CN103305222B - KSc2F7:Yb,Er 上转换荧光纳米棒的制法和用途 - Google Patents
KSc2F7:Yb,Er 上转换荧光纳米棒的制法和用途 Download PDFInfo
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Abstract
一种KSc2F7:Yb,Er上转换纳米棒,它是由ScCl3和NH4F以及KOH共热分解反应、油酸做表面活性剂、十八碳烯做高沸点有机溶剂、Yb3+/Er3+共掺杂的、可溶于非极性有机溶剂的、能发射强烈红色上转换荧光的纳米棒。本发明KSc2F7:Yb,Er的环己烷溶液经上转换荧光检测,分别发射出蓝色、绿色和红色三种不同的荧光。但红色荧光的强度远远高于其它两个颜色,所以最终在980nm光源激发下,显示强烈的红色荧光,其可以应用于制备荧光感应材料。本发明公开了其制法。
Description
技术领域
本发明涉及KSc2F7:Yb,Er纳米棒及其制法和强烈红色上转换荧光的性质。
背景技术
稀土离子拥有非常丰富的光谱特性,它们在颜色显示,发光,医药以及生物标记,太阳能电池和固态激光方面都发挥着非常重要的作用(参见:(a)Y.Liu,S.Zhou,D.Tu,Z.Chen,M.Huang,H.Zhu,E.Ma and X.Chen,Journal of the American Chemical Society 2012,134,15083-15090;(b)T.Maldiney,C.Richard,J.Seguin,N.Wattier,M.Bessodes and D.Scherman,ACS Nano 2011,5,854-862;(c)G.Tian,Z.Gu,L. Zhou,W.Yin,X.Liu,L. Yan,S.Jin,W.Ren,G.Xing,S.Li and Y.Zhao,Advanced Materials2012,24,1226-1231;(d)F.Zhang,R.Che,X.Li,C.Yao,J.Yang,D.Shen,P.Hu,W.Li and D.Zhao,Nano Letters 2012,12,2852-2858;(e)G.Y.Chen,H.L. Qiu,R.W.Fan,S.W.Hao,S.Tan,C.H.Yang and G.Han,Journal of Materials Chemistry 2012,22,20190-20196.)。与一般的荧光材料有机荧光染料和量子点相比,镧系掺杂的材料展示了特殊的光学特性,比如窄的发射区,长的荧光寿命和高的光化学稳定性。更为重要的是,镧系掺杂的纳米材料能把近红外长波长激发光转变成短波长的可见发射光。它们拥有深的渗透深度和低的背景荧光,可以作为很好的生物标记材料。这种材料具有反斯托克斯发射特性,被称为上转换材料。目前,它们已经广泛应用于高分辨三维生物成像,光动力治疗,光催化等等(参见:(a)L.Cheng,K.Yang,Y.Li,J.Chen,C.Wang,M.Shao,S.-T.Lee and Z.Liu,Angewandte Chemie International Edition2011,50,7385-7390;b)C.Li and J.Lin,Journal of Materials Chemistry2010,20,6831-6847;c)A.D.Ostrowski,E.M.Chan,D.J.Gargas,E.M.Katz,G.Han,P.J.Schuck,D.J.Milliron and B.E.Cohen,ACS Nano2012,6,2686-2692;d)H.-T.Wong,M.-K.Tsang,C.-F.Chan,K.-L.Wong,B.Fei and J.Hao,Nanoscale2013,5,3465-3473.)。
在各种各样的上转换纳米材料中,氟化物纳米晶NaYF4,NaGdF4,LiYF4,KMnF3,CaF2和BaYF5拥有低的声子能和合适的较大波长范围的光学透明度,已经引起了光学工作者的极大的兴趣。(参见:(a)M.Haase and H.Angewandte Chem ie International Edition 2011,50,5808-5829;(b)F.Wang and X.Liu,Journal of the American Chemical Society2008,130,5642-5643;(c)F.Wang,R.Deng,J.Wang,Q.Wang,Y.Han,H.Zhu,X.Chen and X.Liu,Nat Mater2011,10,968-973;(d)Y.Liu,D.Tu,H.Zhu,R.Li,W.Luo and X.Chen,Advanced Materials2010,22,3266-3271;(e)G.Chen,T.Y.Ohulchanskyy,A.Kachynski,H.and P.N.Prasad,ACS Nano2011,5,4981-4986;(f)J.Wang,F.Wang,C.Wang,Z.Liu and X.Liu,Angewandte Chemie International Edition2011,50,10369-10372;(g)Wang,Q.Peng and Y.Li,Journal of the American ChemicalSociety2009,131,14200-14201;(h)F.Vetrone,V.Mahalingam and J.A.Capobianco,Chemistry of Materials2009,21,1847-1851.)在上述材料中,六方相的NaYF4纳米材料是迄今为止最有效的上转换基质材料。但是,它仪仪局限于有限的上转换发射波长,比如在单纯的Yb/Er掺杂中只以绿色发光为主。因此,一个紧迫而富有挑战的课题是寻找新的有其他上转换发射波长的纳米材料,以满足各种各样的发光需要。
Sc元素不但在元素周期表IIIB的最上端,而且处于过渡金属元素的起点。它独特的电子结构可能产生不同于Y/Ln的荧光材料。最近,Huang课题组合成了NaxScF3+x上转换纳米粒子,通过调节油酸/十八碳烯的比例,可以得到两种不同晶体结构的上转换材料(Na3ScF6和NaScF4),而且能发射红色上转换荧光(参见:X.Teng,Y.Zhu,W.Wei,S.Wang,J.Huang,R.Naccache,W.Hu,A.I.Y.Tok,Y.Han,Q.Zhang,Q.Fan,W.Huang,J.A.Capobianco and L.Huang,Journal of the American Chemical Society2012,134,8340-8343.)遗憾的是,除了这个工作,拥有不同的化学组分和形态的基于Sc的纳米材料的合成和光学特性一直没人报道。
而且,基于Y/Ln的纳米材料的研究大多数以纳米球为主,纳米棒很少报道。一个原因是Y/Ln纳米材料的结构对合成条件不如Sc元素敏感;另一个原因是,要想得到纳米棒,经常需要苛刻的合成条件或者稀土元素的高水平掺杂。但是,我们发现,通过简单的调节NH4F的量或者是反应温度,可以很容易地合成未见报道的新材料KSc2F7:Yb,Er纳米棒,且该材料表现出强烈的红色上转换荧光。
发明内容
本发明的目的是提供一种KSc2F7:Yb,Er上转换纳米棒的制备方法以及该法制备的KSc2F7:Yb,Er上转换纳米棒。
本发明的技术方案如下:
一种制备KSc2F7:Yb,Er上转换纳米棒的方法,它是以1mmol RECl3(Sc∶Yb∶Er=78∶20∶2)为反应单体,加入15mL油酸和17.5mL十八碳烯,搅拌均匀后,通氮气保护,保持 溶液中处于氮气氛围下,加热到160℃,反应30min,冷却到室温,分别加入1.6,2.8和4.0倍于稀土的物质的量的NH4F和1倍于稀土的物质的量的KOH的10mL的甲醇溶液,搅拌30min。蒸发掉甲醇,氮气保护下分别加热到270-290℃,反应1h,反应结束后,冷却到室温,离心(9500转,10min),依次用10mL水和10mL乙醇洗涤3次,得到白色沉淀,60℃下真空干燥,最终为固体粉末状的KSc2F7:Yb,Er纳米棒。
一种上述制备方法制备的KSc2F7:Yb,Er上转换纳米棒,它能均匀分散在环己烷、甲苯或氯仿中,放置一个月不会沉淀。
本发明的KSc2F7:Yb,Er上转换纳米棒粉末经红外光谱测定,结果表明外面包了一层作为表面活性剂的油酸,它可以限制粒子增长和团聚,并且使纳米棒很好地分散在非极性溶剂中。
本发明的固体粉末经X-射线衍射分析,结果表明在NH4F的物质的量是稀土物质的量的1.6倍时,该纳米材料是纯的正交晶系的KSc2F7纳米晶(JCPDS卡片77-1321),随着NH4F量的增加(加入4.0倍于稀土的物质的量的NH4F时),材料转变成掺杂有单斜晶系的KScF4相(JCPDS卡片48-0677)的KSc2F7纳米棒。
本发明的固体粉末分散在环己烷溶液中,经透射电镜分析,结果表明在NH4F为稀土含量的1.6倍时得到长的纳米棒,随着NH4F量的增加(4.0倍于稀土的物质的量),形态由纯的纳米棒转变成了掺杂有纳米粒子的纳米棒。
本发明的固体粉末分散在环己烷溶液中,经透射电镜分析,结果表明在290℃制得的纳米棒的平均长度是350nm,直径是30nm,可以很好地分散在非极性有机溶剂中。随着温度的降低,纳米棒在逐渐减小,由290℃时的长纳米棒转变成了270℃时长度为30nm,直径为10nm的小纳米棒。
本发明的固体粉末的环己烷溶液经上转换荧光光谱仪检测,在980nm光源激发下,结果表明能发出蓝色,绿色和红色荧光,但红色荧光的强度远远高于其它两个颜色,所以最终显示强烈的红色荧光。
附图说明
图1是本发明的固体粉末的傅里叶变换红外光谱图。
图2为本发明的固体粉末在不同NH4F条件下的X-射线衍射图(其中斜体数字是KSCF4的晶面,星号是不知名的杂质峰,图中顶线上的竖线是KSc2F7的标准卡片图(JCPDS77-1321),图中底线上的竖线是KSCF4的标准卡片图(JCPDS48-0677))。
图3为本发明中在不同量的NH4F条件下得到的材料的透射电镜图。(A)4.0mmol; (B)2.8mmol;(C)1.6mmol。
图4为本发明中在不同温度下得到的材料的透射电镜图。(A)270℃;(B)280℃;(C)290℃。
图5为本发明的固体粉末在980nm光源激发下在环己烷溶液中的上转换荧光光谱图。
具体实施方式
实施例1.纯的KSc2F7:Yb,Er纳米棒的制备
纳米棒的制备方法是在原有文献(参见:F.Wang,Y.Han,C.S.Lim,Y.Lu,J.Wang,J.Xu,H.Chen,C.Zhang,M.Hong and X.Liu,Nature2010,463,1061-1065)的基础上改变反应单体合成制备的。把1mmol RECl3(0.78mmol ScCl3.6H2O,0.2mmol YbCl3.6H2O,0.02mmol ErCl3.6H2O)加入到一个装有15ml油酸和17.5ml十八碳烯的圆底烧瓶中,溶液加热到160℃,搅拌反应30min,冷却到室温。包含有1.6mmol NH4F和1.0mmol KOH的10mL甲醇溶液加入到溶液中,搅拌30min。蒸发掉甲醇,溶液在氮气保护下加热到290℃,反应1h,冷却到室温,加入乙醇沉淀,用10mL水和10mL乙醇洗3次,真空干燥,得到KSc2F7:Yb,Er纳米棒。图1提供了制得的样品的红外光谱图。图5提供了制得的的样品的上转换荧光光谱图。
实施例2.掺杂有KScF4:Yb,Er纳米粒子的KSc2F7:Yb,Er纳米棒的制备
按实施例1的步骤制备掺杂有KScF4:Yb,Er纳米粒子的KSc2F7:Yb,Er纳米棒的制备,但NH4F的物质的量分别为2.8和4mmol,其他步骤相同。图2和图3分别提供了在290℃条件下,NH4F的量分别是稀土含量的4,2.8和1.6倍时的XRD图和TEM图。
实施例3.纯的KSc2F7:Yb,Er纳米棒的制备
按实施例1的步骤制备KSc2F7:Yb,Er纳米棒,但温度变为270℃,其他步骤相同。
实施例4.纯的KSc2F7:Yb,Er纳米棒的制备
按实施例1的步骤制备KSc2F7:Yb,Er纳米棒,但温度变为280℃,其他步骤相同。图4提供了在NH4F的量是稀土含量的1.6倍,温度分别是270,280和290℃时的TEM图。
Claims (4)
1.一种制备KSc2F7:Yb,Er上转换纳米棒的方法,其特征是它包括下列步骤:它是以1mmol RECl3为反应单体,所述的RE为物质的量之比Sc:Yb:Er=78:20:2的三元素混合物,加入15mL油酸和17.5mL十八碳烯,搅拌均匀后,通氮气保护,保持溶液中处于氮气氛围下,加热到160℃,反应30min,冷却到室温,分别加入1.6、2.8或4.0倍于稀土物质的量的NH4F和1倍于稀土物质的量的KOH的10mL甲醇溶液,搅拌30min,蒸发掉甲醇,氮气保护下加热到270-290℃,反应1h,反应结束后,离心,依次用水和乙醇洗涤,得到白色沉淀,真空干燥,最终为固体粉末状的KSc2F7:Yb,Er纳米棒。
2.根据权利要求1所述的制备KSc2F7:Yb,Er上转换纳米棒的方法,其特征是:当NH4F的物质的量降低至稀土物质的量的1.6倍时,形态由掺杂有KScF4纳米粒子的KSc2F7:Yb,Er上转换纳米棒逐渐变成均匀的纯KSc2F7:Yb,Er上转换纳米棒,且物质组分由加入4倍于稀土物质的量的NH4F时的产物:掺杂有KScF4的KSc2F7,转变为加入1.6倍于稀土物质的量的NH4F时的产物:纯的KSc2F7相;随着温度的增加,纳米棒长度逐渐变大,从270℃长度为30nm,直径为10nm,变化为290℃时长度为350nm,直径为30nm的长纳米棒。
3.一种权利要求1所述的制备方法制备的KSc2F7:Yb,Er上转换纳米棒。
4.权利要求3所述的KSc2F7:Yb,Er上转换纳米棒在制备红色上转换荧光材料中的应用。
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