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F/Mn co-doped SnO2 nanopowder and preparation method thereof

A nano-powder and co-doping technology, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., to achieve the effect of uniform particle size, easy dispersion, and simple and easy process

Active Publication Date: 2016-12-14
SHENZHEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The characteristic of hydrothermal reaction is that it reacts in a closed container, and the crystal growth process cannot be seen during the reaction process. The nanoparticles prepared by this method have relatively high purity, good crystal form, uniform particle size distribution, good dispersibility, and no High-temperature calcination is required, which can reduce the agglomeration of particles during the calcination process. The reaction temperature of this method does not need to be very high, so it is an ideal method for preparing nanomaterials. However, there is no relevant preparation of F / Mn by hydrothermal method. Co-doped SnO 2 Related reports on nanopowder

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  • F/Mn co-doped SnO2 nanopowder and preparation method thereof
  • F/Mn co-doped SnO2 nanopowder and preparation method thereof
  • F/Mn co-doped SnO2 nanopowder and preparation method thereof

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Effect test

Embodiment 1

[0045] Preparation of F / Mn Co-doped SnO Using Hydrothermal Method 2 Nano powder, the specific steps are as follows: First, measure 50 ml of deionized water in a beaker, add citric acid to adjust the pH value to 1-2, and at the same time stir and heat to 50°C with a magnetic stirrer and keep it at a constant temperature; then add an appropriate amount of SnCl 4 ·5H 2 O to dissolve; and then different doping amount of MnSO 4 ·H 2 O and NH 4 F was added to the above solution. After continuing to stir for 10-30 min, gradually add the precipitating agent (ammonia, sodium hydroxide or potassium hydroxide) into the above solution and continue stirring for 10-30 min to adjust the pH value to 5-11, then add the dispersant (the addition of the dispersant Amount between 1% and 5%, according to SnCl 4 ·5H 2 O mass to calculate), the resulting mixed solution was transferred to a hydrothermal tank for hydrothermal reaction at different temperatures; then the hydrothermal reaction pro...

Embodiment 2

[0046] The selection of embodiment 2 precipitation agent

[0047] The doped F 0.05 mn 0.05 sn 0.90 o 2 Nano powder, after XRD test, the results are as follows: figure 1 shown.

[0048] figure 1 For doped SnO prepared with different precipitants 2 The XRD pattern of the nanopowder, after being mixed with SnO 2 Compared with the standard card (PDF#-1445), the samples prepared with NaOH, KOH and ammonia water as precipitants all have a tetragonal rutile structure. Among them, the diffraction peaks on (220) and (002) crystal planes of the sample with ammonia water as the precipitant are not very clear, and the diffraction peaks on the (220) and (002) crystal planes of the sample with KOH as the precipitant are slightly more obvious, but in the The samples with NaOH as the precipitant have the clearest diffraction peaks on these two crystal planes, and the peak heights are the highest. At the same time, the diffraction peaks on the three crystal planes of the characteristic...

Embodiment 3

[0049] The selection of embodiment 3 dispersants

[0050] The other conditions of the experiment are certain (the molar ratio of each atom: F:Mn:Sn=0.05:0.05:0.90, pH=9, the hydrothermal temperature is 180°C, the hydrothermal time is 6 h, the precipitant is NaOH), and different Dispersant Preparation of Doped SnO 2 Nano powder, through SEM test such as figure 2 shown.

[0051] Depend on figure 2 As shown, the sample agglomeration without adding dispersant is particularly serious, wherein sodium stearate not only does not reach the dispersion effect, the sample agglomeration of its preparation is more serious than the sample without adding dispersant, is basically a block structure, adding SDS (12 Sodium alkylsulfonate) and TPAB (tetrapropylammonium bromide) as the dispersant have a coral-like appearance, but the dispersion effect is not very obvious. The surface of the sample prepared with PEG-600 as the dispersant looks like There is a layer of film covering the surface...

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Abstract

The invention provides F / Mn co-doped SnO2 nanopowder and the preparation method thereof, and belongs to the technical field of co-doped SnO2 nanopowder. The preparation method includes the following steps that first water is added to a reactor and citric acid is added to adjust pH while the temperature is raised to 40-60 DEG C with stirring, then SnCl4 5H2O is added until dissolved, additionally, MnSO4 H2O and NH4F are added to the above solution, after stirring is continued for 10 minutes, a precipitating agent is gradually added to the above solution and stirring is continued for another 30 minutes, subsequently, the pH is adjusted to 5-11, and a dispersing agent is further added. The resulting mixture is subjected to a hydrothermal reaction at a temperature of 140-200 DEG C. After reacting for 2-36 hours, the product is washed with distilled water and anhydrous ethanol until no Cl- is detected. Finally, the F / Mn co-doped SnO2 nanopowder is obtained by subsequent drying, calcining and milling. The F / Mn co-doped SnO2 nanopowder with a size of about 12 nanometers and uniform dispersion can be prepared by the preparation method.

Description

technical field [0001] The present invention belongs to co-doped SnO 2 Nano powder technology field, especially related to a kind of F / Mn co-doped SnO 2 Nanopowder and its preparation method. Background technique [0002] As an n-type wide bandgap metal oxide semiconductor nanomaterial, nano-tin dioxide has been widely used in various fields, such as catalysts, conductive ceramics, sensors, displays, solar cells and other fields. Since the nano-tin dioxide powder has a large relative area, the surface oxygen defect is also large, and the oxygen coordination number is relatively low, which is very conducive to the generation of electron carriers, so it is beneficial to improve the optical band gap of tin dioxide. It is also beneficial to improve its conductivity. [0003] Due to the special morphology and special nanostructure of nano-tin dioxide material, it has superior performance in optics, catalysis, gas sensing, electricity, etc. Therefore, a large number of experts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/02B82Y30/00
CPCB82Y30/00C01G19/02C01P2002/72C01P2002/85C01P2004/03C01P2004/04C01P2004/64
Inventor 吕维忠吴志军
Owner SHENZHEN UNIV
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