CN100347080C - 微波合成稀土化合物纳米棒的方法 - Google Patents
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Abstract
本发明公开了一种微波合成稀土化合物La1-xRexPO4(Re=Ce,Eu或Tb;x=0.05~0.5)纳米棒的方法,其步骤如下:1)将氧化镧粉末和氧化铈、氧化铕或氧化铽粉末溶解在硝酸溶液中形成混合溶液,2)将混合溶液的pH值调节至2.5~4.5,搅拌下加入NH4H2PO4溶液,生成胶状沉淀物;3)将胶状物在氮气保护和回流条件下于微波炉中加热,然后自然冷却,用离心分离和去离子水充分洗涤后收集并干燥。本发明的合成方法具有快速,简单,效率高和节能的优点。制得的纳米棒的平均直径在12~17纳米,长度在50~1100纳米。
Description
技术领域
本发明涉及稀土化合物纳米棒的制备方法,尤其涉及微波合成稀土化合物La1-xRexPO4(Re=Ce,Eu或Tb;x=0.05~0.5)纳米棒的方法。
背景技术
由于稀土元素的4f电子特性,稀土化合物具有独特的物理化学、光学、电学和磁学性能,它们在电子学、磁性材料、光电材料和催化等领域具有广泛的应用。我国具有丰富的稀土资源,研究和制备稀土化合物的纳米材料对稀土资源的深化利用和拓展其新的应用领域具有重要的科学意义和应用价值。La1-x-RexPO4(Re=Ce,Eu,Tb;0<x<1)是一种重要的双稀土金属化合物,它具有较高的发光量子效率和不同寻常的磁学特性,因此它在特种玻璃、激光技术、荧光灯具和等离子显示器等方面具有重要的应用。例如溶胶-凝胶法制备的La0.95Eu0.05PO4,La0.84Tb0.16PO4和La0.8Ce0.2PO4纳米晶薄膜具有良好的荧光发光性能(M.Yu,J.Lin,J.Fu,et al.,Sol-gel synthesis and photoluminescent properties ofLaPO4:A(A=Eu3+,Ce3+,Tb3+)nanocrystalline thin films,J.of Materials Chemistry,2003,14:1413-1419)。
另一方面,最近几年一维纳米材料的合成和应用引起了人们的极大兴趣。一维纳米材料(如:纳米线,纳米棒,纳米带和纳米管)具有独特的电性能、力学性能、磁性能和电子传递性能。毫无疑问,一维纳米结构的稀土化合物的纳米材料与体相材料相比将具有新的物理和化学性质。因此,一维纳米结构的稀土化合物纳米材料的合成和应用研究引起了人们的广泛关注。例如:与纳米和微米的粒子相比,铕掺杂的磷酸镧纳米线显示了更高的荧光量子效率(L.X.Yu,H.W.Song,S.Z.Lu,et al.,Luminescent Properties of LaPO4:Eu Nanoparticles andNanowires,J.Phys.Chem.B,2004,108:16697-16702);Pr6O11纳米棒作为载体负载的金纳米粒子比用Pr6O11纳米粒子作为载体负载的金纳米粒子具有更高对CO催化氧化的性能(P.X.Huang,F.Wu,B.L.Zhu,et al.,Praseodymiun hydroxide abdoxide nanorods and Au/Pr6O11 nanorod catalysts for CO oxidation,J.Phys.Chem.B,2006:110,1614-1620)。目前,水热技术是合成一维纳米结构稀土化合物的主要方法。如:X.Wang等报道了用水热技术合成稀土氢氧化物纳米棒和纳米管的方法(X.M.Sun,D.P.Yu,B.S.Zou,Y.D.Li,Rare earth compound nanotubes,Adv.Mater.,2003,15:1442-1445);R.X.Yan等用水热处理方法合成了掺杂和未掺杂的稀土离子磷酸盐纳米线和纳米棒(X.M.Sun,X.Wang,Q.Peng and Y.D.Li,Chem.Eur.J.2005,11:2183-2195);L.X.Yu等也用类似的水热技术合成了掺杂Ce3+和Tb3+离子的磷酸镧纳米线和微米棒(H.W.Song,Z.X.Liu,L.M.Yang,S.Z.Lu,Z.H.Zheng J.Phys.Chem.B 2005,109:11450-11455)。但是水热方法需要较高的反应温度、较长的反应时间,因此需要消耗较多的能源。
发明内容
本发明的目的是提供一种工艺简单、快速的采用微波加热合成稀土化合物纳米棒的方法。
本发明合成的稀土化合物纳米棒的表达式为La1-xRexPO4,其中Re=Ce,Eu或Tb;x=0.05~0.5,合成步骤如下:
1)将氧化镧粉末和氧化铈、氧化铕或氧化铽粉末溶解在硝酸溶液中形成混合溶液,混合溶液中稀土离子镧和稀土离子铈、铕或铽的摩尔比为95∶5~50∶50;
2)将上述混合溶液的pH值调节至2.5~4.5,搅拌下加入过量的NH4H2PO4溶液,生成胶状沉淀物;
3)将胶状物在氮气保护和回流条件下于微波炉中加热,时间20~60min,然后自然冷却,用离心分离和去离子水充分洗涤后收集并干燥。
本发明方法的反应过程可以表示如下:
本发明的有益效果在于:
本发明与现有的水热处理合成方法比较,具有工艺简单、成本低廉、快速、节能和效率高的优点。制得的La1-xRexPO4(Re=Ce,Eu,Tb;x=0.05~0.5)纳米棒的平均直径在12~17纳米,长度在50~1100纳米。具有化学性质稳定和光量子产率高的特点,在光学玻璃、激光材料、荧光材料和等离子显示器方面具有广泛的应用。
具体实施方式
实施例1:制备La0.8Ce0.2PO4纳米棒
将0.456g的La2O3粉末和0.115g的Ce2O3粉末溶解在50mL 10%的HNO3溶液中形成混合溶液,混合溶液中La3+离子和Ce3+离子的摩尔比La3+∶Ce3+=80∶20。然后用氨水调节混合溶液的pH值为2.6。在电磁搅拌下加入75mL 0.05mol/L的NH4H2PO4水溶液,生成胶状沉淀物。最后将得到的胶状物转移到250ml圆底烧瓶中并置于微波炉中,先通氮气30min,然后在氮气保护和回流条件下微波加热20min,微波加热功率为最大功率的80%(最大功率为600W),加热结束后继续通氮气至冷却到室温后,沉淀产物用离心分离和去离子水充分洗涤,在80℃真空下干燥后得到La0.8Ce0.2PO4纳米棒。透射电镜观察显示纳米棒平均直径为16纳米,长度在50~600纳米。
实施例2:制备La0.5Ce0.5PO4纳米棒
将0.815g的La2O3粉末和0.820g的Ce2O3粉末溶解在35mL 20%的HNO3溶液中形成混合溶液,混合溶液中La3+离子和Ce3+离子的摩尔比为La3+∶Ce3+=50∶50。然后用氨水调节混合溶液的pH值为4.5,在电磁搅拌下加入70ml的0.15M的NH4H2PO4,生成胶状沉淀物,将得到的胶状物转移到250ml圆底烧瓶中并置于微波炉中,先通氮气40min,然后在氮气保护和回流条件下微波加热20min,微波加热功率为最大功率的70%(最大功率为600W),加热结束后继续通氮气至冷却到室温后,沉淀产物用离心分离和去离子水充分洗涤,在80℃真空下干燥后得到La0.5Ce0.5PO4纳米棒。透射电镜观察显示纳米棒平均直径为13纳米,长度在60~1100纳米。
实施例3:制备La0.95Eu0.05PO4纳米棒
将0.542g的La2O3粉末和0.031g的Eu2O3粉末溶解在50mL 10%的HNO3溶液中形成混合溶液,混合溶液中La3+和Eu3+的摩尔比为La3+∶Eu3+=95∶5。然后用氨水调节混合溶液的pH值为2.9,在电磁搅拌下加入75ml的0.05M的NH4H2PO4水溶液,生成胶状沉淀物,最后将得到的胶状物转移到250ml圆底烧瓶中并置于微波炉中,先通氮气30min,然后在氮气保护和回流条件下微波加热40min,微波加热功率为最大功率的60%(最大功率为600W),加热结束后继续通氮气至冷却到室温后,沉淀产物用离心分离和去离子水充分洗涤,在80℃真空下干燥后得到La0.95Eu0.05PO4纳米棒。透射电镜观察显示纳米棒平均直径为17纳米,长度在50~650纳米。
实施例4:制备La0.8Eu0.2PO4纳米棒
将0.326g的La2O3粉末和0.088g的Eu2O3粉末溶解在50mL 10%的HNO3溶液中形成混合溶液,混合溶液中La3+和Eu3+的摩尔比为La3+∶Eu3+=80∶20。然后用氨水调节混合溶液的pH值为3.3,在电磁搅拌下加入70ml的0.05M的NH4H2PO4水溶液,生成胶状沉淀。最后将得到的胶状物转移到250ml圆底烧瓶中并置于微波炉中,先通氮气20min,然后在氮气保护和回流条件下微波加热20min,微波加热功率为最大功率的60%(最大功率为600W),加热结束后继续通氮气至冷却到室温后,沉淀产物用离心分离和去离子水充分洗涤,在80℃真空下干燥后得到掺杂Eu的制备La0.8Eu0.2PO4纳米棒。透射电镜观察显示纳米棒平均直径为15纳米,长度在55~800纳米。
实施例5:制备La0.8Tb0.2PO4纳米棒
将0.639g的La2O3粉末和0.183g的Tb4O7粉末溶解在25mL浓HNO3溶液中形成混合溶液,混合溶液中La3+和Eu3+的摩尔比为La3+∶Tb3+=80∶20。然后用2M的氢氧化钾溶液调节混合溶液的pH值为2.7,在电磁搅拌下加入75ml的0.07M的NH4H2PO4水溶液,生成胶状沉淀。最后将得到的胶状物转移到250ml圆底烧瓶中并置于微波炉中,先通氮气40min,然后在氮气保护和回流条件下微波加热40min,微波加热功率为最大功率的60%(最大功率为600W),加热结束后继续通氮气至冷却到室温后,沉淀产物用离心分离和去离子水充分洗涤,在80℃真空下干燥后得到La0.8Tb0.2PO4纳米棒。透射电镜观察显示纳米棒平均直径为13纳米,长度在55~870纳米。
Claims (1)
1.微波合成稀土化合物纳米棒的方法,其特征在于稀土化合物纳米棒的表达式为La1-xRexPO4,其中Re=Ce、Eu或Tb;x=0.05~0.5,合成步骤如下:
1)将氧化镧粉末和氧化铈、氧化铕或氧化铽粉末溶解在硝酸溶液中形成混合溶液,混合溶液中稀土离子镧和稀土离子铈、铕或铽的摩尔比为95∶5~50∶50;
2)将上述混合溶液的pH值调节至2.5~4.5,搅拌下加入过量的NH4H2PO4溶液,生成胶状沉淀物;
3)将胶状物在氮气保护和回流条件下于微波炉中加热,时间20~60min,然后自然冷却,用离心分离和去离子水充分洗涤后收集并干燥。
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CN101693520B (zh) * | 2009-10-21 | 2012-07-25 | 济南大学 | 一种稀土元素掺杂的氧化铈纳米棒的工业化制备方法 |
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US5340556A (en) * | 1991-02-04 | 1994-08-23 | Rhone-Poulenc Chimie | Cerium/lanthanum/terbium mixed phosphates |
FR2817771A1 (fr) * | 2000-12-08 | 2002-06-14 | Rhodia Terres Rares | Dispersion colloidale de phosphate de terre rare et procede de preparation |
CN1361750A (zh) * | 1999-06-16 | 2002-07-31 | 罗狄亚化学公司 | 铈和/或镧的磷酸盐凝胶,其制备方法及其在抛光中的应用 |
CN1456714A (zh) * | 2003-05-22 | 2003-11-19 | 北京大学 | 制备磷酸稀土单晶纳米线的方法 |
EP1427673A1 (fr) * | 2001-09-12 | 2004-06-16 | Rhodia Electronics and Catalysis | Dispersion colloidale de particules d'un vanadate ou d'un phospho-vanadate d'une terre rare |
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US5340556A (en) * | 1991-02-04 | 1994-08-23 | Rhone-Poulenc Chimie | Cerium/lanthanum/terbium mixed phosphates |
US5562889A (en) * | 1991-02-04 | 1996-10-08 | Rhone-Poulenc Chimie | Cerium/lanthanum/terbium mixed phosphates |
CN1361750A (zh) * | 1999-06-16 | 2002-07-31 | 罗狄亚化学公司 | 铈和/或镧的磷酸盐凝胶,其制备方法及其在抛光中的应用 |
FR2817771A1 (fr) * | 2000-12-08 | 2002-06-14 | Rhodia Terres Rares | Dispersion colloidale de phosphate de terre rare et procede de preparation |
EP1427673A1 (fr) * | 2001-09-12 | 2004-06-16 | Rhodia Electronics and Catalysis | Dispersion colloidale de particules d'un vanadate ou d'un phospho-vanadate d'une terre rare |
CN1456714A (zh) * | 2003-05-22 | 2003-11-19 | 北京大学 | 制备磷酸稀土单晶纳米线的方法 |
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微波在纳米稀土发光材料制备中的应用 宋羽.化工新型材料,第34卷第3期 2006 * |
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