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1 Supporting Information A General Strategy to Fabricate P as Highly Efficient Cocatalyst via Photo-Reduction Deposition for Hydrogen Evolution Yuming Dong a, *, Linggang Kong a, Pingping Jiang a, Guangli Wang a, Na Zhao a, Huizhen Zhang a, and Bo Tang b, * a Key Laboratory of Synthetic and Biological Colloids, School of Chemical and Material Engineering, Jiangnan University, Wuxi , P.R. China. b College of Chemistry, Chemical Engineering and Materials Science, Shandong Provincial Key Laboratory of Clean Production of Fine Chemicals, Collaborative Innovation Center of Functionalized Probes for Chemical Imaging in Universities of Shandong, Shandong Normal University, Jinan , P.R. China * Corresponding author. dongym@jiangnan.edu.cn (Dr. Y. Dong); tangb@sdnu.edu.cn (Prof. B. Tang); Fax: This supplementary file includes: Totals 12 pages Tables S1 to S2 Figures S1 to S11 S1
2 Supplementary table captions: Table S1. Photocatalytic H 2 evolution on g-c 3 with non-noble-metal cocatalysts. Table S2. Photocatalytic H 2 evolution from water using lactic acid as hole sacrificial agent. Supplementary figure captions: Figure S1. Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20, 30 and 40 min); The data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 20 vol% triethanolamine aqueous solution for 2 h. Figure S2. (a) Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20 and 30 min), and the data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 40 vol% methanol aqueous solution for 2 h; (b) Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20 and 30 min), and the data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 10 vol% lactate acid solution for 2 h. Figure S3. Photocatalytic HER activity of P-20/g-C 3 and Pt-0.5wt%/g-C 3 (0.5 wt% Pt was loaded on g-c 3 in situ by photoreduction of H 2 PtCl 6 ). The data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 20 vol% triethanolamine aqueous solution for 2 h. Figure S4. TEM (left) and HRTEM (right) image of Pt-0.5wt%/g-C 3. Figure S5. (a) XRD patterns and (b) FTIR spectra of P-T/g-C 3 (T=0, 10, 20, 30, 40 and 100 min). Figure S6. Raman spectra of P-T/g-C 3 laser of 785 nm. (T=0, 10, 20 and 100 min) excited by Figure S7. UV-vis diffuse reflectance spectra of P-T/g-C 3 (T=0, 10, 20, 30, 40 and 100 min). Figure S8. SEM image of P-20/g-C 3. Figure S9. TEM image of Ni-20/g-C 3 after treatment in HCl solution (ph=2) for 1 week. Figure S10. EDX-Mapping image of Ni-20/g-C 3 after treatment in HCl solution (ph=2) for 1 week. Figure S11. The property and function of AM 1.5 G filter. S2
3 Table S1. Photocatalytic H 2 evolution on g-c 3 with non-noble-metal cocatalysts. Cocatalysts [Ni(TEOA)] 2 Cl 2 Mass fraction sacrificial agent 2.0 wt% of Ni 2+ triethanolamine Ni(OH) mol% triethanolamine NiS 1.1 wt% triethanolamine Co III (dmgh) 2 pycl / triethanolamine NiS wt% triethanolamine Ni Tu TETN / triethanolamine NiS 1.5 mol% triethanolamine Ni(dmgH) wt% triethanolamine MoS wt% triethanolamine Ni 10wt% triethanolamine NiS 0.97wt% triethanolamine Ni/NiO 2 wt% triethanolamine C 3 N 3 S 2 Ni 0.1 wt% triethanolamine Ni 0.73 wt% triethanolamine Ni 7.4wt% triethanolamine CoP 3.4wt% triethanolamine Ni2P 0.48wt% triethanolamine P / triethanolamine Light source 500 W Xe 350 W Xe 500W Xe 150 W Xe Activity (µmol g -1 h -1 ) Ref S1 152 S2 482 S S4 406 S5 510 S S7 236 S8 252 S S10 84 S S S S S S S This work S3
4 References S1 J. Dong, M. Wang, X. Li, L. Chen, Y. He, L. Sun, ChemSusChem., 2012, 5, S2 J. Yu, S. Wang, B. Cheng, Z. Lin, F. Huang, Catal. Sci. Technol., 2013, 3, S3 J. Hong, Y. Wang, W. Zhang, R. Xu, ChemSusChem, 2013, 6, S4 S. W. Cao, X. F. Liu, Y. P. Yuan, Z. Y. Zhang, J. Fang, S. C. Loo, J. Barber, T. C. Sum, C. Xue, Phys. Chem. Chem. Phys., 2013, 15, S5 L. Yin, Y. P. Yuan, S.W. Cao, Z. Zhang, C. Xue, RSC Adv., 2014, 4, S6 D. Wang, Y. Zhang, W. Chen, Chem. Commun., 2014, 50, S7 Z. Chen, P. Sun, B. Fan, Z. Zhang, X. Fang, J. Phys. Chem. C, 2014, 118, S8 S. W. Cao, Y. P. Yuan, J. Barber, S. C. J. Loo, C. Xue, Appl. Surf. Sci., 2014, 319, 344. S9 H. Zhao, Y. Dong, P. Jiang, G. Wang, H. Miao, R. Wu, L. Kong, J. Zhang, C. Zhang, J. Mater. Chem. A, 2015, 3, S10 L. Bi, D. Xu, L. Zhang, Y. Lin, D. Wang, and T. Xie, Phys. Chem. Chem. Phys., 2015, 17, S11 Y. Lu, D. Chu, M. Zhu, Y. Du and P. Yang, Phys. Chem. Chem. Phys., 2015, 17, S12 G. Zhang, G. Li, X. Wang, ChemCatChem, 2015, 7, S13 Y. Chen, B. Lin, W. Yu, Y. Yang, S. M. Bashir, H. Wang, K. Takanabe, H. S14 Idriss J. M. Basset, Chem. Eur. J., 2015, 21, A. Indra, P. W. Menezes, K. Kailasam, D. Hollmann, M. Schröder, A. Thomas, A. Brückner, M. Driess, Chem. Commun., 2016, 52, 104. S15 L. Kong, Y. Dong, P. Jiang, G. L. Wang, H. Zhang, and N. Zhao, J. Mater. Chem. A, 2016, 4, S16 H. Zhao, P. Jiang, W. Cai, Chem. Asian J., 2017, DOI: /asia S17 H. Zhao, S. Sun, P. Jiang, Z. J. Xu, Chem. Eng. J., 2017, DOI: /j.cej S4
5 Table S2. Photocatalytic H 2 evolution from water using lactic acid as hole sacrificial agent. The Photocatalyst reaction Activity time Light sacrificial agent (µmol mentioned source g -1 h -1 ) in this Ref. article/h PdS/CdS/NiS 5 lactic acid S18 CdS/Pt/WO 3 9 lactic acid 500 W Xe 2900 S19 In 2 S 3 /MoS 2 /CdS 12 lactic acid S20 CdS-WZ 12 lactic acid 350 W Xe 4628 S21 Pt/CdWO 4 /CdS 12 lactic acid S22 WS 2 /CdS 15 lactic acid 4200 S23 Pt/CdS 15 lactic acid UV-LEDs (420 nm) 9374 S24 MoS 2 /CdS 16 lactic acid 6850 S25 titania-based CdS 16 lactic acid S26 WS 2 CdS 16 lactic acid 1984 S27 SiW 11 Co/M/G-CdS 18 lactic acid S28 rgo/cds/mos 2 20 lactic acid 350 W Xe 1980 S29 Ni/CdS 20 lactic acid LED light / S30 CdS-MoS 2 20 lactic acid 9110 S31 MoS 2 /CdS 24 lactic acid S32 Ni/CdS 24 lactic acid S33 Pt/CdS/In 2 O 3 40 lactic acid 9297 CdS/Pt/Ga 2 O 3 40 lactic acid 8971 S34 CoP/CdS 60 lactic acid LED light S35 Zn 0.3 Cd 0.7 S/MoS 2 21 lactic acid 150 W Xe 1200 S36 S5
6 Y Al ZnO 24 lactic acid 5710 S37 NiS/TiO 2 5 lactic acid 698 S38 MoS 2 /TiO 2 25 lactic acid UV-LED 550 S39 CdS/WC/TiO 2 60 lactic acid S40 WS 2 /mpg-cn 12 lactic acid 240 S41 CNS:S-Se-Gr 15 lactic acid 500 W Xe 2580 S42 MoS 2 /HCNS 16 lactic acid 1340 S43 MoS 2 /mpg-cn 16 lactic acid 1030 S44 g-c 3 /Au/CdS 25 lactic acid 1060 S45 P/g-C 3 75 lactic acid This 1732 work References S18. J. Meng, Z. Yu, Y. Li and Y. Li, Catal. Today, 2014, 225, 136. S19. L. J. Zhang, S. Li, B. K. Liu, D. J. Wang and T. F. Xie, ACS Catal., 2014, 4, S20. W. Jiang, Y. Liu, R. Zong, Z. Li, W. Yao and Y. Zhu, J. Mater. Chem. A, 2015, 3, S21. D. Lang, Q. Xiang, G. Qiu, X. Feng and F. Liu, Dalton T., 2014, 43, S22. X. Jia, M. Tahir, L. Pan, Z. F. Huang, X. Zhang, L. Wang and J. J. Zou, Appl. Catal. B-Environ., 2016, 198, 154. S23. X. Zong, J. Han, G. Ma, H. Yan, G. Wu, and C. Li, J. Phys. Chem. C, 2011, 115, S24. Q. Xiang, B. Cheng and J. Yu, Appl. Catal. B-Environ., 2013, 138, 299. S25. J. Zhang, Z. Zhu and X. Feng, Chem-Eur. J., 2014, 20, S26. J. Zhang, Z. Zhu, Y. Tang, K. Müllen and X. Feng, Adv. Mate., 2014, 26, 734. S27. J. Chen, X. J. Wu, L. Yin, B. Li, X. Hong, Z. Fan, B. Chen, C. Xue and H. Zhang, Angew. Chem. Int. Edit., 2015, 54, S28. M. Liu, F. Li, Z. Sun, L. Xu, Y. Song and A. Munventwali, RSC Adv., 2015, 5, S29. Y. Li, H. Wang and S. Peng, J. Phys. Chem. C, 2014, 118, S30. S. Cao, C. J. Wang, X. J. Lv, Y. Chen and W. F. Fu, Appl. Catal. B-Environ., 2015, 162, 381. S31. Q. Liu, X. Li, Q. He, A. Khalil, D. Liu, T. Xiang and L. Song, Small, 2015, 11, S6
7 S32. J. He, L. Chen, F. Wang, Y. Liu, P. Chen, C. T. Au and S. F. Yin, ChemSusChem, 2016, 9, 624. S33. S. Chen, X. Chen, Q. Jiang, J. Yuan, C. Lin and W. Shangguan, Appl. Surf. Sci., 2014, 316, 590. S34. Y. X. Pan, H. Zhuang, J. Hong, Z. Fang, H. Liu, B. Liu and R. Xu, ChemSusChem, 2014, 7, S35. S. Cao, Y. Chen, C. J. Wang, X. J. Lv and W. F. Fu, Chem. Commun., 2015, 51, S36. Y. Lu, D. Wang, P. Yang, Y. Du and C. Lu, Catal. Sci. Technol., 2014, 4, S37. J. Huo, L. Fang, Y. Lei, G. Zeng and H. Zeng, J. Mater. Chem. A, 2014, 2, S38. L. Zhang, B. Tian, F. Chen and J. Zhang, Int. J. Hydrogen Energ., 2012, 37, S39. P. Zhang, T. Tachikawa, M. Fujitsuka and T. Majima, Chem. Commun., 2015, 51(33), S40. Y. X. Pan, T. Zhou, J. Han, J. Hong, Y. Wang, W. Zhang and R. Xu, Catal. Sci. Technol., 2016, 6, S41. Y. Hou, Y. Zhu, Y. Xu and X. Wang, Appl. Catal. B-Environ., 2014, 156, S42. S. S. Shinde, A. Sami and J. H. Lee, Carbon, 2016, 96, 929. S43. D. Zheng, G. Zhang, Y. Hou and X. Wang, Appl. Catal. A: Gen., 2016, 521, 2. S44. Y. Hou, A. B. Laursen, J. Zhang, G. Zhang, Y. Zhu, X. Wang and I. Chorkendorff, Angew. Chem. Int. Edit., 2013, 52, S45. W. Li, C. Feng, S. Dai, J. Yue, F. Hua and H. Hou, Appl. Catal. B-Environ., 2015, 168, 465. S7
8 H 2 evolution (µmol g -1 h -1 ) min 10min 20min 30min 40min Preparation time under irradiation Figure S1. Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20, 30 and 40 min); The data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 20 vol% triethanolamine aqueous solution for 2 h H 2 evolution(µmol g -1 h -1 ) min 10min 20min 30min H 2 evolution (µmol g -1 h -1 ) min 10min 20min 30min Figure S2. (a) Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20 and 30 min), and the data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 40 vol% methanol aqueous solution for 2 h; (b) Photocatalytic HER activity of P-T/g-C 3 (T=0, 10, 20 and 30 min), and the data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 10 vol% lactate acid solution for 2 h. S8
9 12000 H 2 evolution (µmol g -1 h -1 ) P-20/g-C 3 Pt-0.5 wt%/g-c 3 Figure S3. Photocatalytic HER activity of P-20/g-C 3 and Pt-0.5wt%/g-C 3 (0.5 wt% Pt was loaded on g-c 3 in situ by photoreduction of H 2 PtCl 6 ). The data were obtained by photocatalytic processes of 5 mg photocatalyst in 10 ml 20 vol% triethanolamine aqueous solution for 2 h. Figure S4 TEM (left) and HRTEM (right) image of Pt-0.5wt%/g-C 3. a P-100/g-C 3 b P-40/g-C 3 P-100/g-C 3 Intensity (a.u.) P-40/g-C 3 P-30/g-C 3 P-20/g-C 3 P-10/g-C 3 Intensity (a.u.) P-30/g-C 3 P-20/g-C 3 P-10/g-C 3 Pure g-c 3 Pure g-c theta (degree) Wavenumber(cm -1 ) Figure S5. (a) XRD patterns and (b) FTIR spectra of P-T/g-C 3 (T=0, 10, 20, 30, 40 and 100 min). S9
10 P-0/g-C 3 P-10/g-C 3 P-20/g-C 3 Intensity (a.u.) P-100/g-C Raman shift (cm -1 ) Figure S6. Raman spectra of P-T/g-C 3 (T=0, 10, 20 and 100 min) excited by laser of 785 nm Intensity (a.u.) P-0/g-C 3 P-10/g-C 3 P-20/g-C 3 P-30/g-C 3 P-40/g-C 3 P-100/g-C Wavelength (nm) Figure S7. UV-vis diffuse reflectance spectra of P-T/g-C 3 (T=0, 10, 20, 30, 40 and 100 min). S10
11 Figure S8. SEM image of P-20/g-C 3. Figure S9. TEM image of Ni-20/g-C 3 after treatment in HCl solution (ph=2) for 1 week. S11
12 Figure S10. EDX-Mapping image of Ni-20/g-C 3 after treatment in HCl solution (ph=2) for 1 week. Figure S11. The property and function of AM 1.5 G filter. S12
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