Method for preparing Zn<2+> doped SnS2 nano-photocatalysis material Sn(1-x)ZnxS2 with microwave hydrothermal method

A technology of sn1-xznxs2 and microwave hydrothermal method, which is applied in the field of preparation of nano-photocatalytic materials, can solve the problems of not too high deposition rate, short preparation cycle, expensive equipment, etc., and achieve short preparation cycle, moderate conditions, and shape uniform effect

Active Publication Date: 2015-11-18
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0006] The currently reported method of preparing nano-SnS materials by doping is mainly the chemical deposition method [ChakrabortyR, BuonassisiT, SinsermsuksakulP, et al.Antimony-DopedTin(II) SulfideThinFilms[J]. Spray pyrolysis method [ReddyNK, ReddyKTR.SnSfilmsforphotovoltaicapplications:PhysicalinvestigationsonsprayedSnxSyfilms[J].PhysicaBCondensedMatter,2005,368(368):25-31.], wherein the raw materials required by the chemical deposition method are easy to obtain, but the deposition rate should not be too high, The residual gas after the reaction is flammable, explosive or toxic; the spray pyrolysis method has a short preparation cycle and good film quality, but the equipment is expensive

Method used

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  • Method for preparing Zn&lt;2+&gt; doped SnS2 nano-photocatalysis material Sn(1-x)ZnxS2 with microwave hydrothermal method
  • Method for preparing Zn&lt;2+&gt; doped SnS2 nano-photocatalysis material Sn(1-x)ZnxS2 with microwave hydrothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) SnCl 4 ·5H 2 Dissolve O in deionized water and prepare solution A with a concentration of 0.5mol / L, press n Sn :n Zn =16:1 Add a certain amount of zinc gluconate into solution A, stir until fully dissolved to obtain solution B, and simultaneously use 1mol / L of HCl or NH 4 ·H 2 O adjusts the pH of solution B to 1, NaS·9H 2 O was dissolved in deionized water to prepare a solution C with a concentration of 0.1 mol / L.

[0027] 2) Dilute the two solutions of B and C according to the element molar ratio n Sn :n S = 1.0:1.0 was mixed to obtain solution D, and magnetically stirred at 26°C for 5 minutes to form a uniform and stable mixed solution E.

[0028] 3) Put the E solution into a microwave hydrothermal reaction kettle, seal the hydrothermal reaction kettle, control the volume filling ratio to 50%, control the reaction temperature at 120°C, and control the reaction time at 15 minutes, and react to obtain the precursor.

[0029] 4) After the reaction kettle was n...

Embodiment 2

[0031] 1) SnCl 4 ·5H 2 O is dissolved in deionized water, and prepared as a solution A with a concentration of 0.8mol / L, press n Sn :n Zn =18:1 Add a certain amount of zinc gluconate into solution A, stir until fully dissolved to obtain solution B, and simultaneously use 1mol / L of HCl or NH 4 ·H 2O adjusts the pH of solution B to 7, NaS·9H 2 O was dissolved in deionized water to prepare solution C with a concentration of 1.5 mol / L.

[0032] 2) Dilute the two solutions of B and C according to the element molar ratio n Sn :n S = Mix at a ratio of 1.5:2 to obtain solution D, and magnetically stir at 26°C for 10 minutes to form a uniform and stable mixed solution E.

[0033] 3) Put the E solution into a microwave hydrothermal reaction kettle, seal the hydrothermal kettle, control the volume filling ratio to 60%, control the reaction temperature at 160° C., and control the reaction time at 30 minutes to obtain the precursor.

[0034] 4) After the reaction kettle was natural...

Embodiment 3

[0036] 1) SnCl 4 ·5H 2 O is dissolved in deionized water, and prepared as a solution A with a concentration of 1.2mol / L, press n Sn :n Zn =20:1 Add a certain amount of zinc gluconate into solution A, stir until fully dissolved to obtain solution B, and simultaneously use 1mol / L of HCl or NH 4 ·H 2 O adjusts the pH of solution B to 9, NaS·9H 2 O was dissolved in deionized water to prepare solution C with a concentration of 2.4mol / L.

[0037] 2) Dilute the two solutions of B and C according to the element molar ratio n Sn :n S =2.5:4.3 ratio mixed to obtain solution D, magnetically stirred at 26°C for 30min to form a uniform and stable mixed solution.

[0038] 3) Put the E solution into a microwave hydrothermal reaction kettle, seal the hydrothermal kettle, control the volume filling ratio to 60%, control the reaction temperature at 200°C, and control the reaction time at 90min to obtain the precursor.

[0039] 4) After the reaction kettle was naturally cooled to room te...

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Abstract

The invention discloses a method for preparing a Zn<2+> doped SnS2 nano-photocatalysis material Sn(1-x)ZnxS2 with a microwave hydrothermal method. The method comprises steps as follows: 1), preparing an Sn source solution A, adding a zinc source, stirring the mixture until the mixture is sufficiently dissolved to obtain a solution B, meanwhile, regulating pH of the solution B in a range from 1 to 9, and preparing a NaS*9H2O solution C with the concentration of 0.1-2.4 mol / L; 2), mixing the solution B and the solution C in proportion to obtain a solution D, and stabilizing the solution D to obtain a solution E; 3), putting the solution E into a microwave hydrothermal reaction kettle, and sealing the hydrothermal kettle for microwave hydrothermal reaction to obtain a precursor; 4), taking out the precursor after the reaction kettle is naturally cooled to the room temperature, and performing centrifugal washing separation and drying to obtain a final product Sn(1-x)ZnxS2 nano-photocatalysis material. The nano-photocatalysis material is applied to organic dye degradation and has excellent photocatalytic degradation performance.

Description

【Technical field】 [0001] The invention relates to the technical field of nano photocatalytic materials, in particular to a preparation method of nano photocatalytic materials. 【Background technique】 [0002] Tin disulfide (SnS 2 ) belongs to IV: VI binary compounds, with CdI 2 type layered structure. Tin sulfide is insoluble in water, but soluble in hot concentrated hydrochloric acid and concentrated nitric acid, and dissolves in hot concentrated hydrochloric acid to form SnCl 2 . This means that tin sulfide has the properties of a weakly acidic substance. [0003] The space group of the crystal structure of tin sulfide belongs to the Pnma group. The lattice parameters are: a=1.1200nm, b=0.3987nm, c=0.4334nm, the tin sulfide structure is formed by two layers superimposed on each other along the axis, and tin ions are added between the two layers of hexagonal close-packed sulfur ions The sandwich structure (S-Sn-S) is composed of six sulfur ions around each tin ion to f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/04A62D3/10
Inventor 殷立雄柴思敏马建中黄剑锋王菲菲张浩张东东孔新刚
Owner SHAANXI UNIV OF SCI & TECH
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