CN108840313B - Preparation method of multistage spherical nickel diselenide - Google Patents
Preparation method of multistage spherical nickel diselenide Download PDFInfo
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Abstract
The invention relates to a preparation method of multistage spherical nickel diselenide, which comprises the following specific steps: transferring the mixed solution of the aqueous solution of nickel chloride and diethanol amine into a high-pressure reaction kettle, carrying out heating reaction for 6-16 h at 140-180 ℃, centrifugally washing and vacuum drying the generated product to prepare a flower-shaped nickel hydroxide precursor; and then ultrasonically dispersing the precursor into an aqueous solution, adding a mixed solution of selenium powder and hydrazine hydrate, transferring the mixed solution into a high-pressure reaction kettle, reacting for 12-24 h at the temperature of 80-140 ℃, centrifugally washing, and drying in vacuum to obtain the multistage spherical nickel diselenide. The nickel diselenide provided by the invention has the advantages of simple preparation process, easiness in control of reaction conditions, good repeatability, no need of a template agent, a surfactant and the like, and the obtained product has good uniformity in appearance.
Description
Technical Field
The invention relates to a preparation method of spherical nickel diselenide, in particular to a method for preparing nickel diselenide by a two-step solvothermal method.
Background
Selenide materials are important semiconductor materials, and have excellent performances in the aspects of optics, electricity, heat, magnetism and the like, so that the selenide materials are widely applied to the fields of sensing materials, catalysts, magnetic materials, energy storage materials and the like. Due to the small difference between the valence electron configuration of nickel (3d84s2) and the electronegativity of nickel and selenium, nickel and selenium can form various stoichiometric ratios, and thus nickel exhibits multiple oxidation states (Ni0.85Se、NiSe、NiSe2And Ni3Se2). Wherein, NiSe2Has two structures of T and H: the property of non-magnetic metals is exhibited in the H structure, and the same compounds belong to narrow and indirect bandgap semiconductors in the T structure. Therefore, NiSe2The method has a wide application prospect in the fields of lithium ion batteries, sodium ion batteries, electrocatalysts, dye-sensitized solar cells and the like.
In addition, the structure and the size of the material are closely related to the physical and chemical properties of the material, and the multilevel structure has the advantages of both high active sites of the nano material and the structural stability of the micron material, so that the application of the material in various fields can be promoted to a great extent. Therefore, a novel nickel diselenide material is developed by a simple method, and the application of the nickel diselenide material in various fields is studied in depth, so that the nickel diselenide material has very important application, and the maximum potential of the material can be fully exerted.
Disclosure of Invention
The invention aims to provide a method for preparing multi-stage spherical nickel diselenide by a two-step solvothermal method. The invention uses flower-shaped nickel hydroxide as a precursor, uses selenium powder as a selenium source, and prepares the multi-stage spherical nickel diselenide by a solvothermal method. The method has the advantages of wide raw material source, simple preparation process, easily controlled reaction conditions and good repeatability.
The method for preparing nickel diselenide by the two-step solvothermal method provided by the invention takes soluble nickel salt as a nickel source and selenium powder as a selenium source, and comprises the following specific steps:
1) dissolving soluble nickel salt in a mixed solution of water and a diethanol amine solvent, uniformly stirring, transferring the mixed solution into a high-pressure reaction kettle, reacting for a period of time at a constant temperature, and centrifugally washing and vacuum drying the obtained product to obtain the flower-shaped nickel hydroxide precursor.
2) Ultrasonically dispersing a nickel hydroxide precursor into an aqueous solution, adding a mixed solution of selenium powder and hydrazine hydrate, uniformly stirring, transferring the mixed solution into a high-pressure reaction kettle, reacting at a constant temperature for a period of time, and centrifugally washing and vacuum drying the obtained product to obtain the multistage spherical nickel diselenide.
The nickel salt is nickel nitrate, nickel chloride or nickel sulfate, Ni2+The concentration of (b) is 0.05-0.1 mol/L.
The volume ratio of the water to the diethanolamine solution is 1: 1-1: 5
The heating constant-temperature reaction temperature is 140-180 ℃, and the reaction time is 6-16 h.
The temperature of the second step of solvothermal reaction (selenization reaction) is 80-140 ℃, and the reaction time is 12-24 hours.
The molar ratio of the precursor nickel hydroxide to the selenium powder is 1: 3-1: 5, and the volume of the hydrazine hydrate is 6-16 mL.
The washing method comprises the steps of washing the fabric for three times by deionized water and absolute ethyl alcohol respectively, and drying the fabric for 12-24 hours in vacuum under the pressure of 0.05-0.1 MPa.
The invention is based on a two-step solvothermal method to prepare the spherical nickel diselenide material formed by accumulating nano particles. The preparation method has the advantages of simple preparation process, low requirement on equipment, no need of template agent, high purity of the obtained product, good dispersibility, good repeatability and high uniformity of the product appearance.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of the nickel hydroxide precursor produced in example 1.
Fig. 2 is a Scanning Electron Microscope (SEM) photograph of the nickel hydroxide precursor produced in example 1.
Fig. 3 is an X-ray diffraction (XRD) pattern of nickel diselenide produced in example 1.
Fig. 4 is a Scanning Electron Microscope (SEM) photograph of the nickel diselenide produced in example 1.
Fig. 5 is a Transmission Electron Microscope (TEM) photograph of the nickel diselenide produced in example 1.
Detailed Description
For a better understanding of the present invention, further description is provided by the following figures and examples.
Example 1:
dissolving 1.0mmol of nickel chloride in 12mL of deionized water, adding 12mL of diethanolamine, magnetically stirring for 30 minutes, transferring to a high-pressure reaction kettle, heating and reacting at 180 ℃ for 12 hours, naturally cooling, respectively centrifugally washing with deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 80 ℃ for 12 hours to obtain the flower-shaped nickel hydroxide precursor. Weighing 0.5mmol of flower-shaped nickel hydroxide precursor, ultrasonically dispersing into 60mL of deionized water, then adding 2.0mmol of selenium powder and 12mL of hydrazine hydrate, stirring for 30 minutes, transferring the mixed solution into a 100mL high-pressure reaction kettle, reacting for 24 hours at a constant temperature of 100 ℃, naturally cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively, and drying for 12 hours in vacuum at 80 ℃ to obtain the spherical nickel diselenide.
As shown in FIG. 1, the obtained precursor was Ni (OH)2The diffraction peak corresponds to JCPDS card.47-117.
As shown in FIG. 2, the obtained precursor Ni (OH)2Micron assembled by nano sheetsFlower-like structure with a size of about 3-5 μm.
As shown in FIG. 3, the obtained product is nickel diselenide, the diffraction peak of which corresponds to JCPDS card.47-117 of standard card and has higher purity.
As shown in FIG. 4, the prepared nickel diselenide is of a spherical structure formed by stacking nanoparticles, the size of the nanoparticles is 5-20 nm, and the size of the microspheres is consistent with that of the precursor and is 3-5 μm.
As shown in fig. 5, the transmission electron micrograph further proves that the prepared nickel diselenide has a spherical structure formed by stacking nanoparticles, and the nanoparticles are formed by stacking nanoparticles with the size of about 5 nm.
Example 2:
dissolving 1.0mmol of nickel chloride in 8mL of deionized water, adding 16mL of diethanolamine, magnetically stirring for 30 minutes, transferring to a high-pressure reaction kettle, heating and reacting at 180 ℃ for 12 hours, naturally cooling, respectively centrifugally washing with deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 80 ℃ for 12 hours to obtain the flower-shaped nickel hydroxide precursor. Weighing 0.5mmol of flower-shaped nickel hydroxide precursor, ultrasonically dispersing into 60mL of deionized water, then adding 2.0mmol of selenium powder and 12mL of hydrazine hydrate, stirring for 30 minutes, transferring the mixed solution into a 100mL high-pressure reaction kettle, reacting for 24 hours at a constant temperature of 100 ℃, naturally cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively, and drying for 12 hours in vacuum at 80 ℃ to obtain the spherical nickel diselenide.
Example 3:
dissolving 2.0mmol of nickel chloride in 16mL of deionized water, adding 8mL of diethanolamine, magnetically stirring for 30 minutes, transferring to a high-pressure reaction kettle, heating and reacting at 180 ℃ for 12 hours, naturally cooling, respectively centrifugally washing with the deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 80 ℃ for 12 hours to obtain the flower-shaped nickel hydroxide precursor. Weighing 0.5mmol of flower-shaped nickel hydroxide precursor, ultrasonically dispersing into 60mL of deionized water, then adding 2.0mmol of selenium powder and 12mL of hydrazine hydrate, stirring for 30 minutes, transferring the mixed solution into a 100mL high-pressure reaction kettle, reacting for 24 hours at a constant temperature of 100 ℃, naturally cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively, and drying for 12 hours in vacuum at 80 ℃ to obtain the spherical nickel diselenide.
Example 4:
dissolving 2.0mmol of nickel chloride in 12mL of deionized water, adding 12mL of diethanolamine, magnetically stirring for 30 minutes, transferring to a high-pressure reaction kettle, heating and reacting at 180 ℃ for 12 hours, naturally cooling, respectively centrifugally washing with deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 80 ℃ for 12 hours to obtain the flower-shaped nickel hydroxide precursor. Weighing 0.5mmol of flower-shaped nickel hydroxide precursor, ultrasonically dispersing into 60mL of deionized water, then adding 2.0mmol of selenium powder and 8mL of hydrazine hydrate, stirring for 30 minutes, transferring the mixed solution into a 100mL high-pressure reaction kettle, reacting for 24 hours at a constant temperature of 100 ℃, naturally cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively, and drying for 12 hours in vacuum at 80 ℃ to obtain the spherical nickel diselenide.
Example 5:
dissolving 2.0mmol of nickel chloride in 12mL of deionized water, adding 12mL of diethanolamine, magnetically stirring for 30 minutes, transferring to a high-pressure reaction kettle, heating and reacting at 180 ℃ for 12 hours, naturally cooling, respectively centrifugally washing with deionized water and absolute ethyl alcohol for 3 times, and vacuum drying at 80 ℃ for 12 hours to obtain the flower-shaped nickel hydroxide precursor. Weighing 0.5mmol of flower-shaped nickel hydroxide precursor, ultrasonically dispersing into 60mL of deionized water, then adding 2.0mmol of selenium powder and 16mL of hydrazine hydrate, stirring for 30 minutes, transferring the mixed solution into a 100mL high-pressure reaction kettle, reacting for 24 hours at a constant temperature of 100 ℃, naturally cooling, washing the obtained product with deionized water and absolute ethyl alcohol for 3 times respectively, and drying for 12 hours in vacuum at 80 ℃ to obtain the spherical nickel diselenide.
Claims (2)
1. A preparation method of multi-stage spherical nickel diselenide, which is prepared by a two-step solvothermal method, is characterized by comprising the following steps:
1) dissolving soluble nickel salt in mixed solvent of water and diethanolamine, mixing uniformly, controlling Ni2+The ion concentration is 0.05-0.1 mol/L; then, according to the volume ratio of 1: 1-1: 5 of water to diethanolamineTransferring the mixed solution into an autoclave for 140-180 DEG CoC, reacting for 6-16 h at constant temperature, and centrifugally washing and vacuum drying the generated product to obtain a flower-shaped nickel hydroxide precursor;
2) ultrasonically dispersing the obtained flower-shaped nickel hydroxide precursor into water, then adding a mixed solution of selenium powder and hydrazine hydrate, wherein the molar ratio of the nickel hydroxide precursor to the selenium powder is 1: 3-1: 5, and the volume of the hydrazine hydrate is 6-16 mL, transferring the mixed dispersion into a high-pressure reaction kettle, and reacting at 80-140 DEG CoC, reacting for 12-24 hours at constant temperature, and centrifugally washing and vacuum drying the obtained product to obtain the multistage spherical nickel diselenide;
the soluble nickel salt is nickel nitrate, nickel chloride or nickel sulfate.
2. The method of claim 1, wherein the nickel selenide has a composition of NiSe2(ii) a The structure of the obtained product is microspheres consisting of nano-sized nano-particles, the size of the nano-particles is 5-20 nm, and the size of the microspheres is 3-6 mu m.
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| CN109292832A (en) * | 2018-12-07 | 2019-02-01 | 东华大学 | A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof |
| CN110155958B (en) * | 2019-05-13 | 2022-11-04 | 东华大学 | Hydrangea-shaped Cu 2-x Se nano material and its preparation and application |
| CN110808174B (en) * | 2019-11-29 | 2021-11-02 | 江苏理工学院 | Ni for super capacitor3Se4Method for preparing nano-wire |
| CN110950311B (en) * | 2019-12-13 | 2021-04-23 | 西南大学 | Preparation method of nickel selenide micro-nano flower, product and application thereof |
| CN111085276B (en) * | 2019-12-24 | 2020-12-22 | 西南大学 | Preparation method of echinoid cobalt diselenide nanoparticles, and product and application thereof |
| CN112614992B (en) * | 2020-12-10 | 2022-08-16 | 三峡大学 | Nickel composite positive electrode material of water-based zinc-nickel battery and preparation method of nickel composite positive electrode material |
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| CN102874773B (en) * | 2012-09-10 | 2014-06-25 | 江苏大学 | Preparation method of porous nickel selenide hollow nanospheres |
| CN102826617B (en) * | 2012-09-21 | 2015-05-20 | 中国科学院过程工程研究所 | Spherical nickel hydroxide material and preparation method thereof |
| CN103043630B (en) * | 2013-01-11 | 2014-08-27 | 长沙理工大学 | Preparation method of spherical nickel diselenide powder |
| CN104261490B (en) * | 2014-09-22 | 2016-07-06 | 江苏师范大学 | Two-step method prepares the method for nickel sulfide |
| CN105551810B (en) * | 2016-01-01 | 2018-03-27 | 三峡大学 | A kind of solvothermal preparation method of electrode in situ |
| CN105947995B (en) * | 2016-04-22 | 2018-11-02 | 国家纳米科学中心 | The NiSe of surface selenium-rich2Nanometer sheet, preparation method and the usage |
| CN106430122A (en) * | 2016-10-11 | 2017-02-22 | 中国科学技术大学 | NiSe2 transition metal chalcogenide nanosheet as well as preparation method and application thereof |
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