Chalcogenide glasses compositions vs structure
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1 Chalcogenide glasses compositions vs structure A. Pradel Institut Charles Gerhardt Université de Montpellier, France
2 Chalcogenide glass formers Structure Comparison oxide / chalcogenide [SiO 2 /SiS(e) 2 ] Ion conducting chalcogenide glasses (Modifier + Former) Depolymerization of glassy network (edge sharing/corner sharing tetrahedra; bridging / non bridging sulfur/selenium); 29 Si NMR, XPS Phase separation in Ag + conducting chalcogenide glasses; Near field microscopy Mixed Glass Former Effect Heterogeneous versus homogeneous mixing; Li 2 S-SiS 2 -GeS 2 ; Raman, SAXS Mixed Alkali Effect Cation distribution in the glassy network; Li 2 S-Na 2 S-GeS 2 ; REDOR NMR Cation environment and glassy network rearrangement; Ag 2 S-Rb 2 S-GeS 2 ; Raman, EXAFS, SAXS Conclusions
3 Chalcogenide glass formers Role of chalcogen on the structure Homologous to SiO 2 and GeO 2 stoichiometric glasses SiS(e) 2, GeS(e) 2 Ia 0 1 H IIa IIIa IVa Va VIa VIIa 2 He 3 Li 11 Na 19 K 37 Rb 55 Cs 87 Fr 4 Be 12 Mg 20 Ca 38 Sr 56 Ba 88 Ra B IIIb IVb Vb VIb VIIB VIIIb Ib IIb 13 Al 21 Sc 39 Y 57 La 89 Ac 22 Ti 40 Zr 72 Hf 104 Unq 23 V 41 Nb 73 Ta 105 Unp 24 Cr 42 Mo 74 W 106 Unh 25 Mn 43 Tc 75 Re 107 Uns 26 Fe 44 Ru 76 Os 27 Co 45 Rh 77 Ir 28 Ni 46 Pd 78 Pt 29 Cu 47 Ag 79 Au 30 Zn 48 Cd 80 Hg 5 31 Ga 49 In 81 Tl 6 C 14 Si 32 Ge 50 Sn 82 Pb 7 N 15 P 33 As 51 Sb 83 Bi 8 O 16 S 34 Se 52 Te 84 Po 9 F 17 Cl 35 Br 53 I 85 At 10 Ne 18 Ar 36 Kr 54 Xe 86 Rn 58 Ce 90 Th 59 Pr 91 Pa 60 Nd 92 U 61 Pm 93 Np 62 Sm 94 Pu 63 Eu 95 Am 64 Gd 96 Cm 65 Tb 97 Bk 66 Dy 98 Cf 67 Ho 99 Es 68 Er 100 Fm 69 Tm 101 Md 70 Yb 102 No 71 Lu 103 Lr
4 Role of chalcogen on the structure SiO 2 Quartz a b b a c Projection 001 3D-structure. Each (SiO 4 ) Td shares its 4 corners with 4 neighbouring Td
5 Chalcogenide glass formers Role of chalcogen on the structure SiSe 2 Low Temperature form SiS 2, SiSe 2 High Temperature form b a x Blocks of edge sharing Td These «blocks» are linked together by corners : a complex structure b Projection 001 a c Chainsof edge-sharing Td 1D-structure Projection 100 c
6 Chalcogenide glass formers Role of chalcogen on the structure GeS 2 b (High temperature form) b GeS 2 a (Low temperature form) c a c b c a b Projection 100 b a 2D-structure. A plan comprises chains of edge and corner sharing Td (projection (100)). Thesechainsare connected by corners (projection (001)) c b Projection 100 Projection 001 3D-structure. Each Td shares its 4 corners with 4 neighbouring Td
7 Chalcogenide glass formers Role of chalcogen on the structure Zachariasen enounced 4 rules to define what is a glass former (in oxides) Rule # 3 : constituting polyhedra should share only corners! As a matter of fact, GeS 2 can be obtained rather easily (air quenching); SiS(e) 2 require fast quenching Smekal model : co-existence of different types of forces Van der Waals + covalent
8 29 Si MAS NMR Role of chalcogen on the structure Crystalline SiSe 2 E 2 = Td with 2 edges shared with neighbours E 1 = Td with 1 edge shared with neighbours E 0 = Td with no edge shared with neighbours (corner sharing Td) Low-T form E 1 + E 2 High-T form E ppm * Rotation bands
9 29 Si MAS NMR Role of chalcogen on the structure Crystalline SiSe 2 E 2 = Td with 2 edges shared with neighbours E 1 = Td with 1 edge shared with neighbours E 0 = Td with no edge shared with neighbours (corner sharing Td) Low-T form E 1 + E 2 Intermediate-T form High-T form E ppm * Rotation bands
10 29 Si MAS NMR Role of chalcogen on the structure Crystalline SiSe 2 E 2 = Td with 2 edges shared with neighbours E 1 = Td with 1 edge shared with neighbours E 0 = Td with no edge shared with neighbours (corner sharing Td) Low-T form E 1 + E 2 Intermediate-T form E 0 Structure unsolved E 0 High-T form E 2 E 1 E ppm * Rotation bands
11 Chalcogenide glass formers 29 Si MAS NMR Role of chalcogen on the structure Glass SiSe 2 Glass E 0 E 2 = Td with 2 edges shared with neighbours E 1 = Td with 1 edge shared with neighbours E 0 = Td with no edge shared with neighbours (corner sharing Td) Low-T form E 1 + E 2 Intermediate-T form Structure unsolved E 0 High-T form E 2 E 1 E ppm * Rotation bands
12 Chalcogenide glass formers Role of chalcogen on the structure Glass SiS 2 NMR E 2 Chemical shifts amplitude : 28 ppm against 62 ppm in the case of selenide glasses
13 Chalcogenide glass formers Glass GeS 2 Role of chalcogen on the structure GeS 2 b (High temperature form) b Raman spectra Stretching a Projection Bending c-ges g-ges «outrigger raft» model
14 Chalcogenide glass formers To summarize Co-existence of corner-sharing tetrahedra and edge-sharing tetrahedra Predominance of edge-sharing Td for SiS(e) 2 Predominance of corner-sharing Td for GeS(e) 2 29 Si NMR E 0 E 1 E 2
15 Modified chalcogenide glasses Role of modifier on the structure SiS(e) 2 + M 2 S(e) M = Li, Na, Ag
16 Modified chalcogenide glasses Vitreous transition temperature System xli 2 Y-(1-x)SiY 2, Y = O, S, Se Conductivity and Activation Energy Y= O Y= S Y= Se Y= Se Y= S Large decrease in Tg for the first addition of alkali Conductivity in chalcogenides much larger than in oxide (2.5 orders of magnitude) Y= O Large increase in ion conductivity with addition of alkali ions (Li content x 2 à Gain of 2 orders of magnitude in conductivity)
17 For oxide glasses Role of modifier on the structure SiO 2 + Q 4 E 0 E 1 E 2 M 2 O Q 3 M = Li, Na, Ag Q 2 Creation of non bridging oxygen Q 1 Entités Q n Q 0
18 Modified chalcogenide glasses Role of modifier on the structure E 0 E 1 E 2 SiS(e) 2 Q 4 + M 2 S(e) M = Li, Na, Ag Creation of non bridging sulfur E n Q n Entities Q 3 Q 2 Q 1 Q 0
19 Modified chalcogenide glasses Role of modifier on the structure 1st step Identification of crystalline phases; identification of their E n Q n building entities Identification of corresponding chemical shifts in 29 Si NMR spectra 2nd step Obtention of 29 Si NMR spectra of corresponding glassy compositions Identification of their E n Q n building entities by comparison with NMR spectra of crystalline phases
20 Role of modifier on the structure Modified chalcogenide glasses Glass E 0 Q 2 E 1 Q 2 System xna 2 S- (1-x)SiS 2 X = 0.5 E 0 Q 2 Na 2 SiS 3 glass contains both E 1 and E 0 entities E 1 Q 2
21 Role of modifier on the structure Modified chalcogenide glasses + Crystalline compounds E 0 Q 2 E 1 Q 2 Li 2 SiS 3 glass System xli 2 S- (1-x)SiS 2 E 0 Q 2 X = 0.5 Li 2 SiS 3 glass contains both E 1 and E 0 entities BUT 25% E 1 only E 1 Q 2 Li 2 SiS 3 Fast cooling Li 2 SiS 3 Slow cooling
22 Preferential destruction of edgesharing tetrahedra in the case of Liglasses E 0 Q 2 xna 2 S- (1-x)SiS 2 E 1 Q 2 E 0 Q 2 xli 2 S- (1-x)SiS 2 E 1 Q 2
23 Modified chalcogenide glasses Role of modifier on the structure System xm 2 S- (1-x)SiS 2 with M = Li, Na, Ag X = 0.5 E 1 Q 2 E 0 Q 2 E 1 Q 2 E 0 Q 2 E 0 Q 2 Preferentiel destruction of edge-sharing tetrahedra in any case, increasing from Na to Li to Ag
24 Role of modifier on the structure Investigation of crystalline phases in the system xli 2 Se- (1-x)SiSe 2 chemical shifts between different E 2 Q 4 units (SiSe 2 high, intermediate and low T) and between different E 1 Q 2 units (2 E 1 Q 2 sites in intermediate T SiSe E 1 Q 2 site in low T SiSe 2 ) E 0 Q 4 E 1 Q 4 E 2 Q ppm
25 Role of modifier on the structure E 0 Q 0 Isolated Td, Investigation of crystalline phases in the system xli 2 Se- (1-x)SiSe 2 E 0 Q 1 large chemical shifts between different E 0 Q n units ( E 0 Q 4 site in intermediate-t SiSe 2 + E 0 Q 0 site in Li 4 SiSe 4 + E 0 Q 1 sites in Li 6 Si 2 Se 7 (Li 10 Si 3 Se 11 ) E 0 Q 4 E 1 Q 4 E 2 Q 4 29 Si NMR sensitive to Qn entities in selenides
26 Role of modifier on the structure Investigation of crystalline phases in the system xli 2 Se- (1-x)SiSe 2 E 0 Q 1 E 0 Q 0 E 0 Q 2? Isolated Td, E 1 Q 2? Which units for Li 2 SiSe 3 E 0 Q 2 or E 1 Q 2?? E 0 Q 4 E 1 Q 4 E 2 Q 4 29 Si NMR sensitive to Qn entities in selenides
27 Role of modifier on the structure Investigation in the system xli 2 Se- (1-x)SiSe 2 Modified chalcogenide glasses X = 0.5 Li Li2SiSe3 2 3 glass -45ppm E 0 Q 2 glass Crystalline Li2SiSe3 glass Li 2 SiSe 3-85ppm Li2Si Se3 E 1 Q 2 glass glass Which units for Li 2 SiSe 3 E 0 Q 2 or E 1 Q 2??
28 Role of modifier on the structure Modified chalcogenide glasses E 0 Q 1 E 0 Q 0 xli 2 Se- (1-x)SiSe 2 glasses Li 2 Se tends to destroy edgesharing tetrahedra preferentially Stronger trend than in sulfides (25% E 1 left for x = 0.5) X = 0.48 No more E 1 E 0 Q 2 E 0 Q 4 E 1 Q 2 E 1 Q 4 E 2 Q 4
29 Role of modifier on the structure 0.6Na 2 Se- 0.4SiSe 2 glasses Modified chalcogenide glasses Q 1 Q 0 Q 1 only Q 3 Ordered model Random model 2 Q 1 <-- --> Q 3 + Q 0 Distribution of non-bridging Se sites is closer to random than to ordered
30 Role of modifier on the structure XPS investigation S 2p core peaks for M 2 GeS 3 glasses; M = Ag, Li, Na Na 2 GeS 3 Li 2 GeS 3 Ag 2 GeS 3 bs : 33% [33%] nbs : 67% [67%] Splitting between nbs and bs Ag : 0.5 ev Li : 0.8 ev Na : 0.8 ev more homogeneous electronic distribution on sulfur atoms in the silver glass Binding energy (ev) D[E b (Ge3p)-E b (S2p)] Ag 2 GeS ev a much more important electronic redistribution Li 2 GeS ev along Ge-S bonds when the modifier cation Na 2 GeS ev changes from Ag to Na
31 Modified chalcogenide glasses To summarize Existence of bridging and non-bridging S(e) Trend to the destruction of edge-sharing Td increasing from Na to Li to Ag Random distribution of modifier cations on the Td
32 Mixed glass former effect System Li 2 S- [(1-x)SiS 2 -xges 2 ] 0.3 Li 2 S 0.7[(1-x)SiS 2 xges 2 ] 0.5 Li 2 S 0.5[(1-x)SiS 2 xges 2 ]
33 Mixed glass former effect System Li 2 S- [(1-x)SiS 2 -xges 2 ] 0.3 Li 2 S 0.7[(1-x)SiS 2 xges 2 ] 0.5 Li 2 S 0.5[(1-x)SiS 2 xges 2 ] Conductivity and E s 1E-3 I II III E s (S/cm) 1E-4 1E Es (ev) s (S/cm) 1E-4 1E Es (ev) E x 1E x Maximum in s and minimum in activation energy for ~ 50:50 ratio in former content Smooth change in both s and activation energy
34 Mixed glass former effect System Li 2 S- [(1-x)SiS 2 -xges 2 ] 0.3 Li 2 S 0.7[(1-x)SiS 2 xges 2 ] 0.5 Li 2 S 0.5[(1-x)SiS 2 xges 2 ] T g ( o C) Tg T g ( o C) Tg x x density Smooth change in T g r (g/cm 3 ) x 2 T g and a minimum in r for ~50:50 ratio in former content
35 0.3 Li 2 S 0.7[(1-x)SiS 2 xges 2 ] SAXS Porod Law: aggregates or clusters of 50 Å in size Debye-Bueche model: homogeneous glasses
36 Mixed glass former effect Raman Spectroscopy 0.3 Li 2 S 0.7[(1-x)SiS 2 xges 2 ] 0.5 Li 2 S 0.5[(1-x)SiS 2 xges 2 ] ü A sudden change in the structure ü A smooth change in the structure II I III cm -1 cm -1
37 SiS 2 Different medium range order No possible mixing of the two formers GeS 2 amorphous Complete phase Separation (Tenhover 1983) amorphous xli 2 S- (1-x)SiS 2 Addition of Li 2 S Preferential destruction of edge sharing tetrahedra ( 29 Si NMR investigation) x=0.3 different MRO phase separation x=0.5 similar MRO Complete solid solution
38 Mixed glass former effect Raman Spectroscopy cm -1 x = [0.5Li 2 S-0.5SiS 2 ]+ [0.05SiS GeS 2 ] cm -1 x = [0.5Li 2 S-0.5SiS 2 ]+ 0.4GeS 2 x = [0.5Li 2 S-0.5SiS 2 ]+ [0.05 Li 2 S- 0.45GeS 2 ]
39 Mixed glass former effect Conductivity Activation Energy 1E-3 1E-4 0.5Li 2 S-0.5[(1-x)SiS 2 -xges 2 ] Li 2 S-0.7[(1-x)SiS 2 -xges 2 ] s (S/cm) 1E-5 E s (ev) Li 2 S-0.7[(1-x)SiS 2 -xges 2 ] 1E x 0.5Li 2 S-0.5[(1-x)SiS 2 -xges 2 ] x s (phase separated glasses) ~ s (0.5Li2S- 0.5[(1-x)SiS2-xGeS2]) E s (phase separated glasses) ~ E s (0.5Li2S-0.5[(1-x)SiS2-xGeS2])
40 Mixed Glass former effect To summarize Similar structure for the formers à homogeneous mixing Dissimilar structure for the formers à heterogeneous mixing Strong consequence on both thermal and electrical properties
41 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 Vitreous transition temperature Conductivity and Activation Energy Non-linear variation of severalphysicochemicalproperties Minimum in T g and s and maximum in E s Well known «mixed alkali effect» systematically observed when two mobile ions are mixed in a glassy matrix whatever the atoms involved Hardly studied in chalcogenide glasses
42 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 SAXS investigation discarded the existence of any phase separation at a mesoscopic scale ( Å) Structural investigation of the cation environment Ag K-edge EXAFS (35K) Ag K-edge Fourier filtered oscillations of 0.5 [1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 glasses. For all compositions Coordination number N Ag ~ 2.8 Bond length Ag-S ~ 2.50 Å Ds = 0.08Å (disordered environment) No influence of the presence of Rb
43 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 Structural investigation of the cation environment Rb K-edge EXAFS measured at 35K Rb K-edge Fourier filtered oscillations of 0.5 [1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 glasses. For all compositions Coordination number N Rb ~ 4 (Td) Bond length Rb-S ~ 3.37 Å Ds = 0.14Å (highly distorted sites) No influence of the presence of Ag
44 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 Structural investigation of the glassy network Raman (1064 nm) IR spectra Clear structural rearrangements upon gradual replacement of Rb 2 S by Ag 2 S. Nonmonotonic evolution - strong departure for x = 0.2 and 0.4
45 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 Structural investigation of the glassy network X = 0.4 IR Linear combinations of the end-member spectra (x=0 and 1) Raman Experimental spectra A simple linear mixing of the structures of the two end-member glasses cannot reproduce the thiogermanate structure of the cation-mixed glass.
46 Mixed anion effect System 0.5[(1-x)Rb 2 S-xAg 2 S]-0.5GeS 2 Structural investigation of the glassy network n (Ge-S) n (Ge-S - ) Q 1 Q 2 Q 3 3 Q 2 --> Q 4 + 2Q 1 2 Q 2 --> Q 3 + Q 1 Shift of n (Ge-S - ) of Q 2 Td units to higher frequency à local strain effects Increase in Q 2 units for x= 0.2 and 0.4 à a more homogeneous glass structure and a more uniform distribution of anionic sites hosting the Rb + and Ag + cations
47 Mixed Anion Effect To summarize The environment of the cations is not affected by the presence of another cation in the network The network relaxes to adjust to maximize the distance between dissimilar cations creating a more homogeneous matrix Strong consequence on both thermal and electrical properties
48 Conclusions Chalcogenide glasses different from oxide glasses Presence of edge-sharing Td But also many similarities Bridging vs non-bridging chalcogens Mixed glass former effect Mixed alkali effect
49 THANK YOU!
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52 Role of modifier on the structure Modified chalcogenide glasses Isolated Td, E 0 Q 0 Investigation of crystalline phases in the system xli 2 Se- (1-x)SiSe 2 No apparent chemical shift between E n Q 4 units and E n Q 2 units
53 System Li 2 S- [(1-x)SiS 2 -xges 2 ]:: Conductivity and E s Mixed glass former effect: Chalcogenide glasses Conductivity Activation energy 1E-3 1E-4 0.5Li 2 S-0.5[(1-x)SiS 2 -xges 2 ] Li 2 S-0.7[(1-x)SiS 2 -xges 2 ] s (S/cm) 1E-5 E s (ev) Li 2 S-0.7[(1-x)SiS 2 -xges 2 ] 1E x 0.5Li 2 S-0.5[(1-x)SiS 2 -xges 2 ] x
54 Modified chalcogenide glasses Role of modifier on the structure Propriétés : Tg conductivité Role of alkali (silver) on the structure log s (S m -1 ) X Ag Li Na
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56 Role of modifier on the structure SiS 2 Crystalline compounds System xna 2 S- (1-x)SiS 2 X = 0.5 No apparent chemical shift between E n Q 4 units and E n Q 2 units
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