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A kind of method for preparing tin oxide nano microspheres by supercritical method
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A nano-microsphere, supercritical technology, applied in tin oxide, nanotechnology, nanotechnology and other directions, can solve the problems of high cost and gas phase method
Active Publication Date: 2017-03-22
SHANGHAI NAT ENG RES CENT FORNANOTECH
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Problems solved by technology
Gas-phase methods require expensive equipment and thus higher costs
Moreover, the synthesized nanocrystals with controllable morphology and structure, based on the change of morphology and structure, can improve the performance of nanomaterials in many application fields, which is also a basic challenge in the field of nanoscience and technology.
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Embodiment 1
[0018] (1) Configure tin tetrachloride SnCl with a concentration of 0.017 mol / L 4 Solution, and add cetyltrimethylammonium bromide (surfactant mass fraction is 6%);
[0019] (2) Configure a certain concentration of potassium hydroxide solution, wherein the molar ratio of hydroxide: tin ion is 4:1;
[0020] (3) During the stirring process, add the potassium hydroxide solution into the mixed solution of tin tetrachloride and cetyltrimethylammonium bromide, and keep stirring for 30 min;
[0021] (4) Put the above solution into a supercritical reactor-basket for reaction, control a certain pressure (15MPa) and temperature (110°C), and keep the pressure for a certain period of time (8 h);
[0022] (5) Open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure to obtain the precursor powder, which is calcined at 600 ° C to obtain the 2 Nanocrystalline self-assembled SnO 2 nanospheres.
[0023] figure 1 It is the scanning electron microg...
Embodiment 2
[0025] (1) Configure stannous chloride SnCl with a concentration of 0.008 mol / L 2 2H 2 O solution, and add cetyltrimethylammonium bromide (surfactant mass fraction is 6%);
[0026] (2) Configure a certain concentration of sodium hydroxide solution, wherein the molar ratio of hydroxide: tin ion is 4:1;
[0027] (3) During the stirring process, add the sodium hydroxide solution into the mixed solution of stannous chloride and cetyltrimethylammonium bromide, and keep stirring for 30 min;
[0028] (4) Put the above solution into a supercritical reactor-basket for reaction, control a certain pressure (19MPa) and temperature (150°C), and keep the pressure for a certain period of time (6 h);
[0029] (5) Open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure to obtain the precursor powder, which is calcined at a temperature of 550 ° C to obtain the tin oxide SnO 2 Nanocrystalline self-assembled SnO 2 nanospheres.
[0030] image 3 I...
Embodiment 3
[0032] (1) Configure stannous chloride SnCl with a concentration of 0.02 mol / L 2 2H 2 O solution, and add sodium dodecylbenzenesulfonate SDBS (surfactant mass fraction is 6%);
[0033] (2) Configure a certain concentration of sodium hydroxide solution, wherein the molar ratio of hydroxide: tin ion is 4:1;
[0034] (3) During the stirring process, add the sodium hydroxide solution into the mixed solution of stannous chloride and sodium dodecylbenzenesulfonate SDBS, and keep stirring for 30 min;
[0035] (4) Put the above solution into a supercritical reactor-basket for reaction, control a certain pressure (22MPa) and temperature (125°C), and keep the pressure for a certain period of time (3 h);
[0036] (5) Open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure to obtain the precursor powder, which is calcined at 400 ° C to obtain the tin oxide SnO 2 Nanocrystalline self-assembled SnO 2 nanospheres.
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Abstract
The invention provides a method for preparing stannic oxide (SnO<2>) nanometer crystal self-assembly nanometer microspheres through a supercritical method. The method comprises the steps of firstly, preparing a stannic solution with the concentration being 0.008-0.02 mol / L, and adding surfactant; secondly, preparing an alkali solution with a certain concentration, wherein the ratio of the amount of hydroxy substances to the amount of stannic ionic substances is 4:1; in the stirring process, adding the alkali solution to a mixed solution of a stannic source and the surfactant; placing the solution into a supercritical reactor, namely a basket, for reaction, controlling the pressure and the temperature, opening a pressure relieving opening, lowering the pressure in a supercritical reaction kettle to the normal pressure, obtaining precursor powder, conducting calcination at the temperature of 400-600 DEG C, and obtaining the SnO<2> nanometer microspheres obtained through self-assembly of stannic oxide (SnO<2>) nanometer crystals. The SnO<2> nanometer microspheres prepared through the method are high in yield, the preparation method is simple, no toxic organic solvent is used in the process, no pollution is caused to the environment, the prepared SnO<2> material is large in specific surface area, and the stannic oxide nanometer microspheres can be widely applied to the fields such as sensing, catalysis and energy storage.
Description
technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method for preparing tin oxide nano-microspheres by a supercritical method. Background technique [0002] Semiconductor metal oxide nanomaterials are widely used in sensing, catalysis, optoelectronics, energy storage and other fields. Among them, tin dioxide SnO 2 It is an important n-type semiconductor transition metal oxide material, which has a wide band gap, high gas sensitivity and good optical properties, so it has attracted the attention of scientists and can be widely used in lithium-ion Batteries, supercapacitors, sensors and catalysts. [0003] Currently, the preparation of tin dioxide SnO 2 The main methods are: hydrothermal method, co-precipitation method, vapor deposition method and so on. The gas-phase method requires expensive equipment and thus is expensive. Moreover, the synthesized nanocrystals with controllable mo...
Claims
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