稀土发光纳米片材料的制备及性能研究
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摘要
稀土元素由于具有独特的4f能级结构,因而在受到紫外光激发的时表现出优良的光学性能,作为一种有效的发光中心,稀土离子在无机和有机发光材料中已有广泛应用。稀土纳米片材料由于其独特的结构(二维方向片状结构,一维方向纳米尺寸)以及特有的发光性质而引起广泛关注。
本文包含以下几个方面：
1.通过水热合成方法首先制备了Y2(OH)5NO3·nH2O层状材料,并对水热过程中溶液pH对形貌的影响进行了研究。进而制备出稀土Eu3+, Tb3+掺杂的稀土层状发光材料。采用较为普通的烷基磺酸盐和烷基羧酸盐为原料进行离子交换,获得了层间距离扩大的层状化合物。超声剥离、离心后得到了稀土掺杂的纳米片发光材料,由于该纳米片材料表面带有一定的正电荷,因此通过LBL自组装的方法,制备了PSS/纳米片复合材料。
2.由于所制备的纳米片发光材料表面存在一定量的与稀土离子的配位水分子,而配位水分子中高频羟基振动会带来一定的能量损失。因此在纳米片的制备过程引入了β—二酮配体HTTA,其独特的配位能力使得稀土离子周围配位水分子被取代,有效减少配位水分子中高频羟基振动所带来的能量损失,并且通过有机配体天线效应敏化其发光。在该有机—无机复合纳米片发光材料中,其荧光性能得到了显著的增强,单色性效果明显提高,并且其激发光谱从原材料的Eu-O电荷跃迁转移到有机配体的π-π*。经TTA修饰后的纳米片用于胆红素的检测具有很高的灵敏度。
3.采用烷基磺酸盐和多种烷基羧酸盐为原料直接合成了不同阴离子插层的稀土层状材料Y1-xEux(OH)5X-nH2O(X=十二烷基磺酸钠、苯甲酸钠、正辛酸钠、对甲苯磺酸钠、丙酸钠等),经剥离后得到表面带正电荷的纳米荧光材料,并对其结构和荧光性能等进行了分析。
4.首次报道了单层氧化钇纳米片的制备。以LnOBr层状化合物为原料,在微波条件下对其进行离子交换,得到了苯甲酸钠插层的材料。在正丁醇中通过超声剥离,制备了表面带正电荷的稀土氧化物纳米片发光材料。与稀土氢氧化物纳米片相比,由于排除羟基对荧光的猝灭作用,稀土氧化物基纳米片发光材料荧光强度大大增强。采用HTTA有机配体修饰后,由于有机配体天线效应,稀土氧化物纳米片荧光性能进一步增强。该HTTA-氧化钇纳米片复合发光材料可以作为大肠杆菌荧光显像剂。
5.以上述合成的稀土氢氧化物及氧化物纳米片表面带正电荷特性,利用电泳沉积在ITO与FTO导电玻璃基板上制备了透明均匀的发光薄膜。
6.以钠基蒙脱土为原料,在乙醇中剥离制备了表面带负电荷的蒙脱土纳米片材料。与稀土铕离子复合,得到具有良好荧光特性的复合材料。采取碳热还原的方法,制备出了二价铕与蒙脱土纳米片发蓝光的复合材料。此外,在水热条件下分别制备了荧光增强的稀土配合物Eu(TTA)3.Tb(TTA)3与蒙脱土纳米片复合发光材料。
The rare earth elements has a unique4f energy structure, being excited by UV irradiation the rare earth materials exhibit excellent optical properties. The rare earth have been widely used because of the Luninescence properity. The nanosheets of rare earth have attracted widespread concern due to its unique structure:two-dimensional sheet structure, and the thickness of the nanosheets is nearly about lnm. The main content are as follows:
1. The layered compound was synthesized by hydrothermal reaction, and then, the Eu3+/Tb3+-doped rare earth layered material also prepaired. The influence of pH on the morphology of the layered compound was studied in this paper. After ion exchange reaction with organic anion under the microwave condition, the layer space of the compound increases enlarged. Furthermore, stable nanosheet sol was obtained after exfoliation under ultrasonic condition. The morphology of nanosheets were determined by TEM, the size of the nanosheets ranged from severial hundreds nanometers to micro, the thickness of the nanosheets about lnm. The (nanosheets/PSS)n composites were prepared by LBL self-assembly method due to it's positively surface charge.
2. The luminescent intensity of5D0-7F2(electric dipole transition) greatly increased TTA modified hydroxide nanosheets was prepaired, the increase of fluorescent intensity could be ascribed to two reasons:One was that H2O coordinated with Eu3+in nanosheets was substituted by organic ligand of TTA, which reduced the non-radiative transition generated from thermal vibration and enhanced the emission. The other reason was Antenna effect of the ligands. Furthermore, the nanosheets/TTA hybrids exibitted good properties in detecting Bilirubin molecules.
3. We report a new family of lanthanide-based inorganic-organic hybrid frameworks Yi.9Euo.i(OH)5[A]·2H20(A=Alkyl Carboxylate and Alkyl sulfonate) synthesized by homogeneous precipitation, and the RE in the layered compound was9-coordinated. The single layered nanosheets with positive charged nanosheets were obtained in n-butanol after the supersonic treatment, the structure and fluorescent properties of Yi.9Euo.i(OH)5[A]·2H20and nanosheets also studied in this work.
4. The yttrium oxide nanosheets with monolayer was prepared for the first time. Y(1-x)RExOBr as raw materials, after ion exchange under microwave condition we prepaired layered material Y(1-0.05)RE0.05OC6H5COO. Translucent colloidal{Y(1-0.05)RE0.050+}n nanosheets solutions were yielded after repeated ultrasonic treatments of the mixtures within30minutes, compaired with the hydroxide nanosheets there is no coordinated water molecules in{Y(1-0.05)RE0.05O+}n nanosheets surface, there is no non-radiative transition generated from thermal vibration, therefore the luminescent properity of{Y(1-0.05)REo.o5O+}n nanosheets enhanced significantly. Furthermore, the {Y(1-0.05)REo.o5O+}n/TTA hybrids exibitted good properties in Dyeing E. coli cells.
5. As-synthesized{Y(1-0.05)RE0.050+}n and{Yi.9REo.i(OH)5+}n rare earth nanosheets with positive charge characteristics, the{Y(1-0.05)RE0.05O+}n and {Yi.9RE0.1(OH)5+}n transparent thin film were prepaired in ITO and FTO glass substrate by Electrophoretic deposition method.
6. MMT nanosheets with negatively charged were prepaired by supersonic treatment in in ethanol. And the complexes Eu (TTA)3-MMT, Tb(TTA)3-MMT were prepaired by hydrothermal treatment, the fluorescence property the hybrids materials enhanced greatly.
本文包含以下几个方面：
1.通过水热合成方法首先制备了Y2(OH)5NO3·nH2O层状材料,并对水热过程中溶液pH对形貌的影响进行了研究。进而制备出稀土Eu3+, Tb3+掺杂的稀土层状发光材料。采用较为普通的烷基磺酸盐和烷基羧酸盐为原料进行离子交换,获得了层间距离扩大的层状化合物。超声剥离、离心后得到了稀土掺杂的纳米片发光材料,由于该纳米片材料表面带有一定的正电荷,因此通过LBL自组装的方法,制备了PSS/纳米片复合材料。
2.由于所制备的纳米片发光材料表面存在一定量的与稀土离子的配位水分子,而配位水分子中高频羟基振动会带来一定的能量损失。因此在纳米片的制备过程引入了β—二酮配体HTTA,其独特的配位能力使得稀土离子周围配位水分子被取代,有效减少配位水分子中高频羟基振动所带来的能量损失,并且通过有机配体天线效应敏化其发光。在该有机—无机复合纳米片发光材料中,其荧光性能得到了显著的增强,单色性效果明显提高,并且其激发光谱从原材料的Eu-O电荷跃迁转移到有机配体的π-π*。经TTA修饰后的纳米片用于胆红素的检测具有很高的灵敏度。
3.采用烷基磺酸盐和多种烷基羧酸盐为原料直接合成了不同阴离子插层的稀土层状材料Y1-xEux(OH)5X-nH2O(X=十二烷基磺酸钠、苯甲酸钠、正辛酸钠、对甲苯磺酸钠、丙酸钠等),经剥离后得到表面带正电荷的纳米荧光材料,并对其结构和荧光性能等进行了分析。
4.首次报道了单层氧化钇纳米片的制备。以LnOBr层状化合物为原料,在微波条件下对其进行离子交换,得到了苯甲酸钠插层的材料。在正丁醇中通过超声剥离,制备了表面带正电荷的稀土氧化物纳米片发光材料。与稀土氢氧化物纳米片相比,由于排除羟基对荧光的猝灭作用,稀土氧化物基纳米片发光材料荧光强度大大增强。采用HTTA有机配体修饰后,由于有机配体天线效应,稀土氧化物纳米片荧光性能进一步增强。该HTTA-氧化钇纳米片复合发光材料可以作为大肠杆菌荧光显像剂。
5.以上述合成的稀土氢氧化物及氧化物纳米片表面带正电荷特性,利用电泳沉积在ITO与FTO导电玻璃基板上制备了透明均匀的发光薄膜。
6.以钠基蒙脱土为原料,在乙醇中剥离制备了表面带负电荷的蒙脱土纳米片材料。与稀土铕离子复合,得到具有良好荧光特性的复合材料。采取碳热还原的方法,制备出了二价铕与蒙脱土纳米片发蓝光的复合材料。此外,在水热条件下分别制备了荧光增强的稀土配合物Eu(TTA)3.Tb(TTA)3与蒙脱土纳米片复合发光材料。
The rare earth elements has a unique4f energy structure, being excited by UV irradiation the rare earth materials exhibit excellent optical properties. The rare earth have been widely used because of the Luninescence properity. The nanosheets of rare earth have attracted widespread concern due to its unique structure:two-dimensional sheet structure, and the thickness of the nanosheets is nearly about lnm. The main content are as follows:
1. The layered compound was synthesized by hydrothermal reaction, and then, the Eu3+/Tb3+-doped rare earth layered material also prepaired. The influence of pH on the morphology of the layered compound was studied in this paper. After ion exchange reaction with organic anion under the microwave condition, the layer space of the compound increases enlarged. Furthermore, stable nanosheet sol was obtained after exfoliation under ultrasonic condition. The morphology of nanosheets were determined by TEM, the size of the nanosheets ranged from severial hundreds nanometers to micro, the thickness of the nanosheets about lnm. The (nanosheets/PSS)n composites were prepared by LBL self-assembly method due to it's positively surface charge.
2. The luminescent intensity of5D0-7F2(electric dipole transition) greatly increased TTA modified hydroxide nanosheets was prepaired, the increase of fluorescent intensity could be ascribed to two reasons:One was that H2O coordinated with Eu3+in nanosheets was substituted by organic ligand of TTA, which reduced the non-radiative transition generated from thermal vibration and enhanced the emission. The other reason was Antenna effect of the ligands. Furthermore, the nanosheets/TTA hybrids exibitted good properties in detecting Bilirubin molecules.
3. We report a new family of lanthanide-based inorganic-organic hybrid frameworks Yi.9Euo.i(OH)5[A]·2H20(A=Alkyl Carboxylate and Alkyl sulfonate) synthesized by homogeneous precipitation, and the RE in the layered compound was9-coordinated. The single layered nanosheets with positive charged nanosheets were obtained in n-butanol after the supersonic treatment, the structure and fluorescent properties of Yi.9Euo.i(OH)5[A]·2H20and nanosheets also studied in this work.
4. The yttrium oxide nanosheets with monolayer was prepared for the first time. Y(1-x)RExOBr as raw materials, after ion exchange under microwave condition we prepaired layered material Y(1-0.05)RE0.05OC6H5COO. Translucent colloidal{Y(1-0.05)RE0.050+}n nanosheets solutions were yielded after repeated ultrasonic treatments of the mixtures within30minutes, compaired with the hydroxide nanosheets there is no coordinated water molecules in{Y(1-0.05)RE0.05O+}n nanosheets surface, there is no non-radiative transition generated from thermal vibration, therefore the luminescent properity of{Y(1-0.05)REo.o5O+}n nanosheets enhanced significantly. Furthermore, the {Y(1-0.05)REo.o5O+}n/TTA hybrids exibitted good properties in Dyeing E. coli cells.
5. As-synthesized{Y(1-0.05)RE0.050+}n and{Yi.9REo.i(OH)5+}n rare earth nanosheets with positive charge characteristics, the{Y(1-0.05)RE0.05O+}n and {Yi.9RE0.1(OH)5+}n transparent thin film were prepaired in ITO and FTO glass substrate by Electrophoretic deposition method.
6. MMT nanosheets with negatively charged were prepaired by supersonic treatment in in ethanol. And the complexes Eu (TTA)3-MMT, Tb(TTA)3-MMT were prepaired by hydrothermal treatment, the fluorescence property the hybrids materials enhanced greatly.
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