副产物硫酸铵辅助制备氧化镁纳米棒
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摘要
为了寻找规模化合成氧化镁纳米棒的新方法,通过氨水沉淀硫酸镁制备了花状氢氧化镁前驱体,探索了前驱体热分解过程中副产物硫酸铵的存在和煅烧温度对产物物相和形貌的影响。结果表明:表面吸附硫酸铵的花状氢氧化镁800℃煅烧2 h再洗涤,可以得到长度1~2μm、直径30~100 nm的氧化镁纳米棒;沉淀产物花状氢氧化镁经洗涤后再在600~800℃煅烧2 h,可以获得平均直径2μm的氧化镁纳米花;副产物硫酸铵对氧化镁纳米棒形成起了结构导向的作用。
To explore a novel scalable approach for synthesis ofmagnesium oxide(Mg O) nanorods,flower-like magnesium hydroxide(Mg(OH)2) precursors were prepared by chemical precipitation method using magnesium sulfate and ammonia hydroxide as raw materials. The effects of calcinations temperature and the presence of byproduct sulfate ammonia in the calcined precursors on phases and morphologies of the resultants were investigated. The results showed that the flower-like Mg(OH)2 with sulfate ammonia absorbed on the surface can evolve into nanorods with 1-2 μm in length and 30-100 nm in diameter after 2 h annealing at 800 ℃ and subsequent washing while the as-obtained flower-like Mg(OH)2 subjected to washing can yield Mg O nanoflowers with an average diameter of2 μm after 2 h annealing in range of 600-800 ℃. Hence the presence ofbyproduct sulfate ammonia in the calcination process plays a role in the growth of Mg O nanorods.
To explore a novel scalable approach for synthesis ofmagnesium oxide(Mg O) nanorods,flower-like magnesium hydroxide(Mg(OH)2) precursors were prepared by chemical precipitation method using magnesium sulfate and ammonia hydroxide as raw materials. The effects of calcinations temperature and the presence of byproduct sulfate ammonia in the calcined precursors on phases and morphologies of the resultants were investigated. The results showed that the flower-like Mg(OH)2 with sulfate ammonia absorbed on the surface can evolve into nanorods with 1-2 μm in length and 30-100 nm in diameter after 2 h annealing at 800 ℃ and subsequent washing while the as-obtained flower-like Mg(OH)2 subjected to washing can yield Mg O nanoflowers with an average diameter of2 μm after 2 h annealing in range of 600-800 ℃. Hence the presence ofbyproduct sulfate ammonia in the calcination process plays a role in the growth of Mg O nanorods.
引文
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[3]YANG P D,LIEBER C M.Nanorod-superconductor composites:a pathway to materials with high critical current densities[J].Science,1996,273(5283):1836-1840.
[4]SALEHIFAR N,ZARGHAMI Z,RAMEZANI M.A facile,novel and low-temperature synthesis of Mg O nanorods via thermal decomposition using new starting reagent and its photocatalytic activity evaluation[J].Materials Letters,2016,167:226-229.
[5]PASHCHANKA M,HOFFMANN R C,SCHNEIDER J J.Controlled synthesis and characterisation of Mg O nanoparticles,thin films and polycrystalline nanorods derived from a Mg(II)single source precursor[J].Journal of Materials Chemistry,2010,20(5):957-963.
[6]YAN L,ZHUANG J,SUN X M,et al.Formation of rodlike Mg(OH)2nanocrystallites under hydrothermal conditions and the conversion to Mg O nanorods by thermal dehydration[J].Materials Chemistry and Physics,2002,76(2):119-122.
[7]CUI Z,MENG G W,HUANG W D,et al.Preparation and characterization of Mg O nanorods[J].Materials Research Bulletin,2000,35(10):1653-1659.
[8]翟华嶂,安晓强,曹传宝,等.Mg O单晶一维纳米结构的制备与表征[J].稀有金属材料与工程,2008(S1):667-670.
[9]ZHAO M,CHEN X L,WANG W J,et al.Self-catalyzed growth of magnesium oxide nanorods[J].Materials Letters,2006,60(16):2017-2019.
[10]XIA B,LENGGORO I W,OKUYAMA K.Novel route to nanoparticle synthesis by salt-assisted aerosol decomposition[J].Advanced Materials,2001,13(20):1579-1582.
[11]LI Y X,CHEN W F,ZHOU X Z,et al.Synthesis of Ce O2nanoparticles by mechanochemical processing and the inhibiting action of Na Cl on particle agglomeration[J].Materials Letters,2005,59(1):48-52.
[12]CHEN W F,ZHUO M P,LIU Y,et al.Uniform octahedral-shaped Y2O3:Eu3+submicron single crystals:solidstate synthesis,formation mechanism and photoluminescence property[J].Journal of Alloys and Compounds,2016,656:764-770.
[13]CHEN W F,HONG J M,LI Y X.Facile fabrication of perovskite single-crystalline La Mn O3nanocubes via a salt-assisted solution combustion process[J].Journal of Alloys and Compounds,2009,484(1):846-850.
[14]CHEN W F,LIU M,LIN Y C,et al.A novel synthesis route to Sn1-xRExO2-x/2nanorods via microwave-induced salt-assisted solution combustion process[J].Ceramics International,2013,39(7):7545-7549.
[15]GONZLEZ-CORTS S L,IMBERT F E.Fundamentals,properties and applications of solid catalysts prepared by solution combustion synthesis(SCS)[J].Applied Catalysis A:General,2013,452:117-131.
[16]TONG Y P,ZHAO S B,WANG X,et al.Synthesis and characterization of Er2Sn2O7nanocrystals by salt-assistant combustion method[J].Journal of Alloys and Compounds,2009,479(1):746-749.
[17]制盐工业通用试验方法硫酸根的测定:GB/T 13025.8—2012[S].
[18]闫鹏,秦丹,邢娟,等.氧化镁纳米分级结构的合成及生长机理分析[J].物理实验,2011(3):11-17.
[19]MAKHLUF S,DROR R,NITZAN Y,et al.Microwave-assisted synthesis of nanocrystalline Mg O and its use as a bacteriocide[J].Advanced Functional Materials,2005,15(10):1708-1715.