CN113044876A - Preparation method of sea urchin-shaped zinc-cadmium-sulfur material - Google Patents
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Abstract
A method for preparing sea urchin-shaped zinc-cadmium-sulfur material comprises dissolving 3, 3' -diaminodipropylamine in deionized water to obtain solution A; adding zinc acetate dihydrate and cadmium acetate dihydrate into the solution A to obtain a mixed solution B, and adding 4,4' -dipyridyl disulfide serving as a sulfur source into the mixed solution B to obtain a mixed solution C; carrying out hydrothermal reaction on the mixed solution C, respectively centrifugally washing the mixed solution C by deionized water and ethanol, and freeze-drying the washed solution C to obtain echinoid Zn0.3Cd0.7And (4) S material. The invention adopts a one-pot hydrothermal method to synthesize sea urchin-shaped Zn0.3Cd0.7S sulfide, simple preparation process, low cost, high material purity and strong crystallinity. The organic-inorganic hybridization and modification are realized by participating in dialysis reaction, controlling physical and chemical factors and the like. Can be used for preparing single-component tiny crystals and special compound powder with two components or multiple components.
Description
Technical Field
The invention belongs to the field of photocatalytic materials, and particularly relates to a preparation method of a sea urchin-shaped zinc-cadmium-sulfur material.
Background
In the modern society, along with the progress and development of the society, the degree of industrialization and artificial intelligence is higher and higher, the requirement on the used materials is higher and higher, and the traditional materials can not meet the use requirement, so that more and more functional materials and composite materials are developed rapidly. The increasing exhaustion of traditional fossil fuels and the serious environmental pollution caused by the combustion of the traditional fossil fuels prompt people to search clean novel energy, and hydrogen energy is paid much attention as high-efficiency clean energy because of wide application prospect. The hydrogen production method of steam reforming methane, which is commonly used in the industry at present, not only consumes huge energy, but also generates a large amount of carbon dioxide gas. The photocatalytic hydrogen production activity mainly depends on the light absorption capacity of a semiconductor photocatalyst, the separation and migration of photon-generated carriers, the surface reaction kinetics and the like.
ZnS and CdS, which are commonly and commonly used semiconductor materials, are used in the fabrication of light emitting conductor devices. Both have certain use disadvantages. Therefore, considering that Zn and Cd belong to the same subgroup and have similar physicochemical properties, the Zn and Cd are subjected to solid solution replacement of atoms, and on the premise that Zn and Cd belong to the same subgroup and have similar physicochemical propertiesxCd1－xS solid solutions appear in the field of vision of researchers. As a semiconductor material with adjustable band gap, the forbidden band width is gradually reduced from 3.6eV to 2.4eV along with the reduction of Zn content, and the semiconductor material has excellent sunlight response capability (most of visible light and partial ultraviolet light) due to the characteristic of adjustable band gap. In addition, the preparation method has the advantages of convenience and quickness in preparation, low cost, good chemical stability and the like. In the field of optoelectronics, ZnxCd1－xS has great potential and can be applied to the manufacture of high-density optical recording devices, photocatalysis, luminescent devices, fluorescent powder and the like.
In recent years, with ZnxCd1-xS study depth, the researchers know the resultsThe structure and performance are closely related to the preparation method. According to the exploration of people, the Zn is successfully prepared by the conventional methods such as a hydrothermal method, a coprecipitation method, a microemulsion method, a thermal decomposition method and the likexCd1-xS solid solution material. At present, Zn0.3Cd0.7The synthesis method of the S (x is 0.3) material mainly comprises the following steps: coprecipitation of Cd by the method of coprecipitation (Xing C, Zhang Y, Yan W, et al. band structured-controlled solution of Cd1-xZnxS photocatalyst for hydrogen production by water splitting[J]Int.j. hydrogen Energy,2006,31(14):2018-]Solid State Communications,2005,133(3), 145-150-0.1Zn0.9S composites for high visible-light photocatalytic H2-production performance[J]Nanoscale,2012,4(8): 2670-. The coprecipitation method has the advantages of high reaction speed, simple process, easy operation, excellent product quality, higher requirement on temperature, higher energy consumption, easy sintering or melting of the product and difficult control of the reaction. The microemulsion method has the advantages of simple process operation, simple device, convenient operation and uniform particles, but generates a large amount of organic matters, has certain influence on the environment, causes environmental pollution, has relatively difficult control of reaction rate, and needs to increase the treatment of reaction byproducts, so that the reaction cost is increased. The thermal decomposition method has simple reaction operation and high reaction speed, but is easy to cause product agglomeration, and has higher temperature required by the reaction and higher requirements on energy and cost required by production.
Disclosure of Invention
The invention aims to provide a method for preparing a sea urchin-shaped zinc-cadmium-sulfur material with low cost and short period, and the prepared sea urchin-shaped Zn0.3Cd0.7The S material has good crystallinity, novel appearance and excellent performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water and stirring to prepare a solution A with the concentration of 1-5 mmol/L;
step two: 50ml of the solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred to prepare Zn2+And (3) a mixed solution B with the concentration of 0.01-0.05 mol/L, wherein nZn: nCd ═ 3: 7;
step three: taking 2-6 mmol of 4,4' -dipyridyl disulfide as a sulfur source, adding the sulfur source into the mixed solution B, and stirring to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 12-16 h at 120-160 ℃;
step five: after the reaction is finished, centrifugally washing the reaction product by deionized water and ethanol respectively, and freeze-drying the reaction product to obtain echinoid Zn0.3Cd0.7And (4) S material.
The stirring in the first step is magnetic stirring at the rotating speed of 200-500 r/min for 10min at room temperature.
And stirring in the second step is performed for 20-40 min by adopting magnetic stirring.
And the stirring in the third step is carried out for 20-40 min by magnetic stirring at the rotating speed of 200-500 r/min.
And adding the mixed solution C into the polytetrafluoroethylene lining in the step four, wherein the filling ratio of the mixed solution C to the polytetrafluoroethylene lining is 50-70%.
And in the fifth step, deionized water and ethanol are respectively subjected to centrifugal washing for 3-6 times.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts a one-pot hydrothermal method to synthesize sea urchin-shaped Zn0.3Cd0.7S sulfide, simple preparation process, low cost, high material purity and strong crystallinity.
(2) The organic-inorganic hybridization and modification are realized by participating in dialysis reaction, controlling physical and chemical factors and the like. Can be used for preparing single-component tiny crystals and special compound powder with two components or multiple components.
Drawings
FIG. 1 shows Zn in the form of sea urchin prepared in example 20.3Cd0.7XRD diffraction spectrum of SThe abscissa is the angle 2 θ and the ordinate is the intensity.
FIG. 2 shows sea urchin-like Zn prepared in example 20.3Cd0.7SEM image of S.
FIG. 3 is a graph showing the hydrogen production performance obtained in example 2.
Detailed Description
The invention is described in further detail below with reference to the following figures and examples:
example 1:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water, and magnetically stirring at the rotating speed of 350r/min for 10min at room temperature to prepare a solution A with the concentration of 4 mmol/L;
step two: 50ml of the mixed solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred magnetically for 20min to prepare Zn2+A mixed solution B with a concentration of 0.01mol/L, wherein nZn: nCd ═ 3: 7;
step three: adding 3mmol of 4,4' -dipyridyl disulfide serving as a sulfur source into the mixed solution B, and magnetically stirring at the rotating speed of 350r/min for 20min to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 60%, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 12 hours at 140 ℃;
step five: after the reaction is finished, centrifugally washing for 3 times respectively by deionized water and ethanol, and freeze-drying to obtain sea urchin-shaped Zn0.3Cd0.7And (4) S material.
Example 2:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water, and magnetically stirring at the rotating speed of 400r/min for 10min at room temperature to prepare a solution A with the concentration of 2 mmol/L;
step two: 50ml of the mixed solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred magnetically for 40min to prepare Zn2+A mixed solution B with a concentration of 0.03mol/L, wherein nZn: nCd ═ 3: 7;
step three: taking 6mmol of 4,4' -dipyridyl disulfide as a sulfur source, adding the sulfur source into the mixed solution B, and magnetically stirring for 30min at the rotating speed of 400r/min to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 50%, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 16 hours at 160 ℃;
step five: after the reaction is finished, centrifugally washing for 3 times respectively by deionized water and ethanol, and freeze-drying to obtain sea urchin-shaped Zn0.3Cd0.7And (4) S material.
From FIG. 1, it can be seen that the sample prepared in example 2 corresponds to the XRD pattern of the standard card and the standard diffraction patterns of cubic phase ZnS (JCPDS card No. 41-1049) and hexagonal phase CdS (JCPDS card No. 41-1049). The diffraction pattern of ZCS shows a multi-phase characteristic compared to the diffraction patterns of cubic and hexagonal phases. Clearly, the diffraction peaks of the cadmium zinc sulfide compound shift to the low angle and high angle sides, respectively, indicating that the sample is not a compound of zinc sulfide and cadmium sulfide, but a solid solution of zinc sulfide.
As can be seen from FIG. 2, the material prepared in example 2 has a novel morphology and is sea urchin-shaped.
It can be seen from FIG. 3 that the hydrogen production of the sample prepared in example 2 can reach 10.65mmol in one reaction period (4 h).
Example 3:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water, and magnetically stirring at the rotating speed of 500r/min for 10min at room temperature to prepare a solution A with the concentration of 3 mmol/L;
step two: 50ml of the mixed solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred magnetically for 25min to prepare Zn2+A mixed solution B with a concentration of 0.05mol/L, wherein nZn: nCd ═ 3: 7;
step three: taking 5mmol of 4,4' -dipyridyl disulfide as a sulfur source, adding the sulfur source into the mixed solution B, and magnetically stirring at the rotating speed of 500r/min for 35min to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 70%, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 14 hours at 150 ℃;
step five: after the reaction is finished, respectively centrifugally washing the mixture for 3 times by deionized water and ethanol, and then freeze-drying the mixtureDrying to obtain sea urchin-shaped Zn0.3Cd0.7And (4) S material.
Example 4:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water, and magnetically stirring at the rotating speed of 200r/min for 10min at room temperature to prepare a solution A with the concentration of 1 mmol/L;
step two: 50ml of the mixed solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred magnetically for 30min to prepare Zn2+A mixed solution B with a concentration of 0.02mol/L, wherein nZn: nCd ═ 3: 7;
step three: taking 2mmol of 4,4' -dipyridyl disulfide as a sulfur source, adding the sulfur source into the mixed solution B, and magnetically stirring at the rotating speed of 200r/min for 25min to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining according to a filling ratio of 65%, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 15 hours at 120 ℃;
step five: after the reaction is finished, respectively centrifugally washing the reaction product for 5 times by deionized water and ethanol, and then freeze-drying the reaction product to obtain sea urchin-shaped Zn0.3Cd0.7And (4) S material.
Example 5:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water, and magnetically stirring at the rotating speed of 300r/min for 10min at room temperature to prepare a solution A with the concentration of 5 mmol/L;
step two: 50ml of the mixed solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred magnetically for 35min to prepare Zn2+A mixed solution B with a concentration of 0.04mol/L, wherein nZn: nCd ═ 3: 7;
step three: adding 4mmol of 4,4' -dipyridyl disulfide serving as a sulfur source into the mixed solution B, and magnetically stirring at the rotating speed of 300r/min for 40min to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 55%, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 13 hours at 130 ℃;
step five: after the reaction is finished, respectively centrifugally washing for 6 times by deionized water and ethanol, and freeze-drying to obtain sea urchin-shaped Zn0.3Cd0.7And (4) S material.
Claims (6)
1. A preparation method of sea urchin-shaped zinc-cadmium-sulfur material is characterized by comprising the following steps:
the method comprises the following steps: dissolving 3, 3' -diamino dipropylamine in deionized water and stirring to prepare a solution A with the concentration of 1-5 mmol/L;
step two: 50ml of the solution A is added with zinc acetate dihydrate (Zn (Ac) 2.2H 2O) and cadmium acetate dihydrate (Cd (Ac) 2.2H 2O) and stirred to prepare Zn2+And (3) a mixed solution B with the concentration of 0.01-0.05 mol/L, wherein nZn: nCd ═ 3: 7;
step three: taking 2-6 mmol of 4,4' -dipyridyl disulfide as a sulfur source, adding the sulfur source into the mixed solution B, and stirring to obtain a mixed solution C;
step four: adding the mixed solution C into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into an oven to perform hydrothermal reaction for 12-16 h at 120-160 ℃;
step five: after the reaction is finished, centrifugally washing the reaction product by deionized water and ethanol respectively, and freeze-drying the reaction product to obtain echinoid Zn0.3Cd0.7And (4) S material.
2. The method for preparing sea urchin-shaped zinc-cadmium-sulfur material as claimed in claim 1, wherein: the stirring in the first step is magnetic stirring at the rotating speed of 200-500 r/min for 10min at room temperature.
3. The method for preparing sea urchin-shaped zinc-cadmium-sulfur material as claimed in claim 1, wherein: and stirring in the second step is performed for 20-40 min by adopting magnetic stirring.
4. The method for preparing sea urchin-shaped zinc-cadmium-sulfur material as claimed in claim 1, wherein: and the stirring in the third step is carried out for 20-40 min by magnetic stirring at the rotating speed of 200-500 r/min.
5. The method for preparing sea urchin-shaped zinc-cadmium-sulfur material as claimed in claim 1, wherein: and adding the mixed solution C into the polytetrafluoroethylene lining in the step four, wherein the filling ratio of the mixed solution C to the polytetrafluoroethylene lining is 50-70%.
6. The method for preparing sea urchin-shaped zinc-cadmium-sulfur material as claimed in claim 1, wherein: and in the fifth step, deionized water and ethanol are respectively subjected to centrifugal washing for 3-6 times.
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| CN116328791A (en) * | 2023-03-21 | 2023-06-27 | 中南大学 | Photocatalyst, and preparation method and application thereof |
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