Method for synthesizing zinc, cadmium and sulfur solid solution material by two-step process

A solid solution, zinc-cadmium technology, applied in chemical instruments and methods, cadmium compounds, inorganic chemistry, etc., can solve the problems of high energy and cost requirements for production, products prone to sintering or melting, and difficult to control reaction rates, etc. Achieve the effects of controllable grain growth, short preparation period and easy control of reaction conditions

Active Publication Date: 2018-01-09
SHAANXI UNIV OF SCI & TECH
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  • Claims
  • Application Information

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Problems solved by technology

[0005] Currently, Zn 0.5 Cd 0.5 The synthesis methods of S(x=0.5) materials mainly include: co-precipitation method (Xing C, Zhang Y, Yan W, et al.Band structure-controlled solid olution of d1-xZnxS photocatalyst for hydrogen production by water splitting[J].Int .J.Hydrogen Energ.,2006,31(14):2018-2024), microemulsion method (Chen D, Gao L.Microemulsion-mediated synthesis of cadmium zinc sulfide nanocrystals with composition-modulated optical properties[J].Solid State Commun. ,2005,133(3):145-150.), hydrothermal method (Nie Q, Yuan Q, Wang Q, et al.In situ synthesis of Zn x Cd 1-x S nanorod by a hydrothermal route[J].J.Mater.Sci.,2004,39(16-17):5611-5612.), thermal decomposition method (Yu J, Yang B, ChengB.Noble-metal-free carbon nanotube-Cd 0.1 Zn 0.9 S composites for high visible-light photocatalytic H 2 -production performance[J].Nanoscale,2012,4(8):2670-2677.) Among them, the co-precipitation method has fast reaction speed, simple process and easy operation, and excellent product qual

Method used

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  • Method for synthesizing zinc, cadmium and sulfur solid solution material by two-step process
  • Method for synthesizing zinc, cadmium and sulfur solid solution material by two-step process

Examples

Experimental program
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Embodiment 1

[0038] 1) Using zinc acetate dihydrate (Zn(Ac) 2 2H 2 O) and cadmium acetate dihydrate (Zn(Cd) 2 2H 2 O) is raw material (n Zn :n Cd =1:1), weigh 0.5mmol respectively, add to DETA and deionized water (V DETA :V H2O =1:9) in 40ml of mixed solution, magnetic stirring was carried out for 15min to form mixed solution A.

[0039] 2) Using thioacetamide as the sulfur source, weigh 1 mmol, add it into the mixed solution A, perform magnetic stirring for 15 minutes, and perform ultrasonication for 5 minutes to form solution B.

[0040] 3) The solution B is added to the polytetrafluoroethylene lining, the filling ratio is controlled at 30%, the reaction temperature is controlled at 140°C, and the reaction time is controlled at 12h.

[0041] 4) After the reaction is completed, centrifuge and wash 3 times with deionized water and ethanol respectively. After vacuum drying at 40°C for 4 hours, Zn was obtained by grinding 0.5 Cd 0.5 S precursor.

[0042] 5) Zn 0.5 Cd 0.5 Put the...

Embodiment 2

[0046] 1) Using zinc acetate dihydrate (Zn(Ac) 2 2H 2 O) and cadmium acetate dihydrate (Zn(Cd) 2 2H 2 O) is raw material (n Zn :n Cd =1:1), weigh 0.8mmol respectively, add to DETA and deionized water (V DETA :V H2O =1:9) in 40ml of mixed solution, magnetic stirring was carried out for 15min to form mixed solution A.

[0047] 2) Using thioacetamide as the sulfur source, weigh 1.5 mmol, add it into the mixed solution A, perform magnetic stirring for 15 minutes, and perform ultrasonication for 15 minutes to form solution B.

[0048] 3) The solution B is added into the polytetrafluoroethylene lining, the filling ratio is controlled at 35%, the reaction temperature is controlled at 160°C, and the reaction time is controlled at 18h.

[0049] 4) After the reaction is completed, wash by centrifugation with deionized water and ethanol 4 times respectively. After vacuum drying at 50°C for 3 hours, Zn was obtained by grinding 0.5 Cd 0.5 S precursor.

[0050] 5) Zn 0.5 Cd 0.5...

Embodiment 3

[0054] 1) Using zinc acetate dihydrate (Zn(Ac) 2 2H 2 O) and cadmium acetate dihydrate (Zn(Cd) 2 2H 2 O) is raw material (n Zn :n Cd =1:1), weigh 1.0mmol respectively, add to DETA and deionized water (V DETA : V H 2 (0=1:9) mixed solution 40ml, carry out magnetic stirring for 15min to form mixed solution A.

[0055] 2) Use thioacetamide as the sulfur source, weigh 2 mmol, add to the mixed solution A, perform magnetic stirring for 15 minutes, and perform ultrasonication for 30 minutes to form solution B.

[0056] 3) The solution B is added to the polytetrafluoroethylene lining, the filling ratio is controlled at 40%, the reaction temperature is controlled at 180°C, and the reaction time is controlled at 24h.

[0057] 4) After the reaction is completed, centrifuge and wash 6 times with deionized water and ethanol respectively. After vacuum drying at 60°C for 4 hours, Zn was obtained by grinding 0.5 Cd 0.5 S precursor.

[0058] 5) Zn 0.5 Cd 0.5 Put the S precursor in...

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Abstract

The invention discloses a method for synthesizing zinc, cadmium and sulfur solid solution material by a two-step process. The method comprises the following steps of weighing zinc acetate dihydrate and cadmium acetate dihydrate, adding into a mixed solution of DETA and deionized water, stirring to form a mixed solution A; weighing thioacetamide as a sulfur source, adding into the mixed solution A,then stirring and performing ultrasonic treatment in sequence to form a mixed solution B; adding the mixed solution B into a polytetrafluoroethylene lining for hydrothermal reaction; after the completion of the reaction, centrifugally washing the product with deionized water and ethanol respectively for several times, and then drying and grinding to obtain a precursor; subjecting the precursor toa sintering reaction, stopping immediately after the completion of the reaction, and introducing argon gas for protection; when the temperature drops to the room temperature, taking out a sample, andgrinding the sample into powder, namely the zinc, cadmium and sulfur solid solution solid material.

Description

technical field [0001] The present invention relates to Zn 1-x Cd x The preparation method of S material, be specifically related to a kind of two-step synthesis zinc cadmium sulfur solid solution (Zn 0.5 Cd 0.5 S) Method of material. Background technique [0002] Zn 1－x Cd x As a kind of semiconductor photocatalyst with direct wide band gap, S solid solution gradually reduces its band gap from 3.6eV to 2.3eV with the increase of Cd usage. A certain amount of visible light and a part of near ultraviolet light are used in sunlight. Moreover, it has the advantages of cheap and easy to obtain, strong chemical stability and light corrosion resistance, and has attracted widespread attention since it came out. Zn 1－x Cd x S has potential applications in many fields, and is often used in photoluminescent photoconductor devices, photocatalytic degradation of organic matter and photolysis of water to produce hydrogen, phosphors, and other optoelectronic fields. [0003] Zn ...

Claims

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Application Information

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IPC IPC(8): C01G11/00
Inventor 殷立雄张峰李慧敏房佳萌黄剑锋孔新刚程如亮
Owner SHAANXI UNIV OF SCI & TECH
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