CN104925852B - A method for preparing cadmium sulfide-silver sulfide heterojunction nanomaterials in solid state - Google Patents
A method for preparing cadmium sulfide-silver sulfide heterojunction nanomaterials in solid state Download PDFInfo
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- CN104925852B CN104925852B CN201510269649.8A CN201510269649A CN104925852B CN 104925852 B CN104925852 B CN 104925852B CN 201510269649 A CN201510269649 A CN 201510269649A CN 104925852 B CN104925852 B CN 104925852B
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- LVQNPSAQURQSSR-UHFFFAOYSA-N [Ag]=S.[S-2].[Cd+2] Chemical compound [Ag]=S.[S-2].[Cd+2] LVQNPSAQURQSSR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 title abstract description 19
- 239000007787 solid Substances 0.000 title description 2
- 239000000463 material Substances 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 239000002184 metal Substances 0.000 claims abstract description 6
- 150000001661 cadmium Chemical class 0.000 claims abstract description 3
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract 3
- 150000002910 rare earth metals Chemical class 0.000 claims abstract 3
- 150000001408 amides Chemical class 0.000 claims 1
- 229910052793 cadmium Inorganic materials 0.000 claims 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 238000005987 sulfurization reaction Methods 0.000 claims 1
- 239000007790 solid phase Substances 0.000 abstract description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 abstract description 8
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract 1
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 7
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 4
- 229940071536 silver acetate Drugs 0.000 description 4
- 238000003746 solid phase reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052946 acanthite Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 3
- 229940056910 silver sulfide Drugs 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 1
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 description 1
- 229910000331 cadmium sulfate Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Luminescent Compositions (AREA)
Abstract
Description
技术领域technical field
本发明涉及一种固相制备硫化镉-硫化银异质结纳米材料的方法，属于纳米材料制备领域。The invention relates to a method for preparing cadmium sulfide-silver sulfide heterojunction nanomaterials in solid phase, and belongs to the field of nanomaterial preparation.
背景技术Background technique
近年来，纳米材料由于其本身所具有的独特的物理化学特性而受到了科研工作者的广泛关注。硫化镉作为一种十分重要的半导体纳米材料，因其具有特异的光、电、热、磁等性质，而在半导体发光器件、非线性光学材料、光催化等领域表现出巨大的应用前景。然而，硫化镉纳米材料极易发生光腐烛现象，进而影响到它的性能和实际应用。研究发现，利用异质结构可以在一定程度上改善其光腐烛现象，所以利用硫化镉的可见光响应特点，与其它物理化学性能稳定的半导体材料构建异质结构是常见的硫化物异质结思路。其中，纳米级硫化银材料因产生较大的比表面以及量子尺寸效应，在光吸收、传感、催化等方面有更为广泛而又重要的潜在性应用，为此将硫化镉与硫化银复合可有效地改善其光腐烛现象。In recent years, nanomaterials have attracted extensive attention of researchers because of their unique physical and chemical properties. As a very important semiconductor nanomaterial, cadmium sulfide has great application prospects in the fields of semiconductor light-emitting devices, nonlinear optical materials, and photocatalysis because of its specific optical, electrical, thermal, and magnetic properties. However, cadmium sulfide nanomaterials are prone to photocorrosion, which affects its performance and practical application. Studies have found that the use of heterostructures can improve the phenomenon of light decay to a certain extent. Therefore, using the visible light response characteristics of cadmium sulfide to construct heterostructures with other semiconductor materials with stable physical and chemical properties is a common idea for sulfide heterojunctions. . Among them, nanoscale silver sulfide materials have more extensive and important potential applications in light absorption, sensing, and catalysis due to their large specific surface area and quantum size effect. For this reason, cadmium sulfide and silver sulfide composite It can effectively improve its light rot phenomenon.
目前，制备硫化镉-硫化银异质结纳米材料的方法包括水热法和微波法等，然而这些方法涉及到实验条件苛刻、能耗高等不足，因而开发一种简单、高产、环境友好的合成方法仍然十分迫切。低热固相化学法具有操作简单、成本低、产量高和环境友好等优点，已经成为合成纳米材料的一种有效方法。At present, the methods for preparing cadmium sulfide-silver sulfide heterojunction nanomaterials include hydrothermal method and microwave method, etc. However, these methods involve harsh experimental conditions and high energy consumption. Therefore, the development of a simple, high-yield, and environmentally friendly synthesis method is still urgent. Low-heat solid-phase chemistry has become an effective method for the synthesis of nanomaterials due to its advantages of simple operation, low cost, high yield, and environmental friendliness.
发明内容Contents of the invention
本发明的目的在于提供一种固相制备硫化镉-硫化银异质结纳米材料的方法，是以硫代乙酰胺为硫源采用低热固相化学反应来制备硫化镉-硫化银异质结纳米材料。该方法所制备纳米材料有效地改善了硫化镉的光腐烛现象，并实现了硫化镉与硫化银的复合。The object of the present invention is to provide a method for solid-phase preparation of cadmium sulfide-silver sulfide heterojunction nanomaterials, which uses thioacetamide as the sulfur source and adopts low-heat solid-phase chemical reaction to prepare cadmium sulfide-silver sulfide heterojunction nanomaterials. Material. The nanometer material prepared by the method effectively improves the photocorrosion phenomenon of cadmium sulfide, and realizes the composite of cadmium sulfide and silver sulfide.
本发明公开了一种固相制备硫化镉-硫化银异质结纳米材料的方法。本发明的方法是用金属镉盐、金属银盐和硫代乙酰胺一起研磨发生反应进而实现硫化镉-硫化银异质结纳米材料的低热固相化学制备。The invention discloses a method for preparing cadmium sulfide-silver sulfide heterojunction nanomaterials in solid state. The method of the invention is to use the metal cadmium salt, the metal silver salt and the thioacetamide to grind and react together to realize the low-heat solid-phase chemical preparation of the cadmium sulfide-silver sulfide heterojunction nanometer material.
本发明以硫代乙酰胺为硫源固相制备硫化镉-硫化银异质结纳米材料的方法，操作简单、不使用溶剂、高产率、成本低，为硫化镉基复合材料的制备提供了一种新的思路。The method of the present invention uses thioacetamide as a sulfur source to prepare cadmium sulfide-silver sulfide heterojunction nanomaterials in solid phase, which is simple to operate, does not use solvents, has high yield and low cost, and provides a method for the preparation of cadmium sulfide-based composite materials. A new way of thinking.
附图说明Description of drawings
图1为固相制备硫化镉-硫化银异质结纳米材料的透射电镜图。Figure 1 is a transmission electron microscope image of a cadmium sulfide-silver sulfide heterojunction nanomaterial prepared in solid phase.
具体实施方式detailed description
固相制备硫化镉-硫化银异质结纳米材料的方法，按以下步骤进行：The method for solid-phase preparation of cadmium sulfide-silver sulfide heterojunction nanomaterials is carried out in the following steps:
具体实施方式1：准确称取0.0099摩尔的醋酸镉置于玛瑙研钵中，将其充分研细后加入0.01摩尔的硫代乙酰胺，研磨60分钟混合均匀后加入0.0002摩尔醋酸银，再将其充分研磨60分钟并放置3小时以确保固相反应完全。用去离子水和无水乙醇将其洗涤、抽滤，于干燥箱中60度干燥2小时即得硫化镉-硫化银异质结纳米材料。Embodiment 1: Accurately weigh 0.0099 moles of cadmium acetate and place it in an agate mortar, add 0.01 moles of thioacetamide after it is fully ground, grind for 60 minutes and mix evenly, add 0.0002 moles of silver acetate, then mix it Grind thoroughly for 60 minutes and let stand for 3 hours to ensure complete solid phase reaction. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60°C for 2 hours to obtain the cadmium sulfide-silver sulfide heterojunction nanomaterial.
具体实施方式2：准确称取0.0099摩尔的氯化镉置于玛瑙研钵中，将其充分研细后加入0.01摩尔的硫代乙酰胺，研磨60分钟混合均匀后加入0.0002摩尔醋酸银，再将其充分研磨60分钟并放置3小时以确保固相反应完全。用去离子水和无水乙醇将其洗涤、抽滤，于干燥箱中60度干燥2小时即得硫化镉-硫化银异质结纳米材料。Embodiment 2: Accurately weigh 0.0099 moles of cadmium chloride and place it in an agate mortar, add 0.01 moles of thioacetamide after it is fully ground, grind for 60 minutes and mix uniformly, add 0.0002 moles of silver acetate, and then It was thoroughly ground for 60 minutes and left for 3 hours to ensure complete solid phase reaction. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60°C for 2 hours to obtain the cadmium sulfide-silver sulfide heterojunction nanomaterial.
具体实施方式3：准确称取0.0099摩尔的硫酸镉置于玛瑙研钵中，将其充分研细后加入0.01摩尔的硫代乙酰胺，研磨60分钟混合均匀后加入0.0002摩尔醋酸银，再将其充分研磨60分钟并放置3小时以确保固相反应完全。用去离子水和无水乙醇将其洗涤、抽滤，于干燥箱中60度干燥2小时即得硫化镉-硫化银异质结纳米材料。Specific embodiment 3: Accurately weigh 0.0099 moles of cadmium sulfate and place it in an agate mortar, add 0.01 moles of thioacetamide after it is fully ground, grind for 60 minutes and mix evenly, add 0.0002 moles of silver acetate, and then Grind thoroughly for 60 minutes and let stand for 3 hours to ensure complete solid phase reaction. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60°C for 2 hours to obtain the cadmium sulfide-silver sulfide heterojunction nanomaterial.
具体实施方式4：准确称取0.0099摩尔的硝酸镉置于玛瑙研钵中，将其充分研细后加入0.01摩尔的硫代乙酰胺，研磨60分钟混合均匀后加入0.0002摩尔醋酸银，再将其充分研磨60分钟并放置3小时以确保固相反应完全。用去离子水和无水乙醇将其洗涤、抽滤，于干燥箱中60度干燥2小时即得硫化镉-硫化银异质结纳米材料。Specific embodiment 4: Accurately weigh 0.0099 moles of cadmium nitrate and place it in an agate mortar, add 0.01 moles of thioacetamide after it is fully ground, grind for 60 minutes and mix evenly, add 0.0002 moles of silver acetate, then mix it Grind thoroughly for 60 minutes and let stand for 3 hours to ensure complete solid phase reaction. Wash it with deionized water and absolute ethanol, filter it with suction, and dry it in a drying oven at 60°C for 2 hours to obtain the cadmium sulfide-silver sulfide heterojunction nanomaterial.
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| CN107029756A (en) * | 2017-06-01 | 2017-08-11 | 新疆大学 | A kind of method that solid phase prepares zinc sulphide silver sulfide heterojunction composite |
| CN110560188B (en) * | 2019-09-19 | 2021-09-28 | 济南大学 | Preparation method of multi-stage sample injection micro-fluidic chip for synthesizing Ag/Ag2S/CdS heterojunction |
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