CN111321394A - Method for preparing nano flaky cobalt phosphide by vapor deposition - Google Patents
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
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Abstract
The invention provides a method for preparing nano flaky cobalt phosphide by vapor deposition, which comprises the following steps: weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A; dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B; pouring the B into the A, and standing for 12-24h at room temperature; after centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, and putting the precursor and the phosphorus source together into a tubular furnace filled with protective gas; and (4) carrying out a temperature rise process on the tubular furnace according to a temperature rise curve under the atmosphere protection condition, reacting for 2-5 h at 300-500 ℃, and cooling to room temperature to obtain the nano flaky cobalt phosphide. The invention has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing; the raw material is nitrate, chloride or acetate of cobalt, and the price of the raw material is low.
Description
Technical Field
The invention relates to the technical field of preparation of nano flaky cobalt phosphide, in particular to a method for preparing nano flaky cobalt phosphide by vapor deposition.
Background
Cobalt phosphide has good metallic properties and good electrical conductivity, and has been widely studied in many fields, such as use as an electrocatalyst for water cracking, use as a negative electrode material for lithium ion batteries, use as a catalyst for hydrodesulfurization reactions, and the like. The shape of the cobalt phosphide synthesized in China at present is mostly nanospheres, nanowires, nanospheres and the like. For example, chinese patent CN201910027895.0 discloses a nitrogen-doped cobalt phosphide/nanocarbon composite material, a preparation method and an application thereof, which is characterized in that a phosphorus source, a cobalt source and a monomer for synthesizing gel are polymerized under a polymerization assistant to obtain a double-network hydrogel; freeze drying the double-network hydrogel to obtain dry gel; the xerogel is calcined under the protective atmosphere at 750-1000 ℃; and compounding the calcined product with a nano carbon material to obtain the cobalt phosphide/nano carbon composite material. Chinese patent 201811655267.9 discloses a catalyst for the electrolysis of water to produce hydrogen by cobalt phosphide nano-wire and a preparation method thereof, which is characterized in that cobalt sulfate urea, water and glycol are added into a reaction kettle for full dissolution; heating the reaction kettle to 130-170 ℃ for hydrothermal reaction to obtain a cobalt phosphide precursor; after the reaction kettle is naturally cooled to normal temperature, adding ammonia water, ethylene glycol and molybdenum trioxide; heating the reaction kettle to 110-135 ℃ until solid cobalt phosphide is obtained; calcining the obtained solid cobalt phosphide for 2-3 hours in an environment of 500-600 ℃ to obtain a finished product. The above patents all have the disadvantages that the reaction temperature is too high, the appearance of the cobalt phosphide product is not favorable for the electrolyte to enter the electrode material in the electrochemical application, the ion diffusion distance is too long, and the like, and the purposes of saving the productivity and increasing the yield are not favorable for the practical application.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing nano flaky cobalt phosphide by vapor deposition, so as to solve the problems in the background technology.
The technical problem solved by the invention is realized by adopting the following technical scheme: a method for preparing nano flaky cobalt phosphide by vapor deposition comprises the following steps:
weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A;
dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B;
pouring the B into the A, stirring to form a uniform solution, and standing at room temperature for 12-24 h;
after centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; the flaky precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing;
step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, placing the precursor and the phosphorus source into a tubular furnace filled with protective gas, placing the phosphorus source at the upstream of the tubular furnace, and placing the precursor at the downstream;
and (4) setting a heating curve, enabling the tubular furnace to perform a heating process according to the heating curve under the atmosphere protection condition, reacting for 2-5 hours at 300-500 ℃, enabling the evaporated phosphorus element to perform a vapor deposition reaction on the surface of a precursor, converting the flaky precursor into flaky cobalt phosphide, and cooling to room temperature to obtain the nano flaky cobalt phosphide.
Further, in the step (1), the cobalt source is at least one of nitrate, chloride and acetate of cobalt.
Further, the solvent in the step (1) is at least one of deionized water and methanol.
Further, in the step (3), the phosphorus source is a phosphorus simple substance.
Further, the protective gas in the step (4) is at least one of argon and nitrogen.
Further, the temperature rise rate in the step (4) is (3-6) ° c/min.
Compared with the prior art, the invention has the beneficial effects that:
1. the flaky precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has a stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing; the raw material is nitrate, chloride or acetate of cobalt, and the price of the raw material is low.
2. The nano flaky cobalt phosphide prepared by the invention has a stable morphology structure, the orderly arranged nano arrays enable electrolyte to easily enter the electrode, the flaky structure greatly shortens the ion diffusion length, and the enhancement of Faraday redox reaction is facilitated.
3. The preparation method disclosed by the invention is easy to operate in a process section, relatively low in reaction temperature and suitable for industrial production and application in the fields of new energy storage such as super capacitors, fuel cells and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the nano-flake cobalt phosphide of the present invention.
Detailed Description
Example 1
A method for preparing nano flaky cobalt phosphide by vapor deposition comprises the following steps:
weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A;
dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B;
pouring the B into the A, stirring to form a uniform solution, and standing at room temperature for 12-24 h; the cobalt source is cobalt chloride; the solvent is deionized water.
After centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; the lamellar precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing.
Step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, placing the precursor and the phosphorus source into a tubular furnace filled with protective gas, placing the phosphorus source at the upstream of the tubular furnace, and placing the precursor at the downstream; the phosphorus source is a phosphorus simple substance.
Setting a temperature rise curve, enabling the tubular furnace to perform a temperature rise process according to the temperature rise curve under the atmosphere protection condition, reacting for 4 hours at 400 ℃, enabling the evaporated phosphorus element to perform vapor deposition reaction on the surface of a precursor, converting the flaky precursor into flaky cobalt phosphide, and cooling to room temperature to obtain the nano flaky cobalt phosphide; the protective gas is nitrogen; the temperature rise rate was 3 ℃ per minute.
Example 2
A method for preparing nano flaky cobalt phosphide by vapor deposition comprises the following steps:
weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A;
dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B;
pouring the B into the A, stirring to form a uniform solution, and standing at room temperature for 12-24 h; the cobalt source is cobalt acetate; the solvent is methanol.
After centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; the lamellar precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing.
Step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, placing the precursor and the phosphorus source into a tubular furnace filled with protective gas, placing the phosphorus source at the upstream of the tubular furnace, and placing the precursor at the downstream; the phosphorus source is a phosphorus simple substance.
Setting a temperature rise curve, enabling the tubular furnace to perform a temperature rise process according to the temperature rise curve under the atmosphere protection condition, reacting for 2 hours at 300 ℃, enabling the evaporated phosphorus element to perform vapor deposition reaction on the surface of a precursor, converting the flaky precursor into flaky cobalt phosphide, and cooling to room temperature to obtain the nano flaky cobalt phosphide; the protective gas is nitrogen; the temperature rise rate was 5 ℃ per minute.
Example 3
A method for preparing nano flaky cobalt phosphide by vapor deposition comprises the following steps:
weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A;
dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B;
pouring the B into the A, stirring to form a uniform solution, and standing at room temperature for 12-24 h; the cobalt source is nitrate of cobalt; the solvent is deionized water.
After centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; the lamellar precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing.
Step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, placing the precursor and the phosphorus source into a tubular furnace filled with protective gas, placing the phosphorus source at the upstream of the tubular furnace, and placing the precursor at the downstream; the phosphorus source is a phosphorus simple substance.
Setting a temperature rise curve, enabling the tubular furnace to perform a temperature rise process according to the temperature rise curve under the atmosphere protection condition, reacting for 5 hours at 500 ℃, enabling the evaporated phosphorus element to perform vapor deposition reaction on the surface of a precursor, converting the flaky precursor into flaky cobalt phosphide, and cooling to room temperature to obtain the nano flaky cobalt phosphide; the protective gas is argon, and the heating rate is 6 ℃/min.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A method for preparing nano flaky cobalt phosphide by vapor deposition is characterized by comprising the following steps: the method comprises the following steps:
weighing a cobalt source and 2-methylimidazole according to a molar ratio of 1:8, and proportioning the cobalt source and a solvent according to a proportion that 1 mol of cobalt corresponds to 20 ml of solvent to form a solution A;
dissolving weighed 2-methylimidazole in a solvent with the same volume to form a solution B;
pouring the B into the A, stirring to form a uniform solution, and standing at room temperature for 12-24 h;
after centrifugal cleaning, vacuum drying for not less than 12h to obtain a precursor; the flaky precursor nano-array is prepared by standing at room temperature through liquid phase deposition, has stable structure and ordered arrangement, and is beneficial to subsequent synthesis and processing;
step (3), weighing the precursor and a phosphorus source according to a molar ratio of 1:5, placing the precursor and the phosphorus source into a tubular furnace filled with protective gas, placing the phosphorus source at the upstream of the tubular furnace, and placing the precursor at the downstream;
and (4) setting a heating curve, enabling the tubular furnace to perform a heating process according to the heating curve under the atmosphere protection condition, reacting for 2-5 hours at 300-500 ℃, enabling the evaporated phosphorus element to perform a vapor deposition reaction on the surface of a precursor, converting the flaky precursor into flaky cobalt phosphide, and cooling to room temperature to obtain the nano flaky cobalt phosphide.
2. The method for preparing the nano flaky cobalt phosphide by the vapor deposition according to claim 1, wherein the method comprises the following steps: in the step (1), the cobalt source is at least one of nitrate, chloride and acetate of cobalt.
3. The method for preparing the nano flaky cobalt phosphide by the vapor deposition according to claim 1, wherein the method comprises the following steps: the solvent in the step (1) is at least one of deionized water and methanol.
4. The method for preparing the nano flaky cobalt phosphide by the vapor deposition according to claim 1, wherein the method comprises the following steps: and (3) the phosphorus source is a phosphorus simple substance.
5. The method for preparing the nano flaky cobalt phosphide by the vapor deposition according to claim 1, wherein the method comprises the following steps: and (4) the protective gas in the step (4) is at least one of argon and nitrogen.
6. The method for preparing the nano flaky cobalt phosphide by the vapor deposition according to claim 1, wherein the method comprises the following steps: the temperature rise speed in the step (4) is 3-6 ℃ per minute.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112108164A (en) * | 2020-07-27 | 2020-12-22 | 浙江工业大学 | Carbon-coated two-dimensional transition metal phosphide and preparation method and application thereof |
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| CN106000351A (en) * | 2016-05-25 | 2016-10-12 | 北京林业大学 | Preparation and adsorption application of novel micro-porous ball based on ZIF (Co<2+>) metal organic framework material |
| CN107394089A (en) * | 2017-07-31 | 2017-11-24 | 北京理工大学 | A kind of lithium-sulfur cell co-modified diaphragm material of ZIF particles and CNT |
| CN107486165A (en) * | 2017-08-30 | 2017-12-19 | 河南师范大学 | A kind of preparation method of@FP composite adsorbing materials of ZIF 67 and its application in separation and concentration high-salt wastewater containing cadmium |
| CN107824188A (en) * | 2017-10-27 | 2018-03-23 | 广西师范大学 | The preparation method of nickel cobalt layered double hydroxide/graphene elctro-catalyst |
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- 2020-02-28 CN CN202010130123.2A patent/CN111321394A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151336A (en) * | 2014-08-08 | 2014-11-19 | 复旦大学 | Preparation method of metal-organic framework compound with hierarchical pore structure |
| CN106000351A (en) * | 2016-05-25 | 2016-10-12 | 北京林业大学 | Preparation and adsorption application of novel micro-porous ball based on ZIF (Co<2+>) metal organic framework material |
| CN107394089A (en) * | 2017-07-31 | 2017-11-24 | 北京理工大学 | A kind of lithium-sulfur cell co-modified diaphragm material of ZIF particles and CNT |
| CN107486165A (en) * | 2017-08-30 | 2017-12-19 | 河南师范大学 | A kind of preparation method of@FP composite adsorbing materials of ZIF 67 and its application in separation and concentration high-salt wastewater containing cadmium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112108164A (en) * | 2020-07-27 | 2020-12-22 | 浙江工业大学 | Carbon-coated two-dimensional transition metal phosphide and preparation method and application thereof |
| CN112108164B (en) * | 2020-07-27 | 2023-07-14 | 浙江工业大学 | Carbon-coated two-dimensional transition metal phosphide as well as preparation method and application thereof |
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