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Synthesis method of monoclinic crystal phase rare-earth iso-oxy-sulfur superfine nanowire and wire-based superstructure

An ultra-fine nano, synthetic method technology, applied in chemical instruments and methods, single crystal growth, single crystal growth and other directions, can solve the problems of weak S affinity, reduced lattice symmetry, and difficulty, and achieve good luminescence. The effect of performance, good universality, efficient development and application

Inactive Publication Date: 2011-10-19
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reason may be that the ionic radii of O and S are different. Rare earth ions have a strong affinity for O, but a relatively weak affinity for S. It is easy to obtain Ln2 in water system or oxygen-rich environment. O3 or Ln2O2S, it is more difficult to get Ln2OS 2
Compared to Ln2O2S, the proportion of S atoms in Ln2OS2 increases, resulting in Its lattice symmetry is drastically reduced

Method used

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  • Synthesis method of monoclinic crystal phase rare-earth iso-oxy-sulfur superfine nanowire and wire-based superstructure
  • Synthesis method of monoclinic crystal phase rare-earth iso-oxy-sulfur superfine nanowire and wire-based superstructure
  • Synthesis method of monoclinic crystal phase rare-earth iso-oxy-sulfur superfine nanowire and wire-based superstructure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 0.20~6.0g Y(NO 3 ) 3 6H 2 O solid, 0.10-4.50 g thiourea solid, 2-10 mL oleic acid (Aldrich, 90%), 2-10 mL dodecylamine (Alfa Aesar, 98%), and 5-20 mL octadecene (Alfa Aesar , 90%), sealed the reactor and transferred it to an oven, and raised it from room temperature to 180 °C at a rate of 4 °C / min. After 24 h of reaction, the temperature was naturally cooled to room temperature. To obtain a light brown jelly, add n-heptane, heat slightly, then add ethanol to precipitate, and centrifuge to separate the solid. Then the initial product was washed with a mixed solvent of n-heptane / absolute ethanol (volume ratio: 2 / 1), and a precipitate was obtained after centrifugation. Washing was repeated 3-5 times to obtain a light yellow-green solid product, and finally the washed product was vacuum-dried at 60°C for 4 h.

[0034] The dried product was collected, and its composition and phase were tested by X-Ray powder diffractometer (XRD). The results showed that the obtained ...

Embodiment 2

[0036] Add 0.2-6.0 g Gd(NO 3 ) 3 6H 2 O solid, 0.10-4.50g thiourea solid, 2-10 mL oleic acid, 2-10 mL dodecylamine and 5-20 mL octadecene, seal the reaction kettle and transfer it to an oven at 4 ℃ / min The rate was increased from room temperature to 180 °C. After 24 h of reaction, the temperature was naturally cooled to room temperature, and a light brown jelly was obtained. Add n-heptane, heat slightly, then add ethanol, and centrifuge to separate the solid. Then, the obtained primary product was washed with a mixed solvent of n-heptane / absolute ethanol (volume ratio: 2 / 1), and a precipitate was obtained after centrifugation. Washing was repeated 3-5 times to obtain a light yellow-green solid product, and finally the washed product was vacuum-dried at 60°C for 4 h. .

[0037] The dried product was collected, and its composition and phase were tested by X-Ray powder diffractometer (XRD), which showed that the obtained product was pure monoclinic crystal phase structure Gd...

Embodiment 3

[0039] In a clean and dry reaction kettle (volume 50 mL) with polytetrafluoroethylene liner, add 0.2-6.0 g Dy(NO 3 ) 3 6H 2 O solid, 0.10-4.50g thiourea solid, 2-10 mL oleic acid, 2-10 mL dodecylamine and 5-20 mL octadecene, seal the reaction kettle and transfer it to an oven at 4 ℃ / min The rate was increased from room temperature to 200 °C, and after 24 h of reaction, the temperature was naturally cooled to room temperature. A light brown gum was obtained. Add n-heptane, heat slightly, then add ethanol, and centrifuge to separate the solid. Then, the obtained product was washed with a mixed solvent of n-heptane / absolute ethanol (volume ratio: 2 / 1), and a precipitate was obtained after centrifugation. The washing operation was repeated 3-5 times to obtain a light yellow-green solid product, and finally the washed product was vacuum-dried at 60 °C for 4 h.

[0040] The dried product was collected, and its composition and phase were tested by X-Ray powder diffractometer (XR...

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Abstract

The invention discloses a synthesis method of monoclinic crystal phase rare-earth iso-oxy-sulfur Ln2OS2 (Ln=Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er and Yb) superfine nanowire and nanowire-based superstructure, comprising the following steps of: heating rare-earth metal nitrate solid and thiourea solid to 180-200 DEG C for solid-liquid phase reaction in the mixed solvent consisting of fatty acid, fatty amine and octadecene, and separating out reaction products to prepare target products. The method adopts a solid-liquid phase chemical reaction route and replaces an organic metal compound with rare-earth nitrate solid, thereby controllably synthesizing a series of rare-earth iso-oxy-sulfur superfine nanowires and nano wire-based superstructures with high efficiency. The synthesis method has a simple and safe operation process and universality, and can implement large-scale preparation of the product.

Description

technical field [0001] The invention relates to a synthesis method of a rare earth isosulfur nanomaterial, in particular to a novel monoclinic phase rare earth isosulfur (Ln 2 OS 2 , Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Dy, Ho, Er, Yb) controllable synthesis of ultrafine nanowires and nanowire-based superstructures. Background technique [0002] Size and dimension are two important geometric structure parameters that affect the physical and chemical properties of nanomaterials. Among various nanostructures, 1D nanowires (cylindrical structures with a diameter less than 100 nanometers) have different electronic density of states than 0D, 2D and 3D nanostructures due to their radial height confinement and axial preferential growth. The unique physical and chemical properties different from other nanostructures have potential application prospects in the fields of electronics, catalysis, sensing and environmental degradation. [0003] In recent years, the synthesis of ultrath...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/46C30B29/62
Inventor 包建春韩敏郭培戴志晖许兰全袁丹
Owner NANJING NORMAL UNIVERSITY
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