Method for preparing tin oxide nanocrystalline coated by organic ligand

A technology of tin oxide nanocrystals and organic ligands, applied in the direction of tin oxide, etc., can solve the problems of difficulty in controlling the size and shape of nanocrystals, high reaction temperature, and difficult dispersion of nanocrystals, and achieve short preparation cycle, mild reaction conditions, The effect of the method is simple and easy

Active Publication Date: 2010-03-24
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the shortcomings of high reaction temperature during traditional synthesis, difficulty in controlling the size and shape of nanocrystals, and difficulty in dispersing the synthesized nanocrystals in organic solvents

Method used

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  • Method for preparing tin oxide nanocrystalline coated by organic ligand
  • Method for preparing tin oxide nanocrystalline coated by organic ligand

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Preparation of SnO nanocrystals coated with spherical organic ligands:

[0022] Add 0.15mmol of tin source, 0.5g of myristic acid and 25ml of toluene to the polytetrafluoroethylene lining of a 30ml autoclave, then add 2ml of an aqueous solution containing 0.2ml of n-butylamine to the system, seal the autoclave, and put Heat in the furnace at 120°C for 1h (the pressure is kept at 1-10MPa), and after cooling, white nanocrystals are formed in the oil phase. Its particle size is about 2nm. Can be dispersed in non-polar organic solvents such as toluene or chloroform. The nanocrystal precipitate obtained by centrifuging the above oil phase was dissolved in 15 ml of pyridine, and heated to reflux at 60° C. for 6 hours to obtain pyridine-coated tin oxide nanocrystals.

Embodiment 2

[0023] Example 2: Preparation of tin oxide nanocrystals coated with branched organic ligands:

[0024] Add 0.05mmol of tin source, 1ml of oleic acid and 20ml of toluene to the PTFE lining of a 30ml autoclave, then add 5ml of an aqueous solution containing 0.5ml of tert-butylamine into the system, seal the autoclave and put it in a furnace to heat at 180°C 12h (the pressure is maintained at 1-10MPa), white nanocrystals are formed in the oil phase after cooling. The nanocrystals can be dispersed in non-polar organic solvents such as toluene or chloroform. The branch width is about 1.5nm.

Embodiment 3

[0025] Example 3: Preparation of tin oxide nanocrystals coated with branched organic ligands:

[0026] Add 0.02mmol tin source, 0.5g oleylamine and 10ml toluene to the polytetrafluoroethylene lining of a 30ml autoclave, then add 2ml of an aqueous solution containing 0.0012g urea to the system, seal the autoclave and put it into the furnace at 180 Heating at ℃ for 6 hours (the pressure is maintained at 1-10MPa), and white nanocrystals are formed in the oil phase after cooling. Its shape is branch-like. The nanocrystal precipitate obtained by centrifuging the above oil phase was dissolved in 10 ml of pyridine, and heated to reflux at 60° C. for 6 hours to obtain pyridine-coated tin oxide nanocrystals.

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Abstract

The invention provides a synthesis method of tin oxide nano-crystal which is wrapped by organic ligands. The method is that: tin source and organic wrapping agent are added into toluene; the mixture is heated, dissolved and added with water solution of alkaline matter, then sent into a reaction vessel at the temperature of 120-180 DEG C to react for 1-24 hours; the tine source is hydrolyzed; afternucleation and growing process, the tin oxide nano-crystal wrapped with organic ligands is prepared. The whole preparation method of the invention is characterized in that reaction condition is moderate, the operation is simple and the preparation period is short, thereby the preparation method can be easily put into mass production. In addition, the tin oxide nano-crystal with different sizes and shapes such as spherical shape and branch shape can be prepared by adjusting reaction time, temperature, alkaline amount, water amount and organic wrapping agent type; the size and shape of the synthesized tin oxide nano-crystal can also be controlled; the size distribution is narrow, and the nano-crystal can be dissolved into organic solvent with different heteropolarities through surface ligand exchange.

Description

technical field [0001] The invention belongs to organic ligand-coated tin oxide (SnO 2 ) method for preparing nanocrystals, specifically relating to a method for preparing tin oxide nanocrystals using a two-phase method combined with an autoclave. Background technique [0002] Tin dioxide is a wide-bandgap n-type semiconductor (Eg=3.5eV, 300K), which can be used as gas-sensitive materials, moisture-sensitive materials, pressure-sensitive materials and photosensitive materials. It has important applications in gas sensors, catalysts, lithium-ion secondary batteries, fuel cells, solar cells and field effect transistors. In the past two decades, with the development of nanoscience and technology, the synthesis of nano-tin oxide has gradually begun and shows broad application prospects (Penny, M.W.et.al., Charge storage in SnO 2 Nanoparticles: A method and mechanism for charge writing / erasing, Applied Physics Letters, 2007(91), 16). So far, tin oxide nanomaterials can be prep...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02
Inventor 林驭寒赵娜娜李海东毛骏范燕迪王大鹏姬相玲
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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