CN110803723A - Solid-phase synthesis method of high-purity nickel disulfide nanospheres - Google Patents
Solid-phase synthesis method of high-purity nickel disulfide nanospheres Download PDFInfo
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Abstract
A solid phase synthesis method of high-purity nickel disulfide nanospheres comprises the following steps: (1) mixing nickel formate solid and sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature to uniformly mix the nickel formate and the sulfur powder; (2) putting the mixed powder in the step (1) into a quartz beaker, then putting the quartz beaker containing the mixed powder into a high-pressure reaction kettle under the atmospheric atmosphere, and sealing the reaction kettle; (3) placing the sealed high-pressure reaction kettle in the step (2) in a muffle furnace, heating to 300-550 ℃ at a heating rate of 5 ℃ per minute, and then carrying out pyrolysis and vulcanization at constant temperature for 30 minutes; (4) and (4) naturally cooling the high-pressure reaction kettle calcined in the step (3) to room temperature, and taking out black powder in the reaction kettle to obtain the high-purity nickel disulfide nanosphere material.
Description
Technical Field
The invention relates to a solid-phase synthesis technology of high-purity nickel disulfide nanospheres, belonging to the technical field of preparation of nano materials.
Background
Transition metal sulfides have been widely used in the field of electrochemical energy storage devices in recent years due to their abundant redox active sites, good mechanical and thermal stability, and superior electrical conductivity compared to transition metal oxides. The transition metal sulfide is nanocrystallized, so that the specific surface area of the transition metal sulfide can be effectively increased, the redox active sites are increased, and the transmission distance of charges in the redox process is shortened, thereby greatly improving the electrochemical energy storage performance of the transition metal sulfide. Therefore, transition metal sulfides having nanostructures and methods for producing the same have received extensive attention from researchers in recent years.
At present, transition metal nano sulfides are mainly prepared by a liquid phase method. For example, chinese patent CN109110827A discloses a hydrothermal method for preparing nickel disulfide nanospheres. The preparation method is characterized by dispersing nickel acetate, trisodium citrate and thioacetamide in a mixed solvent in proportion, adding polyvinylpyrrolidone K30, adjusting the pH value of a reaction system to 7-9 by using n-propylamine, and carrying out hydrothermal reaction for 12-24 h at 170-190 ℃ to obtain the nickel disulfide nanospheres. Zhengbao Zha et al reported that polyvinylpyrrolidone K30 and ethylene glycol were added to a mixed solution of nickel nitrate and sodium thiosulfate, and a nickel disulfide nanosphere [ j. mater. chem. B, 2019, 7: 143-149]. The morphology of the nickel disulfide can be regulated and controlled by a hydrothermal method, and nickel disulfide nanoparticles with different morphologies are obtained. The disadvantages of the method are long time consumption, large amount of surfactant used in the preparation process, and large amount of waste water which is difficult to treat, which causes potential harm to the environment. The preparation of nickel disulfide by a solid phase method can avoid the use of a surfactant and the generation of harmful wastewater, but the morphology of the nickel disulfide is difficult to control, and the nickel disulfide with a nano structure is obtained. For example, chinese patent CN1079969C discloses a solid phase preparation method of high purity nickel disulfide powder. The method is characterized in that nickel powder and sulfur powder are mixed and then sealed in a quartz glass tube in a vacuum environment, and the temperature is kept for 72-144 h at 200-700 ℃, so that high-purity nickel disulfide powder is obtained. And Chinese patent CN107799769A discloses a solid phase preparation method of a nano nickel disulfide material. The method is characterized in that nickel powder and sublimed sulfur powder are mechanically ball-milled and mixed in a ball mill, and then are calcined for 0.5-4 hours at 350-500 ℃ under the protection of inert gas, so that the nickel disulfide nano material is obtained. The obtained nickel disulfide nano material has irregular appearance and poor dispersibility. Besides, the method for preparing the nano nickel disulfide by the solid phase method is not reported in patents and literatures. Therefore, in view of the wide application and excellent performance of the nano nickel disulfide in the fields of high-performance electrochemical energy storage devices, photocatalysis, sensors, water treatment and the like, the development of an efficient and green preparation method of the nano nickel disulfide has important value.
Disclosure of Invention
The invention aims to provide a solid-phase synthesis method of high-purity nickel disulfide nanospheres.
The invention relates to a solid-phase synthesis method of high-purity nickel disulfide nanospheres, which comprises the following steps:
(1) mixing nickel formate solid and sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature to uniformly mix the nickel formate and the sulfur powder;
(2) putting the mixed powder in the step (1) into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere;
(3) placing the sealed high-pressure reaction kettle in the step (2) in a muffle furnace, heating to 300-550 ℃ at a heating rate of 5 ℃ per minute, and then carrying out pyrolysis and vulcanization at a constant temperature for 30 minutes;
(4) and (4) naturally cooling the high-pressure reaction kettle calcined in the step (3) to room temperature, taking out the black powder in the reaction kettle, and obtaining the high-purity nickel disulfide nanosphere material without subsequent treatment.
The invention has the advantages that: 1. the nickel formate and the sulfur powder are mixed in a stoichiometric ratio to obtain the high-purity nickel disulfide nanospheres in one step, the yield is close to 100%, and no reagent is wasted in the preparation process.
2. And the melted liquid sulfur is used for separately wrapping nickel nanoparticles generated by the pyrolysis of nickel formate and further vulcanizing the nickel nanoparticles into nickel disulfide, so that the high-purity nickel disulfide nanospheres with good dispersibility can be quickly obtained.
3. No hydrogen sulfide waste gas is generated in the preparation process, no harmful waste liquid is generated, and the preparation process is green and environment-friendly.
4. The preparation process is simple, complex post-treatment is not needed, and the high-purity nickel disulfide nanospheres are obtained in one step after the reaction precursor is sealed and calcined at high temperature.
Drawings
Figure 1 is a Scanning Electron Microscope (SEM) photograph of the high-purity nickel disulfide nanospheres obtained in example 1 of the present invention, figure 2 is a Transmission Electron Microscope (TEM) photograph of the high-purity nickel disulfide nanospheres obtained in example 1 of the present invention, figure 3 is the X-ray powder diffraction (XRD) pattern of the high-purity nickel disulfide nanospheres obtained in example 1 of the invention, figure 4 is a Scanning Electron Microscope (SEM) photograph of the high-purity nickel disulfide nanospheres obtained in example 2 of the present invention, figure 5 is the X-ray powder diffraction (XRD) pattern of the high-purity nickel disulfide nanospheres obtained in example 2 of the invention, figure 6 is a Scanning Electron Microscope (SEM) photograph of the high-purity nickel disulfide nanospheres obtained in example 3 of the present invention, fig. 7 is an X-ray powder diffraction (XRD) pattern of the high-purity nickel disulfide nanospheres obtained in example 3 of the present invention.
Detailed Description
The invention relates to a solid-phase synthesis method of high-purity nickel disulfide nanospheres, which comprises the following steps:
(1) mixing nickel formate solid and sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature to uniformly mix the nickel formate and the sulfur powder;
(2) putting the mixed powder in the step (1) into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere;
(3) placing the sealed high-pressure reaction kettle in the step (2) in a muffle furnace, heating to 300-550 ℃ at a heating rate of 5 ℃ per minute, and then carrying out pyrolysis and vulcanization at a constant temperature for 30 minutes;
(4) and (4) naturally cooling the high-pressure reaction kettle calcined in the step (3) to room temperature, taking out the black powder in the reaction kettle, and obtaining the high-purity nickel disulfide nanosphere material without subsequent treatment.
According to the method, nickel formate is used as a nickel source in the step (1), sulfur powder is used as a vulcanizing agent and a separating agent, and the molar ratio of nickel formate solid to sulfur powder is 1: 2.
According to the method, in the step (2), the nickel formate solid and the sulfur powder are sealed in the high-pressure reaction kettle in the air atmosphere, and the sealing process does not need inert atmosphere protection.
According to the method, the high-pressure reaction kettle in the step (3) is directly placed in a muffle furnace to pyrolyze and vulcanize reactants, so that high-purity nickel disulfide nanospheres are obtained; the pyrolysis and vulcanization temperature is 300-550 ℃, and the pyrolysis and vulcanization time is 30 minutes.
According to the method, the high-pressure reaction kettle calcined in the step (4) is naturally cooled to room temperature, black powder in the reaction kettle is taken out, and the high-purity nickel disulfide nanosphere material is obtained without subsequent treatment.
The method takes nickel formate as a nickel source and sulfur powder as a vulcanizing agent, mixes nickel formate solid and sulfur powder, seals the mixture in a high-pressure reaction kettle, directly carries out pyrolysis vulcanization at the temperature of 300-550 ℃, separately wraps nickel nanoparticles generated by pyrolysis of nickel formate by using molten liquid sulfur, and further vulcanizes the nickel nanoparticles into nickel disulfide, thereby quickly obtaining the high-purity nickel disulfide nanospheres. After the reactants are calcined at high temperature in a closed manner, the high-purity nickel disulfide nanospheres can be obtained without any post-treatment. According to the method, the appearance of the nickel disulfide is regulated without additionally adding a surfactant, any solvent is not required to be added in the reaction process, meanwhile, the nickel formate and the sulfur powder react according to the stoichiometric ratio to generate the high-purity nickel disulfide nanospheres, harmful waste liquid and waste gas are not generated in the preparation process, the yield is close to 100%, and the method is a simple, convenient, efficient and green synthesis method. The method is different from the method disclosed in the Chinese patent CN107799769A in that nickel formate is used as a nickel source, nickel disulfide nanoparticles are obtained without high-energy-consumption mechanical ball milling, inert atmosphere protection is not needed in the preparation process, a complex post-treatment process is not needed, nickel nanoparticles generated by pyrolysis of nickel formate are separately wrapped by liquid sulfur, and the nickel nanoparticles are further vulcanized to obtain high-purity nickel disulfide nanospheres.
The invention is described in further detail below with reference to the following figures and specific embodiments:
example 1: mixing the nickel formate solid and the sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature. And (3) placing the mixed powder into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere. And (3) placing the sealed reaction kettle in a muffle furnace, heating to 450 ℃ at the heating rate of 5 ℃ per minute, and then pyrolyzing and vulcanizing for 30 minutes at constant temperature. And after the high-pressure reaction kettle is naturally cooled to room temperature, taking out the black powder in the reaction kettle to obtain the high-purity nickel disulfide nanosphere material. The yield of the obtained high-purity nickel disulfide nanospheres is 98.5 percent. TEM and SEM pictures show that the prepared nickel disulfide is nanospheres with good dispersibility, and the diameter of the nanospheres is about 80 nm. By comparing the XRD spectrogram of the prepared high-purity nickel disulfide nanosphere with a standard nickel disulfide XRD card (PDF card 83-575), the result shows that the obtained product is pure-phase nickel disulfide.
Example 2: mixing the nickel formate solid and the sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature. And (3) placing the mixed powder into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere. And (3) placing the sealed reaction kettle in a muffle furnace, heating to 300 ℃ at a heating rate of 5 ℃ per minute, and then pyrolyzing and vulcanizing at constant temperature for 30 minutes. And after the high-pressure reaction kettle is naturally cooled to room temperature, taking out the black powder in the reaction kettle to obtain the high-purity nickel disulfide nanosphere material. The yield of the obtained high-purity nickel disulfide nanospheres is 97.9 percent. SEM pictures thereof show that the nickel disulfide prepared is highly agglomerated nanospheres, having a diameter of about 20 nm. By comparing the XRD spectrogram of the prepared high-purity nickel disulfide nanosphere with a standard nickel disulfide XRD card (PDF card 83-575), the result shows that the obtained product is pure-phase nickel disulfide.
Example 3: mixing the nickel formate solid and the sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature. And (3) placing the mixed powder into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere. And (3) placing the sealed reaction kettle in a muffle furnace, heating to 550 ℃ at the heating rate of 5 ℃ per minute, and then pyrolyzing and vulcanizing for 30 minutes at constant temperature. And after the high-pressure reaction kettle is naturally cooled to room temperature, taking out the black powder in the reaction kettle to obtain the high-purity nickel disulfide nanosphere material. The yield of the obtained high-purity nickel disulfide nanospheres is 98.7 percent. SEM pictures show that the prepared nickel disulfide is nanospheres with good dispersibility, and the diameter of the nanospheres is about 100 nm. By comparing the XRD spectrogram of the prepared high-purity nickel disulfide nanosphere with a standard nickel disulfide XRD card (PDF card 83-575), the result shows that the obtained product is pure-phase nickel disulfide.
Claims (5)
1. A solid phase synthesis method of high-purity nickel disulfide nanospheres is characterized by comprising the following steps:
(1) mixing nickel formate solid and sulfur powder according to the molar ratio of 1:2, and grinding for 5 minutes at room temperature to uniformly mix the nickel formate and the sulfur powder;
(2) putting the mixed powder in the step (1) into a quartz beaker, and sealing the quartz beaker in a high-pressure reaction kettle in an air atmosphere;
(3) placing the sealed high-pressure reaction kettle in the step (2) in a muffle furnace, heating to 300-550 ℃ at a heating rate of 5 ℃ per minute, and then carrying out pyrolysis and vulcanization at a constant temperature for 30 minutes;
(4) and (4) naturally cooling the high-pressure reaction kettle calcined in the step (3) to room temperature, taking out the black powder in the reaction kettle, and obtaining the high-purity nickel disulfide nanosphere material without subsequent treatment.
2. The solid-phase synthesis method of the high-purity nickel disulfide nanospheres according to claim 1, wherein in the step (1), nickel formate is used as a nickel source, sulfur powder is used as a vulcanizing agent and a separating agent, and the molar ratio of nickel formate solid to sulfur powder is 1: 2.
3. The method for preparing the high-purity nickel disulfide nanospheres according to claim 1, wherein in the step (2), the nickel formate solid and the sulfur powder are sealed in the high-pressure reaction kettle in an air atmosphere, and the sealing process does not need inert atmosphere protection.
4. The preparation method of the high-purity nickel disulfide nanospheres according to claim 1, wherein the high-pressure reaction kettle in step (3) is directly placed in a muffle furnace to pyrolyze the vulcanization reactant to obtain the high-purity nickel disulfide nanospheres; the pyrolysis and vulcanization temperature is 300-550 ℃, and the pyrolysis and vulcanization time is 30 minutes.
5. The method for preparing the high-purity nickel disulfide nanospheres according to claim 1, wherein the high-pressure reaction kettle calcined in the step (4) is naturally cooled to room temperature, black powder in the reaction kettle is taken out, and the high-purity nickel disulfide nanosphere material is obtained without subsequent treatment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114671472A (en) * | 2022-04-02 | 2022-06-28 | 成都大学 | Preparation method of nickel sulfide nanoparticles for preparing formic acid through electrocatalysis |
| CN115417465A (en) * | 2022-10-19 | 2022-12-02 | 中原工学院 | Nickel disulfide electrode material, preparation method and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114671472A (en) * | 2022-04-02 | 2022-06-28 | 成都大学 | Preparation method of nickel sulfide nanoparticles for preparing formic acid through electrocatalysis |
| CN114671472B (en) * | 2022-04-02 | 2024-03-01 | 成都大学 | Preparation method of nickel sulfide nano particles for preparing formic acid by electrocatalytic reaction |
| CN115417465A (en) * | 2022-10-19 | 2022-12-02 | 中原工学院 | Nickel disulfide electrode material, preparation method and application |
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