均匀沉淀水热法微/纳米Sm_2O_3的合成与表征
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摘要
以尿素为沉淀剂,采用均匀沉淀水热法,合成了微/纳米Sm2O3及其前驱体。利用XRD、TG-DTA和扫描电子显微镜(SEM)等表征手段对产物进行测试与分析,确定前驱体的焙烧温度为800℃。考察了反应温度和硝酸钐浓度对微/纳米Sm2O3形貌、尺寸的影响,探讨了Sm2O3及其前驱体的形成过程,提出了不同形貌微/纳米Sm2O3可能的形成机理。结果表明,当反应温度分别为100℃、140℃和170℃时,微/纳米Sm2O3的形貌依次由球状变为树枝状再变为双扇状;当硝酸钐的浓度分别为0.4 mol/L、0.6 mol/L和0.8 mol/L时,球状微/纳米Sm2O3的尺寸依次为1.49~3.18μm、1.32~2.59μm和0.69~1.41μm,且随硝酸钐的浓度的增大而减小。
The precursor of Sm2O3 was synthesized by homogeneous precipitation hydrothermal method using urea as a precipitating agent.The Sm2O3 nanoparticles were then prepared by calcining the precursors at 800 ℃.The structures,morphologies and size of products were characterized by XRD,TG and scanning electron microscope( SEM).The influences of reaction temperature and concentration of Sm( NO3)3·6H2O on the morphologies and size of micro / nano Sm2O3 were studied.The formation process of the precursors of Sm2O3 was discussed.The possible formation mechanism of the morphologies of micro / nano Sm2O3 was proposed.The results show that the micro / nano Sm2O3 with sphere,dendritic and dual-fan shapes are controlledly synthesized with the increase of reaction temperature( 100 ℃,140 ℃and 170 ℃).The size of the sphere micro / nano Sm2O3decreases( 1.49-3.18 μm,1.32-2.59 μm and0.69-1.41 μm) with the increase of the concentration of Sm( NO3)3·6H2O( 0.4 mol / L,0.6 mol / L and0.8 mol / L).
The precursor of Sm2O3 was synthesized by homogeneous precipitation hydrothermal method using urea as a precipitating agent.The Sm2O3 nanoparticles were then prepared by calcining the precursors at 800 ℃.The structures,morphologies and size of products were characterized by XRD,TG and scanning electron microscope( SEM).The influences of reaction temperature and concentration of Sm( NO3)3·6H2O on the morphologies and size of micro / nano Sm2O3 were studied.The formation process of the precursors of Sm2O3 was discussed.The possible formation mechanism of the morphologies of micro / nano Sm2O3 was proposed.The results show that the micro / nano Sm2O3 with sphere,dendritic and dual-fan shapes are controlledly synthesized with the increase of reaction temperature( 100 ℃,140 ℃and 170 ℃).The size of the sphere micro / nano Sm2O3decreases( 1.49-3.18 μm,1.32-2.59 μm and0.69-1.41 μm) with the increase of the concentration of Sm( NO3)3·6H2O( 0.4 mol / L,0.6 mol / L and0.8 mol / L).
引文
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[15]Zhu W Q,Ma J,Xu L,et al.Controlled Synthesis of Nd(OH)3and Nd2O3Nanoparticles by Microemulsion Method[J].Materials Chemistry and Physics,2010,22:362-367.
[2]He X L,Ye F,Zhang H J,et al.Effect of Sm2O3Content on Microstructure and Thermal Conductivity of Spark Plasma Sintered AIN Ceramics[J].Journal of Alloys and Compounds,2009,482(1):345-348.
[3]He H G,Cheng J G,Wang Y H,et al.Effects of Sm2O3Addition on Sintering Behavior and Property of Y-Zr O2Ceramics[J].Journal of the Chinese Rare Earth Society,2010,28(4):426-430.
[4]Cao X Z,Xue X G,Jiang T,et al.Mechanical Properties of UHMWPE/Sm2O3Composite Shielding Material[J].Journal of Rare Earths,2010,28(9):482-484.
[5]Li J S,Zhang Y,Sun H,et al.Preparation,Microstructure and Capability of Sm2O3/Epoxy Resin Composity and Polyacrylic Acid Samarium/Epoxy Resin Composity[J].Acta Materiae Compositae Sinica,2011,28(1):44-49.
[6]Geng S H,Zhu W Q,Chang P M,et al.Preparation of Sm2O3Nanoparticles in the Media of Reverse Microemulsions[J].Acta Phys.-Chim.Sin.,2008,24(9):1609-1614.
[7]Mei Y,Wang W,Sun H,et al.Preparation and Morphology of Nano-size Ceria by A Stripping Precipitationusing Oxalic Acid as A Precipitating Agent[J].Journal of Rare Earths,2012,30(12):1265-1269.
[8]Zhu W Q,Xu L,Ma J,et al.Effect of the Thermodynamic Properties of W/O Microemulsions on Samarium Oxide Nanoparticle Size[J].Journal of Colloid and Interface Science,2009,340:119-125.
[9]Yin L X,Wang D,Huang J F,et al.Controllable Synthesis and Optical Properties of One-dimensional Sm2O3Nanocrystalline[J].Journal of Synthetic Crystals,2014,43(12):3204-3208.
[10]Huang J F,Huang Y,Cao L Y,et al.Sm2O3Optical Thin Film Prepared by the Sol-Gel Process[J].Journal of the Chinese Ceramic Society,2006,34(11):1342-1344.
[11]Xia Y S,Dai H X,He H.Fabrication and Characterization of Sphere-like and Rod-like Eu2O3and Sm2O3Nanoparticles[J].Journal of Beijing University of Technology,2010,36(1):88-91.
[12]Yin L X,Wang F F,Huang J F,et al.Influences of Reaction Time on Sm2O3Microcrystallites Prepared by Hydrothermal Method[J].Journal of Shannxi University of Science&Technology,2014,32(2):47-59.
[13]Huang Y,Huang J F,Cao L Y,et al.Preparation of Sm2O3Crystallite Thin Film by Hydrothemal Method[J].Journal of Synthetic Crystals,2007,36(3):628-630.
[14]Zhu W Q,Zhao R,Qu F,et al.Synthesis and Characterization of Three-dimensional Flower Spherical Micro/nano Sm2O3by Homogeneous Precipitation Hydrothermal Method[J].Fine Chemicals,2014,31(11):1298-1300.
[15]Zhu W Q,Ma J,Xu L,et al.Controlled Synthesis of Nd(OH)3and Nd2O3Nanoparticles by Microemulsion Method[J].Materials Chemistry and Physics,2010,22:362-367.