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1 Supporting Information for Multilayer Hollow Spheres: Microwave-Assisted Metal-Organic-Framework Derivation and Highly Reversible Structure-Matched Stepwise Lithium Storage Wenxiang Guo, Weiwei Sun and Yong Wang* Department of Chemical Engineering, School of Environmental and Chemical Engineering, Shanghai University, Shangda Road 99, Shanghai, P. R. China,

2 Figure S1. XRD patterns of Cu-Ni-BTC and Ni-BTC. 2

3 Figure S2. Thermogravimetric curve of Cu-Ni-BTC in air. 3

4 Figure S3. Nitrogen adsorption isotherms of 4

5 Figure S4. (a-b) TEM images of the Cu-Ni-BTC MOF precursor. 5

6 Figure S5. SEM images of the CuO/NiO product synthesized by one-pot method, in which Ni(NO 3 ) 2 6H 2 O, Cu(NO 3 ) 2 3H 2 O and H 3 BTC are reacted under one-time microwave irradiation. 6

7 Figure S6. SEM images of (a) 120 (prepared at 120 o C) and (b) 180 (prepared at 180 o C). (c)xrd patterns of various composites. 7

8 Table S1 Electrochemical properties of multi-layer hollow of this work and previous NiO and CuO structures. These selected references represent the state-of-the-art properties of NiO/CuO nanostructures, therefore the outstanding electrochemical performances of the product in this work can be clearly demonstrated. Morphology Multilayer hollow sphere CuO sphere-nio nanosheet Electrochemical performances (charge capacity refers to lithium extraction capacity) Initial charge capacity of 856 mah g -1 and the retained capacity of 1086 mah g -1 after 200 cycles at 100 ma g -1. Initial charge capacity of 639 mah g -1, which decreases to 563 mah g -1 after 50 cycles at 80 ma g -1. References this work 1 Porous hexagonal Initial charge capacities of ~790 and 849 mah g -1 for CuO-NiO and CNT/CuO-NiO Hollow NiO microsphere Hollow NiO nanosphere Hollow NiO nanotube Mesoporous NiO nanosphere Urchin-like NiO microsphere Nanosheet-based NiO microsphere NiO nanoparticle NiO fiber CuO-NiO and CNT-supported composite, which decreases to ~320 and 566 mah g -1 after 50 cycles at 100 ma g -1. Initial charge capacity of 975 mah g -1, which decreases to 380 mah g -1 after 30 cycles at 200 ma g -1. Initial charge capacity of 889 mah g -1, which decreases to 393 mah g -1 after 50 cycles at ~215 ma g -1. Initial charge capacity of 620 mah g -1, which can be remained at 600 mah g -1 after 100 cycles at 200 ma g -1. Initial charge capacity of ~860 mah g -1, which decreases to ~447 mah g -1 after 80 cycles at 100 ma g -1. Initial charge capacity of ~600 mah g -1, which increases to ~650 mah g -1 after 50 cycles at 72 ma g -1. Initial charge capacity of ~1180 mah g -1, which decreases to nearly 0 mah g -1 after 30 cycles at 50 ma g -1. Initial charge capacity of 847 mah g -1, which decreases to ~600 mah g -1 after 50 cycles at 717 ma g -1. Initial charge capacity of 696 mah g -1, which can be retained at 638 mah g -1 after 50 cycles at 40 ma g

9 NiO nanofiber NiO nanorod array NiO nanocone array NiO nanoflake Mesoporous NiO nanosheet network 3D flower-like NiO CuO/Cu 2 O hollow polyhedron Hollow CuO octahedra Initial charge capacity of ~784 mah g -1, which decreases to ~550 mah g -1 after 100 cycles at 80 ma g -1. Initial charge capacity of 802 mah g -1, which decreases to 706 mah g -1 after 70 cycles at 1000 ma g -1. Initial charge capacity of 780 mah g -1, which increases to 1058 mah g -1 after 100 cycles at 144 ma g -1. Initial charge capacity of ~720 mah g -1, which can be maintained after 20 cycles at 100 ma g -1. Initial charge capacity of ~689 mah g -1, which increases to ~1000 mah g -1 after 80 cycles at 144 ma g -1. Initial charge capacity of 1186 mah g -1, which decreases to 713 mah g -1 after 40 cycles at 100 ma g -1. Initial charge capacity of 513 mah g -1, which increases to ~740 mah g -1 after 250 cycles at 100 ma g -1. Initial charge capacity of ~480 mah g -1, which can be retained at ~470 mah g -1 after 100 cycles at 100 ma g Initial charge capacity of 614 mah g -1 for hollow cube, Hollow Cu 2 O cube and uichin CuO nanorod Porous CuO nanorod CuO nanowire CuO Nanofiber which decreases to 79 mah g -1 after 50 cycles at 150 ma g -1. Initial charge capacity of ~500 mah g -1 for hollow urchin, which increases to 560 mah g -1 after 50 cycles at 150 ma g -1. Initial charge capacity of 580 mah g -1, which increases to 650 mah g -1 after 100 cycles at 337 ma g -1. Initial charge capacity of ~550 mah g -1, which increases to ~634 mah g -1 after 200 cycles at 337 ma g -1. Initial charge capacity of 867 mah g -1, which decreases to 581 mah g -1 after 50 cycles at 100 ma g -1. Initial charge capacity of 452 mah g -1, which can be retained at ~400 mah g -1 after 100 cycles at 100 ma g

10 Pine-needle-like CuO array Mesoporous CuO nanosheet CuO nanoflower Dandelion-like CuO Bundle-like CuO CuO nanowalnut Initial charge capacity of ~630 mah g -1, which can be retained as 626 mah g -1 after 100 cycles at 674 ma g -1. Initial charge capacity of 533 mah g -1, which increases to 640 mah g -1 after 100 cycles at 674 ma g -1. Initial charge capacity of ~620 mah g -1, which can be retained at 530 mah g -1 after 50 cycles at 16.7 ma g -1. Initial charge capacity of 576 mah g -1, which decreases to 400 mah g -1 after 50 cycles at 67 ma g -1. Initial charge capacity of ~750 mah g -1, which decreases to 666 mah g -1 after 70 cycles at 180 ma g -1. Initial charge capacity of ~600 mah g -1, which decreases to ~420 mah g -1 after 30 cycles at 67 ma g References 1. Chen, H.; Li, C. L.; Li, N.; Xiang, X. K.; Hu, Z. L. Facile Synthesis of CuO-NiO Nanocomposites with High Surface Areas and Their Application for Lithium-Ion Batteries. Micro Nano Lett. 2013, 8, Abbas, S. M.; Hussain, S. T.; Ali, S.; Ahmad, N.; Ali, N.; Abbas, S.; Ali, Z. Modification of Carbon Nanotubes by CuO-Doped NiO Nanocomposite for Use as An Anode Material for Lithium-Ion Batteries. J. Solid State Chem. 2013, 202, Xie, D.; Yuan, W. W.; Dong, Z. M.; Su, Q. M.; Zhang, J.; Du, G. H. Facile Synthesis of Porous NiO Hollow Microspheres and Its Electrochemical Lithium-Storage Performance. Electrochim. Acta 2013, 92, Sasidharan, M.; Gunawardhana, N.; Senthil, C.; Yoshio, M. Micelle Templated NiO Hollow Nanospheres as Anode Materials in Lithium Ion Batteries. J. Mater. Chem. A 2014, 2, Liu, L. X.; Guo, Y. Y.; Wang, Y. P.; Yang, X. J.; Wang, S. X.; Guo, H. Hollow NiO Nanotubes Synthesized by Bio-Templates as The High Performance Anode Materials of Lithium-Ion Batteries. Electrochim. Acta 2013, 114, Zhang, G. H.; Chen, Y. J.; Qu, B. H.; Hu, L. L.; Mei, L.; Lei, D. N.; Li, Q.; Chen, L. B.; Li, Q. H.; Wang, T. H. Synthesis of Mesoporous NiO Nanospheres as Anode Materials for Lithium Ion Batteries. Electrochim. Acta 2012, 80, Zhang, C. M.; Chen, J.; Zeng, Y.; Rui, X. H.; Zhu, J. X.; Zhang, W. Y.; Xu, C.; Lim, T. M.; Hng, H. H.; Yan, Q. Y. A Facile Approach toward Transition Metal Oxide Hierarchical Structures and Their Lithium Storage Properties. Nanoscale 2012, 4,

11 8. Liu, L.; Li, Y.; Yuan, S. M.; Ge, M.; Ren, M. M.; Sun, C. S.; Zhou, Z. Nanosheet-Based NiO Microspheres: Controlled Solvothermal Synthesis and Lithium Storage Performances. J. Phys. Chem. C 2010, 114, Cheng, M.-Y.; Ye, Y.-S.; Chiu, T.-M.; Pan, C.-J.; Hwang, B.-J. Size Effect of Nickel Oxide for Lithium Ion Battery Anode. J. Power Sources 2014, 253, Wang, B.; Cheng, J. L.; Wu, Y. P.; Wang, D.; He, D. N. Porous NiO Fibers Prepared by Electrospinning as High Performance Anode Materials for Lithium Ion Batteries. Electrochem. Commun. 2012, 23, Aravindan, V.; Kumar, P. S.; Sundaramurthy, J.; Ling, W. C.; Ramakrishna, S.; Madhavi, S. Electrospun NiO Nanofibers as High Performance Anode Material for Li-Ion Batteries. J. Power Sources 2013, 227, Yang, W. F.; Cheng, G. H.; Dong, C. Q.; Bai, Q. G.; Chen, X. T.; Peng, Z. Q.; Zhang, Z. H. NiO Nanorod Array Anchored Ni Foam as a Binder-Free Anode for High-Rate Lithium Ion Batteries. J. Mater. Chem. A 2014, 2, Wang, X. H.; Yang, Z. B.; Sun, X. L.; Li, X. W.; Wang, D. S.; Wang, P.; He, D. Y. NiO Nanocone Array Electrode with High Capacity and Rate Capability for Li-Ion Batteries. J. Mater. Chem. 2011, 21, Wu, H.; Xu, M.; Wu, H. Y.; Xu, J. J.; Wang, Y. L.; Peng, Z.; Zheng, G. F. Aligned NiO Nanoflake Arrays Grown on Copper as High Capacity Lithium-Ion Battery Anodes. J. Mater. Chem. 2012, 22, Wang, X. H.; Qiao, L.; Sun, X. L.; Li, X. W.; Hu, D. K.; Zhang, Q.; He, D. Y. Mesoporous NiO Nanosheet Networks as High Performance Anodes for Li Ion Batteries. J. Mater. Chem. A 2013, 1, Li, Q.; Chen, Y. J.; Yang, T.; Lei, D. N.; Zhang, G. H.; Mei, L.; Chen, L. B.; Li, Q. H.; Wang, T. H. Preparation of 3D Flower-Like NiO Hierarchical Architectures and Their Electrochemical Properties in Lithium-Ion Batteries. Electrochim. Acta 2013, 90, Hu, L.; Huang, Y. M.; Zhang, F. P.; Chen, Q. W. CuO/Cu 2 O Composite Hollow Polyhedrons Fabricated from Metal-Organic Framework Templates for Lithium-Ion Battery Anodes with a Long Cycling Life. Nanoscale 2013, 5, Wu, R. B.; Qian, X. K.; Yu, F.; Liu, H.; Zhou, K.; Wei, J.; Huang, Y. Z. MOF-Templated Formation of Porous CuO Hollow Octahedra for Lithium-Ion Battery Anode Materials. J. Mater. Chem. A 2013, 1, Park, J. C.; Kim, J.; Kwon, H.; Song, H. Gram-Scale Synthesis of Cu 2 O Nanocubes and Subsequent Oxidation to CuO Hollow Nanostructures for Lithium-Ion Battery Anode Materials. Adv. Mater. 2009, 21, Wang, Z. Y.; Su, F. B.; Madhavi, S.; Lou, X. W. CuO Nanostructures Supported on Cu Substrate as Integrated Electrodes for Highly Reversible Lithium Storage. Nanoscale 2011, 3, Wang, L. L.; Gong, H. X.; Wang, C. H.; Wang, D. K.; Tang, K. B.; Qian, Y. T. Facile Synthesis of Novel Tunable Highly Porous CuO Nanorods for High Rate Lithium Battery Anodes with Realized Long Cycle Life and High Reversible Capacity. Nanoscale 2012, 4,

12 22. Chen, K. F.; Xue, D. F. Room-Temperature Chemical Transformation Route to CuO Nanowires toward High-Performance Electrode Materials. J. Phys. Chem. C 2013, 117, Sahay, R.; Kumar, P. S.; Aravindan, V.; Sundaramurthy, J.; Ling, C. W.; Mhaisalkar, S. G.; Ramakrishna, S.; Madhavi, S. High Aspect Ratio Electrospun CuO Nanofibers as Anode Material for Lithium-Ion Batteries with Superior Cycleability. J. Phys. Chem. C 2012, 116, Chen, X.; Zhang, N. Q.; Sun, K. N. Facile Fabrication of CuO 1D Pine-Needle-Like Arrays for Super-Rate Lithium Storage. J. Mater. Chem. 2012, 22, Chen, X.; Zhang, N. Q.; Sun, K. N. Facile Fabrication of CuO Mesoporous Nanosheet Cluster Array Electrodes with Super Lithium-Storage Properties. J. Mater. Chem. 2012, 22, Xiang, J. Y.; Tu, J. P.; Yuan, Y. F.; Wang, X. L.; Huang, X. H.; Zeng, Z. Y. Electrochemical Investigation on Nanoflower-Like CuO/Ni Composite Film as Anode for Lithium Ion Batteries. Electrochim. Acta 2009, 54, Xiang, J. Y.; Tu, J. P.; Zhang, L.; Zhou, Y.; Wang, X. L.; Shi, S. J. Self-Assembled Synthesis of Hierarchical Nanostructured CuO with Various Morphologies and Their Application as Anodes for Lithium Ion Batteries. J. Power Sources 2010, 195, Wang, L. L.; Cheng, W.; Gong, H. X.; Wang, C. H.; Wang, D. K.; Tang, K. B.; Qian, Y. T. Facile Synthesis of Nanocrystalline-Assembled Bundle-Like CuO Nanostructure with High Rate Capacities and Enhanced Cycling Stability as An Anode Material for Lithium-Ion Batteries. J. Mater. Chem. 2012, 22, Yu, Q.; Huang, H. W.; Chen, R.; Wang, P.; Yang, H. S.; Gao, M. X.; Peng, X. S.; Ye, Z. Z. Synthesis of CuO Nanowalnuts and Nanoribbons from Aqueous Solution and Their Catalytic and Electrochemical Properties. Nanoscale 2012, 4,

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