Electronic supporting information for paper Tuning the gate-opening pressure and particle size distribution of the switchable metal-organic framework DUT-8(Ni) by controlled nucleation in a micromixer H. Miura, a,b V. Bon, *a I. Senkovska, a S. Ehrling, a S. Watanabe, c M. Ohba b and S. Kaskel a Table of content 1. Schemes and photos of the experimental setup 2 2. Characterization of the micromixer by Villermaux-Dushman method 3 3. PXRD patterns 4 4. Nitrogen physisorption isotherms 6 5. Scanning electron microscopy 8 6. DRIFT spectra 10 7. TG curves 13 Electronic Supplementary Material (ESI) for Dalton Transactions. This journal is © The Royal Society of Chemistry 2017
Welcome message from author
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
Electronic supporting information
for paper
Tuning the gate-opening pressure and particle size distribution of the switchable metal-organic framework DUT-8(Ni) by controlled nucleation in a
micromixer
H. Miura,a,b V. Bon,*a I. Senkovska,a S. Ehrling,a S. Watanabe,c M. Ohbab and S. Kaskela
Table of content
1. Schemes and photos of the experimental setup 22. Characterization of the micromixer by Villermaux-Dushman method 33. PXRD patterns 44. Nitrogen physisorption isotherms 65. Scanning electron microscopy 86. DRIFT spectra 107. TG curves 13
Electronic Supplementary Material (ESI) for Dalton Transactions.This journal is © The Royal Society of Chemistry 2017
1. Schemes and photos of the experimental setup.
Figure S1. Photograph of experimental system using micromixer for the synthesis of samples: (a) m1, (b) m2 and (c) m3-m8.
Figure S2. Schematic representation of the micromixer
(b)
(c)
(a)
2. Villermaux-Dushman method
Figure S3. UV-Vis spectra for resulting solution of the (a) set 1, (b) set 2 and (c) set 3 by Villermaux-Dushman reaction
Figure S4. Dependence of the characteristic mixing time tm on the flow rate for the micromixer.
Table S1. Concentration sets for Villermaux-Dushman reactionC
(mol/L) [H+] [KI] [KIO3] [NaOH] [H3BO3]Set 1 0.02 0.032 0.006 0.09 0.09Set 2 0.015 0.016 0.003 0.045 0.045Set 3 0.015 0.032 0.006 0.09 0.09
(a) (b) (c)
3. PXRD patterns
Figure S5. PXRD patterns for activated DUT-8(Ni) samples, synthesized in batch using different ratio of reactants and the order of mixing (b1, b2, b3, b4, b5 and b6).
Simulated pattern of open phase DUT-8(Ni)
b1
b2
b3
b5
b6
b4
2Ɵ / °
Intensity / a.u
.
Figure S6. PXRD patterns for activated DUT-8(Ni) samples, synthesized by batch synthesis procedures at different temperatures (b7, b8, b9, b10, b11, b12, b13, b14 and b15).
Simulated pattern of open phase DUT-8(Ni)
b7
b8
b9
b11
b12
b10
2Ɵ / °
Intensity / a.u
.
b13
b14
b15
Simulated pattern of close phase DUT-8(Ni)
4. Nitrogen physisorption isotherms
Figure S7. Nitrogen physisorption isotherms for samples b1 – b6 measured at 77 K.
(a) (b)
(c)
Figure S8. Nitrogen physisorption isotherms for (a) b7 – b9, (b) b10 – b12 and (a) b13 – b15 measured at 77 K.
5. Scanning electron microscopy
(a) b1 (b) b2 (c) b3
(d) b4 (e) b5 (f) b6
Figure S9. SEM images for samples b1-b6.
(a) b7 (b) b8 (c) b9
(d) b10 (e) b11 (f) b12
(g) b13 (h) b14 (i) b15
Figure S10. SEM images for samples b7-b15.
6. DRIFT spectra
Figure S11. DRIFT spectra for samples b1- b6.
b1
b2
b3
b5
b6
b4
Figure S12. DRIFT spectra for samples b7- b15.
b7
b8
b9
b11
b12
b10
b13
b14
b15
Figure S13. DRIFT spectra for samples m1, m2 and m3.
Figure S14. DRIFT spectra for samples m3- m8.
m4
m5
m6
m7
m8
m3
m1
m2
m3
7. TG curves
Figure S15. TG curves for samples m3-m8.
0 100 200 300 400 500 600 700 800 900 10000
20
40
60
80
100
m3m4m5m6Weight
loss/%
T /
Related Documents
