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 difficult dispersion of nanocrystals, high reaction temperature, and difficulty in controlling the size and shape of nanocrystals. The method is simple and easy, and the reaction conditions are mild , The effect of short preparation cycle

Active Publication Date: 2008-07-02
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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Problems solved by technology

[0003] In order to solve the shortcomings of high reaction temperature during traditional synthesis, difficulty in contr

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  • Method for preparing tin oxide nanocrystalline coated by organic ligand

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Example Embodiment

[0021] Example 1: Preparation of spherical organic ligand-coated tin oxide nanocrystals:

[0022] Add 0.15mmol tin source, 0.5g tetradecanoic acid and 25ml toluene into the polytetrafluoroethylene lining of a 30ml autoclave, then add 2ml aqueous solution containing 0.2ml n-butylamine into the system, seal the autoclave and put it in The furnace was heated at 120°C for 1 hour (pressure maintained at 1-10MPa), and white nanocrystals were formed in the oil phase after cooling. Its particle size is about 2nm. It can be dispersed in non-polar organic solvents such as toluene or chloroform. The nanocrystalline precipitate obtained by centrifuging the 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.

Example Embodiment

[0023] Example 2: Preparation of tin oxide nanocrystals coated with branch-like organic ligands:

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

Example Embodiment

[0025] Example 3: Preparation of tin oxide nanocrystals coated with branch-like organic ligands:

[0026] Add 0.02mmol tin source, 0.5g oleylamine and 10ml toluene into the polytetrafluoroethylene lining of a 30ml autoclave, then add 2ml of an aqueous solution containing 0.0012g of urea into the system, seal the autoclave and put it in the furnace at 180 Heating at ℃ for 6h (pressure maintained at 1-10MPa), after cooling, white nanocrystals are formed in the oil phase. Its shape is branch-like. The nanocrystalline precipitate obtained by centrifugal separation of the 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; after nucleation 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 prepa...

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Application Information

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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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