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A Stannic Oxide Microballoon with Controllable Crystallite Dimension and its Preparation Method and Application

A technology of tin dioxide and microcrystalline size, which is applied in tin oxide, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., and can solve the problems of small grains that are easy to agglomerate, unfavorable ion penetration, and unfavorable sunlight. Light harvesting and other issues can be achieved to promote nucleation and growth, the process route is simple, and the effect of wide application prospects

Active Publication Date: 2017-01-04
SHANGHAI UNIV OF ENG SCI
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  • Application Information

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Problems solved by technology

However, there are many problems in the practical application of small-sized grains: for example, small grains are very easy to agglomerate, which reduces its reactivity; the size of small grains is much smaller than the wavelength of visible light, and it is not easy to use it as a solar cell photoanode material. Conducive to the capture of sunlight; compared with (sub)micron-sized materials, small nano-sized grains are not easy to recycle; small particles are densely packed, which is not conducive to the penetration of ions, electrolyte solutions or other reaction systems
Peining Zhu et al. used crystalline tin chloride as the tin source and lithium salt as the pore-forming agent to synthesize mesoporous hierarchical SnO by the molten salt method. 2 Microspheres, when used in dye-sensitized solar cells, not only have a high surface area to adsorb dyes, but also have a submicron size to improve the light scattering ability of the battery. However, the size of the microspheres obtained by this high-temperature solid-state method is very uneven, and the microspheres can Can remain impurities (Chem.Commun.,2012,48,10865–10867)
Yu-Fen Wang et al. used crystalline stannous chloride as the tin source and ethylenediamine as the morphology modifier, and synthesized mesoporous hierarchical SnO by ultrasonic combined with solvothermal two-step. 2 Microspheres, but the size of the microspheres obtained by this method is large (about 2.2 microns), and the size of the microspheres is not uniform (J. Power Sources, 2015, 280, 476–482)
Guanglu Shang et al. used stannous sulfate as tin source to solvothermally synthesize the multi-level structure SnO 2 Microspheres, but the size distribution of microspheres is not uniform, and the diameter distribution is wide, ranging from 100 to 800nm. In addition, the crystallinity of nanocrystalline particles as the basic constituent units of microspheres is not ideal (J.Phys.Chem.C 2012 ,116,20140-20145)
[0005] The above studies have shown that the hierarchical structure of SnO 2 Microspheres have a wide range of application prospects, but there is currently no good way to synthesize SnO with uniform size distribution (monodisperse or quasi-monodisperse) 2 Microspheres, and the size control of nanocrystalline particles as the basic unit of microspheres are also rarely mentioned-in fact, this is a key part that affects the surface area and active sites of microspheres

Method used

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  • A Stannic Oxide Microballoon with Controllable Crystallite Dimension and its Preparation Method and Application
  • A Stannic Oxide Microballoon with Controllable Crystallite Dimension and its Preparation Method and Application
  • A Stannic Oxide Microballoon with Controllable Crystallite Dimension and its Preparation Method and Application

Examples

Experimental program
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Effect test

Embodiment 1

[0040] Measure 50 milliliters of n-propanol, add 1.5 milliliters of concentrated hydrochloric acid and 0.4513 gram of tin protochloride dihydrate successively under magnetic stirring condition, form transparent homogeneous solution; The filling rate of the reaction kettle is 60%, the reaction temperature is controlled at 200° C., and the reaction time is 12 hours; after the reaction is completed, the precipitate is taken out, washed repeatedly with pure water, and centrifuged.

[0041] figure 1 For the field emission scanning electron micrograph of the tin dioxide microspheres prepared in Example 1, it can be seen from the figure that the dispersion of the microspheres is good, the size distribution is uniform, and the diameter of a single microsphere is 200 to 300 nanometers; It can also be seen from the scanning electron microscope that the microspheres are formed by the aggregation of small grains, and the grain size of the microcrystals is about 10 nanometers.

Embodiment 2

[0043] Mix 2.5 milliliters of pure water and 47.5 milliliters of n-propanol, add 1.5 milliliters of concentrated hydrochloric acid and 0.4513 grams of stannous chloride dihydrate in sequence under magnetic stirring conditions to form a transparent homogeneous solution; transfer the above-mentioned transparent solution to the reaction kettle Carry out solvothermal reaction, the filling rate of the reactor is 60%, the reaction temperature is controlled at 200° C., and the reaction time is 12 hours; after the reaction is completed, the precipitate is taken out, repeatedly washed with pure water, and centrifuged.

[0044] figure 2 For the field emission scanning electron micrograph of the tin dioxide microspheres prepared in Example 2, it can be seen from the figure that the dispersion of the microspheres is good, the size distribution is uniform, and the diameter of a single microsphere is 200 to 300 nanometers; It can also be seen from the scanning electron microscope that the ...

Embodiment 3

[0046] Mix 5 milliliters of pure water and 45 milliliters of n-propanol, add 1.5 milliliters of concentrated hydrochloric acid and 0.4513 grams of stannous chloride dihydrate successively under the condition of magnetic stirring to form a transparent homogeneous solution; transfer the above-mentioned transparent solution to the reaction kettle Carry out solvothermal reaction, the filling rate of the reactor is 60%, the reaction temperature is controlled at 200° C., and the reaction time is 12 hours; after the reaction is completed, the precipitate is taken out, repeatedly washed with pure water, and centrifuged.

[0047] image 3 The field emission scanning electron microscope image of the tin dioxide microspheres prepared for Example 3 shows that the dispersion of the microspheres is good and the size is very uniform, and the diameter of a single microsphere is 250 nanometers.

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Abstract

This invention involves a kind of stannic oxide microballoon with controllable crystallite dimension and its preparation method and application. This stannic oxide microballoon is composed of stannic oxide microcrystal with fine crystallinity through self-assembly. The grain size of stannic oxide microcrystal is adjustable within range of 5-30nm. The diameter of stannic oxide microballoon is 200-400nm and its specific surface area >40m2 / g; During preparation, add concentrated hydrochloric acid and tin source into the mixed solution of normal propyl alcohol and water in order, forming the transparent homogeneous solution; Conduct solvothermal reaction; After the reaction ends, take out the sediment, wash and separate it. Being compared with the current technology, this invention has simple and easy process route, which does not need surface active agent. And the multilevel structure Sno2 microballoon with equally distributed dimension can be gotten through one-step method, which is composed of stannic oxide microcrystal through self-assembly. Also, the dimension of Sno2 microcrystal can be adjusted and controlled through adjusting the alcohol / water proportion in the reaction system. The microballoon has features of high specific area and submicron level dimension, which has wide application prospect in areas of solar cell, lithium ion battery and photocatalysis.

Description

technical field [0001] The invention belongs to the technical field of preparation of advanced inorganic nanometer materials, and relates to a tin dioxide microsphere with controllable crystallite size, a preparation method and application thereof. Background technique [0002] SnO 2 It is a wide-bandgap n-type semiconductor material with a bandgap of 3.6eV, good chemical stability, fast electron migration, and high visible light transmittance. It is used in new solar cells, lithium-ion batteries, gas sensors, and transparent conductive materials. And the field of photocatalysis has broad application prospects. Therefore, it is of great significance to synthesize tin dioxide nanomaterials with controllable size, shape and structure. [0003] SnO with a grain size of a few nanometers or tens of nanometers 2 Particles have high specific surface area and more active sites, so more physical and chemical properties can be endowed to them. However, there are many problems in th...

Claims

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Application Information

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IPC IPC(8): C01G19/02H01G9/20H01M10/0525B01J23/14B01J35/08B01J35/10
CPCH01M10/0525H01G9/2027C01G19/02B01J23/14C01P2006/40C01P2004/62C01P2006/12C01P2004/03C01P2004/04C01P2004/32C01P2002/72C01P2002/80B01J35/40B01J35/51B01J35/613B01J35/39Y02E10/542Y02E60/10
Inventor 芮一川尹瑞徐菁利张扬陈小丹
Owner SHANGHAI UNIV OF ENG SCI
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