Scale Imaging of Cation Ordering
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1 Supporting information First 14-Layer Twinned Hexagonal Perovskite Ba 14 Mn 1.75 Ta 10.5 O 42 : Atomic- Scale Imaging of Cation Ordering Fengqiong Tao 1, Cécile Genevois 2, Fengqi Lu 1, Xiaojun Kuang 1, *, Florence Porcher 3, Liangju Li 4, Tao Yang 4, Wenbo Li 5, Di, Zhou 5, Mathieu Allix 2, * 1. Guangxi Ministry-Province Jointly-Constructed Cultivation Base for State Key Laboratory of Processing for Nonferrous Metal and Featured Materials, Guangxi Universities Key Laboratory of Non-ferrous Metal Oxide Electronic Functional Materials and Devices, College of Materials Science and Engineering, Guilin University of Technology, Guilin P. R. China 2. UPR3079 CEMHTI, 1D Avenue de la Recherche Scientifique, Orléans Cedex2, and Université d Orléans, Faculté des Sciences, Avenue du Parc Floral, Orléans Cedex 2, France 3. CEA Saclay, Laboratoire Léon Brillouin, F Gif Sur Yvette,France 4. College of Chemistry and Chemical Engineering, Chongqing University, Chongqing, , P. R. China 5. Electronic Materials Research Laboratory, Key Laboratory of the Ministry of Education & International Center for Dielectric Research, Xi'an Jiaotong University, Xi'an ,Shaanxi, P. R. China * kuangxj@glut.edu.cn(x.k.); mathieu.allix@cnrs-orleans.fr(m.a.) S1
2 Intensity (a. u.) 1773 K 12h 1723 K 12h 1673 K 6h 1573 K 6h 1473 K 6h :5H :3C :14H Theta ( o ) Figure S1. XRD patterns of Ba 14 Mn 1.75 Ta 10.5 O 42 (BMT) samples fired at different temperatures for 6-12 h. 5H, 3C and 14H correspond to 5-layer hexagonal Ba 5 Ta 4 O 15, 3-layer cubic Ba 3 MnTa 2 O 9 and 14-layer hexagonal BMT phases, respectively. Figure S2. SAED pattern of BMT recorded along [001] direction. The indexation was performed using the simple 14-layer hexagonal perovskite cell. S2
3 Figure S3. Schematic view of the ab-planes for the simple (in black) and triple (in red) 14-layer phases showing the cell tripling along the [110] axis for the simple 14-layer phase. The green and red spheres denote A and O atoms, respectively Cell parameters(å) c a Temperature (K) Figure S4. Temperature dependency of cell parameters for the 14-layer hexagonal phase BMT. S3
4 Figure S5. Hydrogen-reduction TGA data of BMT from RT to 1473 K. 12 (a) 8 Counts(10 3 ) Theta( ) S4
5 10 (b) Counts(10 3 ) Theta( ) Figure S6. Enlarged plots of the Rietveld fit of NPD data for the 14-layer twinned hexagonal perovskite BMT within different 2Theta ranges of (a) 5-65º and (b) (a) Counts(10 4 ) Theta( ) S5
6 15 (b) Counts(10 4 ) Theta( ) 4 (c) Counts(10 4 ) Theta( ) S6
7 0.2 (d) Counts(10 4 ) Theta( ) Figure S7. Enlarged plots of the Rietveld fit of SPD data for the 14-layer twinned hexagonal perovskite BMT within different 2Theta ranges of (a) 1-8, (b) 8-15º, (c) 15-35º and (d) 35-50º. S7
8 Table S1. Final refined structural parameters for the triple 14-layer phase of BMT* from the two-phase refinement against combined SPD and NPD data. Atom Site x y z Occupancy B iso (Å 2 ) a BVS b Ba1 2a (5) (1) 1.76 Ba2 2a (3) (1) 2.43 Ba3 4b 1/3 2/ (2) (1) 2.64 Ba4 4b 1/3 2/ (2) (1) 2.16 Ba5 6c (4) (3) (1) 2.15 Ba6 6c (4) (3) (1) 2.45 Ba7 6c (7) (3) (1) 2.41 Ba8 6c (7) (3) (1) 2.46 Ba9 6c (9) (4) (1) 1.96 Ta1 6c (5) (3) (8) 4.68 Ta2 6c (4) (3) (8) 4.91 Ta3 2a (6) 0.10(2) 0.166(8) 3.36 Mn3 2a (6) 0.90(2) 0.166(8) 2.37 Ta4 4b 1/3 2/ (7) 0.14(1) 0.166(8) 3.41 Mn4 4b 1/3 2/ (7) 0.86(1) 0.166(8) 2.40 Ta5 6c (4) (3) (8) 4.93 Ta6 6c (4) (3) (8) 5.40 Ta7 2a (3) (8) 4.26 Ta9 4b 1/3 2/ (5) 0.22(1) 0.166(8) 2.64 S8
9 Ta10 4b 1/3 2/ (3) 0.78(1) 0.166(8) 5.50 O1 6c 0.804(1) (6) (2) 2.34 O2 6c 0.831(2) (6) (2) 2.22 O3 12d 0.485(1) 0.339(1) (5) (2) 2.13 O4 12d (9) 0.519(1) (4) (2) 1.95 O5 6c 0.827(1) (6) (2) 2.15 O6 12d 0.832(1) 0.351(1) (4) (2) 2.14 O7 6c 0.502(2) (6) (2) 1.96 O8 6c 0.496(1) (6) (2) 2.12 O9 12d (5) (5) (5) (2) 1.98 O10 12d (6) (6) (5) (2) 1.96 O11 6c 0.821(2) (7) (2) 2.01 O12 6c 0.829(2) (6) (2) 1.99 O13 12d 0.323(1) 0.481(1) (5) (2) 1.98 O14 12d 0.492(1) 0.328(1) (5) (2) 2.03 *a = (2) Å, c = (9) Å, V = (1) Å 3, space group: P6 3 cm, Z = 3. a The atomic displacement parameters B iso were constrained to be equal for the atoms of the same type but on distinctly crystallographic sites to prevent some atoms from getting small negative values when refined independently given the large number of independently crystallographic sites. b The BVSs for the oxygen sites were calculated with the mixed and partial occupancies of the B-sites taken into consideration. S9
10 Table S2. Bond lengths for the triple superstructure of the 14-layer BMT. Bond Lengths(Å) Bond Lengths(Å) Ba1-O1( 3) 2.79(2) Ba9-O1( 1) 2.91(2) Ba1-O9( 6) 3.083(8) Ba9-O2( 1) 3.05(2) Ba1-O12( 3) 3.09(2) Ba9-O3( 2) 2.88(2) Ba9-O4( 2) 3.19(2) Ba2-O2( 3) 2.69(2) Ba9-O5( 2) 2.903(8) Ba2-O10( 6) 2.90(1) Ba9-O6( 2) 2.79(1) Ba2-O11( 3) 3.09(2) Ba9-O6( 2) 3.19(2) Ba3-O4( 3) 2.75(2) Ta1 -O7( 1) 2.02(2) Ba3-O8( 3) 2.904(1) Ta1-O10( 2) 2.07(1) Ba3-O9( 3) 2.734(8) Ta1 -O11( 1) 1.98(2) Ba3-O13( 3) 3.03(2) Ta1 -O14( 2) 1.96(2) Ba4-O3( 3) 2.88(2) Ta2 -O8( 1) 1.95(2) Ba4-O7( 3) 2.905(1) Ta2 -O9( 2) 2.01(1) Ba4-O10( 3) 2.90(1) Ta2 -O12( 1) 1.94(2) Ba4-O14( 3) 2.96(2) Ta2 -O13( 2) 2.02(2) Ba5-O2( 2) 3.116(5) Ta3/Mn3-O11( 3) 2.13(2) Ba5-O3( 2) 2.69(1) Ta3/Mn3-O12( 3) 2.13(2) S10
11 Ba5-O3( 2) 2.99(2) Ta4/Mn4-O13( 3) 2.12(2) Ba5-O5( 1) 2.59(2) Ta4/Mn4-O14( 3) 2.12(2) Ba5-O6( 2) 3.01(2) Ba5-O7( 1) 3.08(2) Ta5 -O1( 1) 1.81(2) Ba5-O10( 2) 3.17(2) Ta5 -O4( 2) 1.92(1) Ta5 -O8( 1) 2.13(2) Ba6-O1( 2) 2.732(6) Ta5 -O9( 2) 2.15(1) Ba6-O4( 2) 2.958(9) Ba6-O5( 1) 2.69(2) Ta6 -O2( 1) 1.86(2) Ba6-O6( 2) 2.57(2) Ta6 -O3( 2) 1.85(2) Ta6 -O7( 1) 2.16(2) Ba7-O8( 1) 2.78(2) Ta6 -O10( 2) 2.06(1) Ba7-O9( 2) 2.89(2) Ba7-O11( 1) 2.76(2) Ta7 -O2( 3) 2.25(2) Ba7-O12( 2) 2.919(6) Ta7 -O5( 3) 1.91(2) Ba7-O13( 2) 2.98(1) Ba7-O13( 2) 2.82(1) Ta9 -O3( 3) 2.33(2) Ba7-O14( 2) 2.87(2) Ta9 -O6( 3) 2.13(2) Ba8-O7( 1) 2.84(2) Ta10/ -O4( 3) 2.19(2) Ba8-O10( 2) 2.91(2) Ta10 -O6( 3) 1.80(1) Ba8-O11( 2) 2.898(5) S11
12 Ba8-O12( 1) 2.92(2) Ba8-O13( 2) 2.73(2) Ba8-O14( 2) 2.86(1) Ba8-O14( 2) 2.95(1) Table S3. Photocatalytic H 2 evolution rates for the BMT powders loaded with various cocatalysts under UV light irradiation. Cocatalyst H 2 evolution rate (µmol/h/g) 1 wt% Pt wt% Ru wt% Pd wt% Au wt% Ag wt% Pt and 0.5 wt% Ag wt% Ru and 0.5 wt% Ag 24.2 S12
13 Figure S8. Photocatalytic H 2 evolution for the BMT powders loaded with various cocatalysts under UV light irradiation. S13
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