Preparation method of spherical nickel diselenide powder

Abstract

The invention belongs to the technical field of preparation of nano materials, and relates to a preparation method of spherical nickel diselenide powder. The method comprises the following steps: 1) mixing Ni<2+>-containing water soluble salt and simple substance selenium powder in a solvent, ultrasonic oscillation for 20-40 minutes, and uniformly stirring to obtain a reaction solution, wherein the solvent is prepared by mixing ethylenediamine and 60-80 wt% hydrazine hydrate in a volume ratio of 1:(3-6); 2) reacting the reaction solution at 100-180 DEG C in a sealed environment for 12-20 hours; and cooling, washing with ethanol and distilled water 2-3 times, and drying at 60-80 DEG C to obtain the spherical nickel diselenide powder of which the average diameter is 2.8-3.2 mu m. The method provided by the invention does not need to previously prepare any template or use any surfactant, and has the advantages of mild reaction, one-step synthesis and simple technique; and the prepared nickel diselenide has the advantages of regular shape and uniform structure, and is beneficial to subsequent application.

Description

technical field

[0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a method for preparing spherical nickel diselenide powder. Background technique

[0002] Due to their special physical and chemical properties, transition metal chalcogenides have attracted great attention in the field of materials science in the past few decades, and have been widely used in optical recording materials, solar cells, superionic conductor materials, catalysts, sensors and lasers. materials and other fields.

[0003] Nickel diselenide is a typical transition metal chalcogenide. Since nickel diselenide has more special properties in terms of electricity and magnetism, and the composition, crystal structure, crystal shape and size of nanomaterials have a great influence on its properties, the controlled synthesis of nickel diselenide has become The focus of research by scientists. At present, the synthesis methods of nickel diselenide include soli...

Examples

Embodiment 1

[0032] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.3159g (0.004mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1: 3, sonicate for 30min, and stir After uniformity, the reaction solution was transferred to a 25 mL high-pressure reactor with a polytetrafluoroethylene liner, the reactor was sealed, and placed in an oven for reaction at 140° C. for 15 hours. The obtained product is washed with ethanol and distilled water for 2-3 times, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0033] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. figure 1 It is a typical SEM image of the sample in Example 1. It can be clearly see...

Embodiment 2

[0035] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.4738g (0.006mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1:6, and ultrasonically shake for 30min. After stirring evenly, the reaction solution was transferred to a 25mL autoclave lined with polytetrafluoroethylene, and the autoclave was sealed, put into an oven, and reacted at 100°C for 20h. The obtained product is washed with ethanol and distilled water for 2-3 times respectively, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0036] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. figure 2 It is a typical SEM image of the sample in Example 2. It can be clearly...

Embodiment 3

[0038] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.6317g (0.008mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1:4, and ultrasonically shake for 30min. After stirring evenly, the reaction solution was transferred to a 25mL autoclave lined with polytetrafluoroethylene, the autoclave was sealed, and put into an oven to react at 180°C for 10h. The obtained product is washed with ethanol and distilled water for 2-3 times respectively, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0039] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. image 3 It is a typical SEM picture of the sample in Example 3. It can be clearly se...

technical field

[0001] The invention belongs to the technical field of nanomaterial preparation, in particular to a method for preparing spherical nickel diselenide powder. Background technique

[0002] Due to their special physical and chemical properties, transition metal chalcogenides have attracted great attention in the field of materials science in the past few decades, and have been widely used in optical recording materials, solar cells, superionic conductor materials, catalysts, sensors and lasers. materials and other fields.

[0003] Nickel diselenide is a typical transition metal chalcogenide. Since nickel diselenide has more special properties in terms of electricity and magnetism, and the composition, crystal structure, crystal shape and size of nanomaterials have a great influence on its properties, the controlled synthesis of nickel diselenide has become The focus of research by scientists. At present, the synthesis methods of nickel diselenide include soli...

Examples

Embodiment 1

[0032] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.3159g (0.004mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1: 3, sonicate for 30min, and stir After uniformity, the reaction solution was transferred to a 25 mL high-pressure reactor with a polytetrafluoroethylene liner, the reactor was sealed, and placed in an oven for reaction at 140° C. for 15 hours. The obtained product is washed with ethanol and distilled water for 2-3 times, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0033] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. figure 1 It is a typical SEM image of the sample in Example 1. It can be clearly see...

Embodiment 2

[0035] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.4738g (0.006mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1:6, and ultrasonically shake for 30min. After stirring evenly, the reaction solution was transferred to a 25mL autoclave lined with polytetrafluoroethylene, and the autoclave was sealed, put into an oven, and reacted at 100°C for 20h. The obtained product is washed with ethanol and distilled water for 2-3 times respectively, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0036] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. figure 2 It is a typical SEM image of the sample in Example 2. It can be clearly...

Embodiment 3

[0038] Add 0.2379g (0.05mol / L) nickel chloride hexahydrate and 0.6317g (0.008mol) elemental selenium to 20mL of a mixed solvent of ethylenediamine and 80% hydrazine hydrate with a volume ratio of 1:4, and ultrasonically shake for 30min. After stirring evenly, the reaction solution was transferred to a 25mL autoclave lined with polytetrafluoroethylene, the autoclave was sealed, and put into an oven to react at 180°C for 10h. The obtained product is washed with ethanol and distilled water for 2-3 times respectively, and then dried at 60°C-80°C to obtain spherical nickel diselenide powder.

[0039] The morphology of the samples obtained under different conditions was characterized by JEOL JSM-6700F scanning electron microscope (SEM) in Japan, and the phase characterization of the samples obtained under different conditions was carried out by Rigaku D / max 2200 X-ray diffractometer (XRD) in Japan. image 3 It is a typical SEM picture of the sample in Example 3. It can be clearly se...

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