Abstract
The synthesis of NiCo2O4 spinel by several nanocasting strategies (i.e., multi-step nanocasting, one-step nanocasting and soft-templating), in which nickel and cobalt nitrates are used as precursors and Pluronic P123 as surfactant, is explored. First, in the multi-step nanocasting, the effect of the impregnation method (evaporation, solid–liquid and two-solvent) of the SBA-15 silica template on the morphology of NiCo2O4 replica is investigated. The evaporation method seems to be the best choice to obtain mesoporous NiCo2O4 powder which, after calcination at 375 °C and subsequent template removal, displays the highest surface area (93.1 m2/g). We have also checked the feasibility of the one-step nanoscating approach for the synthesis of ordered NiCo2O4 arrays, though this methodology entails severe difficulties, mainly related to the different decomposition temperature of the nitrate precursors and the P123 surfactant. Finally, randomly oriented, aggregated NiCo2O4 nanoparticles are obtained by means of P123 surfactant-assisted soft-templating approach.
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Alexandridis P, Holzwarth JF, Hatton TA (1994) Micellization of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymers in aqueous solutions: thermodynamics of copolymer association. Macromolecules 27:2414–2425
Alfredsson V, Anderson MW, Ohsuna T, Terasaki O, Jacob M, Bojrup M (1997) Cubosome description of the inorganic mesoporous structure MCM-48. Chem Mater 9:2066–2070
Angelo ACD, Gonzalez ER, Avaca LA (1991) Mechanistic studies of the oxygen reactions on NiCo2O4 spinel and the hydrogen evolution reaction on amorphous Ni–Co sulphide. Int J Hyd Energy 16:1–7
Beck JS, Vartuli JC, Roth WJ, Leonowicz ME, Kresge CT, Schmitt KD, Chu CTW, Olson DH, Sheppard EW (1992) A new family of mesoporos molecuar sieves prepared with liquid crystal templates. J Am Chem Soc 114:10834–10843
Cabo M, Pellicer E, Rossinyol E, Castell O, Suriñach S, Baró MD (2009) Mesoporous NiCo2O4 spinel: influence of calcination temperature over phase purity and thermal stability. Cryst Growth Des 9:4814
Carreon MA, Guliants VV, Yuan L, Hughett AR, Dozier A, Seisenbaeva GA, Kessler VG (2006) Mesoporous nanocrystalline mixed metal oxides from heterometallic alkoxide precursors: cobalt-nickel oxide spinels for propane oxidation. Eur J Inorg Chem 4983–4988
Chaubal NS, Joshi VY (2010) Nonionic polymeric surfactant template for mesoporous NiCo2O4 formation. J Porous Mater. doi:10.1007/s10934-010-9368-2
Crowley TA, Ziegler KJ, Lyons DM, Erts D, Olin H, Morris MA, Holmes JD (2003) Synthesis of metal and metal oxide nanowire and nanotube arrays within a mesoporous silica template. Chem Mater 15:3518–3522
Cui B, Lin H, Liu Y-Z, Li J-B, Sun P, Zhao X-C, Liu C-J (2009) Photophysical and photocatalytic properties of core-ring structured NiCo2O4 nanoplatelets. J Phys Chem C 113:14083–14087
Dausch DE, Goodwin SH, Exarhos GJ (2003) Chopping of near- and mid-infrared radiation using a curled electrostatic MEMS actuator. Proc Soc Photo-Opt Inst Eng (SPIE) 5074:903–910
Deng J, Zhang L, Dai H, Xia Y, Jiang H, Zhang H, He H (2010) Ultrasound-assisted nanocasting fabrication of ordered mesoporous MnO2 and Co3O4 with high surface areas and polycrystalline walls. J Phys Chem C 114:2694–2700
Dickinson C, Zhou WZ, Hodgkins RP, Shi Y, Zhao D, He H (2006) Formation mechanism of porous single-crystal Cr2O3 and Co3O4 templated by mesoporous silica. Chem Mater 18:3088–3095
Fan J, Yu CZ, Gao F, Lei J, Tian B, Wang L, Luo Q, Tu B, Zhou W, Zhao D (2003) Cubic mesoporous silica with large controllable entrance sizes and advanced adsorption properties. Angew Chem Int Ed 42:3146–3150
Gajjela SR, Ananthanarayanan K, Yap C, Grätzel M, Balaya P (2010) Synthesis of mesoporous titanium dioxide by soft template based approach: characterization and application in dye-sensitized solar cells. Energy Environ Sci 3:838–845
Imperor-Clerc M, Bazin D, Appay M-D, Beaunier P, Davidson A (2004) Crystallization of β-MnO2 nanowires in the pores of SBA-15 silicas: in situ investigation using synchrotron radiation. Chem Mater 16:1813–1821
Jiao K, Zhang B, Yue B, Ren Y, Liu S, Yan S, Dickinson C, Zhou W, He H (2005) Growth of porous single-crystal Cr2O3 in a 3-D mesopore system. Chem Commun 5618–5620
Kleitz F, Choi SH, Ryoo R (2003a) Cubic Ia3d large mesoporous silica: synthesis and replication to platinum nanowires, carbon nanorods and carbon nanotubes. Chem Commun 2136–2137
Kleitz F, Liu D, Anilkumar GM, Park I-S, Solovyov LA, Shmakov AN, Ryoo R (2003b) Large cage face-centered-cubic Fm3m mesoporous silica: synthesis and structure. J Phys Chem B 107:14296–14300
Kobayashi Y, Ke X, Hata H, Schiffer P, Mallouk TE (2008) Soft chemical conversion of layered double hydroxides to superparamagnetic spinel platelets. Chem Mater 20:2374–2381
Lee J, Orilall MC, Warren SC, Kamperman M, DiSalvo FJ, Wiesner U (2008) Direct access to thermally stable and highly crystalline mesoporous transition-metal oxides with uniform pores. Nat Mater 7:222–228
Liu Y, Zhao W, Zhang X (2008) Soft template synthesis of mesoporous Co3O4/RuO2·xH2O composites for electrochemical capacitors. Electrochim Acta 53:3296–3304
Liu J-L, Zhu L-J, Pei Y, Zhuang J-H, Li H, Li H-X, Qiao M-H, Fan K-N (2009) Ce-promoted Ru/SBA-15 catalysts prepared by a “two solvents” impregnation method for selective hydrogenation of benzene to cyclohexene. Appl Catal A Gen 353:282–287
Lu AH, Zhao D, Wan Y (2010) Nanocasting. A versatile strategy for creating nanostructured porous materials. RSC Publishing, Cambridge, UK
Ríos E, Nguyen-Cong H, Marco JF, Gancedo JR, Chartier P, Gautier JL (2000) Indirect oxidation of ethylene glycol by peroxide ions at Ni0.3Co2.7O4 spinel oxide thin film electrodes. Electrochim Acta 45:4431–4440
Tanaka S, Tate MP, Nishiyama N, Ueyama K, Hillhouse HW (2006) Structure of mesoporous silica thin films prepared by contacting PEO106–PPO70–PEO106 films with vaporized TEOS. Chem Mater 18:5461–5466
Verma S, Joshi HM, Jagadale T, Chawla A, Chandra R, Ogale S (2008) Nearly monodispersed multifunctional NiCo2O4 spinel nanoparticles: magnetism, infrared transparency and radiofrequency absorption. J Phys Chem C 112:15106–15112
Wei T-Y, Chen C-H, Chien H-C, Lu S-Y, Hu C-C (2010) A cost-effective supercapacitor material of ultrahigh specific capacitances: spinel nickel cobaltite aerogels from an epoxi-driven sol-gel process. Adv Mater 22:347–351
Yang H, Zhao D (2005) Synthesis of replica mesostructures by the nanocasting strategy. J Mater Chem 15:1217–1231
Yang H, Shi Q, Tian B, Lu Q, Gao F, Xie S, Fan J, Yu C, Tu B, Zhao D (2003) One-step nanocasting synthesis of highly-ordered single crystalline indium oxide nanowire arrays from mesostructured frameworks. J Am Chem Soc 125:4724–4725
Yu C, Yu Y, Zhao D (2000) Highly ordered large caged cubic mesoporous silica structures templated by triblock PEO-PBO-PEO copolymer. Chem Commun 575–576
Yue W, Zhou W (2007) Synthesis of porous single crystals of metal oxides via a solid–liquid route. Chem Mater 19:2359–2363
Zhao D, Feng J, Huo Q, Melosh N, Fredrickson GH, Chmelka BF, Stucky GD (1998a) Triblock copolymer syntheses of mesoporous silica with periodic 50–300 angstrom pores. Science 279:548–552
Zhao D, Huo Q, Feng J, Chmelka BF, Stucky GD (1998b) Nonionic triblock and star diblock copolymer and oligomeric surfactant syntheses of highly ordered, hydrothermally stable, mesoporous silica structures. J Am Chem Soc 120:6024–6036
Zhao Y, Chen X, Yang C, Zhang G (2007) Mesoscopic simulation on phase behaviour of Pluronic P123 aqueous solution. J Phys Chem B 111:13937–13942
Zhu KK, Yue B, Zhou WZ, He HY (2003) Preparation of three-dimensional chromium oxide porous single crystals templated by SBA-15. Chem Commun 98–99
Acknowledgments
The authors thank BASF Corporation for kindly supplying the P123 precursor and MATGAS 2000 AIE for the provision of BET facilities. We acknowledge funding from the Spanish Ministerio de Ciencia e Innovación (MICINN) and the Generalitat de Catalunya through MAT 2010-20616-C02-02 and 2009-SGR-1292 projects, respectively. E.P. is indebted to the DURSI of the Generalitat de Catalunya for the postdoctoral Beatriu de Pinós fellowship. M.D.B. was partially supported by an ICREA ACADEMIA award.
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Cabo, M., Pellicer, E., Rossinyol, E. et al. Influence of the preparation method on the morphology of templated NiCo2O4 spinel. J Nanopart Res 13, 3671–3681 (2011). https://doi.org/10.1007/s11051-011-0287-1
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DOI: https://doi.org/10.1007/s11051-011-0287-1