CN110127749B - Preparation method of cuprous sulfide nanoflower with copper defects - Google Patents
Preparation method of cuprous sulfide nanoflower with copper defects Download PDFInfo
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- CN110127749B CN110127749B CN201910450346.4A CN201910450346A CN110127749B CN 110127749 B CN110127749 B CN 110127749B CN 201910450346 A CN201910450346 A CN 201910450346A CN 110127749 B CN110127749 B CN 110127749B
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- C01G3/00—Compounds of copper
- C01G3/12—Sulfides
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention relates to a preparation method of cuprous sulfide nanoflower with copper defects, and belongs to the technical field of nanomaterials. Uniformly mixing strong base, a surfactant, elemental copper, hydrazine hydrate, sodium sulfide and water, uniformly heating to 180-220 ℃ under a sealed condition, and reacting at a constant temperature for 22-24 hours to obtain a reaction system; cooling the reaction system to room temperature, performing centrifugal separation, removing supernatant, washing with deionized water until the washing liquid is neutral, and drying to obtain the cuprous sulfide nanoflower. The method has the advantages of mild reaction conditions, high yield, relatively uniform product appearance and good repeatability, the average grain diameter of the prepared cuprous sulfide nano flower is 700 nm-1.9 mu m, and the average grain diameter of the nano sheet forming the nano flower is about 400 nm; the cuprous sulfide nanoflower has a hierarchical structure and copper-containing defects, and can be applied to the fields of photocatalysts, solar cells, electrochemical energy storage devices, sensors and the like.
Description
Technical Field
The invention relates to a preparation method of cuprous sulfide nanoflower with copper defects, and belongs to the technical field of nanomaterials.
Background
The cuprous sulfide is low in price, is an important transition metal sulfide, and is a multifunctional semiconductor material with good chemical stability. The nano cuprous sulfide material has small particle size and large specific surface area, and has incomparable optical, electric and electrochemical properties compared with a block material due to quantum size effect, surface effect and macroscopic quantum tunnel effect, so the cuprous sulfide nano material is widely applied to the fields of photocatalysts, solar cells, electrochemical energy storage devices, sensors and the like, and is widely concerned and researched by people. The cuprous sulfide nano material can be prepared by a plurality of methods, such as a chemical precipitation method, a microwave radiation method, a vapor deposition method, an in-phase method, a sol-gel method, a microemulsion method, a hydrothermal synthesis method, a spray pyrolysis method, an ultrasonic synthesis method and the like. These methods have some disadvantages, such as difficult control of the size or morphology of the product, low yield, harsh reaction conditions, complex preparation process, and relatively high cost.
Disclosure of Invention
The method for preparing the cuprous sulfide nanoflower with the copper defect and the hierarchical structure is characterized by mild reaction conditions, simple operation and high yield, and the prepared cuprous sulfide nanoflower has the characteristics of controllable size, regular shape and the like.
A preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
mixing strong base, a surfactant, elemental copper, hydrazine hydrate, sodium sulfide and water, uniformly mixing, uniformly heating to 180-220 ℃ under a sealed condition at a constant speed, and reacting at a constant temperature for 22-24 hours to obtain a reaction system; and cooling the reaction system to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying to obtain the cuprous sulfide nanoflower.
The strong base is a composite base of potassium hydroxide and sodium hydroxide.
Further, the mass ratio of the potassium hydroxide to the sodium hydroxide is within the range of 2 (1-2).
The surfactant is trimethyl hexadecyl ammonium bromide.
The mass ratio of the strong base to the water is 10 (1-5), the mass ratio of the surfactant to the water is 0.72 (1-5), the mass ratio of the elemental copper to the sodium sulfide is 2 (1-15), the mass ratio of the elemental copper to the water is 0.4 (1-5), and the volume ratio of the hydrazine hydrate to the water is 0.05 (1-5).
The addition amount of the deionized water is based on the full reaction of simple substance copper and salt energy, a powder product cannot be obtained without adding water, the more the product is added, but the excessive water is added, the product has a particle-like or uneven appearance;
the sealing is to prevent evaporation of moisture to ensure more complete reaction and to improve yield.
Preferably, the drying temperature is 30-80 ℃; the yield, the product morphology and the stability of the product can be ensured;
preferably, the elemental copper is copper.
The average particle size of the cuprous sulfide nanoflower is 700 nm-1.9 mu m, and the average particle size of nanosheets forming the nanoflower is 350-600 nm;
the molecular formula of the cuprous sulfide nanoflower is Cu7.2S4；
The invention has the beneficial effects that:
(1) the method takes strong base, surfactant, elemental copper, hydrazine hydrate, salt and water as raw materials to prepare the cuprous sulfide nanoflower under mild conditions, and the process has the advantages of low synthesis temperature, low pressure, high yield, regular product morphology and good repeatability;
(2) the cuprous sulfide nanoflower has a hierarchical structure and copper-containing defects, and can be applied to the fields of photocatalysts, solar cells, electrochemical energy storage devices, sensors and the like;
(3) the method disclosed by the invention is simple to operate, the preparation process is easy to control, the method is suitable for industrial production, and the method is low in production cost and environment-friendly.
Drawings
FIG. 1 is an X-ray diffraction pattern of the cuprous sulfide nanoflower of example 1;
FIG. 2 is a scanning electron micrograph of the cuprous sulfide nanoflower of example 1;
FIG. 3 is a scanning electron micrograph of the cuprous sulfide nanoflower of example 2;
FIG. 4 is a scanning electron micrograph of the cuprous sulfide nanoflower of example 3;
FIG. 5 is a scanning electron micrograph of the cuprous sulfide nanoflower of example 4;
FIG. 6 is a scanning electron micrograph of cuprous sulfide nanoflower of example 5;
FIG. 7 is a scanning electron micrograph of cuprous sulfide nanoflower of example 6;
FIG. 8 is a scanning electron micrograph of cuprous sulfide nanoflower of example 7.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 200 ℃ and reacting at a constant temperature for 24 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying at 30 ℃ to obtain cuprous sulfide nanoflowers; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 5.65:4.35, the mass ratio of strong base (composite base of potassium hydroxide and sodium hydroxide) to water is 10:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:1, the mass ratio of elemental copper to sodium sulfide is 2:1, the mass ratio of elemental copper to water is 0.4:1, and the volume ratio of hydrazine hydrate to water is 0.05: 1;
the X-ray diffraction pattern of the cuprous sulfide nanoflower is shown in figure 1, and as can be seen from figure 1, the product has good crystallinity, and the product and Cu are mixed7.2S4PDF #24-0061 card match, indicating that the resulting product is cuprous sulfide Cu with copper defects7.2S4In addition, the half-peak width of the width reflects the thin thickness of the nanosheets forming the nanoflower, which is consistent with a scanning electron microscope picture;
as shown in fig. 2, a scanning electron microscope image of the cuprous sulfide nanoflower in this embodiment shows that the sample is a nanoflower composed of nanosheets, the average particle size of the nanoflower is about 800 nm, the average particle size of the nanosheets composing the nanoflower is about 400 nm, and the overall morphology is uniform.
Example 2: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 200 ℃ and reacting at a constant temperature for 24 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying at 40 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 5.65:4.35, the mass ratio of strong base (composite base of potassium hydroxide and sodium hydroxide) to water is 10:3, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:3, the mass ratio of elemental copper to sodium sulfide is 2:1, the mass ratio of elemental copper to water is 0.4:3, and the volume ratio of hydrazine hydrate to water is 0.05: 3;
as shown in fig. 3, a scanning electron microscope image of the cuprous sulfide nanoflower in this embodiment shows that, as shown in fig. 3, the sample is a nanoflower composed of nanosheets, the average particle size of the nanoflower is about 1.2 μm, the average particle size of the nanosheets composing the nanoflower is about 600nm, and the overall appearance is uniform.
Example 3: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 200 ℃ and reacting at a constant temperature for 24 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying at 50 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 2:1, the mass ratio of strong base (composite base of potassium hydroxide and sodium hydroxide) to water is 2:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:5, the mass ratio of elemental copper to sodium sulfide is 2:1, the mass ratio of elemental copper to water is 0.4:5, and the volume ratio of hydrazine hydrate to water is 0.05: 5;
as shown in fig. 4, a scanning electron microscope image of the cuprous sulfide nanoflower in this embodiment shows that, as shown in fig. 4, the sample is a nanoflower composed of nanosheets, the average particle size of the nanoflower is about 900 nm, the average particle size of the nanosheets composing the nanoflower is about 450 nm, and the overall morphology is relatively uniform.
Example 4: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 200 ℃ and reacting at a constant temperature for 24 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying at 60 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 1:1, the mass ratio of strong base (composite base of potassium hydroxide and sodium hydroxide) to water is 10:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:1, the mass ratio of elemental copper to sodium sulfide is 2:15, the mass ratio of elemental copper to water is 0.4:1, and the volume ratio of hydrazine hydrate to water is 0.05: 1;
as shown in fig. 5, a scanning electron microscope image of the cuprous sulfide nanoflower in this embodiment shows that, as shown in fig. 5, the sample is a nanoflower composed of nanosheets, the average particle size of the nanoflower is about 700 nm, the average particle size of the nanosheets composing the nanoflower is about 350 nm, and the overall morphology is relatively uniform.
Example 5: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 200 ℃, reacting at a constant temperature for 20 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing solution is neutral, and drying at 80 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 2:1.3, the mass ratio of strong base (composite alkali of potassium hydroxide and sodium hydroxide) to water is 10:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:1, the mass ratio of elemental copper to sodium sulfide is 1:1, the mass ratio of elemental copper to water is 0.4:1, and the volume ratio of hydrazine hydrate to water is 0.05: 1;
the scanning electron microscope image of the cuprous sulfide nanoflower in this example is shown in fig. 6, and as can be seen from fig. 6, the average particle size of the cuprous sulfide nanoflower in this example is about 1.5 μm, and the overall morphology is relatively uniform.
Example 6: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 190 ℃, reacting at a constant temperature for 24 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing solution is neutral, and drying at the temperature of 30 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 2:1.6, the mass ratio of strong base (composite alkali of potassium hydroxide and sodium hydroxide) to water is 5:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:2, the mass ratio of elemental copper to sodium sulfide is 2:7, the mass ratio of elemental copper to water is 0.2:1, and the volume ratio of hydrazine hydrate to water is 0.05: 2;
the scanning electron micrograph of the cuprous sulfide nanoflower in the embodiment is shown in fig. 7, and as can be seen from fig. 7, the average particle size of the cuprous sulfide nanoflower in the embodiment is about 1.7 μm, and the overall morphology is relatively uniform.
Example 7: a preparation method of cuprous sulfide nanoflower containing copper defects comprises the following specific steps:
uniformly mixing strong base (composite alkali of potassium hydroxide and sodium hydroxide), surfactant (trimethyl hexadecyl ammonium bromide CTAB), elemental copper (copper sheet), hydrazine hydrate, sodium sulfide nonahydrate and deionized water, sealing in a polytetrafluoroethylene container, placing the polytetrafluoroethylene container in heating equipment, heating at a constant speed to 220 ℃ and reacting at a constant temperature for 22 hours, cooling to room temperature, performing centrifugal separation, removing supernatant, washing with absolute ethyl alcohol and deionized water until the washing liquid is neutral, and drying at 50 ℃ to obtain cuprous sulfide nanoflower; wherein the mass ratio of potassium hydroxide to sodium hydroxide is 1:1, the mass ratio of strong base (composite base of potassium hydroxide and sodium hydroxide) to water is 10:1, the mass ratio of surfactant (trimethyl cetyl ammonium bromide CTAB) to water is 0.72:1, the mass ratio of elemental copper to sodium sulfide is 2:15, the mass ratio of elemental copper to water is 0.4:1, and the volume ratio of hydrazine hydrate to water is 0.05: 1;
the scanning electron microscope image of the cuprous sulfide nanoflower in the embodiment is shown in fig. 8, and as can be seen from fig. 8, the average particle size of the cuprous sulfide nanoflower in the embodiment is about 1.9 μm, and the overall morphology is relatively uniform.
Claims (4)
1. A preparation method of cuprous sulfide nanoflower containing copper defects is characterized by comprising the following specific steps:
uniformly mixing strong base, a surfactant, elemental copper, hydrazine hydrate, sodium sulfide and water, uniformly heating to 180-220 ℃ under a sealed condition, and reacting at a constant temperature for 22-24 hours to obtain a reaction system; cooling the reaction system to room temperature, centrifugally separating, removing supernatant, washing with deionized water until the washing liquid is neutral, and drying to obtain the cuprous sulfide nanoflower containing copper defects, wherein the surfactant is trimethyl hexadecyl ammonium bromide.
2. The method for preparing cuprous sulfide nanoflower containing copper defects according to claim 1, wherein said method comprises the steps of: the strong base is a composite base consisting of potassium hydroxide and sodium hydroxide.
3. The method for preparing cuprous sulfide nanoflower containing copper defects according to claim 2, wherein said method comprises the steps of: the mass ratio of the potassium hydroxide to the sodium hydroxide is 2 (1-2).
4. The method for preparing cuprous sulfide nanoflower containing copper defects according to claim 1, wherein said method comprises the steps of: the mass ratio of the strong base to the water is 10 (1-5), the mass ratio of the surfactant to the water is 0.72 (1-5), the mass ratio of the elemental copper to the sodium sulfide is 2 (1-15), the mass ratio of the elemental copper to the water is 0.4 (1-5), and the volume ratio of the hydrazine hydrate to the water is 0.05 (1-5).
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| CN110683571B (en) * | 2019-09-27 | 2022-07-01 | 中国科学院合肥物质科学研究院 | Preparation method of flower-shaped cuprous sulfide micron particles |
| CN112536022B (en) * | 2020-11-22 | 2023-04-07 | 重庆交通大学 | CQDS/Cu 2 Preparation method of S nanoflower |
| CN112978798B (en) * | 2021-02-02 | 2022-12-16 | 昆明理工大学 | Method and device for preparing molybdenum oxide nano material with adjustable phase, shape and size |
| CN113394414B (en) * | 2021-06-16 | 2022-06-07 | 福州大学 | Construction of flower-core type S-doped manganese-copper electrocatalyst based on metal polyphenol modified sodium alginate/nano-cellulose composite aerogel |
| CN113788493B (en) * | 2021-09-18 | 2023-09-01 | 乌海瑞森新能源材料有限公司 | Microcapsule composite material, preparation method thereof and application thereof in lithium ion battery |
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| CN102807248B (en) * | 2012-07-13 | 2014-06-25 | 安徽师范大学 | Method for preparing cuprous sulfide nanoarray |
| CN103204536A (en) * | 2013-04-08 | 2013-07-17 | 华东师范大学 | Three-dimensional Cu2S@ZnO nanometer heterostructure semiconductor material and preparation method thereof |
| CN104495908B (en) * | 2014-12-31 | 2016-06-08 | 湖南稀土金属材料研究院 | Cuprous sulfide raw powder's production technology and cuprous sulfide powder body |
| CN106082303A (en) * | 2016-06-07 | 2016-11-09 | 上海工程技术大学 | A kind of CuS material of flower-like structure and its preparation method and application |
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