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Preparation method of dye-sensitized metal sulfide semiconductor nanomaterial

A metal sulfide, dye sensitization technology, applied in chemical instruments and methods, zinc sulfide, cadmium sulfide, etc., can solve the problems of low quantum efficiency, uneven grain dispersion, easy to photocorrosion, etc., to achieve uniform dispersion, High photocatalytic degradation rate and adjustable grain size

Inactive Publication Date: 2013-08-14
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Traditional cadmium sulfide (CdS) semiconductor materials can have a good response in the visible light region, but there are disadvantages such as low quantum efficiency and easy photocorrosion. The development of modified CdS materials has become one of the hotspots in the field of photocatalysis research.
[0003] The ZnS / CdS composite semiconductor material prepared by CanLi et al. in ThinSolidFilms.2006, 513, 99-102 by hydrothermal method, although the grain size is adjustable, but the dispersion of grains is not uniform; NarendraM.Gupta et al. in Journal of In Colloid and Interface Science.2009, 333, 263-268, the ZnS / CdS compound semiconductor material prepared by the in-situ method, although the composition can be adjusted in terms of grain composition, the grains are still not uniformly dispersed

Method used

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  • Preparation method of dye-sensitized metal sulfide semiconductor nanomaterial
  • Preparation method of dye-sensitized metal sulfide semiconductor nanomaterial
  • Preparation method of dye-sensitized metal sulfide semiconductor nanomaterial

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step A: Add 0.02 mol of Zn(NO 3 ) 2 ·6H 2 O, 0.01mol of Cd(NO 3 ) 2 ·4H 2 O and 0.01 mol of Al (NO 3 ) 3 ·9H 2 Dissolve O in 15 ml of de-CO 2 In water, add 0.02 mol of sodium dodecyl sulfate (C 12 H 25 NaO 4 S) Dissolve in 85ml of de-CO 2 In water, stir the two solutions to obtain a mixed salt solution; weigh 4g of NaOH and add it to 50ml to remove CO 2 Prepared in water to 2mol·L –1 NaOH solution;

[0023] Step B: 2mol L prepared in Step A –1 The NaOH solution was added dropwise to the mixed salt solution prepared in step A until the pH value of the system reached 8.0, crystallized at 25 °C for 8 hours, and CO was removed. 2 The obtained slurry was fully centrifuged and washed with water, and dried under vacuum conditions to obtain a sulfonate intercalated hydrotalcite precursor, denoted as Zn 2 Cd 1 Al-LDHs;

[0024] Step C: Place the hydrotalcite precursor prepared in Step B in a vulcanization reaction device, and mix it with H at 90°C. 2 S gas rea...

Embodiment 2

[0030] Step A: Add 0.02 mol of Zn(NO 3 ) 2 ·6H 2 O, 0.01mol of Cd(NO 3 ) 2 ·4H 2 O and 0.01 mol of Al (NO 3 ) 3 ·9H 2 Dissolve O in 15 ml of de-CO 2 In water, add 0.03 mol of sodium dodecyl sulfate (C 12 H 25 NaO 4 S) Dissolve in 85ml of de-CO 2 In water, stir the two solutions to obtain a mixed salt solution; weigh 4g of NaOH and add it to 50ml to remove CO 2 Prepared in water to 2mol·L –1 NaOH solution;

[0031] Step B: 2mol L prepared in Step A –1 The NaOH solution was added dropwise to the mixed salt solution prepared in step A, until the pH value of the system reached 8.0, crystallized at 25 °C for 14 hours, and CO was removed. 2 The obtained slurry is fully washed and centrifuged with water for many times, and dried under vacuum conditions to obtain Zn. 2 Cd 1 Al-LDHs;

[0032] Step C: The hydrotalcite precursor prepared in Step B is placed in a vulcanization reaction device, and is mixed with H at 80 °C. 2 S gas reaction for 60min, H 2 The flow rate ...

Embodiment 3

[0036] Step A: 0.01 mol of Zn(NO 3 ) 2 ·6H 2 O, 0.02mol of Cd(NO 3 ) 2 ·4H 2 O and 0.01 mol of Al (NO 3 ) 3 ·9H 2 Dissolve O in 15 ml of de-CO 2 In water, add 0.04 mol of sodium dodecyl sulfate (C 12 H 25 NaO 4 S) Dissolve in 85ml of de-CO 2 In water, stir the two solutions to obtain a mixed salt solution; weigh 4g of NaOH and add it to 50ml to remove CO 2 Prepared in water to 2mol·L –1 NaOH solution;

[0037] Step B: 2mol L prepared in Step A –1 The NaOH solution was added dropwise to the mixed salt solution prepared in step A until the pH value of the system reached 8.0, crystallized at 25 °C for 20 h, and CO was removed with 2 The obtained slurry is fully washed and centrifuged with water for many times, and dried under vacuum conditions to obtain Zn. 1 Cd 2 Al-LDHs;

[0038] Step C: Place the hydrotalcite precursor prepared in Step B in a vulcanization reaction device, and mix it with H at 90°C. 2 S gas reaction for 90min, H 2 The flow rate of S gas is ...

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Abstract

The invention discloses a preparation method of a dye-sensitized metal sulfide semiconductor nanomaterial, belonging to the technical field of preparation of composite semiconductor materials. Aiming at the defects of the traditional hydrothermal method, an in-situ method and the like, the preparation method comprises the following steps of: introducing metal elements of a composite semiconductor into a hydrotalcite laminate according to adjustability and ion exchangeability of composition and structure of the hydrotalcite laminate; performing reversion; performing alkaline liquid etching; loading dye; and adjusting the molar ratio of the metal elements of the laminate to prepare the dye-sensitized porous ZnCdS composite semiconductor nanomaterial with modulated grain size, composition and band gap value and different Zn/Cd ratio. The prepared dye-sensitized composite semiconductor nanomaterial can optically degrade rhodamine-B molecules in the aqueous solution under the condition of visible light irradiation, thus representing high photocatalytic degradation ratio; and the photocatalytic degradation ratio can be regulated and controlled by adjusting the composition of the metal elements.

Description

technical field [0001] The invention belongs to the technical field of compound semiconductor material preparation, and in particular relates to a preparation method of a dye-sensitized metal sulfide semiconductor nanomaterial. Background technique [0002] Semiconductor photocatalytic materials have attracted extensive attention due to their potential industrial applications in terms of environmental cleanliness and efficient utilization of solar energy. The traditional cadmium sulfide (CdS) semiconductor material can have a good response in the visible light region, but there are shortcomings such as low quantum efficiency and easy photocorrosion. The development of modified CdS materials has become one of the hot spots in the field of photocatalysis research. [0003] CanLi et al. in ThinSolidFilms. 2006, 513, 99-102, the ZnS / CdS composite semiconductor material prepared by hydrothermal method, although the grain size is adjustable, but the grain dispersion is not uniform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26C01G11/02C01G9/08C02F1/30C02F101/38
Inventor 张法智常佳朋刘鑫
Owner BEIJING UNIV OF CHEM TECH
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