold and four-fold boron sites p.9/3
66 Quantifying ratio of BO 3 and BO 8 Sites with BO 3 coordination 8 Sites with BO coordination B K edge XANES [Mb] B K edge XANES [Mb] Area of the main peak depends only on the number of nearest oxygens (it does not depend on compound, distances, middle-range order etc.) Ratio of areas of main peaks is a measure of the ratio of three-fold and four-fold boron sites Normalization: Area of main spectral peak at a BO 3 site constitutes 75% of area of main spectral peak at a BO site p.9/3
67 Widths of main peaks BO 3 sites 8 Sites with BO 3 coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height p.30/3
68 Widths of main peaks BO 3 sites 8 Sites with BO 3 coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height (full width at 0. of maximum) p.30/3
69 Widths of main peaks BO 3 sites 8 Sites with BO 3 coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height (full width at 0. of maximum) Searching for any systematic dependence p.30/3
70 Widths of main peaks BO 3 sites 8 Sites with BO 3 coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height (full width at 0. of maximum) Searching for any systematic dependence p.30/3
71 Widths of main peaks BO 3 sites 8 Sites with BO 3 coordination 7 B K edge XANES [Mb] main peak width [ev] spread of B-O distances [A] No obvious relation between the spread of B O distances and the width of the main peak p.30/3
72 Widths of main peaks BO sites 8 Sites with BO coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height p.31/3
73 Widths of main peaks BO sites 8 Sites with BO coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height p.31/3
74 Widths of main peaks BO sites 8 Sites with BO coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height p.31/3
75 Widths of main peaks BO sites 8 Sites with BO coordination B K edge XANES [Mb] Measuring width of the peak at 0% of its maximum height p.31/3
76 Widths of main peaks BO sites 8 Sites with BO coordination 7 B K edge XANES [Mb] main peak width [ev] spread of B-O distances [A] There is some relation between spread of the B O distances in the BO tetrahedron and the width of the main peak p.31/3
77 Peak widths and spread of distances 7 7 main peak width [ev] 5 3 main peak width [ev] spread of B-O distances [A] spread of B-O distances [A] Peaks related to BO 3 and BO units behave differently in this respect p.3/3
78 Peak widths and spread of distances 7 7 main peak width [ev] 5 3 main peak width [ev] spread of B-O distances [A] spread of B-O distances [A] Peaks related to BO 3 and BO units behave differently in this respect Even for spectra at BO sites, there are significant deviations from the statistical relation p.3/3
79 Peak widths and spread of distances 7 7 main peak width [ev] 5 3 main peak width [ev] spread of B-O distances [A] spread of B-O distances [A] Peaks related to BO 3 and BO units behave differently in this respect Even for spectra at BO sites, there are significant deviations from the statistical relation Exceptionally large spread of B O distances yields exceptionally broad peak p.3/3
80 The end is getting near... p.33/3
81 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially p.3/3
82 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially The difference between XANES at BO 3 or BO sites stems from the short-range order p.3/3
83 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially The difference between XANES at BO 3 or BO sites stems from the short-range order The pre-peak in spectra of BO 3 sites is closely related to the core hole (hence not so useful for structural studies) p.3/3
84 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially The difference between XANES at BO 3 or BO sites stems from the short-range order The pre-peak in spectra of BO 3 sites is closely related to the core hole (hence not so useful for structural studies) BPO crystal is not a good model for structural studies of glasses p.3/3
85 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially The difference between XANES at BO 3 or BO sites stems from the short-range order The pre-peak in spectra of BO 3 sites is closely related to the core hole (hence not so useful for structural studies) BPO crystal is not a good model for structural studies of glasses Areas of main peaks depend only on the number of nearest oxygens can be used for quantifying ratio of borons in BO 3 or BO units p.3/3
86 Summary B K edge XANES of sites in BO 3 or BO coordinations differ essentially The difference between XANES at BO 3 or BO sites stems from the short-range order The pre-peak in spectra of BO 3 sites is closely related to the core hole (hence not so useful for structural studies) BPO crystal is not a good model for structural studies of glasses Areas of main peaks depend only on the number of nearest oxygens can be used for quantifying ratio of borons in BO 3 or BO units Width of main peak at BO site is related to the spread of B O distances (with a significant statistical noise for typical situations) p.3/3
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