Abstract
In this report, we consider the peculiarities of sol–gel–xerogel transformations, which occurs in the thin layer at the FeCl2/FeCl3 water solution and gaseous NH3 interface. A thin layer consisting of nanoparticles of Fe(OH)3 and Fe3O4 is formed as a result of interfacial reaction. Depending on the time of treatment with gaseous ammonia, it was possible to obtain either a freestanding layer with a thickness of 1 μm or microtubular structures (scrolls). Synthetic conditions, under which a large number of preferentially oriented microtubes are formed with diameters of about 10 and up to 200-μm long, were determined. The synthesized structures consisted of crystalline Fe3O4 nanoparticles with an average diameter of about 5–10 nm incorporated in an amorphous matrix. Layers and tubes were characterized by X-ray diffraction analysis, scanning and transmission electron microscopy (SEM and TEM), and X-ray photoelectron spectroscopy. The model, concerning sol–gel–xerogel transformations in the thin layer, formed after interaction at the salt solution–gaseous reagent interface, was suggested. The magnetic properties of the products were studied.
Highlights
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A sol–gel–xerogel transformation in the thin layer at the gas–solution interface has been studied.
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Tubular or planar morphology of the products depended on synthesis conditions.
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The opportunity to obtain an array of oriented microtubes was demonstrated for the first time.
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The layers and tubes based on Fe3O4 demonstrated superparamagnetic properties.
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References
Cheetham AK, Mellot CF (1997) In situ studies of the sol-gel synthesis of materials. Chem Mater 9:2269–2279
Castellón E, Zayat M, Levy D (2018) Sol-gel materials for electro-optical and optically active humidity-sensitive devices. J Sol-Gel Sci Technol. https://doi.org/10.1007/s10971-018-4852-2
Shilova OA, Khamova TV, Panova GG, Anikina LM, Artem’eva AM, Kornyukhin DL (2018) Using the sol–gel technology for the treatment of barley seeds. Glass Phys Chem 44:26–32
Stergar J, Maver U (2016) Review of aerogel-based materials in biomedical applications. J Sol-Gel Sci Technol 77:738–752
Ismail WNW (2016) Sol–gel technology for innovative fabric finishing—a review. J Sol-Gel Sci Technol 78:698–707
Jones JR (2013) Review of bioactive glass: from Hench to hybrids. Acta Biomater 9:4457–4486
Segal D (1997) Chemical synthesis of ceramic materials. J Mater Chem 7:1297–1305
Wen J, Wilkes GL (1996) Organic/inorganic hybrid network materials by the sol-gel approach. Chem Mater 8:1667–1681
Guglielmi M, Martucci A (2018) Sol-gel nanocomposites for optical applications. J Sol-Gel Sci Technol 88:551–563
Kalinina MV, Morozova LV, Egorova TL, Arsentyev MY, Khlamov II, Tikhonov PA, Shilova OA (2017) Composite materials based on oxides of d and f elements and carbon layers. Inorg Mater: Appl Res 8:254–259
Begum R, Naseem K, Farooqi ZH (2016) A review of responsive hybrid microgels fabricated with silver nanoparticles: synthesis, classification, characterization and applications. J Sol-Gel Sci Technol 77:497–515
Mackenzie JD, Bescher EP (2007) Chemical routes in the synthesis of nanomaterials using the sol-gel process. Acc Chem Res 40:810–818
Shilova OA, Gubanova NN, Ivanova AG, Arsent’ev MY, Ukleev VA (2017) Composition and structure of platinum-containing thin composite films prepared from silica sols. Russ J Inorg Chem 62:645–653
Zaharescu M, Predoana L, Pandele J (2018) Relevance of thermal analysis for sol–gel-derived nanomaterials. J Sol-Gel Sci Technol 86:7–23
Caruso RA, Antonietti M (2001) Sol-gel nanocoating: an approach to the preparation of structured materials. Chem Mater 13:3272–3282
Aparicio M, Mosa J (2018) Electrochemical characterization of sol–gel coatings for corrosion protection of metal substrates. J Sol-Gel Sci Technol 88:77–89
Mitzi DB (2001) Thin-film deposition of organic-inorganic hybrid materials. Chem Mater 13:3283–3298
Moriguchi I, Maeda H, Teraoka Y, Kagawa S (1997) Preparation of a TiO2 nanoparticulate film using a two-dimensional sol-gel process. Chem Mater 9:1050–1057
Facca F, Puccetti G, Leblanc RM (1999) Synthesis of nanometer scale oxide-based titania films by a two-dimensional sol-gel process at the air-liquid interface. Colloids Surf A: Physicochem Eng Asp 149(1-3):89–98
Oswald M, Hessel V, Riedel R (1999) Formation of ultra-thin ceramic TiO2 films by the Langmuir-Blodgett technique—a two-dimensional sol-gel process at the air-water interface. Thin Solid Films 339:284–289
Moriguchi I, Tsujigo Y, Teraoka Y, Kagawa S (1999) Two-dimensional sol-gel synthesis of hetero-layered nanostructure composed of ultrathin TiO2 and ZrO2 laminae. Adv Mater 11:997–1000
Tanaka S, Nishiyama N, Oku Y, Egashira Y, Ueyama K (2004) Nano-architectural silica thin films with two-dimensionally connected cagelike pores synthesis from vapor phase. J Am Chem Soc 126:4854–4858
Moriguchi I, Tsujigo Y, Teraoka Y, Kagawa S (2000) Two-dimensional sol-gel synthesis of ultrathin zirconia and hetero-layered titania/zirconia films. J Sol-Gel Sci Technol 19:227–230
Mori T, Tanaka H, Dalui A, Mitoma N, Suzuki K, Matsumoto M, Aggarwal N, Patnaik A, Acharya S, Shrestha LK, Sakamoto H, Itami K, Ariga K (2018) Carbon nanosheets by morphology-retained carbonization of two-dimensional assembled anisotropic carbon nanorings. Angew Chem Int Ed 57:9679–9683
Seki T (2018) A wide array of photoinduced motions in molecular and macromolecular assemblies at interfaces. Bull Chem Soc Jpn 91(7):1026–1057
Noskov BA, Bykov AG (2015) Dilational surface rheology of polymer solutions. Russ Chem Rev 84:634–652
Gulina L, Tolstoy V (2011) In: Vyvenko OF (ed) State-of-the-art trends of scientific researches of artificial and natural nanoobjects. Saint-Petersburg State University, Saint-Petersburg, Russia
Gulina LB, Tolstoy VP (2014) Reaction of gaseous hydrogen fluoride with the surface of lanthanum chloride solution to form LaF3·nH2O film and microtubes thereof. Russ J Gen Chem 84:1472–1475
Gulina LB, Tolstoy VP, Tolstobrov EV (2017) Facile synthesis of 2D silver nanocrystals by a gas–solution interface technique. Mendeleev Commun 27:634–636
Gulina LB, Tolstoy VP, Kasatkin IA, Kolesnikov IE, Danilov DV (2017) Formation of oriented LaF3 and LaF3:Eu3+ nanocrystals at the gas—solution interface. J Fluor Chem 200:18–23
Gulina LB, Tolstoy VP, Kasatkin IA, Murin IV (2017) Facile synthesis of scandium fluoride oriented single-crystalline rods and urchin-like structures by a gas-solution interface technique. CrystEngComm 19:5412–5416
Gulina LB, Tolstoy VP, Petrov YV, Danilov DV (2018) Interface-assisted synthesis of single-crystalline ScF3 microtubes. Inorg Chem 57:9779–9781
Gulina LB, Tolstoy VP, Kasatkin IA, Fateev SA (2018) Flower-like silver nanocrystals: facile synthesis via a gas–solution interface technique. J Mater Sci 53:8161–8169
Tolstoy VP, Gulina LB (2014) Synthesis of birnessite structure layers at the solution-air interface and the formation of microtubules from them. Langmuir 30:8366–8372
Gulina LB, Tolstoy VP, Kasatkin IA, Petrov YV (2015) Facile synthesis of LaF3 strained 2D nanoparticles and microtubes at solution-gas interface. J Fluor Chem 180:117–121
Tolstoi VP, Gulina LB (2013) Ozone interaction with manganese acetate solution. Formation of HxMnO2·nH2O layers and microtubes based on them. Russ J Gen Chem 83:1635–1639
Gulina L, Tolstoy V, Kuklo L, Mikhailovskii V, Panchuk V, Semenov V (2018) Synthesis of Fe(OH)3 microtubes at the gas–solution interface and their use for the fabrication of Fe2O3 and Fe microtubes. Eur J Inorg Chem 17:1842–1846
Tolstoy VP, Gulina LB (2013) New way of As2S3 microtubules preparation by roll up thin films synthesized at the air-solution interface. J Nano Electron Phys 5:01003
Gulina LB, Tolstoy VP, Lobinsky AA, Petrov YV (2018) Formation of Fe and Fe2O3 microspirals via interfacial synthesis. Part Part Syst Charact 35:1800186
Farimani MHR, Shahtahmasebi N, Rezaee Roknabadi M, Ghows N, Kazemi A (2013) Study of structural and magnetic properties of superparamagnetic Fe3O4/SiO2 core-shell nanocomposites synthesized with hydrophilic citrate-modified Fe3O4 seeds via a sol-gel approach. Phys E: Low-Dimens Syst Nanostruct 53:207–216
Ko Y, Kwon M, Song Y, Lee SW, Cho J (2018) Thin-film electrode design for high volumetric electrochemical performance using metal sputtering-combined ligand exchange layer-by-layer assembly. Adv Funct Mater. https://doi.org/10.1002/adfm.201804926
Zhang J, Liu M, Liu Z, Yang T, He Q, Yang K, Wang H (2017) Studies of malachite green adsorption on covalently functionalized Fe3O4@SiO2–graphene oxides core–shell magnetic microspheres. J Sol-Gel Sci Technol 82:424–431
Gurenko VE, Tolstoy VP, Gulina LB (2017) The effect of microtube formation with walls, containing Fe3O4 nanoparticles, via gas-solution interface technique by hydrolysis of the FeCl2 and FeCl3 mixed solution with gaseous ammonia. Nanosyst Phys Chem Math 8:471–475
Biesinger MC, Payne BP, Grosvenor AP, Lau LWM, Gerson AR, Smart RSC (2011) Resolving surface chemical states in XPS analysis of first row transition metals, oxides and hydroxides: Cr, Mn, Fe, Co and Ni. Appl Surf Sci 257:2717–2730
Anderson JF, Kuhn M, Diebold U (1996) Epitaxially grown Fe3O4 thin films: an XPS study. Surf Sci Spectra 4:266–272
Yamashita T, Hayes P (2008) Analysis of XPS spectra of Fe2+ and Fe3+ ions in oxide materials. Appl Surf Sci 254:2441–2449
John F, Moulder WFS, Peter ES, Kenneth DB (1995) Handbook of X-ray photoelectron spectroscopy. Physical Electronics, Inc, Minnesota, USA
Thermo scientific data system for XPS. https://xpssimplified.com. Accessed 29 Nov 2018.
Nakayama M, Konishi S, Tagashira H, Ogura K (2005) Electrochemical synthesis of layered manganese oxides intercalated with tetraalkylammonium ions. Langmuir 21:354–359
Wang J, Sun J, Sun Q, Chen Q (2003) One-step hydrothermal process to prepare highly crystalline Fe3O4 nanoparticles with improved magnetic properties. Mater Res Bull 38:1113–1118
Esmaeilpour M, Javidi J, Zahmatkesh S (2016) One-pot synthesis of 1- and 5-substituted 1H-tetrazoles using 1,4-dihydroxyanthraquinone–copper(II) supported on superparamagnetic Fe3O4@SiO2 magnetic porous nanospheres as a recyclable catalyst. Appl Organomet Chem 30:897–904
Lee J, Lee Y, Youn JK, Na HB, Yu T, Kim H, Lee SM, Koo YM, Kwak JH, Park HG, Chang HN, Hwang M, Park JG, Kim J, Hyeon T (2008) Simple synthesis of functionalized superparamagnetic magnetite/silica core/shell nanoparticles and their application as magnetically separable high-performance biocatalysts. Small 4:143–152
Abbas M, Abdel-Hamed MO, Chen J (2017) Efficient one-pot sonochemical synthesis of thickness-controlled silica-coated superparamagnetic iron oxide (Fe3O4/SiO2) nanospheres. Appl Phys A: Mater Sci Process 123(12):775
Faaliyan K, Abdoos H, Borhani E, Afghahi SSS (2018) Magnetite-silica nanoparticles with core-shell structure: single-step synthesis, characterization and magnetic behavior. J Sol-Gel Sci Technol 88:609–617
Acknowledgements
This work was supported by the Russian Science Foundation (grant No. 16-13-10223). We are grateful to the Research Park of St. Petersburg State University for assistance in studies of our samples: Nanotechnology Center, Centre for Innovative Technologies of Composite Nanomaterials, and Centre for X-Ray Diffraction Studies.
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Gurenko, V., Gulina, L. & Tolstoy, V. Sol–gel–xerogel transformations in the thin layer at the salt solution–gaseous reagent interface and the synthesis of new materials with microtubular morphology. J Sol-Gel Sci Technol 92, 342–348 (2019). https://doi.org/10.1007/s10971-019-04949-w
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DOI: https://doi.org/10.1007/s10971-019-04949-w